# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_1-123
_database_code_depnum_ccdc_archive 'CCDC 1030470'
_audit_update_record             
;
2016-10-09 deposited with the CCDC.
2016-10-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H64 Fe2 N16 O12 W'
_chemical_formula_sum            'C56 H64 Fe2 N16 O12 W'
_chemical_formula_weight         1448.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           230
_space_group_name_H-M_alt        'I a -3 d'
_space_group_name_Hall           '-I 4bd 2c 3'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+3/4, x+1/4, -z+1/4'
'-y+3/4, -x+3/4, -z+3/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/4'
'-x+1/4, z+3/4, y+1/4'
'-x+3/4, -z+3/4, -y+3/4'
'x+1/4, -z+1/4, y+3/4'
'z+3/4, y+1/4, -x+1/4'
'z+1/4, -y+1/4, x+3/4'
'-z+1/4, y+3/4, x+1/4'
'-z+3/4, -y+3/4, -x+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'y+5/4, x+3/4, -z+3/4'
'-y+5/4, -x+5/4, -z+5/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'x+5/4, z+3/4, -y+3/4'
'-x+3/4, z+5/4, y+3/4'
'-x+5/4, -z+5/4, -y+5/4'
'x+3/4, -z+3/4, y+5/4'
'z+5/4, y+3/4, -x+3/4'
'z+3/4, -y+3/4, x+5/4'
'-z+3/4, y+5/4, x+3/4'
'-z+5/4, -y+5/4, -x+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'
'-y-3/4, -x-1/4, z-1/4'
'y-3/4, x-3/4, z-3/4'
'-y-1/4, x-1/4, -z-3/4'
'y-1/4, -x-3/4, -z-1/4'
'-x-3/4, -z-1/4, y-1/4'
'x-1/4, -z-3/4, -y-1/4'
'x-3/4, z-3/4, y-3/4'
'-x-1/4, z-1/4, -y-3/4'
'-z-3/4, -y-1/4, x-1/4'
'-z-1/4, y-1/4, -x-3/4'
'z-1/4, -y-3/4, -x-1/4'
'z-3/4, y-3/4, x-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'x+1/2, -y, z'
'-x, y, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z, x, y+1/2'
'z, x+1/2, -y'
'z+1/2, -x, y'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z, x'
'-y, z, x+1/2'
'y, z+1/2, -x'
'-y-1/4, -x+1/4, z+1/4'
'y-1/4, x-1/4, z-1/4'
'-y+1/4, x+1/4, -z-1/4'
'y+1/4, -x-1/4, -z+1/4'
'-x-1/4, -z+1/4, y+1/4'
'x+1/4, -z-1/4, -y+1/4'
'x-1/4, z-1/4, y-1/4'
'-x+1/4, z+1/4, -y-1/4'
'-z-1/4, -y+1/4, x+1/4'
'-z+1/4, y+1/4, -x-1/4'
'z+1/4, -y-1/4, -x+1/4'
'z-1/4, y-1/4, x-1/4'

_cell_length_a                   34.1814(9)
_cell_length_b                   34.1814(9)
_cell_length_c                   34.1814(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     39936(3)
_cell_formula_units_Z            24
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    13055
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      25.6

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_F_000             17564
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    2.221
_shelx_estimated_absorpt_T_min   0.607
_shelx_estimated_absorpt_T_max   0.665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.592
_exptl_absorpt_correction_T_max  0.640
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            158218
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_av_R_equivalents  0.1194
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_theta_min         1.685
_diffrn_reflns_theta_max         27.495
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3837
_reflns_number_gt                2679
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0926P)²+919.6862P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3837
_refine_ls_number_parameters     227
_refine_ls_number_restraints     92
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0573
_refine_ls_wR_factor_ref         0.2101
_refine_ls_wR_factor_gt          0.1567
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0190(2) 0.7166(2) 0.0745(3) 0.0396(17) Uani 1 1 d . . . . .
C2 C 0.0521(2) 0.7783(2) 0.1045(2) 0.0360(16) Uani 1 1 d . . . . .
C3 C 0.1064(2) 0.8979(3) 0.0441(3) 0.046(2) Uani 1 1 d . . . . .
H3 H 0.1215 0.8912 0.0217 0.055 Uiso 1 1 calc R U . . .
C4 C 0.0919(3) 0.9361(3) 0.0469(3) 0.055(2) Uani 1 1 d . . . . .
C5 C 0.0692(3) 0.9453(3) 0.0788(3) 0.066(3) Uani 1 1 d . . . . .
H5 H 0.0581 0.9707 0.0815 0.079 Uiso 1 1 calc R U . . .
C6 C 0.0626(3) 0.9169(4) 0.1071(3) 0.067(3) Uani 1 1 d . . . . .
H6 H 0.0472 0.9227 0.1294 0.081 Uiso 1 1 calc R U . . .
C7 C 0.0787(3) 0.8803(3) 0.1024(3) 0.053(2) Uani 1 1 d . . . . .
H7 H 0.0745 0.8613 0.1222 0.064 Uiso 1 1 calc R U . . .
C8 C 0.1277(3) 0.7310(3) 0.0492(3) 0.063(2) Uani 1 1 d . U . . .
H8 H 0.1000 0.7327 0.0496 0.076 Uiso 1 1 calc R U . . .
C9 C 0.1459(4) 0.6962(4) 0.0387(5) 0.086(3) Uani 1 1 d D U . . .
C10 C 0.1857(4) 0.6927(4) 0.0385(4) 0.089(3) Uani 1 1 d . U . . .
H10 H 0.1978 0.6688 0.0311 0.106 Uiso 1 1 calc R U . . .
C11 C 0.2072(4) 0.7231(4) 0.0490(4) 0.078(3) Uani 1 1 d . U . . .
H11 H 0.2349 0.7211 0.0493 0.094 Uiso 1 1 calc R U . . .
C12 C 0.1896(3) 0.7574(3) 0.0592(3) 0.057(2) Uani 1 1 d . U . . .
H12 H 0.2056 0.7787 0.0668 0.068 Uiso 1 1 calc R U . . .
C13 C 0.1010(3) 0.9659(3) 0.0150(4) 0.068(3) Uani 1 1 d D . . . .
H13A H 0.1105 0.9524 -0.0073 0.103 Uiso 0.46(2) 1 d R U P A 1
H13B H 0.0784 0.9802 0.0072 0.103 Uiso 0.46(2) 1 d R U P A 1
H13C H 0.1283 0.9706 0.0173 0.103 Uiso 0.54(2) 1 d R U P A 2
H13D H 0.0961 0.9558 -0.0104 0.103 Uiso 0.54(2) 1 d R U P A 2
C14 C 0.1194(12) 0.6622(8) 0.0316(14) 0.112(4) Uani 0.46(2) 1 d D U P A 1
H14A H 0.1350 0.6391 0.0235 0.134 Uiso 0.46(2) 1 calc R U P A 1
H14B H 0.1054 0.6555 0.0560 0.134 Uiso 0.46(2) 1 calc R U P A 1
C14' C 0.1243(10) 0.6608(7) 0.0248(13) 0.113(4) Uani 0.54(2) 1 d D U P A 2
H14C H 0.1422 0.6441 0.0093 0.136 Uiso 0.54(2) 1 calc R U P A 2
H14D H 0.1153 0.6455 0.0476 0.136 Uiso 0.54(2) 1 calc R U P A 2
Fe1 Fe 0.1250 0.81617(3) 0.06617(3) 0.0327(4) Uani 1 2 d S T P . .
N1 N 0.0300(2) 0.6990(2) 0.0482(2) 0.0469(17) Uani 1 1 d . . . . .
N2 N 0.0790(2) 0.7929(2) 0.0908(2) 0.0413(16) Uani 1 1 d . . . . .
N3 N 0.10016(19) 0.8704(2) 0.0713(2) 0.0443(17) Uani 1 1 d . . . . .
N4 N 0.1500(2) 0.7625(2) 0.0589(2) 0.0459(17) Uani 1 1 d . . . . .
O2 O 0.0914(4) 0.6717(4) 0.0013(4) 0.141(4) Uani 1 1 d D U . . .
H2A H 0.0704(11) 0.679(2) -0.008(4) 0.170 Uiso 1 1 d D U . B 1
O1 O 0.1275(6) 0.9947(5) 0.0279(6) 0.075(7) Uani 0.46(2) 1 d D . P A 1
H1AC H 0.1476(10) 0.9922(19) 0.0131(10) 0.112 Uiso 0.46(2) 1 d D U P A 1
O1' O 0.0799(9) 1.0001(7) 0.0174(9) 0.179(16) Uani 0.54(2) 1 d D . P A 2
H1BB H 0.0581(13) 1.011(4) 0.022(5) 0.269 Uiso 0.54(2) 1 d D U P A 2
W1 W 0.0000 0.7500 0.1250 0.0294(2) Uani 1 4 d S T P . 2
O3 O 1.0000 1.0000 1.0000 0.113(10) Uiso 0.75 6 d S U P C 1
O4 O 0.2821(13) 0.6250 0.0321(13) 0.213(14) Uiso 0.5 2 d S U P D 1
O3' O 0.9383(9) 0.9383(9) 0.9383(9) 0.238(14) Uiso 0.75 3 d S U P E 2
O4' O 0.2500 0.6250 0.0000 0.199(16) Uiso 0.5 4 d S U P F 2
O5 O 0.1250 0.6815(10) 0.9315(10) 0.175(13) Uiso 0.5 2 d DS U P . .
H5A H 0.104(2) 0.691(3) 0.9380(16) 0.210 Uiso 0.5 1 d D U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.144(11) . ?
C1 W1 2.171(9) . ?
C2 N2 1.145(10) . ?
C2 W1 2.144(8) . ?
C3 N3 1.340(11) . ?
C3 C4 1.400(14) . ?
C3 H3 0.9500 . ?
C4 C5 1.374(15) . ?
C4 C13 1.525(14) . ?
C5 C6 1.387(16) . ?
C5 H5 0.9500 . ?
C6 C7 1.377(15) . ?
C6 H6 0.9500 . ?
C7 N3 1.336(11) . ?
C7 H7 0.9500 . ?
C8 N4 1.361(13) . ?
C8 C9 1.389(16) . ?
C8 H8 0.9500 . ?
C9 C10 1.367(19) . ?
C9 C14' 1.493(18) . ?
C9 C14 1.493(19) . ?
C10 C11 1.322(19) . ?
C10 H10 0.9500 . ?
C11 C12 1.361(15) . ?
C11 H11 0.9500 . ?
C12 N4 1.364(11) . ?
C12 H12 0.9500 . ?
C13 O1' 1.37(2) . ?
C13 O1 1.41(2) . ?
C13 H13A 0.9505 . ?
C13 H13B 0.9507 . ?
C13 H13C 0.9506 . ?
C13 H13D 0.9506 . ?
C14 O2 1.448(19) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14' O2 1.433(18) . ?
C14' H14C 0.9900 . ?
C14' H14D 0.9900 . ?
Fe1 N2 1.954(7) 18_554 ?
Fe1 N2 1.954(7) . ?
Fe1 N4 2.040(7) 18_554 ?
Fe1 N4 2.040(7) . ?
Fe1 N3 2.046(8) . ?
Fe1 N3 2.046(8) 18_554 ?
O2 H2A 0.820(2) . ?
O1 H1AC 0.86(2) . ?
O1' H1BB 0.850(2) . ?
W1 C2 2.144(8) 26_464 ?
W1 C2 2.144(8) 63_666 ?
W1 C2 2.144(8) 88_465 ?
W1 C1 2.171(9) 63_666 ?
W1 C1 2.171(9) 26_464 ?
W1 C1 2.171(9) 88_465 ?
O5 H5A 0.820(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 W1 178.4(7) . . ?
N2 C2 W1 175.0(7) . . ?
N3 C3 C4 123.3(9) . . ?
N3 C3 H3 118.3 . . ?
C4 C3 H3 118.3 . . ?
C5 C4 C3 118.0(9) . . ?
C5 C4 C13 121.9(10) . . ?
C3 C4 C13 120.1(9) . . ?
C4 C5 C6 118.8(11) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C7 C6 C5 119.4(10) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
N3 C7 C6 122.8(10) . . ?
N3 C7 H7 118.6 . . ?
C6 C7 H7 118.6 . . ?
N4 C8 C9 119.4(11) . . ?
N4 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
C10 C9 C8 121.4(12) . . ?
C10 C9 C14' 114.8(18) . . ?
C8 C9 C14' 123.7(19) . . ?
C10 C9 C14 122(2) . . ?
C8 C9 C14 116(2) . . ?
C11 C10 C9 118.9(12) . . ?
C11 C10 H10 120.6 . . ?
C9 C10 H10 120.6 . . ?
C10 C11 C12 120.1(13) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 N4 123.1(12) . . ?
C11 C12 H12 118.4 . . ?
N4 C12 H12 118.4 . . ?
O1' C13 C4 114.7(14) . . ?
O1 C13 C4 112.1(12) . . ?
O1 C13 H13A 111.7 . . ?
C4 C13 H13A 108.7 . . ?
O1 C13 H13B 104.7 . . ?
C4 C13 H13B 112.2 . . ?
H13A C13 H13B 107.4 . . ?
O1' C13 H13C 111.7 . . ?
C4 C13 H13C 104.8 . . ?
O1' C13 H13D 105.7 . . ?
C4 C13 H13D 111.9 . . ?
H13C C13 H13D 107.9 . . ?
O2 C14 C9 109.9(18) . . ?
O2 C14 H14A 109.7 . . ?
C9 C14 H14A 109.7 . . ?
O2 C14 H14B 109.7 . . ?
C9 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
O2 C14' C9 110.8(17) . . ?
O2 C14' H14C 109.5 . . ?
C9 C14' H14C 109.5 . . ?
O2 C14' H14D 109.5 . . ?
C9 C14' H14D 109.5 . . ?
H14C C14' H14D 108.1 . . ?
N2 Fe1 N2 178.0(4) 18_554 . ?
N2 Fe1 N4 91.4(3) 18_554 18_554 ?
N2 Fe1 N4 90.1(3) . 18_554 ?
N2 Fe1 N4 90.1(3) 18_554 . ?
N2 Fe1 N4 91.4(3) . . ?
N4 Fe1 N4 87.5(4) 18_554 . ?
N2 Fe1 N3 88.7(3) 18_554 . ?
N2 Fe1 N3 89.8(3) . . ?
N4 Fe1 N3 90.7(3) 18_554 . ?
N4 Fe1 N3 177.9(3) . . ?
N2 Fe1 N3 89.8(3) 18_554 18_554 ?
N2 Fe1 N3 88.7(3) . 18_554 ?
N4 Fe1 N3 177.9(3) 18_554 18_554 ?
N4 Fe1 N3 90.7(3) . 18_554 ?
N3 Fe1 N3 91.0(4) . 18_554 ?
C2 N2 Fe1 177.8(7) . . ?
C7 N3 C3 117.5(9) . . ?
C7 N3 Fe1 121.7(7) . . ?
C3 N3 Fe1 120.7(6) . . ?
C12 N4 C8 117.1(9) . . ?
C12 N4 Fe1 122.0(7) . . ?
C8 N4 Fe1 120.5(7) . . ?
C14 O2 H2A 156(10) . . ?
C13 O1 H1AC 105(5) . . ?
C13 O1' H1BB 149(10) . . ?
C2 W1 C2 141.9(4) . 26_464 ?
C2 W1 C2 96.12(13) . 63_666 ?
C2 W1 C2 96.12(13) 26_464 63_666 ?
C2 W1 C2 96.12(13) . 88_465 ?
C2 W1 C2 96.12(13) 26_464 88_465 ?
C2 W1 C2 141.9(4) 63_666 88_465 ?
C2 W1 C1 71.8(3) . 63_666 ?
C2 W1 C1 146.3(3) 26_464 63_666 ?
C2 W1 C1 74.2(3) 63_666 63_666 ?
C2 W1 C1 75.6(3) 88_465 63_666 ?
C2 W1 C1 75.6(3) . 26_464 ?
C2 W1 C1 74.2(3) 26_464 26_464 ?
C2 W1 C1 71.8(3) 63_666 26_464 ?
C2 W1 C1 146.3(3) 88_465 26_464 ?
C1 W1 C1 129.3(3) 63_666 26_464 ?
C2 W1 C1 146.3(3) . 88_465 ?
C2 W1 C1 71.8(3) 26_464 88_465 ?
C2 W1 C1 75.6(3) 63_666 88_465 ?
C2 W1 C1 74.2(3) 88_465 88_465 ?
C1 W1 C1 74.6(4) 63_666 88_465 ?
C1 W1 C1 129.3(3) 26_464 88_465 ?
C2 W1 C1 74.3(3) . . ?
C2 W1 C1 75.6(3) 26_464 . ?
C2 W1 C1 146.3(3) 63_666 . ?
C2 W1 C1 71.8(3) 88_465 . ?
C1 W1 C1 129.3(3) 63_666 . ?
C1 W1 C1 74.6(4) 26_464 . ?
C1 W1 C1 129.3(3) 88_465 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 C3 C4 C5 -1.8(15) . . . . ?
N3 C3 C4 C13 178.8(9) . . . . ?
C3 C4 C5 C6 1.7(16) . . . . ?
C13 C4 C5 C6 -178.9(10) . . . . ?
C4 C5 C6 C7 -0.4(18) . . . . ?
C5 C6 C7 N3 -1.2(17) . . . . ?
N4 C8 C9 C10 1(2) . . . . ?
N4 C8 C9 C14' -176(2) . . . . ?
N4 C8 C9 C14 175(2) . . . . ?
C8 C9 C10 C11 0(2) . . . . ?
C14' C9 C10 C11 177(2) . . . . ?
C14 C9 C10 C11 -173(2) . . . . ?
C9 C10 C11 C12 -1(2) . . . . ?
C10 C11 C12 N4 -0.7(19) . . . . ?
C5 C4 C13 O1' -10(2) . . . . ?
C3 C4 C13 O1' 169.3(19) . . . . ?
C5 C4 C13 O1 72.1(15) . . . . ?
C3 C4 C13 O1 -108.5(14) . . . . ?
C10 C9 C14 O2 -128(3) . . . . ?
C8 C9 C14 O2 58(4) . . . . ?
C10 C9 C14' O2 -141(3) . . . . ?
C8 C9 C14' O2 36(4) . . . . ?
C6 C7 N3 C3 1.2(14) . . . . ?
C6 C7 N3 Fe1 178.1(8) . . . . ?
C4 C3 N3 C7 0.4(13) . . . . ?
C4 C3 N3 Fe1 -176.7(7) . . . . ?
C11 C12 N4 C8 2.3(15) . . . . ?
C11 C12 N4 Fe1 -170.4(9) . . . . ?
C9 C8 N4 C12 -2.4(16) . . . . ?
C9 C8 N4 Fe1 170.3(10) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1AC N1 0.86(2) 2.31(3) 2.85(2) 121(4) 82_465
O5 H5A O2 0.820(2) 2.30(2) 2.67(3) 108(3) 1_556

_refine_diff_density_max         1.916
_refine_diff_density_min         -1.575
_refine_diff_density_rms         0.175

####################################################################### 
# 
# 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_1-296
_database_code_depnum_ccdc_archive 'CCDC 1030471'
_audit_update_record             
;
2016-10-09 deposited with the CCDC.
2016-10-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H64 Fe2 N16 O12 W'
_chemical_formula_sum            'C56 H64 Fe2 N16 O12 W'
_chemical_formula_weight         1448.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           230
_space_group_name_H-M_alt        'I a -3 d'
_space_group_name_Hall           '-I 4bd 2c 3'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+3/4, x+1/4, -z+1/4'
'-y+3/4, -x+3/4, -z+3/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/4'
'-x+1/4, z+3/4, y+1/4'
'-x+3/4, -z+3/4, -y+3/4'
'x+1/4, -z+1/4, y+3/4'
'z+3/4, y+1/4, -x+1/4'
'z+1/4, -y+1/4, x+3/4'
'-z+1/4, y+3/4, x+1/4'
'-z+3/4, -y+3/4, -x+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'y+5/4, x+3/4, -z+3/4'
'-y+5/4, -x+5/4, -z+5/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'x+5/4, z+3/4, -y+3/4'
'-x+3/4, z+5/4, y+3/4'
'-x+5/4, -z+5/4, -y+5/4'
'x+3/4, -z+3/4, y+5/4'
'z+5/4, y+3/4, -x+3/4'
'z+3/4, -y+3/4, x+5/4'
'-z+3/4, y+5/4, x+3/4'
'-z+5/4, -y+5/4, -x+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'
'-y-3/4, -x-1/4, z-1/4'
'y-3/4, x-3/4, z-3/4'
'-y-1/4, x-1/4, -z-3/4'
'y-1/4, -x-3/4, -z-1/4'
'-x-3/4, -z-1/4, y-1/4'
'x-1/4, -z-3/4, -y-1/4'
'x-3/4, z-3/4, y-3/4'
'-x-1/4, z-1/4, -y-3/4'
'-z-3/4, -y-1/4, x-1/4'
'-z-1/4, y-1/4, -x-3/4'
'z-1/4, -y-3/4, -x-1/4'
'z-3/4, y-3/4, x-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'x+1/2, -y, z'
'-x, y, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z, x, y+1/2'
'z, x+1/2, -y'
'z+1/2, -x, y'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z, x'
'-y, z, x+1/2'
'y, z+1/2, -x'
'-y-1/4, -x+1/4, z+1/4'
'y-1/4, x-1/4, z-1/4'
'-y+1/4, x+1/4, -z-1/4'
'y+1/4, -x-1/4, -z+1/4'
'-x-1/4, -z+1/4, y+1/4'
'x+1/4, -z-1/4, -y+1/4'
'x-1/4, z-1/4, y-1/4'
'-x+1/4, z+1/4, -y-1/4'
'-z-1/4, -y+1/4, x+1/4'
'-z+1/4, y+1/4, -x-1/4'
'z+1/4, -y-1/4, -x+1/4'
'z-1/4, y-1/4, x-1/4'

_cell_length_a                   34.8807(9)
_cell_length_b                   34.8807(9)
_cell_length_c                   34.8807(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     42438(3)
_cell_formula_units_Z            24
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    11768
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      21.8

_exptl_crystal_description       block
_exptl_crystal_colour            greeb
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_F_000             17564
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    2.091
_shelx_estimated_absorpt_T_min   0.623
_shelx_estimated_absorpt_T_max   0.680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_T_max  0.658
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            136867
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_av_R_equivalents  0.0974
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         1.651
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4076
_reflns_number_gt                2794
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0906P)²+379.2870P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4076
_refine_ls_number_parameters     227
_refine_ls_number_restraints     92
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0526
_refine_ls_wR_factor_ref         0.1894
_refine_ls_wR_factor_gt          0.1462
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0191(2) 0.7177(2) 0.0751(2) 0.0550(17) Uani 1 1 d . . . . .
C2 C 0.0504(2) 0.7791(2) 0.1061(2) 0.0511(16) Uani 1 1 d . . . . .
C3 C 0.1064(3) 0.9030(3) 0.0468(3) 0.073(2) Uani 1 1 d . . . . .
H3 H 0.1226 0.8967 0.0266 0.088 Uiso 1 1 calc R U . . .
C4 C 0.0914(3) 0.9405(3) 0.0483(3) 0.085(3) Uani 1 1 d . . . . .
C5 C 0.0673(4) 0.9489(4) 0.0774(4) 0.110(4) Uani 1 1 d . . . . .
H5 H 0.0568 0.9733 0.0794 0.132 Uiso 1 1 calc R U . . .
C6 C 0.0583(4) 0.9212(4) 0.1041(4) 0.115(4) Uani 1 1 d . . . . .
H6 H 0.0411 0.9264 0.1237 0.138 Uiso 1 1 calc R U . . .
C7 C 0.0754(3) 0.8853(3) 0.1012(3) 0.089(3) Uani 1 1 d . . . . .
H7 H 0.0703 0.8671 0.1200 0.107 Uiso 1 1 calc R U . . .
C8 C 0.1293(3) 0.7294(3) 0.0518(4) 0.101(3) Uani 1 1 d . U . . .
H8 H 0.1028 0.7313 0.0543 0.121 Uiso 1 1 calc R U . . .
C9 C 0.1455(5) 0.6956(4) 0.0405(5) 0.139(3) Uani 1 1 d D U . . .
C10 C 0.1842(5) 0.6923(5) 0.0385(5) 0.138(4) Uani 1 1 d . U . . .
H10 H 0.1952 0.6691 0.0312 0.166 Uiso 1 1 calc R U . . .
C11 C 0.2060(4) 0.7212(4) 0.0467(4) 0.126(3) Uani 1 1 d . U . . .
H11 H 0.2325 0.7190 0.0450 0.151 Uiso 1 1 calc R U . . .
C12 C 0.1891(3) 0.7557(3) 0.0580(4) 0.102(3) Uani 1 1 d . U . . .
H12 H 0.2049 0.7761 0.0646 0.122 Uiso 1 1 calc R U . . .
C13 C 0.1033(4) 0.9702(4) 0.0179(4) 0.117(4) Uani 1 1 d D . . . .
H13A H 0.1128 0.9567 -0.0045 0.176 Uiso 0.49(2) 1 d R U P A 1
H13B H 0.0807 0.9845 0.0101 0.176 Uiso 0.49(2) 1 d R U P A 1
H13C H 0.1306 0.9749 0.0201 0.176 Uiso 0.51(2) 1 d R U P A 2
H13D H 0.0984 0.9601 -0.0075 0.176 Uiso 0.51(2) 1 d R U P A 2
C14 C 0.1184(10) 0.6623(9) 0.0406(10) 0.172(5) Uani 0.49(2) 1 d D U P A 1
H14A H 0.1319 0.6382 0.0373 0.207 Uiso 0.49(2) 1 calc R U P A 1
H14B H 0.1034 0.6614 0.0639 0.207 Uiso 0.49(2) 1 calc R U P A 1
C14' C 0.1308(8) 0.6588(7) 0.0211(13) 0.178(5) Uani 0.51(2) 1 d D U P A 2
H14C H 0.1476 0.6508 0.0004 0.214 Uiso 0.51(2) 1 calc R U P A 2
H14D H 0.1282 0.6380 0.0393 0.214 Uiso 0.51(2) 1 calc R U P A 2
Fe1 Fe 0.1250 0.81796(3) 0.06796(3) 0.0529(4) Uani 1 2 d S T P . .
N1 N 0.0297(2) 0.7006(2) 0.0491(2) 0.0736(19) Uani 1 1 d . . . . .
N2 N 0.07660(18) 0.79419(19) 0.09382(19) 0.0616(16) Uani 1 1 d . . . . .
N3 N 0.09859(18) 0.8762(2) 0.0724(2) 0.0643(17) Uani 1 1 d . . . . .
N4 N 0.1517(2) 0.7604(2) 0.0595(2) 0.0724(19) Uani 1 1 d . . . . .
O2 O 0.0943(5) 0.6713(4) 0.0069(5) 0.210(4) Uani 1 1 d D U . . .
H2A H 0.0763(14) 0.679(2) -0.006(3) 0.252 Uiso 1 1 d D U . B 1
O1 O 0.1320(7) 0.9966(5) 0.0306(9) 0.157(12) Uani 0.49(2) 1 d D . P A 1
H1AC H 0.1538(10) 0.9964(17) 0.0194(13) 0.236 Uiso 0.49(2) 1 d D U P A 1
O1' O 0.0811(9) 1.0014(6) 0.0207(10) 0.225(18) Uani 0.51(2) 1 d D . P A 2
H1BB H 0.0620(13) 1.014(3) 0.029(5) 0.338 Uiso 0.51(2) 1 d D U P A 2
W1 W 0.0000 0.7500 0.1250 0.03911(19) Uani 1 4 d S T P . 2
O3 O 1.0000 1.0000 1.0000 0.325(16) Uiso 0.75 6 d S U P C 1
O4 O 0.2840(15) 0.6250 0.0340(15) 0.331(16) Uiso 0.5 2 d S U P D 1
O3' O 0.9345(9) 0.9345(9) 0.9345(9) 0.333(16) Uiso 0.75 3 d S U P E 2
O4' O 0.2500 0.6250 0.0000 0.330(16) Uiso 0.5 4 d S U P F 2
O5 O 0.1250 0.6798(14) 0.9298(14) 0.327(16) Uiso 0.5 2 d DS U P . .
H5A H 0.118(5) 0.6675(13) 0.949(2) 0.392 Uiso 0.5 1 d D U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.148(9) . ?
C1 W1 2.177(8) . ?
C2 N2 1.138(9) . ?
C2 W1 2.135(7) . ?
C3 N3 1.322(11) . ?
C3 C4 1.408(13) . ?
C3 H3 0.9300 . ?
C4 C5 1.350(15) . ?
C4 C13 1.540(15) . ?
C5 C6 1.379(17) . ?
C5 H5 0.9300 . ?
C6 C7 1.389(15) . ?
C6 H6 0.9300 . ?
C7 N3 1.328(12) . ?
C7 H7 0.9300 . ?
C8 N4 1.359(13) . ?
C8 C9 1.367(17) . ?
C8 H8 0.9300 . ?
C9 C10 1.36(2) . ?
C9 C14 1.496(18) . ?
C9 C14' 1.539(19) . ?
C10 C11 1.29(2) . ?
C10 H10 0.9300 . ?
C11 C12 1.395(16) . ?
C11 H11 0.9300 . ?
C12 N4 1.317(12) . ?
C12 H12 0.9300 . ?
C13 O1' 1.34(2) . ?
C13 O1 1.43(2) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9701 . ?
C13 H13C 0.9700 . ?
C13 H13D 0.9700 . ?
C14 O2 1.477(19) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14' O2 1.436(18) . ?
C14' H14C 0.9700 . ?
C14' H14D 0.9700 . ?
Fe1 N2 2.086(6) 18_554 ?
Fe1 N2 2.086(6) . ?
Fe1 N4 2.233(7) 18_554 ?
Fe1 N4 2.233(7) . ?
Fe1 N3 2.236(7) 18_554 ?
Fe1 N3 2.236(7) . ?
O2 H2A 0.820(2) . ?
O1 H1AC 0.86(2) . ?
O1' H1BB 0.850(2) . ?
W1 C2 2.135(7) 26_464 ?
W1 C2 2.135(7) 63_666 ?
W1 C2 2.135(7) 88_465 ?
W1 C1 2.177(8) 63_666 ?
W1 C1 2.177(8) 26_464 ?
W1 C1 2.177(8) 88_465 ?
O5 H5A 0.820(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 W1 178.8(7) . . ?
N2 C2 W1 175.8(7) . . ?
N3 C3 C4 123.7(9) . . ?
N3 C3 H3 118.2 . . ?
C4 C3 H3 118.2 . . ?
C5 C4 C3 117.5(10) . . ?
C5 C4 C13 122.5(11) . . ?
C3 C4 C13 120.0(10) . . ?
C4 C5 C6 119.6(11) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C5 C6 C7 119.2(11) . . ?
C5 C6 H6 120.4 . . ?
C7 C6 H6 120.4 . . ?
N3 C7 C6 122.0(10) . . ?
N3 C7 H7 119.0 . . ?
C6 C7 H7 119.0 . . ?
N4 C8 C9 120.4(12) . . ?
N4 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C10 C9 C8 119.8(14) . . ?
C10 C9 C14 124(2) . . ?
C8 C9 C14 114(2) . . ?
C10 C9 C14' 103.8(17) . . ?
C8 C9 C14' 135.4(17) . . ?
C11 C10 C9 120.6(15) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C10 C11 C12 119.1(14) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 H11 120.5 . . ?
N4 C12 C11 122.5(13) . . ?
N4 C12 H12 118.8 . . ?
C11 C12 H12 118.8 . . ?
O1' C13 C4 110.0(16) . . ?
O1 C13 C4 114.1(16) . . ?
O1 C13 H13A 108.8 . . ?
C4 C13 H13A 108.6 . . ?
O1 C13 H13B 109.0 . . ?
C4 C13 H13B 108.7 . . ?
H13A C13 H13B 107.4 . . ?
O1' C13 H13C 115.3 . . ?
C4 C13 H13C 108.7 . . ?
O1' C13 H13D 105.2 . . ?
C4 C13 H13D 109.6 . . ?
H13C C13 H13D 107.9 . . ?
O2 C14 C9 101.2(18) . . ?
O2 C14 H14A 111.5 . . ?
C9 C14 H14A 111.5 . . ?
O2 C14 H14B 111.5 . . ?
C9 C14 H14B 111.5 . . ?
H14A C14 H14B 109.3 . . ?
O2 C14' C9 101.1(18) . . ?
O2 C14' H14C 111.6 . . ?
C9 C14' H14C 111.6 . . ?
O2 C14' H14D 111.6 . . ?
C9 C14' H14D 111.6 . . ?
H14C C14' H14D 109.4 . . ?
N2 Fe1 N2 177.2(4) 18_554 . ?
N2 Fe1 N4 92.1(3) 18_554 18_554 ?
N2 Fe1 N4 89.9(3) . 18_554 ?
N2 Fe1 N4 89.9(3) 18_554 . ?
N2 Fe1 N4 92.1(3) . . ?
N4 Fe1 N4 86.3(4) 18_554 . ?
N2 Fe1 N3 89.9(3) 18_554 18_554 ?
N2 Fe1 N3 88.2(2) . 18_554 ?
N4 Fe1 N3 176.4(3) 18_554 18_554 ?
N4 Fe1 N3 90.6(3) . 18_554 ?
N2 Fe1 N3 88.2(2) 18_554 . ?
N2 Fe1 N3 89.9(3) . . ?
N4 Fe1 N3 90.6(3) 18_554 . ?
N4 Fe1 N3 176.4(3) . . ?
N3 Fe1 N3 92.5(4) 18_554 . ?
C2 N2 Fe1 175.1(7) . . ?
C3 N3 C7 117.9(8) . . ?
C3 N3 Fe1 120.7(6) . . ?
C7 N3 Fe1 121.3(6) . . ?
C12 N4 C8 117.5(9) . . ?
C12 N4 Fe1 122.1(7) . . ?
C8 N4 Fe1 120.1(7) . . ?
C14 O2 H2A 161(10) . . ?
C13 O1 H1AC 118(5) . . ?
C13 O1' H1BB 155(10) . . ?
C2 W1 C2 95.46(12) 26_464 63_666 ?
C2 W1 C2 95.46(12) 26_464 88_465 ?
C2 W1 C2 144.1(4) 63_666 88_465 ?
C2 W1 C2 144.1(4) 26_464 . ?
C2 W1 C2 95.46(12) 63_666 . ?
C2 W1 C2 95.46(12) 88_465 . ?
C2 W1 C1 144.9(3) 26_464 63_666 ?
C2 W1 C1 75.4(3) 63_666 63_666 ?
C2 W1 C1 76.0(3) 88_465 63_666 ?
C2 W1 C1 71.0(3) . 63_666 ?
C2 W1 C1 75.4(3) 26_464 26_464 ?
C2 W1 C1 71.0(3) 63_666 26_464 ?
C2 W1 C1 144.9(3) 88_465 26_464 ?
C2 W1 C1 76.0(3) . 26_464 ?
C1 W1 C1 129.7(2) 63_666 26_464 ?
C2 W1 C1 71.0(3) 26_464 88_465 ?
C2 W1 C1 76.0(3) 63_666 88_465 ?
C2 W1 C1 75.4(3) 88_465 88_465 ?
C2 W1 C1 144.9(3) . 88_465 ?
C1 W1 C1 73.9(4) 63_666 88_465 ?
C1 W1 C1 129.7(2) 26_464 88_465 ?
C2 W1 C1 76.0(3) 26_464 . ?
C2 W1 C1 144.9(3) 63_666 . ?
C2 W1 C1 71.0(3) 88_465 . ?
C2 W1 C1 75.4(3) . . ?
C1 W1 C1 129.7(2) 63_666 . ?
C1 W1 C1 73.9(4) 26_464 . ?
C1 W1 C1 129.7(2) 88_465 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 C3 C4 C5 -1.4(16) . . . . ?
N3 C3 C4 C13 177.7(10) . . . . ?
C3 C4 C5 C6 0(2) . . . . ?
C13 C4 C5 C6 -178.9(13) . . . . ?
C4 C5 C6 C7 2(2) . . . . ?
C5 C6 C7 N3 -3(2) . . . . ?
N4 C8 C9 C10 3(3) . . . . ?
N4 C8 C9 C14 168.6(16) . . . . ?
N4 C8 C9 C14' -163(3) . . . . ?
C8 C9 C10 C11 -1(3) . . . . ?
C14 C9 C10 C11 -165(2) . . . . ?
C14' C9 C10 C11 169(2) . . . . ?
C9 C10 C11 C12 1(3) . . . . ?
C10 C11 C12 N4 -2(2) . . . . ?
C5 C4 C13 O1' -12(3) . . . . ?
C3 C4 C13 O1' 169(2) . . . . ?
C5 C4 C13 O1 78.3(18) . . . . ?
C3 C4 C13 O1 -100.8(17) . . . . ?
C10 C9 C14 O2 -122(3) . . . . ?
C8 C9 C14 O2 73(3) . . . . ?
C10 C9 C14' O2 -153(3) . . . . ?
C8 C9 C14' O2 15(5) . . . . ?
C4 C3 N3 C7 0.1(14) . . . . ?
C4 C3 N3 Fe1 -178.5(7) . . . . ?
C6 C7 N3 C3 2.3(16) . . . . ?
C6 C7 N3 Fe1 -179.1(9) . . . . ?
C11 C12 N4 C8 3.9(18) . . . . ?
C11 C12 N4 Fe1 -169.5(10) . . . . ?
C9 C8 N4 C12 -4.3(19) . . . . ?
C9 C8 N4 Fe1 169.3(12) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1AC N1 0.86(2) 2.30(3) 2.88(3) 125(4) 82_465
O5 H5A O2 0.820(2) 2.20(2) 2.91(4) 145(8) 1_556

_refine_diff_density_max         2.130
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.135

####################################################################### 
# 
# 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 1030472'
_audit_update_record             
;
2016-10-07 deposited with the CCDC.
2016-10-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H56 Fe2 N16 W'
_chemical_formula_sum            'C56 H56 Fe2 N16 W'
_chemical_formula_weight         1248.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_H-M_alt        'F d d d'
_space_group_name_Hall           '-F 2uv 2vw'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'

_cell_length_a                   14.1192(9)
_cell_length_b                   26.6083(17)
_cell_length_c                   30.5398(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     11473.4(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    10006
_cell_measurement_theta_min      2.78
_cell_measurement_theta_max      27.4

_exptl_crystal_description       prismatic
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_F_000             5040
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    2.550
_shelx_estimated_absorpt_T_min   0.580
_shelx_estimated_absorpt_T_max   0.630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.548
_exptl_absorpt_correction_T_max  0.600
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19009
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         1.764
_diffrn_reflns_theta_max         27.593
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3328
_reflns_number_gt                3036
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0610P)²+34.9566P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3328
_refine_ls_number_parameters     174
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0273
_refine_ls_wR_factor_ref         0.0894
_refine_ls_wR_factor_gt          0.0868
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5017(3) 0.66443(13) 0.59934(11) 0.0431(7) Uani 1 1 d . . . . .
C2 C 0.5797(2) 0.57655(12) 0.57368(10) 0.0383(6) Uani 1 1 d . . . . .
C3 C 0.5009(4) 0.38976(16) 0.54012(16) 0.0655(11) Uani 1 1 d . . . . .
H3 H 0.5007 0.3814 0.5105 0.079 Uiso 1 1 calc R U . . .
C4 C 0.5004(4) 0.35153(18) 0.57000(19) 0.0746(13) Uani 1 1 d . . . . .
H4 H 0.5009 0.3184 0.5604 0.090 Uiso 1 1 calc R U . . .
C5 C 0.4992(4) 0.3615(2) 0.6135(2) 0.0738(13) Uani 1 1 d . . . . .
C6 C 0.5006(4) 0.4113(2) 0.62556(16) 0.0746(14) Uani 1 1 d . . . . .
H6 H 0.5011 0.4200 0.6550 0.089 Uiso 1 1 calc R U . . .
C7 C 0.5012(3) 0.44801(17) 0.59411(14) 0.0637(10) Uani 1 1 d . . . . .
H7 H 0.5012 0.4814 0.6032 0.076 Uiso 1 1 calc R U . . .
C8 C 0.4973(5) 0.3213(3) 0.6487(2) 0.108(2) Uani 1 1 d . . . . .
H8A H 0.4943 0.2888 0.6353 0.163 Uiso 1 1 calc R U . . .
H8B H 0.4426 0.3261 0.6670 0.163 Uiso 1 1 calc R U . . .
H8C H 0.5536 0.3237 0.6662 0.163 Uiso 1 1 calc R U . . .
C9 C 0.3284(5) 0.5448(2) 0.5551(2) 0.0916(17) Uani 1 1 d . U . . .
H9 H 0.3765 0.5530 0.5746 0.110 Uiso 1 1 calc R U . . .
C10 C 0.2356(5) 0.5577(3) 0.5670(2) 0.106(2) Uani 1 1 d . . . . .
H10 H 0.2238 0.5740 0.5934 0.127 Uiso 1 1 calc R U . . .
C11 C 0.1599(5) 0.5457(3) 0.5381(3) 0.102(2) Uani 1 1 d . . . . .
C12 C 0.1861(4) 0.5206(2) 0.4967(2) 0.0861(16) Uani 1 1 d . . . . .
H12 H 0.1413 0.5118 0.4757 0.103 Uiso 1 1 calc R U . . .
C13 C 0.2792(4) 0.5112(2) 0.49137(18) 0.0772(14) Uani 1 1 d . U . . .
H13 H 0.2955 0.4953 0.4654 0.093 Uiso 1 1 calc R U . . .
C14 C 0.0590(6) 0.5581(3) 0.5479(4) 0.152(4) Uani 1 1 d . . . . .
H14A H 0.0549 0.5736 0.5762 0.228 Uiso 1 1 calc R U . . .
H14B H 0.0219 0.5279 0.5477 0.228 Uiso 1 1 calc R U . . .
H14C H 0.0353 0.5809 0.5261 0.228 Uiso 1 1 calc R U . . .
Fe1 Fe 0.5000 0.5000 0.5000 0.04220(16) Uani 1 2 d S . P . .
N1 N 0.4367(3) 0.68485(15) 0.58677(12) 0.0653(10) Uani 1 1 d . . . . .
N2 N 0.5533(2) 0.55075(12) 0.54607(10) 0.0510(7) Uani 1 1 d . . . . .
N3 N 0.5017(2) 0.43853(12) 0.55089(11) 0.0533(7) Uani 1 1 d . . . . .
N4 N 0.3529(2) 0.52191(14) 0.51864(12) 0.0526(8) Uani 1 1 d . U . . .
W1 W 0.6250 0.6250 0.6250 0.02826(9) Uani 1 4 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.134(5) . ?
C1 W1 2.178(4) . ?
C2 N2 1.149(4) . ?
C2 W1 2.128(3) . ?
C3 N3 1.339(5) . ?
C3 C4 1.367(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.355(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.375(8) . ?
C5 C8 1.516(7) . ?
C6 C7 1.370(7) . ?
C6 H6 0.9300 . ?
C7 N3 1.344(5) . ?
C7 H7 0.9300 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N4 1.316(6) . ?
C9 C10 1.402(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.422(11) . ?
C10 H10 0.9300 . ?
C11 C12 1.477(9) . ?
C11 C14 1.494(9) . ?
C12 C13 1.348(8) . ?
C12 H12 0.9300 . ?
C13 N4 1.363(6) . ?
C13 H13 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
Fe1 N2 2.090(3) 17_666 ?
Fe1 N2 2.090(3) . ?
Fe1 N4 2.230(3) . ?
Fe1 N4 2.230(3) 17_666 ?
Fe1 N3 2.256(3) . ?
Fe1 N3 2.257(3) 17_666 ?
W1 C2 2.128(3) 8 ?
W1 C2 2.128(3) 11 ?
W1 C2 2.128(3) 14 ?
W1 C1 2.178(4) 11 ?
W1 C1 2.178(4) 8 ?
W1 C1 2.178(4) 14 ?

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
N1 C1 W1 178.6(3) . . ?
N2 C2 W1 178.5(3) . . ?
N3 C3 C4 123.9(5) . . ?
N3 C3 H3 118.1 . . ?
C4 C3 H3 118.1 . . ?
C5 C4 C3 120.6(5) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 116.8(5) . . ?
C4 C5 C8 123.9(6) . . ?
C6 C5 C8 119.3(6) . . ?
C7 C6 C5 120.0(5) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
N3 C7 C6 123.7(4) . . ?
N3 C7 H7 118.2 . . ?
C6 C7 H7 118.2 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 125.4(6) . . ?
N4 C9 H9 117.3 . . ?
C10 C9 H9 117.3 . . ?
C9 C10 C11 119.0(6) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 H10 120.5 . . ?
C10 C11 C12 116.5(6) . . ?
C10 C11 C14 122.9(7) . . ?
C12 C11 C14 120.7(8) . . ?
C13 C12 C11 115.5(6) . . ?
C13 C12 H12 122.3 . . ?
C11 C12 H12 122.3 . . ?
C12 C13 N4 129.3(5) . . ?
C12 C13 H13 115.4 . . ?
N4 C13 H13 115.4 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 Fe1 N2 180.00(17) 17_666 . ?
N2 Fe1 N4 90.33(13) 17_666 . ?
N2 Fe1 N4 89.67(13) . . ?
N2 Fe1 N4 89.67(13) 17_666 17_666 ?
N2 Fe1 N4 90.33(13) . 17_666 ?
N4 Fe1 N4 180.0 . 17_666 ?
N2 Fe1 N3 89.95(13) 17_666 . ?
N2 Fe1 N3 90.05(13) . . ?
N4 Fe1 N3 91.36(13) . . ?
N4 Fe1 N3 88.64(13) 17_666 . ?
N2 Fe1 N3 90.05(13) 17_666 17_666 ?
N2 Fe1 N3 89.95(13) . 17_666 ?
N4 Fe1 N3 88.64(13) . 17_666 ?
N4 Fe1 N3 91.36(13) 17_666 17_666 ?
N3 Fe1 N3 180.00(17) . 17_666 ?
C2 N2 Fe1 175.1(3) . . ?
C3 N3 C7 115.1(4) . . ?
C3 N3 Fe1 122.2(3) . . ?
C7 N3 Fe1 122.7(3) . . ?
C9 N4 C13 114.4(5) . . ?
C9 N4 Fe1 125.6(4) . . ?
C13 N4 Fe1 120.0(3) . . ?
C2 W1 C2 85.12(17) 8 11 ?
C2 W1 C2 105.43(18) 8 14 ?
C2 W1 C2 144.99(18) 11 14 ?
C2 W1 C2 144.99(18) 8 . ?
C2 W1 C2 105.43(18) 11 . ?
C2 W1 C2 85.12(17) 14 . ?
C2 W1 C1 74.51(13) 8 . ?
C2 W1 C1 142.86(13) 11 . ?
C2 W1 C1 71.55(13) 14 . ?
C2 W1 C1 77.67(13) . . ?
C2 W1 C1 71.55(13) 8 11 ?
C2 W1 C1 77.66(13) 11 11 ?
C2 W1 C1 74.51(13) 14 11 ?
C2 W1 C1 142.86(13) . 11 ?
C1 W1 C1 122.42(19) . 11 ?
C2 W1 C1 77.67(13) 8 8 ?
C2 W1 C1 71.55(13) 11 8 ?
C2 W1 C1 142.86(12) 14 8 ?
C2 W1 C1 74.51(13) . 8 ?
C1 W1 C1 73.91(18) . 8 ?
C1 W1 C1 137.82(17) 11 8 ?
C2 W1 C1 142.86(13) 8 14 ?
C2 W1 C1 74.51(13) 11 14 ?
C2 W1 C1 77.66(13) 14 14 ?
C2 W1 C1 71.55(13) . 14 ?
C1 W1 C1 137.82(17) . 14 ?
C1 W1 C1 73.91(18) 11 14 ?
C1 W1 C1 122.42(19) 8 14 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 C3 C4 C5 1.0(8) . . . . ?
C3 C4 C5 C6 -1.4(8) . . . . ?
C3 C4 C5 C8 179.2(5) . . . . ?
C4 C5 C6 C7 1.3(9) . . . . ?
C8 C5 C6 C7 -179.2(5) . . . . ?
C5 C6 C7 N3 -0.9(9) . . . . ?
N4 C9 C10 C11 0.2(12) . . . . ?
C9 C10 C11 C12 -0.9(11) . . . . ?
C9 C10 C11 C14 -179.8(7) . . . . ?
C10 C11 C12 C13 1.0(10) . . . . ?
C14 C11 C12 C13 179.9(7) . . . . ?
C11 C12 C13 N4 -0.4(10) . . . . ?
C4 C3 N3 C7 -0.5(7) . . . . ?
C4 C3 N3 Fe1 -178.9(4) . . . . ?
C6 C7 N3 C3 0.5(7) . . . . ?
C6 C7 N3 Fe1 178.8(4) . . . . ?
C10 C9 N4 C13 0.5(10) . . . . ?
C10 C9 N4 Fe1 -178.9(6) . . . . ?
C12 C13 N4 C9 -0.4(9) . . . . ?
C12 C13 N4 Fe1 179.0(5) . . . . ?

_refine_diff_density_max         1.715
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.096

####################################################################### 
# 
# 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 1030473'
_audit_update_record             
;
2016-10-07 deposited with the CCDC.
2016-10-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H56 Fe2 N16 O8 W'
_chemical_formula_sum            'C56 H56 Fe2 N16 O8 W'
_chemical_formula_weight         1376.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_H-M_alt        'I 41/a m d'
_space_group_name_Hall           '-I 4bd 2'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z+1/2'
'x, -y, -z'
'y+1/4, x+3/4, -z+1/4'
'-y+1/4, -x+1/4, -z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1'
'x+1/2, -y+1/2, -z+1/2'
'y+3/4, x+5/4, -z+3/4'
'-y+3/4, -x+3/4, -z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z-1/2'
'-x, y, z'
'-y-1/4, -x-3/4, z-1/4'
'y-1/4, x-1/4, z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
'-y+1/4, -x-1/4, z+1/4'
'y+1/4, x+1/4, z-1/4'

_cell_length_a                   20.2282(6)
_cell_length_b                   20.2282(6)
_cell_length_c                   13.8297(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5658.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    11768
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      21.8

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_F_000             2776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    2.604
_shelx_estimated_absorpt_T_min   0.562
_shelx_estimated_absorpt_T_max   0.624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.541
_exptl_absorpt_correction_T_max  0.594
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22827
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.014
_diffrn_reflns_theta_max         27.561
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             1734
_reflns_number_gt                1671
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0209P)²+62.2959P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1734
_refine_ls_number_parameters     128
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0306
_refine_ls_wR_factor_ref         0.0747
_refine_ls_wR_factor_gt          0.0741
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4370(2) 0.2500 0.4976(3) 0.0193(9) Uani 1 2 d S T P . .
C2 C 0.5000 0.1496(2) 0.5812(3) 0.0192(9) Uani 1 2 d S T P . .
C3 C 0.3534(3) 0.0567(3) 0.4969(3) 0.0450(11) Uani 1 1 d . . . . .
H3 H 0.3762 0.0966 0.4944 0.054 Uiso 1 1 calc R U . . .
C4 C 0.2846(3) 0.0581(3) 0.4974(4) 0.0557(14) Uani 1 1 d . . . . .
H4 H 0.2624 0.0984 0.4959 0.067 Uiso 1 1 calc R U . . .
C5 C 0.2495(4) 0.0000 0.5000 0.057(2) Uani 1 2 d S T P . .
C6 C 0.1715(5) 0.0000 0.5000 0.078(3) Uani 1 2 d DS T P . .
H6A H 0.1547 0.0366 0.5368 0.094 Uiso 0.5 1 d R U P . .
H6B H 0.1547 0.0029 0.4352 0.094 Uiso 0.5 1 d R U P . .
C7 C 0.5000 0.0035(3) 0.2733(4) 0.055(2) Uani 1 2 d S T P . .
H7 H 0.5000 -0.0420 0.2830 0.066 Uiso 1 2 calc R U P . .
C8 C 0.5000 0.0262(3) 0.1779(4) 0.0430(16) Uani 1 2 d S T P . .
H8 H 0.5000 -0.0037 0.1268 0.052 Uiso 1 2 calc R U P . .
C9 C 0.5000 0.0902(4) 0.1608(5) 0.074(3) Uani 1 2 d DS T P . .
C10 C 0.5000 0.1304(5) 0.2397(7) 0.097(3) Uani 1 2 d S TU P . .
H10 H 0.5000 0.1760 0.2312 0.117 Uiso 1 2 calc R U P . .
C11 C 0.5000 0.1046(4) 0.3317(5) 0.082(4) Uani 1 2 d S T P . .
H11 H 0.5000 0.1337 0.3838 0.099 Uiso 1 2 calc R U P . .
C12 C 0.5245(5) 0.1190(6) 0.0607(6) 0.050(2) Uani 0.5 1 d D . P . .
H12A H 0.5683 0.1046 0.0447 0.060 Uiso 0.5 1 d R U P . .
H12B H 0.5227 0.1664 0.0603 0.060 Uiso 0.5 1 d R U P . .
Fe1 Fe 0.5000 0.0000 0.5000 0.0246(2) Uani 1 4 d S T P . .
N1 N 0.4041(2) 0.2500 0.4292(3) 0.0316(11) Uani 1 2 d S T P . .
N2 N 0.5000 0.0952(2) 0.5559(3) 0.0310(11) Uani 1 2 d S T P . .
N3 N 0.5000 0.0412(2) 0.3496(3) 0.0288(10) Uani 1 2 d S T P . .
N4 N 0.3884(3) 0.0000 0.5000 0.0368(11) Uani 1 2 d S T P . .
O1 O 0.1559(5) -0.0606(3) 0.5442(7) 0.102(4) Uani 0.5 1 d D . P . .
H1C H 0.1160 -0.0696 0.5298 0.122 Uiso 0.5 1 d R U P . .
O2 O 0.4772(3) 0.0919(3) -0.0011(5) 0.0514(19) Uani 0.5 1 d D U P . .
H2C H 0.4818 0.1090 -0.0569 0.062 Uiso 0.5 1 d R U P . .
W1 W 0.5000 0.2500 0.6250 0.00903(10) Uani 1 8 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.155(6) . ?
C1 W1 2.175(5) . ?
C2 N2 1.153(6) . ?
C2 W1 2.120(5) . ?
C3 N4 1.349(6) . ?
C3 C4 1.393(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.374(7) . ?
C4 H4 0.9300 . ?
C5 C4 1.374(7) 6_556 ?
C5 C6 1.578(13) . ?
C6 O1 1.405(2) . ?
C6 O1 1.405(2) 6_556 ?
C6 H6A 0.9600 . ?
C6 H6B 0.9601 . ?
C7 N3 1.301(7) . ?
C7 C8 1.396(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.316(10) . ?
C8 H8 0.9300 . ?
C9 C10 1.361(13) . ?
C9 C12 1.582(10) . ?
C9 C12 1.582(10) 22_655 ?
C10 C11 1.376(11) . ?
C10 H10 0.9300 . ?
C11 N3 1.307(8) . ?
C11 H11 0.9300 . ?
C12 C12 0.989(19) 22_655 ?
C12 O2 1.016(10) 22_655 ?
C12 O2 1.394(10) . ?
C12 H12A 0.9599 . ?
C12 H12B 0.9599 . ?
Fe1 N2 2.076(4) 17_656 ?
Fe1 N2 2.076(4) . ?
Fe1 N3 2.241(4) 17_656 ?
Fe1 N3 2.241(4) . ?
Fe1 N4 2.257(6) 17_656 ?
Fe1 N4 2.257(6) . ?
N4 C3 1.348(6) 6_556 ?
O1 H1C 0.8501 . ?
O2 O2 0.923(13) 22_655 ?
O2 C12 1.015(10) 22_655 ?
O2 H2C 0.8499 . ?
W1 C2 2.120(5) 20_657 ?
W1 C2 2.120(5) 27_566 ?
W1 C2 2.120(5) 10_554 ?
W1 C1 2.175(5) 27_566 ?
W1 C1 2.175(5) 20_657 ?
W1 C1 2.175(5) 10_554 ?

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
N1 C1 W1 179.2(4) . . ?
N2 C2 W1 178.9(4) . . ?
N4 C3 C4 122.8(5) . . ?
N4 C3 H3 118.6 . . ?
C4 C3 H3 118.6 . . ?
C5 C4 C3 119.9(6) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C4 117.8(7) . 6_556 ?
C4 C5 C6 121.1(4) . . ?
C4 C5 C6 121.1(4) 6_556 . ?
O1 C6 O1 154.0(13) . 6_556 ?
O1 C6 C5 103.0(7) . . ?
O1 C6 C5 103.0(7) 6_556 . ?
O1 C6 H6A 111.2 . . ?
O1 C6 H6A 58.6 6_556 . ?
C5 C6 H6A 110.7 . . ?
O1 C6 H6B 112.2 . . ?
O1 C6 H6B 57.5 6_556 . ?
C5 C6 H6B 110.7 . . ?
H6A C6 H6B 108.8 . . ?
N3 C7 C8 125.0(6) . . ?
N3 C7 H7 117.5 . . ?
C8 C7 H7 117.5 . . ?
C9 C8 C7 119.5(6) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C8 C9 C10 116.4(7) . . ?
C8 C9 C12 121.3(7) . . ?
C10 C9 C12 118.7(8) . . ?
C8 C9 C12 121.3(7) . 22_655 ?
C10 C9 C12 118.7(8) . 22_655 ?
C12 C9 C12 36.4(7) . 22_655 ?
C9 C10 C11 120.9(8) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
N3 C11 C10 123.2(7) . . ?
N3 C11 H11 118.4 . . ?
C10 C11 H11 118.4 . . ?
C12 C12 O2 88.1(7) 22_655 22_655 ?
C12 C12 O2 46.7(5) 22_655 . ?
O2 C12 O2 41.4(7) 22_655 . ?
C12 C12 C9 71.8(3) 22_655 . ?
O2 C12 C9 121.9(11) 22_655 . ?
O2 C12 C9 100.2(7) . . ?
C12 C12 H12A 157.6 22_655 . ?
O2 C12 H12A 70.9 22_655 . ?
O2 C12 H12A 112.0 . . ?
C9 C12 H12A 112.3 . . ?
C12 C12 H12B 87.8 22_655 . ?
O2 C12 H12B 122.2 22_655 . ?
O2 C12 H12B 111.3 . . ?
C9 C12 H12B 111.2 . . ?
H12A C12 H12B 109.6 . . ?
N2 Fe1 N2 180.0 17_656 . ?
N2 Fe1 N3 90.08(16) 17_656 17_656 ?
N2 Fe1 N3 89.93(16) . 17_656 ?
N2 Fe1 N3 89.93(16) 17_656 . ?
N2 Fe1 N3 90.07(16) . . ?
N3 Fe1 N3 180.0 17_656 . ?
N2 Fe1 N4 90.0 17_656 17_656 ?
N2 Fe1 N4 90.0 . 17_656 ?
N3 Fe1 N4 90.0 17_656 17_656 ?
N3 Fe1 N4 90.0 . 17_656 ?
N2 Fe1 N4 90.0 17_656 . ?
N2 Fe1 N4 90.0 . . ?
N3 Fe1 N4 90.0 17_656 . ?
N3 Fe1 N4 90.0 . . ?
N4 Fe1 N4 180.0 17_656 . ?
C2 N2 Fe1 175.8(4) . . ?
C7 N3 C11 114.9(5) . . ?
C7 N3 Fe1 122.4(4) . . ?
C11 N3 Fe1 122.7(4) . . ?
C3 N4 C3 116.7(6) 6_556 . ?
C3 N4 Fe1 121.7(3) 6_556 . ?
C3 N4 Fe1 121.7(3) . . ?
C6 O1 H1C 107.4 . . ?
O2 O2 C12 91.9(7) 22_655 22_655 ?
O2 O2 C12 46.7(5) 22_655 . ?
C12 O2 C12 45.2(9) 22_655 . ?
O2 O2 H2C 83.7 22_655 . ?
C12 O2 H2C 123.2 22_655 . ?
C12 O2 H2C 108.7 . . ?
C2 W1 C2 146.8(2) 20_657 27_566 ?
C2 W1 C2 94.67(6) 20_657 10_554 ?
C2 W1 C2 94.67(6) 27_566 10_554 ?
C2 W1 C2 94.67(6) 20_657 . ?
C2 W1 C2 94.67(6) 27_566 . ?
C2 W1 C2 146.8(2) 10_554 . ?
C2 W1 C1 142.48(16) 20_657 . ?
C2 W1 C1 70.70(17) 27_566 . ?
C2 W1 C1 76.63(9) 10_554 . ?
C2 W1 C1 76.63(9) . . ?
C2 W1 C1 76.63(9) 20_657 27_566 ?
C2 W1 C1 76.63(9) 27_566 27_566 ?
C2 W1 C1 70.70(17) 10_554 27_566 ?
C2 W1 C1 142.48(16) . 27_566 ?
C1 W1 C1 131.02(15) . 27_566 ?
C2 W1 C1 76.63(9) 20_657 20_657 ?
C2 W1 C1 76.63(9) 27_566 20_657 ?
C2 W1 C1 142.48(16) 10_554 20_657 ?
C2 W1 C1 70.70(17) . 20_657 ?
C1 W1 C1 131.02(15) . 20_657 ?
C1 W1 C1 71.8(2) 27_566 20_657 ?
C2 W1 C1 70.70(17) 20_657 10_554 ?
C2 W1 C1 142.48(16) 27_566 10_554 ?
C2 W1 C1 76.63(9) 10_554 10_554 ?
C2 W1 C1 76.63(9) . 10_554 ?
C1 W1 C1 71.8(2) . 10_554 ?
C1 W1 C1 131.02(15) 27_566 10_554 ?
C1 W1 C1 131.02(15) 20_657 10_554 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 C3 C4 C5 -0.7(7) . . . . ?
C3 C4 C5 C4 0.3(3) . . . 6_556 ?
C3 C4 C5 C6 -179.7(3) . . . . ?
C4 C5 C6 O1 -155.3(5) . . . . ?
C4 C5 C6 O1 24.7(5) 6_556 . . . ?
C4 C5 C6 O1 24.7(5) . . . 6_556 ?
C4 C5 C6 O1 -155.3(5) 6_556 . . 6_556 ?
N3 C7 C8 C9 0.000(1) . . . . ?
C7 C8 C9 C10 0.000(1) . . . . ?
C7 C8 C9 C12 158.5(4) . . . . ?
C7 C8 C9 C12 -158.5(4) . . . 22_655 ?
C8 C9 C10 C11 0.000(1) . . . . ?
C12 C9 C10 C11 -159.1(4) . . . . ?
C12 C9 C10 C11 159.1(4) 22_655 . . . ?
C9 C10 C11 N3 0.000(1) . . . . ?
C8 C9 C12 C12 101.5(4) . . . 22_655 ?
C10 C9 C12 C12 -100.4(4) . . . 22_655 ?
C8 C9 C12 O2 25.7(12) . . . 22_655 ?
C10 C9 C12 O2 -176.2(9) . . . 22_655 ?
C12 C9 C12 O2 -75.8(11) 22_655 . . 22_655 ?
C8 C9 C12 O2 64.0(7) . . . . ?
C10 C9 C12 O2 -137.9(5) . . . . ?
C12 C9 C12 O2 -37.5(7) 22_655 . . . ?
C8 C7 N3 C11 0.000(1) . . . . ?
C8 C7 N3 Fe1 180.000(0) . . . . ?
C10 C11 N3 C7 0.000(1) . . . . ?
C10 C11 N3 Fe1 180.000(1) . . . . ?
C4 C3 N4 C3 0.3(3) . . . 6_556 ?
C4 C3 N4 Fe1 -179.7(3) . . . . ?
C12 C12 O2 O2 180.004(1) 22_655 . . 22_655 ?
C9 C12 O2 O2 -127.3(9) . . . 22_655 ?
O2 C12 O2 C12 179.996(1) 22_655 . . 22_655 ?
C9 C12 O2 C12 52.7(9) . . . 22_655 ?

_refine_diff_density_max         1.226
_refine_diff_density_min         -1.238
_refine_diff_density_rms         0.113

####################################################################### 
# 
# 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 1030474'
_audit_update_record             
;
2016-10-07 deposited with the CCDC.
2016-10-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H56 Fe2 N16 W'
_chemical_formula_sum            'C56 H56 Fe2 N16 W'
_chemical_formula_weight         1248.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   20.5490(18)
_cell_length_b                   20.5490(18)
_cell_length_c                   13.464(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5685.5(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3363
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      21.9

_exptl_crystal_description       prismatic
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_F_000             2520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    2.573
_shelx_estimated_absorpt_T_min   0.601
_shelx_estimated_absorpt_T_max   0.655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.573
_exptl_absorpt_correction_T_max  0.629
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18712
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.808
_diffrn_reflns_theta_max         27.612
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3286
_reflns_number_gt                2358
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0374P)²+1.9328P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3286
_refine_ls_number_parameters     182
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0853
_refine_ls_wR_factor_gt          0.0766
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.56176(19) 0.74956(18) 0.4952(4) 0.0702(12) Uani 1 1 d . . . . .
C2 C 0.50246(18) 0.64992(18) 0.5798(4) 0.0629(11) Uani 1 1 d . . . . .
C3 C 0.3648(2) 0.4389(2) 0.5566(4) 0.0906(15) Uani 1 1 d . . . . .
H3 H 0.3897 0.4012 0.5531 0.109 Uiso 1 1 calc R U . . .
C4 C 0.2994(3) 0.4321(3) 0.5778(5) 0.0977(16) Uani 1 1 d . . . . .
C5 C 0.2635(3) 0.4885(3) 0.5857(5) 0.1047(19) Uani 1 1 d . . . . .
H5 H 0.2196 0.4866 0.6022 0.126 Uiso 1 1 calc R U . . .
C6 C 0.2924(3) 0.5470(3) 0.5694(5) 0.1069(18) Uani 1 1 d . . . . .
H6 H 0.2681 0.5851 0.5726 0.128 Uiso 1 1 calc R U . . .
C7 C 0.3578(2) 0.5494(2) 0.5481(4) 0.0907(15) Uani 1 1 d . . . . .
H7 H 0.3772 0.5897 0.5384 0.109 Uiso 1 1 calc R U . . .
C8 C 0.4621(5) 0.6018(3) 0.3265(6) 0.156(3) Uani 1 1 d . . . . .
H8 H 0.4676 0.6315 0.3780 0.187 Uiso 1 1 calc R U . . .
C9 C 0.4439(7) 0.6268(5) 0.2388(8) 0.223(6) Uani 1 1 d D . . . .
H9 H 0.4371 0.6712 0.2300 0.268 Uiso 0.5 1 d R U P A .
C10 C 0.4344(5) 0.5826(6) 0.1583(8) 0.171(4) Uani 1 1 d . . . . .
H10 H 0.4219 0.5972 0.0958 0.205 Uiso 1 1 calc R U . . .
C11 C 0.4445(3) 0.5169(5) 0.1769(6) 0.123(2) Uani 1 1 d D . . . .
H11 H 0.4388 0.4857 0.1277 0.148 Uiso 0.5 1 d R U P A .
C12 C 0.4635(2) 0.5002(3) 0.2704(5) 0.1026(18) Uani 1 1 d . . . . .
H12 H 0.4706 0.4560 0.2808 0.123 Uiso 1 1 calc R U . . .
C13 C 0.2691(3) 0.3669(3) 0.5889(6) 0.143(3) Uani 1 1 d . . . . .
H13A H 0.2370 0.3683 0.6407 0.171 Uiso 1 1 calc R U . . .
H13B H 0.3020 0.3356 0.6058 0.171 Uiso 1 1 calc R U . . .
H13C H 0.2488 0.3545 0.5276 0.171 Uiso 1 1 calc R U . . .
C14 C 0.4314(7) 0.4801(7) 0.0916(10) 0.143(6) Uani 0.506(9) 1 d D . P A 1
H14A H 0.4277 0.4349 0.1088 0.214 Uiso 0.506(9) 1 d R U P A 1
H14B H 0.4665 0.4857 0.0453 0.214 Uiso 0.506(9) 1 d R U P A 1
H14C H 0.3915 0.4947 0.0620 0.214 Uiso 0.506(9) 1 d R U P A 1
C14' C 0.4351(12) 0.6918(8) 0.2092(15) 0.246(11) Uani 0.494(9) 1 d D U P A 2
H14D H 0.4645 0.7187 0.2465 0.369 Uiso 0.494(9) 1 d R U P A 2
H14E H 0.3912 0.7052 0.2221 0.369 Uiso 0.494(9) 1 d R U P A 2
H14F H 0.4442 0.6963 0.1396 0.369 Uiso 0.494(9) 1 d R U P A 2
Fe1 Fe 0.5000 0.5000 0.5000 0.0705(3) Uani 1 2 d S . P . .
N1 N 0.5944(2) 0.7477(2) 0.4267(4) 0.1007(14) Uani 1 1 d . . . . .
N2 N 0.50371(17) 0.59650(15) 0.5539(3) 0.0768(11) Uani 1 1 d . . . . .
N3 N 0.39487(18) 0.49546(16) 0.5408(3) 0.0797(11) Uani 1 1 d . . . . .
N4 N 0.4733(2) 0.53881(18) 0.3494(3) 0.0836(12) Uani 1 1 d . . . . .
W1 W 0.5000 0.7500 0.6250 0.05476(13) Uani 1 4 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.142(6) . ?
C1 W1 2.159(5) . ?
C2 N2 1.152(5) . ?
C2 W1 2.145(4) . ?
C3 N3 1.333(5) . ?
C3 C4 1.380(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.379(7) . ?
C4 C13 1.485(7) . ?
C5 C6 1.357(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.375(7) . ?
C6 H6 0.9300 . ?
C7 N3 1.348(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.342(10) . ?
C8 N4 1.351(7) . ?
C8 H8 0.9300 . ?
C9 C14' 1.406(14) . ?
C9 C10 1.429(12) . ?
C9 H9 0.9300 . ?
C10 C11 1.387(10) . ?
C10 H10 0.9300 . ?
C11 C12 1.362(9) . ?
C11 C14 1.402(13) . ?
C11 H11 0.9300 . ?
C12 N4 1.343(7) . ?
C12 H12 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H11 0.5219 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C14' H9 0.5103 . ?
C14' H14D 0.9600 . ?
C14' H14E 0.9600 . ?
C14' H14F 0.9600 . ?
Fe1 N2 2.113(3) 9_666 ?
Fe1 N2 2.113(3) . ?
Fe1 N3 2.231(4) . ?
Fe1 N3 2.231(4) 9_666 ?
Fe1 N4 2.246(4) 9_666 ?
Fe1 N4 2.246(4) . ?
W1 C2 2.145(4) 12_767 ?
W1 C2 2.145(4) 15_566 ?
W1 C2 2.145(4) 6_564 ?
W1 C1 2.159(5) 12_767 ?
W1 C1 2.159(5) 6_564 ?
W1 C1 2.159(5) 15_566 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 W1 178.3(4) . . ?
N2 C2 W1 178.9(4) . . ?
N3 C3 C4 125.0(4) . . ?
N3 C3 H3 117.5 . . ?
C4 C3 H3 117.5 . . ?
C5 C4 C3 116.8(5) . . ?
C5 C4 C13 121.8(5) . . ?
C3 C4 C13 121.4(5) . . ?
C6 C5 C4 119.9(5) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C7 119.5(5) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 H6 120.3 . . ?
N3 C7 C6 122.6(5) . . ?
N3 C7 H7 118.7 . . ?
C6 C7 H7 118.7 . . ?
C9 C8 N4 128.0(8) . . ?
C9 C8 H8 116.0 . . ?
N4 C8 H8 116.0 . . ?
C8 C9 C14' 130.5(14) . . ?
C8 C9 C10 117.6(8) . . ?
C14' C9 C10 111.9(13) . . ?
C8 C9 H9 121.9 . . ?
C14' C9 H9 9.3 . . ?
C10 C9 H9 120.5 . . ?
C11 C10 C9 117.5(8) . . ?
C11 C10 H10 121.3 . . ?
C9 C10 H10 121.3 . . ?
C12 C11 C10 117.1(8) . . ?
C12 C11 C14 132.5(10) . . ?
C10 C11 C14 110.4(10) . . ?
C12 C11 H11 121.3 . . ?
C10 C11 H11 121.6 . . ?
C14 C11 H11 11.2 . . ?
N4 C12 C11 128.8(6) . . ?
N4 C12 H12 115.6 . . ?
C11 C12 H12 115.6 . . ?
C4 C13 H13A 109.5 . . ?
C4 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C4 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H11 20.3 . . ?
C11 C14 H14A 109.9 . . ?
H11 C14 H14A 90.8 . . ?
C11 C14 H14B 108.9 . . ?
H11 C14 H14B 111.1 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.6 . . ?
H11 C14 H14C 124.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C9 C14' H9 17.0 . . ?
C9 C14' H14D 108.5 . . ?
H9 C14' H14D 97.9 . . ?
C9 C14' H14E 110.0 . . ?
H9 C14' H14E 102.4 . . ?
H14D C14' H14E 109.5 . . ?
C9 C14' H14F 110.0 . . ?
H9 C14' H14F 126.9 . . ?
H14D C14' H14F 109.5 . . ?
H14E C14' H14F 109.5 . . ?
N2 Fe1 N2 180.00(6) 9_666 . ?
N2 Fe1 N3 90.59(13) 9_666 . ?
N2 Fe1 N3 89.41(13) . . ?
N2 Fe1 N3 89.41(13) 9_666 9_666 ?
N2 Fe1 N3 90.59(13) . 9_666 ?
N3 Fe1 N3 180.0 . 9_666 ?
N2 Fe1 N4 89.19(15) 9_666 9_666 ?
N2 Fe1 N4 90.81(15) . 9_666 ?
N3 Fe1 N4 89.96(15) . 9_666 ?
N3 Fe1 N4 90.04(15) 9_666 9_666 ?
N2 Fe1 N4 90.81(15) 9_666 . ?
N2 Fe1 N4 89.19(15) . . ?
N3 Fe1 N4 90.05(15) . . ?
N3 Fe1 N4 89.95(15) 9_666 . ?
N4 Fe1 N4 180.0 9_666 . ?
C2 N2 Fe1 175.8(4) . . ?
C3 N3 C7 116.2(4) . . ?
C3 N3 Fe1 121.7(3) . . ?
C7 N3 Fe1 122.1(3) . . ?
C12 N4 C8 111.1(5) . . ?
C12 N4 Fe1 122.8(3) . . ?
C8 N4 Fe1 126.0(5) . . ?
C2 W1 C2 147.1(2) 12_767 15_566 ?
C2 W1 C2 94.61(7) 12_767 6_564 ?
C2 W1 C2 94.61(7) 15_566 6_564 ?
C2 W1 C2 94.61(7) 12_767 . ?
C2 W1 C2 94.61(7) 15_566 . ?
C2 W1 C2 147.1(2) 6_564 . ?
C2 W1 C1 70.49(16) 12_767 . ?
C2 W1 C1 142.44(17) 15_566 . ?
C2 W1 C1 77.79(15) 6_564 . ?
C2 W1 C1 75.69(15) . . ?
C2 W1 C1 75.68(15) 12_767 12_767 ?
C2 W1 C1 77.79(15) 15_566 12_767 ?
C2 W1 C1 70.49(16) 6_564 12_767 ?
C2 W1 C1 142.44(17) . 12_767 ?
C1 W1 C1 130.89(15) . 12_767 ?
C2 W1 C1 142.44(17) 12_767 6_564 ?
C2 W1 C1 70.49(16) 15_566 6_564 ?
C2 W1 C1 75.68(15) 6_564 6_564 ?
C2 W1 C1 77.79(15) . 6_564 ?
C1 W1 C1 72.0(2) . 6_564 ?
C1 W1 C1 130.89(14) 12_767 6_564 ?
C2 W1 C1 77.79(15) 12_767 15_566 ?
C2 W1 C1 75.68(15) 15_566 15_566 ?
C2 W1 C1 142.44(17) 6_564 15_566 ?
C2 W1 C1 70.49(16) . 15_566 ?
C1 W1 C1 130.89(14) . 15_566 ?
C1 W1 C1 72.0(2) 12_767 15_566 ?
C1 W1 C1 130.89(15) 6_564 15_566 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 C3 C4 C5 -1.9(10) . . . . ?
N3 C3 C4 C13 176.6(6) . . . . ?
C3 C4 C5 C6 2.3(10) . . . . ?
C13 C4 C5 C6 -176.2(7) . . . . ?
C4 C5 C6 C7 -2.0(10) . . . . ?
C5 C6 C7 N3 1.3(10) . . . . ?
N4 C8 C9 C14' -175.9(17) . . . . ?
N4 C8 C9 C10 0.6(19) . . . . ?
C8 C9 C10 C11 0.1(17) . . . . ?
C14' C9 C10 C11 177.3(14) . . . . ?
C9 C10 C11 C12 -0.8(13) . . . . ?
C9 C10 C11 C14 178.4(11) . . . . ?
C10 C11 C12 N4 1.0(11) . . . . ?
C14 C11 C12 N4 -178.0(11) . . . . ?
C4 C3 N3 C7 1.1(9) . . . . ?
C4 C3 N3 Fe1 -177.1(5) . . . . ?
C6 C7 N3 C3 -0.8(8) . . . . ?
C6 C7 N3 Fe1 177.4(5) . . . . ?
C11 C12 N4 C8 -0.3(9) . . . . ?
C11 C12 N4 Fe1 176.8(5) . . . . ?
C9 C8 N4 C12 -0.5(14) . . . . ?
C9 C8 N4 Fe1 -177.5(9) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C12 H12 N2 0.93 2.53 3.162(7) 125.7 9_666
C8 H8 N2 0.93 2.59 3.181(10) 122.3 .
C7 H7 N2 0.93 2.61 3.152(6) 117.6 .
C3 H3 N2 0.93 2.62 3.170(6) 118.3 9_666
C12 H12 N2 0.93 2.53 3.162(7) 125.7 9_666
C8 H8 N2 0.93 2.59 3.181(10) 122.3 .
C7 H7 N2 0.93 2.61 3.152(6) 117.6 .
C3 H3 N2 0.93 2.62 3.170(6) 118.3 9_666
C3 H3 N2 0.93 2.62 3.170(6) 118.3 9_666
C7 H7 N2 0.93 2.61 3.152(6) 117.6 .
C8 H8 N2 0.93 2.59 3.181(10) 122.3 .
C12 H12 N2 0.93 2.53 3.162(7) 125.7 9_666
C3 H3 N2 0.93 2.62 3.170(6) 118.3 9_666
C7 H7 N2 0.93 2.61 3.152(6) 117.6 .
C8 H8 N2 0.93 2.59 3.181(10) 122.3 .
C12 H12 N2 0.93 2.53 3.162(7) 125.7 9_666

_refine_diff_density_max         0.712
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.071

####################################################################### 
# 
# 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_1-200
_database_code_depnum_ccdc_archive 'CCDC 1469213'
_audit_update_record             
;
2016-10-09 deposited with the CCDC.
2016-10-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H64 Fe2 N16 O12 W'
_chemical_formula_sum            'C56 H64 Fe2 N16 O12 W'
_chemical_formula_weight         1448.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           230
_space_group_name_H-M_alt        'I a -3 d'
_space_group_name_Hall           '-I 4bd 2c 3'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+3/4, x+1/4, -z+1/4'
'-y+3/4, -x+3/4, -z+3/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+1/4'
'-x+1/4, z+3/4, y+1/4'
'-x+3/4, -z+3/4, -y+3/4'
'x+1/4, -z+1/4, y+3/4'
'z+3/4, y+1/4, -x+1/4'
'z+1/4, -y+1/4, x+3/4'
'-z+1/4, y+3/4, x+1/4'
'-z+3/4, -y+3/4, -x+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'y+5/4, x+3/4, -z+3/4'
'-y+5/4, -x+5/4, -z+5/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'x+5/4, z+3/4, -y+3/4'
'-x+3/4, z+5/4, y+3/4'
'-x+5/4, -z+5/4, -y+5/4'
'x+3/4, -z+3/4, y+5/4'
'z+5/4, y+3/4, -x+3/4'
'z+3/4, -y+3/4, x+5/4'
'-z+3/4, y+5/4, x+3/4'
'-z+5/4, -y+5/4, -x+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'
'-y-3/4, -x-1/4, z-1/4'
'y-3/4, x-3/4, z-3/4'
'-y-1/4, x-1/4, -z-3/4'
'y-1/4, -x-3/4, -z-1/4'
'-x-3/4, -z-1/4, y-1/4'
'x-1/4, -z-3/4, -y-1/4'
'x-3/4, z-3/4, y-3/4'
'-x-1/4, z-1/4, -y-3/4'
'-z-3/4, -y-1/4, x-1/4'
'-z-1/4, y-1/4, -x-3/4'
'z-1/4, -y-3/4, -x-1/4'
'z-3/4, y-3/4, x-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'x+1/2, -y, z'
'-x, y, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z, x, y+1/2'
'z, x+1/2, -y'
'z+1/2, -x, y'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z, x'
'-y, z, x+1/2'
'y, z+1/2, -x'
'-y-1/4, -x+1/4, z+1/4'
'y-1/4, x-1/4, z-1/4'
'-y+1/4, x+1/4, -z-1/4'
'y+1/4, -x-1/4, -z+1/4'
'-x-1/4, -z+1/4, y+1/4'
'x+1/4, -z-1/4, -y+1/4'
'x-1/4, z-1/4, y-1/4'
'-x+1/4, z+1/4, -y-1/4'
'-z-1/4, -y+1/4, x+1/4'
'-z+1/4, y+1/4, -x-1/4'
'z+1/4, -y-1/4, -x+1/4'
'z-1/4, y-1/4, x-1/4'

_cell_length_a                   34.502(3)
_cell_length_b                   34.502(3)
_cell_length_c                   34.502(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     41073(9)
_cell_formula_units_Z            24
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    7664
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      21.6

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_F_000             17564
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    2.160
_shelx_estimated_absorpt_T_min   0.614
_shelx_estimated_absorpt_T_max   0.672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.601
_exptl_absorpt_correction_T_max  0.648
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            162599
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_av_R_equivalents  0.1626
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_theta_min         1.669
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3939
_reflns_number_gt                2490
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0973P)²+673.0773P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3939
_refine_ls_number_parameters     227
_refine_ls_number_restraints     92
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.0598
_refine_ls_wR_factor_ref         0.2213
_refine_ls_wR_factor_gt          0.1617
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0188(3) 0.7172(3) 0.0747(3) 0.052(2) Uani 1 1 d . . . . .
C2 C 0.0512(2) 0.7788(2) 0.1052(3) 0.0468(19) Uani 1 1 d . . . . .
C3 C 0.1063(3) 0.9002(3) 0.0448(3) 0.066(3) Uani 1 1 d . . . . .
H3 H 0.1217 0.8934 0.0231 0.079 Uiso 1 1 calc R U . . .
C4 C 0.0918(3) 0.9384(4) 0.0469(3) 0.074(3) Uani 1 1 d . . . . .
C5 C 0.0684(4) 0.9477(4) 0.0774(4) 0.091(4) Uani 1 1 d . . . . .
H5 H 0.0574 0.9728 0.0796 0.109 Uiso 1 1 calc R U . . .
C6 C 0.0612(4) 0.9196(5) 0.1054(4) 0.098(4) Uani 1 1 d . . . . .
H6 H 0.0451 0.9254 0.1269 0.117 Uiso 1 1 calc R U . . .
C7 C 0.0775(3) 0.8832(4) 0.1018(3) 0.082(3) Uani 1 1 d . . . . .
H7 H 0.0729 0.8645 0.1215 0.098 Uiso 1 1 calc R U . . .
C8 C 0.1281(4) 0.7301(3) 0.0506(4) 0.081(3) Uani 1 1 d . U . . .
H8 H 0.1006 0.7319 0.0522 0.097 Uiso 1 1 calc R U . . .
C9 C 0.1454(5) 0.6960(4) 0.0397(5) 0.110(3) Uani 1 1 d D U . . .
C10 C 0.1850(5) 0.6922(5) 0.0387(5) 0.112(3) Uani 1 1 d . U . . .
H10 H 0.1967 0.6683 0.0315 0.135 Uiso 1 1 calc R U . . .
C11 C 0.2061(4) 0.7221(5) 0.0479(4) 0.102(3) Uani 1 1 d . U . . .
H11 H 0.2335 0.7201 0.0471 0.122 Uiso 1 1 calc R U . . .
C12 C 0.1893(3) 0.7563(4) 0.0586(4) 0.079(3) Uani 1 1 d . U . . .
H12 H 0.2055 0.7773 0.0660 0.095 Uiso 1 1 calc R U . . .
C13 C 0.1025(4) 0.9680(4) 0.0156(4) 0.096(4) Uani 1 1 d D . . . .
H13A H 0.1120 0.9545 -0.0067 0.144 Uiso 0.46(3) 1 d R U P A 1
H13B H 0.0799 0.9822 0.0078 0.144 Uiso 0.46(3) 1 d R U P A 1
H13C H 0.1298 0.9727 0.0179 0.144 Uiso 0.54(3) 1 d R U P A 2
H13D H 0.0975 0.9579 -0.0098 0.144 Uiso 0.54(3) 1 d R U P A 2
C14 C 0.1182(10) 0.6626(9) 0.0353(11) 0.138(5) Uani 0.46(3) 1 d D U P A 1
H14A H 0.1328 0.6386 0.0296 0.166 Uiso 0.46(3) 1 calc R U P A 1
H14B H 0.1032 0.6587 0.0594 0.166 Uiso 0.46(3) 1 calc R U P A 1
C14' C 0.1259(9) 0.6601(7) 0.0243(12) 0.140(4) Uani 0.54(3) 1 d D U P A 2
H14C H 0.1438 0.6457 0.0070 0.168 Uiso 0.54(3) 1 calc R U P A 2
H14D H 0.1184 0.6428 0.0460 0.168 Uiso 0.54(3) 1 calc R U P A 2
Fe1 Fe 0.1250 0.81694(4) 0.06694(4) 0.0459(4) Uani 1 2 d S T P . .
N1 N 0.0297(2) 0.6998(3) 0.0486(3) 0.065(2) Uani 1 1 d . . . . .
N2 N 0.0776(2) 0.7935(2) 0.0925(2) 0.0557(19) Uani 1 1 d . . . . .
N3 N 0.0997(2) 0.8733(3) 0.0714(2) 0.062(2) Uani 1 1 d . . . . .
N4 N 0.1507(2) 0.7612(2) 0.0590(2) 0.061(2) Uani 1 1 d . . . . .
O2 O 0.0921(4) 0.6718(4) 0.0033(5) 0.168(4) Uani 1 1 d D U . . .
H2A H 0.0720(12) 0.680(2) -0.007(4) 0.202 Uiso 1 1 d D U . B 1
O1 O 0.1297(7) 0.9958(6) 0.0282(8) 0.110(10) Uani 0.46(3) 1 d D . P A 1
H1AC H 0.1498(11) 0.993(2) 0.0140(11) 0.165 Uiso 0.46(3) 1 d D U P A 1
O1' O 0.0805(10) 1.0015(8) 0.0175(9) 0.200(18) Uani 0.54(3) 1 d D . P A 2
H1BB H 0.0613(16) 1.016(3) 0.023(4) 0.300 Uiso 0.54(3) 1 d D U P A 2
W1 W 0.0000 0.7500 0.1250 0.0403(2) Uani 1 4 d S T P . 2
O3 O 1.0000 1.0000 1.0000 0.129(11) Uiso 0.75 6 d S U P C 1
O4 O 0.2832(15) 0.6250 0.0332(15) 0.264(18) Uiso 0.5 2 d S U P D 1
O3' O 0.9355(9) 0.9355(9) 0.9355(9) 0.294(18) Uiso 0.75 3 d S U P E 2
O4' O 0.2500 0.6250 0.0000 0.25(2) Uiso 0.5 4 d S U P F 2
O5 O 0.1250 0.6815(10) 0.9315(10) 0.199(16) Uiso 0.5 2 d DS U P . .
H5A H 0.104(2) 0.689(4) 0.9398(15) 0.239 Uiso 0.5 1 d D U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.147(11) . ?
C1 W1 2.170(10) . ?
C2 N2 1.131(10) . ?
C2 W1 2.139(8) . ?
C3 N3 1.324(12) . ?
C3 C4 1.413(16) . ?
C3 H3 0.9500 . ?
C4 C5 1.365(16) . ?
C4 C13 1.531(17) . ?
C5 C6 1.390(19) . ?
C5 H5 0.9500 . ?
C6 C7 1.382(19) . ?
C6 H6 0.9500 . ?
C7 N3 1.342(14) . ?
C7 H7 0.9500 . ?
C8 N4 1.360(14) . ?
C8 C9 1.372(18) . ?
C8 H8 0.9500 . ?
C9 C10 1.37(2) . ?
C9 C14 1.494(19) . ?
C9 C14' 1.508(19) . ?
C10 C11 1.30(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.367(17) . ?
C11 H11 0.9500 . ?
C12 N4 1.341(13) . ?
C12 H12 0.9500 . ?
C13 O1' 1.39(3) . ?
C13 O1 1.41(2) . ?
C13 H13A 0.9594 . ?
C13 H13B 0.9596 . ?
C13 H13C 0.9595 . ?
C13 H13D 0.9595 . ?
C14 O2 1.458(19) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14' O2 1.430(18) . ?
C14' H14C 0.9900 . ?
C14' H14D 0.9900 . ?
Fe1 N2 2.026(7) 18_554 ?
Fe1 N2 2.026(7) . ?
Fe1 N3 2.136(9) . ?
Fe1 N3 2.136(9) 18_554 ?
Fe1 N4 2.134(8) 18_554 ?
Fe1 N4 2.134(8) . ?
O2 H2A 0.820(2) . ?
O1 H1AC 0.86(2) . ?
O1' H1BB 0.850(2) . ?
W1 C2 2.139(8) 26_464 ?
W1 C2 2.139(8) 63_666 ?
W1 C2 2.139(8) 88_465 ?
W1 C1 2.171(10) 63_666 ?
W1 C1 2.171(10) 26_464 ?
W1 C1 2.171(10) 88_465 ?
O5 H5A 0.820(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 W1 178.2(8) . . ?
N2 C2 W1 175.9(8) . . ?
N3 C3 C4 124.0(10) . . ?
N3 C3 H3 118.0 . . ?
C4 C3 H3 118.0 . . ?
C5 C4 C3 117.9(11) . . ?
C5 C4 C13 122.0(12) . . ?
C3 C4 C13 120.1(11) . . ?
C4 C5 C6 118.5(13) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
C7 C6 C5 120.0(12) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
N3 C7 C6 122.2(12) . . ?
N3 C7 H7 118.9 . . ?
C6 C7 H7 118.9 . . ?
N4 C8 C9 119.1(12) . . ?
N4 C8 H8 120.5 . . ?
C9 C8 H8 120.5 . . ?
C8 C9 C10 121.5(14) . . ?
C8 C9 C14 115(2) . . ?
C10 C9 C14 123(2) . . ?
C8 C9 C14' 127.4(18) . . ?
C10 C9 C14' 110.9(18) . . ?
C11 C10 C9 118.4(15) . . ?
C11 C10 H10 120.8 . . ?
C9 C10 H10 120.8 . . ?
C10 C11 C12 120.8(15) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
N4 C12 C11 122.3(13) . . ?
N4 C12 H12 118.9 . . ?
C11 C12 H12 118.9 . . ?
O1' C13 C4 113.1(16) . . ?
O1 C13 C4 113.5(15) . . ?
O1 C13 H13A 110.4 . . ?
C4 C13 H13A 109.0 . . ?
O1 C13 H13B 106.2 . . ?
C4 C13 H13B 110.2 . . ?
H13A C13 H13B 107.4 . . ?
O1' C13 H13C 113.3 . . ?
C4 C13 H13C 107.0 . . ?
O1' C13 H13D 104.5 . . ?
C4 C13 H13D 111.0 . . ?
H13C C13 H13D 107.9 . . ?
O2 C14 C9 107.2(19) . . ?
O2 C14 H14A 110.3 . . ?
C9 C14 H14A 110.3 . . ?
O2 C14 H14B 110.3 . . ?
C9 C14 H14B 110.3 . . ?
H14A C14 H14B 108.5 . . ?
O2 C14' C9 107.9(18) . . ?
O2 C14' H14C 110.1 . . ?
C9 C14' H14C 110.1 . . ?
O2 C14' H14D 110.1 . . ?
C9 C14' H14D 110.1 . . ?
H14C C14' H14D 108.4 . . ?
N2 Fe1 N2 177.2(5) 18_554 . ?
N2 Fe1 N3 87.9(3) 18_554 . ?
N2 Fe1 N3 90.2(3) . . ?
N2 Fe1 N3 90.2(3) 18_554 18_554 ?
N2 Fe1 N3 87.9(3) . 18_554 ?
N3 Fe1 N3 92.1(4) . 18_554 ?
N2 Fe1 N4 91.8(3) 18_554 18_554 ?
N2 Fe1 N4 90.3(3) . 18_554 ?
N3 Fe1 N4 90.6(3) . 18_554 ?
N3 Fe1 N4 176.7(3) 18_554 18_554 ?
N2 Fe1 N4 90.3(3) 18_554 . ?
N2 Fe1 N4 91.8(3) . . ?
N3 Fe1 N4 176.7(3) . . ?
N3 Fe1 N4 90.6(3) 18_554 . ?
N4 Fe1 N4 86.7(5) 18_554 . ?
C2 N2 Fe1 176.2(8) . . ?
C3 N3 C7 117.4(10) . . ?
C3 N3 Fe1 121.2(7) . . ?
C7 N3 Fe1 121.4(8) . . ?
C12 N4 C8 117.8(10) . . ?
C12 N4 Fe1 121.9(8) . . ?
C8 N4 Fe1 120.0(7) . . ?
C14 O2 H2A 156(10) . . ?
C13 O1 H1AC 107(5) . . ?
C13 O1' H1BB 158(10) . . ?
C2 W1 C2 95.88(15) 26_464 63_666 ?
C2 W1 C2 95.88(15) 26_464 88_465 ?
C2 W1 C2 142.7(5) 63_666 88_465 ?
C2 W1 C2 142.7(5) 26_464 . ?
C2 W1 C2 95.88(15) 63_666 . ?
C2 W1 C2 95.87(15) 88_465 . ?
C2 W1 C1 75.5(3) 26_464 . ?
C2 W1 C1 145.6(3) 63_666 . ?
C2 W1 C1 71.8(3) 88_465 . ?
C2 W1 C1 74.9(3) . . ?
C2 W1 C1 145.6(3) 26_464 63_666 ?
C2 W1 C1 74.9(3) 63_666 63_666 ?
C2 W1 C1 75.5(3) 88_465 63_666 ?
C2 W1 C1 71.8(3) . 63_666 ?
C1 W1 C1 129.7(3) . 63_666 ?
C2 W1 C1 74.9(3) 26_464 26_464 ?
C2 W1 C1 71.8(3) 63_666 26_464 ?
C2 W1 C1 145.6(3) 88_465 26_464 ?
C2 W1 C1 75.5(3) . 26_464 ?
C1 W1 C1 73.8(5) . 26_464 ?
C1 W1 C1 129.7(3) 63_666 26_464 ?
C2 W1 C1 71.8(3) 26_464 88_465 ?
C2 W1 C1 75.5(3) 63_666 88_465 ?
C2 W1 C1 74.9(3) 88_465 88_465 ?
C2 W1 C1 145.6(3) . 88_465 ?
C1 W1 C1 129.7(3) . 88_465 ?
C1 W1 C1 73.8(5) 63_666 88_465 ?
C1 W1 C1 129.7(3) 26_464 88_465 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 C3 C4 C5 -2.3(17) . . . . ?
N3 C3 C4 C13 177.3(11) . . . . ?
C3 C4 C5 C6 2.0(19) . . . . ?
C13 C4 C5 C6 -177.7(13) . . . . ?
C4 C5 C6 C7 0(2) . . . . ?
C5 C6 C7 N3 -2(2) . . . . ?
N4 C8 C9 C10 3(2) . . . . ?
N4 C8 C9 C14 173.7(18) . . . . ?
N4 C8 C9 C14' -171(2) . . . . ?
C8 C9 C10 C11 -1(3) . . . . ?
C14 C9 C10 C11 -171(2) . . . . ?
C14' C9 C10 C11 174(2) . . . . ?
C9 C10 C11 C12 1(3) . . . . ?
C10 C11 C12 N4 -2(2) . . . . ?
C5 C4 C13 O1' -12(3) . . . . ?
C3 C4 C13 O1' 168(2) . . . . ?
C5 C4 C13 O1 74.0(18) . . . . ?
C3 C4 C13 O1 -105.7(17) . . . . ?
C8 C9 C14 O2 65(4) . . . . ?
C10 C9 C14 O2 -125(3) . . . . ?
C8 C9 C14' O2 31(4) . . . . ?
C10 C9 C14' O2 -144(2) . . . . ?
C4 C3 N3 C7 0.6(15) . . . . ?
C4 C3 N3 Fe1 -177.3(8) . . . . ?
C6 C7 N3 C3 1.4(17) . . . . ?
C6 C7 N3 Fe1 179.3(10) . . . . ?
C11 C12 N4 C8 3.8(18) . . . . ?
C11 C12 N4 Fe1 -170.0(10) . . . . ?
C9 C8 N4 C12 -4.1(18) . . . . ?
C9 C8 N4 Fe1 169.9(11) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1AC N1 0.86(2) 2.30(3) 2.86(3) 123(4) 82_465
O5 H5A O2 0.820(2) 2.30(2) 2.74(3) 115(3) 1_556

_refine_diff_density_max         1.431
_refine_diff_density_min         -1.501
_refine_diff_density_rms         0.154

####################################################################### 
# 
# 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 1469214'
_audit_update_record             
;
2016-10-09 deposited with the CCDC.
2016-10-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H56 Fe2 N16 O8 W'
_chemical_formula_sum            'C56 H56 Fe2 N16 O8 W'
_chemical_formula_weight         1376.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_H-M_alt        'I 41/a m d'
_space_group_name_Hall           '-I 4bd 2'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z+1/2'
'x, -y, -z'
'y+1/4, x+3/4, -z+1/4'
'-y+1/4, -x+1/4, -z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1'
'x+1/2, -y+1/2, -z+1/2'
'y+3/4, x+5/4, -z+3/4'
'-y+3/4, -x+3/4, -z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z-1/2'
'-x, y, z'
'-y-1/4, -x-3/4, z-1/4'
'y-1/4, x-1/4, z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
'-y+1/4, -x-1/4, z+1/4'
'y+1/4, x+1/4, z-1/4'

_cell_length_a                   20.173(2)
_cell_length_b                   20.173(2)
_cell_length_c                   14.554(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5922.3(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2855
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      17.5

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_F_000             2776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    2.488
_shelx_estimated_absorpt_T_min   0.636
_shelx_estimated_absorpt_T_max   0.707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_T_max  0.689
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23390
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_av_R_equivalents  0.1114
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.725
_diffrn_reflns_theta_max         27.584
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             1791
_reflns_number_gt                1152
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1584P)²+12.3257P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1791
_refine_ls_number_parameters     131
_refine_ls_number_restraints     142
_refine_ls_R_factor_all          0.1357
_refine_ls_R_factor_gt           0.0967
_refine_ls_wR_factor_ref         0.2808
_refine_ls_wR_factor_gt          0.2366
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_restrained_S_all      1.265
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.5000 0.2500 0.6250 0.0691(5) Uani 1 8 d S T P . .
Fe1 Fe 0.5000 0.0000 0.5000 0.1080(13) Uani 1 4 d S T P . .
N1 N 0.5989(12) 0.2500 0.4429(12) 0.140(7) Uani 1 2 d S T P . .
N2 N 0.5000 0.0962(9) 0.5545(12) 0.114(5) Uani 1 2 d S T P . .
N4 N 0.6067(15) 0.0000 0.5000 0.178(7) Uani 1 2 d S TU P . .
O2 O 0.736(3) 0.1705(5) 0.392(3) 0.255(12) Uani 0.5 1 d D U P . .
H2A H 0.7551 0.2124 0.3559 0.382 Uiso 0.5 1 d DR U P . .
C1 C 0.5623(9) 0.2500 0.5050(14) 0.086(4) Uani 1 2 d S T P . .
C2 C 0.5000 0.1491(9) 0.5790(13) 0.091(5) Uani 1 2 d S T P . .
C3 C 0.6404(14) 0.0576(13) 0.493(2) 0.195(6) Uani 1 1 d . U . . .
H3 H 0.6177 0.0974 0.4861 0.234 Uiso 1 1 calc R U . . .
C4 C 0.7096(16) 0.0569(16) 0.497(3) 0.212(7) Uani 1 1 d D U . . .
C5 C 0.739(3) 0.0000 0.5000 0.214(9) Uani 1 2 d S TU P . .
H5 H 0.7848 0.0000 0.5000 0.257 Uiso 1 2 calc R U P . .
C6 C 0.736(3) 0.122(2) 0.463(4) 0.221(8) Uani 0.5 1 d D U P . .
H12A H 0.7276 0.1494 0.5158 0.266 Uiso 0.5 1 calc R U P . .
H12B H 0.7835 0.1127 0.4660 0.266 Uiso 0.5 1 calc R U P . .
N3 N 0.5000 0.044(4) 0.359(4) 0.299(12) Uani 1 2 d DS TU P . .
C11 C 0.5000 0.112(4) 0.350(4) 0.302(12) Uani 1 2 d DS TU P . .
C7 C 0.5000 0.010(3) 0.278(5) 0.306(13) Uani 1 2 d DS TU P . .
C9 C 0.544(3) 0.102(4) 0.200(4) 0.307(13) Uani 0.5 1 d D U P . .
C10 C 0.539(3) 0.141(2) 0.280(6) 0.307(12) Uani 0.5 1 d D U P . .
C8 C 0.5000 0.048(4) 0.198(3) 0.310(13) Uani 1 2 d DS TU P . .
C12 C 0.5000 0.205(3) 0.274(5) 0.312(13) Uani 1 2 d DS TU P . .
O1 O 0.559(2) 0.2500 0.260(3) 0.318(13) Uani 1 2 d DS TU P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C2 2.143(17) 20_657 ?
W1 C2 2.143(17) 27_566 ?
W1 C2 2.143(17) 10_554 ?
W1 C2 2.143(17) . ?
W1 C1 2.15(2) 10_554 ?
W1 C1 2.15(2) 20_657 ?
W1 C1 2.15(2) 27_566 ?
W1 C1 2.15(2) . ?
Fe1 N2 2.096(19) . ?
Fe1 N2 2.096(19) 17_656 ?
Fe1 N4 2.15(3) . ?
Fe1 N4 2.15(3) 17_656 ?
Fe1 N3 2.23(5) 17_656 ?
Fe1 N3 2.23(5) . ?
N1 C1 1.17(2) . ?
N2 C2 1.12(2) . ?
N4 C3 1.35(3) . ?
N4 C3 1.35(3) 6_556 ?
O2 C6 1.42(2) . ?
O2 H2A 1.0699 . ?
C3 C4 1.40(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.29(4) . ?
C4 C6 1.50(2) . ?
C5 C4 1.29(4) 6_556 ?
C5 H5 0.9300 . ?
C6 H12A 0.9700 . ?
C6 H12B 0.9700 . ?
N3 C11 1.37(2) . ?
N3 C7 1.37(2) . ?
C11 C10 1.405(18) 22_655 ?
C11 C10 1.405(18) . ?
C7 C8 1.40(2) . ?
C9 C10 1.407(19) . ?
C9 C8 1.412(19) . ?
C9 C9 1.77(12) 22_655 ?
C10 C12 1.51(2) . ?
C10 C10 1.56(14) 22_655 ?
C8 C9 1.412(19) 22_655 ?
C12 C10 1.51(2) 22_655 ?
C12 O1 1.517(19) . ?
C12 O1 1.517(19) 10_554 ?
C12 C12 1.83(13) 10_554 ?
O1 C12 1.517(19) 10_554 ?

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
C2 W1 C2 143.6(10) 20_657 27_566 ?
C2 W1 C2 95.6(3) 20_657 10_554 ?
C2 W1 C2 95.6(3) 27_566 10_554 ?
C2 W1 C2 95.6(3) 20_657 . ?
C2 W1 C2 95.6(3) 27_566 . ?
C2 W1 C2 143.6(10) 10_554 . ?
C2 W1 C1 143.9(7) 20_657 10_554 ?
C2 W1 C1 72.5(7) 27_566 10_554 ?
C2 W1 C1 75.3(4) 10_554 10_554 ?
C2 W1 C1 75.3(4) . 10_554 ?
C2 W1 C1 75.3(4) 20_657 20_657 ?
C2 W1 C1 75.3(4) 27_566 20_657 ?
C2 W1 C1 72.5(7) 10_554 20_657 ?
C2 W1 C1 143.9(7) . 20_657 ?
C1 W1 C1 131.2(6) 10_554 20_657 ?
C2 W1 C1 75.3(4) 20_657 27_566 ?
C2 W1 C1 75.3(4) 27_566 27_566 ?
C2 W1 C1 143.9(7) 10_554 27_566 ?
C2 W1 C1 72.5(7) . 27_566 ?
C1 W1 C1 131.2(6) 10_554 27_566 ?
C1 W1 C1 71.4(9) 20_657 27_566 ?
C2 W1 C1 72.5(7) 20_657 . ?
C2 W1 C1 143.9(7) 27_566 . ?
C2 W1 C1 75.3(4) 10_554 . ?
C2 W1 C1 75.3(4) . . ?
C1 W1 C1 71.4(9) 10_554 . ?
C1 W1 C1 131.2(6) 20_657 . ?
C1 W1 C1 131.2(6) 27_566 . ?
N2 Fe1 N2 180.0 . 17_656 ?
N2 Fe1 N4 90.000(2) . . ?
N2 Fe1 N4 90.000(1) 17_656 . ?
N2 Fe1 N4 90.000(1) . 17_656 ?
N2 Fe1 N4 90.000(2) 17_656 17_656 ?
N4 Fe1 N4 180.0 . 17_656 ?
N2 Fe1 N3 91(2) . 17_656 ?
N2 Fe1 N3 89(2) 17_656 17_656 ?
N4 Fe1 N3 90.000(2) . 17_656 ?
N4 Fe1 N3 90.000(6) 17_656 17_656 ?
N2 Fe1 N3 89(2) . . ?
N2 Fe1 N3 91(2) 17_656 . ?
N4 Fe1 N3 90.000(6) . . ?
N4 Fe1 N3 90.000(2) 17_656 . ?
N3 Fe1 N3 180.0 17_656 . ?
C2 N2 Fe1 176.3(17) . . ?
C3 N4 C3 120(3) . 6_556 ?
C3 N4 Fe1 120.2(16) . . ?
C3 N4 Fe1 120.2(16) 6_556 . ?
C6 O2 H2A 154.3 . . ?
N1 C1 W1 176.5(17) . . ?
N2 C2 W1 179.7(18) . . ?
N4 C3 C4 119(3) . . ?
N4 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 118(3) . . ?
C5 C4 C6 129(4) . . ?
C3 C4 C6 110(4) . . ?
C4 C5 C4 126(5) . 6_556 ?
C4 C5 H5 117.1 . . ?
C4 C5 H5 117.1 6_556 . ?
O2 C6 C4 147(5) . . ?
O2 C6 H12A 100.0 . . ?
C4 C6 H12A 100.0 . . ?
O2 C6 H12B 100.0 . . ?
C4 C6 H12B 100.0 . . ?
H12A C6 H12B 104.2 . . ?
C11 N3 C7 115(4) . . ?
C11 N3 Fe1 119(5) . . ?
C7 N3 Fe1 126(5) . . ?
N3 C11 C10 119(2) . 22_655 ?
N3 C11 C10 119(2) . . ?
C10 C11 C10 67(7) 22_655 . ?
N3 C7 C8 116(4) . . ?
C10 C9 C8 113.4(18) . . ?
C10 C9 C9 86(3) . 22_655 ?
C8 C9 C9 51(3) . 22_655 ?
C11 C10 C9 114.5(18) . . ?
C11 C10 C12 96(6) . . ?
C9 C10 C12 117(8) . . ?
C11 C10 C10 56(3) . 22_655 ?
C9 C10 C10 94(3) . 22_655 ?
C12 C10 C10 59(3) . 22_655 ?
C7 C8 C9 114(2) . 22_655 ?
C7 C8 C9 114(2) . . ?
C9 C8 C9 78(6) 22_655 . ?
C10 C12 C10 62(6) . 22_655 ?
C10 C12 O1 97(2) . . ?
C10 C12 O1 158(6) 22_655 . ?
C10 C12 O1 158(6) . 10_554 ?
C10 C12 O1 97(2) 22_655 10_554 ?
O1 C12 O1 104(6) . 10_554 ?
C10 C12 C12 149(3) . 10_554 ?
C10 C12 C12 149(3) 22_655 10_554 ?
O1 C12 C12 53(3) . 10_554 ?
O1 C12 C12 53(3) 10_554 10_554 ?
C12 O1 C12 74(6) 10_554 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N4 C3 C4 -2(3) 6_556 . . . ?
Fe1 N4 C3 C4 178(3) . . . . ?
N4 C3 C4 C5 5(5) . . . . ?
N4 C3 C4 C6 165(3) . . . . ?
C3 C4 C5 C4 -2(3) . . . 6_556 ?
C6 C4 C5 C4 -158(6) . . . 6_556 ?
C5 C4 C6 O2 107(11) . . . . ?
C3 C4 C6 O2 -50(11) . . . . ?
C7 N3 C11 C10 39(4) . . . 22_655 ?
Fe1 N3 C11 C10 -141(4) . . . 22_655 ?
C7 N3 C11 C10 -39(4) . . . . ?
Fe1 N3 C11 C10 141(4) . . . . ?
C11 N3 C7 C8 0.000(3) . . . . ?
Fe1 N3 C7 C8 180.000(7) . . . . ?
N3 C11 C10 C9 33(8) . . . . ?
C10 C11 C10 C9 -78(6) 22_655 . . . ?
N3 C11 C10 C12 157(5) . . . . ?
C10 C11 C10 C12 46(6) 22_655 . . . ?
N3 C11 C10 C10 112(3) . . . 22_655 ?
C8 C9 C10 C11 11(8) . . . . ?
C9 C9 C10 C11 55(5) 22_655 . . . ?
C8 C9 C10 C12 -101(6) . . . . ?
C9 C9 C10 C12 -57(4) 22_655 . . . ?
C8 C9 C10 C10 -44(5) . . . 22_655 ?
C9 C9 C10 C10 -0.001(6) 22_655 . . 22_655 ?
N3 C7 C8 C9 -43(3) . . . 22_655 ?
N3 C7 C8 C9 43(3) . . . . ?
C10 C9 C8 C7 -48(7) . . . . ?
C9 C9 C8 C7 -111(3) 22_655 . . . ?
C10 C9 C8 C9 63(6) . . . 22_655 ?
C11 C10 C12 C10 -44(6) . . . 22_655 ?
C9 C10 C12 C10 78(6) . . . 22_655 ?
C11 C10 C12 O1 141(4) . . . . ?
C9 C10 C12 O1 -97(6) . . . . ?
C10 C10 C12 O1 -175(6) 22_655 . . . ?
C11 C10 C12 O1 -58(21) . . . 10_554 ?
C9 C10 C12 O1 64(21) . . . 10_554 ?
C10 C10 C12 O1 -14(17) 22_655 . . 10_554 ?
C11 C10 C12 C12 128(6) . . . 10_554 ?
C9 C10 C12 C12 -110(7) . . . 10_554 ?
C10 C10 C12 C12 172(10) 22_655 . . 10_554 ?
C10 C12 O1 C12 -172(4) . . . 10_554 ?
C10 C12 O1 C12 176(17) 22_655 . . 10_554 ?
O1 C12 O1 C12 15(7) 10_554 . . 10_554 ?

_refine_diff_density_max         1.842
_refine_diff_density_min         -1.219
_refine_diff_density_rms         0.203

