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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1040548'
_audit_update_record             
;
2014-12-19 deposited with the CCDC.
2015-02-25 downloaded from the CCDC.
;
_publcif_datablock.id            {f0bf37f7-7b9d-4964-8ec3-af7a53765cd5}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         
;
C25 H23 F12 Fe2 O10
;
_chemical_formula_sum            'C25 H23 F12 Fe2 O10'
_chemical_formula_weight         823.13

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1        '
_symmetry_space_group_name_Hall  '-P 1        '
_symmetry_int_tables_number      2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.507(2)
_cell_length_b                   11.729(3)
_cell_length_c                   16.605(4)
_cell_angle_alpha                102.703(2)
_cell_angle_beta                 96.771(2)
_cell_angle_gamma                112.595(2)
_cell_volume                     1625.0(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5813
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      27.89

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_method    none
_exptl_crystal_F_000             826
_exptl_absorpt_coefficient_mu    1.012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7859
_exptl_absorpt_correction_T_max  0.9055
_exptl_absorpt_process_details   ?

_exptl_special_details           ?

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '0.3 deg wide ω exposures'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         'none (area detector data)'
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_decay_%        0
_diffrn_reflns_number            13069
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         28.22
_reflns_number_total             7052
_reflns_number_gt                5055
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       SMART
_computing_cell_refinement       'SMART, SAINT'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0586P)²+1.0283P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       noref
_refine_ls_number_reflns         7052
_refine_ls_number_parameters     466
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1249
_refine_ls_wR_factor_gt          0.1106
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.073
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.77611(5) 0.33016(4) 0.24754(3) 0.02711(13) Uani 1 1 d . . .
Fe2 Fe 0.79862(5) 0.05556(4) 0.17173(3) 0.02655(13) Uani 1 1 d . . .
O1 O 0.6566(3) 0.2769(2) 0.33714(13) 0.0299(5) Uani 1 1 d . A .
O2 O 0.9145(3) 0.5022(2) 0.34330(14) 0.0328(5) Uani 1 1 d . A .
O3 O 0.6410(3) 0.4258(2) 0.21380(14) 0.0304(5) Uani 1 1 d . . .
O4 O 0.9056(3) 0.4120(2) 0.16794(14) 0.0291(5) Uani 1 1 d . . .
O5 O 0.9347(2) 0.2357(2) 0.24732(13) 0.0275(5) Uani 1 1 d . . .
O6 O 0.9015(2) 0.1132(2) 0.08002(13) 0.0272(5) Uani 1 1 d . . .
O7 O 0.6419(2) 0.1359(2) 0.16229(13) 0.0259(5) Uani 1 1 d . . .
O8 O 0.6462(3) -0.0995(2) 0.08346(14) 0.0307(5) Uani 1 1 d . . .
O9 O 0.7086(3) 0.0008(2) 0.26562(15) 0.0339(5) Uani 1 1 d . . .
O10 O 0.9538(3) -0.0124(2) 0.19785(14) 0.0310(5) Uani 1 1 d . . .
F12 F 1.1072(2) 0.5001(2) 0.07240(14) 0.0454(5) Uani 1 1 d . . .
F6 F 0.6353(2) 0.70489(19) 0.17406(16) 0.0490(6) Uani 1 1 d . . .
F11 F 1.0881(2) 0.6810(2) 0.09855(15) 0.0465(5) Uani 1 1 d . . .
F10 F 1.1998(2) 0.6320(2) 0.19761(15) 0.0527(6) Uani 1 1 d . . .
F5 F 0.4455(3) 0.5170(2) 0.13410(19) 0.0628(7) Uani 1 1 d . . .
C13 C 0.7493(5) 0.4794(4) 0.4407(2) 0.0461(10) Uani 1 1 d . A .
H13 H 0.7291 0.5246 0.4895 0.055 Uiso 1 1 calc R . .
C17 C 1.0431(4) 0.1934(3) 0.0918(2) 0.0281(7) Uani 1 1 d . . .
C19 C 0.4901(4) 0.0680(3) 0.1349(2) 0.0294(7) Uani 1 1 d . . .
C20 C 1.1097(4) 0.1987(3) 0.0146(2) 0.0348(8) Uani 1 1 d . . .
H20A H 1.1588 0.1386 0.0055 0.052 Uiso 1 1 calc R . .
H20B H 1.1881 0.2865 0.0226 0.052 Uiso 1 1 calc R . .
H20C H 1.0258 0.1746 -0.0349 0.052 Uiso 1 1 calc R . .
C21 C 0.8275(4) 0.5806(3) 0.1635(2) 0.0316(7) Uani 1 1 d . . .
H21 H 0.8540 0.6601 0.1503 0.038 Uiso 1 1 calc R . .
C26 C 1.1374(4) 0.2756(3) 0.1720(2) 0.0312(7) Uani 1 1 d . . .
H26 H 1.2468 0.3188 0.1767 0.037 Uiso 1 1 calc R . .
C27 C 1.0812(4) 0.2973(3) 0.2438(2) 0.0298(7) Uani 1 1 d . . .
F4 F 0.5424(3) 0.6144(3) 0.26676(18) 0.0699(8) Uani 1 1 d . . .
C29 C 0.4994(4) -0.1371(3) 0.0630(2) 0.0296(7) Uani 1 1 d . . .
C31 C 0.5792(4) 0.5933(3) 0.1919(3) 0.0404(9) Uani 1 1 d . . .
C32 C 0.6528(4) 0.3510(3) 0.4033(2) 0.0372(8) Uani 1 1 d . . .
C36 C 0.4208(4) -0.0600(3) 0.0880(2) 0.0305(7) Uani 1 1 d . . .
H36 H 0.3100 -0.0997 0.0711 0.037 Uiso 1 1 calc R . .
C38 C 0.9263(4) 0.5187(3) 0.1556(2) 0.0286(7) Uani 1 1 d . . .
C45 C 0.9932(4) -0.0358(3) 0.2667(2) 0.0359(8) Uani 1 1 d . . .
C46 C 1.0813(4) 0.5841(3) 0.1303(2) 0.0362(8) Uani 1 1 d . . .
C49 C 0.4059(4) -0.2738(3) 0.0078(2) 0.0363(8) Uani 1 1 d . . .
H49A H 0.4727 -0.3022 -0.0242 0.055 Uiso 1 1 calc R . .
H49B H 0.3176 -0.2781 -0.0317 0.055 Uiso 1 1 calc R . .
H49C H 0.3665 -0.3302 0.0434 0.055 Uiso 1 1 calc R . .
C53 C 0.7725(5) -0.0247(3) 0.3271(2) 0.0395(8) Uani 1 1 d . . .
C55 C 0.6895(4) 0.5263(3) 0.1906(2) 0.0300(7) Uani 1 1 d . . .
C60 C 0.8767(4) 0.5453(3) 0.4086(2) 0.0374(8) Uani 1 1 d . . .
C62 C 0.9123(5) -0.0391(4) 0.3312(2) 0.0410(9) Uani 1 1 d . . .
H62 H 0.9548 -0.0519 0.3814 0.049 Uiso 1 1 calc R . .
C65 C 1.1347(4) -0.0636(4) 0.2740(3) 0.0457(9) Uani 1 1 d . . .
H65A H 1.1322 -0.1181 0.2194 0.069 Uiso 1 1 calc R . .
H65B H 1.1351 -0.1086 0.3172 0.069 Uiso 1 1 calc R . .
H65C H 1.2292 0.0176 0.2902 0.069 Uiso 1 1 calc R . .
C70 C 1.1864(4) 0.3970(4) 0.3229(2) 0.0408(9) Uani 1 1 d . . .
H70A H 1.1486 0.4640 0.3382 0.061 Uiso 1 1 calc R . .
H70B H 1.2925 0.4359 0.3139 0.061 Uiso 1 1 calc R . .
H70C H 1.1874 0.3570 0.3688 0.061 Uiso 1 1 calc R . .
C73 C 0.6828(5) -0.0450(4) 0.3958(3) 0.0523(11) Uani 1 1 d . . .
H73A H 0.6651 0.0316 0.4185 0.078 Uiso 1 1 calc R . .
H73B H 0.7430 -0.0597 0.4413 0.078 Uiso 1 1 calc R . .
H73C H 0.5819 -0.1202 0.3721 0.078 Uiso 1 1 calc R . .
C1X C 0.3905(4) 0.1379(3) 0.1555(2) 0.0363(8) Uani 1 1 d . . .
H1X1 H 0.4085 0.1710 0.2171 0.055 Uiso 1 1 calc R . .
H1X2 H 0.2801 0.0785 0.1321 0.055 Uiso 1 1 calc R . .
H1X3 H 0.4177 0.2100 0.1307 0.055 Uiso 1 1 calc R . .
C50 C 0.5217(5) 0.2847(4) 0.4457(2) 0.0457(9) Uani 1 1 d D A 1
F1 F 0.5278(13) 0.1763(9) 0.4594(8) 0.029(2) Uiso 0.34 1 d PD A 1
F2 F 0.5201(9) 0.3613(6) 0.5186(4) 0.0257(15) Uiso 0.34 1 d PD A 1
F3 F 0.3776(9) 0.2440(11) 0.3865(6) 0.034(2) Uiso 0.34 1 d PD A 1
F1X F 0.5559(11) 0.2111(9) 0.4849(6) 0.062(3) Uiso 0.34 1 d PD A 2
F2X F 0.4849(10) 0.3713(7) 0.5000(5) 0.049(3) Uiso 0.34 1 d PD A 2
F3X F 0.3832(10) 0.2156(9) 0.3954(6) 0.056(3) Uiso 0.34 1 d PD A 2
F1Y F 0.4971(12) 0.1623(8) 0.4417(6) 0.049(4) Uiso 0.32 1 d PD A 3
F2Y F 0.5553(10) 0.3416(8) 0.5308(5) 0.050(3) Uiso 0.32 1 d PD A 3
F3Y F 0.3919(10) 0.2751(9) 0.4081(6) 0.049(3) Uiso 0.32 1 d PD A 3
C59 C 0.9810(5) 0.6860(4) 0.4587(2) 0.0441(9) Uani 1 1 d D A 1
F7 F 0.8923(8) 0.7580(7) 0.4659(6) 0.0349(17) Uiso 0.34 1 d PD A 1
F8 F 1.0446(12) 0.6966(9) 0.5376(5) 0.029(2) Uiso 0.34 1 d PD A 1
F9 F 1.0927(9) 0.7458(6) 0.4204(4) 0.0308(14) Uiso 0.34 1 d PD A 1
F7X F 0.9383(10) 0.7635(7) 0.4361(5) 0.061(2) Uiso 0.34 1 d PD A 2
F8X F 1.0154(11) 0.7119(9) 0.5421(5) 0.051(3) Uiso 0.34 1 d PD A 2
F9X F 1.1379(8) 0.7209(7) 0.4425(4) 0.0461(17) Uiso 0.34 1 d PD A 2
F7Y F 0.8865(9) 0.7483(8) 0.4919(6) 0.046(2) Uiso 0.32 1 d PD A 3
F8Y F 1.0747(10) 0.6948(9) 0.5217(5) 0.046(3) Uiso 0.32 1 d PD A 3
F9Y F 1.0410(10) 0.7558(7) 0.4088(4) 0.043(2) Uiso 0.32 1 d PD A 3


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 2.039(2) . ?
Fe1 O4 2.054(2) . ?
Fe1 O2 2.094(2) . ?
Fe1 O3 2.106(2) . ?
Fe1 O7 2.178(2) . ?
Fe1 O5 2.188(2) . ?
Fe2 O8 1.964(2) . ?
Fe2 O10 1.976(2) . ?
Fe2 O9 1.977(2) . ?
Fe2 O6 2.007(2) . ?
Fe2 O5 2.015(2) . ?
Fe2 O7 2.055(2) . ?
O1 C32 1.255(4) . ?
O2 C60 1.244(4) . ?
O3 C55 1.255(4) . ?
O4 C38 1.256(4) . ?
O5 C27 1.315(4) . ?
O6 C17 1.272(4) . ?
O7 C19 1.314(4) . ?
O8 C29 1.267(4) . ?
O9 C53 1.277(4) . ?
O10 C45 1.281(4) . ?
F12 C46 1.334(4) . ?
F6 C31 1.325(4) . ?
F11 C46 1.338(4) . ?
F10 C46 1.332(4) . ?
F5 C31 1.341(4) . ?
C13 C32 1.374(5) . ?
C13 C60 1.401(5) . ?
C13 H13 0.9500 . ?
C17 C26 1.413(5) . ?
C17 C20 1.500(4) . ?
C19 C36 1.377(5) . ?
C19 C1X 1.495(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C38 1.392(4) . ?
C21 C55 1.398(4) . ?
C21 H21 0.9500 . ?
C26 C27 1.375(5) . ?
C26 H26 0.9500 . ?
C27 C70 1.487(5) . ?
F4 C31 1.328(4) . ?
C29 C36 1.405(5) . ?
C29 C49 1.506(4) . ?
C31 C55 1.533(5) . ?
C32 C50 1.536(5) . ?
C36 H36 0.9500 . ?
C38 C46 1.535(4) . ?
C45 C62 1.389(5) . ?
C45 C65 1.498(5) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C53 C62 1.398(5) . ?
C53 C73 1.508(5) . ?
C60 C59 1.531(5) . ?
C62 H62 0.9500 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C1X H1X1 0.9800 . ?
C1X H1X2 0.9800 . ?
C1X H1X3 0.9800 . ?
C50 F2 1.344(7) . ?
C50 F1 1.361(8) . ?
C50 F3 1.431(8) . ?
C59 F8 1.335(8) . ?
C59 F9 1.345(7) . ?
C59 F7 1.402(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O4 171.30(9) . . ?
O1 Fe1 O2 85.32(9) . . ?
O4 Fe1 O2 86.80(9) . . ?
O1 Fe1 O3 92.48(9) . . ?
O4 Fe1 O3 83.29(8) . . ?
O2 Fe1 O3 86.16(9) . . ?
O1 Fe1 O7 89.35(8) . . ?
O4 Fe1 O7 98.94(8) . . ?
O2 Fe1 O7 170.72(9) . . ?
O3 Fe1 O7 101.67(9) . . ?
O1 Fe1 O5 103.64(8) . . ?
O4 Fe1 O5 81.32(8) . . ?
O2 Fe1 O5 99.56(9) . . ?
O3 Fe1 O5 163.23(8) . . ?
O7 Fe1 O5 74.32(8) . . ?
O8 Fe2 O10 97.28(9) . . ?
O8 Fe2 O9 94.39(10) . . ?
O10 Fe2 O9 88.02(9) . . ?
O8 Fe2 O6 87.63(9) . . ?
O10 Fe2 O6 89.37(9) . . ?
O9 Fe2 O6 176.88(9) . . ?
O8 Fe2 O5 166.87(9) . . ?
O10 Fe2 O5 94.29(9) . . ?
O9 Fe2 O5 92.18(9) . . ?
O6 Fe2 O5 86.31(9) . . ?
O8 Fe2 O7 88.36(9) . . ?
O10 Fe2 O7 172.11(9) . . ?
O9 Fe2 O7 86.05(9) . . ?
O6 Fe2 O7 96.40(8) . . ?
O5 Fe2 O7 80.77(9) . . ?
C32 O1 Fe1 126.5(2) . . ?
C60 O2 Fe1 126.1(2) . . ?
C55 O3 Fe1 125.7(2) . . ?
C38 O4 Fe1 126.0(2) . . ?
C27 O5 Fe2 121.8(2) . . ?
C27 O5 Fe1 120.71(18) . . ?
Fe2 O5 Fe1 102.88(9) . . ?
C17 O6 Fe2 124.7(2) . . ?
C19 O7 Fe2 123.7(2) . . ?
C19 O7 Fe1 130.6(2) . . ?
Fe2 O7 Fe1 101.92(9) . . ?
C29 O8 Fe2 127.8(2) . . ?
C53 O9 Fe2 128.0(2) . . ?
C45 O10 Fe2 127.7(2) . . ?
C32 C13 C60 121.7(3) . . ?
C32 C13 H13 119.2 . . ?
C60 C13 H13 119.2 . . ?
O6 C17 C26 123.9(3) . . ?
O6 C17 C20 116.5(3) . . ?
C26 C17 C20 119.6(3) . . ?
O7 C19 C36 124.0(3) . . ?
O7 C19 C1X 116.3(3) . . ?
C36 C19 C1X 119.7(3) . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C38 C21 C55 120.3(3) . . ?
C38 C21 H21 119.9 . . ?
C55 C21 H21 119.9 . . ?
C27 C26 C17 124.2(3) . . ?
C27 C26 H26 117.9 . . ?
C17 C26 H26 117.9 . . ?
O5 C27 C26 123.7(3) . . ?
O5 C27 C70 115.9(3) . . ?
C26 C27 C70 120.3(3) . . ?
O8 C29 C36 124.4(3) . . ?
O8 C29 C49 116.6(3) . . ?
C36 C29 C49 119.0(3) . . ?
F6 C31 F4 107.8(3) . . ?
F6 C31 F5 106.6(3) . . ?
F4 C31 F5 107.2(3) . . ?
F6 C31 C55 114.3(3) . . ?
F4 C31 C55 111.1(3) . . ?
F5 C31 C55 109.5(3) . . ?
O1 C32 C13 128.5(3) . . ?
O1 C32 C50 113.5(3) . . ?
C13 C32 C50 118.1(3) . . ?
C19 C36 C29 125.9(3) . . ?
C19 C36 H36 117.0 . . ?
C29 C36 H36 117.0 . . ?
O4 C38 C21 127.5(3) . . ?
O4 C38 C46 113.4(3) . . ?
C21 C38 C46 119.1(3) . . ?
O10 C45 C62 124.2(3) . . ?
O10 C45 C65 115.4(3) . . ?
C62 C45 C65 120.3(3) . . ?
F10 C46 F12 107.1(3) . . ?
F10 C46 F11 107.5(3) . . ?
F12 C46 F11 107.3(3) . . ?
F10 C46 C38 109.9(3) . . ?
F12 C46 C38 111.4(3) . . ?
F11 C46 C38 113.3(3) . . ?
C29 C49 H49A 109.5 . . ?
C29 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C29 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
O9 C53 C62 123.9(3) . . ?
O9 C53 C73 115.4(3) . . ?
C62 C53 C73 120.7(3) . . ?
O3 C55 C21 127.9(3) . . ?
O3 C55 C31 114.0(3) . . ?
C21 C55 C31 118.1(3) . . ?
O2 C60 C13 127.1(3) . . ?
O2 C60 C59 116.1(3) . . ?
C13 C60 C59 116.7(3) . . ?
C45 C62 C53 124.4(3) . . ?
C45 C62 H62 117.8 . . ?
C53 C62 H62 117.8 . . ?
C45 C65 H65A 109.5 . . ?
C45 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C45 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C27 C70 H70A 109.5 . . ?
C27 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C27 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C53 C73 H73A 109.5 . . ?
C53 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C53 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C19 C1X H1X1 109.5 . . ?
C19 C1X H1X2 109.5 . . ?
H1X1 C1X H1X2 109.5 . . ?
C19 C1X H1X3 109.5 . . ?
H1X1 C1X H1X3 109.5 . . ?
H1X2 C1X H1X3 109.5 . . ?
F2 C50 F1 109.5(7) . . ?
F2 C50 F3 108.6(7) . . ?
F1 C50 F3 106.8(8) . . ?
F2 C50 C32 114.2(4) . . ?
F1 C50 C32 111.0(5) . . ?
F3 C50 C32 106.5(5) . . ?
F8 C59 F9 110.2(7) . . ?
F8 C59 F7 106.5(7) . . ?
F9 C59 F7 104.6(5) . . ?
F8 C59 C60 111.6(5) . . ?
F9 C59 C60 113.2(4) . . ?
F7 C59 C60 110.2(4) . . ?

_diffrn_measured_fraction_theta_max 0.880
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.086
####################################################################### 
# 
# 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 1040549'
_audit_update_record             
;
2014-12-19 deposited with the CCDC.
2015-02-25 downloaded from the CCDC.
;
_publcif_datablock.id            {5ebc7331-781b-4f32-9c36-3b3be38700a4}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         
;
C35 H25 F24 Fe3 O14
;
_chemical_formula_sum            'C35 H25 F24 Fe3 O14'
_chemical_formula_weight         1293.10

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_int_tables_number      4


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

_cell_length_a                   9.7834(7)
_cell_length_b                   20.8414(16)
_cell_length_c                   12.0955(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.5700(19)
_cell_angle_gamma                90.00
_cell_volume                     2407.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9783
_cell_measurement_theta_min      2.89
_cell_measurement_theta_max      28.32

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_method    none
_exptl_crystal_F_000             1282
_exptl_absorpt_coefficient_mu    1.045
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6984
_exptl_absorpt_correction_T_max  0.8848
_exptl_absorpt_process_details   ?

_exptl_special_details           ?

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         'none (area detector data)'
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_decay_%        0
_diffrn_reflns_number            45822
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.89
_diffrn_reflns_theta_max         28.39
_reflns_number_total             11964
_reflns_number_gt                11256
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 v.2014.1-1 (Bruker AXS Inc., 2014)'
_computing_cell_refinement       'SAINT V.8.27 (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT V.8.27 (Bruker AXS Inc., 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0310P)²+1.5439P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       noref
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.044(8)
_refine_ls_number_reflns         11964
_refine_ls_number_parameters     736
_refine_ls_number_restraints     91
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0291
_refine_ls_wR_factor_ref         0.0675
_refine_ls_wR_factor_gt          0.0656
_refine_ls_goodness_of_fit_ref   1.026
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.66037(3) 0.592040(15) 0.44523(3) 0.01328(7) Uani 1 1 d . . .
Fe2 Fe 0.46568(3) 0.470372(15) 0.32777(3) 0.01445(7) Uani 1 1 d . . .
Fe3 Fe 0.78164(3) 0.560189(16) 0.72194(3) 0.01607(7) Uani 1 1 d . . .
O1 O 0.47020(19) 0.40186(9) 0.20526(15) 0.0209(4) Uani 1 1 d . A .
O2 O 0.35296(19) 0.52434(8) 0.20152(14) 0.0199(4) Uani 1 1 d . A .
O3 O 0.59618(17) 0.41691(8) 0.44653(14) 0.0169(3) Uani 1 1 d . C .
O4 O 0.30553(18) 0.41529(8) 0.36781(15) 0.0193(4) Uani 1 1 d . C .
O5 O 0.66233(17) 0.52483(8) 0.32700(14) 0.0156(3) Uani 1 1 d . . .
O6 O 0.79896(17) 0.53334(8) 0.54995(14) 0.0147(3) Uani 1 1 d . . .
O7 O 0.54405(18) 0.65457(8) 0.34556(15) 0.0197(4) Uani 1 1 d . . .
O8 O 0.82347(18) 0.64074(8) 0.42424(14) 0.0176(3) Uani 1 1 d . . .
O9 O 0.47036(16) 0.54995(8) 0.44158(13) 0.0137(3) Uani 1 1 d . . .
O10 O 0.64156(17) 0.62721(8) 0.59538(14) 0.0154(3) Uani 1 1 d . . .
O11 O 0.76879(18) 0.60206(9) 0.87335(14) 0.0207(4) Uani 1 1 d . . .
O12 O 0.94811(17) 0.61782(8) 0.72542(14) 0.0178(3) Uani 1 1 d . . .
O13 O 0.86402(18) 0.47806(9) 0.80728(14) 0.0211(4) Uani 1 1 d . B .
O14 O 0.59464(18) 0.51498(8) 0.70301(15) 0.0190(3) Uani 1 1 d . B .
C2 C 0.8003(3) 0.43234(13) 0.8397(2) 0.0236(5) Uani 1 1 d . . .
C3 C 0.6558(3) 0.42209(14) 0.8168(2) 0.0272(6) Uani 1 1 d . B .
H3 H 0.6192 0.3858 0.8482 0.033 Uiso 1 1 calc R . .
C4 C 0.5651(2) 0.46439(13) 0.7487(2) 0.0203(5) Uani 1 1 d . . .
C6 C 0.8052(3) 0.66346(13) 1.0390(2) 0.0222(5) Uani 1 1 d . . .
C7 C 0.8424(2) 0.64601(12) 0.92556(19) 0.0179(5) Uani 1 1 d . . .
C8 C 0.9526(3) 0.67853(12) 0.8934(2) 0.0186(5) Uani 1 1 d . . .
H8 H 0.9973 0.7131 0.9383 0.022 Uiso 1 1 calc R . .
C9 C 0.9972(2) 0.66067(12) 0.7968(2) 0.0170(4) Uani 1 1 d . . .
C10 C 1.1277(3) 0.69317(14) 0.7720(2) 0.0246(5) Uani 1 1 d . . .
C11 C 0.9757(3) 0.71544(14) 0.3693(2) 0.0259(6) Uani 1 1 d . . .
H11A H 1.0281 0.7172 0.4481 0.039 Uiso 1 1 calc R . .
H11B H 0.9704 0.7586 0.3363 0.039 Uiso 1 1 calc R . .
H11C H 1.0235 0.6866 0.3260 0.039 Uiso 1 1 calc R . .
C12 C 0.8310(3) 0.69102(12) 0.3654(2) 0.0169(5) Uani 1 1 d . . .
C13 C 0.7156(3) 0.72234(12) 0.2991(2) 0.0194(5) Uani 1 1 d . . .
H13 H 0.7314 0.7599 0.2593 0.023 Uiso 1 1 calc R . .
C14 C 0.5792(3) 0.70113(12) 0.2886(2) 0.0186(5) Uani 1 1 d . . .
C15 C 0.4613(3) 0.73270(14) 0.2065(3) 0.0287(6) Uani 1 1 d . . .
H15A H 0.4451 0.7100 0.1338 0.043 Uiso 1 1 calc R . .
H15B H 0.4857 0.7775 0.1954 0.043 Uiso 1 1 calc R . .
H15C H 0.3761 0.7312 0.2366 0.043 Uiso 1 1 calc R . .
C16 C 0.5356(3) 0.69086(13) 0.7160(2) 0.0238(5) Uani 1 1 d . . .
H16A H 0.5327 0.6653 0.7834 0.036 Uiso 1 1 calc R . .
H16B H 0.4574 0.7213 0.7019 0.036 Uiso 1 1 calc R . .
H16C H 0.6243 0.7144 0.7281 0.036 Uiso 1 1 calc R . .
C17 C 0.5240(2) 0.64742(11) 0.6160(2) 0.0160(4) Uani 1 1 d . . .
C18 C 0.3939(2) 0.62977(12) 0.5530(2) 0.0183(5) Uani 1 1 d . . .
H18 H 0.3146 0.6524 0.5661 0.022 Uiso 1 1 calc R . .
C19 C 0.3704(2) 0.58122(11) 0.47138(19) 0.0159(4) Uani 1 1 d . . .
C20 C 0.2238(2) 0.56313(13) 0.4155(2) 0.0220(5) Uani 1 1 d . . .
H20A H 0.2042 0.5768 0.3361 0.033 Uiso 1 1 calc R . .
H20B H 0.1582 0.5842 0.4546 0.033 Uiso 1 1 calc R . .
H20C H 0.2128 0.5165 0.4193 0.033 Uiso 1 1 calc R . .
C21 C 1.0213(3) 0.48249(14) 0.6053(2) 0.0245(5) Uani 1 1 d . . .
H21A H 1.0671 0.5209 0.6431 0.037 Uiso 1 1 calc R . .
H21B H 1.0872 0.4590 0.5698 0.037 Uiso 1 1 calc R . .
H21C H 0.9913 0.4549 0.6612 0.037 Uiso 1 1 calc R . .
C22 C 0.8967(2) 0.50187(12) 0.5169(2) 0.0172(5) Uani 1 1 d . . .
C23 C 0.8901(2) 0.48559(12) 0.4036(2) 0.0199(5) Uani 1 1 d . . .
H23 H 0.9716 0.4675 0.3854 0.024 Uiso 1 1 calc R . .
C24 C 0.7747(3) 0.49381(12) 0.3163(2) 0.0186(5) Uani 1 1 d . . .
C25 C 0.7719(3) 0.46568(16) 0.2022(2) 0.0285(6) Uani 1 1 d . . .
H25A H 0.7276 0.4233 0.1968 0.043 Uiso 1 1 calc R . .
H25B H 0.8679 0.4615 0.1913 0.043 Uiso 1 1 calc R . .
H25C H 0.7184 0.4939 0.1435 0.043 Uiso 1 1 calc R . .
C27 C 0.3934(3) 0.39993(12) 0.1079(2) 0.0212(5) Uani 1 1 d . . .
C28 C 0.3098(3) 0.44837(13) 0.0507(2) 0.0235(5) Uani 1 1 d . A .
H28 H 0.2602 0.4415 -0.0250 0.028 Uiso 1 1 calc R . .
C29 C 0.2973(3) 0.50689(13) 0.1026(2) 0.0213(5) Uani 1 1 d . . .
C32 C 0.3207(3) 0.36030(12) 0.4099(2) 0.0189(5) Uani 1 1 d . . .
C33 C 0.4439(3) 0.33013(12) 0.4640(2) 0.0202(5) Uani 1 1 d . C .
H33 H 0.4404 0.2878 0.4923 0.024 Uiso 1 1 calc R . .
C34 C 0.5723(3) 0.36118(12) 0.4771(2) 0.0172(5) Uani 1 1 d . . .
C35 C 0.7061(3) 0.32459(12) 0.5309(2) 0.0216(5) Uani 1 1 d . C .
F7 F 0.6830(2) 0.26935(10) 0.5774(2) 0.0549(6) Uani 1 1 d . . .
F8 F 0.7772(2) 0.31090(12) 0.45283(17) 0.0555(6) Uani 1 1 d . . .
F9 F 0.7895(2) 0.35889(9) 0.60821(17) 0.0453(5) Uani 1 1 d . . .
F13 F 0.67017(17) 0.67634(9) 1.02524(14) 0.0315(4) Uani 1 1 d . . .
F14 F 0.8337(2) 0.61476(9) 1.11171(14) 0.0397(5) Uani 1 1 d . . .
F15 F 0.8761(2) 0.71432(9) 1.08852(14) 0.0382(4) Uani 1 1 d . . .
F16 F 1.10199(18) 0.71713(9) 0.66700(15) 0.0368(4) Uani 1 1 d . . .
F17 F 1.22963(17) 0.65079(10) 0.77767(17) 0.0427(5) Uani 1 1 d . . .
F18 F 1.1756(2) 0.74041(12) 0.84196(19) 0.0581(7) Uani 1 1 d . . .
C26 C 0.3905(4) 0.33439(15) 0.0511(2) 0.0384(8) Uani 1 1 d D A 1
F4 F 0.3254(8) 0.2915(2) 0.1058(4) 0.0169(12) Uiso 0.34 1 d PD A 1
F5 F 0.3209(13) 0.3386(5) -0.0583(7) 0.035(3) Uiso 0.34 1 d PD A 1
F6 F 0.5158(6) 0.3104(4) 0.0585(6) 0.0284(14) Uiso 0.34 1 d PD A 1
F4X F 0.3894(9) 0.2881(3) 0.1073(6) 0.0484(18) Uiso 0.34 1 d PD A 2
F5X F 0.3037(8) 0.3299(4) -0.0528(5) 0.0173(18) Uiso 0.34 1 d PD A 2
F6X F 0.5375(7) 0.3302(4) 0.0290(7) 0.055(2) Uiso 0.34 1 d PD A 2
F4Y F 0.2851(7) 0.2968(3) 0.0998(5) 0.0226(17) Uiso 0.32 1 d PD A 3
F5Y F 0.3555(7) 0.3311(3) -0.0567(4) 0.0164(14) Uiso 0.32 1 d PD A 3
F6Y F 0.4966(7) 0.2985(4) 0.0818(6) 0.037(2) Uiso 0.32 1 d PD A 3
C30 C 0.2021(3) 0.55822(15) 0.0357(2) 0.0329(6) Uani 1 1 d D A 1
F10 F 0.0992(7) 0.5732(4) 0.0915(5) 0.0193(11) Uiso 0.34 1 d PD A 1
F11 F 0.2703(7) 0.6121(2) 0.0277(5) 0.0104(10) Uiso 0.34 1 d PD A 1
F12 F 0.1461(9) 0.5353(4) -0.0731(6) 0.0205(18) Uiso 0.34 1 d PD A 1
F10X F 0.1351(8) 0.5931(4) 0.0953(6) 0.050(2) Uiso 0.34 1 d PD A 2
F11X F 0.3025(8) 0.6065(3) 0.0100(6) 0.043(2) Uiso 0.34 1 d PD A 2
F12X F 0.1191(6) 0.5419(3) -0.0562(5) 0.0225(14) Uiso 0.34 1 d PD A 2
F10Y F 0.0758(7) 0.5552(4) 0.0750(6) 0.040(2) Uiso 0.32 1 d PD A 3
F11Y F 0.2399(8) 0.6143(3) 0.0508(6) 0.039(2) Uiso 0.32 1 d PD A 3
F12Y F 0.1627(7) 0.5482(4) -0.0754(5) 0.0211(18) Uiso 0.32 1 d PD A 3
C1 C 0.8972(3) 0.38288(17) 0.9110(3) 0.0388(7) Uani 1 1 d D B 1
F19 F 0.8296(5) 0.3298(3) 0.9348(6) 0.0165(10) Uiso 0.34 1 d PD B 1
F20 F 0.9974(8) 0.3636(4) 0.8444(6) 0.0281(17) Uiso 0.34 1 d PD B 1
F21 F 0.9775(7) 0.4031(4) 0.9990(5) 0.0288(16) Uiso 0.34 1 d PD B 1
F19X F 0.8392(7) 0.3215(3) 0.8981(6) 0.0395(18) Uiso 0.34 1 d PD B 2
F20X F 1.0132(7) 0.3725(3) 0.8717(6) 0.0296(16) Uiso 0.34 1 d PD B 2
F21X F 0.9398(7) 0.3992(4) 1.0127(5) 0.0314(15) Uiso 0.34 1 d PD B 2
F19Y F 0.8234(7) 0.3429(3) 0.9704(6) 0.0422(19) Uiso 0.32 1 d PD B 3
F20Y F 0.9713(8) 0.3533(4) 0.8654(7) 0.0381(18) Uiso 0.32 1 d PD B 3
F21Y F 0.9679(7) 0.4203(3) 1.0143(5) 0.0203(13) Uiso 0.32 1 d PD B 3
C31 C 0.1830(3) 0.32318(13) 0.3990(3) 0.0266(6) Uani 1 1 d D C 1
F1 F 0.1153(8) 0.3433(3) 0.4800(8) 0.0153(15) Uiso 0.34 1 d PD C 1
F2 F 0.1901(10) 0.2622(4) 0.4134(11) 0.018(2) Uiso 0.34 1 d PD C 1
F3 F 0.0957(6) 0.3345(3) 0.2968(5) 0.0133(11) Uiso 0.34 1 d PD C 1
F1X F 0.0966(7) 0.3468(3) 0.4475(5) 0.0307(19) Uiso 0.34 1 d PD C 2
F2X F 0.2116(8) 0.2593(3) 0.4277(7) 0.018(2) Uiso 0.34 1 d PD C 2
F3X F 0.1206(7) 0.3210(3) 0.2816(5) 0.0347(19) Uiso 0.34 1 d PD C 2
F1Y F 0.1352(9) 0.3380(4) 0.5032(6) 0.036(3) Uiso 0.32 1 d PD C 3
F2Y F 0.1978(9) 0.2599(3) 0.3912(7) 0.0199(19) Uiso 0.32 1 d PD C 3
F3Y F 0.0805(7) 0.3437(3) 0.3223(6) 0.034(2) Uiso 0.32 1 d PD C 3
C5 C 0.4080(3) 0.44994(14) 0.7225(2) 0.0258(6) Uani 1 1 d D B 1
F22 F 0.3568(10) 0.4553(7) 0.6076(6) 0.010(2) Uiso 0.34 1 d PD B 1
F23 F 0.3749(7) 0.3916(3) 0.7532(7) 0.0160(13) Uiso 0.34 1 d PD B 1
F24 F 0.3478(9) 0.4946(5) 0.7817(7) 0.024(2) Uiso 0.34 1 d PD B 1
F22X F 0.3573(10) 0.4465(5) 0.6156(7) 0.028(3) Uiso 0.34 1 d PD B 2
F23X F 0.3727(7) 0.4032(3) 0.7808(5) 0.0306(18) Uiso 0.34 1 d PD B 2
F24X F 0.3362(7) 0.5037(3) 0.7610(6) 0.025(2) Uiso 0.34 1 d PD B 2
F22Y F 0.3471(8) 0.4637(5) 0.6167(7) 0.023(3) Uiso 0.32 1 d PD B 3
F23Y F 0.3860(7) 0.3815(3) 0.7291(6) 0.0272(19) Uiso 0.32 1 d PD B 3
F24Y F 0.3385(6) 0.4768(3) 0.7804(6) 0.0240(16) Uiso 0.32 1 d PD B 3


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O8 1.9537(17) . ?
Fe1 O7 1.9620(17) . ?
Fe1 O10 2.0037(16) . ?
Fe1 O5 2.0049(17) . ?
Fe1 O9 2.0473(16) . ?
Fe1 O6 2.0474(17) . ?
Fe2 O2 2.0199(17) . ?
Fe2 O3 2.0338(17) . ?
Fe2 O1 2.0652(18) . ?
Fe2 O4 2.0826(17) . ?
Fe2 O9 2.1494(16) . ?
Fe2 O5 2.2354(16) . ?
Fe3 O12 2.0166(17) . ?
Fe3 O14 2.0260(17) . ?
Fe3 O11 2.0570(17) . ?
Fe3 O13 2.0695(18) . ?
Fe3 O6 2.1961(16) . ?
Fe3 O10 2.2932(17) . ?
O1 C27 1.253(3) . ?
O2 C29 1.256(3) . ?
O3 C34 1.256(3) . ?
O4 C32 1.250(3) . ?
O5 C24 1.306(3) . ?
O6 C22 1.293(3) . ?
O7 C14 1.280(3) . ?
O8 C12 1.278(3) . ?
O9 C19 1.290(3) . ?
O10 C17 1.299(3) . ?
O11 C7 1.249(3) . ?
O12 C9 1.262(3) . ?
O13 C2 1.248(3) . ?
O14 C4 1.253(3) . ?
C2 C3 1.397(4) . ?
C2 C1 1.533(4) . ?
C3 C4 1.387(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.530(3) . ?
C6 F13 1.322(3) . ?
C6 F14 1.332(3) . ?
C6 F15 1.335(3) . ?
C6 C7 1.538(3) . ?
C7 C8 1.398(3) . ?
C8 C9 1.384(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.531(3) . ?
C10 F18 1.316(3) . ?
C10 F17 1.323(3) . ?
C10 F16 1.337(3) . ?
C11 C12 1.496(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.397(4) . ?
C13 C14 1.385(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.501(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.495(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.384(3) . ?
C18 C19 1.397(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.495(3) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.492(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.400(3) . ?
C23 C24 1.378(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.495(3) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C27 C28 1.386(4) . ?
C27 C26 1.526(4) . ?
C28 C29 1.389(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.529(4) . ?
C32 C33 1.390(4) . ?
C32 C31 1.534(3) . ?
C33 C34 1.391(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.532(3) . ?
C35 F9 1.311(3) . ?
C35 F8 1.320(3) . ?
C35 F7 1.322(3) . ?
C26 F6 1.308(7) . ?
C26 F4 1.351(6) . ?
C26 F5 1.352(9) . ?
C30 F11 1.320(6) . ?
C30 F10 1.365(6) . ?
C30 F12 1.395(7) . ?
C1 F21 1.251(7) . ?
C1 F19 1.352(6) . ?
C1 F20 1.454(7) . ?
C31 F2 1.282(8) . ?
C31 F1 1.361(7) . ?
C31 F3 1.362(6) . ?
C5 F23 1.332(6) . ?
C5 F22 1.376(8) . ?
C5 F24 1.382(8) . ?

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
O8 Fe1 O7 87.48(7) . . ?
O8 Fe1 O10 99.58(7) . . ?
O7 Fe1 O10 99.12(7) . . ?
O8 Fe1 O5 97.78(7) . . ?
O7 Fe1 O5 96.90(7) . . ?
O10 Fe1 O5 156.79(7) . . ?
O8 Fe1 O9 169.49(7) . . ?
O7 Fe1 O9 82.46(7) . . ?
O10 Fe1 O9 85.08(6) . . ?
O5 Fe1 O9 80.49(6) . . ?
O8 Fe1 O6 86.63(7) . . ?
O7 Fe1 O6 173.97(7) . . ?
O10 Fe1 O6 80.61(7) . . ?
O5 Fe1 O6 85.18(7) . . ?
O9 Fe1 O6 103.49(6) . . ?
O2 Fe2 O3 173.98(8) . . ?
O2 Fe2 O1 86.32(7) . . ?
O3 Fe2 O1 91.14(7) . . ?
O2 Fe2 O4 99.68(7) . . ?
O3 Fe2 O4 85.54(7) . . ?
O1 Fe2 O4 85.44(7) . . ?
O2 Fe2 O9 89.23(7) . . ?
O3 Fe2 O9 92.74(7) . . ?
O1 Fe2 O9 172.83(7) . . ?
O4 Fe2 O9 100.87(6) . . ?
O2 Fe2 O5 92.46(7) . . ?
O3 Fe2 O5 82.68(6) . . ?
O1 Fe2 O5 101.25(7) . . ?
O4 Fe2 O5 166.53(7) . . ?
O9 Fe2 O5 73.30(6) . . ?
O12 Fe3 O14 169.93(7) . . ?
O12 Fe3 O11 86.24(7) . . ?
O14 Fe3 O11 93.97(7) . . ?
O12 Fe3 O13 104.90(7) . . ?
O14 Fe3 O13 85.17(7) . . ?
O11 Fe3 O13 89.97(7) . . ?
O12 Fe3 O6 86.73(6) . . ?
O14 Fe3 O6 91.63(7) . . ?
O11 Fe3 O6 169.64(7) . . ?
O13 Fe3 O6 99.20(7) . . ?
O12 Fe3 O10 90.79(6) . . ?
O14 Fe3 O10 79.28(6) . . ?
O11 Fe3 O10 101.10(7) . . ?
O13 Fe3 O10 161.44(7) . . ?
O6 Fe3 O10 71.40(6) . . ?
C27 O1 Fe2 126.51(17) . . ?
C29 O2 Fe2 127.70(17) . . ?
C34 O3 Fe2 125.88(16) . . ?
C32 O4 Fe2 124.86(16) . . ?
C24 O5 Fe1 123.74(15) . . ?
C24 O5 Fe2 119.55(15) . . ?
Fe1 O5 Fe2 102.12(7) . . ?
C22 O6 Fe1 123.13(15) . . ?
C22 O6 Fe3 129.59(15) . . ?
Fe1 O6 Fe3 104.86(7) . . ?
C14 O7 Fe1 130.28(16) . . ?
C12 O8 Fe1 130.26(16) . . ?
C19 O9 Fe1 121.15(15) . . ?
C19 O9 Fe2 131.07(15) . . ?
Fe1 O9 Fe2 103.72(7) . . ?
C17 O10 Fe1 123.56(15) . . ?
C17 O10 Fe3 119.64(14) . . ?
Fe1 O10 Fe3 102.87(7) . . ?
C7 O11 Fe3 128.40(16) . . ?
C9 O12 Fe3 128.37(15) . . ?
C2 O13 Fe3 128.41(17) . . ?
C4 O14 Fe3 129.09(16) . . ?
O13 C2 C3 127.5(2) . . ?
O13 C2 C1 113.6(2) . . ?
C3 C2 C1 118.9(2) . . ?
C4 C3 C2 120.6(2) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
O14 C4 C3 128.2(2) . . ?
O14 C4 C5 113.1(2) . . ?
C3 C4 C5 118.8(2) . . ?
F13 C6 F14 107.3(2) . . ?
F13 C6 F15 107.6(2) . . ?
F14 C6 F15 107.2(2) . . ?
F13 C6 C7 111.1(2) . . ?
F14 C6 C7 110.6(2) . . ?
F15 C6 C7 112.8(2) . . ?
O11 C7 C8 127.6(2) . . ?
O11 C7 C6 113.7(2) . . ?
C8 C7 C6 118.7(2) . . ?
C9 C8 C7 120.5(2) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
O12 C9 C8 128.7(2) . . ?
O12 C9 C10 112.8(2) . . ?
C8 C9 C10 118.4(2) . . ?
F18 C10 F17 107.9(2) . . ?
F18 C10 F16 107.4(2) . . ?
F17 C10 F16 106.4(2) . . ?
F18 C10 C9 113.6(2) . . ?
F17 C10 C9 110.2(2) . . ?
F16 C10 C9 111.0(2) . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O8 C12 C13 124.5(2) . . ?
O8 C12 C11 115.5(2) . . ?
C13 C12 C11 120.0(2) . . ?
C14 C13 C12 123.1(2) . . ?
C14 C13 H13 118.5 . . ?
C12 C13 H13 118.5 . . ?
O7 C14 C13 124.0(2) . . ?
O7 C14 C15 115.5(2) . . ?
C13 C14 C15 120.5(2) . . ?
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 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O10 C17 C18 123.7(2) . . ?
O10 C17 C16 116.0(2) . . ?
C18 C17 C16 120.4(2) . . ?
C17 C18 C19 124.9(2) . . ?
C17 C18 H18 117.6 . . ?
C19 C18 H18 117.6 . . ?
O9 C19 C18 123.0(2) . . ?
O9 C19 C20 117.2(2) . . ?
C18 C19 C20 119.7(2) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O6 C22 C23 123.1(2) . . ?
O6 C22 C21 117.3(2) . . ?
C23 C22 C21 119.5(2) . . ?
C24 C23 C22 125.1(2) . . ?
C24 C23 H23 117.4 . . ?
C22 C23 H23 117.4 . . ?
O5 C24 C23 123.5(2) . . ?
O5 C24 C25 116.0(2) . . ?
C23 C24 C25 120.4(2) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O1 C27 C28 127.9(2) . . ?
O1 C27 C26 113.6(2) . . ?
C28 C27 C26 118.5(2) . . ?
C27 C28 C29 121.0(2) . . ?
C27 C28 H28 119.5 . . ?
C29 C28 H28 119.5 . . ?
O2 C29 C28 128.5(2) . . ?
O2 C29 C30 112.9(2) . . ?
C28 C29 C30 118.6(2) . . ?
O4 C32 C33 128.3(2) . . ?
O4 C32 C31 113.8(2) . . ?
C33 C32 C31 117.9(2) . . ?
C32 C33 C34 120.8(2) . . ?
C32 C33 H33 119.6 . . ?
C34 C33 H33 119.6 . . ?
O3 C34 C33 128.1(2) . . ?
O3 C34 C35 112.9(2) . . ?
C33 C34 C35 118.9(2) . . ?
F9 C35 F8 106.6(2) . . ?
F9 C35 F7 108.0(2) . . ?
F8 C35 F7 106.4(2) . . ?
F9 C35 C34 111.9(2) . . ?
F8 C35 C34 109.8(2) . . ?
F7 C35 C34 113.9(2) . . ?
F6 C26 F4 104.4(5) . . ?
F6 C26 F5 110.9(7) . . ?
F4 C26 F5 109.3(6) . . ?
F6 C26 C27 112.7(4) . . ?
F4 C26 C27 109.6(3) . . ?
F5 C26 C27 109.8(5) . . ?
F11 C30 F10 106.3(5) . . ?
F11 C30 F12 108.8(5) . . ?
F10 C30 F12 111.4(5) . . ?
F11 C30 C29 112.0(3) . . ?
F10 C30 C29 109.1(3) . . ?
F12 C30 C29 109.2(4) . . ?
F21 C1 F19 109.9(5) . . ?
F21 C1 F20 101.0(5) . . ?
F19 C1 F20 108.2(5) . . ?
F21 C1 C2 116.7(4) . . ?
F19 C1 C2 113.5(3) . . ?
F20 C1 C2 106.4(4) . . ?
F2 C31 F1 103.1(6) . . ?
F2 C31 F3 107.5(7) . . ?
F1 C31 F3 107.0(6) . . ?
F2 C31 C32 117.9(5) . . ?
F1 C31 C32 109.8(4) . . ?
F3 C31 C32 110.8(3) . . ?
F23 C5 F22 107.4(7) . . ?
F23 C5 F24 108.3(6) . . ?
F22 C5 F24 111.5(7) . . ?
F23 C5 C4 114.6(3) . . ?
F22 C5 C4 108.8(4) . . ?
F24 C5 C4 106.4(4) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.060
####################################################################### 
# 
# 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_2a
_database_code_depnum_ccdc_archive 'CCDC 1040550'
_audit_update_record             
;
2014-12-19 deposited with the CCDC.
2015-02-25 downloaded from the CCDC.
;
_publcif_datablock.id            {e864158d-b382-4d40-b093-12c7fc9f9218}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         
;
C35 H25 F24 Fe3 O14
;
_chemical_formula_sum            'C35 H25 F24 Fe3 O14'
_chemical_formula_weight         1293.10

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_int_tables_number      4

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

_cell_length_a                   9.7979(13)
_cell_length_b                   20.819(3)
_cell_length_c                   12.0998(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.659(3)
_cell_angle_gamma                90.00
_cell_volume                     2408.2(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9429
_cell_measurement_theta_min      2.89
_cell_measurement_theta_max      28.29

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_method    none
_exptl_crystal_F_000             1282
_exptl_absorpt_coefficient_mu    1.045
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7310
_exptl_absorpt_correction_T_max  0.9027
_exptl_absorpt_process_details   ?

_exptl_special_details           ?

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         'none (area detector data)'
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_decay_%        0
_diffrn_reflns_number            56462
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.89
_diffrn_reflns_theta_max         28.36
_reflns_number_total             11929
_reflns_number_gt                11010
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 v.2014.1-1 (Bruker AXS Inc., 2014)'
_computing_cell_refinement       'SAINT V.8.27 (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT V.8.27 (Bruker AXS Inc., 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0424P)²+0.9379P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       noref
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.007(7)
_refine_ls_number_reflns         11929
_refine_ls_number_parameters     718
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0293
_refine_ls_wR_factor_ref         0.0718
_refine_ls_wR_factor_gt          0.0687
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.085
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.33964(3) 0.409139(15) 0.55476(3) 0.01385(7) Uani 1 1 d . . .
Fe2 Fe 0.53430(3) 0.530796(15) 0.67220(3) 0.01499(7) Uani 1 1 d . . .
Fe3 Fe 0.21839(3) 0.440983(15) 0.27806(3) 0.01649(7) Uani 1 1 d . . .
O1 O 0.64707(18) 0.47685(8) 0.79845(14) 0.0207(4) Uani 1 1 d . A .
O2 O 0.52978(18) 0.59934(8) 0.79445(14) 0.0212(4) Uani 1 1 d . A .
O3 O 0.40362(17) 0.58434(8) 0.55340(14) 0.0174(3) Uani 1 1 d . . .
O4 O 0.69445(17) 0.58579(8) 0.63247(15) 0.0202(3) Uani 1 1 d . . .
O5 O 0.53002(16) 0.45127(7) 0.55845(13) 0.0143(3) Uani 1 1 d . . .
O6 O 0.35838(17) 0.37397(8) 0.40462(13) 0.0162(3) Uani 1 1 d . . .
O7 O 0.45601(18) 0.34654(8) 0.65445(15) 0.0206(3) Uani 1 1 d . . .
O8 O 0.17670(17) 0.36048(8) 0.57584(14) 0.0181(3) Uani 1 1 d . . .
O9 O 0.33774(17) 0.47624(8) 0.67286(13) 0.0166(3) Uani 1 1 d . . .
O10 O 0.20065(16) 0.46790(8) 0.44976(13) 0.0157(3) Uani 1 1 d . . .
O11 O 0.23106(17) 0.39896(8) 0.12674(14) 0.0211(4) Uani 1 1 d . . .
O12 O 0.05169(17) 0.38325(8) 0.27461(13) 0.0183(3) Uani 1 1 d . . .
O13 O 0.13592(17) 0.52314(9) 0.19276(14) 0.0220(4) Uani 1 1 d . B .
O14 O 0.40560(17) 0.48630(8) 0.29689(14) 0.0199(3) Uani 1 1 d . B .
C27 C 0.7026(3) 0.49434(12) 0.8975(2) 0.0214(5) Uani 1 1 d . . .
C28 C 0.6902(3) 0.55276(12) 0.9498(2) 0.0244(5) Uani 1 1 d . A .
H28 H 0.7391 0.5596 1.0258 0.029 Uiso 1 1 calc R . .
C29 C 0.6068(3) 0.60123(12) 0.8920(2) 0.0220(5) Uani 1 1 d . . .
C31 C 0.8176(3) 0.67798(13) 0.6011(2) 0.0277(6) Uani 1 1 d . . .
C32 C 0.6796(2) 0.64089(11) 0.5899(2) 0.0182(5) Uani 1 1 d . . .
C33 C 0.5561(3) 0.67100(12) 0.5359(2) 0.0207(5) Uani 1 1 d . . .
H33 H 0.5596 0.7134 0.5075 0.025 Uiso 1 1 calc R . .
C34 C 0.4276(3) 0.64019(11) 0.52288(19) 0.0174(4) Uani 1 1 d . . .
C35 C 0.2937(3) 0.67660(12) 0.4689(2) 0.0219(5) Uani 1 1 d . . .
C2 C 0.2001(3) 0.56876(13) 0.1605(2) 0.0250(5) Uani 1 1 d . . .
C3 C 0.3441(3) 0.57913(13) 0.1832(2) 0.0278(6) Uani 1 1 d . B .
H3 H 0.3802 0.6156 0.1521 0.033 Uiso 1 1 calc R . .
C4 C 0.4349(2) 0.53685(13) 0.2508(2) 0.0206(5) Uani 1 1 d . . .
C5 C 0.5921(3) 0.55105(14) 0.2774(2) 0.0271(6) Uani 1 1 d . B .
C6 C 0.1941(3) 0.33765(12) -0.0391(2) 0.0232(5) Uani 1 1 d . . .
C7 C 0.1574(2) 0.35516(12) 0.07447(19) 0.0185(5) Uani 1 1 d . . .
C8 C 0.0475(3) 0.32258(12) 0.1066(2) 0.0201(5) Uani 1 1 d . . .
H8 H 0.0031 0.2878 0.0618 0.024 Uiso 1 1 calc R . .
C9 C 0.0027(2) 0.34049(11) 0.20305(19) 0.0175(4) Uani 1 1 d . . .
C10 C -0.1277(3) 0.30778(13) 0.2283(2) 0.0250(5) Uani 1 1 d . . .
C11 C 0.0242(3) 0.28584(13) 0.6308(2) 0.0255(5) Uani 1 1 d . . .
H11A H -0.0244 0.3155 0.6720 0.038 Uiso 1 1 calc R . .
H11B H 0.0293 0.2433 0.6661 0.038 Uiso 1 1 calc R . .
H11C H -0.0272 0.2828 0.5518 0.038 Uiso 1 1 calc R . .
C12 C 0.1689(3) 0.31010(11) 0.63478(19) 0.0173(4) Uani 1 1 d . . .
C13 C 0.2844(3) 0.27881(12) 0.7008(2) 0.0206(5) Uani 1 1 d . . .
H13 H 0.2687 0.2411 0.7405 0.025 Uiso 1 1 calc R . .
C14 C 0.4212(3) 0.29996(11) 0.7114(2) 0.0194(5) Uani 1 1 d . . .
C15 C 0.5391(3) 0.26834(14) 0.7939(2) 0.0288(6) Uani 1 1 d . . .
H15A H 0.6203 0.2641 0.7594 0.043 Uiso 1 1 calc R . .
H15B H 0.5095 0.2257 0.8135 0.043 Uiso 1 1 calc R . .
H15C H 0.5643 0.2946 0.8625 0.043 Uiso 1 1 calc R . .
C16 C -0.0211(3) 0.51873(13) 0.3947(2) 0.0247(5) Uani 1 1 d . . .
H16A H 0.0088 0.5465 0.3390 0.037 Uiso 1 1 calc R . .
H16B H -0.0872 0.5420 0.4300 0.037 Uiso 1 1 calc R . .
H16C H -0.0665 0.4803 0.3567 0.037 Uiso 1 1 calc R . .
C17 C 0.1035(2) 0.49947(11) 0.4834(2) 0.0176(4) Uani 1 1 d . . .
C18 C 0.1100(2) 0.51559(12) 0.5962(2) 0.0210(5) Uani 1 1 d . . .
H18 H 0.0285 0.5336 0.6142 0.025 Uiso 1 1 calc R . .
C19 C 0.2252(2) 0.50746(11) 0.6839(2) 0.0188(5) Uani 1 1 d . . .
C20 C 0.2284(3) 0.53542(15) 0.7981(2) 0.0282(5) Uani 1 1 d . . .
H20A H 0.2761 0.5057 0.8567 0.042 Uiso 1 1 calc R . .
H20B H 0.1324 0.5425 0.8069 0.042 Uiso 1 1 calc R . .
H20C H 0.2785 0.5765 0.8056 0.042 Uiso 1 1 calc R . .
C21 C 0.4644(3) 0.31034(13) 0.2840(2) 0.0238(5) Uani 1 1 d . . .
H21A H 0.3764 0.2863 0.2725 0.036 Uiso 1 1 calc R . .
H21B H 0.5432 0.2802 0.2978 0.036 Uiso 1 1 calc R . .
H21C H 0.4660 0.3359 0.2164 0.036 Uiso 1 1 calc R . .
C22 C 0.4760(2) 0.35381(11) 0.38380(19) 0.0172(4) Uani 1 1 d . . .
C23 C 0.6059(2) 0.37146(11) 0.4468(2) 0.0189(5) Uani 1 1 d . . .
H23 H 0.6849 0.3488 0.4335 0.023 Uiso 1 1 calc R . .
C24 C 0.6298(2) 0.41996(11) 0.52827(19) 0.0167(4) Uani 1 1 d . . .
C25 C 0.7764(2) 0.43798(13) 0.5844(2) 0.0226(5) Uani 1 1 d . . .
H25A H 0.7869 0.4847 0.5822 0.034 Uiso 1 1 calc R . .
H25B H 0.8417 0.4176 0.5445 0.034 Uiso 1 1 calc R . .
H25C H 0.7965 0.4235 0.6634 0.034 Uiso 1 1 calc R . .
F1 F 0.80010(17) 0.74060(7) 0.58817(16) 0.0335(4) Uani 1 1 d . . .
F2 F 0.8847(2) 0.65824(10) 0.5232(2) 0.0590(6) Uani 1 1 d . . .
F3 F 0.9012(2) 0.66815(11) 0.7010(2) 0.0695(8) Uani 1 1 d . . .
F7 F 0.2227(2) 0.69038(12) 0.54726(17) 0.0564(6) Uani 1 1 d . . .
F8 F 0.3167(2) 0.73184(9) 0.4225(2) 0.0544(6) Uani 1 1 d . . .
F9 F 0.21045(19) 0.64222(9) 0.39192(16) 0.0456(5) Uani 1 1 d . . .
F13 F 0.32987(16) 0.32489(8) -0.02515(13) 0.0315(4) Uani 1 1 d . . .
F14 F 0.1661(2) 0.38647(9) -0.11163(13) 0.0403(4) Uani 1 1 d . . .
F15 F 0.12411(19) 0.28692(9) -0.08865(14) 0.0386(4) Uani 1 1 d . . .
F16 F -0.10219(18) 0.28419(9) 0.33299(14) 0.0370(4) Uani 1 1 d . . .
F17 F -0.1756(2) 0.26060(11) 0.15790(18) 0.0587(6) Uani 1 1 d . . .
F18 F -0.22983(17) 0.35030(10) 0.22234(16) 0.0436(5) Uani 1 1 d . . .
F19 F 0.64598(15) 0.54593(8) 0.38735(13) 0.0291(3) Uani 1 1 d . . .
F20 F 0.6225(2) 0.60917(11) 0.2458(2) 0.0663(7) Uani 1 1 d . . .
F21 F 0.65843(18) 0.50867(12) 0.22561(16) 0.0525(6) Uani 1 1 d . . .
C26 C 0.7977(3) 0.44294(15) 0.9646(2) 0.0330(6) Uani 1 1 d D A 1
F4 F 0.8999(6) 0.4272(3) 0.9081(4) 0.0175(11) Uiso 0.34 1 d PD A 1
F5 F 0.8542(10) 0.4668(4) 1.0722(6) 0.028(2) Uiso 0.34 1 d PD A 1
F6 F 0.7291(7) 0.3895(2) 0.9737(5) 0.0121(10) Uiso 0.34 1 d PD A 1
F4X F 0.9241(6) 0.4459(4) 0.9240(5) 0.0394(18) Uiso 0.34 1 d PD A 2
F5X F 0.8388(7) 0.4539(3) 1.0755(5) 0.0197(16) Uiso 0.34 1 d PD A 2
F6X F 0.7580(7) 0.3869(3) 0.9504(6) 0.041(2) Uiso 0.34 1 d PD A 2
F4Y F 0.8624(8) 0.4073(4) 0.9051(6) 0.051(2) Uiso 0.32 1 d PD A 3
F5Y F 0.8811(6) 0.4590(3) 1.0566(5) 0.0210(14) Uiso 0.32 1 d PD A 3
F6Y F 0.6958(8) 0.3949(3) 0.9909(6) 0.043(2) Uiso 0.32 1 d PD A 3
C30 C 0.6098(4) 0.66671(15) 0.9493(2) 0.0394(8) Uani 1 1 d D A 1
F10 F 0.6761(8) 0.7094(2) 0.8937(4) 0.0162(12) Uiso 0.34 1 d PD A 1
F11 F 0.4838(6) 0.6910(3) 0.9409(6) 0.0261(13) Uiso 0.34 1 d PD A 1
F12 F 0.6733(10) 0.6724(4) 1.0549(5) 0.0176(19) Uiso 0.34 1 d PD A 1
F10X F 0.6115(8) 0.7130(3) 0.8929(5) 0.0458(16) Uiso 0.34 1 d PD A 2
F11X F 0.4631(7) 0.6706(4) 0.9711(6) 0.0545(19) Uiso 0.34 1 d PD A 2
F12X F 0.7017(7) 0.6651(3) 1.0546(5) 0.0228(19) Uiso 0.34 1 d PD A 2
F10Y F 0.7152(7) 0.7046(3) 0.9008(5) 0.0259(18) Uiso 0.32 1 d PD A 3
F11Y F 0.5043(7) 0.7032(3) 0.9176(6) 0.039(2) Uiso 0.32 1 d PD A 3
F12Y F 0.6433(8) 0.6654(4) 1.0589(5) 0.028(2) Uiso 0.32 1 d PD A 3
C1 C 0.1030(3) 0.61848(16) 0.0888(3) 0.0384(7) Uani 1 1 d D B 1
F22 F 0.0020(8) 0.6369(4) 0.1548(6) 0.0280(17) Uiso 0.34 1 d PD B 1
F23 F 0.0215(7) 0.5978(4) 0.0020(5) 0.0317(17) Uiso 0.34 1 d PD B 1
F24 F 0.1697(5) 0.6713(3) 0.0650(6) 0.0175(10) Uiso 0.34 1 d PD B 1
F22X F -0.0128(7) 0.6292(3) 0.1284(6) 0.0319(18) Uiso 0.34 1 d PD B 2
F23X F 0.0597(7) 0.6020(3) -0.0122(5) 0.0300(14) Uiso 0.34 1 d PD B 2
F24X F 0.1610(6) 0.6796(3) 0.1017(6) 0.0403(18) Uiso 0.34 1 d PD B 2
F22Y F 0.0290(8) 0.6481(3) 0.1355(7) 0.0400(18) Uiso 0.32 1 d PD B 3
F23Y F 0.0324(6) 0.5809(3) -0.0148(4) 0.0191(12) Uiso 0.32 1 d PD B 3
F24Y F 0.1768(7) 0.6586(3) 0.0303(6) 0.0414(19) Uiso 0.32 1 d PD B 3


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O8 1.9541(17) . ?
Fe1 O7 1.9622(17) . ?
Fe1 O9 2.0014(16) . ?
Fe1 O6 2.0041(16) . ?
Fe1 O10 2.0511(16) . ?
Fe1 O5 2.0529(15) . ?
Fe2 O1 2.0189(16) . ?
Fe2 O3 2.0350(16) . ?
Fe2 O2 2.0628(17) . ?
Fe2 O4 2.0821(17) . ?
Fe2 O5 2.1476(16) . ?
Fe2 O9 2.2374(16) . ?
Fe3 O12 2.0210(17) . ?
Fe3 O14 2.0307(17) . ?
Fe3 O11 2.0574(17) . ?
Fe3 O13 2.0684(17) . ?
Fe3 O10 2.1951(16) . ?
Fe3 O6 2.2917(16) . ?
O1 C27 1.257(3) . ?
O2 C29 1.254(3) . ?
O3 C34 1.258(3) . ?
O4 C32 1.253(3) . ?
O5 C24 1.293(3) . ?
O6 C22 1.301(3) . ?
O7 C14 1.278(3) . ?
O8 C12 1.280(3) . ?
O9 C19 1.311(3) . ?
O10 C17 1.294(3) . ?
O11 C7 1.246(3) . ?
O12 C9 1.261(3) . ?
O13 C2 1.248(3) . ?
O14 C4 1.253(3) . ?
C27 C28 1.389(4) . ?
C27 C26 1.530(4) . ?
C28 C29 1.387(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.527(4) . ?
C31 F3 1.319(3) . ?
C31 F1 1.320(3) . ?
C31 F2 1.328(3) . ?
C31 C32 1.537(3) . ?
C32 C33 1.391(3) . ?
C33 C34 1.390(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.532(3) . ?
C35 F9 1.309(3) . ?
C35 F8 1.321(3) . ?
C35 F7 1.324(3) . ?
C2 C3 1.394(4) . ?
C2 C1 1.539(4) . ?
C3 C4 1.385(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.531(3) . ?
C5 F20 1.322(3) . ?
C5 F19 1.324(3) . ?
C5 F21 1.331(3) . ?
C6 F15 1.329(3) . ?
C6 F13 1.331(3) . ?
C6 F14 1.332(3) . ?
C6 C7 1.538(3) . ?
C7 C8 1.398(3) . ?
C8 C9 1.385(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.537(3) . ?
C10 F17 1.317(3) . ?
C10 F18 1.326(3) . ?
C10 F16 1.330(3) . ?
C11 C12 1.496(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.395(3) . ?
C13 C14 1.390(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.503(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.493(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.393(3) . ?
C18 C19 1.379(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.494(3) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.493(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.382(3) . ?
C23 C24 1.395(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.495(3) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 F6 1.317(6) . ?
C26 F4 1.369(6) . ?
C26 F5 1.390(7) . ?
C30 F12 1.298(7) . ?
C30 F11 1.317(6) . ?
C30 F10 1.363(6) . ?
C1 F23 1.249(7) . ?
C1 F24 1.343(6) . ?
C1 F22 1.452(7) . ?

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
O8 Fe1 O7 87.52(7) . . ?
O8 Fe1 O9 97.64(7) . . ?
O7 Fe1 O9 96.88(7) . . ?
O8 Fe1 O6 99.71(7) . . ?
O7 Fe1 O6 99.10(7) . . ?
O9 Fe1 O6 156.82(7) . . ?
O8 Fe1 O10 86.53(7) . . ?
O7 Fe1 O10 173.91(7) . . ?
O9 Fe1 O10 85.25(7) . . ?
O6 Fe1 O10 80.60(6) . . ?
O8 Fe1 O5 169.46(7) . . ?
O7 Fe1 O5 82.39(7) . . ?
O9 Fe1 O5 80.61(6) . . ?
O6 Fe1 O5 84.98(6) . . ?
O10 Fe1 O5 103.61(6) . . ?
O1 Fe2 O3 173.95(7) . . ?
O1 Fe2 O2 86.35(7) . . ?
O3 Fe2 O2 91.06(7) . . ?
O1 Fe2 O4 99.53(7) . . ?
O3 Fe2 O4 85.70(7) . . ?
O2 Fe2 O4 85.46(7) . . ?
O1 Fe2 O5 89.24(7) . . ?
O3 Fe2 O5 92.79(7) . . ?
O2 Fe2 O5 172.95(7) . . ?
O4 Fe2 O5 100.71(6) . . ?
O1 Fe2 O9 92.50(7) . . ?
O3 Fe2 O9 82.63(6) . . ?
O2 Fe2 O9 101.23(7) . . ?
O4 Fe2 O9 166.62(6) . . ?
O5 Fe2 O9 73.44(6) . . ?
O12 Fe3 O14 169.98(7) . . ?
O12 Fe3 O11 86.26(7) . . ?
O14 Fe3 O11 93.91(7) . . ?
O12 Fe3 O13 104.83(7) . . ?
O14 Fe3 O13 85.19(7) . . ?
O11 Fe3 O13 90.04(7) . . ?
O12 Fe3 O10 86.57(6) . . ?
O14 Fe3 O10 91.84(7) . . ?
O11 Fe3 O10 169.59(7) . . ?
O13 Fe3 O10 99.08(6) . . ?
O12 Fe3 O6 90.82(6) . . ?
O14 Fe3 O6 79.30(6) . . ?
O11 Fe3 O6 101.06(6) . . ?
O13 Fe3 O6 161.44(6) . . ?
O10 Fe3 O6 71.52(6) . . ?
C27 O1 Fe2 127.68(16) . . ?
C29 O2 Fe2 126.39(16) . . ?
C34 O3 Fe2 125.77(15) . . ?
C32 O4 Fe2 124.94(16) . . ?
C24 O5 Fe1 121.23(14) . . ?
C24 O5 Fe2 131.30(14) . . ?
Fe1 O5 Fe2 103.49(6) . . ?
C22 O6 Fe1 123.64(15) . . ?
C22 O6 Fe3 119.50(14) . . ?
Fe1 O6 Fe3 102.89(7) . . ?
C14 O7 Fe1 130.34(16) . . ?
C12 O8 Fe1 130.37(16) . . ?
C19 O9 Fe1 123.92(15) . . ?
C19 O9 Fe2 119.48(14) . . ?
Fe1 O9 Fe2 102.07(7) . . ?
C17 O10 Fe1 122.84(15) . . ?
C17 O10 Fe3 130.09(15) . . ?
Fe1 O10 Fe3 104.74(7) . . ?
C7 O11 Fe3 128.44(15) . . ?
C9 O12 Fe3 128.18(15) . . ?
C2 O13 Fe3 128.10(16) . . ?
C4 O14 Fe3 129.03(16) . . ?
O1 C27 C28 128.7(2) . . ?
O1 C27 C26 112.9(2) . . ?
C28 C27 C26 118.4(2) . . ?
C29 C28 C27 120.5(2) . . ?
C29 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
O2 C29 C28 128.2(2) . . ?
O2 C29 C30 113.8(2) . . ?
C28 C29 C30 118.0(2) . . ?
F3 C31 F1 107.5(2) . . ?
F3 C31 F2 107.4(3) . . ?
F1 C31 F2 107.0(2) . . ?
F3 C31 C32 111.1(2) . . ?
F1 C31 C32 113.4(2) . . ?
F2 C31 C32 110.2(2) . . ?
O4 C32 C33 128.0(2) . . ?
O4 C32 C31 113.7(2) . . ?
C33 C32 C31 118.2(2) . . ?
C34 C33 C32 121.2(2) . . ?
C34 C33 H33 119.4 . . ?
C32 C33 H33 119.4 . . ?
O3 C34 C33 128.0(2) . . ?
O3 C34 C35 112.6(2) . . ?
C33 C34 C35 119.3(2) . . ?
F9 C35 F8 108.1(2) . . ?
F9 C35 F7 106.5(2) . . ?
F8 C35 F7 106.3(2) . . ?
F9 C35 C34 112.0(2) . . ?
F8 C35 C34 113.7(2) . . ?
F7 C35 C34 109.7(2) . . ?
O13 C2 C3 127.9(2) . . ?
O13 C2 C1 113.4(2) . . ?
C3 C2 C1 118.7(2) . . ?
C4 C3 C2 120.7(2) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
O14 C4 C3 128.0(2) . . ?
O14 C4 C5 112.8(2) . . ?
C3 C4 C5 119.2(2) . . ?
F20 C5 F19 107.4(2) . . ?
F20 C5 F21 107.9(2) . . ?
F19 C5 F21 106.9(2) . . ?
F20 C5 C4 113.3(2) . . ?
F19 C5 C4 110.9(2) . . ?
F21 C5 C4 110.2(2) . . ?
F15 C6 F13 107.5(2) . . ?
F15 C6 F14 107.3(2) . . ?
F13 C6 F14 106.9(2) . . ?
F15 C6 C7 113.2(2) . . ?
F13 C6 C7 110.9(2) . . ?
F14 C6 C7 110.7(2) . . ?
O11 C7 C8 127.6(2) . . ?
O11 C7 C6 113.8(2) . . ?
C8 C7 C6 118.6(2) . . ?
C9 C8 C7 120.6(2) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
O12 C9 C8 128.7(2) . . ?
O12 C9 C10 112.6(2) . . ?
C8 C9 C10 118.6(2) . . ?
F17 C10 F18 107.8(2) . . ?
F17 C10 F16 107.8(2) . . ?
F18 C10 F16 106.3(2) . . ?
F17 C10 C9 113.3(2) . . ?
F18 C10 C9 110.1(2) . . ?
F16 C10 C9 111.2(2) . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O8 C12 C13 124.2(2) . . ?
O8 C12 C11 115.5(2) . . ?
C13 C12 C11 120.3(2) . . ?
C14 C13 C12 123.3(2) . . ?
C14 C13 H13 118.3 . . ?
C12 C13 H13 118.3 . . ?
O7 C14 C13 123.8(2) . . ?
O7 C14 C15 115.7(2) . . ?
C13 C14 C15 120.5(2) . . ?
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 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O10 C17 C18 123.5(2) . . ?
O10 C17 C16 116.8(2) . . ?
C18 C17 C16 119.7(2) . . ?
C19 C18 C17 125.3(2) . . ?
C19 C18 H18 117.4 . . ?
C17 C18 H18 117.4 . . ?
O9 C19 C18 123.2(2) . . ?
O9 C19 C20 116.1(2) . . ?
C18 C19 C20 120.7(2) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O6 C22 C23 123.7(2) . . ?
O6 C22 C21 116.0(2) . . ?
C23 C22 C21 120.3(2) . . ?
C22 C23 C24 125.0(2) . . ?
C22 C23 H23 117.5 . . ?
C24 C23 H23 117.5 . . ?
O5 C24 C23 123.0(2) . . ?
O5 C24 C25 117.1(2) . . ?
C23 C24 C25 119.9(2) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
F6 C26 F4 106.4(5) . . ?
F6 C26 F5 109.2(5) . . ?
F4 C26 F5 111.6(5) . . ?
F6 C26 C27 111.9(3) . . ?
F4 C26 C27 109.3(3) . . ?
F5 C26 C27 108.6(4) . . ?
F12 C30 F11 106.2(6) . . ?
F12 C30 F10 104.4(5) . . ?
F11 C30 F10 104.6(5) . . ?
F12 C30 C29 119.1(4) . . ?
F11 C30 C29 112.5(4) . . ?
F10 C30 C29 108.8(3) . . ?
F23 C1 F24 110.7(5) . . ?
F23 C1 F22 99.6(5) . . ?
F24 C1 F22 108.9(5) . . ?
F23 C1 C2 116.4(4) . . ?
F24 C1 C2 113.7(3) . . ?
F22 C1 C2 106.2(4) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        28.36
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.061
####################################################################### 
# 
# 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 1040551'
_audit_update_record             
;
2014-12-19 deposited with the CCDC.
2015-02-25 downloaded from the CCDC.
;
_publcif_datablock.id            {3aa1466c-c655-48d4-8c5f-edb9801ab9c4}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         
;
C35 H19 F30 Fe3 O14
;
_chemical_formula_sum            'C35 H19 F30 Fe3 O14'
_chemical_formula_weight         1401.05

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_int_tables_number      15

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

_cell_length_a                   20.934(3)
_cell_length_b                   13.481(2)
_cell_length_c                   17.739(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.848(2)
_cell_angle_gamma                90.00
_cell_volume                     4999.8(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9952
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      28.23

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_density_method    none
_exptl_crystal_F_000             2756
_exptl_absorpt_coefficient_mu    1.031
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7473
_exptl_absorpt_correction_T_max  0.8524
_exptl_absorpt_process_details   ?

_exptl_special_details           ?

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '0.3 deg wide ω exposures'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         'none (area detector data)'
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_decay_%        0
_diffrn_reflns_number            21346
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.80
_diffrn_reflns_theta_max         28.26
_reflns_number_total             5851
_reflns_number_gt                5035
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       SMART
_computing_cell_refinement       'SMART, SAINT'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0563P)²+11.5693P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       noref
_refine_ls_number_reflns         5851
_refine_ls_number_parameters     391
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.1149
_refine_ls_wR_factor_gt          0.1087
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.17770(3) 0.2500 0.02158(12) Uani 1 2 d S . .
Fe2 Fe 0.123880(16) 0.31698(2) 0.30584(2) 0.02489(11) Uani 1 1 d . . .
O1 O -0.01675(9) 0.06750(12) 0.17542(9) 0.0276(4) Uani 1 1 d . . .
O2 O -0.02876(8) 0.26591(12) 0.16333(9) 0.0228(3) Uani 1 1 d . . .
O3 O 0.08856(8) 0.20326(12) 0.21962(9) 0.0251(3) Uani 1 1 d . . .
O4 O 0.15847(8) 0.20728(13) 0.37373(10) 0.0297(4) Uani 1 1 d . . .
O5 O 0.21716(9) 0.34114(14) 0.27849(11) 0.0338(4) Uani 1 1 d . A .
O6 O 0.13121(8) 0.44038(12) 0.37351(9) 0.0277(4) Uani 1 1 d . B .
O7 O 0.08541(8) 0.40919(12) 0.22488(9) 0.0276(4) Uani 1 1 d . . .
C2 C 0.06472(13) 0.5485(2) 0.14851(15) 0.0332(6) Uani 1 1 d . . .
C3 C -0.01401(11) -0.02516(18) 0.18352(13) 0.0254(5) Uani 1 1 d . . .
C4 C -0.00276(12) 0.26299(17) 0.09863(13) 0.0256(5) Uani 1 1 d . . .
C5 C 0.10544(13) 0.56617(19) 0.28327(15) 0.0311(5) Uani 1 1 d . B .
H5 H 0.1043 0.6358 0.2752 0.037 Uiso 1 1 calc R . .
C6 C 0.08626(11) 0.50240(18) 0.22487(14) 0.0269(5) Uani 1 1 d . . .
C7 C 0.12640(12) 0.52883(19) 0.35404(14) 0.0280(5) Uani 1 1 d . . .
C8 C 0.06045(12) 0.23176(19) 0.09057(14) 0.0289(5) Uani 1 1 d . . .
H8 H 0.0744 0.2253 0.0407 0.035 Uiso 1 1 calc R . .
C9 C 0.10417(12) 0.20962(18) 0.14925(14) 0.0281(5) Uani 1 1 d . . .
C10 C 0.22516(14) 0.1037(2) 0.44957(17) 0.0404(6) Uani 1 1 d . . .
C11 C -0.02730(14) -0.08274(19) 0.10996(15) 0.0335(6) Uani 1 1 d . . .
C12 C 0.27060(13) 0.2337(2) 0.36669(17) 0.0373(6) Uani 1 1 d . A .
H12 H 0.3115 0.2135 0.3867 0.045 Uiso 1 1 calc R . .
C13 C 0.21614(13) 0.18854(19) 0.39243(15) 0.0315(5) Uani 1 1 d . . .
C14 C 0.26627(12) 0.3078(2) 0.31227(16) 0.0333(6) Uani 1 1 d . . .
C15 C -0.04284(13) 0.2951(2) 0.03082(14) 0.0323(5) Uani 1 1 d . . .
H15A H -0.0780 0.2478 0.0215 0.048 Uiso 1 1 calc R . .
H15B H -0.0164 0.2972 -0.0132 0.048 Uiso 1 1 calc R . .
H15C H -0.0604 0.3612 0.0397 0.048 Uiso 1 1 calc R . .
C17 C 0.0000 -0.0766(2) 0.2500 0.0263(7) Uani 1 2 d S . .
H17 H 0.0000 -0.1470 0.2500 0.032 Uiso 1 2 calc SR . .
C18 C 0.17310(13) 0.1949(2) 0.13515(17) 0.0396(6) Uani 1 1 d . . .
H18A H 0.1966 0.2563 0.1468 0.059 Uiso 1 1 calc R . .
H18B H 0.1776 0.1775 0.0820 0.059 Uiso 1 1 calc R . .
H18C H 0.1904 0.1413 0.1674 0.059 Uiso 1 1 calc R . .
F1 F -0.08053(11) -0.05337(16) 0.07450(12) 0.0627(6) Uani 1 1 d . . .
F2 F -0.03024(11) -0.18000(12) 0.12111(11) 0.0528(5) Uani 1 1 d . . .
F3 F 0.02039(11) -0.06683(15) 0.06384(10) 0.0567(5) Uani 1 1 d . . .
F4 F 0.17761(9) 0.10050(15) 0.49688(11) 0.0528(5) Uani 1 1 d . . .
F5 F 0.22666(12) 0.01696(14) 0.41492(12) 0.0633(6) Uani 1 1 d . . .
F6 F 0.27969(9) 0.11335(15) 0.49180(10) 0.0529(5) Uani 1 1 d . . .
F10 F 0.01862(8) 0.49610(12) 0.11314(9) 0.0384(4) Uani 1 1 d . . .
F11 F 0.11363(9) 0.55272(16) 0.10354(9) 0.0509(5) Uani 1 1 d . . .
F12 F 0.04214(11) 0.64078(13) 0.15546(10) 0.0549(5) Uani 1 1 d . . .
C1 C 0.32885(14) 0.3573(2) 0.28896(19) 0.0425(7) Uani 1 1 d D A 1
F7 F 0.3343(4) 0.3430(7) 0.2130(4) 0.0410(16) Uiso 0.34 1 d PD A 1
F8 F 0.3285(3) 0.4523(4) 0.3051(5) 0.0272(13) Uiso 0.34 1 d PD A 1
F9 F 0.3812(3) 0.3145(5) 0.3278(4) 0.0321(12) Uiso 0.34 1 d PD A 1
F7X F 0.3284(4) 0.3750(6) 0.2125(4) 0.054(2) Uiso 0.33 1 d PD A 2
F8X F 0.3368(4) 0.4437(5) 0.3240(4) 0.049(2) Uiso 0.33 1 d PD A 2
F9X F 0.3806(3) 0.3039(4) 0.2991(4) 0.0381(14) Uiso 0.33 1 d PD A 2
F7Y F 0.3482(4) 0.3227(5) 0.2298(4) 0.052(2) Uiso 0.33 1 d PD A 3
F8Y F 0.3227(3) 0.4555(5) 0.2794(4) 0.051(2) Uiso 0.33 1 d PD A 3
F9Y F 0.3779(3) 0.3456(6) 0.3438(4) 0.062(2) Uiso 0.33 1 d PD A 3
C16 C 0.14567(14) 0.6024(2) 0.41693(16) 0.0375(6) Uani 1 1 d D B 1
F13 F 0.1424(4) 0.6977(3) 0.3981(3) 0.0217(11) Uiso 0.34 1 d PD B 1
F14 F 0.1076(4) 0.5847(6) 0.4771(4) 0.0312(17) Uiso 0.34 1 d PD B 1
F15 F 0.2112(3) 0.5780(5) 0.4377(4) 0.0230(12) Uiso 0.34 1 d PD B 1
F13X F 0.1601(3) 0.6956(4) 0.3841(3) 0.0369(17) Uiso 0.33 1 d PD B 2
F14X F 0.1016(3) 0.6134(5) 0.4635(4) 0.0478(19) Uiso 0.33 1 d PD B 2
F15X F 0.1977(3) 0.5849(5) 0.4550(3) 0.0305(14) Uiso 0.33 1 d PD B 2
F13Y F 0.1209(3) 0.6937(4) 0.4056(3) 0.0420(18) Uiso 0.33 1 d PD B 3
F14Y F 0.1214(4) 0.5763(6) 0.4834(4) 0.048(3) Uiso 0.33 1 d PD B 3
F15Y F 0.2058(3) 0.6048(6) 0.4336(4) 0.0423(19) Uiso 0.33 1 d PD B 3


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O3 1.9862(17) 2 ?
Fe1 O3 1.9862(17) . ?
Fe1 O1 2.0084(17) . ?
Fe1 O1 2.0084(17) 2 ?
Fe1 O2 2.0120(16) 2 ?
Fe1 O2 2.0120(16) . ?
Fe2 O4 2.0186(17) . ?
Fe2 O7 2.0350(17) . ?
Fe2 O6 2.0527(18) . ?
Fe2 O5 2.0613(19) . ?
Fe2 O2 2.2013(17) 2 ?
Fe2 O3 2.2636(17) . ?
O1 C3 1.258(3) . ?
O2 C4 1.295(3) . ?
O2 Fe2 2.2013(17) 2 ?
O3 C9 1.309(3) . ?
O4 C13 1.262(3) . ?
O5 C14 1.248(3) . ?
O6 C7 1.244(3) . ?
O7 C6 1.257(3) . ?
C2 F10 1.328(3) . ?
C2 F11 1.330(3) . ?
C2 F12 1.339(3) . ?
C2 C6 1.537(3) . ?
C3 C17 1.387(3) . ?
C3 C11 1.532(3) . ?
C4 C8 1.403(3) . ?
C4 C15 1.496(3) . ?
C5 C6 1.390(4) . ?
C5 C7 1.403(3) . ?
C5 H5 0.9500 . ?
C7 C16 1.532(4) . ?
C8 C9 1.384(4) . ?
C8 H8 0.9500 . ?
C9 C18 1.490(4) . ?
C10 F5 1.322(4) . ?
C10 F4 1.334(4) . ?
C10 F6 1.340(3) . ?
C10 C13 1.533(4) . ?
C11 F1 1.313(3) . ?
C11 F2 1.328(3) . ?
C11 F3 1.339(3) . ?
C12 C13 1.389(4) . ?
C12 C14 1.389(4) . ?
C12 H12 0.9500 . ?
C14 C1 1.544(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C17 C3 1.387(3) 2 ?
C17 H17 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C1 F8 1.313(6) . ?
C1 F7 1.371(7) . ?
C1 F9 1.391(6) . ?
C16 F13 1.329(5) . ?
C16 F14 1.385(7) . ?
C16 F15 1.441(6) . ?

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 O3 160.02(10) 2 . ?
O3 Fe1 O1 99.92(7) 2 . ?
O3 Fe1 O1 94.84(7) . . ?
O3 Fe1 O1 94.84(7) 2 2 ?
O3 Fe1 O1 99.92(7) . 2 ?
O1 Fe1 O1 84.59(10) . 2 ?
O3 Fe1 O2 86.45(7) 2 2 ?
O3 Fe1 O2 81.77(7) . 2 ?
O1 Fe1 O2 167.50(7) . 2 ?
O1 Fe1 O2 84.15(7) 2 2 ?
O3 Fe1 O2 81.77(7) 2 . ?
O3 Fe1 O2 86.45(7) . . ?
O1 Fe1 O2 84.15(7) . . ?
O1 Fe1 O2 167.50(7) 2 . ?
O2 Fe1 O2 107.54(9) 2 . ?
O4 Fe2 O7 170.45(7) . . ?
O4 Fe2 O6 103.34(7) . . ?
O7 Fe2 O6 86.16(7) . . ?
O4 Fe2 O5 86.58(7) . . ?
O7 Fe2 O5 94.80(7) . . ?
O6 Fe2 O5 88.02(7) . . ?
O4 Fe2 O2 85.69(7) . 2 ?
O7 Fe2 O2 92.02(6) . 2 ?
O6 Fe2 O2 98.65(6) . 2 ?
O5 Fe2 O2 170.77(7) . 2 ?
O4 Fe2 O3 90.14(7) . . ?
O7 Fe2 O3 80.35(7) . . ?
O6 Fe2 O3 163.02(6) . . ?
O5 Fe2 O3 103.26(7) . . ?
O2 Fe2 O3 71.75(6) 2 . ?
C3 O1 Fe1 130.81(16) . . ?
C4 O2 Fe1 122.43(15) . . ?
C4 O2 Fe2 130.91(15) . 2 ?
Fe1 O2 Fe2 103.59(7) . 2 ?
C9 O3 Fe1 123.42(16) . . ?
C9 O3 Fe2 120.76(15) . . ?
Fe1 O3 Fe2 102.25(7) . . ?
C13 O4 Fe2 127.86(17) . . ?
C14 O5 Fe2 126.70(18) . . ?
C7 O6 Fe2 127.71(16) . . ?
C6 O7 Fe2 127.29(16) . . ?
F10 C2 F11 107.6(2) . . ?
F10 C2 F12 106.6(2) . . ?
F11 C2 F12 107.5(2) . . ?
F10 C2 C6 112.1(2) . . ?
F11 C2 C6 110.2(2) . . ?
F12 C2 C6 112.6(2) . . ?
O1 C3 C17 126.9(2) . . ?
O1 C3 C11 113.6(2) . . ?
C17 C3 C11 119.5(2) . . ?
O2 C4 C8 122.7(2) . . ?
O2 C4 C15 117.4(2) . . ?
C8 C4 C15 119.9(2) . . ?
C6 C5 C7 120.7(2) . . ?
C6 C5 H5 119.6 . . ?
C7 C5 H5 119.6 . . ?
O7 C6 C5 128.5(2) . . ?
O7 C6 C2 113.6(2) . . ?
C5 C6 C2 117.9(2) . . ?
O6 C7 C5 127.6(2) . . ?
O6 C7 C16 113.8(2) . . ?
C5 C7 C16 118.6(2) . . ?
C9 C8 C4 125.5(2) . . ?
C9 C8 H8 117.3 . . ?
C4 C8 H8 117.3 . . ?
O3 C9 C8 123.0(2) . . ?
O3 C9 C18 116.2(2) . . ?
C8 C9 C18 120.8(2) . . ?
F5 C10 F4 107.4(3) . . ?
F5 C10 F6 107.8(2) . . ?
F4 C10 F6 107.0(2) . . ?
F5 C10 C13 110.9(2) . . ?
F4 C10 C13 111.7(2) . . ?
F6 C10 C13 111.8(2) . . ?
F1 C11 F2 108.9(2) . . ?
F1 C11 F3 107.4(2) . . ?
F2 C11 F3 106.9(2) . . ?
F1 C11 C3 111.7(2) . . ?
F2 C11 C3 112.4(2) . . ?
F3 C11 C3 109.3(2) . . ?
C13 C12 C14 121.1(2) . . ?
C13 C12 H12 119.4 . . ?
C14 C12 H12 119.4 . . ?
O4 C13 C12 128.0(2) . . ?
O4 C13 C10 114.1(2) . . ?
C12 C13 C10 117.9(2) . . ?
O5 C14 C12 128.1(3) . . ?
O5 C14 C1 113.9(3) . . ?
C12 C14 C1 118.0(2) . . ?
C4 C15 H15A 109.5 . . ?
C4 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C4 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C3 C17 C3 120.0(3) 2 . ?
C3 C17 H17 120.0 2 . ?
C3 C17 H17 120.0 . . ?
C9 C18 H18A 109.5 . . ?
C9 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C9 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
F8 C1 F7 110.6(6) . . ?
F8 C1 F9 108.0(5) . . ?
F7 C1 F9 109.1(5) . . ?
F8 C1 C14 110.5(4) . . ?
F7 C1 C14 108.4(4) . . ?
F9 C1 C14 110.3(3) . . ?
F13 C16 F14 109.6(5) . . ?
F13 C16 F15 108.8(4) . . ?
F14 C16 F15 109.9(5) . . ?
F13 C16 C7 115.7(3) . . ?
F14 C16 C7 108.0(4) . . ?
F15 C16 C7 104.6(3) . . ?

_diffrn_measured_fraction_theta_max 0.943
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.074
####################################################################### 
# 
# 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 1040552'
_audit_update_record             
;
2014-12-19 deposited with the CCDC.
2015-02-25 downloaded from the CCDC.
;
_publcif_datablock.id            {545cc2a2-c4a5-432f-b151-e652404169f8}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         
;
C25 H23 F12 Fe Mn O10
;
_chemical_formula_sum            'C25 H23 F12 Fe Mn O10'
_chemical_formula_weight         822.22

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1        '
_symmetry_int_tables_number      2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.4640(6)
_cell_length_b                   11.8255(8)
_cell_length_c                   16.5080(11)
_cell_angle_alpha                102.0220(18)
_cell_angle_beta                 97.8590(18)
_cell_angle_gamma                112.6820(17)
_cell_volume                     1618.30(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9996
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      28.75

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_density_method    none
_exptl_crystal_F_000             824
_exptl_absorpt_coefficient_mu    0.958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8314
_exptl_absorpt_correction_T_max  0.8540
_exptl_absorpt_process_details   ?

_exptl_special_details           ?

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         'none (area detector data)'
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_decay_%        0
_diffrn_reflns_number            48869
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         28.88
_reflns_number_total             8376
_reflns_number_gt                6206
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 v.2014.1-1 (Bruker AXS Inc., 2014)'
_computing_cell_refinement       'SAINT V.8.27 (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT V.8.27 (Bruker AXS Inc., 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0511P)²+1.7558P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       noref
_refine_ls_number_reflns         8376
_refine_ls_number_parameters     466
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0444
_refine_ls_wR_factor_ref         0.1110
_refine_ls_wR_factor_gt          0.0987
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.066
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.80410(4) 0.55373(3) 0.67206(2) 0.01638(9) Uani 1 1 d . . .
Mn1 Mn 0.77601(4) 0.82378(3) 0.74773(2) 0.01641(10) Uani 1 1 d . . .
O1 O 0.7186(2) 0.50292(17) 0.76783(12) 0.0238(4) Uani 1 1 d . . .
O2 O 0.9617(2) 0.48836(16) 0.69998(12) 0.0224(4) Uani 1 1 d . . .
O3 O 0.90328(19) 0.61041(16) 0.57940(11) 0.0179(4) Uani 1 1 d . . .
O4 O 0.94165(19) 0.73335(15) 0.74629(11) 0.0178(3) Uani 1 1 d . . .
O5 O 0.6487(2) 0.39863(16) 0.58432(11) 0.0211(4) Uani 1 1 d . . .
O6 O 0.64197(19) 0.62951(15) 0.66114(11) 0.0172(3) Uani 1 1 d . . .
O7 O 0.6517(2) 0.77243(17) 0.83988(12) 0.0254(4) Uani 1 1 d . B .
O8 O 0.9186(2) 0.99626(17) 0.84772(12) 0.0243(4) Uani 1 1 d . A .
O9 O 0.6397(2) 0.92320(16) 0.71136(12) 0.0218(4) Uani 1 1 d . . .
O10 O 0.9104(2) 0.91334(16) 0.66819(11) 0.0201(4) Uani 1 1 d . . .
C1 C 0.6974(4) 0.4593(3) 0.8993(2) 0.0427(8) Uani 1 1 d . . .
H1A H 0.6778 0.5345 0.9201 0.064 Uiso 1 1 calc R . .
H1B H 0.7611 0.4482 0.9464 0.064 Uiso 1 1 calc R . .
H1C H 0.5966 0.3832 0.8766 0.064 Uiso 1 1 calc R . .
C2 C 0.7843(4) 0.4777(3) 0.82992(18) 0.0283(6) Uani 1 1 d . . .
C3 C 0.9242(4) 0.4637(3) 0.8347(2) 0.0326(7) Uani 1 1 d . . .
H3 H 0.9688 0.4523 0.8859 0.039 Uiso 1 1 calc R . .
C4 C 1.0030(3) 0.4653(2) 0.76962(18) 0.0248(6) Uani 1 1 d . . .
C5 C 1.1444(3) 0.4355(3) 0.7774(2) 0.0362(7) Uani 1 1 d . . .
H5A H 1.1406 0.3826 0.7222 0.054 Uiso 1 1 calc R . .
H5B H 1.1436 0.3892 0.8202 0.054 Uiso 1 1 calc R . .
H5C H 1.2410 0.5155 0.7948 0.054 Uiso 1 1 calc R . .
C6 C 1.1073(3) 0.6968(3) 0.51191(18) 0.0250(6) Uani 1 1 d . . .
H6A H 1.1571 0.6379 0.5024 0.037 Uiso 1 1 calc R . .
H6B H 1.1854 0.7842 0.5195 0.037 Uiso 1 1 calc R . .
H6C H 1.0204 0.6724 0.4625 0.037 Uiso 1 1 calc R . .
C7 C 1.0448(3) 0.6908(2) 0.59014(16) 0.0180(5) Uani 1 1 d . . .
C8 C 1.1420(3) 0.7730(2) 0.67020(17) 0.0204(5) Uani 1 1 d . . .
H8 H 1.2520 0.8159 0.6746 0.024 Uiso 1 1 calc R . .
C9 C 1.0884(3) 0.7952(2) 0.74209(17) 0.0201(5) Uani 1 1 d . . .
C10 C 1.1952(3) 0.8966(3) 0.82125(19) 0.0308(6) Uani 1 1 d . . .
H10A H 1.1598 0.9648 0.8330 0.046 Uiso 1 1 calc R . .
H10B H 1.3030 0.9321 0.8136 0.046 Uiso 1 1 calc R . .
H10C H 1.1931 0.8598 0.8693 0.046 Uiso 1 1 calc R . .
C11 C 0.4076(3) 0.2240(2) 0.50834(18) 0.0267(6) Uani 1 1 d . . .
H11A H 0.4754 0.1968 0.4772 0.040 Uiso 1 1 calc R . .
H11B H 0.3176 0.2180 0.4676 0.040 Uiso 1 1 calc R . .
H11C H 0.3694 0.1686 0.5447 0.040 Uiso 1 1 calc R . .
C12 C 0.5003(3) 0.3598(2) 0.56283(16) 0.0194(5) Uani 1 1 d . . .
C13 C 0.4206(3) 0.4349(2) 0.58676(17) 0.0215(5) Uani 1 1 d . . .
H13 H 0.3086 0.3945 0.5695 0.026 Uiso 1 1 calc R . .
C14 C 0.4896(3) 0.5614(2) 0.63284(16) 0.0191(5) Uani 1 1 d . . .
C15 C 0.3893(3) 0.6302(3) 0.65227(19) 0.0254(6) Uani 1 1 d . . .
H15A H 0.4078 0.6628 0.7142 0.038 Uiso 1 1 calc R . .
H15B H 0.2779 0.5711 0.6281 0.038 Uiso 1 1 calc R . .
H15C H 0.4166 0.7017 0.6272 0.038 Uiso 1 1 calc R . .
C17 C 0.6503(4) 0.8471(3) 0.90578(18) 0.0305(6) Uani 1 1 d . . .
C18 C 0.7504(4) 0.9757(3) 0.9426(2) 0.0406(8) Uani 1 1 d . A .
H18 H 0.7312 1.0217 0.9910 0.049 Uiso 1 1 calc R . .
C19 C 0.8775(3) 1.0394(2) 0.91086(17) 0.0266(6) Uani 1 1 d . . .
C21 C 0.5830(3) 1.0931(3) 0.6948(2) 0.0308(7) Uani 1 1 d . . .
C22 C 0.6922(3) 1.0252(2) 0.69099(17) 0.0193(5) Uani 1 1 d . . .
C23 C 0.8310(3) 1.0804(2) 0.66538(17) 0.0212(5) Uani 1 1 d . . .
H23 H 0.8585 1.1605 0.6537 0.025 Uiso 1 1 calc R . .
C24 C 0.9299(3) 1.0190(2) 0.65681(16) 0.0187(5) Uani 1 1 d . . .
C25 C 1.0850(3) 1.0856(3) 0.6323(2) 0.0271(6) Uani 1 1 d . . .
F7 F 0.5513(3) 1.1133(2) 0.77051(16) 0.0615(7) Uani 1 1 d . . .
F8 F 0.64173(19) 1.20556(15) 0.67796(13) 0.0387(4) Uani 1 1 d . . .
F9 F 0.4464(2) 1.02045(17) 0.63706(16) 0.0538(6) Uani 1 1 d . . .
F10 F 1.2060(2) 1.13486(18) 0.70001(13) 0.0444(5) Uani 1 1 d . . .
F11 F 1.1117(2) 1.00364(16) 0.57444(12) 0.0372(4) Uani 1 1 d . . .
F12 F 1.0899(2) 1.18152(16) 0.59990(13) 0.0378(4) Uani 1 1 d . . .
C20 C 0.9796(4) 1.1813(3) 0.95849(19) 0.0330(7) Uani 1 1 d D A 1
F4 F 1.0356(8) 1.2000(5) 1.0426(3) 0.0141(12) Uiso 0.34 1 d PD A 1
F5 F 0.8916(7) 1.2480(5) 0.9533(5) 0.0295(13) Uiso 0.34 1 d PD A 1
F6 F 1.1002(7) 1.2369(5) 0.9260(4) 0.0268(11) Uiso 0.34 1 d PD A 1
F4X F 1.0710(8) 1.1949(6) 1.0258(4) 0.041(2) Uiso 0.33 1 d PD A 2
F5X F 0.8799(7) 1.2442(6) 0.9853(5) 0.0390(17) Uiso 0.33 1 d PD A 2
F6X F 1.0430(8) 1.2464(5) 0.9081(4) 0.0386(14) Uiso 0.33 1 d PD A 2
F4Y F 1.0002(9) 1.2091(7) 1.0411(4) 0.040(2) Uiso 0.33 1 d PD A 3
F5Y F 0.9333(8) 1.2509(6) 0.9270(4) 0.0403(16) Uiso 0.33 1 d PD A 3
F6Y F 1.1394(6) 1.2165(5) 0.9454(3) 0.0259(12) Uiso 0.33 1 d PD A 3
C16 C 0.5188(4) 0.7829(3) 0.9484(2) 0.0402(8) Uani 1 1 d D B 1
F1 F 0.3719(8) 0.7397(9) 0.8867(5) 0.0320(19) Uiso 0.34 1 d PD B 1
F2 F 0.5018(9) 0.6739(7) 0.9580(6) 0.037(2) Uiso 0.34 1 d PD B 1
F3 F 0.5179(7) 0.8600(5) 1.0202(4) 0.0217(11) Uiso 0.34 1 d PD B 1
F1X F 0.3780(9) 0.7162(8) 0.8968(6) 0.046(2) Uiso 0.33 1 d PD B 2
F2X F 0.5520(8) 0.7133(6) 0.9900(4) 0.0399(15) Uiso 0.33 1 d PD B 2
F3X F 0.4798(8) 0.8726(6) 1.0010(4) 0.0371(17) Uiso 0.33 1 d PD B 2
F1Y F 0.3912(9) 0.7644(8) 0.9107(6) 0.044(2) Uiso 0.33 1 d PD B 3
F2Y F 0.5325(10) 0.6665(7) 0.9569(5) 0.0306(19) Uiso 0.33 1 d PD B 3
F3Y F 0.5605(8) 0.8417(6) 1.0338(4) 0.0425(17) Uiso 0.33 1 d PD B 3


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O5 1.9636(18) . ?
Fe1 O2 1.9706(17) . ?
Fe1 O1 1.9712(18) . ?
Fe1 O3 2.0011(17) . ?
Fe1 O4 2.0137(17) . ?
Fe1 O6 2.0596(16) . ?
Mn1 O7 2.0951(19) . ?
Mn1 O10 2.1119(17) . ?
Mn1 O8 2.1381(19) . ?
Mn1 O9 2.1581(17) . ?
Mn1 O6 2.1952(17) . ?
Mn1 O4 2.2122(16) . ?
O1 C2 1.274(3) . ?
O2 C4 1.280(3) . ?
O3 C7 1.270(3) . ?
O4 C9 1.316(3) . ?
O5 C12 1.268(3) . ?
O6 C14 1.307(3) . ?
O7 C17 1.255(3) . ?
O8 C19 1.241(3) . ?
O9 C22 1.252(3) . ?
O10 C24 1.249(3) . ?
C1 C2 1.502(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.390(4) . ?
C3 C4 1.389(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.505(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.496(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.407(4) . ?
C8 C9 1.368(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.490(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.501(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.402(4) . ?
C13 C14 1.370(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.495(3) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C17 C18 1.388(4) . ?
C17 C16 1.534(4) . ?
C18 C19 1.388(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.536(4) . ?
C21 F7 1.320(4) . ?
C21 F8 1.335(3) . ?
C21 F9 1.336(4) . ?
C21 C22 1.534(3) . ?
C22 C23 1.392(3) . ?
C23 C24 1.393(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.531(4) . ?
C25 F10 1.328(3) . ?
C25 F11 1.335(3) . ?
C25 F12 1.340(3) . ?
C20 F6 1.327(6) . ?
C20 F5 1.356(6) . ?
C20 F4 1.356(6) . ?
C16 F2 1.283(8) . ?
C16 F3 1.340(6) . ?
C16 F1 1.442(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Fe1 O2 97.37(7) . . ?
O5 Fe1 O1 94.90(8) . . ?
O2 Fe1 O1 88.05(8) . . ?
O5 Fe1 O3 87.88(7) . . ?
O2 Fe1 O3 89.81(7) . . ?
O1 Fe1 O3 176.70(8) . . ?
O5 Fe1 O4 166.63(7) . . ?
O2 Fe1 O4 94.45(7) . . ?
O1 Fe1 O4 91.73(7) . . ?
O3 Fe1 O4 85.92(7) . . ?
O5 Fe1 O6 87.75(7) . . ?
O2 Fe1 O6 171.90(7) . . ?
O1 Fe1 O6 85.25(7) . . ?
O3 Fe1 O6 96.67(7) . . ?
O4 Fe1 O6 81.23(7) . . ?
O7 Mn1 O10 168.48(7) . . ?
O7 Mn1 O8 83.93(7) . . ?
O10 Mn1 O8 86.11(7) . . ?
O7 Mn1 O9 91.98(7) . . ?
O10 Mn1 O9 81.55(7) . . ?
O8 Mn1 O9 86.00(7) . . ?
O7 Mn1 O6 90.57(7) . . ?
O10 Mn1 O6 100.15(7) . . ?
O8 Mn1 O6 169.62(7) . . ?
O9 Mn1 O6 103.03(7) . . ?
O7 Mn1 O4 106.83(7) . . ?
O10 Mn1 O4 80.45(6) . . ?
O8 Mn1 O4 99.16(7) . . ?
O9 Mn1 O4 160.87(7) . . ?
O6 Mn1 O4 73.98(6) . . ?
C2 O1 Fe1 128.22(18) . . ?
C4 O2 Fe1 127.92(17) . . ?
C7 O3 Fe1 125.31(16) . . ?
C9 O4 Fe1 121.76(15) . . ?
C9 O4 Mn1 121.81(14) . . ?
Fe1 O4 Mn1 102.74(7) . . ?
C12 O5 Fe1 128.33(16) . . ?
C14 O6 Fe1 124.35(15) . . ?
C14 O6 Mn1 130.14(15) . . ?
Fe1 O6 Mn1 101.82(7) . . ?
C17 O7 Mn1 126.59(18) . . ?
C19 O8 Mn1 125.84(18) . . ?
C22 O9 Mn1 125.52(16) . . ?
C24 O10 Mn1 126.39(16) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 124.2(3) . . ?
O1 C2 C1 115.4(3) . . ?
C3 C2 C1 120.5(3) . . ?
C4 C3 C2 124.2(3) . . ?
C4 C3 H3 117.9 . . ?
C2 C3 H3 117.9 . . ?
O2 C4 C3 124.2(3) . . ?
O2 C4 C5 115.7(3) . . ?
C3 C4 C5 120.1(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O3 C7 C8 123.6(2) . . ?
O3 C7 C6 116.7(2) . . ?
C8 C7 C6 119.7(2) . . ?
C9 C8 C7 124.2(2) . . ?
C9 C8 H8 117.9 . . ?
C7 C8 H8 117.9 . . ?
O4 C9 C8 123.7(2) . . ?
O4 C9 C10 115.5(2) . . ?
C8 C9 C10 120.8(2) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O5 C12 C13 124.3(2) . . ?
O5 C12 C11 116.3(2) . . ?
C13 C12 C11 119.4(2) . . ?
C14 C13 C12 125.9(2) . . ?
C14 C13 H13 117.1 . . ?
C12 C13 H13 117.1 . . ?
O6 C14 C13 124.0(2) . . ?
O6 C14 C15 116.0(2) . . ?
C13 C14 C15 120.0(2) . . ?
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 C17 C18 128.3(3) . . ?
O7 C17 C16 113.3(2) . . ?
C18 C17 C16 118.4(3) . . ?
C19 C18 C17 122.1(3) . . ?
C19 C18 H18 118.9 . . ?
C17 C18 H18 118.9 . . ?
O8 C19 C18 128.0(3) . . ?
O8 C19 C20 115.4(2) . . ?
C18 C19 C20 116.6(2) . . ?
F7 C21 F8 107.6(2) . . ?
F7 C21 F9 107.7(3) . . ?
F8 C21 F9 106.6(2) . . ?
F7 C21 C22 111.3(2) . . ?
F8 C21 C22 113.6(2) . . ?
F9 C21 C22 109.7(2) . . ?
O9 C22 C23 128.6(2) . . ?
O9 C22 C21 113.0(2) . . ?
C23 C22 C21 118.4(2) . . ?
C22 C23 C24 120.4(2) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
O10 C24 C23 128.0(2) . . ?
O10 C24 C25 113.1(2) . . ?
C23 C24 C25 118.9(2) . . ?
F10 C25 F11 107.0(2) . . ?
F10 C25 F12 106.9(2) . . ?
F11 C25 F12 107.2(2) . . ?
F10 C25 C24 110.6(2) . . ?
F11 C25 C24 111.4(2) . . ?
F12 C25 C24 113.4(2) . . ?
F6 C20 F5 105.1(5) . . ?
F6 C20 F4 108.5(5) . . ?
F5 C20 F4 106.9(5) . . ?
F6 C20 C19 114.0(3) . . ?
F5 C20 C19 109.6(3) . . ?
F4 C20 C19 112.2(3) . . ?
F2 C16 F3 111.1(5) . . ?
F2 C16 F1 97.8(6) . . ?
F3 C16 F1 109.0(6) . . ?
F2 C16 C17 116.6(5) . . ?
F3 C16 C17 114.2(3) . . ?
F1 C16 C17 106.3(4) . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.085
####################################################################### 
# 
# 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 1040553'
_audit_update_record             
;
2014-12-19 deposited with the CCDC.
2015-02-25 downloaded from the CCDC.
;
_publcif_datablock.id            {d4ba260d-094c-49a5-8acc-056ff0c5e0a9}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         
;
C35 H25 F24 Fe Ni2 O14
;
_chemical_formula_sum            'C35 H25 F24 Fe Ni2 O14'
_chemical_formula_weight         1298.82

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 2(1)'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_int_tables_number      4

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

_cell_length_a                   9.7682(7)
_cell_length_b                   20.7583(15)
_cell_length_c                   12.0575(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.1260(17)
_cell_angle_gamma                90.00
_cell_volume                     2381.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9714
_cell_measurement_theta_min      2.90
_cell_measurement_theta_max      27.88

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_density_method    none
_exptl_crystal_F_000             1290
_exptl_absorpt_coefficient_mu    1.238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8079
_exptl_absorpt_correction_T_max  0.8458
_exptl_absorpt_process_details   ?

_exptl_special_details           ?

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         'none (area detector data)'
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_decay_%        0
_diffrn_reflns_number            60549
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.90
_diffrn_reflns_theta_max         27.99
_reflns_number_total             11379
_reflns_number_gt                10161
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 v.2014.1-1 (Bruker AXS Inc., 2014)'
_computing_cell_refinement       'SAINT V.8.27 (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT V.8.27 (Bruker AXS Inc., 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0211P)²+2.5008P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       noref
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(8)
_refine_ls_number_reflns         11379
_refine_ls_number_parameters     709
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_ref         0.0698
_refine_ls_wR_factor_gt          0.0657
_refine_ls_goodness_of_fit_ref   1.061
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni -0.03436(4) 0.881929(17) 0.82870(3) 0.01476(8) Uani 1 1 d . . .
Ni2 Ni 0.27534(4) 0.972189(18) 1.21365(3) 0.01815(9) Uani 1 1 d . . .
Fe1 Fe 0.15470(4) 1.002967(19) 0.94173(4) 0.01360(9) Uani 1 1 d . . .
O1 O 0.2531(2) 1.01147(11) 1.36139(19) 0.0234(5) Uani 1 1 d . . .
O2 O 0.4452(2) 1.02651(10) 1.21923(18) 0.0188(5) Uani 1 1 d . . .
O3 O 0.3701(2) 0.89479(11) 1.30193(18) 0.0226(5) Uani 1 1 d . B .
O4 O 0.0913(2) 0.92685(10) 1.19608(19) 0.0192(5) Uani 1 1 d . B .
O5 O 0.2935(2) 0.94371(10) 1.04740(18) 0.0153(4) Uani 1 1 d . . .
O6 O 0.1549(2) 0.93590(10) 0.82228(18) 0.0161(4) Uani 1 1 d . . .
O7 O 0.3176(2) 1.05235(10) 0.92099(18) 0.0181(5) Uani 1 1 d . . .
O8 O 0.0355(2) 1.06507(10) 0.84116(19) 0.0196(5) Uani 1 1 d . . .
O9 O 0.1388(2) 1.03876(10) 1.09252(17) 0.0147(4) Uani 1 1 d . . .
O10 O -0.0340(2) 0.95895(9) 0.94021(17) 0.0144(4) Uani 1 1 d . . .
O11 O -0.1518(2) 0.93521(10) 0.70666(18) 0.0191(5) Uani 1 1 d . . .
O12 O -0.0164(2) 0.81358(10) 0.71449(18) 0.0208(5) Uani 1 1 d . A .
O13 O 0.0971(2) 0.83035(10) 0.94746(18) 0.0161(4) Uani 1 1 d . . .
O14 O -0.1981(2) 0.82957(10) 0.85910(19) 0.0195(5) Uani 1 1 d . . .
C1 C 0.2927(4) 1.07174(17) 1.5294(3) 0.0268(7) Uani 1 1 d . . .
C2 C 0.3305(4) 1.05426(16) 1.4166(3) 0.0214(7) Uani 1 1 d . . .
C3 C 0.4446(3) 1.08605(15) 1.3882(3) 0.0213(7) Uani 1 1 d . . .
H3 H 0.4897 1.1202 1.4351 0.026 Uiso 1 1 calc R . .
C4 C 0.4923(3) 1.06844(15) 1.2933(3) 0.0182(6) Uani 1 1 d . . .
C5 C 0.6262(3) 1.10105(17) 1.2730(3) 0.0237(7) Uani 1 1 d . . .
C7 C 0.3076(4) 0.84898(17) 1.3362(3) 0.0253(7) Uani 1 1 d . . .
C8 C 0.1649(4) 0.83633(18) 1.3155(3) 0.0290(8) Uani 1 1 d . B .
H8 H 0.1325 0.7998 1.3494 0.035 Uiso 1 1 calc R . .
C9 C 0.0684(3) 0.87644(16) 1.2457(3) 0.0198(6) Uani 1 1 d . . .
C10 C -0.0887(4) 0.85903(17) 1.2207(3) 0.0261(7) Uani 1 1 d . B .
C11 C 0.5187(3) 0.89372(17) 1.1017(3) 0.0257(7) Uani 1 1 d . . .
H11A H 0.5624 0.9319 1.1428 0.038 Uiso 1 1 calc R . .
H11B H 0.5862 0.8725 1.0647 0.038 Uiso 1 1 calc R . .
H11C H 0.4908 0.8638 1.1554 0.038 Uiso 1 1 calc R . .
C12 C 0.3920(3) 0.91341(14) 1.0136(3) 0.0174(6) Uani 1 1 d . . .
C13 C 0.3853(3) 0.89834(15) 0.8996(3) 0.0204(7) Uani 1 1 d . . .
H13 H 0.4679 0.8815 0.8813 0.024 Uiso 1 1 calc R . .
C14 C 0.2686(3) 0.90597(15) 0.8113(3) 0.0189(6) Uani 1 1 d . . .
C15 C 0.2676(4) 0.87898(19) 0.6962(3) 0.0279(7) Uani 1 1 d . . .
H15A H 0.2407 0.8334 0.6939 0.042 Uiso 1 1 calc R . .
H15B H 0.3615 0.8830 0.6809 0.042 Uiso 1 1 calc R . .
H15C H 0.1998 0.9028 0.6383 0.042 Uiso 1 1 calc R . .
C16 C 0.4678(4) 1.12814(18) 0.8665(3) 0.0272(8) Uani 1 1 d . . .
H16A H 0.5186 1.1327 0.9461 0.041 Uiso 1 1 calc R . .
H16B H 0.4611 1.1702 0.8289 0.041 Uiso 1 1 calc R . .
H16C H 0.5184 1.0981 0.8274 0.041 Uiso 1 1 calc R . .
C17 C 0.3235(3) 1.10285(14) 0.8620(3) 0.0170(6) Uani 1 1 d . . .
C18 C 0.2072(3) 1.13343(15) 0.7945(3) 0.0203(7) Uani 1 1 d . . .
H18 H 0.2222 1.1709 0.7535 0.024 Uiso 1 1 calc R . .
C19 C 0.0700(3) 1.11177(14) 0.7840(3) 0.0185(6) Uani 1 1 d . . .
C20 C -0.0496(4) 1.14309(17) 0.7001(3) 0.0287(8) Uani 1 1 d . . .
H20A H -0.0604 1.1225 0.6255 0.043 Uiso 1 1 calc R . .
H20B H -0.0293 1.1890 0.6936 0.043 Uiso 1 1 calc R . .
H20C H -0.1367 1.1382 0.7266 0.043 Uiso 1 1 calc R . .
C21 C 0.0301(3) 1.10342(16) 1.2115(3) 0.0229(7) Uani 1 1 d . . .
H21A H 0.0277 1.0781 1.2797 0.034 Uiso 1 1 calc R . .
H21B H -0.0494 1.1335 1.1960 0.034 Uiso 1 1 calc R . .
H21C H 0.1183 1.1277 1.2241 0.034 Uiso 1 1 calc R . .
C22 C 0.0202(3) 1.05916(13) 1.1121(3) 0.0159(6) Uani 1 1 d . . .
C23 C -0.1098(3) 1.04057(15) 1.0485(3) 0.0191(6) Uani 1 1 d . . .
H23 H -0.1894 1.0636 1.0604 0.023 Uiso 1 1 calc R . .
C24 C -0.1346(3) 0.99108(14) 0.9684(2) 0.0152(6) Uani 1 1 d . . .
C25 C -0.2818(3) 0.97286(17) 0.9123(3) 0.0222(6) Uani 1 1 d . . .
H25A H -0.3040 0.9885 0.8336 0.033 Uiso 1 1 calc R . .
H25B H -0.3468 0.9923 0.9539 0.033 Uiso 1 1 calc R . .
H25C H -0.2914 0.9259 0.9127 0.033 Uiso 1 1 calc R . .
C26 C -0.2989(4) 0.96657(17) 0.5351(3) 0.0307(8) Uani 1 1 d . . .
C27 C -0.2003(3) 0.91701(16) 0.6065(3) 0.0201(6) Uani 1 1 d . . .
C28 C -0.1784(4) 0.85893(16) 0.5558(3) 0.0230(7) Uani 1 1 d . A .
H28 H -0.2247 0.8513 0.4787 0.028 Uiso 1 1 calc R . .
C29 C -0.0902(4) 0.81178(15) 0.6153(3) 0.0217(7) Uani 1 1 d . . .
C31 C 0.2024(3) 0.73694(15) 1.0327(3) 0.0211(7) Uani 1 1 d . . .
C32 C 0.0705(3) 0.77448(14) 0.9758(3) 0.0164(6) Uani 1 1 d . . .
C33 C -0.0590(3) 0.74408(14) 0.9586(3) 0.0197(7) Uani 1 1 d . . .
H33 H -0.0637 0.7015 0.9862 0.024 Uiso 1 1 calc R . .
C34 C -0.1820(3) 0.77426(15) 0.9023(3) 0.0189(6) Uani 1 1 d . . .
C35 C -0.3216(4) 0.73723(16) 0.8903(3) 0.0283(8) Uani 1 1 d . . .
F1 F 0.1559(2) 1.08273(11) 1.51532(18) 0.0353(5) Uani 1 1 d . . .
F2 F 0.3252(3) 1.02378(12) 1.60370(19) 0.0495(7) Uani 1 1 d . . .
F3 F 0.3590(3) 1.12379(13) 1.5782(2) 0.0470(6) Uani 1 1 d . . .
F4 F 0.6756(3) 1.14632(13) 1.3474(2) 0.0555(8) Uani 1 1 d . . .
F5 F 0.7277(2) 1.05778(11) 1.2774(2) 0.0410(6) Uani 1 1 d . . .
F6 F 0.6032(2) 1.12748(11) 1.16998(19) 0.0380(5) Uani 1 1 d . . .
F10 F -0.1556(2) 0.89853(15) 1.2775(2) 0.0535(7) Uani 1 1 d . . .
F11 F -0.1119(3) 0.79932(13) 1.2499(3) 0.0644(9) Uani 1 1 d . . .
F12 F -0.1473(2) 0.86528(10) 1.11187(16) 0.0279(4) Uani 1 1 d . . .
F13 F -0.4082(3) 0.97683(18) 0.5820(2) 0.0810(11) Uani 1 1 d . . .
F14 F -0.2352(4) 1.02155(11) 0.5329(2) 0.0750(11) Uani 1 1 d . . .
F15 F -0.3495(3) 0.94903(11) 0.42949(18) 0.0406(6) Uani 1 1 d . . .
F19 F 0.2701(3) 0.71856(15) 0.9546(2) 0.0589(8) Uani 1 1 d . . .
F20 F 0.2904(2) 0.77108(11) 1.1067(2) 0.0458(7) Uani 1 1 d . . .
F21 F 0.1768(3) 0.68348(12) 1.0831(3) 0.0611(8) Uani 1 1 d . . .
F22 F -0.3911(3) 0.75862(13) 0.9648(3) 0.0685(10) Uani 1 1 d . . .
F23 F -0.3041(2) 0.67464(9) 0.9072(2) 0.0359(5) Uani 1 1 d . . .
F24 F -0.4030(3) 0.74515(15) 0.7883(3) 0.0788(11) Uani 1 1 d . . .
C30 C -0.0808(5) 0.74830(19) 0.5552(3) 0.0486(13) Uani 1 1 d D A 1
F16 F 0.0510(8) 0.7316(5) 0.5581(8) 0.047(2) Uiso 0.34 1 d PD A 1
F17 F -0.1290(11) 0.7006(3) 0.6077(6) 0.0298(15) Uiso 0.34 1 d PD A 1
F18 F -0.1756(9) 0.7471(4) 0.4497(6) 0.019(2) Uiso 0.34 1 d PD A 1
F16X F 0.0229(8) 0.7125(4) 0.5893(6) 0.0325(16) Uiso 0.33 1 d PD A 2
F17X F -0.1902(7) 0.7066(3) 0.6027(5) 0.0214(14) Uiso 0.33 1 d PD A 2
F18X F -0.1208(8) 0.7488(4) 0.4461(5) 0.0154(16) Uiso 0.33 1 d PD A 2
F16Y F 0.0685(7) 0.7532(4) 0.5284(6) 0.0357(18) Uiso 0.33 1 d PD A 3
F17Y F -0.0581(10) 0.6988(3) 0.6127(6) 0.0341(17) Uiso 0.33 1 d PD A 3
F18Y F -0.1510(13) 0.7372(5) 0.4534(8) 0.029(3) Uiso 0.33 1 d PD A 3
C6 C 0.4100(4) 0.8007(2) 1.4099(4) 0.0384(9) Uani 1 1 d D B 1
F7 F 0.4849(9) 0.8217(5) 1.5002(6) 0.025(2) Uiso 0.34 1 d PD B 1
F8 F 0.5098(10) 0.7834(5) 1.3448(8) 0.029(2) Uiso 0.34 1 d PD B 1
F9 F 0.3436(7) 0.7456(3) 1.4316(8) 0.0171(14) Uiso 0.34 1 d PD B 1
F7X F 0.4482(9) 0.8166(5) 1.5129(6) 0.033(2) Uiso 0.33 1 d PD B 2
F8X F 0.5279(8) 0.7931(4) 1.3706(8) 0.027(2) Uiso 0.33 1 d PD B 2
F9X F 0.3569(9) 0.7384(4) 1.3972(8) 0.043(3) Uiso 0.33 1 d PD B 2
F7Y F 0.4762(8) 0.8398(3) 1.5126(6) 0.0188(16) Uiso 0.33 1 d PD B 3
F8Y F 0.4936(10) 0.7729(4) 1.3671(9) 0.036(2) Uiso 0.33 1 d PD B 3
F9Y F 0.3422(8) 0.7591(4) 1.4668(7) 0.042(2) Uiso 0.33 1 d PD B 3


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O11 1.984(2) . ?
Ni1 O13 2.003(2) . ?
Ni1 O12 2.012(2) . ?
Ni1 O14 2.035(2) . ?
Ni1 O10 2.088(2) . ?
Ni1 O6 2.178(2) . ?
Ni2 O2 1.995(2) . ?
Ni2 O4 1.998(2) . ?
Ni2 O1 2.015(2) . ?
Ni2 O3 2.031(2) . ?
Ni2 O5 2.136(2) . ?
Ni2 O9 2.222(2) . ?
Fe1 O7 1.956(2) . ?
Fe1 O8 1.961(2) . ?
Fe1 O9 2.002(2) . ?
Fe1 O6 2.003(2) . ?
Fe1 O5 2.047(2) . ?
Fe1 O10 2.053(2) . ?
O1 C2 1.255(4) . ?
O2 C4 1.257(4) . ?
O3 C7 1.250(4) . ?
O4 C9 1.251(4) . ?
O5 C12 1.291(4) . ?
O6 C14 1.305(4) . ?
O7 C17 1.276(4) . ?
O8 C19 1.278(4) . ?
O9 C22 1.304(4) . ?
O10 C24 1.296(3) . ?
O11 C27 1.251(4) . ?
O12 C29 1.249(4) . ?
O13 C32 1.253(4) . ?
O14 C34 1.256(4) . ?
C1 F3 1.327(4) . ?
C1 F1 1.328(4) . ?
C1 F2 1.329(4) . ?
C1 C2 1.531(5) . ?
C2 C3 1.403(5) . ?
C3 C4 1.380(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.540(4) . ?
C5 F4 1.313(4) . ?
C5 F6 1.329(4) . ?
C5 F5 1.330(4) . ?
C7 C8 1.384(5) . ?
C7 C6 1.547(5) . ?
C8 C9 1.389(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.539(4) . ?
C10 F12 1.313(4) . ?
C10 F11 1.322(4) . ?
C10 F10 1.330(4) . ?
C11 C12 1.493(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.396(4) . ?
C13 C14 1.381(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.495(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.493(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.391(4) . ?
C18 C19 1.393(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.508(5) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.496(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.382(4) . ?
C23 C24 1.392(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.492(4) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 F14 1.303(5) . ?
C26 F15 1.308(4) . ?
C26 F13 1.334(5) . ?
C26 C27 1.534(4) . ?
C27 C28 1.390(5) . ?
C28 C29 1.391(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.517(5) . ?
C31 F20 1.300(4) . ?
C31 F21 1.316(4) . ?
C31 F19 1.324(4) . ?
C31 C32 1.529(4) . ?
C32 C33 1.387(4) . ?
C33 C34 1.388(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.543(4) . ?
C35 F24 1.314(4) . ?
C35 F23 1.320(4) . ?
C35 F22 1.320(4) . ?
C30 F17 1.319(8) . ?
C30 F16 1.326(9) . ?
C30 F18 1.393(8) . ?
C6 F7 1.245(8) . ?
C6 F9 1.368(7) . ?
C6 F8 1.429(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11 Ni1 O13 175.56(10) . . ?
O11 Ni1 O12 90.63(9) . . ?
O13 Ni1 O12 88.34(9) . . ?
O11 Ni1 O14 94.91(9) . . ?
O13 Ni1 O14 89.34(9) . . ?
O12 Ni1 O14 86.60(9) . . ?
O11 Ni1 O10 88.11(8) . . ?
O13 Ni1 O10 92.40(8) . . ?
O12 Ni1 O10 173.02(9) . . ?
O14 Ni1 O10 100.34(8) . . ?
O11 Ni1 O6 92.24(9) . . ?
O13 Ni1 O6 83.61(8) . . ?
O12 Ni1 O6 97.58(9) . . ?
O14 Ni1 O6 171.67(9) . . ?
O10 Ni1 O6 75.61(8) . . ?
O2 Ni2 O4 172.63(9) . . ?
O2 Ni2 O1 89.84(9) . . ?
O4 Ni2 O1 90.53(9) . . ?
O2 Ni2 O3 98.79(9) . . ?
O4 Ni2 O3 88.57(9) . . ?
O1 Ni2 O3 89.12(9) . . ?
O2 Ni2 O5 86.70(8) . . ?
O4 Ni2 O5 91.99(9) . . ?
O1 Ni2 O5 172.03(9) . . ?
O3 Ni2 O5 98.50(8) . . ?
O2 Ni2 O9 92.36(8) . . ?
O4 Ni2 O9 80.32(8) . . ?
O1 Ni2 O9 99.22(9) . . ?
O3 Ni2 O9 166.11(8) . . ?
O5 Ni2 O9 73.77(8) . . ?
O7 Fe1 O8 87.84(9) . . ?
O7 Fe1 O9 98.90(9) . . ?
O8 Fe1 O9 99.21(9) . . ?
O7 Fe1 O6 97.97(9) . . ?
O8 Fe1 O6 96.29(9) . . ?
O9 Fe1 O6 157.44(8) . . ?
O7 Fe1 O5 87.22(9) . . ?
O8 Fe1 O5 174.94(9) . . ?
O9 Fe1 O5 80.49(8) . . ?
O6 Fe1 O5 85.49(8) . . ?
O7 Fe1 O10 170.61(9) . . ?
O8 Fe1 O10 83.20(9) . . ?
O9 Fe1 O10 85.34(8) . . ?
O6 Fe1 O10 80.30(8) . . ?
O5 Fe1 O10 101.79(8) . . ?
C2 O1 Ni2 125.6(2) . . ?
C4 O2 Ni2 125.7(2) . . ?
C7 O3 Ni2 125.2(2) . . ?
C9 O4 Ni2 126.7(2) . . ?
C12 O5 Fe1 122.15(19) . . ?
C12 O5 Ni2 131.2(2) . . ?
Fe1 O5 Ni2 103.50(9) . . ?
C14 O6 Fe1 122.89(19) . . ?
C14 O6 Ni1 120.49(18) . . ?
Fe1 O6 Ni1 101.11(9) . . ?
C17 O7 Fe1 130.0(2) . . ?
C19 O8 Fe1 129.8(2) . . ?
C22 O9 Fe1 122.68(19) . . ?
C22 O9 Ni2 120.55(18) . . ?
Fe1 O9 Ni2 101.97(9) . . ?
C24 O10 Fe1 120.09(18) . . ?
C24 O10 Ni1 132.27(19) . . ?
Fe1 O10 Ni1 102.53(9) . . ?
C27 O11 Ni1 125.2(2) . . ?
C29 O12 Ni1 123.7(2) . . ?
C32 O13 Ni1 123.4(2) . . ?
C34 O14 Ni1 122.2(2) . . ?
F3 C1 F1 107.0(3) . . ?
F3 C1 F2 107.0(3) . . ?
F1 C1 F2 107.1(3) . . ?
F3 C1 C2 113.3(3) . . ?
F1 C1 C2 111.5(3) . . ?
F2 C1 C2 110.6(3) . . ?
O1 C2 C3 128.3(3) . . ?
O1 C2 C1 113.7(3) . . ?
C3 C2 C1 118.1(3) . . ?
C4 C3 C2 121.0(3) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
O2 C4 C3 129.4(3) . . ?
O2 C4 C5 112.3(3) . . ?
C3 C4 C5 118.3(3) . . ?
F4 C5 F6 107.5(3) . . ?
F4 C5 F5 107.5(3) . . ?
F6 C5 F5 106.4(3) . . ?
F4 C5 C4 113.5(3) . . ?
F6 C5 C4 111.1(3) . . ?
F5 C5 C4 110.4(3) . . ?
O3 C7 C8 129.2(3) . . ?
O3 C7 C6 112.4(3) . . ?
C8 C7 C6 118.3(3) . . ?
C7 C8 C9 120.8(3) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
O4 C9 C8 128.4(3) . . ?
O4 C9 C10 112.4(3) . . ?
C8 C9 C10 119.2(3) . . ?
F12 C10 F11 107.2(3) . . ?
F12 C10 F10 107.4(3) . . ?
F11 C10 F10 107.9(3) . . ?
F12 C10 C9 111.2(3) . . ?
F11 C10 C9 113.0(3) . . ?
F10 C10 C9 109.8(3) . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O5 C12 C13 123.3(3) . . ?
O5 C12 C11 117.7(3) . . ?
C13 C12 C11 119.0(3) . . ?
C14 C13 C12 125.4(3) . . ?
C14 C13 H13 117.3 . . ?
C12 C13 H13 117.3 . . ?
O6 C14 C13 123.3(3) . . ?
O6 C14 C15 116.5(3) . . ?
C13 C14 C15 120.2(3) . . ?
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 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O7 C17 C18 124.5(3) . . ?
O7 C17 C16 115.5(3) . . ?
C18 C17 C16 120.0(3) . . ?
C17 C18 C19 123.2(3) . . ?
C17 C18 H18 118.4 . . ?
C19 C18 H18 118.4 . . ?
O8 C19 C18 124.2(3) . . ?
O8 C19 C20 115.5(3) . . ?
C18 C19 C20 120.3(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O9 C22 C23 123.5(3) . . ?
O9 C22 C21 116.5(3) . . ?
C23 C22 C21 120.0(3) . . ?
C22 C23 C24 125.7(3) . . ?
C22 C23 H23 117.1 . . ?
C24 C23 H23 117.1 . . ?
O10 C24 C23 122.6(3) . . ?
O10 C24 C25 117.4(3) . . ?
C23 C24 C25 119.9(3) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
F14 C26 F15 107.5(3) . . ?
F14 C26 F13 107.5(4) . . ?
F15 C26 F13 107.2(3) . . ?
F14 C26 C27 110.9(3) . . ?
F15 C26 C27 114.2(3) . . ?
F13 C26 C27 109.3(3) . . ?
O11 C27 C28 128.6(3) . . ?
O11 C27 C26 113.0(3) . . ?
C28 C27 C26 118.3(3) . . ?
C27 C28 C29 121.5(3) . . ?
C27 C28 H28 119.3 . . ?
C29 C28 H28 119.3 . . ?
O12 C29 C28 128.9(3) . . ?
O12 C29 C30 113.5(3) . . ?
C28 C29 C30 117.5(3) . . ?
F20 C31 F21 107.9(3) . . ?
F20 C31 F19 106.7(3) . . ?
F21 C31 F19 105.3(3) . . ?
F20 C31 C32 112.9(3) . . ?
F21 C31 C32 114.1(3) . . ?
F19 C31 C32 109.5(3) . . ?
O13 C32 C33 128.3(3) . . ?
O13 C32 C31 112.8(3) . . ?
C33 C32 C31 118.8(3) . . ?
C32 C33 C34 121.8(3) . . ?
C32 C33 H33 119.1 . . ?
C34 C33 H33 119.1 . . ?
O14 C34 C33 128.9(3) . . ?
O14 C34 C35 113.1(3) . . ?
C33 C34 C35 118.0(3) . . ?
F24 C35 F23 107.3(3) . . ?
F24 C35 F22 107.4(3) . . ?
F23 C35 F22 107.1(3) . . ?
F24 C35 C34 111.1(3) . . ?
F23 C35 C34 113.3(3) . . ?
F22 C35 C34 110.4(3) . . ?
F17 C30 F16 104.0(7) . . ?
F17 C30 F18 100.9(6) . . ?
F16 C30 F18 117.4(6) . . ?
F17 C30 C29 110.9(5) . . ?
F16 C30 C29 112.2(5) . . ?
F18 C30 C29 110.6(4) . . ?
F7 C6 F9 109.6(7) . . ?
F7 C6 F8 103.3(7) . . ?
F9 C6 F8 107.9(7) . . ?
F7 C6 C7 116.8(5) . . ?
F9 C6 C7 112.2(4) . . ?
F8 C6 C7 106.3(5) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.068

loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max

loop_
_publcif_info_exptl_table_header_item
?
