#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:46:54 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180235 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/21/7112108.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_7112108
loop_
_publ_author_name
'Szymon Chorazy'
'Robert Podgajny'
'Wojciech Nogas'
'Wojciech Nitek'
'Marcin Koziel'
'Michal Rams'
'Ewa Juszynska-Galazka'
'Jan Zukrowski'
'Czeslaw Kapusta'
'Koji Nakabayashi'
'Takashi Fujimoto'
'Shin-ichi Ohkoshi'
'Barbara Sieklucka'
_publ_section_title
;
 Charge transfer phase transition with reversed thermal hysteresis loop in
 the mixed-valence Fe9[W(CN)8]6.xMeOH cluster
;
_journal_name_full               Chem.Commun.
_journal_page_first              3484
_journal_paper_doi               10.1039/C3CC48029A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C72 H72 Fe9 N48 O24 W6'
_chemical_formula_sum            'C90 H168 Fe9 N48 O42 W6'
_chemical_formula_weight         4200.24
_chemical_name_common            'Compound X'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2013-11-28T21:18:09-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 113.6570(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.3480(4)
_cell_length_b                   19.0770(3)
_cell_length_c                   32.3450(5)
_cell_measurement_reflns_used    89741
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     16022.0(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0219031
_diffrn_orient_matrix_UB_12      0.0411763
_diffrn_orient_matrix_UB_13      0.0001638
_diffrn_orient_matrix_UB_21      -0.0315444
_diffrn_orient_matrix_UB_22      0.0297715
_diffrn_orient_matrix_UB_23      -0.013589
_diffrn_orient_matrix_UB_31      0.002892
_diffrn_orient_matrix_UB_32      0.0128762
_diffrn_orient_matrix_UB_33      0.030896
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1217
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            57634
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.502
_diffrn_reflns_theta_min         1.325
_exptl_absorpt_coefficient_mu    5.153
_exptl_absorpt_correction_T_max  0.4573
_exptl_absorpt_correction_T_min  0.3070
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8004
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.284
_refine_diff_density_min         -3.839
_refine_diff_density_rms         0.395
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    307.679
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         18205
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0980P)²+162.8645P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.1747
_reflns_number_gt                14691
_reflns_number_total             18205
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3cc48029a.txt
_cod_data_source_block           1_LT
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7112108
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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_calc_flag
W1 W -0.07580(2) 0.34649(2) 0.11744(2) 0.01994(10) Uani 1 d
W2 W 0.17953(2) 0.17597(2) 0.23377(2) 0.01607(9) Uani 1 d
W3 W -0.06141(2) -0.04147(2) 0.12402(2) 0.01599(9) Uani 1 d
Fe1 Fe 0 0.15774(7) 0.25 0.0117(3) Uani 1 d
Fe2 Fe 0.10717(4) 0.43232(6) 0.23788(4) 0.0190(2) Uani 1 d
Fe5 Fe -0.21518(5) 0.14313(6) 0.09258(4) 0.0225(3) Uani 1 d
Fe3 Fe 0.12962(4) -0.09580(6) 0.24628(4) 0.0178(2) Uani 1 d
Fe4 Fe 0.03097(5) 0.15801(6) 0.06889(4) 0.0216(3) Uani 1 d
C16 C -0.1344(6) 0.4252(7) 0.0945(3) 0.063(4) Uani 1 d
N16 N -0.1684(6) 0.4651(7) 0.0814(4) 0.096(5) Uani 1 d
N28 N 0.2822(3) 0.2714(5) 0.2941(3) 0.043(2) Uani 1 d
C18 C -0.0424(4) 0.4240(5) 0.0874(3) 0.044(3) Uani 1 d
N18 N -0.0250(5) 0.4639(6) 0.0713(4) 0.079(4) Uani 1 d
C17 C -0.1158(3) 0.3326(4) 0.0450(2) 0.0233(17) Uani 1 d
N17 N -0.1384(3) 0.3241(5) 0.0068(3) 0.039(2) Uani 1 d
C11 C -0.0460(3) 0.2679(4) 0.1692(3) 0.0202(16) Uani 1 d
N11 N -0.0281(3) 0.2297(3) 0.1992(2) 0.0197(13) Uani 1 d
C13 C -0.0028(3) 0.3846(4) 0.1657(3) 0.0236(17) Uani 1 d
N13 N 0.0349(3) 0.4038(4) 0.1926(2) 0.0230(14) Uani 1 d
C15 C -0.1379(3) 0.2744(5) 0.1068(3) 0.0276(19) Uani 1 d
N15 N -0.1697(3) 0.2327(4) 0.1004(2) 0.0288(16) Uani 1 d
C12 C -0.0905(3) 0.3840(4) 0.1743(3) 0.0216(16) Uani 1 d
N12 N -0.0955(3) 0.4027(4) 0.2057(2) 0.0282(16) Uani 1 d
C14 C -0.0303(3) 0.2752(4) 0.0972(2) 0.0184(15) Uani 1 d
N14 N -0.0077(3) 0.2360(4) 0.0860(2) 0.0269(16) Uani 1 d
C28 C 0.2468(3) 0.2371(4) 0.2730(3) 0.0259(18) Uani 1 d
C26 C 0.2408(4) 0.1109(5) 0.2325(3) 0.033(2) Uani 1 d
N26 N 0.2733(4) 0.0751(5) 0.2314(4) 0.054(3) Uani 1 d
C27 C 0.2063(3) 0.2312(5) 0.1873(3) 0.0300(19) Uani 1 d
N27 N 0.2192(4) 0.2600(5) 0.1638(3) 0.051(2) Uani 1 d
C21 C 0.1080(3) 0.1706(4) 0.2416(2) 0.0165(15) Uani 1 d
N21 N 0.0704(3) 0.1655(3) 0.2459(2) 0.0196(14) Uani 1 d
C22 C 0.1509(3) 0.2796(4) 0.2333(3) 0.0190(15) Uani 1 d
N22 N 0.1370(3) 0.3360(3) 0.2335(3) 0.0247(15) Uani 1 d
C25 C 0.2000(3) 0.1564(4) 0.3041(3) 0.0207(17) Uani 1 d
N25 N 0.2077(3) 0.1474(4) 0.3414(2) 0.0268(16) Uani 1 d
C23 C 0.1590(3) 0.0667(4) 0.2354(3) 0.0209(16) Uani 1 d
N23 N 0.1482(3) 0.0099(3) 0.2385(2) 0.0224(14) Uani 1 d
C24 C 0.1223(3) 0.1607(4) 0.1664(3) 0.0183(16) Uani 1 d
N24 N 0.0907(3) 0.1565(4) 0.1313(2) 0.0238(15) Uani 1 d
C36 C -0.0706(4) -0.1538(5) 0.1254(3) 0.033(2) Uani 1 d
N36 N -0.0746(5) -0.2141(5) 0.1267(3) 0.061(3) Uani 1 d
C38 C -0.0234(3) -0.0899(5) 0.0835(3) 0.0257(18) Uani 1 d
N38 N -0.0050(3) -0.1136(4) 0.0621(3) 0.0351(19) Uani 1 d
C37 C -0.1236(4) -0.0644(5) 0.0599(3) 0.036(2) Uani 1 d
N37 N -0.1574(4) -0.0751(5) 0.0263(3) 0.055(3) Uani 1 d
C31 C -0.0337(3) 0.0373(4) 0.1760(2) 0.0184(15) Uani 1 d
N31 N -0.0214(3) 0.0801(3) 0.2024(2) 0.0199(14) Uani 1 d
C33 C -0.0960(3) -0.0660(4) 0.1703(3) 0.0211(16) Uani 1 d
N33 N -0.1126(3) -0.0774(4) 0.1973(2) 0.0250(15) Uani 1 d
C35 C -0.1208(4) 0.0368(4) 0.1101(3) 0.0250(18) Uani 1 d
N35 N -0.1527(3) 0.0780(4) 0.1044(2) 0.0305(17) Uani 1 d
C32 C 0.0126(3) -0.0724(4) 0.1731(2) 0.0188(15) Uani 1 d
N32 N 0.0532(3) -0.0869(4) 0.1998(2) 0.0254(15) Uani 1 d
C34 C -0.0293(3) 0.0391(4) 0.0971(2) 0.0204(16) Uani 1 d
N34 N -0.0094(3) 0.0813(4) 0.0842(2) 0.0245(15) Uani 1 d
O63 O 0.1771(3) 0.4683(4) 0.2799(2) 0.0355(15) Uani 1 d
C64 C 0.2142(5) 0.4306(9) 0.3213(5) 0.084(5) Uani 1 d
H64A H 0.2453 0.4591 0.3358 0.126 Uiso 1 calc
H64B H 0.2236 0.3853 0.3123 0.126 Uiso 1 calc
H64C H 0.1979 0.4228 0.3424 0.126 Uiso 1 calc
O61 O 0.1230(3) 0.4674(3) 0.1847(2) 0.0316(14) Uani 1 d
C62 C 0.1115(5) 0.4284(8) 0.1439(4) 0.063(4) Uani 1 d
H62A H 0.1224 0.4552 0.1235 0.094 Uiso 1 calc
H62B H 0.0744 0.4196 0.1294 0.094 Uiso 1 calc
H62C H 0.13 0.3836 0.1511 0.094 Uiso 1 calc
O65 O 0.0828(3) 0.5313(3) 0.2411(2) 0.0414(17) Uani 1 d
C66 C 0.0351(8) 0.5642(9) 0.2068(7) 0.110(7) Uani 1 d
H66A H 0.0319 0.6123 0.2159 0.164 Uiso 1 calc
H66B H 0.0048 0.537 0.2047 0.164 Uiso 1 calc
H66C H 0.0372 0.5647 0.1773 0.164 Uiso 1 calc
O55 O -0.2595(3) 0.0526(4) 0.0835(3) 0.0435(17) Uani 1 d
C56 C -0.2423(7) -0.0075(7) 0.1140(6) 0.094(6) Uani 1 d
H56A H -0.2686 -0.0443 0.1039 0.141 Uiso 1 calc
H56B H -0.2369 0.0072 0.1447 0.141 Uiso 1 calc
H56C H -0.21 -0.0256 0.114 0.141 Uiso 1 calc
O53 O -0.2826(3) 0.2007(4) 0.07327(19) 0.0339(15) Uani 1 d
C54 C -0.2941(8) 0.2640(14) 0.0997(6) 0.143(10) Uani 1 d
H54A H -0.3292 0.2814 0.0826 0.214 Uiso 1 calc
H54B H -0.2694 0.3019 0.1034 0.214 Uiso 1 calc
H54C H -0.291 0.2479 0.1295 0.214 Uiso 1 calc
O51 O -0.2328(3) 0.1353(4) 0.0234(2) 0.0432(17) Uani 1 d
C52 C -0.2298(11) 0.1808(13) -0.0049(7) 0.142(9) Uani 1 d
O71 O 0.2094(2) -0.1131(3) 0.2882(2) 0.0310(14) Uani 1 d
C72 C 0.2505(4) -0.0811(5) 0.2817(4) 0.043(3) Uani 1 d
H72A H 0.2832 -0.0972 0.305 0.065 Uiso 1 calc
H72B H 0.2479 -0.0301 0.2837 0.065 Uiso 1 calc
H72C H 0.2491 -0.0936 0.2518 0.065 Uiso 1 calc
O75 O 0.1193(3) -0.2049(3) 0.2500(2) 0.0443(18) Uani 1 d
C76 C 0.1412(8) -0.2539(9) 0.2834(7) 0.123(8) Uani 1 d
H76A H 0.1263 -0.3001 0.2724 0.184 Uiso 1 calc
H76B H 0.1343 -0.2412 0.3099 0.184 Uiso 1 calc
H76C H 0.1784 -0.2553 0.2919 0.184 Uiso 1 calc
O73 O 0.1501(3) -0.1224(3) 0.1916(2) 0.0354(15) Uani 1 d
C74 C 0.1364(4) -0.0846(6) 0.1503(3) 0.044(3) Uani 1 d
H74A H 0.1509 -0.1083 0.1311 0.066 Uiso 1 calc
H74B H 0.1501 -0.0369 0.1568 0.066 Uiso 1 calc
H74C H 0.0988 -0.0829 0.1346 0.066 Uiso 1 calc
O45 O 0.0712(3) 0.0898(3) 0.0466(2) 0.0347(15) Uani 1 d
C46 C 0.0695(7) 0.0176(7) 0.0419(5) 0.076(5) Uani 1 d
H46A H 0.095 0.0027 0.0304 0.113 Uiso 1 calc
H46B H 0.035 0.0034 0.0206 0.113 Uiso 1 calc
H46C H 0.0771 -0.0043 0.0713 0.113 Uiso 1 calc
O41 O -0.0223(3) 0.1574(3) 0.0034(2) 0.0339(15) Uani 1 d
C42 C -0.0751(5) 0.1721(8) -0.0133(4) 0.073(5) Uani 1 d
H42A H -0.0902 0.1676 -0.0463 0.11 Uiso 1 calc
H42B H -0.0802 0.22 -0.005 0.11 Uiso 1 calc
H42C H -0.0919 0.1389 -0.0004 0.11 Uiso 1 calc
O43 O 0.0685(3) 0.2316(3) 0.0478(2) 0.0392(17) Uani 1 d
C44 C 0.0955(7) 0.2899(7) 0.0715(5) 0.082(5) Uani 1 d
H44A H 0.1094 0.3159 0.0528 0.123 Uiso 1 calc
H44B H 0.1238 0.2746 0.0993 0.123 Uiso 1 calc
H44C H 0.0721 0.3202 0.0791 0.123 Uiso 1 calc
O3 O 0.1629(4) 0.1268(8) 0.0558(4) 0.109(5) Uani 1 d
C3 C 0.2050(6) 0.1035(12) 0.0931(5) 0.109(7) Uani 1 d
H3B H 0.2364 0.1253 0.0934 0.164 Uiso 1 calc
H3C H 0.2077 0.0525 0.0916 0.164 Uiso 1 calc
H3A H 0.2006 0.1164 0.1207 0.164 Uiso 1 calc
O9 O 0.0423(6) 0.5674(7) 0.0644(5) 0.119(5) Uiso 1 d
C9 C 0.0234(8) 0.6166(10) 0.0287(6) 0.109(6) Uiso 1 d
H9A H -0.01 0.6345 0.0262 0.163 Uiso 1 calc
H9B H 0.0194 0.5938 0.0003 0.163 Uiso 1 calc
H9C H 0.0478 0.6556 0.0348 0.163 Uiso 1 calc
O1 O 0.1152(5) 0.5904(6) 0.1502(4) 0.091(3) Uiso 1 d
C1 C 0.1612(9) 0.6076(15) 0.1448(9) 0.165(11) Uiso 1 d
H1C H 0.1596 0.6564 0.1349 0.247 Uiso 1 calc
H1B H 0.165 0.5767 0.1221 0.247 Uiso 1 calc
H1A H 0.1908 0.6016 0.1736 0.247 Uiso 1 calc
O1S O -0.0598(6) -0.3531(7) 0.1438(5) 0.118(5) Uiso 1 d
C1S C -0.0626(12) -0.3881(15) 0.1041(8) 0.163(10) Uiso 1 d
O4 O 0.0853(6) -0.2872(8) 0.1778(5) 0.139(5) Uiso 1 d
C4 C 0.0572(7) -0.2574(10) 0.1341(6) 0.106(6) Uiso 1 d
H4B H 0.047 -0.2093 0.1375 0.159 Uiso 1 calc
H4A H 0.0263 -0.2856 0.1179 0.159 Uiso 1 calc
H4C H 0.079 -0.2569 0.117 0.159 Uiso 1 calc
O2 O -0.1120(6) -0.4081(7) 0.1849(4) 0.107(4) Uiso 1 d
C2 C -0.1630(8) -0.4038(15) 0.1556(8) 0.170(11) Uiso 1 d
H2B H -0.1798 -0.4491 0.1544 0.255 Uiso 1 calc
H2C H -0.1654 -0.3913 0.1255 0.255 Uiso 1 calc
H2A H -0.1801 -0.3677 0.1663 0.255 Uiso 1 calc
O10 O 0 -0.2240(15) 0.25 0.184(11) Uiso 1 d
C10 C 0.0216(10) -0.2522(13) 0.2228(8) 0.057(6) Uiso 0.5 d
H10C H 0.0533 -0.2771 0.2413 0.086 Uiso 0.5 calc
H10B H 0.0297 -0.2146 0.206 0.086 Uiso 0.5 calc
H10A H -0.0027 -0.285 0.2015 0.086 Uiso 0.5 calc
O5 O 0.2367(6) 0.3113(9) 0.0878(5) 0.053(4) Uiso 0.5 d
C5 C 0.2911(7) 0.3123(12) 0.1006(7) 0.043(5) Uiso 0.5 d
H5B H 0.3067 0.3476 0.1242 0.065 Uiso 0.5 calc
H5C H 0.2985 0.3238 0.0743 0.065 Uiso 0.5 calc
H5A H 0.3054 0.2661 0.1122 0.065 Uiso 0.5 calc
O2S O 0.1786(7) 0.2855(9) 0.0002(6) 0.061(5) Uiso 0.5 d
C2S C 0.2011(13) 0.3273(15) -0.0230(11) 0.081(9) Uiso 0.5 d
H2SB H 0.2008 0.3765 -0.0143 0.122 Uiso 0.5 calc
H2SC H 0.1814 0.3224 -0.0556 0.122 Uiso 0.5 calc
H2SA H 0.2367 0.3122 -0.0151 0.122 Uiso 0.5 calc
O6 O -0.2429(8) 0.5052(11) 0.0005(7) 0.077(6) Uiso 0.5 d
C6 C -0.2704(9) 0.4718(13) 0.0214(8) 0.055(6) Uiso 0.5 d
H6C H -0.2517 0.4753 0.0542 0.082 Uiso 0.5 calc
H6B H -0.2748 0.4223 0.0125 0.082 Uiso 0.5 calc
H6A H -0.3042 0.4939 0.0124 0.082 Uiso 0.5 calc
O7 O -0.3713(9) -0.0305(11) 0.0178(7) 0.081(6) Uiso 0.5 d
C7 C -0.3572(16) 0.0256(16) 0.0461(11) 0.105(12) Uiso 0.5 d
H7A H -0.3298 0.0117 0.0749 0.158 Uiso 0.5 calc
H7B H -0.387 0.0423 0.0514 0.158 Uiso 0.5 calc
H7C H -0.3447 0.0631 0.0324 0.158 Uiso 0.5 calc
O8 O 0.0830(5) 0.2430(7) -0.0255(4) 0.032(3) Uiso 0.5 d
C8 C 0.041(2) 0.286(4) -0.030(3) 0.28(4) Uiso 0.5 d
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.849 6.8722 '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
C16 W1 C15 85.5(5) . .
C16 W1 C14 144.7(3) . .
C15 W1 C14 95.7(3) . .
C16 W1 C11 140.1(4) . .
C15 W1 C11 73.7(3) . .
C14 W1 C11 72.5(3) . .
C16 W1 C13 113.6(5) . .
C15 W1 C13 144.8(3) . .
C14 W1 C13 85.1(3) . .
C11 W1 C13 73.0(3) . .
C16 W1 C12 71.0(4) . .
C15 W1 C12 85.6(3) . .
C14 W1 C12 144.3(3) . .
C11 W1 C12 73.7(3) . .
C13 W1 C12 74.3(3) . .
C16 W1 C17 73.5(4) . .
C15 W1 C17 73.2(3) . .
C14 W1 C17 73.2(3) . .
C11 W1 C17 128.8(3) . .
C13 W1 C17 139.1(3) . .
C12 W1 C17 139.7(3) . .
C16 W1 C18 77.6(5) . .
C15 W1 C18 146.7(3) . .
C14 W1 C18 82.7(4) . .
C11 W1 C18 135.5(4) . .
C13 W1 C18 68.4(3) . .
C12 W1 C18 114.8(4) . .
C17 W1 C18 74.6(3) . .
C22 W2 C25 96.3(3) . .
C22 W2 C21 70.8(3) . .
C25 W2 C21 74.5(3) . .
C22 W2 C26 147.4(3) . .
C25 W2 C26 92.5(3) . .
C21 W2 C26 141.7(3) . .
C22 W2 C24 89.4(3) . .
C25 W2 C24 145.5(3) . .
C21 W2 C24 75.4(3) . .
C26 W2 C24 100.9(3) . .
C22 W2 C28 75.4(3) . .
C25 W2 C28 70.8(3) . .
C21 W2 C28 127.6(3) . .
C26 W2 C28 78.1(3) . .
C24 W2 C28 142.9(3) . .
C22 W2 C23 141.7(3) . .
C25 W2 C23 76.6(3) . .
C21 W2 C23 71.1(3) . .
C26 W2 C23 70.9(3) . .
C24 W2 C23 78.1(3) . .
C28 W2 C23 133.3(3) . .
C22 W2 C27 77.7(3) . .
C25 W2 C27 141.9(3) . .
C21 W2 C27 134.7(3) . .
C26 W2 C27 76.1(3) . .
C24 W2 C27 72.6(3) . .
C28 W2 C27 71.2(3) . .
C23 W2 C27 130.1(3) . .
C34 W3 C32 92.8(3) . .
C34 W3 C33 145.9(3) . .
C32 W3 C33 90.5(3) . .
C34 W3 C31 74.7(3) . .
C32 W3 C31 70.9(3) . .
C33 W3 C31 74.5(3) . .
C34 W3 C35 80.9(3) . .
C32 W3 C35 142.6(3) . .
C33 W3 C35 76.1(3) . .
C31 W3 C35 71.9(3) . .
C34 W3 C37 94.1(4) . .
C32 W3 C37 146.6(3) . .
C33 W3 C37 101.5(4) . .
C31 W3 C37 142.4(3) . .
C35 W3 C37 70.8(3) . .
C34 W3 C36 142.6(3) . .
C32 W3 C36 78.6(3) . .
C33 W3 C36 71.2(3) . .
C31 W3 C36 133.2(3) . .
C35 W3 C36 126.9(4) . .
C37 W3 C36 76.1(4) . .
C34 W3 C38 70.8(3) . .
C32 W3 C38 76.0(3) . .
C33 W3 C38 142.4(3) . .
C31 W3 C38 130.1(3) . .
C35 W3 C38 133.8(3) . .
C37 W3 C38 75.5(3) . .
C36 W3 C38 71.8(3) . .
N11 Fe1 N11 95.5(4) . 2
N11 Fe1 N31 174.2(3) . 2
N11 Fe1 N31 88.8(3) 2 2
N11 Fe1 N31 88.8(3) . .
N11 Fe1 N31 174.2(3) 2 .
N31 Fe1 N31 87.1(4) 2 .
N11 Fe1 N21 88.5(3) . .
N11 Fe1 N21 85.9(3) 2 .
N31 Fe1 N21 95.6(3) 2 .
N31 Fe1 N21 90.4(3) . .
N11 Fe1 N21 85.9(3) . 2
N11 Fe1 N21 88.5(3) 2 2
N31 Fe1 N21 90.4(3) 2 2
N31 Fe1 N21 95.6(3) . 2
N21 Fe1 N21 171.7(4) . 2
O63 Fe2 O65 85.0(3) . .
O63 Fe2 N22 91.8(3) . .
O65 Fe2 N22 175.0(3) . .
O63 Fe2 O61 88.2(3) . .
O65 Fe2 O61 86.1(3) . .
N22 Fe2 O61 90.1(3) . .
O63 Fe2 N13 175.2(3) . .
O65 Fe2 N13 91.1(3) . .
N22 Fe2 N13 92.0(3) . .
O61 Fe2 N13 88.8(3) . .
O63 Fe2 N12 87.7(3) . 2
O65 Fe2 N12 91.8(3) . 2
N22 Fe2 N12 91.8(3) . 2
O61 Fe2 N12 175.5(3) . 2
N13 Fe2 N12 95.2(3) . 2
N25 Fe5 N35 96.2(3) 2 .
N25 Fe5 O53 89.4(3) 2 .
N35 Fe5 O53 172.6(3) . .
N25 Fe5 O55 89.1(3) 2 .
N35 Fe5 O55 87.2(3) . .
O53 Fe5 O55 88.1(3) . .
N25 Fe5 O51 172.5(3) 2 .
N35 Fe5 O51 88.6(3) . .
O53 Fe5 O51 85.4(3) . .
O55 Fe5 O51 85.3(3) . .
N25 Fe5 N15 92.3(3) 2 .
N35 Fe5 N15 91.6(3) . .
O53 Fe5 N15 93.0(3) . .
O55 Fe5 N15 178.3(3) . .
O51 Fe5 N15 93.4(3) . .
N32 Fe3 N33 94.5(3) . 2
N32 Fe3 O75 89.7(3) . .
N33 Fe3 O75 91.7(3) 2 .
N32 Fe3 N23 94.2(3) . .
N33 Fe3 N23 95.7(3) 2 .
O75 Fe3 N23 171.4(3) . .
N32 Fe3 O73 88.4(3) . .
N33 Fe3 O73 175.2(3) 2 .
O75 Fe3 O73 84.4(3) . .
N23 Fe3 O73 88.0(3) . .
N32 Fe3 O71 173.1(3) . .
N33 Fe3 O71 91.6(3) 2 .
O75 Fe3 O71 87.0(3) . .
N23 Fe3 O71 88.4(3) . .
O73 Fe3 O71 85.3(3) . .
N34 Fe4 O43 174.9(3) . .
N34 Fe4 O45 94.3(3) . .
O43 Fe4 O45 83.1(3) . .
N34 Fe4 O41 89.7(3) . .
O43 Fe4 O41 85.7(3) . .
O45 Fe4 O41 85.2(3) . .
N34 Fe4 N24 94.2(3) . .
O43 Fe4 N24 90.1(3) . .
O45 Fe4 N24 88.9(3) . .
O41 Fe4 N24 173.1(3) . .
N34 Fe4 N14 92.5(3) . .
O43 Fe4 N14 89.9(3) . .
O45 Fe4 N14 172.6(3) . .
O41 Fe4 N14 91.8(3) . .
N24 Fe4 N14 93.6(3) . .
N16 C16 W1 176.1(15) . .
N18 C18 W1 179.0(12) . .
N17 C17 W1 177.5(9) . .
N11 C11 W1 174.9(7) . .
C11 N11 Fe1 176.5(7) . .
N13 C13 W1 177.0(7) . .
C13 N13 Fe2 173.8(7) . .
N15 C15 W1 176.1(8) . .
C15 N15 Fe5 168.6(7) . .
N12 C12 W1 176.2(8) . .
C12 N12 Fe2 177.2(7) . 2
N14 C14 W1 177.7(7) . .
C14 N14 Fe4 174.5(7) . .
N28 C28 W2 178.3(9) . .
N26 C26 W2 179.0(11) . .
N27 C27 W2 178.7(9) . .
N21 C21 W2 177.8(7) . .
C21 N21 Fe1 176.8(6) . .
N22 C22 W2 178.1(7) . .
C22 N22 Fe2 173.4(7) . .
N25 C25 W2 175.4(8) . .
C25 N25 Fe5 172.0(8) . 2
N23 C23 W2 176.3(7) . .
C23 N23 Fe3 178.3(7) . .
N24 C24 W2 175.6(7) . .
C24 N24 Fe4 174.5(7) . .
N36 C36 W3 178.8(12) . .
N38 C38 W3 178.3(8) . .
N37 C37 W3 177.9(10) . .
N31 C31 W3 176.7(7) . .
C31 N31 Fe1 179.4(7) . .
N33 C33 W3 176.2(7) . .
C33 N33 Fe3 170.3(7) . 2
N35 C35 W3 177.0(7) . .
C35 N35 Fe5 174.0(8) . .
N32 C32 W3 177.8(7) . .
C32 N32 Fe3 170.3(7) . .
N34 C34 W3 176.2(8) . .
C34 N34 Fe4 173.5(7) . .
C64 O63 Fe2 125.5(7) . .
O63 C64 H64A 109.5 . .
O63 C64 H64B 109.5 . .
H64A C64 H64B 109.5 . .
O63 C64 H64C 109.5 . .
H64A C64 H64C 109.5 . .
H64B C64 H64C 109.5 . .
C62 O61 Fe2 123.7(7) . .
O61 C62 H62A 109.5 . .
O61 C62 H62B 109.5 . .
H62A C62 H62B 109.5 . .
O61 C62 H62C 109.5 . .
H62A C62 H62C 109.5 . .
H62B C62 H62C 109.5 . .
C66 O65 Fe2 125.3(8) . .
O65 C66 H66A 109.5 . .
O65 C66 H66B 109.5 . .
H66A C66 H66B 109.5 . .
O65 C66 H66C 109.5 . .
H66A C66 H66C 109.5 . .
H66B C66 H66C 109.5 . .
C56 O55 Fe5 122.4(8) . .
O55 C56 H56A 109.5 . .
O55 C56 H56B 109.5 . .
H56A C56 H56B 109.5 . .
O55 C56 H56C 109.5 . .
H56A C56 H56C 109.5 . .
H56B C56 H56C 109.5 . .
C54 O53 Fe5 127.3(7) . .
O53 C54 H54A 109.5 . .
O53 C54 H54B 109.5 . .
H54A C54 H54B 109.5 . .
O53 C54 H54C 109.5 . .
H54A C54 H54C 109.5 . .
H54B C54 H54C 109.5 . .
C52 O51 Fe5 131.0(12) . .
C72 O71 Fe3 124.4(6) . .
O71 C72 H72A 109.5 . .
O71 C72 H72B 109.5 . .
H72A C72 H72B 109.5 . .
O71 C72 H72C 109.5 . .
H72A C72 H72C 109.5 . .
H72B C72 H72C 109.5 . .
C76 O75 Fe3 133.3(10) . .
O75 C76 H76A 109.5 . .
O75 C76 H76B 109.5 . .
H76A C76 H76B 109.5 . .
O75 C76 H76C 109.5 . .
H76A C76 H76C 109.5 . .
H76B C76 H76C 109.5 . .
C74 O73 Fe3 126.4(6) . .
O73 C74 H74A 109.5 . .
O73 C74 H74B 109.5 . .
H74A C74 H74B 109.5 . .
O73 C74 H74C 109.5 . .
H74A C74 H74C 109.5 . .
H74B C74 H74C 109.5 . .
C46 O45 Fe4 132.4(7) . .
O45 C46 H46A 109.5 . .
O45 C46 H46B 109.5 . .
H46A C46 H46B 109.5 . .
O45 C46 H46C 109.5 . .
H46A C46 H46C 109.5 . .
H46B C46 H46C 109.5 . .
C42 O41 Fe4 128.9(6) . .
O41 C42 H42A 109.5 . .
O41 C42 H42B 109.5 . .
H42A C42 H42B 109.5 . .
O41 C42 H42C 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
C44 O43 Fe4 127.7(7) . .
O43 C44 H44A 109.5 . .
O43 C44 H44B 109.5 . .
H44A C44 H44B 109.5 . .
O43 C44 H44C 109.5 . .
H44A C44 H44C 109.5 . .
H44B C44 H44C 109.5 . .
O3 C3 H3B 109.5 . .
O3 C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
O3 C3 H3A 109.5 . .
H3B C3 H3A 109.5 . .
H3C C3 H3A 109.5 . .
O9 C9 H9A 109.5 . .
O9 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
O9 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
O1 C1 H1C 109.5 . .
O1 C1 H1B 109.5 . .
H1C C1 H1B 109.5 . .
O1 C1 H1A 109.5 . .
H1C C1 H1A 109.5 . .
H1B C1 H1A 109.5 . .
O4 C4 H4B 109.5 . .
O4 C4 H4A 109.5 . .
H4B C4 H4A 109.5 . .
O4 C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
O2 C2 H2B 109.5 . .
O2 C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
O2 C2 H2A 109.5 . .
H2B C2 H2A 109.5 . .
H2C C2 H2A 109.5 . .
C10 O10 C10 134(3) 2 .
O10 C10 H10C 109.5 . .
O10 C10 H10B 109.5 . .
H10C C10 H10B 109.5 . .
O10 C10 H10A 109.5 . .
H10C C10 H10A 109.5 . .
H10B C10 H10A 109.5 . .
O5 C5 H5B 109.5 . .
O5 C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
O5 C5 H5A 109.5 . .
H5B C5 H5A 109.5 . .
H5C C5 H5A 109.5 . .
O2S C2S H2SB 109.5 . .
O2S C2S H2SC 109.5 . .
H2SB C2S H2SC 109.5 . .
O2S C2S H2SA 109.5 . .
H2SB C2S H2SA 109.5 . .
H2SC C2S H2SA 109.5 . .
O6 C6 H6C 109.5 . .
O6 C6 H6B 109.5 . .
H6C C6 H6B 109.5 . .
O6 C6 H6A 109.5 . .
H6C C6 H6A 109.5 . .
H6B C6 H6A 109.5 . .
O7 C7 H7A 109.5 . .
O7 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
O7 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 C16 2.140(12) .
W1 C15 2.149(10) .
W1 C14 2.149(8) .
W1 C11 2.152(7) .
W1 C13 2.158(9) .
W1 C12 2.162(8) .
W1 C17 2.172(7) .
W1 C18 2.183(10) .
W2 C22 2.135(8) .
W2 C25 2.142(8) .
W2 C21 2.144(8) .
W2 C26 2.149(9) .
W2 C24 2.152(8) .
W2 C28 2.161(9) .
W2 C23 2.170(8) .
W2 C27 2.207(9) .
W3 C34 2.141(8) .
W3 C32 2.144(8) .
W3 C33 2.147(8) .
W3 C31 2.156(7) .
W3 C35 2.158(9) .
W3 C37 2.160(9) .
W3 C36 2.161(9) .
W3 C38 2.206(8) .
Fe1 N11 2.042(6) .
Fe1 N11 2.042(6) 2
Fe1 N31 2.045(6) 2
Fe1 N31 2.045(6) .
Fe1 N21 2.058(7) .
Fe1 N21 2.058(7) 2
Fe2 O63 2.020(6) .
Fe2 O65 2.027(7) .
Fe2 N22 2.051(7) .
Fe2 O61 2.055(6) .
Fe2 N13 2.057(7) .
Fe2 N12 2.058(7) 2
Fe5 N25 2.062(7) 2
Fe5 N35 2.069(8) .
Fe5 O53 2.072(7) .
Fe5 O55 2.087(7) .
Fe5 O51 2.092(7) .
Fe5 N15 2.094(8) .
Fe3 N32 2.091(7) .
Fe3 N33 2.095(7) 2
Fe3 O75 2.112(7) .
Fe3 N23 2.125(7) .
Fe3 O73 2.133(6) .
Fe3 O71 2.146(6) .
Fe4 N34 2.037(7) .
Fe4 O43 2.038(6) .
Fe4 O45 2.042(6) .
Fe4 O41 2.049(6) .
Fe4 N24 2.050(7) .
Fe4 N14 2.052(8) .
C16 N16 1.165(15) .
N28 C28 1.161(11) .
C18 N18 1.142(14) .
C17 N17 1.151(11) .
C11 N11 1.155(10) .
C13 N13 1.133(11) .
C15 N15 1.158(11) .
C12 N12 1.141(10) .
N12 Fe2 2.059(7) 2
C14 N14 1.134(10) .
C26 N26 1.159(13) .
C27 N27 1.110(12) .
C21 N21 1.133(11) .
C22 N22 1.146(10) .
C25 N25 1.149(10) .
N25 Fe5 2.063(7) 2
C23 N23 1.141(10) .
C24 N24 1.131(11) .
C36 N36 1.158(12) .
C38 N38 1.117(11) .
C37 N37 1.143(12) .
C31 N31 1.130(10) .
C33 N33 1.165(10) .
N33 Fe3 2.095(7) 2
C35 N35 1.157(11) .
C32 N32 1.160(10) .
C34 N34 1.154(11) .
O63 C64 1.511(17) .
C64 H64A 0.98 .
C64 H64B 0.98 .
C64 H64C 0.98 .
O61 C62 1.435(13) .
C62 H62A 0.98 .
C62 H62B 0.98 .
C62 H62C 0.98 .
O65 C66 1.501(19) .
C66 H66A 0.98 .
C66 H66B 0.98 .
C66 H66C 0.98 .
O55 C56 1.462(15) .
C56 H56A 0.98 .
C56 H56B 0.98 .
C56 H56C 0.98 .
O53 C54 1.59(3) .
C54 H54A 0.98 .
C54 H54B 0.98 .
C54 H54C 0.98 .
O51 C52 1.29(2) .
O71 C72 1.405(12) .
C72 H72A 0.98 .
C72 H72B 0.98 .
C72 H72C 0.98 .
O75 C76 1.373(17) .
C76 H76A 0.98 .
C76 H76B 0.98 .
C76 H76C 0.98 .
O73 C74 1.428(11) .
C74 H74A 0.98 .
C74 H74B 0.98 .
C74 H74C 0.98 .
O45 C46 1.383(14) .
C46 H46A 0.98 .
C46 H46B 0.98 .
C46 H46C 0.98 .
O41 C42 1.402(14) .
C42 H42A 0.98 .
C42 H42B 0.98 .
C42 H42C 0.98 .
O43 C44 1.392(14) .
C44 H44A 0.98 .
C44 H44B 0.98 .
C44 H44C 0.98 .
O3 C3 1.385(14) .
C3 H3B 0.98 .
C3 H3C 0.98 .
C3 H3A 0.98 .
O9 C9 1.417(15) .
C9 H9A 0.98 .
C9 H9B 0.98 .
C9 H9C 0.98 .
O1 C1 1.423(16) .
C1 H1C 0.98 .
C1 H1B 0.98 .
C1 H1A 0.98 .
O1S C1S 1.420(17) .
O4 C4 1.433(15) .
C4 H4B 0.98 .
C4 H4A 0.98 .
C4 H4C 0.98 .
O2 C2 1.375(16) .
C2 H2B 0.98 .
C2 H2C 0.98 .
C2 H2A 0.98 .
O10 C10 1.368(16) 2
O10 C10 1.368(16) .
C10 H10C 0.98 .
C10 H10B 0.98 .
C10 H10A 0.98 .
O5 C5 1.426(16) .
C5 H5B 0.98 .
C5 H5C 0.98 .
C5 H5A 0.98 .
O2S C2S 1.409(18) .
C2S H2SB 0.98 .
C2S H2SC 0.98 .
C2S H2SA 0.98 .
O6 C6 1.377(17) .
C6 H6C 0.98 .
C6 H6B 0.98 .
C6 H6A 0.98 .
O7 C7 1.358(18) .
C7 H7A 0.98 .
C7 H7B 0.98 .
C7 H7C 0.98 .
O8 C8 1.40(2) .
