##############################################################################
###                                                                        ###
###        Electronic paper (Acta Crystallographica Section E)             ###
###                                                                        ###
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#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section E. It conforms to the requirements of Notes      #
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# of the IUCr Commission on Journals.                                        #
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#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
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#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
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data_global
_audit_creation_method     SHELXL-97
_journal_date_recd_electronic     2009-11-02
_journal_date_accepted     2009-12-18
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2010
_journal_volume     66
_journal_issue      1
_journal_page_first     m103
_journal_page_last     m104
_journal_paper_category     QM
_journal_coeditor_code     PB2013
_publ_contact_author_name     'Butcher, Ray J.'
_publ_contact_author_address
;
Department of Chemistry
Howard University
525 College Street NW
Washington DC 20059, USA
;
_publ_contact_author_email     rbutcher99@yahoo.com
_publ_contact_author_fax     ?
_publ_contact_author_phone     '703 585-6631'
_publ_section_title
;
Tris(ethane-1,2-diamine-κ²N,N')nickel(II) diiodide
;
loop_
    _publ_author_name
    _publ_author_address
    'Brewer, Greg'
;
Department of Chemistry
Catholic University
620 Michigan Av. NE
Washington
DC 20059, USA
;
    'Butcher, Ray J.'
;
Department of Chemistry
Howard University
525 College Street NW
Washington
DC 20059, USA
;
    'Jasinski, Jerry P.'
;
Department of Chemistry
Keene State College
229 Main Street
Keene, NH 03435-2001, USA
;
data_I
_chemical_name_systematic
;
Tris(ethane-1,2-diamine-κ²N,N')nickel(II) diiodide
;
_chemical_name_common     ?
_chemical_formula_moiety     'C6 H24 N6 Ni 2+, 2(I -)'
_chemical_formula_sum     'C6 H24 I2 N6 Ni'
_chemical_formula_iupac     '[Ni (C2 H8 N2)3] I2'
_chemical_formula_weight     492.82
_chemical_melting_point     ?
_symmetry_cell_setting     orthorhombic
_symmetry_space_group_name_H-M     'P b c a'
_symmetry_space_group_name_Hall     '-P 2ac 2ab'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x+1/2, -y, z+1/2'
    '-x, y+1/2, -z+1/2'
    'x+1/2, -y+1/2, -z'
    '-x, -y, -z'
    'x-1/2, y, -z-1/2'
    'x, -y-1/2, z-1/2'
    '-x-1/2, y-1/2, z'
_cell_length_a     14.7502(6)
_cell_length_b     13.4881(4)
_cell_length_c     15.9624(7)
_cell_angle_alpha     90.00
_cell_angle_beta     90.00
_cell_angle_gamma     90.00
_cell_volume     3175.8(2)
_cell_formula_units_Z     8
_cell_measurement_reflns_used     8584
_cell_measurement_theta_min     4.5798
_cell_measurement_theta_max     32.4384
_cell_measurement_temperature     200(2)
_exptl_crystal_description     prism
_exptl_crystal_colour     'pale purple'
_exptl_crystal_size_max     0.55
_exptl_crystal_size_mid     0.47
_exptl_crystal_size_min     0.38
_exptl_crystal_density_diffrn     2.061
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     1888
_exptl_absorpt_coefficient_mu     5.097
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_exptl_absorpt_correction_T_min     0.33678
_exptl_absorpt_correction_T_max     1.00000
_exptl_special_details
;
;
_diffrn_ambient_temperature     200(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Oxford Diffraction Gemini R Mo'
_diffrn_measurement_method     'ω scans'
_diffrn_detector_area_resol_mean     10.5081
_diffrn_reflns_number     19070
_diffrn_reflns_av_R_equivalents     0.0421
_diffrn_reflns_av_sigmaI/netI     0.0632
_diffrn_reflns_theta_min     4.59
_diffrn_reflns_theta_max     32.52
_diffrn_reflns_theta_full     25.00
_diffrn_measured_fraction_theta_max     0.914
_diffrn_measured_fraction_theta_full     0.990
_diffrn_reflns_limit_h_min     -21
_diffrn_reflns_limit_h_max     19
_diffrn_reflns_limit_k_min     -10
_diffrn_reflns_limit_k_max     19
_diffrn_reflns_limit_l_min     -24
_diffrn_reflns_limit_l_max     16
_diffrn_standards_number     ?
_diffrn_standards_interval_count     ?
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     ?
_refine_special_details
;
Refinement of F² against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F², conventional
R-factors R are based on F, with F set to zero for
negative F². The threshold expression of F² >
σ(F²) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F² are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger.
;
_reflns_number_total     5271
_reflns_number_gt     2835
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0793
_refine_ls_R_factor_gt     0.0340
_refine_ls_wR_factor_gt     0.0761
_refine_ls_wR_factor_ref     0.0909
_refine_ls_goodness_of_fit_ref     0.963
_refine_ls_restrained_S_all     0.961
_refine_ls_number_reflns     5271
_refine_ls_number_parameters     161
_refine_ls_number_restraints     36
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
                 'calc w=1/[σ²(Fo²)+(0.0430P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.001
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     1.648
_refine_diff_density_min     -1.088
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'C' 'C' 0.0033 0.0016
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'H' 'H' 0.0000 0.0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'N' 'N' 0.0061 0.0033
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Ni' 'Ni' 0.3393 1.1124
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'I' 'I' -0.4742 1.8119
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2009)
;
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_computing_structure_solution     'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics     'SHELXTL (Sheldrick, 2008)'
_computing_publication_material     'SHELXTL (Sheldrick, 2008)'
loop_
    _atom_site_type_symbol
    _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
    I I1 0.611433(17) 0.132498(19) 0.122134(16) 0.03800(7) Uani d . 1 . .
    I I2 0.362274(19) 0.435966(17) 0.131522(15) 0.03860(7) Uani d . 1 . .
    Ni Ni 0.42318(3) 0.25520(3) 0.37608(3) 0.02275(10) Uani d . 1 . .
    N N31 0.4175(2) 0.20616(19) 0.25125(19) 0.0332(7) Uani d . 1 A .
    H H31A 0.3959 0.2561 0.2174 0.040 Uiso calc R 1 . .
    H H31B 0.4746 0.1891 0.2331 0.040 Uiso calc R 1 . .
    N N32 0.3624(2) 0.11503(19) 0.39826(18) 0.0293(7) Uani d . 1 A .
    H H32A 0.3902 0.0842 0.4428 0.035 Uiso calc R 1 . .
    H H32B 0.3019 0.1228 0.4106 0.035 Uiso calc R 1 . .
    C C31 0.3571(3) 0.1199(3) 0.2463(2) 0.0391(9) Uani d . 1 . .
    H H31C 0.3696 0.0821 0.1944 0.047 Uiso calc R 1 A .
    H H31D 0.2931 0.1419 0.2450 0.047 Uiso calc R 1 . .
    C C32 0.3731(3) 0.0550(2) 0.3218(2) 0.0358(9) Uani d . 1 A .
    H H32C 0.3291 -0.0005 0.3222 0.043 Uiso calc R 1 . .
    H H32D 0.4350 0.0267 0.3196 0.043 Uiso calc R 1 . .
    N N11A 0.5571(3) 0.2044(3) 0.4045(3) 0.0245(10) Uani d PD 0.707(4) A 1
    H H11A 0.5682 0.2102 0.4611 0.029 Uiso calc PR 0.707(4) A 1
    H H11B 0.5634 0.1389 0.3896 0.029 Uiso calc PR 0.707(4) A 1
    C C11A 0.6215(5) 0.2661(5) 0.3569(5) 0.0366(12) Uani d PDU 0.707(4) A 1
    H H11C 0.6215 0.2466 0.2972 0.044 Uiso calc PR 0.707(4) A 1
    H H11D 0.6836 0.2579 0.3793 0.044 Uiso calc PR 0.707(4) A 1
    C C12A 0.5913(4) 0.3713(4) 0.3662(4) 0.0398(13) Uani d PD 0.707(4) A 1
    H H12A 0.5980 0.3921 0.4254 0.048 Uiso calc PR 0.707(4) A 1
    H H12B 0.6302 0.4147 0.3314 0.048 Uiso calc PR 0.707(4) A 1
    N N12A 0.4962(4) 0.3832(5) 0.3404(6) 0.0336(8) Uani d PD 0.707(4) A 1
    H H12C 0.4930 0.3916 0.2832 0.040 Uiso calc PR 0.707(4) A 1
    H H12D 0.4716 0.4383 0.3656 0.040 Uiso calc PR 0.707(4) A 1
    N N11B 0.5522(9) 0.1873(8) 0.3751(7) 0.0245(10) Uani d PD 0.293(4) A 2
    H H11E 0.5596 0.1490 0.4223 0.029 Uiso calc PR 0.293(4) A 2
    H H11F 0.5580 0.1471 0.3289 0.029 Uiso calc PR 0.293(4) A 2
    C C11B 0.6210(11) 0.2659(11) 0.3730(12) 0.0366(12) Uani d PDU 0.293(4) A 2
    H H11G 0.6800 0.2376 0.3555 0.044 Uiso calc PR 0.293(4) A 2
    H H11H 0.6283 0.2945 0.4297 0.044 Uiso calc PR 0.293(4) A 2
    C C12B 0.5934(8) 0.3463(9) 0.3126(9) 0.0398(13) Uani d PD 0.293(4) A 2
    H H12E 0.6378 0.4013 0.3144 0.048 Uiso calc PR 0.293(4) A 2
    H H12F 0.5919 0.3197 0.2548 0.048 Uiso calc PR 0.293(4) A 2
    N N12B 0.5030(10) 0.3828(13) 0.3364(15) 0.0336(8) Uani d PD 0.293(4) A 2
    H H12G 0.4757 0.4135 0.2915 0.040 Uiso calc PR 0.293(4) A 2
    H H12H 0.5077 0.4279 0.3794 0.040 Uiso calc PR 0.293(4) A 2
    N N21A 0.4089(4) 0.2980(6) 0.5029(5) 0.0373(9) Uani d PD 0.707(4) A 1
    H H21A 0.3906 0.2446 0.5347 0.045 Uiso calc PR 0.707(4) A 1
    H H21B 0.4635 0.3202 0.5235 0.045 Uiso calc PR 0.707(4) A 1
    C C21A 0.3404(4) 0.3778(4) 0.5075(4) 0.0418(13) Uani d PD 0.707(4) A 1
    H H21C 0.3179 0.3841 0.5657 0.050 Uiso calc PR 0.707(4) A 1
    H H21D 0.3683 0.4417 0.4912 0.050 Uiso calc PR 0.707(4) A 1
    C C22A 0.2648(4) 0.3553(4) 0.4514(3) 0.0352(13) Uani d PDU 0.707(4) A 1
    H H22A 0.2226 0.4123 0.4493 0.042 Uiso calc PR 0.707(4) A 1
    H H22B 0.2311 0.2969 0.4725 0.042 Uiso calc PR 0.707(4) A 1
    N N22A 0.3007(5) 0.3345(5) 0.3666(3) 0.0279(10) Uani d PD 0.707(4) A 1
    H H22C 0.3105 0.3931 0.3385 0.033 Uiso calc PR 0.707(4) A 1
    H H22D 0.2591 0.2979 0.3367 0.033 Uiso calc PR 0.707(4) A 1
    N N21B 0.3959(10) 0.3014(15) 0.5003(12) 0.0373(9) Uani d PD 0.293(4) A 2
    H H21E 0.4126 0.2528 0.5376 0.045 Uiso calc PR 0.293(4) A 2
    H H21F 0.4281 0.3581 0.5125 0.045 Uiso calc PR 0.293(4) A 2
    C C21B 0.2973(9) 0.3207(9) 0.5064(8) 0.0418(13) Uani d PD 0.293(4) A 2
    H H21G 0.2635 0.2573 0.5066 0.050 Uiso calc PR 0.293(4) A 2
    H H21H 0.2835 0.3566 0.5590 0.050 Uiso calc PR 0.293(4) A 2
    C C22B 0.2706(12) 0.3802(11) 0.4348(8) 0.0352(13) Uani d PDU 0.293(4) A 2
    H H22E 0.3050 0.4431 0.4343 0.042 Uiso calc PR 0.293(4) A 2
    H H22F 0.2052 0.3961 0.4382 0.042 Uiso calc PR 0.293(4) A 2
    N N22B 0.2895(13) 0.3231(14) 0.3576(9) 0.0279(10) Uani d PD 0.293(4) A 2
    H H22G 0.2901 0.3644 0.3117 0.033 Uiso calc PR 0.293(4) A 2
    H H22H 0.2461 0.2752 0.3495 0.033 Uiso calc PR 0.293(4) A 2
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    I1 0.02763(13) 0.04501(14) 0.04135(15) -0.00301(10) 0.00464(11) -0.00509(12)
    I2 0.05250(17) 0.02837(11) 0.03493(14) -0.00384(10) -0.00855(12)
                                                                    -0.00025(11)
    Ni 0.0228(2) 0.01934(17) 0.0261(2) 0.00048(15) -0.00030(19) 0.00281(17)
    N31 0.0388(18) 0.0298(14) 0.0311(16) 0.0024(13) 0.0089(14) -0.0018(14)
    N32 0.0307(16) 0.0246(13) 0.0327(16) -0.0070(12) -0.0054(13) 0.0054(13)
    C31 0.047(2) 0.045(2) 0.0248(18) -0.0084(18) 0.0037(18) -0.0089(18)
    C32 0.051(2) 0.0238(16) 0.033(2) -0.0079(16) 0.0012(18) -0.0016(16)
    N11A 0.0270(18) 0.0242(19) 0.022(3) -0.0039(15) -0.007(2) -0.0052(18)
    C11A 0.035(2) 0.0383(17) 0.036(3) 0.0028(14) 0.0021(18) -0.0046(18)
    C12A 0.031(3) 0.051(3) 0.037(3) -0.020(2) 0.010(3) 0.001(3)
    N12A 0.0333(19) 0.0277(15) 0.0398(19) -0.0044(13) 0.0086(16) 0.0071(15)
    N11B 0.0270(18) 0.0242(19) 0.022(3) -0.0039(15) -0.007(2) -0.0052(18)
    C11B 0.035(2) 0.0383(17) 0.036(3) 0.0028(14) 0.0021(18) -0.0046(18)
    C12B 0.031(3) 0.051(3) 0.037(3) -0.020(2) 0.010(3) 0.001(3)
    N12B 0.0333(19) 0.0277(15) 0.0398(19) -0.0044(13) 0.0086(16) 0.0071(15)
    N21A 0.052(2) 0.0343(17) 0.0254(17) -0.0082(18) -0.0119(18) 0.0056(15)
    C21A 0.055(4) 0.033(3) 0.037(3) -0.003(2) -0.001(3) -0.002(3)
    C22A 0.039(2) 0.036(3) 0.031(2) 0.0025(19) 0.0101(19) -0.003(2)
    N22A 0.027(2) 0.0278(19) 0.0286(19) 0.0027(16) -0.0043(16) 0.0020(16)
    N21B 0.052(2) 0.0343(17) 0.0254(17) -0.0082(18) -0.0119(18) 0.0056(15)
    C21B 0.055(4) 0.033(3) 0.037(3) -0.003(2) -0.001(3) -0.002(3)
    C22B 0.039(2) 0.036(3) 0.031(2) 0.0025(19) 0.0101(19) -0.003(2)
    N22B 0.027(2) 0.0278(19) 0.0286(19) 0.0027(16) -0.0043(16) 0.0020(16)
_geom_special_details
;
All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes.
;
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
    Ni N31 . 2.101(3) y
    Ni N22A . 2.105(7) y
    Ni N11B . 2.113(13) ?
    Ni N12A . 2.113(7) y
    Ni N21A . 2.116(7) y
    Ni N21B . 2.117(19) ?
    Ni N32 . 2.122(3) y
    Ni N11A . 2.140(5) y
    Ni N12B . 2.180(18) ?
    Ni N22B . 2.194(18) ?
    N31 C31 . 1.467(4) ?
    N31 H31A . 0.9200 ?
    N31 H31B . 0.9200 ?
    N32 C32 . 1.473(4) ?
    N32 H32A . 0.9200 ?
    N32 H32B . 0.9200 ?
    C31 C32 . 1.508(5) ?
    C31 H31C . 0.9900 ?
    C31 H31D . 0.9900 ?
    C32 H32C . 0.9900 ?
    C32 H32D . 0.9900 ?
    N11A C11A . 1.473(7) ?
    N11A H11A . 0.9200 ?
    N11A H11B . 0.9200 ?
    C11A C12A . 1.495(8) ?
    C11A H11C . 0.9900 ?
    C11A H11D . 0.9900 ?
    C12A N12A . 1.470(8) ?
    C12A H12A . 0.9900 ?
    C12A H12B . 0.9900 ?
    N12A H12C . 0.9200 ?
    N12A H12D . 0.9200 ?
    N11B C11B . 1.467(14) ?
    N11B H11E . 0.9200 ?
    N11B H11F . 0.9200 ?
    C11B C12B . 1.507(14) ?
    C11B H11G . 0.9900 ?
    C11B H11H . 0.9900 ?
    C12B N12B . 1.472(14) ?
    C12B H12E . 0.9900 ?
    C12B H12F . 0.9900 ?
    N12B H12G . 0.9200 ?
    N12B H12H . 0.9200 ?
    N21A C21A . 1.478(8) ?
    N21A H21A . 0.9200 ?
    N21A H21B . 0.9200 ?
    C21A C22A . 1.462(8) ?
    C21A H21C . 0.9900 ?
    C21A H21D . 0.9900 ?
    C22A N22A . 1.482(6) ?
    C22A H22A . 0.9900 ?
    C22A H22B . 0.9900 ?
    N22A H22C . 0.9200 ?
    N22A H22D . 0.9200 ?
    N21B C21B . 1.481(14) ?
    N21B H21E . 0.9200 ?
    N21B H21F . 0.9200 ?
    C21B C22B . 1.450(14) ?
    C21B H21G . 0.9900 ?
    C21B H21H . 0.9900 ?
    C22B N22B . 1.480(14) ?
    C22B H22E . 0.9900 ?
    C22B H22F . 0.9900 ?
    N22B H22G . 0.9200 ?
    N22B H22H . 0.9200 ?
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
    _geom_angle_publ_flag
    N31 Ni N22A . . 93.25(16) y
    N31 Ni N11B . . 83.9(3) ?
    N22A Ni N11B . . 173.3(4) ?
    N31 Ni N12A . . 91.3(3) y
    N22A Ni N12A . . 90.2(2) y
    N11B Ni N12A . . 83.8(3) ?
    N31 Ni N21A . . 171.6(2) y
    N22A Ni N21A . . 81.1(2) y
    N11B Ni N21A . . 102.4(4) ?
    N12A Ni N21A . . 94.9(3) y
    N31 Ni N21B . . 166.7(4) ?
    N22A Ni N21B . . 75.8(4) ?
    N11B Ni N21B . . 107.8(5) ?
    N12A Ni N21B . . 96.2(6) ?
    N21A Ni N21B . . 5.4(5) ?
    N31 Ni N32 . . 81.99(11) y
    N22A Ni N32 . . 95.9(2) y
    N11B Ni N32 . . 89.7(3) ?
    N12A Ni N32 . . 171.2(2) y
    N21A Ni N32 . . 92.4(2) y
    N21B Ni N32 . . 91.5(6) ?
    N31 Ni N11A . . 97.93(14) y
    N22A Ni N11A . . 166.02(19) y
    N11B Ni N11A . . 14.3(3) ?
    N12A Ni N11A . . 81.26(19) y
    N21A Ni N11A . . 88.6(2) y
    N21B Ni N11A . . 94.0(4) ?
    N32 Ni N11A . . 93.98(14) y
    N31 Ni N12B . . 89.7(6) ?
    N22A Ni N12B . . 92.4(4) ?
    N11B Ni N12B . . 81.6(4) ?
    N12A Ni N12B . . 2.6(6) ?
    N21A Ni N12B . . 96.7(7) ?
    N21B Ni N12B . . 98.2(8) ?
    N32 Ni N12B . . 168.6(5) ?
    N11A Ni N12B . . 79.4(4) ?
    N31 Ni N22B . . 88.1(4) ?
    N22A Ni N22B . . 6.7(5) ?
    N11B Ni N22B . . 171.8(5) ?
    N12A Ni N22B . . 94.6(5) ?
    N21A Ni N22B . . 85.7(4) ?
    N21B Ni N22B . . 80.4(5) ?
    N32 Ni N22B . . 90.9(5) ?
    N11A Ni N22B . . 172.7(4) ?
    N12B Ni N22B . . 96.7(6) ?
    C31 N31 Ni . . 109.0(2) ?
    C31 N31 H31A . . 109.9 ?
    Ni N31 H31A . . 109.9 ?
    C31 N31 H31B . . 109.9 ?
    Ni N31 H31B . . 109.9 ?
    H31A N31 H31B . . 108.3 ?
    C32 N32 Ni . . 107.9(2) ?
    C32 N32 H32A . . 110.1 ?
    Ni N32 H32A . . 110.1 ?
    C32 N32 H32B . . 110.1 ?
    Ni N32 H32B . . 110.1 ?
    H32A N32 H32B . . 108.4 ?
    N31 C31 C32 . . 108.8(3) ?
    N31 C31 H31C . . 109.9 ?
    C32 C31 H31C . . 109.9 ?
    N31 C31 H31D . . 109.9 ?
    C32 C31 H31D . . 109.9 ?
    H31C C31 H31D . . 108.3 ?
    N32 C32 C31 . . 109.0(3) ?
    N32 C32 H32C . . 109.9 ?
    C31 C32 H32C . . 109.9 ?
    N32 C32 H32D . . 109.9 ?
    C31 C32 H32D . . 109.9 ?
    H32C C32 H32D . . 108.3 ?
    C11A N11A Ni . . 107.8(3) ?
    C11A N11A H11A . . 110.2 ?
    Ni N11A H11A . . 110.2 ?
    C11A N11A H11B . . 110.2 ?
    Ni N11A H11B . . 110.2 ?
    H11A N11A H11B . . 108.5 ?
    N11A C11A C12A . . 107.0(5) ?
    N11A C11A H11C . . 110.3 ?
    C12A C11A H11C . . 110.3 ?
    N11A C11A H11D . . 110.3 ?
    C12A C11A H11D . . 110.3 ?
    H11C C11A H11D . . 108.6 ?
    N12A C12A C11A . . 111.1(5) ?
    N12A C12A H12A . . 109.4 ?
    C11A C12A H12A . . 109.4 ?
    N12A C12A H12B . . 109.4 ?
    C11A C12A H12B . . 109.4 ?
    H12A C12A H12B . . 108.0 ?
    C12A N12A Ni . . 108.7(4) ?
    C12A N12A H12C . . 109.9 ?
    Ni N12A H12C . . 109.9 ?
    C12A N12A H12D . . 109.9 ?
    Ni N12A H12D . . 109.9 ?
    H12C N12A H12D . . 108.3 ?
    C11B N11B Ni . . 108.0(9) ?
    C11B N11B H11E . . 110.1 ?
    Ni N11B H11E . . 110.1 ?
    C11B N11B H11F . . 110.1 ?
    Ni N11B H11F . . 110.1 ?
    H11E N11B H11F . . 108.4 ?
    N11B C11B C12B . . 110.4(12) ?
    N11B C11B H11G . . 109.6 ?
    C12B C11B H11G . . 109.6 ?
    N11B C11B H11H . . 109.6 ?
    C12B C11B H11H . . 109.6 ?
    H11G C11B H11H . . 108.1 ?
    N12B C12B C11B . . 108.7(12) ?
    N12B C12B H12E . . 110.0 ?
    C11B C12B H12E . . 110.0 ?
    N12B C12B H12F . . 110.0 ?
    C11B C12B H12F . . 110.0 ?
    H12E C12B H12F . . 108.3 ?
    C12B N12B Ni . . 107.5(10) ?
    C12B N12B H12G . . 110.2 ?
    Ni N12B H12G . . 110.2 ?
    C12B N12B H12H . . 110.2 ?
    Ni N12B H12H . . 110.2 ?
    H12G N12B H12H . . 108.5 ?
    C21A N21A Ni . . 108.3(4) ?
    C21A N21A H21A . . 110.0 ?
    Ni N21A H21A . . 110.0 ?
    C21A N21A H21B . . 110.0 ?
    Ni N21A H21B . . 110.0 ?
    H21A N21A H21B . . 108.4 ?
    C22A C21A N21A . . 109.8(5) ?
    C22A C21A H21C . . 109.7 ?
    N21A C21A H21C . . 109.7 ?
    C22A C21A H21D . . 109.7 ?
    N21A C21A H21D . . 109.7 ?
    H21C C21A H21D . . 108.2 ?
    C21A C22A N22A . . 109.1(5) ?
    C21A C22A H22A . . 109.9 ?
    N22A C22A H22A . . 109.9 ?
    C21A C22A H22B . . 109.9 ?
    N22A C22A H22B . . 109.9 ?
    H22A C22A H22B . . 108.3 ?
    C22A N22A Ni . . 109.7(4) ?
    C22A N22A H22C . . 109.7 ?
    Ni N22A H22C . . 109.7 ?
    C22A N22A H22D . . 109.7 ?
    Ni N22A H22D . . 109.7 ?
    H22C N22A H22D . . 108.2 ?
    C21B N21B Ni . . 107.4(10) ?
    C21B N21B H21E . . 110.2 ?
    Ni N21B H21E . . 110.2 ?
    C21B N21B H21F . . 110.2 ?
    Ni N21B H21F . . 110.2 ?
    H21E N21B H21F . . 108.5 ?
    C22B C21B N21B . . 108.2(12) ?
    C22B C21B H21G . . 110.1 ?
    N21B C21B H21G . . 110.1 ?
    C22B C21B H21H . . 110.1 ?
    N21B C21B H21H . . 110.1 ?
    H21G C21B H21H . . 108.4 ?
    C21B C22B N22B . . 108.5(12) ?
    C21B C22B H22E . . 110.0 ?
    N22B C22B H22E . . 110.0 ?
    C21B C22B H22F . . 110.0 ?
    N22B C22B H22F . . 110.0 ?
    H22E C22B H22F . . 108.4 ?
    C22B N22B Ni . . 105.9(10) ?
    C22B N22B H22G . . 110.5 ?
    Ni N22B H22G . . 110.5 ?
    C22B N22B H22H . . 110.5 ?
    Ni N22B H22H . . 110.5 ?
    H22G N22B H22H . . 108.7 ?
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_2
    _geom_torsion_site_symmetry_3
    _geom_torsion_site_symmetry_4
    _geom_torsion
    _geom_torsion_publ_flag
    N22A Ni N31 C31 . . . . -81.5(3) ?
    N11B Ni N31 C31 . . . . 104.6(4) ?
    N12A Ni N31 C31 . . . . -171.7(3) ?
    N21A Ni N31 C31 . . . . -34.1(14) ?
    N21B Ni N31 C31 . . . . -47(2) ?
    N32 Ni N31 C31 . . . . 14.0(2) ?
    N11A Ni N31 C31 . . . . 106.9(3) ?
    N12B Ni N31 C31 . . . . -173.8(4) ?
    N22B Ni N31 C31 . . . . -77.1(6) ?
    N31 Ni N32 C32 . . . . 14.7(2) ?
    N22A Ni N32 C32 . . . . 107.2(3) ?
    N11B Ni N32 C32 . . . . -69.1(4) ?
    N12A Ni N32 C32 . . . . -25.7(15) ?
    N21A Ni N32 C32 . . . . -171.5(3) ?
    N21B Ni N32 C32 . . . . -176.9(4) ?
    N11A Ni N32 C32 . . . . -82.7(3) ?
    N12B Ni N32 C32 . . . . -29(3) ?
    N22B Ni N32 C32 . . . . 102.7(4) ?
    Ni N31 C31 C32 . . . . -39.9(3) ?
    Ni N32 C32 C31 . . . . -40.5(3) ?
    N31 C31 C32 N32 . . . . 54.4(4) ?
    N31 Ni N11A C11A . . . . 69.7(4) ?
    N22A Ni N11A C11A . . . . -73.1(10) ?
    N11B Ni N11A C11A . . . . 79.1(15) ?
    N12A Ni N11A C11A . . . . -20.4(4) ?
    N21A Ni N11A C11A . . . . -115.6(4) ?
    N21B Ni N11A C11A . . . . -116.1(7) ?
    N32 Ni N11A C11A . . . . 152.1(4) ?
    N12B Ni N11A C11A . . . . -18.5(7) ?
    N22B Ni N11A C11A . . . . -76(4) ?
    Ni N11A C11A C12A . . . . 44.7(6) ?
    N11A C11A C12A N12A . . . . -54.8(7) ?
    C11A C12A N12A Ni . . . . 36.2(7) ?
    N31 Ni N12A C12A . . . . -106.1(5) ?
    N22A Ni N12A C12A . . . . 160.6(5) ?
    N11B Ni N12A C12A . . . . -22.4(6) ?
    N21A Ni N12A C12A . . . . 79.5(5) ?
    N21B Ni N12A C12A . . . . 84.8(6) ?
    N32 Ni N12A C12A . . . . -66.1(18) ?
    N11A Ni N12A C12A . . . . -8.3(5) ?
    N12B Ni N12A C12A . . . . -53(17) ?
    N22B Ni N12A C12A . . . . 165.6(6) ?
    N31 Ni N11B C11B . . . . 106.4(10) ?
    N22A Ni N11B C11B . . . . 41(3) ?
    N12A Ni N11B C11B . . . . 14.4(10) ?
    N21A Ni N11B C11B . . . . -79.3(11) ?
    N21B Ni N11B C11B . . . . -80.2(12) ?
    N32 Ni N11B C11B . . . . -171.7(10) ?
    N11A Ni N11B C11B . . . . -64.3(15) ?
    N12B Ni N11B C11B . . . . 15.8(12) ?
    N22B Ni N11B C11B . . . . 94(4) ?
    Ni N11B C11B C12B . . . . -42.4(16) ?
    N11B C11B C12B N12B . . . . 55.6(19) ?
    C11B C12B N12B Ni . . . . -38.7(17) ?
    N31 Ni N12B C12B . . . . -70.9(13) ?
    N22A Ni N12B C12B . . . . -164.2(13) ?
    N11B Ni N12B C12B . . . . 12.9(13) ?
    N12A Ni N12B C12B . . . . 162(18) ?
    N21A Ni N12B C12B . . . . 114.5(13) ?
    N21B Ni N12B C12B . . . . 119.8(13) ?
    N32 Ni N12B C12B . . . . -28(4) ?
    N11A Ni N12B C12B . . . . 27.2(12) ?
    N22B Ni N12B C12B . . . . -159.0(13) ?
    N31 Ni N21A C21A . . . . -63.5(16) ?
    N22A Ni N21A C21A . . . . -15.4(5) ?
    N11B Ni N21A C21A . . . . 158.8(5) ?
    N12A Ni N21A C21A . . . . 74.0(5) ?
    N21B Ni N21A C21A . . . . -30(8) ?
    N32 Ni N21A C21A . . . . -111.0(5) ?
    N11A Ni N21A C21A . . . . 155.1(5) ?
    N12B Ni N21A C21A . . . . 75.9(6) ?
    N22B Ni N21A C21A . . . . -20.3(7) ?
    Ni N21A C21A C22A . . . . 41.1(6) ?
    N21A C21A C22A N22A . . . . -52.7(7) ?
    C21A C22A N22A Ni . . . . 37.8(6) ?
    N31 Ni N22A C22A . . . . 161.9(4) ?
    N11B Ni N22A C22A . . . . -134(3) ?
    N12A Ni N22A C22A . . . . -106.9(5) ?
    N21A Ni N22A C22A . . . . -11.9(5) ?
    N21B Ni N22A C22A . . . . -10.5(7) ?
    N32 Ni N22A C22A . . . . 79.6(4) ?
    N11A Ni N22A C22A . . . . -55.0(11) ?
    N12B Ni N22A C22A . . . . -108.3(8) ?
    N22B Ni N22A C22A . . . . 121(5) ?
    N31 Ni N21B C21B . . . . -13(3) ?
    N22A Ni N21B C21B . . . . 22.5(10) ?
    N11B Ni N21B C21B . . . . -163.3(10) ?
    N12A Ni N21B C21B . . . . 111.1(11) ?
    N21A Ni N21B C21B . . . . -172(9) ?
    N32 Ni N21B C21B . . . . -73.1(12) ?
    N11A Ni N21B C21B . . . . -167.2(11) ?
    N12B Ni N21B C21B . . . . 112.9(12) ?
    N22B Ni N21B C21B . . . . 17.5(12) ?
    Ni N21B C21B C22B . . . . -47.1(15) ?
    N21B C21B C22B N22B . . . . 61.4(18) ?
    C21B C22B N22B Ni . . . . -42.9(16) ?
    N31 Ni N22B C22B . . . . -173.6(11) ?
    N22A Ni N22B C22B . . . . -34(4) ?
    N11B Ni N22B C22B . . . . -161(3) ?
    N12A Ni N22B C22B . . . . -82.5(12) ?
    N21A Ni N22B C22B . . . . 12.2(11) ?
    N21B Ni N22B C22B . . . . 13.1(12) ?
    N32 Ni N22B C22B . . . . 104.5(11) ?
    N11A Ni N22B C22B . . . . -27(5) ?
    N12B Ni N22B C22B . . . . -84.1(13) ?
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
    N31 H31A I2 . 0.92 2.83 3.731(3) 166.6
    N31 H31B I1 . 0.92 2.79 3.663(3) 158.4
    N32 H32A I2 7_566 0.92 3.05 3.786(3) 138.0
    N32 H32B I1 6_556 0.92 2.86 3.724(3) 156.7
    N11A H11B I2 3_645 0.92 2.97 3.854(4) 162.2
    N12A H12C I2 . 0.92 3.15 3.940(8) 144.7
    N11B H11F I2 3_645 0.92 3.15 3.619(12) 114.0
    N12B H12G I2 . 0.92 3.07 3.94(2) 158.6
    N12B H12H I1 3_655 0.92 3.27 3.824(16) 120.8
    N21A H21A I2 7_566 0.92 2.92 3.826(8) 170.8
    N21A H21B I1 7_566 0.92 2.77 3.665(7) 165.7
    N22A H22D I1 6_556 0.92 3.19 3.905(7) 136.3
    N21B H21E I2 7_566 0.92 3.05 3.86(2) 148.2
    N21B H21F I1 7_566 0.92 3.22 3.832(16) 125.4
    N22B H22G I2 . 0.92 3.21 4.061(16) 153.8
    N22B H22H I1 6_556 0.92 2.80 3.69(2) 162.6
