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

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

data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1033942'
_audit_update_record             
;
2017-09-08 deposited with the CCDC.
2017-09-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C77.33 H85.60 Fe2.98 N16.67 Ni6.02 O26.80'
_chemical_formula_weight         2197.22

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_H-M_alt        'P 4/n n c'
_space_group_name_Hall           '-P 4a 2bc'

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

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

_cell_length_a                   25.3484(5)
_cell_length_b                   25.3484(5)
_cell_length_c                   25.3324(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     16277.1(7)
_cell_formula_units_Z            6
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    34419
_cell_measurement_theta_min      6.54
_cell_measurement_theta_max      72.05

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            orange-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_F_000             6760
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    4.797
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.393
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            45088
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         6.534
_diffrn_reflns_theta_max         64.994
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measured_fraction_theta_full 0.910
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_Laue_measured_fraction_full 0.910
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_point_group_measured_fraction_full 0.910
_reflns_number_total             6716
_reflns_number_gt                4762
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond ver.3.1'
_computing_publication_material  'publCIF J.Appl.Cryst. 2010, 43, 920'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0767P)²] 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         6716
_refine_ls_number_parameters     356
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.1421
_refine_ls_wR_factor_gt          0.1307
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.7500 0.2500 0.7500 0.0388(3) Uani 0.67 4 d S T P . .
Ni1A Ni 0.7500 0.2500 0.7500 0.0388(3) Uani 0.33 4 d S T P . .
Ni1 Ni 0.80012(2) 0.15367(2) 0.68108(2) 0.0484(2) Uani 0.7112 1 d . . P . .
Fe1A Fe 0.80012(2) 0.15367(2) 0.68108(2) 0.0484(2) Uani 0.2888 1 d . . P . .
Ni2 Ni 0.67911(2) 0.15557(2) 0.69860(2) 0.0506(2) Uani 0.7112 1 d . . P . .
Fe2A Fe 0.67911(2) 0.15557(2) 0.69860(2) 0.0506(2) Uani 0.2888 1 d . . P . .
N1 N 0.82543(11) 0.19600(11) 0.61492(12) 0.0556(8) Uani 1 1 d . . . . .
O1 O 0.74008(8) 0.20644(8) 0.67255(9) 0.0443(6) Uani 1 1 d . . . . .
N11 N 0.88449(11) 0.30087(11) 0.67133(12) 0.0540(8) Uani 1 1 d . . . . .
O11 O 0.82774(8) 0.20644(8) 0.74069(8) 0.0437(6) Uani 1 1 d . . . . .
O21 O 0.76982(10) 0.09302(9) 0.63297(10) 0.0591(7) Uani 1 1 d . . . . .
O22 O 0.68286(10) 0.10569(9) 0.63760(10) 0.0664(7) Uani 1 1 d . . . . .
O31 O 0.62450(10) 0.10188(8) 0.72890(10) 0.0585(7) Uani 1 1 d . . . . .
O32 O 0.63395(10) 0.11005(9) 0.81605(10) 0.0590(7) Uani 1 1 d . . . . .
O61 O 0.7500 0.12830(12) 0.7500 0.0503(8) Uani 1 2 d S T P . .
C1 C 0.86597(16) 0.18324(16) 0.58317(17) 0.0690(11) Uani 1 1 d . . . . .
H1 H 0.8857 0.1522 0.5904 0.090 Uiso 1 1 calc R U . . .
C2 C 0.87972(17) 0.21407(18) 0.54016(16) 0.0748(12) Uani 1 1 d . . . . .
H2 H 0.9079 0.2038 0.5177 0.097 Uiso 1 1 calc R U . . .
C3 C 0.85248(16) 0.25916(17) 0.53041(16) 0.0719(12) Uani 1 1 d . . . . .
H3 H 0.8622 0.2815 0.5019 0.094 Uiso 1 1 calc R U . . .
C4 C 0.81035(14) 0.27204(14) 0.56273(14) 0.0538(9) Uani 1 1 d . . . . .
H4 H 0.7904 0.3031 0.5564 0.070 Uiso 1 1 calc R U . . .
C5 C 0.79779(13) 0.23948(13) 0.60384(15) 0.0488(9) Uani 1 1 d . . . . .
C6 C 0.7500 0.2500 0.64014(19) 0.0454(12) Uani 1 2 d S T P . .
C11 C 0.91612(17) 0.31136(16) 0.63053(15) 0.0680(11) Uani 1 1 d . . . . .
H11 H 0.9074 0.3400 0.6080 0.088 Uiso 1 1 calc R U . . .
C12 C 0.96098(17) 0.28246(19) 0.61957(17) 0.0794(13) Uani 1 1 d . . . . .
H12 H 0.9833 0.2922 0.5910 0.103 Uiso 1 1 calc R U . . .
C13 C 0.97276(17) 0.24031(18) 0.64977(17) 0.0767(13) Uani 1 1 d . . . . .
H13 H 1.0032 0.2198 0.6424 0.100 Uiso 1 1 calc R U . . .
C14 C 0.93986(15) 0.22694(15) 0.69215(16) 0.0648(11) Uani 1 1 d . . . . .
H14 H 0.9467 0.1967 0.7133 0.084 Uiso 1 1 calc R U . . .
C15 C 0.89703(14) 0.25921(14) 0.70218(15) 0.0510(9) Uani 1 1 d . . . . .
C16 C 0.8607(2) 0.2500 0.7500 0.0478(12) Uani 1 2 d S T P . .
C21 C 0.72360(17) 0.08241(13) 0.62035(14) 0.0532(9) Uani 1 1 d . . . . .
C22 C 0.71377(16) 0.03845(13) 0.58279(14) 0.0691(11) Uani 1 1 d . . . . .
H22A H 0.7450 0.0333 0.5605 0.104 Uiso 1 1 calc R U . . .
H22B H 0.6834 0.0471 0.5605 0.104 Uiso 1 1 calc R U . . .
H22C H 0.7065 0.0060 0.6026 0.104 Uiso 1 1 calc R U . . .
C31 C 0.60955(15) 0.09516(13) 0.7749(2) 0.0602(11) Uani 1 1 d . . . . .
C32 C 0.55751(15) 0.06619(16) 0.78497(18) 0.0868(14) Uani 1 1 d . . . . .
H32A H 0.5336 0.0891 0.8049 0.130 Uiso 1 1 calc R U . . .
H32B H 0.5644 0.0340 0.8053 0.130 Uiso 1 1 calc R U . . .
H32C H 0.5412 0.0569 0.7512 0.130 Uiso 1 1 calc R U . . .
Fe3 Fe 0.2500 0.2500 0.2500 0.0344(4) Uani 0.6704 8 d S T P . .
Ni3A Ni 0.2500 0.2500 0.2500 0.0344(4) Uani 0.3296 8 d S T P . .
Ni3 Ni 0.23743(2) 0.16494(2) 0.34559(2) 0.0452(2) Uani 0.7112 1 d . . P . .
Fe3A Fe 0.23743(2) 0.16494(2) 0.34559(2) 0.0452(2) Uani 0.2888 1 d . . P . .
N41 N 0.20904(10) 0.10106(10) 0.30281(11) 0.0474(7) Uani 1 1 d . . . . .
O41 O 0.20210(7) 0.18900(7) 0.20631(9) 0.0384(5) Uani 1 1 d . . . . .
O51 O 0.18200(10) 0.15033(10) 0.40310(10) 0.0663(7) Uani 1 1 d . . . . .
O52 O 0.12216(9) 0.21383(9) 0.39114(9) 0.0585(7) Uani 1 1 d . . . . .
O71 O 0.2500 0.2500 0.37172(17) 0.0478(11) Uani 1 4 d S T P . .
C41 C 0.21423(13) 0.04995(13) 0.31559(17) 0.0651(11) Uani 1 1 d . . . . .
H41 H 0.2335 0.0409 0.3465 0.085 Uiso 1 1 calc R U . . .
C42 C 0.19244(15) 0.00990(14) 0.28522(19) 0.0692(12) Uani 1 1 d . . . . .
H42 H 0.1965 -0.0260 0.2951 0.090 Uiso 1 1 calc R U . . .
C43 C 0.16513(15) 0.02333(14) 0.24090(17) 0.0666(11) Uani 1 1 d . . . . .
H43 H 0.1503 -0.0033 0.2191 0.087 Uiso 1 1 calc R U . . .
C44 C 0.15920(12) 0.07569(12) 0.22780(14) 0.0505(9) Uani 1 1 d . . . . .
H44 H 0.1404 0.0855 0.1969 0.066 Uiso 1 1 calc R U . . .
C45 C 0.18080(12) 0.11369(12) 0.26011(15) 0.0451(9) Uani 1 1 d . . . . .
C46 C 0.17229(12) 0.17229(12) 0.2500 0.0404(11) Uani 1 2 d S T P . .
C51 C 0.13765(15) 0.17062(15) 0.41068(15) 0.0575(10) Uani 1 1 d . . . . .
C52 C 0.09879(17) 0.14113(16) 0.44625(17) 0.0958(15) Uani 1 1 d . . . . .
H52A H 0.0897 0.1633 0.4766 0.144 Uiso 1 1 calc R U . . .
H52B H 0.1151 0.1083 0.4587 0.144 Uiso 1 1 calc R U . . .
H52C H 0.0668 0.1328 0.4262 0.144 Uiso 1 1 calc R U . . .
H61 H 0.7500 0.0950 0.7500 0.050 Uiso 1 2 d S . P . .
H71 H 0.2500 0.2500 0.4047 0.050 Uiso 1 4 d S . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 2.265(2) . ?
Fe1 O1 2.265(2) 2_556 ?
Fe1 O1 2.265(2) 4_656 ?
Fe1 O1 2.265(2) 3_655 ?
Fe1 O11 2.271(2) . ?
Fe1 O11 2.271(2) 2_556 ?
Fe1 O11 2.271(2) 4_656 ?
Fe1 O11 2.271(2) 3_655 ?
Ni1 O32 2.005(3) 4_656 ?
Ni1 O1 2.038(2) . ?
Ni1 N1 2.091(3) . ?
Ni1 O21 2.107(2) . ?
Ni1 O11 2.135(2) . ?
Ni1 O61 2.2530(10) . ?
Ni2 O22 1.999(2) . ?
Ni2 O11 2.014(2) 4_656 ?
Ni2 N11 2.073(3) 3_655 ?
Ni2 O31 2.087(2) . ?
Ni2 O1 2.118(2) . ?
Ni2 O61 2.3242(11) . ?
N1 C5 1.336(4) . ?
N1 C1 1.344(4) . ?
O1 C6 1.399(3) . ?
N11 C11 1.335(4) . ?
N11 C15 1.352(4) . ?
N11 Fe2A 2.072(3) 3_655 ?
N11 Ni2 2.072(3) 3_655 ?
O11 C16 1.405(3) . ?
O11 Fe2A 2.014(2) 4_656 ?
O11 Ni2 2.014(2) 4_656 ?
O21 C21 1.244(4) . ?
O22 C21 1.267(4) . ?
O31 C31 1.237(5) . ?
O32 C31 1.269(4) . ?
O32 Fe1A 2.005(3) 4_656 ?
O32 Ni1 2.005(3) 4_656 ?
O61 Fe1A 2.2530(10) 4_656 ?
O61 Ni1 2.2530(10) 4_656 ?
O61 Fe2A 2.3242(11) 4_656 ?
O61 Ni2 2.3242(11) 4_656 ?
O61 H61 0.8441 . ?
C1 C2 1.385(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.358(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.385(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.366(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.544(4) . ?
C6 O1 1.399(3) 3_655 ?
C6 C5 1.544(4) 3_655 ?
C11 C12 1.381(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.347(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.401(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.383(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.539(4) . ?
C16 O11 1.405(3) 2_556 ?
C16 C15 1.539(4) 2_556 ?
C21 C22 1.486(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C31 C32 1.531(5) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
Fe3 O41 2.256(2) . ?
Fe3 O41 2.256(2) 8 ?
Fe3 O41 2.256(2) 5 ?
Fe3 O41 2.256(2) 3 ?
Fe3 O41 2.256(2) 2 ?
Fe3 O41 2.256(2) 6 ?
Fe3 O41 2.256(2) 4 ?
Fe3 O41 2.256(2) 7 ?
Ni3 O52 2.008(2) 7 ?
Ni3 O41 2.030(2) 5 ?
Ni3 O51 2.058(2) . ?
Ni3 N41 2.077(3) . ?
Ni3 O41 2.109(2) 4 ?
Ni3 O71 2.2778(14) . ?
N41 C45 1.336(4) . ?
N41 C41 1.342(4) . ?
O41 C46 1.405(3) . ?
O41 Fe3A 2.030(2) 5 ?
O41 Ni3 2.030(2) 5 ?
O41 Fe3A 2.109(2) 4 ?
O41 Ni3 2.109(2) 4 ?
O51 C51 1.251(4) . ?
O52 C51 1.264(4) . ?
O52 Fe3A 2.009(2) 6 ?
O52 Ni3 2.009(2) 6 ?
O71 Fe3A 2.2777(14) 6 ?
O71 Ni3 2.2777(14) 6 ?
O71 Fe3A 2.2777(14) 3 ?
O71 Ni3 2.2777(14) 3 ?
O71 Fe3A 2.2777(14) 7 ?
O71 Ni3 2.2777(14) 7 ?
O71 H71 0.8355 . ?
C41 C42 1.388(5) . ?
C41 H41 0.9500 . ?
C42 C43 1.362(5) . ?
C42 H42 0.9500 . ?
C43 C44 1.376(5) . ?
C43 H43 0.9500 . ?
C44 C45 1.377(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.523(4) . ?
C46 O41 1.405(3) 5 ?
C46 C45 1.523(4) 5 ?
C51 C52 1.530(5) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O1 167.25(10) . 2_556 ?
O1 Fe1 O1 121.66(11) . 4_656 ?
O1 Fe1 O1 59.98(10) 2_556 4_656 ?
O1 Fe1 O1 59.98(11) . 3_655 ?
O1 Fe1 O1 121.66(11) 2_556 3_655 ?
O1 Fe1 O1 167.26(10) 4_656 3_655 ?
O1 Fe1 O11 76.67(7) . . ?
O1 Fe1 O11 115.03(7) 2_556 . ?
O1 Fe1 O11 75.92(8) 4_656 . ?
O1 Fe1 O11 92.91(7) 3_655 . ?
O1 Fe1 O11 115.04(7) . 2_556 ?
O1 Fe1 O11 76.67(7) 2_556 2_556 ?
O1 Fe1 O11 92.91(7) 4_656 2_556 ?
O1 Fe1 O11 75.92(8) 3_655 2_556 ?
O11 Fe1 O11 59.62(10) . 2_556 ?
O1 Fe1 O11 75.92(8) . 4_656 ?
O1 Fe1 O11 92.91(7) 2_556 4_656 ?
O1 Fe1 O11 76.67(7) 4_656 4_656 ?
O1 Fe1 O11 115.03(7) 3_655 4_656 ?
O11 Fe1 O11 121.83(10) . 4_656 ?
O11 Fe1 O11 168.08(11) 2_556 4_656 ?
O1 Fe1 O11 92.91(7) . 3_655 ?
O1 Fe1 O11 75.92(8) 2_556 3_655 ?
O1 Fe1 O11 115.03(7) 4_656 3_655 ?
O1 Fe1 O11 76.67(7) 3_655 3_655 ?
O11 Fe1 O11 168.08(11) . 3_655 ?
O11 Fe1 O11 121.83(10) 2_556 3_655 ?
O11 Fe1 O11 59.61(10) 4_656 3_655 ?
O32 Ni1 O1 171.23(9) 4_656 . ?
O32 Ni1 N1 93.22(11) 4_656 . ?
O1 Ni1 N1 78.89(10) . . ?
O32 Ni1 O21 85.55(9) 4_656 . ?
O1 Ni1 O21 98.35(9) . . ?
N1 Ni1 O21 91.29(10) . . ?
O32 Ni1 O11 92.67(9) 4_656 . ?
O1 Ni1 O11 84.76(9) . . ?
N1 Ni1 O11 98.33(10) . . ?
O21 Ni1 O11 170.30(9) . . ?
O32 Ni1 O61 106.53(9) 4_656 . ?
O1 Ni1 O61 81.28(8) . . ?
N1 Ni1 O61 160.17(10) . . ?
O21 Ni1 O61 91.97(9) . . ?
O11 Ni1 O61 79.38(8) . . ?
O22 Ni2 O11 177.67(10) . 4_656 ?
O22 Ni2 N11 96.67(11) . 3_655 ?
O11 Ni2 N11 81.16(10) 4_656 3_655 ?
O22 Ni2 O31 84.46(9) . . ?
O11 Ni2 O31 94.56(9) 4_656 . ?
N11 Ni2 O31 87.37(10) 3_655 . ?
O22 Ni2 O1 96.28(9) . . ?
O11 Ni2 O1 84.90(9) 4_656 . ?
N11 Ni2 O1 98.01(10) 3_655 . ?
O31 Ni2 O1 174.44(10) . . ?
O22 Ni2 O61 102.02(9) . . ?
O11 Ni2 O61 80.18(8) 4_656 . ?
N11 Ni2 O61 161.19(10) 3_655 . ?
O31 Ni2 O61 96.48(9) . . ?
O1 Ni2 O61 77.97(8) . . ?
C5 N1 C1 118.3(3) . . ?
C5 N1 Ni1 115.5(2) . . ?
C1 N1 Ni1 126.2(3) . . ?
C6 O1 Ni1 116.49(13) . . ?
C6 O1 Ni2 142.62(14) . . ?
Ni1 O1 Ni2 96.45(9) . . ?
C6 O1 Fe1 96.0(2) . . ?
Ni1 O1 Fe1 98.35(9) . . ?
Ni2 O1 Fe1 96.19(9) . . ?
C11 N11 C15 117.5(3) . . ?
C11 N11 Fe2A 128.3(3) . 3_655 ?
C15 N11 Fe2A 114.0(2) . 3_655 ?
C11 N11 Ni2 128.3(3) . 3_655 ?
C15 N11 Ni2 114.0(2) . 3_655 ?
Fe2A N11 Ni2 0.0 3_655 3_655 ?
C16 O11 Fe2A 115.24(13) . 4_656 ?
C16 O11 Ni2 115.24(13) . 4_656 ?
Fe2A O11 Ni2 0.0 4_656 4_656 ?
C16 O11 Ni1 143.72(15) . . ?
Fe2A O11 Ni1 96.35(8) 4_656 . ?
Ni2 O11 Ni1 96.35(8) 4_656 . ?
C16 O11 Fe1 96.7(2) . . ?
Fe2A O11 Fe1 99.04(9) 4_656 . ?
Ni2 O11 Fe1 99.04(9) 4_656 . ?
Ni1 O11 Fe1 95.36(8) . . ?
C21 O21 Ni1 130.5(2) . . ?
C21 O22 Ni2 126.9(2) . . ?
C31 O31 Ni2 129.7(3) . . ?
C31 O32 Fe1A 126.9(2) . 4_656 ?
C31 O32 Ni1 126.9(2) . 4_656 ?
Fe1A O32 Ni1 0.0 4_656 4_656 ?
Fe1A O61 Ni1 0.0 4_656 4_656 ?
Fe1A O61 Ni1 146.8 4_656 . ?
Ni1 O61 Ni1 146.83(15) 4_656 . ?
Fe1A O61 Ni2 85.02(4) 4_656 . ?
Ni1 O61 Ni2 85.02(4) 4_656 . ?
Ni1 O61 Ni2 85.24(4) . . ?
Fe1A O61 Fe2A 85.24(4) 4_656 4_656 ?
Ni1 O61 Fe2A 85.24(4) 4_656 4_656 ?
Ni1 O61 Fe2A 85.02(4) . 4_656 ?
Ni2 O61 Fe2A 145.4 . 4_656 ?
Fe1A O61 Ni2 85.24(4) 4_656 4_656 ?
Ni1 O61 Ni2 85.24(4) 4_656 4_656 ?
Ni1 O61 Ni2 85.02(4) . 4_656 ?
Ni2 O61 Ni2 145.39(14) . 4_656 ?
Fe2A O61 Ni2 0.0 4_656 4_656 ?
Fe1A O61 H61 106.6 4_656 . ?
Ni1 O61 H61 106.6 4_656 . ?
Ni1 O61 H61 106.6 . . ?
Ni2 O61 H61 107.3 . . ?
Fe2A O61 H61 107.3 4_656 . ?
Ni2 O61 H61 107.3 4_656 . ?
N1 C1 C2 121.8(4) . . ?
N1 C1 H1 119.1 . . ?
C2 C1 H1 119.1 . . ?
C3 C2 C1 119.3(4) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C4 118.9(4) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C5 C4 C3 119.2(4) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
N1 C5 C4 122.4(4) . . ?
N1 C5 C6 115.4(3) . . ?
C4 C5 C6 122.2(3) . . ?
O1 C6 O1 108.1(4) 3_655 . ?
O1 C6 C5 110.75(15) 3_655 3_655 ?
O1 C6 C5 110.17(15) . 3_655 ?
O1 C6 C5 110.17(15) 3_655 . ?
O1 C6 C5 110.75(15) . . ?
C5 C6 C5 106.9(4) 3_655 . ?
N11 C11 C12 123.0(4) . . ?
N11 C11 H11 118.5 . . ?
C12 C11 H11 118.5 . . ?
C13 C12 C11 119.3(4) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C12 C13 C14 119.7(4) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C15 C14 C13 117.7(4) . . ?
C15 C14 H14 121.1 . . ?
C13 C14 H14 121.1 . . ?
N11 C15 C14 122.7(3) . . ?
N11 C15 C16 115.6(3) . . ?
C14 C15 C16 121.6(3) . . ?
O11 C16 O11 107.0(4) 2_556 . ?
O11 C16 C15 110.06(15) 2_556 2_556 ?
O11 C16 C15 111.63(16) . 2_556 ?
O11 C16 C15 111.64(16) 2_556 . ?
O11 C16 C15 110.06(15) . . ?
C15 C16 C15 106.5(4) 2_556 . ?
O21 C21 O22 125.3(3) . . ?
O21 C21 C22 119.0(4) . . ?
O22 C21 C22 115.7(4) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O31 C31 O32 125.7(4) . . ?
O31 C31 C32 119.1(4) . . ?
O32 C31 C32 115.2(4) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O41 Fe3 O41 168.05(9) . 8 ?
O41 Fe3 O41 60.20(11) . 5 ?
O41 Fe3 O41 121.24(11) 8 5 ?
O41 Fe3 O41 121.24(11) . 3 ?
O41 Fe3 O41 60.20(11) 8 3 ?
O41 Fe3 O41 168.05(9) 5 3 ?
O41 Fe3 O41 114.89(10) . 2 ?
O41 Fe3 O41 76.07(5) 8 2 ?
O41 Fe3 O41 76.07(5) 5 2 ?
O41 Fe3 O41 93.47(10) 3 2 ?
O41 Fe3 O41 76.07(5) . 6 ?
O41 Fe3 O41 114.89(10) 8 6 ?
O41 Fe3 O41 93.47(10) 5 6 ?
O41 Fe3 O41 76.07(5) 3 6 ?
O41 Fe3 O41 60.20(11) 2 6 ?
O41 Fe3 O41 93.47(10) . 4 ?
O41 Fe3 O41 76.07(5) 8 4 ?
O41 Fe3 O41 76.07(5) 5 4 ?
O41 Fe3 O41 114.89(10) 3 4 ?
O41 Fe3 O41 121.24(11) 2 4 ?
O41 Fe3 O41 168.05(9) 6 4 ?
O41 Fe3 O41 76.07(5) . 7 ?
O41 Fe3 O41 93.47(10) 8 7 ?
O41 Fe3 O41 114.89(10) 5 7 ?
O41 Fe3 O41 76.07(5) 3 7 ?
O41 Fe3 O41 168.05(9) 2 7 ?
O41 Fe3 O41 121.24(11) 6 7 ?
O41 Fe3 O41 60.20(11) 4 7 ?
O52 Ni3 O41 173.93(9) 7 5 ?
O52 Ni3 O51 85.18(9) 7 . ?
O41 Ni3 O51 97.42(9) 5 . ?
O52 Ni3 N41 95.27(10) 7 . ?
O41 Ni3 N41 79.31(9) 5 . ?
O51 Ni3 N41 89.57(11) . . ?
O52 Ni3 O41 93.85(9) 7 4 ?
O41 Ni3 O41 84.36(11) 5 4 ?
O51 Ni3 O41 171.69(10) . 4 ?
N41 Ni3 O41 98.74(9) . 4 ?
O52 Ni3 O71 104.96(10) 7 . ?
O41 Ni3 O71 80.42(10) 5 . ?
O51 Ni3 O71 93.45(11) . . ?
N41 Ni3 O71 159.73(11) . . ?
O41 Ni3 O71 78.81(9) 4 . ?
C45 N41 C41 118.6(3) . . ?
C45 N41 Ni3 114.9(2) . . ?
C41 N41 Ni3 126.4(3) . . ?
C46 O41 Fe3A 116.28(11) . 5 ?
C46 O41 Ni3 116.28(11) . 5 ?
Fe3A O41 Ni3 0.0 5 5 ?
C46 O41 Fe3A 142.60(13) . 4 ?
Fe3A O41 Fe3A 96.22(10) 5 4 ?
Ni3 O41 Fe3A 96.22(10) 5 4 ?
C46 O41 Ni3 142.60(13) . 4 ?
Fe3A O41 Ni3 96.2 5 4 ?
Ni3 O41 Ni3 96.22(10) 5 4 ?
Fe3A O41 Ni3 0.0 4 4 ?
C46 O41 Fe3 96.28(19) . . ?
Fe3A O41 Fe3 98.79(8) 5 . ?
Ni3 O41 Fe3 98.79(8) 5 . ?
Fe3A O41 Fe3 96.48(7) 4 . ?
Ni3 O41 Fe3 96.48(7) 4 . ?
C51 O51 Ni3 130.4(2) . . ?
C51 O52 Fe3A 126.2(2) . 6 ?
C51 O52 Ni3 126.2(2) . 6 ?
Fe3A O52 Ni3 0.0 6 6 ?
Fe3A O71 Ni3 0.0 6 6 ?
Fe3A O71 Fe3A 85.15(6) 6 3 ?
Ni3 O71 Fe3A 85.15(6) 6 3 ?
Fe3A O71 Ni3 85.2 6 3 ?
Ni3 O71 Ni3 85.15(6) 6 3 ?
Fe3A O71 Ni3 0.0 3 3 ?
Fe3A O71 Fe3A 146.2(2) 6 7 ?
Ni3 O71 Fe3A 146.2(2) 6 7 ?
Fe3A O71 Fe3A 85.15(6) 3 7 ?
Ni3 O71 Fe3A 85.15(6) 3 7 ?
Fe3A O71 Ni3 146.2 6 7 ?
Ni3 O71 Ni3 146.2(2) 6 7 ?
Fe3A O71 Ni3 85.2 3 7 ?
Ni3 O71 Ni3 85.15(6) 3 7 ?
Fe3A O71 Ni3 0.0 7 7 ?
Fe3A O71 Ni3 85.2 6 . ?
Ni3 O71 Ni3 85.16(6) 6 . ?
Fe3A O71 Ni3 146.2 3 . ?
Ni3 O71 Ni3 146.2(2) 3 . ?
Fe3A O71 Ni3 85.2 7 . ?
Ni3 O71 Ni3 85.15(6) 7 . ?
Fe3A O71 H71 106.9 6 . ?
Ni3 O71 H71 106.9 6 . ?
Fe3A O71 H71 106.9 3 . ?
Ni3 O71 H71 106.9 3 . ?
Fe3A O71 H71 106.9 7 . ?
Ni3 O71 H71 106.9 7 . ?
Ni3 O71 H71 106.9 . . ?
N41 C41 C42 122.2(4) . . ?
N41 C41 H41 118.9 . . ?
C42 C41 H41 118.9 . . ?
C43 C42 C41 118.4(3) . . ?
C43 C42 H42 120.8 . . ?
C41 C42 H42 120.8 . . ?
C42 C43 C44 119.7(4) . . ?
C42 C43 H43 120.2 . . ?
C44 C43 H43 120.2 . . ?
C43 C44 C45 119.2(4) . . ?
C43 C44 H44 120.4 . . ?
C45 C44 H44 120.4 . . ?
N41 C45 C44 121.8(3) . . ?
N41 C45 C46 116.5(3) . . ?
C44 C45 C46 121.7(3) . . ?
O41 C46 O41 107.2(3) 5 . ?
O41 C46 C45 110.45(16) 5 . ?
O41 C46 C45 110.50(15) . . ?
O41 C46 C45 110.49(15) 5 5 ?
O41 C46 C45 110.46(16) . 5 ?
C45 C46 C45 107.7(4) . 5 ?
O51 C51 O52 125.1(3) . . ?
O51 C51 C52 117.9(3) . . ?
O52 C51 C52 117.0(3) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?

_refine_diff_density_max         0.430
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.056

# SQUEEZE RESULTS (Version = 290617)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.011 -0.009 0.007 7700 1571 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 1 0 2.465
0 2 0 3.487
2 2 0 4.935
1 3 0 5.519
4 4 0 9.906
0 1 1 2.466
1 2 1 4.273
0 3 1 5.519
1 3 1 5.789
0 5 1 8.921
1 6 1 10.805
0 0 2 3.489
1 1 2 4.274
0 2 2 4.936
1 2 2 5.236
2 2 2 6.049
0 4 2 7.818
0 1 3 5.522
1 3 3 7.620
2 2 4 8.572
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
TITL shelxl    P 4/n n c    R = 0.12
CELL   25.3484   25.3484   25.3324     90.00     90.00     90.00
SPGR P4/nnc
# Solvent Accessible Volume =      7682
# Electrons Found in S.A.V. =      1543
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
C101 0.981 0.137 0.078 !       3.31 eA-3
C102 0.502 0.058 0.133 !       3.26 eA-3
C103 0.478 0.633 0.971 !       3.10 eA-3
C104 0.460 0.058 0.141 !       2.80 eA-3
C105 0.441 0.556 0.126 !       2.56 eA-3
C106 0.898 0.773 0.015 !       2.05 eA-3
C107 0.470 0.643 0.008 !       1.88 eA-3
C108 0.899 0.993 0.055 !       1.87 eA-3
C109 0.750 0.753 0.266 !       1.49 eA-3
C110 0.753 0.603 0.449 !       1.43 eA-3
C111 0.601 0.540 0.085 !       1.30 eA-3
C112 0.822 0.577 0.232 !       1.20 eA-3
Q113 0.250 0.245 0.031 !       1.08 eA-3
C114 0.750 0.755 0.148 !       1.07 eA-3
C115 0.244 0.228 0.496 !       1.06 eA-3
C116 0.785 0.600 0.414 !       0.94 eA-3
C117 0.515 0.557 0.469 !       0.93 eA-3
C118 0.750 0.752 0.008 !       0.88 eA-3
C119 0.678 0.899 0.186 !       0.87 eA-3
C120 0.649 0.944 0.209 !       0.84 eA-3
C121 0.249 0.262 0.695 !       0.82 eA-3
Q122 0.265 0.132 0.026 !       0.78 eA-3
C123 0.031 0.487 0.501 !       0.76 eA-3
C124 0.703 0.595 0.297 !       0.75 eA-3
C125 0.094 0.353 0.727 !       0.75 eA-3
Q126 0.318 0.856 0.568 !       0.75 eA-3
Q127 0.531 0.833 0.772 !       0.74 eA-3
C128 0.820 0.693 0.162 !       0.73 eA-3
C129 0.750 0.751 0.117 !       0.73 eA-3
C130 0.750 0.748 0.414 !       0.72 eA-3
Q131 0.247 0.798 0.185 !       0.72 eA-3
C132 0.512 0.568 0.164 !       0.69 eA-3
C133 0.507 0.426 0.568 !       0.66 eA-3
C134 0.651 0.580 0.217 !       0.64 eA-3
C135 0.542 0.555 0.068 !       0.64 eA-3
C136 0.898 0.644 0.313 !       0.63 eA-3
Q137 0.126 0.161 0.407 !       0.60 eA-3
C138 0.795 0.836 0.132 !       0.59 eA-3
Q139 0.467 0.594 0.093 !       0.59 eA-3
Q140 0.048 0.919 0.275 !       0.59 eA-3
C141 0.939 0.750 0.250 !       0.59 eA-3
C142 0.400 0.154 0.896 !       0.58 eA-3
C143 0.727 0.574 0.268 !       0.57 eA-3
Q144 0.409 0.797 0.639 !       0.56 eA-3
C145 0.602 0.902 0.282 !       0.55 eA-3
Q146 0.135 0.398 0.422 !       0.55 eA-3
C147 0.409 0.586 0.015 !       0.55 eA-3
C148 0.386 0.132 0.902 !       0.55 eA-3
C149 0.109 0.095 0.756 !       0.54 eA-3
Q150 0.109 0.779 0.188 !       0.54 eA-3
Q151 0.094 0.474 0.325 !       0.54 eA-3
Q152 0.242 0.163 0.401 !       0.54 eA-3
C153 0.868 0.853 0.199 !       0.53 eA-3
C154 0.883 0.625 0.228 !       0.53 eA-3
Q155 0.384 0.554 0.134 !       0.52 eA-3
C156 0.672 0.935 0.290 !       0.52 eA-3
Q157 0.159 0.069 0.210 !       0.52 eA-3
Q158 0.578 0.282 0.360 !       0.52 eA-3
C159 0.904 0.650 0.155 !       0.52 eA-3
Q160 0.031 0.012 0.672 !       0.51 eA-3
Q161 0.281 0.157 0.100 !       0.51 eA-3
Q162 0.376 0.418 0.084 !       0.51 eA-3
Q163 0.250 0.752 0.297 !       0.50 eA-3
;

_shelxl_version_number           2014/6

# start Validation Reply Form
_vrf_CHEMW03_shelxl              
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: This alert is generated because squeeze program has been
used to exlude the solvent molecules during the refinement. The cif 
file contains the complete molecular formula; however some of the 
atoms reported are not listed in the fractional coordinates' list.
;
_vrf_PLAT230_shelxl              
;
PROBLEM: Hirshfeld Test Diff for    O31    --  C31     ..        8.7 s.u.  
RESPONSE: The thermal ellipsoids for both atoms look normal and there is
no disorder or wrong assignment of the chemical types.
;
_vrf_PLAT420_shelxl              
;
PROBLEM: D-H Without Acceptor       O61    --  H61    ...     Please Check 
RESPONSE: These are tetradentate hydroxyl groups which are nested within 
the clusters, thus rendering the intermolecular hydrogen bonds impossible.  
The closest intramolecular OH...O distances are larger than 3.0 A.
;
_vrf_PLAT910_shelxl              
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         14 Note  
RESPONSE: This alert is probably due to instrument limitations. The number
of mising reflections is very small and in any case the ratio of reflections
to parameters refined is well above the ideal value of ten.
;
# end Validation Reply Form



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

data_shelxl_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1033943'
_audit_update_record             
;
2017-09-08 deposited with the CCDC.
2017-09-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C77.33 H85.60 Fe1.54 N16.67 Ni7.46 O26.80'
_chemical_formula_weight         2201.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_H-M_alt        'P 4/n n c'
_space_group_name_Hall           '-P 4a 2bc'

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

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

_cell_length_a                   25.4547(4)
_cell_length_b                   25.4547(4)
_cell_length_c                   25.6338(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     16609.2(6)
_cell_formula_units_Z            6
_cell_measurement_temperature    220(2)
_cell_measurement_reflns_used    38444
_cell_measurement_theta_min      6.50
_cell_measurement_theta_max      71.97

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            orange-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_F_000             6778
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_exptl_absorpt_coefficient_mu    3.492
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.576
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      220(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            50692
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         6.503
_diffrn_reflns_theta_max         64.982
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.926
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.926
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.926
_reflns_number_total             6986
_reflns_number_gt                4921
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond ver.3.1.'
_computing_publication_material  'publCIF J.Appl.Cryst. 2010, 43, 920'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1105P)²] 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         6986
_refine_ls_number_parameters     353
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0546
_refine_ls_wR_factor_ref         0.1842
_refine_ls_wR_factor_gt          0.1712
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.7500 0.2500 0.7500 0.0588(3) Uani 0.73 4 d S T P . .
Ni1A Ni 0.7500 0.2500 0.7500 0.0588(3) Uani 0.27 4 d S T P . .
Ni1 Ni 0.79982(3) 0.15506(2) 0.68181(3) 0.0685(2) Uani 0.8988 1 d . . P . .
Fe1A Fe 0.79982(3) 0.15506(2) 0.68181(3) 0.0685(2) Uani 0.1013 1 d . . P . .
Ni2 Ni 0.68041(3) 0.15626(2) 0.69995(3) 0.0693(2) Uani 0.8988 1 d . . P . .
Fe2A Fe 0.68041(3) 0.15626(2) 0.69995(3) 0.0693(2) Uani 0.1013 1 d . . P . .
N1 N 0.82464(12) 0.19620(12) 0.61723(13) 0.0712(9) Uani 1 1 d . . . . .
O1 O 0.73954(9) 0.20669(9) 0.67386(10) 0.0648(7) Uani 1 1 d . . . . .
N11 N 0.88244(12) 0.30142(12) 0.67298(14) 0.0716(9) Uani 1 1 d . . . . .
O11 O 0.82705(9) 0.20687(9) 0.74013(10) 0.0629(6) Uani 1 1 d . . . . .
O21 O 0.77069(12) 0.09523(10) 0.63498(11) 0.0821(8) Uani 1 1 d . . . . .
O22 O 0.68400(12) 0.10746(11) 0.63911(12) 0.0885(9) Uani 1 1 d . . . . .
O31 O 0.62741(11) 0.10211(10) 0.72900(12) 0.0815(8) Uani 1 1 d . . . . .
O32 O 0.63471(11) 0.11117(10) 0.81536(12) 0.0820(8) Uani 1 1 d . . . . .
O61 O 0.7500 0.12922(13) 0.7500 0.0692(9) Uani 1 2 d S T P . .
C1 C 0.86553(18) 0.18343(18) 0.58568(19) 0.0869(12) Uani 1 1 d . . . . .
H1 H 0.8854 0.1532 0.5932 0.113 Uiso 1 1 calc R U . . .
C2 C 0.87848(18) 0.2130(2) 0.54364(19) 0.0970(14) Uani 1 1 d . . . . .
H2 H 0.9066 0.2026 0.5223 0.126 Uiso 1 1 calc R U . . .
C3 C 0.85167(19) 0.25723(18) 0.53190(19) 0.0879(13) Uani 1 1 d . . . . .
H3 H 0.8609 0.2780 0.5030 0.114 Uiso 1 1 calc R U . . .
C4 C 0.81042(17) 0.27062(17) 0.56381(18) 0.0792(11) Uani 1 1 d . . . . .
H4 H 0.7909 0.3013 0.5571 0.103 Uiso 1 1 calc R U . . .
C5 C 0.79735(16) 0.23842(14) 0.60647(16) 0.0664(10) Uani 1 1 d . . . . .
C6 C 0.7500 0.2500 0.6411(2) 0.0630(14) Uani 1 2 d S T P . .
C11 C 0.91268(19) 0.31294(18) 0.63210(17) 0.0889(13) Uani 1 1 d . . . . .
H11 H 0.9030 0.3410 0.6103 0.116 Uiso 1 1 calc R U . . .
C12 C 0.95828(19) 0.2846(2) 0.6207(2) 0.1009(15) Uani 1 1 d . . . . .
H12 H 0.9802 0.2946 0.5929 0.131 Uiso 1 1 calc R U . . .
C13 C 0.97024(19) 0.2424(2) 0.6505(2) 0.1027(16) Uani 1 1 d . . . . .
H13 H 1.0001 0.2222 0.6425 0.133 Uiso 1 1 calc R U . . .
C14 C 0.93902(17) 0.22869(18) 0.69268(19) 0.0845(12) Uani 1 1 d . . . . .
H14 H 0.9471 0.1995 0.7136 0.110 Uiso 1 1 calc R U . . .
C15 C 0.89524(15) 0.25987(15) 0.70287(17) 0.0715(11) Uani 1 1 d . . . . .
C16 C 0.8599(2) 0.2500 0.7500 0.0668(14) Uani 1 2 d S T P . .
C21 C 0.7239(2) 0.08531(15) 0.62210(17) 0.0770(11) Uani 1 1 d . . . . .
C22 C 0.7155(2) 0.04244(15) 0.58235(17) 0.0922(14) Uani 1 1 d . . . . .
H22A H 0.7493 0.0281 0.5720 0.138 Uiso 1 1 calc R U . . .
H22B H 0.6941 0.0148 0.5975 0.138 Uiso 1 1 calc R U . . .
H22C H 0.6978 0.0568 0.5520 0.138 Uiso 1 1 calc R U . . .
C31 C 0.61098(17) 0.09599(15) 0.7753(2) 0.0783(11) Uani 1 1 d . . . . .
C32 C 0.56070(18) 0.0673(2) 0.7836(2) 0.1112(17) Uani 1 1 d . . . . .
H32A H 0.5459 0.0575 0.7501 0.167 Uiso 1 1 calc R U . . .
H32B H 0.5673 0.0359 0.8041 0.167 Uiso 1 1 calc R U . . .
H32C H 0.5362 0.0898 0.8021 0.167 Uiso 1 1 calc R U . . .
Fe3 Fe 0.2500 0.2500 0.2500 0.0540(4) Uani 0.7304 8 d S T P . .
Ni3A Ni 0.2500 0.2500 0.2500 0.0540(4) Uani 0.2696 8 d S T P . .
Ni3 Ni 0.23727(2) 0.16598(2) 0.34379(3) 0.0652(2) Uani 0.8988 1 d . . P . .
Fe3A Fe 0.23727(2) 0.16598(2) 0.34379(3) 0.0652(2) Uani 0.1013 1 d . . P . .
N41 N 0.20938(12) 0.10227(11) 0.30272(14) 0.0703(9) Uani 1 1 d . . . . .
O41 O 0.20274(9) 0.18898(9) 0.20665(11) 0.0598(6) Uani 1 1 d . . . . .
O51 O 0.18285(11) 0.15172(11) 0.40142(12) 0.0861(8) Uani 1 1 d . . . . .
O52 O 0.12328(10) 0.21409(11) 0.38889(11) 0.0830(8) Uani 1 1 d . . . . .
O71 O 0.2500 0.2500 0.3691(2) 0.0696(13) Uani 1 4 d S T P . .
C41 C 0.21530(16) 0.05151(15) 0.31583(19) 0.0857(13) Uani 1 1 d . . . . .
H41 H 0.2351 0.0429 0.3456 0.111 Uiso 1 1 calc R U . . .
C42 C 0.19322(19) 0.01175(15) 0.2869(2) 0.0918(14) Uani 1 1 d . . . . .
H42 H 0.1966 -0.0234 0.2977 0.119 Uiso 1 1 calc R U . . .
C43 C 0.16628(19) 0.02374(16) 0.2422(2) 0.0877(13) Uani 1 1 d . . . . .
H43 H 0.1524 -0.0030 0.2210 0.114 Uiso 1 1 calc R U . . .
C44 C 0.15996(15) 0.07601(15) 0.22901(18) 0.0745(11) Uani 1 1 d . . . . .
H44 H 0.1412 0.0853 0.1988 0.097 Uiso 1 1 calc R U . . .
C45 C 0.18137(14) 0.11416(14) 0.26031(16) 0.0654(10) Uani 1 1 d . . . . .
C46 C 0.17299(14) 0.17299(14) 0.2500 0.0613(13) Uani 1 2 d S T P . .
C51 C 0.13862(18) 0.17105(17) 0.40814(17) 0.0787(11) Uani 1 1 d . . . . .
C52 C 0.0999(2) 0.1408(2) 0.4411(2) 0.1173(19) Uani 1 1 d . . . . .
H52A H 0.0671 0.1602 0.4432 0.176 Uiso 1 1 calc R U . . .
H52B H 0.0935 0.1067 0.4255 0.176 Uiso 1 1 calc R U . . .
H52C H 0.1141 0.1361 0.4759 0.176 Uiso 1 1 calc R U . . .
H61 H 0.7500 0.0950 0.7500 0.050 Uiso 1 2 d S . P . .
H71 H 0.2500 0.2500 0.4047 0.050 Uiso 1 4 d S . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 2.257(3) . ?
Fe1 O1 2.258(3) 2_556 ?
Fe1 O1 2.258(3) 4_656 ?
Fe1 O1 2.258(3) 3_655 ?
Fe1 O11 2.262(2) . ?
Fe1 O11 2.262(2) 2_556 ?
Fe1 O11 2.262(2) 4_656 ?
Fe1 O11 2.262(2) 3_655 ?
Ni1 O32 2.008(3) 4_656 ?
Ni1 O1 2.031(2) . ?
Ni1 N1 2.058(3) . ?
Ni1 O21 2.076(3) . ?
Ni1 O11 2.111(2) . ?
Ni1 O61 2.2576(12) . ?
Ni2 O22 1.996(3) . ?
Ni2 O11 2.014(3) 4_656 ?
Ni2 N11 2.049(3) 3_655 ?
Ni2 O31 2.068(3) . ?
Ni2 O1 2.088(2) . ?
Ni2 O61 2.2930(12) . ?
N1 C5 1.309(4) . ?
N1 C1 1.358(5) . ?
O1 C6 1.411(4) . ?
N11 C11 1.333(5) . ?
N11 C15 1.346(5) . ?
N11 Fe2A 2.049(3) 3_655 ?
N11 Ni2 2.049(3) 3_655 ?
O11 C16 1.403(4) . ?
O11 Fe2A 2.014(3) 4_656 ?
O11 Ni2 2.014(3) 4_656 ?
O21 C21 1.263(5) . ?
O22 C21 1.240(5) . ?
O31 C31 1.267(5) . ?
O32 C31 1.253(5) . ?
O32 Fe1A 2.008(3) 4_656 ?
O32 Ni1 2.008(3) 4_656 ?
O61 Fe1A 2.2575(12) 4_656 ?
O61 Ni1 2.2575(12) 4_656 ?
O61 Fe2A 2.2929(12) 4_656 ?
O61 Ni2 2.2929(12) 4_656 ?
O61 H61 0.8710 . ?
C1 C2 1.356(6) . ?
C1 H1 0.9400 . ?
C2 C3 1.350(6) . ?
C2 H2 0.9400 . ?
C3 C4 1.374(6) . ?
C3 H3 0.9400 . ?
C4 C5 1.407(6) . ?
C4 H4 0.9400 . ?
C5 C6 1.526(5) . ?
C6 O1 1.411(4) 3_655 ?
C6 C5 1.526(5) 3_655 ?
C11 C12 1.398(6) . ?
C11 H11 0.9400 . ?
C12 C13 1.350(6) . ?
C12 H12 0.9400 . ?
C13 C14 1.387(6) . ?
C13 H13 0.9400 . ?
C14 C15 1.393(6) . ?
C14 H14 0.9400 . ?
C15 C16 1.527(5) . ?
C16 O11 1.403(4) 2_556 ?
C16 C15 1.527(5) 2_556 ?
C21 C22 1.508(5) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
C31 C32 1.489(6) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 H32C 0.9700 . ?
Fe3 O41 2.257(2) . ?
Fe3 O41 2.257(2) 8 ?
Fe3 O41 2.257(2) 5 ?
Fe3 O41 2.257(2) 3 ?
Fe3 O41 2.257(2) 2 ?
Fe3 O41 2.257(2) 6 ?
Fe3 O41 2.257(2) 4 ?
Fe3 O41 2.257(2) 7 ?
Ni3 O52 2.013(3) 7 ?
Ni3 O41 2.015(2) 5 ?
Ni3 O51 2.058(3) . ?
Ni3 N41 2.060(3) . ?
Ni3 O41 2.085(2) 4 ?
Ni3 O71 2.2584(16) . ?
N41 C45 1.335(5) . ?
N41 C41 1.344(4) . ?
O41 C46 1.405(4) . ?
O41 Fe3A 2.015(2) 5 ?
O41 Ni3 2.015(2) 5 ?
O41 Fe3A 2.085(2) 4 ?
O41 Ni3 2.085(2) 4 ?
O51 C51 1.241(5) . ?
O52 C51 1.263(5) . ?
O52 Fe3A 2.013(3) 6 ?
O52 Ni3 2.013(3) 6 ?
O71 Fe3A 2.2584(16) 6 ?
O71 Ni3 2.2584(16) 6 ?
O71 Fe3A 2.2584(16) 3 ?
O71 Ni3 2.2584(16) 3 ?
O71 Fe3A 2.2584(16) 7 ?
O71 Ni3 2.2584(16) 7 ?
O71 H71 0.9120 . ?
C41 C42 1.375(6) . ?
C41 H41 0.9400 . ?
C42 C43 1.369(6) . ?
C42 H42 0.9400 . ?
C43 C44 1.382(5) . ?
C43 H43 0.9400 . ?
C44 C45 1.373(5) . ?
C44 H44 0.9400 . ?
C45 C46 1.536(5) . ?
C46 O41 1.405(4) 5 ?
C46 C45 1.536(5) 5 ?
C51 C52 1.511(6) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C52 H52C 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O1 166.45(12) . 2_556 ?
O1 Fe1 O1 121.53(13) . 4_656 ?
O1 Fe1 O1 60.32(13) 2_556 4_656 ?
O1 Fe1 O1 60.32(13) . 3_655 ?
O1 Fe1 O1 121.54(13) 2_556 3_655 ?
O1 Fe1 O1 166.45(12) 4_656 3_655 ?
O1 Fe1 O11 76.62(9) . . ?
O1 Fe1 O11 115.85(9) 2_556 . ?
O1 Fe1 O11 75.96(9) 4_656 . ?
O1 Fe1 O11 92.18(9) 3_655 . ?
O1 Fe1 O11 115.85(9) . 2_556 ?
O1 Fe1 O11 76.62(9) 2_556 2_556 ?
O1 Fe1 O11 92.18(9) 4_656 2_556 ?
O1 Fe1 O11 75.96(9) 3_655 2_556 ?
O11 Fe1 O11 59.75(11) . 2_556 ?
O1 Fe1 O11 75.96(9) . 4_656 ?
O1 Fe1 O11 92.18(9) 2_556 4_656 ?
O1 Fe1 O11 76.62(9) 4_656 4_656 ?
O1 Fe1 O11 115.85(9) 3_655 4_656 ?
O11 Fe1 O11 121.92(11) . 4_656 ?
O11 Fe1 O11 167.16(13) 2_556 4_656 ?
O1 Fe1 O11 92.18(9) . 3_655 ?
O1 Fe1 O11 75.96(9) 2_556 3_655 ?
O1 Fe1 O11 115.85(9) 4_656 3_655 ?
O1 Fe1 O11 76.62(9) 3_655 3_655 ?
O11 Fe1 O11 167.16(13) . 3_655 ?
O11 Fe1 O11 121.93(11) 2_556 3_655 ?
O11 Fe1 O11 59.75(11) 4_656 3_655 ?
O32 Ni1 O1 172.33(11) 4_656 . ?
O32 Ni1 N1 93.29(12) 4_656 . ?
O1 Ni1 N1 79.74(12) . . ?
O32 Ni1 O21 84.79(11) 4_656 . ?
O1 Ni1 O21 98.45(11) . . ?
N1 Ni1 O21 91.02(12) . . ?
O32 Ni1 O11 92.84(11) 4_656 . ?
O1 Ni1 O11 85.11(10) . . ?
N1 Ni1 O11 98.69(11) . . ?
O21 Ni1 O11 170.13(11) . . ?
O32 Ni1 O61 106.03(10) 4_656 . ?
O1 Ni1 O61 80.90(10) . . ?
N1 Ni1 O61 160.64(11) . . ?
O21 Ni1 O61 91.91(11) . . ?
O11 Ni1 O61 79.51(9) . . ?
O22 Ni2 O11 176.86(12) . 4_656 ?
O22 Ni2 N11 95.70(13) . 3_655 ?
O11 Ni2 N11 81.21(12) 4_656 3_655 ?
O22 Ni2 O31 84.05(12) . . ?
O11 Ni2 O31 95.18(11) 4_656 . ?
N11 Ni2 O31 87.86(12) 3_655 . ?
O22 Ni2 O1 95.70(11) . . ?
O11 Ni2 O1 85.36(10) 4_656 . ?
N11 Ni2 O1 97.56(11) 3_655 . ?
O31 Ni2 O1 174.57(11) . . ?
O22 Ni2 O61 102.42(11) . . ?
O11 Ni2 O61 80.68(9) 4_656 . ?
N11 Ni2 O61 161.77(12) 3_655 . ?
O31 Ni2 O61 95.87(10) . . ?
O1 Ni2 O61 78.87(9) . . ?
C5 N1 C1 118.5(4) . . ?
C5 N1 Ni1 115.1(3) . . ?
C1 N1 Ni1 126.4(3) . . ?
C6 O1 Ni1 115.02(15) . . ?
C6 O1 Ni2 143.80(17) . . ?
Ni1 O1 Ni2 96.59(10) . . ?
C6 O1 Fe1 96.3(2) . . ?
Ni1 O1 Fe1 98.06(11) . . ?
Ni2 O1 Fe1 96.21(10) . . ?
C11 N11 C15 118.7(4) . . ?
C11 N11 Fe2A 126.9(3) . 3_655 ?
C15 N11 Fe2A 114.2(3) . 3_655 ?
C11 N11 Ni2 126.9(3) . 3_655 ?
C15 N11 Ni2 114.2(3) . 3_655 ?
Fe2A N11 Ni2 0.0 3_655 3_655 ?
C16 O11 Fe2A 114.79(15) . 4_656 ?
C16 O11 Ni2 114.79(15) . 4_656 ?
Fe2A O11 Ni2 0.0 4_656 4_656 ?
C16 O11 Ni1 144.32(17) . . ?
Fe2A O11 Ni1 96.29(10) 4_656 . ?
Ni2 O11 Ni1 96.29(10) 4_656 . ?
C16 O11 Fe1 96.7(2) . . ?
Fe2A O11 Fe1 98.25(10) 4_656 . ?
Ni2 O11 Fe1 98.25(10) 4_656 . ?
Ni1 O11 Fe1 95.61(9) . . ?
C21 O21 Ni1 129.4(3) . . ?
C21 O22 Ni2 126.5(3) . . ?
C31 O31 Ni2 129.4(3) . . ?
C31 O32 Fe1A 127.0(3) . 4_656 ?
C31 O32 Ni1 127.0(3) . 4_656 ?
Fe1A O32 Ni1 0.0 4_656 4_656 ?
Fe1A O61 Ni1 0.0 4_656 4_656 ?
Fe1A O61 Ni1 146.1 4_656 . ?
Ni1 O61 Ni1 146.12(16) 4_656 . ?
Fe1A O61 Fe2A 85.02(5) 4_656 4_656 ?
Ni1 O61 Fe2A 85.02(5) 4_656 4_656 ?
Ni1 O61 Fe2A 84.94(5) . 4_656 ?
Fe1A O61 Ni2 85.02(5) 4_656 4_656 ?
Ni1 O61 Ni2 85.02(5) 4_656 4_656 ?
Ni1 O61 Ni2 84.94(5) . 4_656 ?
Fe2A O61 Ni2 0.0 4_656 4_656 ?
Fe1A O61 Ni2 84.94(5) 4_656 . ?
Ni1 O61 Ni2 84.94(5) 4_656 . ?
Ni1 O61 Ni2 85.02(5) . . ?
Fe2A O61 Ni2 145.1 4_656 . ?
Ni2 O61 Ni2 145.06(16) 4_656 . ?
Fe1A O61 H61 106.9 4_656 . ?
Ni1 O61 H61 106.9 4_656 . ?
Ni1 O61 H61 106.9 . . ?
Fe2A O61 H61 107.5 4_656 . ?
Ni2 O61 H61 107.5 4_656 . ?
Ni2 O61 H61 107.5 . . ?
C2 C1 N1 121.8(4) . . ?
C2 C1 H1 119.1 . . ?
N1 C1 H1 119.1 . . ?
C3 C2 C1 121.2(5) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C2 C3 C4 117.4(4) . . ?
C2 C3 H3 121.3 . . ?
C4 C3 H3 121.3 . . ?
C3 C4 C5 119.9(4) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
N1 C5 C4 121.1(4) . . ?
N1 C5 C6 117.1(3) . . ?
C4 C5 C6 121.8(4) . . ?
O1 C6 O1 107.0(4) 3_655 . ?
O1 C6 C5 110.14(17) 3_655 3_655 ?
O1 C6 C5 110.37(17) . 3_655 ?
O1 C6 C5 110.37(17) 3_655 . ?
O1 C6 C5 110.14(17) . . ?
C5 C6 C5 108.8(5) 3_655 . ?
N11 C11 C12 122.0(5) . . ?
N11 C11 H11 119.0 . . ?
C12 C11 H11 119.0 . . ?
C13 C12 C11 118.7(5) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
C12 C13 C14 120.8(5) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C13 C14 C15 117.4(5) . . ?
C13 C14 H14 121.3 . . ?
C15 C14 H14 121.3 . . ?
N11 C15 C14 122.3(4) . . ?
N11 C15 C16 115.9(3) . . ?
C14 C15 C16 121.7(4) . . ?
O11 C16 O11 106.8(4) 2_556 . ?
O11 C16 C15 109.71(17) 2_556 2_556 ?
O11 C16 C15 111.41(18) . 2_556 ?
O11 C16 C15 111.41(18) 2_556 . ?
O11 C16 C15 109.71(17) . . ?
C15 C16 C15 107.8(5) 2_556 . ?
O22 C21 O21 126.1(4) . . ?
O22 C21 C22 116.9(4) . . ?
O21 C21 C22 117.0(4) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O32 C31 O31 124.8(4) . . ?
O32 C31 C32 116.6(5) . . ?
O31 C31 C32 118.6(5) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O41 Fe3 O41 167.39(11) . 8 ?
O41 Fe3 O41 60.58(13) . 5 ?
O41 Fe3 O41 121.02(13) 8 5 ?
O41 Fe3 O41 121.02(13) . 3 ?
O41 Fe3 O41 60.58(13) 8 3 ?
O41 Fe3 O41 167.39(11) 5 3 ?
O41 Fe3 O41 115.59(11) . 2 ?
O41 Fe3 O41 75.98(6) 8 2 ?
O41 Fe3 O41 75.98(6) 5 2 ?
O41 Fe3 O41 93.02(12) 3 2 ?
O41 Fe3 O41 75.97(6) . 6 ?
O41 Fe3 O41 115.59(11) 8 6 ?
O41 Fe3 O41 93.02(12) 5 6 ?
O41 Fe3 O41 75.98(6) 3 6 ?
O41 Fe3 O41 60.58(13) 2 6 ?
O41 Fe3 O41 93.02(12) . 4 ?
O41 Fe3 O41 75.98(6) 8 4 ?
O41 Fe3 O41 75.98(6) 5 4 ?
O41 Fe3 O41 115.59(11) 3 4 ?
O41 Fe3 O41 121.02(13) 2 4 ?
O41 Fe3 O41 167.39(11) 6 4 ?
O41 Fe3 O41 75.98(6) . 7 ?
O41 Fe3 O41 93.02(12) 8 7 ?
O41 Fe3 O41 115.59(11) 5 7 ?
O41 Fe3 O41 75.98(6) 3 7 ?
O41 Fe3 O41 167.39(11) 2 7 ?
O41 Fe3 O41 121.02(13) 6 7 ?
O41 Fe3 O41 60.58(13) 4 7 ?
O52 Ni3 O41 174.19(11) 7 5 ?
O52 Ni3 O51 84.63(11) 7 . ?
O41 Ni3 O51 97.58(11) 5 . ?
O52 Ni3 N41 94.61(12) 7 . ?
O41 Ni3 N41 80.06(11) 5 . ?
O51 Ni3 N41 89.77(13) . . ?
O52 Ni3 O41 93.29(10) 7 4 ?
O41 Ni3 O41 85.33(14) 5 4 ?
O51 Ni3 O41 171.13(12) . 4 ?
N41 Ni3 O41 99.00(12) . 4 ?
O52 Ni3 O71 104.95(12) 7 . ?
O41 Ni3 O71 80.35(12) 5 . ?
O51 Ni3 O71 93.28(13) . . ?
N41 Ni3 O71 160.40(13) . . ?
O41 Ni3 O71 78.90(11) 4 . ?
C45 N41 C41 118.8(4) . . ?
C45 N41 Ni3 115.0(2) . . ?
C41 N41 Ni3 126.2(3) . . ?
C46 O41 Fe3A 115.72(13) . 5 ?
C46 O41 Ni3 115.72(13) . 5 ?
Fe3A O41 Ni3 0.0 5 5 ?
C46 O41 Fe3A 143.52(15) . 4 ?
Fe3A O41 Fe3A 96.51(12) 5 4 ?
Ni3 O41 Fe3A 96.51(12) 5 4 ?
C46 O41 Ni3 143.52(15) . 4 ?
Fe3A O41 Ni3 96.5 5 4 ?
Ni3 O41 Ni3 96.51(12) 5 4 ?
Fe3A O41 Ni3 0.0 4 4 ?
C46 O41 Fe3 95.6(2) . . ?
Fe3A O41 Fe3 98.25(9) 5 . ?
Ni3 O41 Fe3 98.25(9) 5 . ?
Fe3A O41 Fe3 96.21(9) 4 . ?
Ni3 O41 Fe3 96.21(9) 4 . ?
C51 O51 Ni3 129.8(3) . . ?
C51 O52 Fe3A 126.2(3) . 6 ?
C51 O52 Ni3 126.2(3) . 6 ?
Fe3A O52 Ni3 0.0 6 6 ?
Fe3A O71 Ni3 0.0 6 6 ?
Fe3A O71 Fe3A 85.26(7) 6 3 ?
Ni3 O71 Fe3A 85.26(7) 6 3 ?
Fe3A O71 Ni3 85.3 6 3 ?
Ni3 O71 Ni3 85.26(7) 6 3 ?
Fe3A O71 Ni3 0.0 3 3 ?
Fe3A O71 Fe3A 146.6(3) 6 7 ?
Ni3 O71 Fe3A 146.6(3) 6 7 ?
Fe3A O71 Fe3A 85.26(7) 3 7 ?
Ni3 O71 Fe3A 85.26(7) 3 7 ?
Fe3A O71 Ni3 146.6 6 7 ?
Ni3 O71 Ni3 146.6(3) 6 7 ?
Fe3A O71 Ni3 85.3 3 7 ?
Ni3 O71 Ni3 85.26(7) 3 7 ?
Fe3A O71 Ni3 0.0 7 7 ?
Fe3A O71 Ni3 85.3 6 . ?
Ni3 O71 Ni3 85.26(7) 6 . ?
Fe3A O71 Ni3 146.6 3 . ?
Ni3 O71 Ni3 146.6(3) 3 . ?
Fe3A O71 Ni3 85.3 7 . ?
Ni3 O71 Ni3 85.26(7) 7 . ?
Fe3A O71 H71 106.7 6 . ?
Ni3 O71 H71 106.7 6 . ?
Fe3A O71 H71 106.7 3 . ?
Ni3 O71 H71 106.7 3 . ?
Fe3A O71 H71 106.7 7 . ?
Ni3 O71 H71 106.7 7 . ?
Ni3 O71 H71 106.7 . . ?
N41 C41 C42 121.8(4) . . ?
N41 C41 H41 119.1 . . ?
C42 C41 H41 119.1 . . ?
C43 C42 C41 119.5(4) . . ?
C43 C42 H42 120.3 . . ?
C41 C42 H42 120.3 . . ?
C42 C43 C44 118.6(4) . . ?
C42 C43 H43 120.7 . . ?
C44 C43 H43 120.7 . . ?
C45 C44 C43 119.4(4) . . ?
C45 C44 H44 120.3 . . ?
C43 C44 H44 120.3 . . ?
N41 C45 C44 121.9(4) . . ?
N41 C45 C46 115.8(3) . . ?
C44 C45 C46 122.3(4) . . ?
O41 C46 O41 108.3(4) 5 . ?
O41 C46 C45 110.45(18) 5 . ?
O41 C46 C45 110.10(17) . . ?
O41 C46 C45 110.10(17) 5 5 ?
O41 C46 C45 110.44(18) . 5 ?
C45 C46 C45 107.5(4) . 5 ?
O51 C51 O52 124.8(4) . . ?
O51 C51 C52 117.9(4) . . ?
O52 C51 C52 117.3(4) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?

_refine_diff_density_max         0.565
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.055


# SQUEEZE RESULTS (Version = 290617)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.012 -0.010 0.005 8117 1373 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 1 0 2.455
0 2 0 3.473
2 2 0 4.914
1 3 0 5.496
0 8 0 14.021
0 1 1 2.446
1 2 1 4.249
0 3 1 5.492
1 3 1 5.761
0 0 2 3.448
1 1 2 4.234
0 2 2 4.897
1 2 2 5.197
2 2 2 6.008
1 3 2 6.493
0 4 2 7.773
0 1 3 5.461
1 2 3 6.477
0 0 4 6.909
2 2 4 8.492
0 0 6 10.395
0 0 8 13.921
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
TITL shelxl    P 4/n n c    R = 0.11
CELL   25.4547   25.4547   25.6338     90.00     90.00     90.00
SPGR P4/nnc
# Solvent Accessible Volume =      8093
# Electrons Found in S.A.V. =      1345
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
C101 0.522 0.130 0.420 !       2.69 eA-3
C102 0.533 0.133 0.470 !       2.41 eA-3
C103 0.999 0.449 0.132 !       2.19 eA-3
C104 0.039 0.444 0.150 !       2.04 eA-3
C105 0.947 0.060 0.375 !       1.80 eA-3
C106 0.771 0.893 0.486 !       1.55 eA-3
C107 0.054 0.863 0.009 !       1.45 eA-3
C108 0.890 0.511 0.441 !       1.24 eA-3
C109 0.587 0.541 0.079 !       0.92 eA-3
Q110 0.750 0.252 0.297 !       0.86 eA-3
C111 0.250 0.251 0.016 !       0.86 eA-3
C112 0.943 0.522 0.462 !       0.83 eA-3
C113 0.834 0.561 0.234 !       0.83 eA-3
C114 0.932 0.631 0.301 !       0.81 eA-3
C115 0.930 0.665 0.289 !       0.77 eA-3
C116 0.727 0.564 0.049 !       0.74 eA-3
C117 0.942 0.623 0.329 !       0.68 eA-3
Q118 0.656 0.323 0.344 !       0.68 eA-3
Q119 0.166 0.266 0.389 !       0.66 eA-3
C120 0.899 0.566 0.074 !       0.64 eA-3
Q121 0.300 0.653 0.367 !       0.60 eA-3
C122 0.659 0.565 0.227 !       0.59 eA-3
Q123 0.750 0.751 0.695 !       0.58 eA-3
C124 0.576 0.705 0.222 !       0.54 eA-3
C125 0.092 0.152 0.823 !       0.54 eA-3
Q126 0.838 0.980 0.772 !       0.52 eA-3
Q127 0.594 0.232 0.124 !       0.52 eA-3
Q128 0.654 0.201 0.273 !       0.51 eA-3
;

# start Validation Reply Form
_vrf_CHEMW03_shelxl              
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: This alert is generated because squeeze program has been
used to exlude the solvent molecules during the refinement. The cif 
file contains the complete molecular formula; however some of the 
atoms reported are not listed in the fractional coordinates' list.
;
_vrf_PLAT420_shelxl              
;
PROBLEM: D-H Without Acceptor       O61    --  H61    ...     Please Check 
RESPONSE: These are tetradentate hydroxyl groups which are nested within 
the clusters, thus rendering the intermolecular hydrogen bonds impossible.  
The closest intramolecular OH...O distances are larger than 3.0 A.
;
_vrf_PLAT910_shelxl              
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         16 Note  
RESPONSE: This alert is probably due to instrument limitations. The number
of mising reflections is very small and in any case the ratio of reflections
to parameters refined is well above the ideal value of ten.
;
# end Validation Reply Form

_shelxl_version_number           2014/6



####################################################################### 
# 
# 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_shelxl_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1033944'
_audit_update_record             
;
2017-09-08 deposited with the CCDC.
2017-09-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C77.33 H85.60 Fe1.19 N16.67 Ni7.81 O26.80'
_chemical_formula_weight         2202.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_H-M_alt        'P 4/n n c'
_space_group_name_Hall           '-P 4a 2bc'

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

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

_cell_length_a                   25.4102(5)
_cell_length_b                   25.4102(5)
_cell_length_c                   25.5493(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     16496.6(7)
_cell_formula_units_Z            6
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    39142
_cell_measurement_theta_min      6.51
_cell_measurement_theta_max      72.00

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            orange-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_F_000             6782
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.31
_exptl_absorpt_coefficient_mu    3.220
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            51269
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         6.508
_diffrn_reflns_theta_max         64.987
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measured_fraction_theta_full 0.862
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_Laue_measured_fraction_full 0.862
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_point_group_measured_fraction_full 0.862
_reflns_number_total             6459
_reflns_number_gt                4570
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond ver.3.1'
_computing_publication_material  'publCIF J.Appl.Cryst. 2010, 43, 920'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1211P)²] 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         6459
_refine_ls_number_parameters     353
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0633
_refine_ls_wR_factor_ref         0.1969
_refine_ls_wR_factor_gt          0.1852
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.7500 0.2500 0.7500 0.0596(4) Uani 0.78 4 d S T P . .
Ni1A Ni 0.7500 0.2500 0.7500 0.0596(4) Uani 0.22 4 d S T P . .
Ni1 Ni 0.79975(3) 0.15488(3) 0.68186(3) 0.0686(3) Uani 0.9487 1 d . . P . .
Fe1A Fe 0.79975(3) 0.15488(3) 0.68186(3) 0.0686(3) Uani 0.0513 1 d . . P . .
Ni2 Ni 0.68051(3) 0.15629(3) 0.69979(3) 0.0697(3) Uani 0.9487 1 d . . P . .
Fe2A Fe 0.68051(3) 0.15629(3) 0.69979(3) 0.0697(3) Uani 0.0513 1 d . . P . .
N1 N 0.82511(15) 0.19540(15) 0.61714(13) 0.0715(10) Uani 1 1 d . . . . .
O1 O 0.73950(11) 0.20648(12) 0.67360(10) 0.0661(8) Uani 1 1 d . . . . .
N11 N 0.88274(14) 0.30130(14) 0.67253(13) 0.0719(10) Uani 1 1 d . . . . .
O11 O 0.82700(12) 0.20652(11) 0.74021(10) 0.0644(7) Uani 1 1 d . . . . .
O21 O 0.77082(14) 0.09516(12) 0.63521(11) 0.0799(9) Uani 1 1 d . . . . .
O22 O 0.68363(13) 0.10796(13) 0.63837(12) 0.0852(9) Uani 1 1 d . . . . .
O31 O 0.62720(12) 0.10221(12) 0.72933(11) 0.0786(9) Uani 1 1 d . . . . .
O32 O 0.63453(13) 0.11109(12) 0.81525(11) 0.0806(9) Uani 1 1 d . . . . .
O61 O 0.7500 0.12966(16) 0.7500 0.0691(11) Uani 1 2 d S T P . .
C1 C 0.8661(2) 0.1828(2) 0.58575(18) 0.0851(14) Uani 1 1 d . . . . .
H1 H 0.8863 0.1524 0.5940 0.111 Uiso 1 1 calc R U . . .
C2 C 0.8798(2) 0.2116(2) 0.54283(18) 0.0975(17) Uani 1 1 d . . . . .
H2 H 0.9082 0.2010 0.5210 0.127 Uiso 1 1 calc R U . . .
C3 C 0.8511(2) 0.2566(2) 0.53207(19) 0.0881(15) Uani 1 1 d . . . . .
H3 H 0.8596 0.2774 0.5023 0.114 Uiso 1 1 calc R U . . .
C4 C 0.81097(19) 0.2712(2) 0.56386(16) 0.0757(13) Uani 1 1 d . . . . .
H4 H 0.7922 0.3029 0.5577 0.098 Uiso 1 1 calc R U . . .
C5 C 0.79751(19) 0.23823(19) 0.60638(16) 0.0706(12) Uani 1 1 d . . . . .
C6 C 0.7500 0.2500 0.6418(2) 0.0614(15) Uani 1 2 d S T P . .
C11 C 0.9133(2) 0.3133(2) 0.63112(17) 0.0848(14) Uani 1 1 d . . . . .
H11 H 0.9039 0.3420 0.6092 0.110 Uiso 1 1 calc R U . . .
C12 C 0.9583(2) 0.2847(3) 0.6198(2) 0.1016(18) Uani 1 1 d . . . . .
H12 H 0.9802 0.2946 0.5914 0.132 Uiso 1 1 calc R U . . .
C13 C 0.9708(2) 0.2415(2) 0.6504(2) 0.0957(17) Uani 1 1 d . . . . .
H13 H 1.0009 0.2207 0.6425 0.124 Uiso 1 1 calc R U . . .
C14 C 0.9394(2) 0.2293(2) 0.69217(18) 0.0844(14) Uani 1 1 d . . . . .
H14 H 0.9477 0.2002 0.7140 0.110 Uiso 1 1 calc R U . . .
C15 C 0.89533(18) 0.25981(18) 0.70226(16) 0.0668(12) Uani 1 1 d . . . . .
C16 C 0.8603(3) 0.2500 0.7500 0.0628(16) Uani 1 2 d S T P . .
C21 C 0.7236(3) 0.08522(19) 0.62213(16) 0.0752(13) Uani 1 1 d . . . . .
C22 C 0.7157(2) 0.04259(18) 0.58220(17) 0.0893(15) Uani 1 1 d . . . . .
H22A H 0.7499 0.0277 0.5725 0.134 Uiso 1 1 calc R U . . .
H22B H 0.6934 0.0149 0.5970 0.134 Uiso 1 1 calc R U . . .
H22C H 0.6987 0.0574 0.5511 0.134 Uiso 1 1 calc R U . . .
C31 C 0.61160(19) 0.09546(17) 0.7744(2) 0.0763(13) Uani 1 1 d . . . . .
C32 C 0.5599(2) 0.0670(2) 0.7835(2) 0.1059(18) Uani 1 1 d . . . . .
H32A H 0.5529 0.0648 0.8212 0.159 Uiso 1 1 calc R U . . .
H32B H 0.5313 0.0864 0.7664 0.159 Uiso 1 1 calc R U . . .
H32C H 0.5619 0.0315 0.7688 0.159 Uiso 1 1 calc R U . . .
Fe3 Fe 0.2500 0.2500 0.2500 0.0537(5) Uani 0.78 8 d S T P . .
Ni3A Ni 0.2500 0.2500 0.2500 0.0537(5) Uani 0.22 8 d S T P . .
Ni3 Ni 0.23720(3) 0.16583(3) 0.34397(2) 0.0654(3) Uani 0.9487 1 d . . P . .
Fe3A Fe 0.23720(3) 0.16583(3) 0.34397(2) 0.0654(3) Uani 0.0513 1 d . . P . .
N41 N 0.20955(14) 0.10263(14) 0.30304(14) 0.0702(10) Uani 1 1 d . . . . .
O41 O 0.20253(10) 0.18866(11) 0.20685(10) 0.0596(7) Uani 1 1 d . . . . .
O51 O 0.18281(14) 0.15076(14) 0.40059(12) 0.0888(10) Uani 1 1 d . . . . .
O52 O 0.12250(12) 0.21446(13) 0.38883(11) 0.0831(9) Uani 1 1 d . . . . .
O71 O 0.2500 0.2500 0.3694(2) 0.0757(17) Uani 1 4 d S T P . .
C41 C 0.2158(2) 0.0509(2) 0.3163(2) 0.0860(14) Uani 1 1 d . . . . .
H41 H 0.2362 0.0420 0.3461 0.112 Uiso 1 1 calc R U . . .
C42 C 0.1929(2) 0.01084(19) 0.2869(2) 0.0891(15) Uani 1 1 d . . . . .
H42 H 0.1961 -0.0248 0.2976 0.116 Uiso 1 1 calc R U . . .
C43 C 0.1658(2) 0.0233(2) 0.2426(2) 0.0898(15) Uani 1 1 d . . . . .
H43 H 0.1513 -0.0035 0.2212 0.117 Uiso 1 1 calc R U . . .
C44 C 0.15984(18) 0.07587(19) 0.22948(18) 0.0745(13) Uani 1 1 d . . . . .
H44 H 0.1408 0.0855 0.1989 0.097 Uiso 1 1 calc R U . . .
C45 C 0.18130(18) 0.11362(18) 0.26051(15) 0.0643(11) Uani 1 1 d . . . . .
C46 C 0.17278(17) 0.17278(17) 0.2500 0.0579(15) Uani 1 2 d S T P . .
C51 C 0.1383(2) 0.1714(2) 0.40744(18) 0.0785(13) Uani 1 1 d . . . . .
C52 C 0.1000(2) 0.1408(2) 0.4416(2) 0.1115(19) Uani 1 1 d . . . . .
H52A H 0.1168 0.1082 0.4536 0.167 Uiso 1 1 calc R U . . .
H52B H 0.0901 0.1622 0.4719 0.167 Uiso 1 1 calc R U . . .
H52C H 0.0685 0.1321 0.4212 0.167 Uiso 1 1 calc R U . . .
H61 H 0.7500 0.0950 0.7500 0.050 Uiso 1 2 d S . P . .
H71 H 0.2500 0.2500 0.4047 0.050 Uiso 1 4 d S . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 2.259(3) 2_556 ?
Fe1 O1 2.259(3) 4_656 ?
Fe1 O1 2.259(3) 3_655 ?
Fe1 O1 2.259(3) . ?
Fe1 O11 2.261(3) 2_556 ?
Fe1 O11 2.261(3) 4_656 ?
Fe1 O11 2.261(3) 3_655 ?
Fe1 O11 2.261(3) . ?
Ni1 O32 2.008(3) 4_656 ?
Ni1 O1 2.027(3) . ?
Ni1 N1 2.052(4) . ?
Ni1 O21 2.065(3) . ?
Ni1 O11 2.103(3) . ?
Ni1 O61 2.2450(14) . ?
Ni2 O22 1.994(3) . ?
Ni2 O11 2.004(3) 4_656 ?
Ni2 N11 2.056(4) 3_655 ?
Ni2 O31 2.072(3) . ?
Ni2 O1 2.079(3) . ?
Ni2 O61 2.2850(15) . ?
N1 C5 1.324(5) . ?
N1 C1 1.353(5) . ?
O1 C6 1.398(4) . ?
N11 C15 1.338(5) . ?
N11 C11 1.348(5) . ?
N11 Fe2A 2.057(4) 3_655 ?
N11 Ni2 2.057(4) 3_655 ?
O11 C16 1.413(4) . ?
O11 Fe2A 2.004(3) 4_656 ?
O11 Ni2 2.004(3) 4_656 ?
O21 C21 1.271(6) . ?
O22 C21 1.240(6) . ?
O31 C31 1.230(5) . ?
O32 C31 1.259(5) . ?
O32 Fe1A 2.008(3) 4_656 ?
O32 Ni1 2.008(3) 4_656 ?
O61 Fe1A 2.2449(14) 4_656 ?
O61 Ni1 2.2449(14) 4_656 ?
O61 Fe2A 2.2851(15) 4_656 ?
O61 Ni2 2.2851(15) 4_656 ?
O61 H61 0.8807 . ?
C1 C2 1.364(7) . ?
C1 H1 0.9500 . ?
C2 C3 1.385(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.356(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.414(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.538(6) . ?
C6 O1 1.399(4) 3_655 ?
C6 C5 1.538(6) 3_655 ?
C11 C12 1.384(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.385(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.369(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.386(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.531(6) . ?
C16 O11 1.413(4) 2_556 ?
C16 C15 1.531(6) 2_556 ?
C21 C22 1.501(6) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C31 C32 1.518(6) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
Fe3 O41 2.258(3) . ?
Fe3 O41 2.258(3) 8 ?
Fe3 O41 2.258(3) 5 ?
Fe3 O41 2.258(3) 3 ?
Fe3 O41 2.258(3) 2 ?
Fe3 O41 2.258(3) 6 ?
Fe3 O41 2.258(3) 4 ?
Fe3 O41 2.258(3) 7 ?
Ni3 O52 2.009(3) 7 ?
Ni3 O41 2.019(3) 5 ?
Ni3 O51 2.037(3) . ?
Ni3 N41 2.041(4) . ?
Ni3 O41 2.090(3) 4 ?
Ni3 O71 2.2589(16) . ?
N41 C45 1.332(5) . ?
N41 C41 1.367(5) . ?
O41 C46 1.396(4) . ?
O41 Fe3A 2.019(3) 5 ?
O41 Ni3 2.019(3) 5 ?
O41 Fe3A 2.090(3) 4 ?
O41 Ni3 2.090(3) 4 ?
O51 C51 1.259(6) . ?
O52 C51 1.259(5) . ?
O52 Fe3A 2.009(3) 6 ?
O52 Ni3 2.009(3) 6 ?
O71 Fe3A 2.2589(16) 6 ?
O71 Ni3 2.2589(16) 6 ?
O71 Ni3 2.2589(16) 3 ?
O71 Fe3A 2.2589(16) 3 ?
O71 Fe3A 2.2589(16) 7 ?
O71 Ni3 2.2589(16) 7 ?
O71 H71 0.9021 . ?
C41 C42 1.392(7) . ?
C41 H41 0.9500 . ?
C42 C43 1.360(7) . ?
C42 H42 0.9500 . ?
C43 C44 1.386(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.359(6) . ?
C44 H44 0.9500 . ?
C45 C46 1.542(6) . ?
C46 O41 1.396(4) 5 ?
C46 C45 1.542(6) 5 ?
C51 C52 1.519(6) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O1 60.48(15) 2_556 4_656 ?
O1 Fe1 O1 121.38(15) 2_556 3_655 ?
O1 Fe1 O1 166.44(14) 4_656 3_655 ?
O1 Fe1 O1 166.44(14) 2_556 . ?
O1 Fe1 O1 121.38(15) 4_656 . ?
O1 Fe1 O1 60.47(15) 3_655 . ?
O1 Fe1 O11 76.55(10) 2_556 2_556 ?
O1 Fe1 O11 92.38(10) 4_656 2_556 ?
O1 Fe1 O11 75.77(10) 3_655 2_556 ?
O1 Fe1 O11 115.91(9) . 2_556 ?
O1 Fe1 O11 92.38(10) 2_556 4_656 ?
O1 Fe1 O11 76.55(10) 4_656 4_656 ?
O1 Fe1 O11 115.91(9) 3_655 4_656 ?
O1 Fe1 O11 75.77(10) . 4_656 ?
O11 Fe1 O11 167.30(12) 2_556 4_656 ?
O1 Fe1 O11 75.77(10) 2_556 3_655 ?
O1 Fe1 O11 115.91(9) 4_656 3_655 ?
O1 Fe1 O11 76.55(10) 3_655 3_655 ?
O1 Fe1 O11 92.38(10) . 3_655 ?
O11 Fe1 O11 121.50(14) 2_556 3_655 ?
O11 Fe1 O11 60.13(14) 4_656 3_655 ?
O1 Fe1 O11 115.91(9) 2_556 . ?
O1 Fe1 O11 75.77(10) 4_656 . ?
O1 Fe1 O11 92.38(10) 3_655 . ?
O1 Fe1 O11 76.55(10) . . ?
O11 Fe1 O11 60.13(14) 2_556 . ?
O11 Fe1 O11 121.50(14) 4_656 . ?
O11 Fe1 O11 167.30(12) 3_655 . ?
O32 Ni1 O1 172.11(13) 4_656 . ?
O32 Ni1 N1 92.67(14) 4_656 . ?
O1 Ni1 N1 80.14(14) . . ?
O32 Ni1 O21 84.84(13) 4_656 . ?
O1 Ni1 O21 98.41(12) . . ?
N1 Ni1 O21 90.88(13) . . ?
O32 Ni1 O11 92.63(12) 4_656 . ?
O1 Ni1 O11 85.35(11) . . ?
N1 Ni1 O11 98.91(12) . . ?
O21 Ni1 O11 170.01(12) . . ?
O32 Ni1 O61 106.35(11) 4_656 . ?
O1 Ni1 O61 80.79(11) . . ?
N1 Ni1 O61 160.93(14) . . ?
O21 Ni1 O61 92.14(12) . . ?
O11 Ni1 O61 79.27(10) . . ?
O22 Ni2 O11 176.37(14) . 4_656 ?
O22 Ni2 N11 95.00(14) . 3_655 ?
O11 Ni2 N11 81.42(13) 4_656 3_655 ?
O22 Ni2 O31 84.50(13) . . ?
O11 Ni2 O31 94.68(12) 4_656 . ?
N11 Ni2 O31 87.70(14) 3_655 . ?
O22 Ni2 O1 95.50(12) . . ?
O11 Ni2 O1 85.65(11) 4_656 . ?
N11 Ni2 O1 97.65(13) 3_655 . ?
O31 Ni2 O1 174.62(12) . . ?
O22 Ni2 O61 103.22(13) . . ?
O11 Ni2 O61 80.38(11) 4_656 . ?
N11 Ni2 O61 161.66(13) 3_655 . ?
O31 Ni2 O61 95.99(11) . . ?
O1 Ni2 O61 78.76(11) . . ?
C5 N1 C1 118.6(4) . . ?
C5 N1 Ni1 114.4(3) . . ?
C1 N1 Ni1 126.9(3) . . ?
C6 O1 Ni1 115.34(17) . . ?
C6 O1 Ni2 144.09(19) . . ?
Ni1 O1 Ni2 96.57(13) . . ?
C6 O1 Fe1 95.3(2) . . ?
Ni1 O1 Fe1 97.91(11) . . ?
Ni2 O1 Fe1 96.16(11) . . ?
C15 N11 C11 119.1(4) . . ?
C15 N11 Fe2A 114.0(3) . 3_655 ?
C11 N11 Fe2A 126.7(3) . 3_655 ?
C15 N11 Ni2 114.0(3) . 3_655 ?
C11 N11 Ni2 126.7(3) . 3_655 ?
Fe2A N11 Ni2 0.0 3_655 3_655 ?
C16 O11 Fe2A 114.80(15) . 4_656 ?
C16 O11 Ni2 114.80(15) . 4_656 ?
Fe2A O11 Ni2 0.0 4_656 4_656 ?
C16 O11 Ni1 144.10(18) . . ?
Fe2A O11 Ni1 96.51(12) 4_656 . ?
Ni2 O11 Ni1 96.51(12) 4_656 . ?
C16 O11 Fe1 96.7(3) . . ?
Fe2A O11 Fe1 98.29(12) 4_656 . ?
Ni2 O11 Fe1 98.29(12) 4_656 . ?
Ni1 O11 Fe1 95.64(11) . . ?
C21 O21 Ni1 129.3(3) . . ?
C21 O22 Ni2 125.7(3) . . ?
C31 O31 Ni2 130.1(3) . . ?
C31 O32 Fe1A 126.2(3) . 4_656 ?
C31 O32 Ni1 126.2(3) . 4_656 ?
Fe1A O32 Ni1 0.0 4_656 4_656 ?
Fe1A O61 Ni1 0.0 4_656 4_656 ?
Fe1A O61 Ni1 146.8 4_656 . ?
Ni1 O61 Ni1 146.8(2) 4_656 . ?
Fe1A O61 Ni2 85.16(6) 4_656 . ?
Ni1 O61 Ni2 85.16(6) 4_656 . ?
Ni1 O61 Ni2 85.14(6) . . ?
Fe1A O61 Fe2A 85.14(6) 4_656 4_656 ?
Ni1 O61 Fe2A 85.14(6) 4_656 4_656 ?
Ni1 O61 Fe2A 85.16(6) . 4_656 ?
Ni2 O61 Fe2A 145.5 . 4_656 ?
Fe1A O61 Ni2 85.14(6) 4_656 4_656 ?
Ni1 O61 Ni2 85.14(6) 4_656 4_656 ?
Ni1 O61 Ni2 85.16(6) . 4_656 ?
Ni2 O61 Ni2 145.5(2) . 4_656 ?
Fe2A O61 Ni2 0.0 4_656 4_656 ?
Fe1A O61 H61 106.6 4_656 . ?
Ni1 O61 H61 106.6 4_656 . ?
Ni1 O61 H61 106.6 . . ?
Ni2 O61 H61 107.2 . . ?
Fe2A O61 H61 107.2 4_656 . ?
Ni2 O61 H61 107.2 4_656 . ?
N1 C1 C2 123.2(5) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C1 C2 C3 117.9(5) . . ?
C1 C2 H2 121.0 . . ?
C3 C2 H2 121.0 . . ?
C4 C3 C2 120.2(5) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 118.8(5) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 121.2(4) . . ?
N1 C5 C6 117.0(4) . . ?
C4 C5 C6 121.8(4) . . ?
O1 C6 O1 108.9(4) . 3_655 ?
O1 C6 C5 110.2(2) . 3_655 ?
O1 C6 C5 109.7(2) 3_655 3_655 ?
O1 C6 C5 109.7(2) . . ?
O1 C6 C5 110.3(2) 3_655 . ?
C5 C6 C5 108.0(5) 3_655 . ?
N11 C11 C12 121.4(5) . . ?
N11 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C11 C12 C13 119.2(5) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
C14 C13 C12 119.0(5) . . ?
C14 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
C13 C14 C15 119.4(5) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
N11 C15 C14 121.9(4) . . ?
N11 C15 C16 116.2(4) . . ?
C14 C15 C16 121.8(4) . . ?
O11 C16 O11 106.5(5) . 2_556 ?
O11 C16 C15 111.2(2) . 2_556 ?
O11 C16 C15 109.54(18) 2_556 2_556 ?
O11 C16 C15 109.54(18) . . ?
O11 C16 C15 111.2(2) 2_556 . ?
C15 C16 C15 108.8(5) 2_556 . ?
O22 C21 O21 126.4(4) . . ?
O22 C21 C22 117.0(5) . . ?
O21 C21 C22 116.6(5) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O31 C31 O32 125.6(5) . . ?
O31 C31 C32 119.2(5) . . ?
O32 C31 C32 115.1(5) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O41 Fe3 O41 167.33(13) . 8 ?
O41 Fe3 O41 60.07(13) . 5 ?
O41 Fe3 O41 121.56(13) 8 5 ?
O41 Fe3 O41 121.56(13) . 3 ?
O41 Fe3 O41 60.07(13) 8 3 ?
O41 Fe3 O41 167.33(13) 5 3 ?
O41 Fe3 O41 115.43(13) . 2 ?
O41 Fe3 O41 76.21(6) 8 2 ?
O41 Fe3 O41 76.21(6) 5 2 ?
O41 Fe3 O41 92.71(13) 3 2 ?
O41 Fe3 O41 76.21(6) . 6 ?
O41 Fe3 O41 115.43(13) 8 6 ?
O41 Fe3 O41 92.71(13) 5 6 ?
O41 Fe3 O41 76.21(6) 3 6 ?
O41 Fe3 O41 60.07(13) 2 6 ?
O41 Fe3 O41 92.71(13) . 4 ?
O41 Fe3 O41 76.21(6) 8 4 ?
O41 Fe3 O41 76.21(6) 5 4 ?
O41 Fe3 O41 115.43(13) 3 4 ?
O41 Fe3 O41 121.56(13) 2 4 ?
O41 Fe3 O41 167.33(13) 6 4 ?
O41 Fe3 O41 76.21(6) . 7 ?
O41 Fe3 O41 92.71(13) 8 7 ?
O41 Fe3 O41 115.43(13) 5 7 ?
O41 Fe3 O41 76.21(6) 3 7 ?
O41 Fe3 O41 167.33(13) 2 7 ?
O41 Fe3 O41 121.56(13) 6 7 ?
O41 Fe3 O41 60.07(13) 4 7 ?
O52 Ni3 O41 173.55(12) 7 5 ?
O52 Ni3 O51 84.64(12) 7 . ?
O41 Ni3 O51 97.41(12) 5 . ?
O52 Ni3 N41 94.11(14) 7 . ?
O41 Ni3 N41 79.85(12) 5 . ?
O51 Ni3 N41 88.99(15) . . ?
O52 Ni3 O41 93.35(11) 7 4 ?
O41 Ni3 O41 85.41(14) 5 4 ?
O51 Ni3 O41 172.11(13) . 4 ?
N41 Ni3 O41 98.77(13) . 4 ?
O52 Ni3 O71 105.48(13) 7 . ?
O41 Ni3 O71 80.53(12) 5 . ?
O51 Ni3 O71 94.10(14) . . ?
N41 Ni3 O71 160.37(14) . . ?
O41 Ni3 O71 79.06(12) 4 . ?
C45 N41 C41 117.7(4) . . ?
C45 N41 Ni3 116.0(3) . . ?
C41 N41 Ni3 126.2(3) . . ?
C46 O41 Fe3A 115.73(16) . 5 ?
C46 O41 Ni3 115.73(16) . 5 ?
Fe3A O41 Ni3 0.0 5 5 ?
C46 O41 Fe3A 143.80(19) . 4 ?
Fe3A O41 Fe3A 96.24(11) 5 4 ?
Ni3 O41 Fe3A 96.24(11) 5 4 ?
C46 O41 Ni3 143.80(19) . 4 ?
Fe3A O41 Ni3 96.2 5 4 ?
Ni3 O41 Ni3 96.24(11) 5 4 ?
Fe3A O41 Ni3 0.0 4 4 ?
C46 O41 Fe3 95.9(2) . . ?
Fe3A O41 Fe3 97.99(11) 5 . ?
Ni3 O41 Fe3 97.99(11) 5 . ?
Fe3A O41 Fe3 95.94(11) 4 . ?
Ni3 O41 Fe3 95.94(11) 4 . ?
C51 O51 Ni3 129.1(3) . . ?
C51 O52 Fe3A 125.0(3) . 6 ?
C51 O52 Ni3 125.0(3) . 6 ?
Fe3A O52 Ni3 0.0 6 6 ?
Ni3 O71 Fe3A 85.3 . 6 ?
Ni3 O71 Ni3 85.26(7) . 6 ?
Fe3A O71 Ni3 0.0 6 6 ?
Ni3 O71 Ni3 146.6(3) . 3 ?
Fe3A O71 Ni3 85.3 6 3 ?
Ni3 O71 Ni3 85.26(7) 6 3 ?
Ni3 O71 Fe3A 146.6 . 3 ?
Fe3A O71 Fe3A 85.26(7) 6 3 ?
Ni3 O71 Fe3A 85.26(7) 6 3 ?
Ni3 O71 Fe3A 0.00(3) 3 3 ?
Ni3 O71 Fe3A 85.3 . 7 ?
Fe3A O71 Fe3A 146.6(3) 6 7 ?
Ni3 O71 Fe3A 146.6(3) 6 7 ?
Ni3 O71 Fe3A 85.26(7) 3 7 ?
Fe3A O71 Fe3A 85.26(7) 3 7 ?
Ni3 O71 Ni3 85.26(7) . 7 ?
Fe3A O71 Ni3 146.6 6 7 ?
Ni3 O71 Ni3 146.6(3) 6 7 ?
Ni3 O71 Ni3 85.26(7) 3 7 ?
Fe3A O71 Ni3 85.3 3 7 ?
Fe3A O71 Ni3 0.0 7 7 ?
Ni3 O71 H71 106.7 . . ?
Fe3A O71 H71 106.7 6 . ?
Ni3 O71 H71 106.7 6 . ?
Ni3 O71 H71 106.7 3 . ?
Fe3A O71 H71 106.7 3 . ?
Fe3A O71 H71 106.7 7 . ?
Ni3 O71 H71 106.7 7 . ?
N41 C41 C42 121.4(5) . . ?
N41 C41 H41 119.3 . . ?
C42 C41 H41 119.3 . . ?
C43 C42 C41 119.3(5) . . ?
C43 C42 H42 120.4 . . ?
C41 C42 H42 120.4 . . ?
C42 C43 C44 118.8(5) . . ?
C42 C43 H43 120.6 . . ?
C44 C43 H43 120.6 . . ?
C45 C44 C43 119.7(5) . . ?
C45 C44 H44 120.2 . . ?
C43 C44 H44 120.2 . . ?
N41 C45 C44 123.0(4) . . ?
N41 C45 C46 115.0(4) . . ?
C44 C45 C46 122.0(4) . . ?
O41 C46 O41 108.1(5) 5 . ?
O41 C46 C45 110.47(19) 5 . ?
O41 C46 C45 110.07(19) . . ?
O41 C46 C45 110.07(19) 5 5 ?
O41 C46 C45 110.47(19) . 5 ?
C45 C46 C45 107.7(5) . 5 ?
O52 C51 O51 126.5(5) . . ?
O52 C51 C52 117.3(5) . . ?
O51 C51 C52 116.2(5) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?

_refine_diff_density_max         0.700
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.065

# SQUEEZE RESULTS (Version = 290617)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.010 -0.009 0.007 7981 1443 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 1 0 2.459
0 2 0 3.479
2 2 0 4.923
1 3 0 5.505
0 1 1 2.452
1 2 1 4.258
0 3 1 5.502
1 3 1 5.772
0 0 2 3.460
1 1 2 4.246
0 2 2 4.909
1 2 2 5.209
2 2 2 6.022
0 4 2 7.789
2 5 2 10.030
0 1 3 5.478
1 2 3 6.495
2 2 4 8.516
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
TITL shelxl    P 4/n n c    R = 0.13
CELL   25.4102   25.4102   25.5493     90.00     90.00     90.00
SPGR P4/nnc
# Solvent Accessible Volume =      7955
# Electrons Found in S.A.V. =      1417
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
C101 0.131 0.979 0.417 !       2.72 eA-3
C102 0.538 0.133 0.471 !       2.43 eA-3
C103 0.500 0.051 0.142 !       2.34 eA-3
C104 0.448 0.460 0.148 !       2.09 eA-3
C105 0.938 0.446 0.627 !       1.96 eA-3
C106 0.137 0.548 0.990 !       1.68 eA-3
C107 0.617 0.766 0.486 !       1.60 eA-3
C108 0.734 0.917 0.006 !       1.50 eA-3
C109 0.508 0.603 0.444 !       1.35 eA-3
C110 0.584 0.964 0.429 !       1.13 eA-3
C111 0.561 0.982 0.463 !       1.04 eA-3
C112 0.250 0.248 0.016 !       0.97 eA-3
Q113 0.330 0.876 0.178 !       0.96 eA-3
C114 0.778 0.916 0.067 !       0.95 eA-3
C115 0.924 0.835 0.204 !       0.94 eA-3
C116 0.751 0.952 0.030 !       0.93 eA-3
Q117 0.291 0.137 0.153 !       0.88 eA-3
Q118 0.272 0.679 0.320 !       0.87 eA-3
C119 0.250 0.252 0.641 !       0.87 eA-3
C120 0.910 0.920 0.087 !       0.83 eA-3
Q121 0.635 0.734 0.656 !       0.81 eA-3
Q122 0.171 0.683 0.183 !       0.80 eA-3
C123 0.891 0.625 0.316 !       0.80 eA-3
C124 0.874 0.907 0.364 !       0.78 eA-3
C125 0.640 0.914 0.228 !       0.77 eA-3
C126 0.595 0.842 0.345 !       0.72 eA-3
Q127 0.197 0.265 0.159 !       0.69 eA-3
Q128 0.276 0.781 0.247 !       0.69 eA-3
C129 0.097 0.094 0.891 !       0.69 eA-3
Q130 0.371 0.855 0.794 !       0.68 eA-3
C131 0.886 0.927 0.424 !       0.67 eA-3
C132 0.892 0.673 0.285 !       0.67 eA-3
C133 0.594 0.939 0.108 !       0.67 eA-3
C134 0.791 0.580 0.229 !       0.65 eA-3
Q135 0.233 0.627 0.181 !       0.65 eA-3
Q136 0.795 0.802 0.655 !       0.65 eA-3
C137 0.048 0.146 0.789 !       0.65 eA-3
Q138 0.627 0.293 0.297 !       0.64 eA-3
Q139 0.778 0.719 0.753 !       0.63 eA-3
Q140 0.685 0.151 0.199 !       0.63 eA-3
Q141 0.687 0.294 0.302 !       0.61 eA-3
C142 0.584 0.923 0.346 !       0.57 eA-3
C143 0.593 0.906 0.251 !       0.54 eA-3
C144 0.963 0.954 0.089 !       0.54 eA-3
C145 0.750 0.922 0.248 !       0.54 eA-3
C146 0.094 0.108 0.702 !       0.53 eA-3
C147 0.628 0.861 0.340 !       0.52 eA-3
Q148 0.208 0.945 0.092 !       0.52 eA-3
C149 0.702 0.625 0.105 !       0.52 eA-3
C150 0.791 0.607 0.243 !       0.52 eA-3
Q151 0.158 0.020 0.228 !       0.51 eA-3
;

_shelxl_version_number           2014/6

# start Validation Reply Form
_vrf_CHEMW03_shelxl              
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: This alert is generated because squeeze program has been
used to exlude the solvent molecules during the refinement. The cif 
file contains the complete molecular formula; however some of the 
atoms reported are not listed in the fractional coordinates' list.
;
_vrf_PLAT420_shelxl              
;
PROBLEM: D-H Without Acceptor       O61    --  H61    ...     Please Check 
RESPONSE: These are tetradentate hydroxyl groups which are nested within 
the clusters, thus rendering the intermolecular hydrogen bonds impossible.  
The closest intramolecular OH...O distances are larger than 3.0 A.
;
_vrf_PLAT910_shelxl              
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         15 Note  
RESPONSE: This alert is probably due to instrument limitations. The number
of mising reflections is very small and in any case the ratio of reflections
to parameters refined is well above the ideal value of ten.
;
# end Validation Reply Form



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

data_shelxl_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1033941'
_audit_update_record             
;
2017-09-08 deposited with the CCDC.
2017-09-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C77.33 H85.60 Fe9 N16.67 Ni0 O26.80'
_chemical_formula_weight         2180.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_H-M_alt        'P 4/n n c'
_space_group_name_Hall           '-P 4a 2bc'

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

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

_cell_length_a                   25.6264(5)
_cell_length_b                   25.6264(5)
_cell_length_c                   25.3002(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     16615.0(7)
_cell_formula_units_Z            6
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    22572
_cell_measurement_theta_min      6.51
_cell_measurement_theta_max      72.03

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            orange-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_F_000             6688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    9.752
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.201
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38901
_diffrn_reflns_av_unetI/netI     0.2693
_diffrn_reflns_av_R_equivalents  0.3563
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         6.517
_diffrn_reflns_theta_max         49.980
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.564
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.564
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.564
_reflns_number_total             4254
_reflns_number_gt                2342
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

 All metal ions were assumed to be iron(II) and refined as 
 such, albeit the presence of small amounts of nickel(II) in 
 the reaction.
;

_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond ver.3.1.'
_computing_publication_material  'publCIF J.Appl.Cryst. 2010, 43, 920'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] 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     SHELXL
_refine_ls_extinction_coef       0.106(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4254
_refine_ls_number_parameters     240
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2477
_refine_ls_R_factor_gt           0.2074
_refine_ls_wR_factor_ref         0.4775
_refine_ls_wR_factor_gt          0.4505
_refine_ls_goodness_of_fit_ref   1.567
_refine_ls_restrained_S_all      1.567
_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
Fe1 Fe 0.7500 0.2500 0.7500 0.057(3) Uani 1 4 d S T P . .
NI1 Fe 0.79952(17) 0.15328(15) 0.68010(15) 0.0658(18) Uani 1 1 d . . . . .
NI2 Fe 0.67877(17) 0.15501(14) 0.69831(15) 0.0639(18) Uani 1 1 d . . . . .
N1 N 0.8194(9) 0.1979(8) 0.6163(10) 0.093(8) Uani 1 1 d . . . . .
O1 O 0.7430(6) 0.2069(6) 0.6734(7) 0.065(5) Uani 1 1 d . . . . .
N11 N 0.8870(9) 0.2973(7) 0.6701(7) 0.073(6) Uani 1 1 d . . . . .
O11 O 0.8256(6) 0.2069(7) 0.7422(6) 0.070(5) Uani 1 1 d . . . . .
O21 O 0.7739(7) 0.0944(7) 0.6314(7) 0.089(6) Uani 1 1 d . . . . .
O22 O 0.6785(8) 0.1061(7) 0.6345(6) 0.103(7) Uani 1 1 d . . . . .
O31 O 0.6232(8) 0.1013(6) 0.7318(6) 0.088(6) Uani 1 1 d . . . . .
O32 O 0.6338(7) 0.1104(6) 0.8168(7) 0.084(6) Uani 1 1 d . . . . .
O61 O 0.7500 0.1258(7) 0.7500 0.085(9) Uani 1 2 d S T P . .
C1 C 0.8657(11) 0.1878(11) 0.5773(11) 0.080(8) Uiso 1 1 d . . . . .
H1 H 0.8855 0.1571 0.5834 0.096 Uiso 1 1 calc R U . . .
C2 C 0.8795(11) 0.2150(10) 0.5396(11) 0.086(9) Uiso 1 1 d . . . . .
H2 H 0.9075 0.2037 0.5178 0.103 Uiso 1 1 calc R U . . .
C3 C 0.8534(12) 0.2647(12) 0.5280(13) 0.113(11) Uiso 1 1 d . . . . .
H3 H 0.8635 0.2884 0.5010 0.136 Uiso 1 1 calc R U . . .
C4 C 0.8103(10) 0.2721(11) 0.5634(10) 0.076(8) Uiso 1 1 d . . . . .
H4 H 0.7895 0.3024 0.5584 0.091 Uiso 1 1 calc R U . . .
C5 C 0.7974(9) 0.2404(9) 0.6022(9) 0.048(6) Uiso 1 1 d . . . . .
C6 C 0.7500 0.2500 0.6429(15) 0.067(11) Uiso 1 2 d S . P . .
C11 C 0.9204(10) 0.3071(10) 0.6303(10) 0.074(8) Uiso 1 1 d . . . . .
H11 H 0.9142 0.3368 0.6087 0.089 Uiso 1 1 calc R U . . .
C12 C 0.9643(13) 0.2752(13) 0.6189(14) 0.128(12) Uiso 1 1 d . . . . .
H12 H 0.9873 0.2839 0.5908 0.154 Uiso 1 1 calc R U . . .
C13 C 0.9730(12) 0.2314(11) 0.6493(10) 0.094(9) Uiso 1 1 d . . . . .
H13 H 1.0012 0.2082 0.6429 0.113 Uiso 1 1 calc R U . . .
C14 C 0.9358(13) 0.2236(13) 0.6918(12) 0.108(11) Uiso 1 1 d . . . . .
H14 H 0.9410 0.1949 0.7149 0.130 Uiso 1 1 calc R U . . .
C15 C 0.8938(10) 0.2551(10) 0.7006(10) 0.058(7) Uiso 1 1 d . . . . .
C16 C 0.8570(15) 0.2500 0.7500 0.063(10) Uiso 1 2 d S . P . .
C21 C 0.7281(15) 0.0810(13) 0.6182(12) 0.102(10) Uiso 1 1 d . . . . .
C22 C 0.7119(11) 0.0357(10) 0.5830(11) 0.099(9) Uiso 1 1 d . . . . .
H22A H 0.6738 0.0350 0.5799 0.128 Uiso 1 1 calc R U . . .
H22B H 0.7274 0.0400 0.5478 0.128 Uiso 1 1 calc R U . . .
H22C H 0.7240 0.0028 0.5985 0.128 Uiso 1 1 calc R U . . .
C31 C 0.6072(14) 0.0891(14) 0.7736(16) 0.107(11) Uiso 1 1 d . . . . .
C32 C 0.5631(13) 0.0640(13) 0.7901(13) 0.116(11) Uiso 1 1 d . . . . .
H32A H 0.5635 0.0608 0.8287 0.150 Uiso 1 1 calc R U . . .
H32B H 0.5323 0.0840 0.7792 0.150 Uiso 1 1 calc R U . . .
H32C H 0.5617 0.0291 0.7742 0.150 Uiso 1 1 calc R U . . .
Fe3 Fe 0.2500 0.2500 0.2500 0.047(3) Uani 1 8 d S T P . .
NI3 Fe 0.23753(15) 0.16487(14) 0.34767(14) 0.0576(18) Uani 1 1 d . . . . .
N41 N 0.2073(7) 0.1051(7) 0.3019(8) 0.065(6) Uani 1 1 d . . . . .
O41 O 0.2000(5) 0.1889(5) 0.2051(6) 0.047(4) Uani 1 1 d . . . . .
O51 O 0.1789(6) 0.1486(7) 0.4065(6) 0.077(6) Uani 1 1 d . . . . .
O52 O 0.1236(6) 0.2127(6) 0.3942(7) 0.077(5) Uani 1 1 d . . . . .
O71 O 0.2500 0.2500 0.3750(11) 0.042(7) Uani 1 4 d S T P . .
C41 C 0.2149(13) 0.0508(13) 0.3167(12) 0.110(10) Uiso 1 1 d . . . . .
H41 H 0.2347 0.0407 0.3467 0.132 Uiso 1 1 calc R U . . .
C42 C 0.1910(13) 0.0154(14) 0.2838(13) 0.117(11) Uiso 1 1 d . . . . .
H42 H 0.1929 -0.0200 0.2948 0.140 Uiso 1 1 calc R U . . .
C43 C 0.1655(11) 0.0239(12) 0.2387(11) 0.097(10) Uiso 1 1 d . . . . .
H43 H 0.1530 -0.0032 0.2165 0.116 Uiso 1 1 calc R U . . .
C44 C 0.1589(9) 0.0803(10) 0.2265(10) 0.063(7) Uiso 1 1 d . . . . .
H44 H 0.1380 0.0917 0.1977 0.075 Uiso 1 1 calc R U . . .
C45 C 0.1833(10) 0.1138(10) 0.2575(9) 0.056(7) Uiso 1 1 d . . . . .
C46 C 0.1739(10) 0.1739(10) 0.2500 0.055(10) Uiso 1 2 d S . P . .
C51 C 0.1350(10) 0.1685(10) 0.4142(9) 0.052(6) Uiso 1 1 d . . . . .
C52 C 0.0942(12) 0.1391(12) 0.4409(12) 0.116(11) Uiso 1 1 d . . . . .
H52A H 0.0627 0.1606 0.4434 0.151 Uiso 1 1 calc R U . . .
H52B H 0.0865 0.1074 0.4208 0.151 Uiso 1 1 calc R U . . .
H52C H 0.1060 0.1297 0.4765 0.151 Uiso 1 1 calc R U . . .
H61 H 0.7500 0.0950 0.7500 0.050 Uiso 1 2 d S . P . .
H71 H 0.2500 0.2500 0.4047 0.050 Uiso 1 4 d S . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 2.237(17) 2_556 ?
Fe1 O1 2.237(17) 4_656 ?
Fe1 O1 2.237(17) 3_655 ?
Fe1 O1 2.237(17) . ?
Fe1 O11 2.239(16) 2_556 ?
Fe1 O11 2.239(16) 4_656 ?
Fe1 O11 2.239(16) 3_655 ?
Fe1 O11 2.239(16) . ?
NI1 O1 2.004(16) . ?
NI1 O32 2.033(19) 4_656 ?
NI1 N1 2.04(2) . ?
NI1 O21 2.056(17) . ?
NI1 O11 2.192(16) . ?
NI1 O61 2.288(7) . ?
NI2 O11 2.012(18) 4_656 ?
NI2 O22 2.044(15) . ?
NI2 O31 2.153(19) . ?
NI2 N11 2.20(2) 3_655 ?
NI2 O1 2.209(16) . ?
NI2 O61 2.367(7) . ?
N1 C5 1.28(3) . ?
N1 C1 1.56(3) . ?
O1 C6 1.36(2) . ?
N11 C15 1.34(3) . ?
N11 C11 1.34(3) . ?
N11 NI2 2.20(2) 3_655 ?
O11 C16 1.38(2) . ?
O11 NI2 2.012(18) 4_656 ?
O21 C21 1.27(3) . ?
O22 C21 1.48(3) . ?
O31 C31 1.18(4) . ?
O32 C31 1.40(4) . ?
O32 NI1 2.033(19) 4_656 ?
O61 NI1 2.288(7) 4_656 ?
O61 NI2 2.367(7) 4_656 ?
O61 H61 0.7901 . ?
C1 C2 1.23(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.47(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.43(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.32(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.61(3) . ?
C6 O1 1.36(2) 3_655 ?
C6 C5 1.61(3) 3_655 ?
C11 C12 1.42(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.38(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.45(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.37(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.57(3) . ?
C16 O11 1.38(2) 2_556 ?
C16 C15 1.57(3) 2_556 ?
C21 C22 1.52(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C31 C32 1.37(4) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
Fe3 O41 2.321(15) 8 ?
Fe3 O41 2.321(15) 5 ?
Fe3 O41 2.321(15) 2 ?
Fe3 O41 2.321(15) 3 ?
Fe3 O41 2.321(15) 6 ?
Fe3 O41 2.321(15) 7 ?
Fe3 O41 2.321(15) 4 ?
Fe3 O41 2.321(15) . ?
NI3 O52 2.033(17) 7 ?
NI3 O41 2.037(15) 5 ?
NI3 N41 2.07(2) . ?
NI3 O51 2.156(15) . ?
NI3 O41 2.173(12) 4 ?
NI3 O71 2.311(9) . ?
N41 C45 1.30(3) . ?
N41 C41 1.45(3) . ?
O41 C46 1.37(2) . ?
O41 NI3 2.037(15) 5 ?
O41 NI3 2.173(12) 4 ?
O51 C51 1.25(3) . ?
O52 C51 1.27(2) . ?
O52 NI3 2.033(17) 6 ?
O71 NI3 2.311(9) 6 ?
O71 NI3 2.311(9) 3 ?
O71 NI3 2.311(9) 7 ?
O71 H71 0.7513 . ?
C41 C42 1.37(4) . ?
C41 H41 0.9500 . ?
C42 C43 1.33(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.49(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.32(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.57(3) . ?
C46 O41 1.37(2) 5 ?
C46 C45 1.57(3) 5 ?
C51 C52 1.46(3) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O1 60.0(8) 2_556 4_656 ?
O1 Fe1 O1 120.9(8) 2_556 3_655 ?
O1 Fe1 O1 170.8(8) 4_656 3_655 ?
O1 Fe1 O1 170.8(8) 2_556 . ?
O1 Fe1 O1 120.9(8) 4_656 . ?
O1 Fe1 O1 60.0(8) 3_655 . ?
O1 Fe1 O11 75.5(6) 2_556 2_556 ?
O1 Fe1 O11 95.6(6) 4_656 2_556 ?
O1 Fe1 O11 76.4(6) 3_655 2_556 ?
O1 Fe1 O11 112.9(5) . 2_556 ?
O1 Fe1 O11 95.6(6) 2_556 4_656 ?
O1 Fe1 O11 75.5(6) 4_656 4_656 ?
O1 Fe1 O11 112.9(5) 3_655 4_656 ?
O1 Fe1 O11 76.4(6) . 4_656 ?
O11 Fe1 O11 169.9(8) 2_556 4_656 ?
O1 Fe1 O11 76.4(6) 2_556 3_655 ?
O1 Fe1 O11 112.9(5) 4_656 3_655 ?
O1 Fe1 O11 75.5(6) 3_655 3_655 ?
O1 Fe1 O11 95.6(6) . 3_655 ?
O11 Fe1 O11 120.9(9) 2_556 3_655 ?
O11 Fe1 O11 60.1(9) 4_656 3_655 ?
O1 Fe1 O11 112.9(5) 2_556 . ?
O1 Fe1 O11 76.3(6) 4_656 . ?
O1 Fe1 O11 95.6(6) 3_655 . ?
O1 Fe1 O11 75.5(6) . . ?
O11 Fe1 O11 60.1(9) 2_556 . ?
O11 Fe1 O11 120.9(9) 4_656 . ?
O11 Fe1 O11 169.9(8) 3_655 . ?
O1 NI1 O32 168.9(6) . 4_656 ?
O1 NI1 N1 74.3(8) . . ?
O32 NI1 N1 97.1(8) 4_656 . ?
O1 NI1 O21 102.8(7) . . ?
O32 NI1 O21 84.0(7) 4_656 . ?
N1 NI1 O21 91.0(8) . . ?
O1 NI1 O11 81.4(7) . . ?
O32 NI1 O11 93.1(7) 4_656 . ?
N1 NI1 O11 98.0(7) . . ?
O21 NI1 O11 170.9(7) . . ?
O1 NI1 O61 82.8(6) . . ?
O32 NI1 O61 105.7(6) 4_656 . ?
N1 NI1 O61 157.1(8) . . ?
O21 NI1 O61 93.5(6) . . ?
O11 NI1 O61 78.9(5) . . ?
O11 NI2 O22 175.0(8) 4_656 . ?
O11 NI2 O31 95.2(6) 4_656 . ?
O22 NI2 O31 85.3(6) . . ?
O11 NI2 N11 80.4(7) 4_656 3_655 ?
O22 NI2 N11 94.7(8) . 3_655 ?
O31 NI2 N11 88.6(7) . 3_655 ?
O11 NI2 O1 81.8(6) 4_656 . ?
O22 NI2 O1 98.4(6) . . ?
O31 NI2 O1 171.8(7) . . ?
N11 NI2 O1 98.3(7) 3_655 . ?
O11 NI2 O61 80.7(6) 4_656 . ?
O22 NI2 O61 104.2(7) . . ?
O31 NI2 O61 95.2(6) . . ?
N11 NI2 O61 160.9(6) 3_655 . ?
O1 NI2 O61 76.9(5) . . ?
C5 N1 C1 107(2) . . ?
C5 N1 NI1 126(2) . . ?
C1 N1 NI1 126.5(18) . . ?
C6 O1 NI1 120.7(10) . . ?
C6 O1 NI2 138.5(10) . . ?
NI1 O1 NI2 95.8(7) . . ?
C6 O1 Fe1 94.6(17) . . ?
NI1 O1 Fe1 102.0(7) . . ?
NI2 O1 Fe1 96.3(6) . . ?
C15 N11 C11 120(2) . . ?
C15 N11 NI2 111.1(16) . 3_655 ?
C11 N11 NI2 128.7(18) . 3_655 ?
C16 O11 NI2 117.0(10) . 4_656 ?
C16 O11 NI1 141.5(10) . . ?
NI2 O11 NI1 96.0(7) 4_656 . ?
C16 O11 Fe1 95.6(17) . . ?
NI2 O11 Fe1 102.2(7) 4_656 . ?
NI1 O11 Fe1 96.2(6) . . ?
C21 O21 NI1 131(2) . . ?
C21 O22 NI2 118.8(18) . . ?
C31 O31 NI2 139(2) . . ?
C31 O32 NI1 131(2) . 4_656 ?
NI1 O61 NI1 144.2(9) . 4_656 ?
NI1 O61 NI2 84.4(3) . 4_656 ?
NI1 O61 NI2 84.5(3) 4_656 4_656 ?
NI1 O61 NI2 84.5(3) . . ?
NI1 O61 NI2 84.4(3) 4_656 . ?
NI2 O61 NI2 143.2(9) 4_656 . ?
NI1 O61 H61 107.9 . . ?
NI1 O61 H61 107.9 4_656 . ?
NI2 O61 H61 108.4 4_656 . ?
NI2 O61 H61 108.4 . . ?
C2 C1 N1 128(3) . . ?
C2 C1 H1 116.1 . . ?
N1 C1 H1 116.1 . . ?
C1 C2 C3 121(3) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 H2 119.6 . . ?
C4 C3 C2 110(3) . . ?
C4 C3 H3 125.0 . . ?
C2 C3 H3 125.0 . . ?
C5 C4 C3 125(3) . . ?
C5 C4 H4 117.4 . . ?
C3 C4 H4 117.4 . . ?
N1 C5 C4 129(3) . . ?
N1 C5 C6 106(2) . . ?
C4 C5 C6 125(2) . . ?
O1 C6 O1 111(3) . 3_655 ?
O1 C6 C5 112.8(10) . 3_655 ?
O1 C6 C5 109.8(11) 3_655 3_655 ?
O1 C6 C5 109.8(11) . . ?
O1 C6 C5 112.8(10) 3_655 . ?
C5 C6 C5 100(3) 3_655 . ?
N11 C11 C12 123(3) . . ?
N11 C11 H11 118.4 . . ?
C12 C11 H11 118.4 . . ?
C13 C12 C11 119(3) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
C12 C13 C14 115(3) . . ?
C12 C13 H13 122.6 . . ?
C14 C13 H13 122.6 . . ?
C15 C14 C13 124(3) . . ?
C15 C14 H14 118.0 . . ?
C13 C14 H14 118.0 . . ?
N11 C15 C14 119(3) . . ?
N11 C15 C16 117(2) . . ?
C14 C15 C16 124(3) . . ?
O11 C16 O11 109(3) . 2_556 ?
O11 C16 C15 107.6(11) . . ?
O11 C16 C15 113.4(12) 2_556 . ?
O11 C16 C15 113.4(12) . 2_556 ?
O11 C16 C15 107.6(11) 2_556 2_556 ?
C15 C16 C15 106(3) . 2_556 ?
O21 C21 O22 127(3) . . ?
O21 C21 C22 128(3) . . ?
O22 C21 C22 105(3) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O31 C31 C32 134(4) . . ?
O31 C31 O32 115(3) . . ?
C32 C31 O32 110(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O41 Fe3 O41 121.4(7) 8 5 ?
O41 Fe3 O41 76.1(3) 8 2 ?
O41 Fe3 O41 76.1(3) 5 2 ?
O41 Fe3 O41 59.6(7) 8 3 ?
O41 Fe3 O41 170.0(6) 5 3 ?
O41 Fe3 O41 95.1(7) 2 3 ?
O41 Fe3 O41 113.0(6) 8 6 ?
O41 Fe3 O41 95.1(7) 5 6 ?
O41 Fe3 O41 59.6(7) 2 6 ?
O41 Fe3 O41 76.1(3) 3 6 ?
O41 Fe3 O41 95.1(7) 8 7 ?
O41 Fe3 O41 113.0(6) 5 7 ?
O41 Fe3 O41 170.0(6) 2 7 ?
O41 Fe3 O41 76.1(3) 3 7 ?
O41 Fe3 O41 121.4(7) 6 7 ?
O41 Fe3 O41 76.1(3) 8 4 ?
O41 Fe3 O41 76.1(3) 5 4 ?
O41 Fe3 O41 121.4(7) 2 4 ?
O41 Fe3 O41 113.0(6) 3 4 ?
O41 Fe3 O41 170.0(6) 6 4 ?
O41 Fe3 O41 59.6(7) 7 4 ?
O41 Fe3 O41 170.0(6) 8 . ?
O41 Fe3 O41 59.6(7) 5 . ?
O41 Fe3 O41 113.0(6) 2 . ?
O41 Fe3 O41 121.4(7) 3 . ?
O41 Fe3 O41 76.1(3) 6 . ?
O41 Fe3 O41 76.1(3) 7 . ?
O41 Fe3 O41 95.1(7) 4 . ?
O52 NI3 O41 173.7(6) 7 5 ?
O52 NI3 N41 100.1(7) 7 . ?
O41 NI3 N41 74.4(6) 5 . ?
O52 NI3 O51 86.4(6) 7 . ?
O41 NI3 O51 96.4(6) 5 . ?
N41 NI3 O51 89.0(7) . . ?
O52 NI3 O41 92.3(6) 7 4 ?
O41 NI3 O41 85.6(8) 5 4 ?
N41 NI3 O41 98.1(7) . 4 ?
O51 NI3 O41 172.9(6) . 4 ?
O52 NI3 O71 103.3(6) 7 . ?
O41 NI3 O71 82.1(6) 5 . ?
N41 NI3 O71 156.5(7) . . ?
O51 NI3 O71 94.1(7) . . ?
O41 NI3 O71 79.3(6) 4 . ?
C45 N41 C41 117(2) . . ?
C45 N41 NI3 122.2(17) . . ?
C41 N41 NI3 120.9(18) . . ?
C46 O41 NI3 119.8(8) . 5 ?
C46 O41 NI3 142.0(9) . 4 ?
NI3 O41 NI3 95.5(6) 5 4 ?
C46 O41 Fe3 93.0(15) . . ?
NI3 O41 Fe3 98.7(5) 5 . ?
NI3 O41 Fe3 94.9(5) 4 . ?
C51 O51 NI3 130.9(16) . . ?
C51 O52 NI3 131.9(16) . 6 ?
NI3 O71 NI3 84.9(4) . 6 ?
NI3 O71 NI3 145.2(13) . 3 ?
NI3 O71 NI3 84.9(4) 6 3 ?
NI3 O71 NI3 84.9(4) . 7 ?
NI3 O71 NI3 145.2(13) 6 7 ?
NI3 O71 NI3 84.9(4) 3 7 ?
NI3 O71 H71 107.4 . . ?
NI3 O71 H71 107.4 6 . ?
NI3 O71 H71 107.4 3 . ?
NI3 O71 H71 107.4 7 . ?
C42 C41 N41 115(3) . . ?
C42 C41 H41 122.7 . . ?
N41 C41 H41 122.7 . . ?
C43 C42 C41 129(4) . . ?
C43 C42 H42 115.6 . . ?
C41 C42 H42 115.6 . . ?
C42 C43 C44 113(3) . . ?
C42 C43 H43 123.4 . . ?
C44 C43 H43 123.4 . . ?
C45 C44 C43 117(2) . . ?
C45 C44 H44 121.5 . . ?
C43 C44 H44 121.5 . . ?
N41 C45 C44 129(3) . . ?
N41 C45 C46 110(2) . . ?
C44 C45 C46 120(2) . . ?
O41 C46 O41 114(3) 5 . ?
O41 C46 C45 109.5(11) 5 . ?
O41 C46 C45 107.4(10) . . ?
O41 C46 C45 107.4(10) 5 5 ?
O41 C46 C45 109.5(11) . 5 ?
C45 C46 C45 108(3) . 5 ?
O51 C51 O52 121(2) . . ?
O51 C51 C52 121(3) . . ?
O52 C51 C52 119(2) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?

_refine_diff_density_max         1.157
_refine_diff_density_min         -1.742
_refine_diff_density_rms         0.265

# SQUEEZE RESULTS (Version = 290617)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.008 0.006 -0.008 7961 1727 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 1 0 2.438
0 2 0 3.449
2 2 0 4.881
1 3 0 5.459
4 4 0 9.798
5 5 0 12.281
0 1 1 2.454
1 2 1 4.235
0 3 1 5.466
1 3 1 5.733
2 3 1 6.469
1 6 1 10.690
0 0 2 3.494
1 1 2 4.262
0 2 2 4.913
1 2 2 5.208
2 2 2 6.007
1 3 2 6.487
5 5 2 12.784
7 7 2 17.696
0 1 3 5.522
2 6 3 12.185
3 4 5 12.362
0 5 5 12.362
3 6 7 17.075
0 6 8 17.656
0 9 9 22.666
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
TITL shelxl    P 4/n n c    R = 0.25
CELL   25.6264   25.6264   25.3002     90.00     90.00     90.00
SPGR P4/nnc
# Solvent Accessible Volume =      7934
# Electrons Found in S.A.V. =      1695
# Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others
C101 0.160 0.250 0.750 !       3.47 eA-3
C102 0.724 0.728 0.309 !       2.49 eA-3
C103 0.750 0.754 0.023 !       1.98 eA-3
C104 0.871 0.665 0.151 !       1.67 eA-3
Q105 0.750 0.753 0.609 !       1.64 eA-3
C106 0.742 0.822 0.373 !       1.49 eA-3
C107 0.885 0.791 0.269 !       1.46 eA-3
C108 0.788 0.750 0.250 !       1.42 eA-3
C109 0.685 0.858 0.414 !       1.41 eA-3
C110 0.444 0.464 0.138 !       1.40 eA-3
C111 0.772 0.682 0.196 !       1.38 eA-3
C112 0.966 0.904 0.191 !       1.35 eA-3
C113 0.473 0.623 0.029 !       1.35 eA-3
C114 0.118 0.506 0.556 !       1.34 eA-3
Q115 0.843 0.955 0.197 !       1.30 eA-3
Q116 0.228 0.623 0.207 !       1.29 eA-3
C117 0.654 0.586 0.209 !       1.29 eA-3
C118 0.917 0.886 0.171 !       1.27 eA-3
C119 0.610 0.591 0.326 !       1.27 eA-3
C120 0.595 0.773 0.153 !       1.27 eA-3
C121 0.382 0.177 0.680 !       1.25 eA-3
C122 0.421 0.501 0.397 !       1.25 eA-3
Q123 0.636 0.799 0.638 !       1.25 eA-3
Q124 0.642 0.015 0.105 !       1.24 eA-3
C125 0.975 0.376 0.409 !       1.24 eA-3
Q126 0.033 0.017 0.302 !       1.24 eA-3
Q127 0.664 0.187 0.659 !       1.23 eA-3
C128 0.499 0.914 0.342 !       1.23 eA-3
Q129 0.979 0.085 0.215 !       1.21 eA-3
Q130 0.305 0.404 0.435 !       1.20 eA-3
C131 0.353 0.491 0.944 !       1.20 eA-3
Q132 0.663 0.996 0.066 !       1.19 eA-3
Q133 0.493 0.690 0.276 !       1.19 eA-3
C134 0.750 0.755 0.102 !       1.17 eA-3
C135 0.678 0.898 0.089 !       1.17 eA-3
Q136 0.166 0.433 0.194 !       1.16 eA-3
C137 0.089 0.453 0.636 !       1.16 eA-3
Q138 0.265 0.628 0.189 !       1.16 eA-3
C139 0.730 0.563 0.477 !       1.15 eA-3
C140 0.638 0.827 0.340 !       1.15 eA-3
C141 0.859 0.859 0.195 !       1.15 eA-3
C142 0.730 0.633 0.115 !       1.14 eA-3
Q143 0.867 0.994 0.118 !       1.13 eA-3
Q144 0.740 0.959 0.096 !       1.11 eA-3
Q145 0.289 0.859 0.247 !       1.10 eA-3
C146 0.862 0.748 0.201 !       1.10 eA-3
C147 0.619 0.514 0.132 !       1.09 eA-3
Q148 0.220 0.220 0.137 !       1.09 eA-3
Q149 0.248 0.650 0.703 !       1.08 eA-3
Q150 0.272 0.485 0.582 !       1.07 eA-3
C151 0.786 0.792 0.053 !       1.06 eA-3
C152 0.509 0.359 0.021 !       1.06 eA-3
Q153 0.338 0.196 0.157 !       1.06 eA-3
Q154 0.301 0.135 0.345 !       1.05 eA-3
C155 0.365 0.561 0.493 !       1.05 eA-3
C156 0.540 0.587 0.224 !       1.05 eA-3
Q157 0.612 0.464 0.916 !       1.04 eA-3
Q158 0.722 0.960 0.163 !       1.04 eA-3
Q159 0.412 0.390 0.424 !       1.03 eA-3
Q160 0.717 0.819 0.772 !       1.03 eA-3
Q161 0.054 0.141 0.000 !       1.02 eA-3
Q162 0.110 0.064 0.495 !       1.02 eA-3
Q163 0.478 0.490 0.200 !       1.02 eA-3
C164 0.940 0.058 0.365 !       1.02 eA-3
Q165 0.996 0.142 0.470 !       1.02 eA-3
C166 0.024 0.663 0.491 !       1.01 eA-3
C167 0.992 0.546 0.074 !       1.01 eA-3
Q168 0.316 0.525 0.191 !       1.01 eA-3
Q169 0.397 0.831 0.558 !       1.01 eA-3
Q170 0.499 0.578 0.285 !       0.99 eA-3
C171 0.922 0.504 0.470 !       0.99 eA-3
C172 0.588 0.955 0.135 !       0.99 eA-3
Q173 0.202 0.798 0.343 !       0.98 eA-3
Q174 0.902 0.052 0.111 !       0.98 eA-3
C175 0.770 0.963 0.250 !       0.98 eA-3
C176 0.179 0.250 0.008 !       0.98 eA-3
Q177 0.483 0.250 0.250 !       0.98 eA-3
C178 0.245 0.057 0.930 !       0.96 eA-3
Q179 0.359 0.220 0.276 !       0.96 eA-3
C180 0.259 0.388 0.546 !       0.95 eA-3
C181 0.063 0.220 0.041 !       0.95 eA-3
Q182 0.054 0.921 0.250 !       0.94 eA-3
C183 0.920 0.866 0.080 !       0.94 eA-3
C184 0.075 0.543 0.447 !       0.93 eA-3
C185 0.539 0.951 0.337 !       0.93 eA-3
Q186 0.369 0.357 0.479 !       0.93 eA-3
C187 0.543 0.654 0.189 !       0.93 eA-3
Q188 0.680 0.734 0.553 !       0.93 eA-3
C189 0.912 0.781 0.021 !       0.93 eA-3
Q190 0.343 0.537 0.010 !       0.92 eA-3
C191 0.799 0.647 0.322 !       0.92 eA-3
Q192 0.704 0.296 0.708 !       0.92 eA-3
Q193 0.666 0.674 0.526 !       0.91 eA-3
Q194 0.085 0.591 0.607 !       0.91 eA-3
Q195 0.201 0.881 0.054 !       0.91 eA-3
C196 0.907 0.575 0.393 !       0.91 eA-3
Q197 0.848 0.314 0.862 !       0.91 eA-3
Q198 0.528 0.010 0.320 !       0.91 eA-3
C199 0.670 0.600 0.109 !       0.90 eA-3
;

_shelxl_version_number           2014/6

# start Validation Reply Form
_vrf_CHEMW03_shelxl              
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: This alert is generated because squeeze program has been
used to exlude the solvent molecules during the refinement. The cif 
file contains the complete molecular formula; however some of the 
atoms reported are not listed in the fractional coordinates' list.
;
_vrf_RINTA01_shelxl              
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: The crystals showed poor diffraction ability and data were
collected only to establish the gross structure of the compound. Repeating
efforts to improve the quality of the crystals were not successful and the
present data represent the 'best' we could measure. The cif is deposited
only as proof of initial refinement according to those described in the
supporting information.
;
_vrf_THETM01_shelxl              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: A full data set was collected to 2theta=143 deg but only the
data to 2theta=100 deg were used in the refinement due to the very low 
diffraction ability of the crystals at higher theta angles. Even in this
case the ratio of data/parameters refined is well above the ideal value
of 10.
;
_vrf_PLAT020_shelxl              
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.356 Report
RESPONSE: See comment for _vrf_RINTA01_shelxl.
;
_vrf_PLAT082_shelxl              
;
PROBLEM: High R1 Value ..................................       0.21 Report
RESPONSE: See comment for _vrf_RINTA01_shelxl.
;
_vrf_PLAT084_shelxl              
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.48 Report
RESPONSE: See comment for _vrf_RINTA01_shelxl.
;
_vrf_PLAT201_shelxl              
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         24 Report
RESPONSE: Only the metal atoms and the heteroatoms were refined anisotropi-
cally; the rest were refined isotropically due to bad data set as explained
above.
;
_vrf_PLAT213_shelxl              
;
PROBLEM: Atom O61             has ADP max/min Ratio .....        4.7 oblate
RESPONSE: See comment for _vrf_RINTA01 for the quality of the data set which
causes such problems in the structure.
;
_vrf_PLAT341_shelxl              
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.04 Ang.  
RESPONSE: See comment for _vrf_RINTA01 for the quality of the data set which
causes such problems in the structure.
;
_vrf_PLAT420_shelxl              
;
PROBLEM: D-H Without Acceptor       O61    --  H61    ...     Please Check 
RESPONSE: These are tetradentate hydroxyl groups which are nested within 
the clusters, thus rendering the intermolecular hydrogen bonds impossible.  
The closest intramolecular OH...O distances are larger than 3.0 A.
;
_vrf_PLAT910_shelxl              
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         16 Note  
RESPONSE: This alert is probably due to instrument limitations. The number
of mising reflections is very small and in any case the ratio of reflections
to parameters refined is well above the ideal value of ten.
;
# end Validation Reply Form



