#------------------------------------------------------------------------------
#$Date: 2017-09-12 05:05:33 +0200 (Tue 12 de Sep de 2017) $
#$Revision: 200584 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/41/7044177.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7044177
loop_
_publ_author_name
'Georgopoulou, Anastasia N.'
'Al-Ameed, Karrar'
'Boudalis, Athanassios'
'Anagnostopoulos, Dimitrios F.'
'Psycharis, Vassilis'
'McGrady, John E.'
'Sanakis, Yiannis'
'Raptopoulou, Catherine P.'
_publ_section_title
;
 Site preferences in hetero-metallic [Fe9-xNix] clusters: a combined
 crystallographic, spectroscopic and theoretical analysis
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02930F
_journal_year                    2017
_chemical_formula_sum            'C77.33 H85.6 Fe9 N16.67 Ni0 O26.8'
_chemical_formula_weight         2180.00
_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_Hall           '-P 4a 2bc'
_space_group_name_H-M_alt        'P 4/n n c'
_symmetry_space_group_name_Hall  '-P 4a 2bc'
_symmetry_space_group_name_H-M   'P 4/n n c :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-09-08 deposited with the CCDC.
2017-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   25.6264(5)
_cell_length_b                   25.6264(5)
_cell_length_c                   25.3002(5)
_cell_measurement_reflns_used    22572
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      72.03
_cell_measurement_theta_min      6.51
_cell_volume                     16615.0(6)
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_molecular_graphics    'Diamond ver.3.1.'
_computing_publication_material  'publCIF J.Appl.Cryst. 2010, 43, 920'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.564
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.3563
_diffrn_reflns_av_unetI/netI     0.2693
_diffrn_reflns_Laue_measured_fraction_full 0.564
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38901
_diffrn_reflns_point_group_measured_fraction_full 0.564
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         49.980
_diffrn_reflns_theta_min         6.517
_exptl_absorpt_coefficient_mu    9.752
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.201
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             6688
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_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
;
_refine_diff_density_max         1.157
_refine_diff_density_min         -1.742
_refine_diff_density_rms         0.265
_refine_ls_extinction_coef       0.106(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.567
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.567
_refine_ls_R_factor_all          0.2477
_refine_ls_R_factor_gt           0.2074
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4505
_refine_ls_wR_factor_ref         0.4775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2342
_reflns_number_total             4254
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt02930f2.cif
_cod_data_source_block           shelxl_CCDC3
_cod_original_cell_volume        16615.0(7)
_cod_original_formula_sum        'C77.33 H85.60 Fe9 N16.67 Ni0 O26.80'
_cod_database_code               7044177
_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.
;
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014/6
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'
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
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
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'
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
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 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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_
_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 ' '
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
