#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/13/2201383.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2201383
loop_
_publ_author_name
'Muga, Iñaki'
'Vitoria, Pablo'
'Gutiérrez-Zorrilla, Juan M.'
'Luque, Antonio'
'Román, Pascual'
_publ_section_title
;
 Tris[bis(diethylenetriamine)nickel(II)] bis[hexacyanoferrate(III)]
 decahydrate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m524
_journal_page_last               m526
_journal_paper_doi               10.1107/S160053680201591X
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac
'[Ni (C4 H13 N3 )2 ]3 [Fe (C N )6 ]2 , 10H2 O'
_chemical_formula_moiety         'C36 H98 Fe2 N30 Ni3 O10'
_chemical_formula_sum            'C36 H98 Fe2 N30 Ni3 O10'
_chemical_formula_weight         1399.27
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 104.510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.195(3)
_cell_length_b                   12.6020(10)
_cell_length_c                   19.747(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.18
_cell_measurement_theta_min      11.55
_cell_volume                     6551.7(11)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997); PLATON (Spek, 1990)
;
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF99 (Beurskens et al., 1999)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'ω/2θ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9775
_diffrn_reflns_theta_full        29.98
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        4
_diffrn_standards_interval_count 90
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.348
_exptl_absorpt_correction_T_max  0.704
_exptl_absorpt_correction_T_min  0.520
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_meas      1.42
_exptl_crystal_density_method    flotation
_exptl_crystal_description       prism
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.569
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         9512
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.1005P)²+3.0322P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1534
_refine_ls_wR_factor_ref         0.1775
_reflns_number_gt                6070
_reflns_number_total             9512
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ci6144.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2201383
_cod_database_fobs_code          2201383
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_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Fe1 0.153739(18) 0.51677(4) 0.04818(3) 0.04908(13) Uani d . 1 . . Fe
N1 0.0963(2) 0.6928(4) -0.0469(3) 0.1150(17) Uani d . 1 . . N
N2 0.15369(15) 0.4022(3) -0.09032(17) 0.0752(9) Uani d . 1 . . N
N3 0.2168(2) 0.3370(3) 0.1330(2) 0.1030(15) Uani d . 1 . . N
N4 0.14491(16) 0.6553(4) 0.1738(2) 0.0858(11) Uani d . 1 . . N
N5 0.0586(2) 0.3949(5) 0.0605(3) 0.134(2) Uani d . 1 . . N
N6 0.25714(14) 0.6216(3) 0.0561(2) 0.0765(10) Uani d . 1 . . N
C1 0.11671(18) 0.6258(4) -0.0107(2) 0.0769(12) Uani d . 1 . . C
C2 0.15449(14) 0.4421(3) -0.03746(18) 0.0567(8) Uani d . 1 . . C
C3 0.19290(18) 0.4046(3) 0.10272(19) 0.0662(10) Uani d . 1 . . C
C4 0.14876(14) 0.6016(3) 0.1285(2) 0.0618(9) Uani d . 1 . . C
C5 0.09326(18) 0.4420(5) 0.0541(2) 0.0829(13) Uani d . 1 . . C
C6 0.21750(14) 0.5841(3) 0.05090(18) 0.0545(8) Uani d . 1 . . C
Ni1 0.171048(15) 0.00904(3) 0.10503(2) 0.04315(12) Uani d . 1 . . Ni
N11 0.21585(11) 0.1171(2) 0.05996(17) 0.0616(7) Uani d D 1 . . N
H11A 0.2212 0.1781 0.0844 0.074 Uiso calc R 1 . . H
H11B 0.2461 0.0880 0.0604 0.074 Uiso calc R 1 . . H
C12 0.18627(16) 0.1377(4) -0.0136(2) 0.0787(12) Uani d D 1 . . C
H12A 0.1937 0.2086 -0.0275 0.094 Uiso calc R 1 . . H
H12B 0.1964 0.0874 -0.0448 0.094 Uiso calc R 1 . . H
C13 0.13205(15) 0.1279(3) -0.0198(2) 0.0754(12) Uani d D 1 . . C
H13A 0.1209 0.1842 0.0064 0.090 Uiso calc R 1 . . H
H13B 0.1135 0.1341 -0.0684 0.090 Uiso calc R 1 . . H
N14 0.12200(12) 0.0257(2) 0.00738(16) 0.0594(7) Uani d D 1 . . N
H14 0.1299 -0.0251 -0.0209 0.071 Uiso calc R 1 . . H
C15 0.07044(16) 0.0050(4) 0.0136(3) 0.0788(13) Uani d . 1 . . C
H15A 0.0477 -0.0044 -0.0325 0.095 Uiso calc R 1 . . H
H15B 0.0584 0.0646 0.0360 0.095 Uiso calc R 1 . . H
C16 0.07114(16) -0.0958(4) 0.0574(3) 0.0790(12) Uani d . 1 . . C
H16A 0.0381 -0.1068 0.0665 0.095 Uiso calc R 1 . . H
H16B 0.0789 -0.1570 0.0321 0.095 Uiso calc R 1 . . H
N17 0.10952(12) -0.0840(3) 0.12320(17) 0.0640(8) Uani d . 1 . . N
H17A 0.1210 -0.1483 0.1400 0.077 Uiso calc R 1 . . H
H17B 0.0960 -0.0517 0.1549 0.077 Uiso calc R 1 . . H
N21 0.21168(12) -0.1267(2) 0.08456(15) 0.0587(7) Uani d . 1 . . N
H21A 0.1907 -0.1828 0.0747 0.070 Uiso calc R 1 . . H
H21B 0.2245 -0.1143 0.0475 0.070 Uiso calc R 1 . . H
C22 0.25324(17) -0.1493(3) 0.1470(2) 0.0725(11) Uani d . 1 . . C
H22A 0.2833 -0.1707 0.1325 0.087 Uiso calc R 1 . . H
H22B 0.2434 -0.2077 0.1728 0.087 Uiso calc R 1 . . H
C23 0.26536(16) -0.0539(4) 0.1937(2) 0.0802(12) Uani d . 1 . . C
H23A 0.2865 -0.0751 0.2389 0.096 Uiso calc R 1 . . H
H23B 0.2843 -0.0030 0.1734 0.096 Uiso calc R 1 . . H
N24 0.22033(12) -0.0059(2) 0.20262(15) 0.0561(7) Uani d . 1 . . N
H24 0.2059 -0.0534 0.2266 0.067 Uiso calc R 1 . . H
C25 0.22230(19) 0.0943(4) 0.2391(2) 0.0898(15) Uani d . 1 . . C
H25A 0.2441 0.1430 0.2222 0.108 Uiso calc R 1 . . H
H25B 0.2369 0.0831 0.2887 0.108 Uiso calc R 1 . . H
C26 0.17200(18) 0.1409(4) 0.2289(2) 0.0805(13) Uani d . 1 . . C
H26A 0.1752 0.2124 0.2476 0.097 Uiso calc R 1 . . H
H26B 0.1524 0.0997 0.2544 0.097 Uiso calc R 1 . . H
N27 0.14506(12) 0.1442(2) 0.15521(16) 0.0617(7) Uani d . 1 . . N
H27A 0.1519 0.2052 0.1356 0.074 Uiso calc R 1 . . H
H27B 0.1113 0.1402 0.1505 0.074 Uiso calc R 1 . . H
Ni2 0.0000 0.53368(5) 0.2500 0.04854(15) Uani d SD 1 . . Ni
N31 0.08041(12) 0.5092(3) 0.26368(19) 0.0648(8) Uani d D 1 B . N
H31A 0.0904 0.5382 0.2276 0.078 Uiso calc R 1 . . H
H31B 0.0978 0.5407 0.3034 0.078 Uiso calc R 1 . . H
C32 0.09063(18) 0.3968(4) 0.2669(3) 0.1039(18) Uani d D 1 . . C
H32A 0.1208 0.3842 0.3044 0.125 Uiso calc PR 0.50 A 3 H
H32B 0.0985 0.3758 0.2236 0.125 Uiso calc PR 0.50 A 3 H
H32C 0.1048 0.3774 0.3154 0.125 Uiso calc PR 0.50 A 4 H
H32D 0.1163 0.3823 0.2417 0.125 Uiso calc PR 0.50 A 4 H
C331 0.05044(15) 0.3281(5) 0.2780(5) 0.081(2) Uiso d PD 0.50 B 3 C
H33A 0.0530 0.2598 0.2565 0.097 Uiso calc PR 0.50 B 3 H
H33B 0.0555 0.3164 0.3279 0.097 Uiso calc PR 0.50 B 3 H
C332 0.04699(17) 0.3293(5) 0.2387(4) 0.074(2) Uiso d PD 0.50 B 4 C
H33C 0.0432 0.3208 0.1888 0.088 Uiso calc PR 0.50 B 4 H
H33D 0.0533 0.2597 0.2601 0.088 Uiso calc PR 0.50 B 4 H
N34 0.0000 0.3702(4) 0.2500 0.0958(19) Uani d SD 1 . . N
H34 -0.0045 0.3527 0.20410 0.115 Uiso calc PR 0.50 . . H
N41 -0.01047(14) 0.5598(3) 0.13861(16) 0.0705(9) Uani d . 1 . . N
H41A 0.0140 0.5263 0.1235 0.085 Uiso calc R 1 B . H
H41B -0.0408 0.5342 0.1149 0.085 Uiso calc R 1 . . H
C42 -0.0080(2) 0.6734(4) 0.1270(2) 0.0817(12) Uani d . 1 B . C
H42A 0.0264 0.6921 0.1264 0.098 Uiso calc PR 0.50 C 1 H
H42B -0.0299 0.6905 0.0814 0.098 Uiso calc PR 0.50 C 1 H
H42C 0.0113 0.6862 0.0927 0.098 Uiso d PR 0.50 C 2 H
H42D -0.0421 0.7001 0.1078 0.098 Uiso d PR 0.50 C 2 H
C431 -0.0232(4) 0.7367(7) 0.1796(5) 0.078(2) Uani d PD 0.50 B 1 C
H43A -0.0599 0.7350 0.1714 0.093 Uiso calc PR 0.50 B 1 H
H43B -0.0130 0.8098 0.1760 0.093 Uiso calc PR 0.50 B 1 H
C432 0.0160(4) 0.7327(7) 0.1905(5) 0.077(2) Uani d P 0.50 B 2 C
H43C 0.0526 0.7255 0.1996 0.093 Uiso calc PR 0.50 B 2 H
H43D 0.0077 0.8074 0.1830 0.093 Uiso calc PR 0.50 B 2 H
N44 0.0000 0.6968(3) 0.2500 0.0606(10) Uani d SD 1 . . N
H44 0.03281 0.7186 0.2571 0.073 Uiso calc PR 0.50 . . H
O5 0.3299(3) 0.3243(6) 0.2161(4) 0.125(3) Uani d P 0.629(9) . . O
O6 0.3788(4) 0.2552(9) 0.2049(4) 0.106(4) Uani d P 0.371(9) . . O
O1 0.13696(14) 0.1335(3) 0.39314(19) 0.1025(11) Uani d . 1 . . O
O2 0.00448(17) 0.2222(4) 0.0888(3) 0.1446(18) Uani d . 1 . . O
O3 0.4181(4) 0.4840(8) 0.1936(5) 0.261(5) Uani d . 1 . . O
O4 0.0305(2) 0.0509(5) 0.1717(3) 0.163(2) Uani d . 1 . . O
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'
Fe Fe 0.3463 0.8444 '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'
Ni Ni 0.3393 1.1124 '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'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
5 5 6
5 7 6
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
C1 Fe1 C6 . . 91.94(19)
C1 Fe1 C5 . . 93.5(2)
C6 Fe1 C5 . . 174.2(2)
C1 Fe1 C3 . . 176.39(18)
C6 Fe1 C3 . . 86.54(17)
C5 Fe1 C3 . . 88.2(2)
C1 Fe1 C2 . . 86.41(17)
C6 Fe1 C2 . . 91.84(15)
C5 Fe1 C2 . . 90.62(18)
C3 Fe1 C2 . . 90.37(16)
C1 Fe1 C4 . . 88.13(18)
C6 Fe1 C4 . . 88.92(15)
C5 Fe1 C4 . . 89.13(18)
C3 Fe1 C4 . . 95.11(17)
C2 Fe1 C4 . . 174.50(17)
N1 C1 Fe1 . . 177.0(5)
N2 C2 Fe1 . . 176.5(3)
N3 C3 Fe1 . . 177.5(4)
N4 C4 Fe1 . . 176.9(4)
N5 C5 Fe1 . . 176.6(6)
N6 C6 Fe1 . . 176.1(4)
N24 Ni1 N14 . . 179.36(13)
N24 Ni1 N21 . . 81.79(11)
N14 Ni1 N21 . . 98.59(11)
N24 Ni1 N17 . . 98.35(13)
N14 Ni1 N17 . . 82.15(13)
N21 Ni1 N17 . . 93.23(13)
N24 Ni1 N11 . . 98.10(13)
N14 Ni1 N11 . . 81.37(13)
N21 Ni1 N11 . . 93.16(13)
N17 Ni1 N11 . . 163.04(12)
N24 Ni1 N27 . . 81.67(12)
N14 Ni1 N27 . . 97.94(12)
N21 Ni1 N27 . . 163.46(12)
N17 Ni1 N27 . . 89.76(13)
N11 Ni1 N27 . . 88.57(13)
C12 N11 Ni1 . . 106.7(2)
C12 N11 H11A . . 110.4
Ni1 N11 H11A . . 110.4
C12 N11 H11B . . 110.4
Ni1 N11 H11B . . 110.4
H11A N11 H11B . . 108.6
C13 C12 N11 . . 110.7(3)
C13 C12 H12A . . 109.5
N11 C12 H12A . . 109.5
C13 C12 H12B . . 109.5
N11 C12 H12B . . 109.5
H12A C12 H12B . . 108.1
N14 C13 C12 . . 109.1(3)
N14 C13 H13A . . 109.9
C12 C13 H13A . . 109.9
N14 C13 H13B . . 109.9
C12 C13 H13B . . 109.9
H13A C13 H13B . . 108.3
C13 N14 C15 . . 117.7(3)
C13 N14 Ni1 . . 107.4(2)
C15 N14 Ni1 . . 108.2(3)
C13 N14 H14 . . 107.7
C15 N14 H14 . . 107.7
Ni1 N14 H14 . . 107.7
N14 C15 C16 . . 108.6(3)
N14 C15 H15A . . 110.0
C16 C15 H15A . . 110.0
N14 C15 H15B . . 110.0
C16 C15 H15B . . 110.0
H15A C15 H15B . . 108.4
N17 C16 C15 . . 108.9(3)
N17 C16 H16A . . 109.9
C15 C16 H16A . . 109.9
N17 C16 H16B . . 109.9
C15 C16 H16B . . 109.9
H16A C16 H16B . . 108.3
C16 N17 Ni1 . . 108.7(3)
C16 N17 H17A . . 109.9
Ni1 N17 H17A . . 109.9
C16 N17 H17B . . 109.9
Ni1 N17 H17B . . 109.9
H17A N17 H17B . . 108.3
C22 N21 Ni1 . . 108.8(2)
C22 N21 H21A . . 109.9
Ni1 N21 H21A . . 109.9
C22 N21 H21B . . 109.9
Ni1 N21 H21B . . 109.9
H21A N21 H21B . . 108.3
N21 C22 C23 . . 111.2(3)
N21 C22 H22A . . 109.4
C23 C22 H22A . . 109.4
N21 C22 H22B . . 109.4
C23 C22 H22B . . 109.4
H22A C22 H22B . . 108.0
N24 C23 C22 . . 110.8(4)
N24 C23 H23A . . 109.5
C22 C23 H23A . . 109.5
N24 C23 H23B . . 109.5
C22 C23 H23B . . 109.5
H23A C23 H23B . . 108.1
C23 N24 C25 . . 120.6(4)
C23 N24 Ni1 . . 107.6(2)
C25 N24 Ni1 . . 108.6(3)
C23 N24 H24 . . 106.4
C25 N24 H24 . . 106.4
Ni1 N24 H24 . . 106.4
N24 C25 C26 . . 111.5(4)
N24 C25 H25A . . 109.3
C26 C25 H25A . . 109.3
N24 C25 H25B . . 109.3
C26 C25 H25B . . 109.3
H25A C25 H25B . . 108.0
C25 C26 N27 . . 111.7(3)
C25 C26 H26A . . 109.3
N27 C26 H26A . . 109.3
C25 C26 H26B . . 109.3
N27 C26 H26B . . 109.3
H26A C26 H26B . . 107.9
C26 N27 Ni1 . . 107.0(2)
C26 N27 H27A . . 110.3
Ni1 N27 H27A . . 110.3
C26 N27 H27B . . 110.3
Ni1 N27 H27B . . 110.3
H27A N27 H27B . . 108.6
N44 Ni2 N34 . . 180.0000(10)
N44 Ni2 N31 . 2 98.22(9)
N34 Ni2 N31 . 2 81.78(9)
N44 Ni2 N31 . . 98.22(9)
N34 Ni2 N31 . . 81.78(9)
N31 Ni2 N31 2 . 163.57(18)
N44 Ni2 N41 . 2 81.27(10)
N34 Ni2 N41 . 2 98.73(10)
N31 Ni2 N41 2 2 91.15(14)
N31 Ni2 N41 . 2 91.34(14)
N44 Ni2 N41 . . 81.27(10)
N34 Ni2 N41 . . 98.73(10)
N31 Ni2 N41 2 . 91.34(14)
N31 Ni2 N41 . . 91.15(14)
N41 Ni2 N41 2 . 162.5(2)
C32 N31 Ni2 . . 108.9(2)
C32 N31 H31A . . 109.9
Ni2 N31 H31A . . 109.9
C32 N31 H31B . . 109.9
Ni2 N31 H31B . . 109.9
H31A N31 H31B . . 108.3
N31 C32 C332 . . 115.3(4)
N31 C32 C331 . . 116.6(4)
N31 C32 H32A . . 108.1
C331 C32 H32A . . 108.1
N31 C32 H32B . . 108.1
C331 C32 H32B . . 108.1
H32A C32 H32B . . 107.3
N31 C32 H32C . . 108.4
C332 C32 H32C . . 108.4
N31 C32 H32D . . 108.4
C332 C32 H32D . . 108.4
H32C C32 H32D . . 107.5
N34 C331 C32 . . 113.6(4)
N34 C331 H33A . . 108.8
C32 C331 H33A . . 108.8
N34 C331 H33B . . 108.8
C32 C331 H33B . . 108.8
H33A C331 H33B . . 107.7
N34 C332 C32 . . 113.6(4)
N34 C332 H33C . . 108.8
C32 C332 H33C . . 108.8
N34 C332 H33D . . 108.8
C32 C332 H33D . . 108.8
H33C C332 H33D . . 107.7
C331 N34 C332 . 2 126.9(5)
C331 N34 C332 2 . 126.9(5)
C331 N34 Ni2 . . 111.6(3)
C331 N34 Ni2 2 . 111.6(3)
C332 N34 Ni2 2 . 110.9(3)
C332 N34 Ni2 . . 110.9(3)
C331 N34 H34 . . 99.7
C331 N34 H34 2 . 69.7
C332 N34 H34 2 . 99.4
C332 N34 H34 . . 70.3
Ni2 N34 H34 . . 104.1
C42 N41 Ni2 . . 108.1(3)
C42 N41 H41A . . 110.1
Ni2 N41 H41A . . 110.1
C42 N41 H41B . . 110.1
Ni2 N41 H41B . . 110.1
H41A N41 H41B . . 108.4
C431 C42 N41 . . 113.3(5)
N41 C42 C432 . . 113.3(5)
C431 C42 H42A . . 108.9
N41 C42 H42A . . 108.9
C431 C42 H42B . . 108.9
N41 C42 H42B . . 108.9
H42A C42 H42B . . 107.7
N41 C42 H42C . . 109.2
C432 C42 H42C . . 108.0
N41 C42 H42D . . 109.1
C432 C42 H42D . . 109.5
H42C C42 H42D . . 107.6
C42 C431 N44 . . 111.1(6)
C42 C431 H43A . . 109.4
N44 C431 H43A . . 109.4
C42 C431 H43B . . 109.4
N44 C431 H43B . . 109.4
H42D C431 H43B . . 105.5
H43A C431 H43B . . 108.0
N44 C432 C42 . . 112.4(6)
N44 C432 H43C . . 109.1
C42 C432 H43C . . 109.1
N44 C432 H43D . . 109.1
C42 C432 H43D . . 109.1
H43C C432 H43D . . 107.9
H43D C432 H44 . . 107.4
C432 N44 C431 . 2 121.7(5)
C432 N44 C431 2 . 121.7(5)
C432 N44 Ni2 2 . 108.5(4)
C432 N44 Ni2 . . 108.5(4)
C431 N44 Ni2 2 . 110.1(4)
C431 N44 Ni2 . . 110.1(4)
C432 N44 H44 2 . 105.5
C431 N44 H44 . . 102.5
Ni2 N44 H44 . . 107.6
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 C1 . 1.915(4) yes
Fe1 C2 . 1.940(4) yes
Fe1 C3 . 1.928(4) yes
Fe1 C4 . 1.945(4) yes
Fe1 C5 . 1.924(4) yes
Fe1 C6 . 1.919(4) yes
N1 C1 . 1.154(6) ?
N2 C2 . 1.154(5) ?
N3 C3 . 1.145(5) ?
N4 C4 . 1.148(5) ?
N5 C5 . 1.148(6) ?
N6 C6 . 1.158(5) ?
Ni1 N11 . 2.162(3) yes
Ni1 N14 . 2.062(3) yes
Ni1 N17 . 2.146(3) yes
Ni1 N21 . 2.129(3) yes
Ni1 N24 . 2.062(3) yes
Ni1 N27 . 2.176(3) yes
N11 C12 . 1.497(5) ?
N11 H11A . 0.90 ?
N11 H11B . 0.90 ?
C12 C13 . 1.454(5) ?
C12 H12A . 0.97 ?
C12 H12B . 0.97 ?
C13 N14 . 1.447(4) ?
C13 H13A . 0.97 ?
C13 H13B . 0.97 ?
N14 C15 . 1.461(6) ?
N14 H14 . 0.91 ?
C15 C16 . 1.535(7) ?
C15 H15A . 0.97 ?
C15 H15B . 0.97 ?
C16 N17 . 1.456(5) ?
C16 H16A . 0.97 ?
C16 H16B . 0.97 ?
N17 H17A . 0.90 ?
N17 H17B . 0.90 ?
N21 C22 . 1.477(5) ?
N21 H21A . 0.90 ?
N21 H21B . 0.90 ?
C22 C23 . 1.500(6) ?
C22 H22A . 0.97 ?
C22 H22B . 0.97 ?
C23 N24 . 1.416(5) ?
C23 H23A . 0.97 ?
C23 H23B . 0.97 ?
N24 C25 . 1.448(5) ?
N24 H24 . 0.91 ?
C25 C26 . 1.456(6) ?
C25 H25A . 0.97 ?
C25 H25B . 0.97 ?
C26 N27 . 1.456(5) ?
C26 H26A . 0.97 ?
C26 H26B . 0.97 ?
N27 H27A . 0.90 ?
N27 H27B . 0.90 ?
Ni2 N31 . 2.157(3) yes
Ni2 N34 . 2.060(5) yes
Ni2 N41 . 2.171(3) yes
Ni2 N44 . 2.056(4) yes
Ni2 N31 2 2.157(3) ?
Ni2 N41 2 2.171(3) ?
N31 C32 . 1.443(5) ?
N31 H31A . 0.90 ?
N31 H31B . 0.90 ?
C32 C332 . 1.453(5) ?
C32 C331 . 1.453(5) ?
C32 H32A . 0.97 ?
C32 H32B . 0.97 ?
C32 H32C . 0.97 ?
C32 H32D . 0.97 ?
C331 N34 . 1.446(4) ?
C331 H33A . 0.97 ?
C331 H33B . 0.97 ?
C332 N34 . 1.446(4) ?
C332 H33C . 0.97 ?
C332 H33D . 0.97 ?
N34 C331 2 1.446(4) ?
N34 C332 2 1.446(4) ?
N34 H34 . 0.9112 ?
N41 C42 . 1.453(6) ?
N41 H41A . 0.90 ?
N41 H41B . 0.90 ?
C42 C431 . 1.450(11) ?
C42 C432 . 1.467(11) ?
C42 H42A . 0.97 ?
C42 H42B . 0.97 ?
C42 H42C . 0.97 ?
C42 H42D . 0.97 ?
C431 N44 . 1.464(8) ?
C431 H43A . 0.97 ?
C431 H43B . 0.97 ?
C432 N44 . 1.425(8) ?
C432 H43C . 0.97 ?
C432 H43D . 0.97 ?
N44 C432 2 1.425(8) ?
N44 C431 2 1.464(8) ?
N44 H44 . 0.91 ?
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
O1 N6 2.806(6) 4_545 yes
O1 N1 2.841(7) 6_566 yes
O1 O3 2.727(11) 4_545 yes
O2 N5 2.762(8) . yes
O2 O4 2.694(8) . yes
O2 N1 2.865(7) 5_565 yes
O3 O4 2.808(11) 4_555 yes
O3 O6 3.101(15) . yes
O3 O5 3.243(13) . yes
O3 O4 3.305(12) 3_555 yes
O5 N3 3.106(9) . yes
O5 N4 2.998(8) 4_545 yes
O6 N2 2.973(10) 7_555 yes
O6 N4 2.916(10) 4_545 yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N11 H11A N3 . 0.90 2.24 3.122(5) 167.5
N11 H11B N2 7 0.90 2.64 3.455(5) 150.9
N14 H14 O1 6 0.91 2.22 3.121(5) 168.2
N17 H17A N4 1_545 0.90 2.60 3.498(6) 172.1
N17 H17B O4 . 0.90 2.29 3.075(6) 145.5
N21 H21B N6 7 0.90 2.23 3.101(5) 164.2
N24 H24 O5 4_545 0.91 2.27 3.182(8) 178.3
N27 H27A N3 . 0.90 2.43 3.214(6) 145.1
N27 H27B O4 . 0.90 2.59 3.421(7) 152.9
N31 H31A N4 . 0.90 2.51 3.342(5) 154.3
N31 H31B N2 6_566 0.90 2.37 3.264(5) 169.8
N41 H41A N5 . 0.90 2.55 3.417(7) 161.2
N44 H44 O6 4 0.91 2.38 3.276(11) 169.1
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
N24 Ni1 N11 C12 . . 179.2(2)
N14 Ni1 N11 C12 . . -1.2(2)
N21 Ni1 N11 C12 . . 97.0(2)
N17 Ni1 N11 C12 . . -14.9(6)
N27 Ni1 N11 C12 . . -99.4(2)
Ni1 N11 C12 C13 . . 28.8(4)
N11 C12 C13 N14 . . -53.7(5)
C12 C13 N14 C15 . . 173.0(4)
C12 C13 N14 Ni1 . . 50.6(4)
N21 Ni1 N14 C13 . . -118.1(2)
N17 Ni1 N14 C13 . . 149.8(3)
N11 Ni1 N14 C13 . . -26.2(2)
N27 Ni1 N14 C13 . . 61.1(3)
N21 Ni1 N14 C15 . . 113.9(3)
N17 Ni1 N14 C15 . . 21.8(2)
N11 Ni1 N14 C15 . . -154.2(3)
N27 Ni1 N14 C15 . . -66.9(3)
C13 N14 C15 C16 . . -168.0(3)
Ni1 N14 C15 C16 . . -46.1(4)
N14 C15 C16 N17 . . 53.4(5)
C15 C16 N17 Ni1 . . -33.1(4)
N24 Ni1 N17 C16 . . -173.4(3)
N14 Ni1 N17 C16 . . 7.0(3)
N21 Ni1 N17 C16 . . -91.2(3)
N11 Ni1 N17 C16 . . 20.7(6)
N27 Ni1 N17 C16 . . 105.0(3)
N24 Ni1 N21 C22 . . -4.4(3)
N14 Ni1 N21 C22 . . 175.1(3)
N17 Ni1 N21 C22 . . -102.3(3)
N11 Ni1 N21 C22 . . 93.4(3)
N27 Ni1 N21 C22 . . -2.2(6)
Ni1 N21 C22 C23 . . -19.4(5)
N21 C22 C23 N24 . . 45.4(5)
C22 C23 N24 C25 . . -173.0(4)
C22 C23 N24 Ni1 . . -47.7(4)
N21 Ni1 N24 C23 . . 28.4(3)
N17 Ni1 N24 C23 . . 120.5(3)
N11 Ni1 N24 C23 . . -63.6(3)
N27 Ni1 N24 C23 . . -151.0(3)
N21 Ni1 N24 C25 . . 160.5(3)
N17 Ni1 N24 C25 . . -107.4(3)
N11 Ni1 N24 C25 . . 68.5(3)
N27 Ni1 N24 C25 . . -18.9(3)
C23 N24 C25 C26 . . 167.1(4)
Ni1 N24 C25 C26 . . 42.3(5)
N24 C25 C26 N27 . . -50.1(6)
C25 C26 N27 Ni1 . . 30.8(5)
N24 Ni1 N27 C26 . . -6.3(3)
N14 Ni1 N27 C26 . . 174.2(3)
N21 Ni1 N27 C26 . . -8.4(6)
N17 Ni1 N27 C26 . . 92.2(3)
N11 Ni1 N27 C26 . . -104.7(3)
N44 Ni2 N31 C32 . . 178.7(3)
N34 Ni2 N31 C32 . . -1.3(3)
N41 Ni2 N31 C32 2 . 97.4(3)
N41 Ni2 N31 C32 . . -99.9(3)
Ni2 N31 C32 C332 . . 19.1(6)
Ni2 N31 C32 C331 . . -14.7(6)
N31 C32 C331 N34 . . 29.7(9)
N31 C32 C332 N34 . . -34.5(8)
C32 C331 N34 C331 . 2 150.7(8)
C32 C331 N34 Ni2 . . -29.3(8)
C32 C332 N34 C332 . 2 -148.3(7)
C32 C332 N34 Ni2 . . 31.7(7)
N31 Ni2 N34 C331 2 . -163.5(4)
N31 Ni2 N34 C331 . . 16.5(4)
N41 Ni2 N34 C331 2 . -73.6(4)
N41 Ni2 N34 C331 . . 106.4(4)
N31 Ni2 N34 C331 2 2 16.5(4)
N31 Ni2 N34 C331 . 2 -163.5(4)
N41 Ni2 N34 C331 2 2 106.4(4)
N41 Ni2 N34 C331 . 2 -73.6(4)
N31 Ni2 N34 C332 2 2 -16.2(4)
N31 Ni2 N34 C332 . 2 163.8(4)
N41 Ni2 N34 C332 2 2 73.7(4)
N41 Ni2 N34 C332 . 2 -106.3(4)
N31 Ni2 N34 C332 2 . 163.8(4)
N31 Ni2 N34 C332 . . -16.2(4)
N41 Ni2 N34 C332 2 . -106.3(4)
N41 Ni2 N34 C332 . . 73.7(4)
N44 Ni2 N41 C42 . . 3.9(3)
N34 Ni2 N41 C42 . . -176.1(3)
N31 Ni2 N41 C42 2 . 102.0(3)
N31 Ni2 N41 C42 . . -94.2(3)
Ni2 N41 C42 C431 . . -27.1(6)
Ni2 N41 C42 C432 . . 18.3(6)
N41 C42 C431 N44 . . 45.1(9)
N41 C42 C432 N44 . . -42.2(9)
C42 C432 N44 C432 . 2 -136.0(8)
C42 C432 N44 Ni2 . . 44.0(8)
C42 C431 N44 C431 . 2 140.2(8)
C42 C431 N44 Ni2 . . -39.8(8)
N31 Ni2 N44 C432 2 2 64.4(5)
N31 Ni2 N44 C432 . 2 -115.6(5)
N41 Ni2 N44 C432 2 2 -25.5(5)
N41 Ni2 N44 C432 . 2 154.5(5)
N31 Ni2 N44 C432 2 . -115.6(5)
N31 Ni2 N44 C432 . . 64.4(5)
N41 Ni2 N44 C432 2 . 154.5(5)
N41 Ni2 N44 C432 . . -25.5(5)
N31 Ni2 N44 C431 2 2 108.9(5)
N31 Ni2 N44 C431 . 2 -71.1(5)
N41 Ni2 N44 C431 2 2 19.0(5)
N41 Ni2 N44 C431 . 2 -161.0(5)
N31 Ni2 N44 C431 2 . -71.1(5)
N31 Ni2 N44 C431 . . 108.9(5)
N41 Ni2 N44 C431 2 . -161.0(5)
N41 Ni2 N44 C431 . . 19.0(5)
