# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
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data_complex7_1hUV
_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;
Dinitro-(3,3-diamino-N-methyldipropylamine)nickel(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H19 N5 Ni O4'
_chemical_formula_sum            'C7 H19 N5 Ni O4'
_chemical_formula_weight         295.98

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'
O O 0.0106 0.0060 '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'


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

_cell_length_a                   7.100(5)
_cell_length_b                   23.968(5)
_cell_length_c                   10.935(5)
_cell_angle_alpha                90.000
_cell_angle_beta                 103.945(5)
_cell_angle_gamma                90.000
_cell_volume                     1806.0(16)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6565
_cell_measurement_theta_min      3.0583
_cell_measurement_theta_max      29.0631

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)

_exptl_crystal_description       Block
_exptl_crystal_colour            Violet
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936
_exptl_absorpt_coefficient_mu    1.625

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.57157
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13216
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.11
_diffrn_reflns_theta_max         29.24
_reflns_number_total             7582
_reflns_number_gt                6654
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'POV-RAY for Windows, 3.62 (Cason, 2009)'
_computing_publication_material  'WinGX, 1.80.05 (Farrugia, 1999)'


_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 > 2sigma(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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0429P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.496(12)
_refine_ls_number_reflns         7582
_refine_ls_number_parameters     500
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0753
_refine_ls_wR_factor_gt          0.0731
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3222(6) -0.15497(17) -0.3648(3) 0.0240(8) Uani 1 1 d . . .
H1A H 0.2095 -0.1758 -0.4153 0.029 Uiso 1 1 calc R . .
H1B H 0.4416 -0.1724 -0.3788 0.029 Uiso 1 1 calc R . .
C2 C 0.3118(6) -0.09529(17) -0.4085(3) 0.0238(8) Uani 1 1 d . . .
H2A H 0.3364 -0.0941 -0.4938 0.029 Uiso 1 1 calc R . .
H2B H 0.4162 -0.0738 -0.3515 0.029 Uiso 1 1 calc R . .
C3 C 0.1187(5) -0.06705(16) -0.4128(3) 0.0219(8) Uani 1 1 d . . .
H3A H 0.1099 -0.0332 -0.4658 0.026 Uiso 1 1 calc R . .
H3B H 0.0136 -0.0926 -0.4552 0.026 Uiso 1 1 calc R . .
C4 C -0.1205(5) -0.02760(17) -0.3205(3) 0.0198(8) Uani 1 1 d . . .
H4A H -0.2081 -0.0565 -0.3678 0.024 Uiso 1 1 calc R . .
H4B H -0.1247 0.0046 -0.3778 0.024 Uiso 1 1 calc R . .
C5 C -0.2007(5) -0.00900(18) -0.2115(3) 0.0222(8) Uani 1 1 d . . .
H5A H -0.1086 0.0178 -0.1601 0.027 Uiso 1 1 calc R . .
H5B H -0.3241 0.0111 -0.2454 0.027 Uiso 1 1 calc R . .
C6 C -0.2378(5) -0.05492(17) -0.1268(3) 0.0202(8) Uani 1 1 d . . .
H6A H -0.3086 -0.0395 -0.0667 0.024 Uiso 1 1 calc R . .
H6B H -0.3212 -0.0836 -0.1783 0.024 Uiso 1 1 calc R . .
C7 C 0.2181(5) -0.00534(16) -0.2338(3) 0.0205(8) Uani 1 1 d . . .
H7A H 0.2134 0.0242 -0.2964 0.031 Uiso 1 1 calc R . .
H7B H 0.3501 -0.0204 -0.2085 0.031 Uiso 1 1 calc R . .
H7C H 0.1811 0.0100 -0.1599 0.031 Uiso 1 1 calc R . .
C11 C 0.5508(6) -0.04889(18) 0.3265(3) 0.0239(8) Uani 1 1 d . . .
H11A H 0.5214 -0.0893 0.3186 0.029 Uiso 1 1 calc R . .
H11B H 0.6049 -0.0404 0.4168 0.029 Uiso 1 1 calc R . .
C12 C 0.6982(6) -0.03425(17) 0.2518(4) 0.0270(9) Uani 1 1 d . . .
H12A H 0.8079 -0.0608 0.2749 0.032 Uiso 1 1 calc R . .
H12B H 0.6370 -0.0396 0.1611 0.032 Uiso 1 1 calc R . .
C13 C 0.7774(5) 0.02406(16) 0.2706(3) 0.0186(8) Uani 1 1 d . . .
H13A H 0.8929 0.0260 0.2350 0.022 Uiso 1 1 calc R . .
H13B H 0.8222 0.0308 0.3624 0.022 Uiso 1 1 calc R . .
C14 C 0.7551(5) 0.12224(17) 0.2524(4) 0.0221(8) Uani 1 1 d . . .
H14A H 0.8670 0.1218 0.2131 0.027 Uiso 1 1 calc R . .
H14B H 0.8081 0.1208 0.3448 0.027 Uiso 1 1 calc R . .
C15 C 0.6525(7) 0.17693(17) 0.2212(4) 0.0316(10) Uani 1 1 d . . .
H15A H 0.5753 0.1757 0.1328 0.038 Uiso 1 1 calc R . .
H15B H 0.7507 0.2068 0.2274 0.038 Uiso 1 1 calc R . .
C16 C 0.5195(6) 0.19183(16) 0.3053(3) 0.0211(8) Uani 1 1 d . . .
H16A H 0.5906 0.1884 0.3947 0.025 Uiso 1 1 calc R . .
H16B H 0.4756 0.2310 0.2897 0.025 Uiso 1 1 calc R . .
C17 C 0.5938(4) 0.0656(2) 0.0760(3) 0.0255(8) Uani 1 1 d . . .
H17A H 0.5160 0.0978 0.0382 0.038 Uiso 1 1 calc R . .
H17B H 0.5196 0.0313 0.0512 0.038 Uiso 1 1 calc R . .
H17C H 0.7136 0.0642 0.0465 0.038 Uiso 1 1 calc R . .
C21 C -0.2594(5) 0.19829(17) -0.1443(4) 0.0225(8) Uani 1 1 d . . .
H21A H -0.3466 0.2257 -0.1976 0.027 Uiso 1 1 calc R . .
H21B H -0.3266 0.1832 -0.0820 0.027 Uiso 1 1 calc R . .
C22 C -0.2157(5) 0.15103(17) -0.2263(4) 0.0234(8) Uani 1 1 d . . .
H22A H -0.3355 0.1289 -0.2575 0.028 Uiso 1 1 calc R . .
H22B H -0.1176 0.1261 -0.1737 0.028 Uiso 1 1 calc R . .
C23 C -0.1412(6) 0.17039(18) -0.3389(3) 0.0231(9) Uani 1 1 d . . .
H23A H -0.1437 0.1381 -0.3956 0.028 Uiso 1 1 calc R . .
H23B H -0.2332 0.1984 -0.3857 0.028 Uiso 1 1 calc R . .
C24 C 0.0888(5) 0.21086(17) -0.4354(3) 0.0226(8) Uani 1 1 d . . .
H24A H -0.0192 0.2355 -0.4778 0.027 Uiso 1 1 calc R . .
H24B H 0.0812 0.1766 -0.4871 0.027 Uiso 1 1 calc R . .
C25 C 0.2788(5) 0.24028(17) -0.4354(3) 0.0235(8) Uani 1 1 d . . .
H25A H 0.3009 0.2384 -0.5213 0.028 Uiso 1 1 calc R . .
H25B H 0.3864 0.2201 -0.3781 0.028 Uiso 1 1 calc R . .
C26 C 0.2839(6) 0.30132(17) -0.3945(3) 0.0270(9) Uani 1 1 d . . .
H26A H 0.4005 0.3196 -0.4108 0.032 Uiso 1 1 calc R . .
H26B H 0.1680 0.3209 -0.4445 0.032 Uiso 1 1 calc R . .
C27 C 0.1995(5) 0.15130(16) -0.2543(4) 0.0213(8) Uani 1 1 d . . .
H27A H 0.1919 0.1203 -0.3137 0.032 Uiso 1 1 calc R . .
H27B H 0.1702 0.1376 -0.1764 0.032 Uiso 1 1 calc R . .
H27C H 0.3305 0.1672 -0.2351 0.032 Uiso 1 1 calc R . .
N2 N 0.3713(4) -0.12781(14) 0.0577(3) 0.0230(7) Uani 1 1 d . . .
N3 N 0.3227(5) -0.15910(13) -0.2305(3) 0.0197(7) Uani 1 1 d . A .
H3C H 0.4436 -0.1480 -0.1853 0.024 Uiso 1 1 calc R . .
H3D H 0.3108 -0.1963 -0.2130 0.024 Uiso 1 1 calc R . .
N4 N 0.0816(4) -0.05043(13) -0.2893(2) 0.0152(6) Uani 1 1 d . A .
N5 N -0.0570(4) -0.08107(14) -0.0562(3) 0.0202(7) Uani 1 1 d . A .
H5C H -0.0892 -0.1083 -0.0056 0.024 Uiso 1 1 calc R . .
H5D H 0.0136 -0.0545 -0.0039 0.024 Uiso 1 1 calc R . .
N12 N 0.3877(4) 0.0691(2) 0.5193(2) 0.0299(6) Uani 1 1 d . . .
N13 N 0.3731(5) -0.01685(14) 0.2794(3) 0.0233(7) Uani 1 1 d . B .
H13C H 0.2857 -0.0273 0.3251 0.028 Uiso 1 1 calc R . .
H13D H 0.3217 -0.0275 0.1973 0.028 Uiso 1 1 calc R . .
N14 N 0.6424(3) 0.07092(16) 0.2143(2) 0.0141(4) Uani 1 1 d . B .
N15 N 0.3506(5) 0.15450(15) 0.2799(3) 0.0259(7) Uani 1 1 d . B .
H15C H 0.2750 0.1636 0.2016 0.031 Uiso 1 1 calc R . .
H15D H 0.2792 0.1628 0.3374 0.031 Uiso 1 1 calc R . .
N22 N 0.3452(5) 0.27530(16) 0.0302(3) 0.0309(9) Uani 1 1 d . . .
N23 N -0.0805(4) 0.22610(13) -0.0784(3) 0.0190(7) Uani 1 1 d . C .
H23C H -0.0064 0.2004 -0.0253 0.023 Uiso 1 1 calc R . .
H23D H -0.1135 0.2536 -0.0287 0.023 Uiso 1 1 calc R . .
N24 N 0.0568(4) 0.19492(13) -0.3111(3) 0.0179(6) Uani 1 1 d . C .
N25 N 0.2881(5) 0.30571(13) -0.2591(3) 0.0218(7) Uani 1 1 d . C .
H25C H 0.2738 0.3429 -0.2421 0.026 Uiso 1 1 calc R . .
H25D H 0.4105 0.2954 -0.2150 0.026 Uiso 1 1 calc R . .
O3 O 0.3588(4) -0.08460(11) -0.0112(2) 0.0218(6) Uani 1 1 d . A .
O4 O 0.2485(4) -0.16438(11) 0.0099(2) 0.0229(6) Uani 1 1 d . A .
O13 O 0.2337(3) 0.06721(17) 0.4357(2) 0.0313(6) Uani 1 1 d . B .
O14 O 0.5364(3) 0.07118(15) 0.47397(18) 0.0234(4) Uani 1 1 d . B .
O23 O 0.2180(4) 0.31143(12) -0.0177(2) 0.0284(6) Uani 1 1 d . C .
O24 O 0.3346(4) 0.23287(12) -0.0385(2) 0.0234(6) Uani 1 1 d . C .
Ni1 Ni 0.12120(6) -0.116407(15) -0.15817(4) 0.01522(10) Uani 1 1 d . . .
Ni2 Ni 0.38978(5) 0.06923(2) 0.28313(3) 0.01539(9) Uani 1 1 d . . .
Ni3 Ni 0.09228(6) 0.261768(16) -0.18319(4) 0.01651(10) Uani 1 1 d . . .
N1 N -0.063(4) -0.1741(12) -0.253(3) 0.024(5) Uiso 0.107(8) 1 d PD A 1
O1 O -0.222(4) -0.1600(14) -0.310(3) 0.040(6) Uiso 0.107(8) 1 d PD A 1
O2 O -0.032(6) -0.2248(11) -0.251(3) 0.018(5) Uiso 0.107(8) 1 d PD A 1
N1A N -0.1473(6) -0.20712(15) -0.2771(3) 0.0225(9) Uani 0.893(8) 1 d PD A 2
O1A O -0.1139(5) -0.15429(13) -0.2714(3) 0.0216(8) Uani 0.893(8) 1 d PD A 2
O2A O -0.0160(5) -0.23623(17) -0.2102(4) 0.0303(9) Uani 0.893(8) 1 d PD A 2
N11 N 0.1751(5) 0.0715(3) 0.1075(4) 0.0210(11) Uani 0.678(8) 1 d PD B 3
O11 O 0.1081(9) 0.1155(2) 0.0516(5) 0.0312(14) Uani 0.678(8) 1 d PD B 3
O12 O 0.1108(7) 0.02730(19) 0.0576(4) 0.0336(14) Uani 0.678(8) 1 d PD B 3
N11A N 0.0853(10) 0.0758(4) 0.0276(7) 0.011(2) Uiso 0.322(8) 1 d PD B 4
O11A O 0.1739(12) 0.0468(4) 0.1245(8) 0.017(2) Uiso 0.322(8) 1 d PD B 4
O12A O 0.1431(18) 0.1268(5) 0.0334(13) 0.027(3) Uiso 0.322(8) 1 d PD B 4
N21 N -0.113(3) 0.3237(13) -0.270(3) 0.024(5) Uiso 0.122(8) 1 d PD C 5
O22 O -0.092(5) 0.3735(12) -0.283(3) 0.018(5) Uiso 0.122(8) 1 d PD C 5
O21 O -0.264(4) 0.3045(12) -0.326(2) 0.040(6) Uiso 0.122(8) 1 d PD C 5
N21A N -0.1873(6) 0.34957(17) -0.3052(3) 0.0260(11) Uani 0.878(8) 1 d PD C 6
O21A O -0.1472(5) 0.29739(13) -0.2973(3) 0.0238(9) Uani 0.878(8) 1 d PD C 6
O22A O -0.0532(6) 0.38009(17) -0.2407(4) 0.0326(11) Uani 0.878(8) 1 d PD C 6


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N3 1.471(4) . ?
C1 C2 1.504(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.519(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N4 1.491(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.496(5) . ?
C4 C5 1.507(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.502(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N5 1.470(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 N4 1.480(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C11 N13 1.461(5) . ?
C11 C12 1.516(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.502(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N14 1.508(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 N14 1.472(5) . ?
C14 C15 1.499(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.511(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 N15 1.468(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 N14 1.474(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C21 N23 1.461(4) . ?
C21 C22 1.522(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.524(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 N24 1.486(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 N24 1.481(5) . ?
C24 C25 1.522(5) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.528(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 N25 1.477(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 N24 1.484(5) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
N2 O4 1.258(4) . ?
N2 O3 1.272(4) . ?
N3 Ni1 2.065(3) . ?
N3 H3C 0.9200 . ?
N3 H3D 0.9200 . ?
N4 Ni1 2.108(3) . ?
N5 Ni1 2.059(3) . ?
N5 H5C 0.9200 . ?
N5 H5D 0.9200 . ?
N12 O13 1.246(3) . ?
N12 O14 1.271(3) . ?
N13 Ni2 2.066(4) . ?
N13 H13C 0.9200 . ?
N13 H13D 0.9200 . ?
N14 Ni2 2.106(2) . ?
N15 Ni2 2.062(4) . ?
N15 H15C 0.9200 . ?
N15 H15D 0.9200 . ?
N22 O24 1.255(4) . ?
N22 O23 1.269(5) . ?
N23 Ni3 2.056(3) . ?
N23 H23C 0.9200 . ?
N23 H23D 0.9200 . ?
N24 Ni3 2.102(3) . ?
N25 Ni3 2.070(3) . ?
N25 H25C 0.9200 . ?
N25 H25D 0.9200 . ?
O3 Ni1 2.169(3) . ?
O4 Ni1 2.171(3) . ?
O13 Ni2 2.214(2) . ?
O14 Ni2 2.096(2) . ?
O23 Ni3 2.170(3) . ?
O24 Ni3 2.152(3) . ?
Ni1 N1 2.01(3) . ?
Ni1 O1A 2.037(3) . ?
Ni2 O11A 2.089(9) . ?
Ni2 N11 2.145(4) . ?
Ni3 O21A 2.038(3) . ?
Ni3 N21 2.13(3) . ?
N1 O1 1.200(10) . ?
N1 O2 1.234(19) . ?
N1A O2A 1.250(5) . ?
N1A O1A 1.287(4) . ?
N11 O12 1.227(6) . ?
N11 O11 1.255(7) . ?
N11A O12A 1.287(9) . ?
N11A O11A 1.296(8) . ?
N21 O21 1.194(10) . ?
N21 O22 1.216(19) . ?
N21A O22A 1.271(5) . ?
N21A O21A 1.281(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 C1 C2 111.7(3) . . ?
N3 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N3 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 107.9 . . ?
C1 C2 C3 114.1(3) . . ?
C1 C2 H2A 108.7 . . ?
C3 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
C3 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
N4 C3 C2 116.5(3) . . ?
N4 C3 H3A 108.2 . . ?
C2 C3 H3A 108.2 . . ?
N4 C3 H3B 108.2 . . ?
C2 C3 H3B 108.2 . . ?
H3A C3 H3B 107.3 . . ?
N4 C4 C5 116.9(3) . . ?
N4 C4 H4A 108.1 . . ?
C5 C4 H4A 108.1 . . ?
N4 C4 H4B 108.1 . . ?
C5 C4 H4B 108.1 . . ?
H4A C4 H4B 107.3 . . ?
C6 C5 C4 115.3(4) . . ?
C6 C5 H5A 108.5 . . ?
C4 C5 H5A 108.5 . . ?
C6 C5 H5B 108.5 . . ?
C4 C5 H5B 108.5 . . ?
H5A C5 H5B 107.5 . . ?
N5 C6 C5 112.1(3) . . ?
N5 C6 H6A 109.2 . . ?
C5 C6 H6A 109.2 . . ?
N5 C6 H6B 109.2 . . ?
C5 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N13 C11 C12 109.8(3) . . ?
N13 C11 H11A 109.7 . . ?
C12 C11 H11A 109.7 . . ?
N13 C11 H11B 109.7 . . ?
C12 C11 H11B 109.7 . . ?
H11A C11 H11B 108.2 . . ?
C13 C12 C11 115.2(3) . . ?
C13 C12 H12A 108.5 . . ?
C11 C12 H12A 108.5 . . ?
C13 C12 H12B 108.5 . . ?
C11 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?
C12 C13 N14 117.2(3) . . ?
C12 C13 H13A 108.0 . . ?
N14 C13 H13A 108.0 . . ?
C12 C13 H13B 108.0 . . ?
N14 C13 H13B 108.0 . . ?
H13A C13 H13B 107.2 . . ?
N14 C14 C15 117.7(3) . . ?
N14 C14 H14A 107.9 . . ?
C15 C14 H14A 107.9 . . ?
N14 C14 H14B 107.9 . . ?
C15 C14 H14B 107.9 . . ?
H14A C14 H14B 107.2 . . ?
C14 C15 C16 114.2(3) . . ?
C14 C15 H15A 108.7 . . ?
C16 C15 H15A 108.7 . . ?
C14 C15 H15B 108.7 . . ?
C16 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
N15 C16 C15 110.0(3) . . ?
N15 C16 H16A 109.7 . . ?
C15 C16 H16A 109.7 . . ?
N15 C16 H16B 109.7 . . ?
C15 C16 H16B 109.7 . . ?
H16A C16 H16B 108.2 . . ?
N14 C17 H17A 109.5 . . ?
N14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N23 C21 C22 110.7(3) . . ?
N23 C21 H21A 109.5 . . ?
C22 C21 H21A 109.5 . . ?
N23 C21 H21B 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 108.1 . . ?
C21 C22 C23 114.1(3) . . ?
C21 C22 H22A 108.7 . . ?
C23 C22 H22A 108.7 . . ?
C21 C22 H22B 108.7 . . ?
C23 C22 H22B 108.7 . . ?
H22A C22 H22B 107.6 . . ?
N24 C23 C22 116.8(3) . . ?
N24 C23 H23A 108.1 . . ?
C22 C23 H23A 108.1 . . ?
N24 C23 H23B 108.1 . . ?
C22 C23 H23B 108.1 . . ?
H23A C23 H23B 107.3 . . ?
N24 C24 C25 116.8(3) . . ?
N24 C24 H24A 108.1 . . ?
C25 C24 H24A 108.1 . . ?
N24 C24 H24B 108.1 . . ?
C25 C24 H24B 108.1 . . ?
H24A C24 H24B 107.3 . . ?
C24 C25 C26 113.7(3) . . ?
C24 C25 H25A 108.8 . . ?
C26 C25 H25A 108.8 . . ?
C24 C25 H25B 108.8 . . ?
C26 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
N25 C26 C25 110.8(3) . . ?
N25 C26 H26A 109.5 . . ?
C25 C26 H26A 109.5 . . ?
N25 C26 H26B 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 108.1 . . ?
N24 C27 H27A 109.5 . . ?
N24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O4 N2 O3 112.2(3) . . ?
C1 N3 Ni1 120.9(2) . . ?
C1 N3 H3C 107.1 . . ?
Ni1 N3 H3C 107.1 . . ?
C1 N3 H3D 107.1 . . ?
Ni1 N3 H3D 107.1 . . ?
H3C N3 H3D 106.8 . . ?
C7 N4 C3 109.0(3) . . ?
C7 N4 C4 108.9(3) . . ?
C3 N4 C4 105.1(2) . . ?
C7 N4 Ni1 107.6(2) . . ?
C3 N4 Ni1 113.1(2) . . ?
C4 N4 Ni1 113.1(2) . . ?
C6 N5 Ni1 117.6(2) . . ?
C6 N5 H5C 107.9 . . ?
Ni1 N5 H5C 107.9 . . ?
C6 N5 H5D 107.9 . . ?
Ni1 N5 H5D 107.9 . . ?
H5C N5 H5D 107.2 . . ?
O13 N12 O14 112.3(2) . . ?
C11 N13 Ni2 118.5(2) . . ?
C11 N13 H13C 107.7 . . ?
Ni2 N13 H13C 107.7 . . ?
C11 N13 H13D 107.7 . . ?
Ni2 N13 H13D 107.7 . . ?
H13C N13 H13D 107.1 . . ?
C14 N14 C17 109.9(3) . . ?
C14 N14 C13 104.9(2) . . ?
C17 N14 C13 108.8(3) . . ?
C14 N14 Ni2 111.5(2) . . ?
C17 N14 Ni2 110.88(16) . . ?
C13 N14 Ni2 110.6(2) . . ?
C16 N15 Ni2 120.0(2) . . ?
C16 N15 H15C 107.3 . . ?
Ni2 N15 H15C 107.3 . . ?
C16 N15 H15D 107.3 . . ?
Ni2 N15 H15D 107.3 . . ?
H15C N15 H15D 106.9 . . ?
O24 N22 O23 111.9(3) . . ?
C21 N23 Ni3 118.7(2) . . ?
C21 N23 H23C 107.6 . . ?
Ni3 N23 H23C 107.6 . . ?
C21 N23 H23D 107.6 . . ?
Ni3 N23 H23D 107.6 . . ?
H23C N23 H23D 107.1 . . ?
C24 N24 C27 109.0(3) . . ?
C24 N24 C23 105.2(3) . . ?
C27 N24 C23 108.9(3) . . ?
C24 N24 Ni3 113.2(2) . . ?
C27 N24 Ni3 107.3(2) . . ?
C23 N24 Ni3 113.2(2) . . ?
C26 N25 Ni3 120.8(2) . . ?
C26 N25 H25C 107.1 . . ?
Ni3 N25 H25C 107.1 . . ?
C26 N25 H25D 107.1 . . ?
Ni3 N25 H25D 107.1 . . ?
H25C N25 H25D 106.8 . . ?
N2 O3 Ni1 94.8(2) . . ?
N2 O4 Ni1 95.1(2) . . ?
N12 O13 Ni2 92.44(15) . . ?
N12 O14 Ni2 97.32(17) . . ?
N22 O23 Ni3 94.5(2) . . ?
N22 O24 Ni3 95.8(2) . . ?
N1 Ni1 O1A 17.1(7) . . ?
N1 Ni1 N5 98.7(9) . . ?
O1A Ni1 N5 89.53(14) . . ?
N1 Ni1 N3 83.6(9) . . ?
O1A Ni1 N3 95.08(14) . . ?
N5 Ni1 N3 169.67(12) . . ?
N1 Ni1 N4 101.7(9) . . ?
O1A Ni1 N4 88.02(12) . . ?
N5 Ni1 N4 93.51(12) . . ?
N3 Ni1 N4 95.88(12) . . ?
N1 Ni1 O3 156.4(8) . . ?
O1A Ni1 O3 169.89(11) . . ?
N5 Ni1 O3 85.63(12) . . ?
N3 Ni1 O3 88.34(12) . . ?
N4 Ni1 O3 101.12(11) . . ?
N1 Ni1 O4 99.0(9) . . ?
O1A Ni1 O4 113.05(12) . . ?
N5 Ni1 O4 86.81(11) . . ?
N3 Ni1 O4 82.88(11) . . ?
N4 Ni1 O4 158.94(11) . . ?
O3 Ni1 O4 57.87(10) . . ?
N15 Ni2 N13 169.27(10) . . ?
N15 Ni2 O11A 99.9(2) . . ?
N13 Ni2 O11A 72.5(2) . . ?
N15 Ni2 O14 91.59(13) . . ?
N13 Ni2 O14 93.12(13) . . ?
O11A Ni2 O14 157.1(2) . . ?
N15 Ni2 N14 95.61(14) . . ?
N13 Ni2 N14 93.55(14) . . ?
O11A Ni2 N14 103.0(2) . . ?
O14 Ni2 N14 95.38(9) . . ?
N15 Ni2 N11 84.03(19) . . ?
N13 Ni2 N11 88.98(19) . . ?
O11A Ni2 N11 16.8(2) . . ?
O14 Ni2 N11 164.99(10) . . ?
N14 Ni2 N11 99.32(12) . . ?
N15 Ni2 O13 86.83(14) . . ?
N13 Ni2 O13 87.50(14) . . ?
O11A Ni2 O13 102.7(2) . . ?
O14 Ni2 O13 57.94(9) . . ?
N14 Ni2 O13 153.31(9) . . ?
N11 Ni2 O13 107.37(12) . . ?
O21A Ni3 N23 89.63(14) . . ?
O21A Ni3 N25 94.77(14) . . ?
N23 Ni3 N25 169.57(12) . . ?
O21A Ni3 N24 87.90(12) . . ?
N23 Ni3 N24 93.55(12) . . ?
N25 Ni3 N24 96.05(13) . . ?
O21A Ni3 N21 19.5(6) . . ?
N23 Ni3 N21 96.0(7) . . ?
N25 Ni3 N21 85.3(7) . . ?
N24 Ni3 N21 105.9(8) . . ?
O21A Ni3 O24 170.43(11) . . ?
N23 Ni3 O24 86.28(12) . . ?
N25 Ni3 O24 87.90(12) . . ?
N24 Ni3 O24 100.98(11) . . ?
N21 Ni3 O24 152.8(7) . . ?
O21A Ni3 O23 113.30(13) . . ?
N23 Ni3 O23 86.79(11) . . ?
N25 Ni3 O23 82.78(12) . . ?
N24 Ni3 O23 158.80(12) . . ?
N21 Ni3 O23 95.1(7) . . ?
O24 Ni3 O23 57.86(11) . . ?
O1 N1 O2 115(3) . . ?
O1 N1 Ni1 119(3) . . ?
O2 N1 Ni1 125(3) . . ?
O2A N1A O1A 114.7(4) . . ?
N1A O1A Ni1 125.6(3) . . ?
O12 N11 O11 116.9(5) . . ?
O12 N11 Ni2 119.0(4) . . ?
O11 N11 Ni2 124.2(4) . . ?
O12A N11A O11A 112.5(10) . . ?
N11A O11A Ni2 130.9(7) . . ?
O21 N21 O22 116(3) . . ?
O21 N21 Ni3 113(3) . . ?
O22 N21 Ni3 130(2) . . ?
O22A N21A O21A 113.6(4) . . ?
N21A O21A Ni3 126.1(3) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 C1 C2 C3 -68.9(4) . . . . ?
C1 C2 C3 N4 75.1(4) . . . . ?
N4 C4 C5 C6 -68.1(4) . . . . ?
C4 C5 C6 N5 67.6(4) . . . . ?
N13 C11 C12 C13 67.8(4) . . . . ?
C11 C12 C13 N14 -71.5(4) . . . . ?
N14 C14 C15 C16 75.8(5) . . . . ?
C14 C15 C16 N15 -69.5(5) . . . . ?
N23 C21 C22 C23 -68.3(4) . . . . ?
C21 C22 C23 N24 69.7(4) . . . . ?
N24 C24 C25 C26 -75.5(4) . . . . ?
C24 C25 C26 N25 69.0(4) . . . . ?
C2 C1 N3 Ni1 48.9(4) . . . . ?
C2 C3 N4 C7 67.1(4) . . . . ?
C2 C3 N4 C4 -176.3(3) . . . . ?
C2 C3 N4 Ni1 -52.5(4) . . . . ?
C5 C4 N4 C7 -65.4(4) . . . . ?
C5 C4 N4 C3 178.0(3) . . . . ?
C5 C4 N4 Ni1 54.2(4) . . . . ?
C5 C6 N5 Ni1 -58.5(4) . . . . ?
C12 C11 N13 Ni2 -59.0(4) . . . . ?
C15 C14 N14 C17 69.1(4) . . . . ?
C15 C14 N14 C13 -174.0(4) . . . . ?
C15 C14 N14 Ni2 -54.2(4) . . . . ?
C12 C13 N14 C14 177.4(3) . . . . ?
C12 C13 N14 C17 -65.0(4) . . . . ?
C12 C13 N14 Ni2 57.1(4) . . . . ?
C15 C16 N15 Ni2 52.4(4) . . . . ?
C22 C21 N23 Ni3 59.0(4) . . . . ?
C25 C24 N24 C27 -66.5(4) . . . . ?
C25 C24 N24 C23 176.9(3) . . . . ?
C25 C24 N24 Ni3 52.9(4) . . . . ?
C22 C23 N24 C24 -178.8(3) . . . . ?
C22 C23 N24 C27 64.5(4) . . . . ?
C22 C23 N24 Ni3 -54.8(4) . . . . ?
C25 C26 N25 Ni3 -49.4(4) . . . . ?
O4 N2 O3 Ni1 -0.2(3) . . . . ?
O3 N2 O4 Ni1 0.2(3) . . . . ?
O14 N12 O13 Ni2 0.3(4) . . . . ?
O13 N12 O14 Ni2 -0.3(4) . . . . ?
O24 N22 O23 Ni3 0.6(3) . . . . ?
O23 N22 O24 Ni3 -0.6(3) . . . . ?
C6 N5 Ni1 N1 -61.0(9) . . . . ?
C6 N5 Ni1 O1A -46.5(3) . . . . ?
C6 N5 Ni1 N3 -163.2(6) . . . . ?
C6 N5 Ni1 N4 41.5(3) . . . . ?
C6 N5 Ni1 O3 142.4(3) . . . . ?
C6 N5 Ni1 O4 -159.6(3) . . . . ?
C1 N3 Ni1 N1 72.7(10) . . . . ?
C1 N3 Ni1 O1A 60.0(3) . . . . ?
C1 N3 Ni1 N5 176.2(6) . . . . ?
C1 N3 Ni1 N4 -28.5(3) . . . . ?
C1 N3 Ni1 O3 -129.5(3) . . . . ?
C1 N3 Ni1 O4 172.7(3) . . . . ?
C7 N4 Ni1 N1 -177.2(9) . . . . ?
C3 N4 Ni1 N1 -56.8(9) . . . . ?
C4 N4 Ni1 N1 62.5(9) . . . . ?
C7 N4 Ni1 O1A 172.6(2) . . . . ?
C3 N4 Ni1 O1A -67.1(2) . . . . ?
C4 N4 Ni1 O1A 52.3(2) . . . . ?
C7 N4 Ni1 N5 83.1(2) . . . . ?
C3 N4 Ni1 N5 -156.5(2) . . . . ?
C4 N4 Ni1 N5 -37.1(2) . . . . ?
C7 N4 Ni1 N3 -92.5(2) . . . . ?
C3 N4 Ni1 N3 27.8(2) . . . . ?
C4 N4 Ni1 N3 147.2(2) . . . . ?
C7 N4 Ni1 O3 -3.1(2) . . . . ?
C3 N4 Ni1 O3 117.3(2) . . . . ?
C4 N4 Ni1 O3 -123.4(2) . . . . ?
C7 N4 Ni1 O4 -7.1(4) . . . . ?
C3 N4 Ni1 O4 113.3(3) . . . . ?
C4 N4 Ni1 O4 -127.4(3) . . . . ?
N2 O3 Ni1 N1 -13(2) . . . . ?
N2 O3 Ni1 O1A 27.5(8) . . . . ?
N2 O3 Ni1 N5 89.1(2) . . . . ?
N2 O3 Ni1 N3 -82.5(2) . . . . ?
N2 O3 Ni1 N4 -178.1(2) . . . . ?
N2 O3 Ni1 O4 0.16(19) . . . . ?
N2 O4 Ni1 N1 174.7(9) . . . . ?
N2 O4 Ni1 O1A -175.1(2) . . . . ?
N2 O4 Ni1 N5 -87.0(2) . . . . ?
N2 O4 Ni1 N3 92.4(2) . . . . ?
N2 O4 Ni1 N4 4.5(4) . . . . ?
N2 O4 Ni1 O3 -0.16(19) . . . . ?
C16 N15 Ni2 N13 178.2(5) . . . . ?
C16 N15 Ni2 O11A -137.6(3) . . . . ?
C16 N15 Ni2 O14 62.2(3) . . . . ?
C16 N15 Ni2 N14 -33.3(3) . . . . ?
C16 N15 Ni2 N11 -132.1(3) . . . . ?
C16 N15 Ni2 O13 120.0(3) . . . . ?
C11 N13 Ni2 N15 -167.5(5) . . . . ?
C11 N13 Ni2 O11A 146.6(4) . . . . ?
C11 N13 Ni2 O14 -51.6(3) . . . . ?
C11 N13 Ni2 N14 44.0(3) . . . . ?
C11 N13 Ni2 N11 143.3(3) . . . . ?
C11 N13 Ni2 O13 -109.3(3) . . . . ?
N12 O14 Ni2 N15 85.4(3) . . . . ?
N12 O14 Ni2 N13 -84.9(3) . . . . ?
N12 O14 Ni2 O11A -35.1(7) . . . . ?
N12 O14 Ni2 N14 -178.8(3) . . . . ?
N12 O14 Ni2 N11 12.8(9) . . . . ?
N12 O14 Ni2 O13 0.2(3) . . . . ?
C14 N14 Ni2 N15 30.5(2) . . . . ?
C17 N14 Ni2 N15 -92.2(3) . . . . ?
C13 N14 Ni2 N15 146.9(2) . . . . ?
C14 N14 Ni2 N13 -155.1(2) . . . . ?
C17 N14 Ni2 N13 82.2(3) . . . . ?
C13 N14 Ni2 N13 -38.7(2) . . . . ?
C14 N14 Ni2 O11A 132.1(3) . . . . ?
C17 N14 Ni2 O11A 9.3(4) . . . . ?
C13 N14 Ni2 O11A -111.5(3) . . . . ?
C14 N14 Ni2 O14 -61.6(2) . . . . ?
C17 N14 Ni2 O14 175.7(3) . . . . ?
C13 N14 Ni2 O14 54.8(3) . . . . ?
C14 N14 Ni2 N11 115.4(3) . . . . ?
C17 N14 Ni2 N11 -7.4(4) . . . . ?
C13 N14 Ni2 N11 -128.2(3) . . . . ?
C14 N14 Ni2 O13 -63.6(4) . . . . ?
C17 N14 Ni2 O13 173.7(3) . . . . ?
C13 N14 Ni2 O13 52.8(5) . . . . ?
N12 O13 Ni2 N15 -94.0(3) . . . . ?
N12 O13 Ni2 N13 95.1(3) . . . . ?
N12 O13 Ni2 O11A 166.5(4) . . . . ?
N12 O13 Ni2 O14 -0.2(3) . . . . ?
N12 O13 Ni2 N14 2.2(5) . . . . ?
N12 O13 Ni2 N11 -176.8(3) . . . . ?
C21 N23 Ni3 O21A 46.4(3) . . . . ?
C21 N23 Ni3 N25 161.5(6) . . . . ?
C21 N23 Ni3 N24 -41.5(3) . . . . ?
C21 N23 Ni3 N21 64.9(8) . . . . ?
C21 N23 Ni3 O24 -142.3(3) . . . . ?
C21 N23 Ni3 O23 159.8(3) . . . . ?
C26 N25 Ni3 O21A -59.2(3) . . . . ?
C26 N25 Ni3 N23 -173.9(6) . . . . ?
C26 N25 Ni3 N24 29.2(3) . . . . ?
C26 N25 Ni3 N21 -76.3(8) . . . . ?
C26 N25 Ni3 O24 130.0(3) . . . . ?
C26 N25 Ni3 O23 -172.1(3) . . . . ?
C24 N24 Ni3 O21A 66.5(2) . . . . ?
C27 N24 Ni3 O21A -173.1(2) . . . . ?
C23 N24 Ni3 O21A -53.0(3) . . . . ?
C24 N24 Ni3 N23 156.0(2) . . . . ?
C27 N24 Ni3 N23 -83.6(2) . . . . ?
C23 N24 Ni3 N23 36.5(3) . . . . ?
C24 N24 Ni3 N25 -28.0(2) . . . . ?
C27 N24 Ni3 N25 92.3(2) . . . . ?
C23 N24 Ni3 N25 -147.5(3) . . . . ?
C24 N24 Ni3 N21 58.8(7) . . . . ?
C27 N24 Ni3 N21 179.2(7) . . . . ?
C23 N24 Ni3 N21 -60.7(8) . . . . ?
C24 N24 Ni3 O24 -117.1(2) . . . . ?
C27 N24 Ni3 O24 3.3(2) . . . . ?
C23 N24 Ni3 O24 123.4(2) . . . . ?
C24 N24 Ni3 O23 -113.7(3) . . . . ?
C27 N24 Ni3 O23 6.7(5) . . . . ?
C23 N24 Ni3 O23 126.8(3) . . . . ?
N22 O24 Ni3 O21A -23.3(8) . . . . ?
N22 O24 Ni3 N23 -88.2(2) . . . . ?
N22 O24 Ni3 N25 83.2(2) . . . . ?
N22 O24 Ni3 N24 178.9(2) . . . . ?
N22 O24 Ni3 N21 7.6(16) . . . . ?
N22 O24 Ni3 O23 0.4(2) . . . . ?
N22 O23 Ni3 O21A 175.5(2) . . . . ?
N22 O23 Ni3 N23 87.2(2) . . . . ?
N22 O23 Ni3 N25 -92.4(2) . . . . ?
N22 O23 Ni3 N24 -4.3(4) . . . . ?
N22 O23 Ni3 N21 -177.1(7) . . . . ?
N22 O23 Ni3 O24 -0.38(19) . . . . ?
O1A Ni1 N1 O1 -6(2) . . . . ?
N5 Ni1 N1 O1 52(3) . . . . ?
N3 Ni1 N1 O1 -138(3) . . . . ?
N4 Ni1 N1 O1 -43(3) . . . . ?
O3 Ni1 N1 O1 151(2) . . . . ?
O4 Ni1 N1 O1 140(3) . . . . ?
O1A Ni1 N1 O2 179(6) . . . . ?
N5 Ni1 N1 O2 -123(3) . . . . ?
N3 Ni1 N1 O2 47(3) . . . . ?
N4 Ni1 N1 O2 142(3) . . . . ?
O3 Ni1 N1 O2 -24(5) . . . . ?
O4 Ni1 N1 O2 -35(3) . . . . ?
O2A N1A O1A Ni1 -3.5(5) . . . . ?
N1 Ni1 O1A N1A 11(4) . . . . ?
N5 Ni1 O1A N1A -112.1(3) . . . . ?
N3 Ni1 O1A N1A 58.7(3) . . . . ?
N4 Ni1 O1A N1A 154.4(3) . . . . ?
O3 Ni1 O1A N1A -50.7(9) . . . . ?
O4 Ni1 O1A N1A -25.7(4) . . . . ?
N15 Ni2 N11 O12 -172.8(4) . . . . ?
N13 Ni2 N11 O12 -0.9(4) . . . . ?
O11A Ni2 N11 O12 -11.9(9) . . . . ?
O14 Ni2 N11 O12 -99.2(8) . . . . ?
N14 Ni2 N11 O12 92.5(4) . . . . ?
O13 Ni2 N11 O12 -88.0(4) . . . . ?
N15 Ni2 N11 O11 6.5(5) . . . . ?
N13 Ni2 N11 O11 178.3(5) . . . . ?
O11A Ni2 N11 O11 167.4(12) . . . . ?
O14 Ni2 N11 O11 80.1(9) . . . . ?
N14 Ni2 N11 O11 -88.2(5) . . . . ?
O13 Ni2 N11 O11 91.3(5) . . . . ?
O12A N11A O11A Ni2 -0.3(12) . . . . ?
N15 Ni2 O11A N11A 21.0(8) . . . . ?
N13 Ni2 O11A N11A -166.8(9) . . . . ?
O14 Ni2 O11A N11A 140.0(6) . . . . ?
N14 Ni2 O11A N11A -77.2(8) . . . . ?
N11 Ni2 O11A N11A 1.7(5) . . . . ?
O13 Ni2 O11A N11A 109.9(8) . . . . ?
O21A Ni3 N21 O21 14.8(16) . . . . ?
N23 Ni3 N21 O21 -57(2) . . . . ?
N25 Ni3 N21 O21 133(2) . . . . ?
N24 Ni3 N21 O21 38(2) . . . . ?
O24 Ni3 N21 O21 -150.4(17) . . . . ?
O23 Ni3 N21 O21 -144(2) . . . . ?
O21A Ni3 N21 O22 -156(5) . . . . ?
N23 Ni3 N21 O22 132(3) . . . . ?
N25 Ni3 N21 O22 -37(3) . . . . ?
N24 Ni3 N21 O22 -132(3) . . . . ?
O24 Ni3 N21 O22 39(4) . . . . ?
O23 Ni3 N21 O22 45(3) . . . . ?
O22A N21A O21A Ni3 5.5(5) . . . . ?
N23 Ni3 O21A N21A 111.4(3) . . . . ?
N25 Ni3 O21A N21A -59.2(3) . . . . ?
N24 Ni3 O21A N21A -155.1(3) . . . . ?
N21 Ni3 O21A N21A 2(2) . . . . ?
O24 Ni3 O21A N21A 46.7(10) . . . . ?
O23 Ni3 O21A N21A 25.0(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3C N22 0.92 2.70 3.215(5) 116.5 2_645
N3 H3D O2 0.92 2.47 2.94(3) 111.7 .
N3 H3D O2A 0.92 2.52 3.083(5) 120.1 .
N5 H5C O23 0.92 2.17 3.007(4) 150.8 2_545
N5 H5C O22A 0.92 2.65 3.286(6) 126.6 2_545
N5 H5D O12 0.92 2.13 3.000(5) 156.8 .
N13 H13D O12 0.92 2.28 2.879(5) 122.4 .
N15 H15C O12A 0.92 2.05 2.821(14) 140.3 .
N15 H15C O11 0.92 2.12 2.828(6) 133.1 .
N23 H23C O12A 0.92 2.08 2.957(13) 159.1 .
N23 H23C O11 0.92 2.28 3.150(6) 158.5 .
N23 H23D O4 0.92 2.22 3.051(4) 150.1 2
N23 H23D O2A 0.92 2.56 3.194(5) 126.2 2
N25 H25C O22A 0.92 2.49 3.054(5) 119.7 .
N25 H25C O22 0.92 2.63 3.11(3) 112.8 .

_diffrn_measured_fraction_theta_max 0.905
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.077


_database_code_depnum_ccdc_archive 'CCDC 994148'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex7_100K
_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;
Dinitro-(3,3-diamino-N-methyldipropylamine)nickel(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H19 N5 Ni O4'
_chemical_formula_sum            'C7 H19 N5 Ni O4'
_chemical_formula_weight         295.98

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'
O O 0.0106 0.0060 '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'


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

_cell_length_a                   7.119(5)
_cell_length_b                   23.688(5)
_cell_length_c                   10.909(5)
_cell_angle_alpha                90.000
_cell_angle_beta                 103.360(5)
_cell_angle_gamma                90.000
_cell_volume                     1789.9(15)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6843
_cell_measurement_theta_min      2.9351
_cell_measurement_theta_max      30.4403

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/m

_exptl_crystal_description       Block
_exptl_crystal_colour            Violet
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936

_exptl_absorpt_coefficient_mu    1.639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.78739
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13098
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.94
_diffrn_reflns_theta_max         30.51
_reflns_number_total             5590
_reflns_number_gt                4896
_reflns_threshold_expression     >2sigma(I)


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'POV-RAY for Windows, 3.62 (Cason, 2009)'
_computing_publication_material  'WinGX, 1.80.05 (Farrugia, 1999)'


_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 > 2sigma(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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0260P)²+0.6777P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5590
_refine_ls_number_parameters     242
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0251
_refine_ls_wR_factor_ref         0.0607
_refine_ls_wR_factor_gt          0.0575
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.28068(19) 0.01828(5) 0.61575(12) 0.0153(2) Uani 1 1 d . . .
H1A H 0.1608 -0.0027 0.5787 0.018 Uiso 1 1 calc R . .
H1B H 0.3896 -0.0015 0.5920 0.018 Uiso 1 1 calc R . .
C2 C 0.2652(2) 0.07763(6) 0.56288(12) 0.0172(2) Uani 1 1 d . . .
H2A H 0.2737 0.0759 0.4737 0.021 Uiso 1 1 calc R . .
H2B H 0.3767 0.0999 0.6094 0.021 Uiso 1 1 calc R . .
C3 C 0.0799(2) 0.10833(6) 0.56999(12) 0.0168(2) Uani 1 1 d . . .
H3A H 0.0701 0.1427 0.5173 0.020 Uiso 1 1 calc R . .
H3B H -0.0304 0.0837 0.5317 0.020 Uiso 1 1 calc R . .
C4 C -0.14027(19) 0.15056(6) 0.67484(12) 0.0169(2) Uani 1 1 d . . .
H4A H -0.2336 0.1220 0.6311 0.020 Uiso 1 1 calc R . .
H4B H -0.1458 0.1829 0.6166 0.020 Uiso 1 1 calc R . .
C5 C -0.20731(19) 0.17091(6) 0.78985(13) 0.0182(3) Uani 1 1 d . . .
H5A H -0.1074 0.1962 0.8396 0.022 Uiso 1 1 calc R . .
H5B H -0.3267 0.1934 0.7613 0.022 Uiso 1 1 calc R . .
C6 C -0.24672(19) 0.12379(6) 0.87446(13) 0.0180(3) Uani 1 1 d . . .
H6A H -0.3115 0.1395 0.9380 0.022 Uiso 1 1 calc R . .
H6B H -0.3346 0.0958 0.8234 0.022 Uiso 1 1 calc R . .
C7 C 0.20204(19) 0.16964(5) 0.74800(12) 0.0174(2) Uani 1 1 d . . .
H7A H 0.3322 0.1538 0.7600 0.026 Uiso 1 1 calc R . .
H7B H 0.1823 0.1832 0.8290 0.026 Uiso 1 1 calc R . .
H7C H 0.1873 0.2012 0.6884 0.026 Uiso 1 1 calc R . .
C11 C 0.53107(19) 0.12723(5) 1.31929(13) 0.0166(2) Uani 1 1 d . . .
H11A H 0.4939 0.0870 1.3062 0.020 Uiso 1 1 calc R . .
H11B H 0.5897 0.1329 1.4100 0.020 Uiso 1 1 calc R . .
C12 C 0.6767(2) 0.14193(6) 1.24265(13) 0.0189(3) Uani 1 1 d . . .
H12A H 0.6121 0.1397 1.1521 0.023 Uiso 1 1 calc R . .
H12B H 0.7807 0.1132 1.2593 0.023 Uiso 1 1 calc R . .
C13 C 0.76766(18) 0.19995(5) 1.26915(13) 0.0168(2) Uani 1 1 d . . .
H13A H 0.8129 0.2041 1.3616 0.020 Uiso 1 1 calc R . .
H13B H 0.8832 0.2012 1.2332 0.020 Uiso 1 1 calc R . .
C17 C 0.6022(3) 0.2500 1.08051(17) 0.0190(4) Uani 1 2 d S . .
H17A H 0.5264 0.2836 1.0481 0.028 Uiso 0.50 1 calc PR . .
H17B H 0.5288 0.2160 1.0482 0.028 Uiso 0.50 1 calc PR . .
H17C H 0.7238 0.2504 1.0530 0.028 Uiso 1 2 calc SR . .
N2 N 0.36452(17) 0.05116(5) 1.04552(10) 0.0182(2) Uani 1 1 d . . .
N3 N 0.31146(15) 0.01885(5) 0.75457(10) 0.0140(2) Uani 1 1 d . . .
H3C H 0.4297 0.0352 0.7871 0.017 Uiso 1 1 calc R . .
H3D H 0.3191 -0.0180 0.7817 0.017 Uiso 1 1 calc R . .
N4 N 0.05754(15) 0.12550(4) 0.69768(10) 0.01291(19) Uani 1 1 d . . .
N5 N -0.06650(16) 0.09555(5) 0.93883(10) 0.0149(2) Uani 1 1 d . . .
H5C H -0.0988 0.0676 0.9887 0.018 Uiso 1 1 calc R . .
H5D H 0.0065 0.1215 0.9920 0.018 Uiso 1 1 calc R . .
N12 N 0.3826(3) 0.2500 1.52173(17) 0.0261(4) Uani 1 2 d S . .
N13 N 0.35807(16) 0.16314(5) 1.28117(11) 0.0181(2) Uani 1 1 d . . .
H13C H 0.2756 0.1538 1.3317 0.022 Uiso 1 1 calc R . .
H13D H 0.2974 0.1532 1.2001 0.022 Uiso 1 1 calc R . .
N14 N 0.6440(2) 0.2500 1.22035(14) 0.0124(3) Uani 1 2 d S . .
O3 O 0.24340(14) 0.01327(4) 0.99929(9) 0.01812(19) Uani 1 1 d . . .
O4 O 0.34792(13) 0.09457(4) 0.97651(9) 0.01731(18) Uani 1 1 d . . .
O13 O 0.2274(2) 0.2500 1.43717(14) 0.0243(3) Uani 1 2 d S . .
O14 O 0.5315(2) 0.2500 1.47676(13) 0.0201(3) Uani 1 2 d S . .
Ni1 Ni 0.10902(2) 0.059720(6) 0.833217(14) 0.01104(4) Uani 1 1 d . . .
Ni2 Ni 0.38772(3) 0.2500 1.28576(2) 0.01100(5) Uani 1 2 d S . .
N1 N -0.09382(16) 0.00162(5) 0.74695(10) 0.0151(2) Uani 1 1 d . . .
O1 O -0.25796(14) 0.01400(4) 0.68439(9) 0.0212(2) Uani 1 1 d . . .
O2 O -0.04934(15) -0.04965(4) 0.75965(10) 0.0217(2) Uani 1 1 d . . .
N11 N 0.1791(2) 0.2500 1.11134(14) 0.0138(3) Uani 1 2 d S . .
O11 O 0.11418(17) 0.29459(4) 1.05855(10) 0.0285(2) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N3 1.4793(17) . ?
C1 C2 1.5139(18) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.524(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N4 1.4947(17) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.4951(19) . ?
C4 C5 1.5201(19) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.5153(19) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N5 1.4732(18) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 N4 1.4803(17) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C11 N13 1.4753(18) . ?
C11 C12 1.515(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.5185(19) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N14 1.4991(16) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C17 N14 1.485(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
N2 O4 1.2639(15) . ?
N2 O3 1.2657(15) . ?
N3 Ni1 2.0790(14) . ?
N3 H3C 0.9200 . ?
N3 H3D 0.9200 . ?
N4 Ni1 2.1209(12) . ?
N5 Ni1 2.0674(13) . ?
N5 H5C 0.9200 . ?
N5 H5D 0.9200 . ?
N12 O13 1.265(2) . ?
N12 O14 1.267(2) . ?
N13 Ni2 2.0679(12) . ?
N13 H13C 0.9200 . ?
N13 H13D 0.9200 . ?
N14 C13 1.4991(16) 4_565 ?
N14 Ni2 2.1070(19) . ?
O3 Ni1 2.1463(12) . ?
O4 Ni1 2.1884(13) . ?
O13 Ni2 2.2141(16) . ?
O14 Ni2 2.0985(16) . ?
Ni1 N1 2.0583(13) . ?
Ni2 N13 2.0679(12) 4_565 ?
Ni2 N11 2.1261(18) . ?
N1 O1 1.2444(16) . ?
N1 O2 1.2547(14) . ?
N11 O11 1.2401(13) 4_565 ?
N11 O11 1.2401(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 C1 C2 111.23(10) . . ?
N3 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N3 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
C1 C2 C3 114.29(11) . . ?
C1 C2 H2A 108.7 . . ?
C3 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
C3 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
N4 C3 C2 117.21(11) . . ?
N4 C3 H3A 108.0 . . ?
C2 C3 H3A 108.0 . . ?
N4 C3 H3B 108.0 . . ?
C2 C3 H3B 108.0 . . ?
H3A C3 H3B 107.2 . . ?
N4 C4 C5 116.85(11) . . ?
N4 C4 H4A 108.1 . . ?
C5 C4 H4A 108.1 . . ?
N4 C4 H4B 108.1 . . ?
C5 C4 H4B 108.1 . . ?
H4A C4 H4B 107.3 . . ?
C6 C5 C4 114.01(11) . . ?
C6 C5 H5A 108.8 . . ?
C4 C5 H5A 108.8 . . ?
C6 C5 H5B 108.8 . . ?
C4 C5 H5B 108.8 . . ?
H5A C5 H5B 107.6 . . ?
N5 C6 C5 111.19(11) . . ?
N5 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
N5 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N13 C11 C12 110.18(11) . . ?
N13 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
N13 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
C11 C12 C13 114.77(11) . . ?
C11 C12 H12A 108.6 . . ?
C13 C12 H12A 108.6 . . ?
C11 C12 H12B 108.6 . . ?
C13 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
N14 C13 C12 117.30(11) . . ?
N14 C13 H13A 108.0 . . ?
C12 C13 H13A 108.0 . . ?
N14 C13 H13B 108.0 . . ?
C12 C13 H13B 108.0 . . ?
H13A C13 H13B 107.2 . . ?
N14 C17 H17A 109.5 . . ?
N14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O4 N2 O3 112.23(11) . . ?
C1 N3 Ni1 118.29(8) . . ?
C1 N3 H3C 107.7 . . ?
Ni1 N3 H3C 107.7 . . ?
C1 N3 H3D 107.7 . . ?
Ni1 N3 H3D 107.7 . . ?
H3C N3 H3D 107.1 . . ?
C7 N4 C3 108.86(10) . . ?
C7 N4 C4 109.18(10) . . ?
C3 N4 C4 104.59(10) . . ?
C7 N4 Ni1 105.49(8) . . ?
C3 N4 Ni1 114.28(8) . . ?
C4 N4 Ni1 114.34(8) . . ?
C6 N5 Ni1 119.52(9) . . ?
C6 N5 H5C 107.4 . . ?
Ni1 N5 H5C 107.4 . . ?
C6 N5 H5D 107.4 . . ?
Ni1 N5 H5D 107.4 . . ?
H5C N5 H5D 107.0 . . ?
O13 N12 O14 112.69(16) . . ?
C11 N13 Ni2 119.54(9) . . ?
C11 N13 H13C 107.4 . . ?
Ni2 N13 H13C 107.4 . . ?
C11 N13 H13D 107.4 . . ?
Ni2 N13 H13D 107.4 . . ?
H13C N13 H13D 107.0 . . ?
C17 N14 C13 109.07(9) . 4_565 ?
C17 N14 C13 109.07(9) . . ?
C13 N14 C13 104.52(14) 4_565 . ?
C17 N14 Ni2 111.36(11) . . ?
C13 N14 Ni2 111.29(8) 4_565 . ?
C13 N14 Ni2 111.29(8) . . ?
N2 O3 Ni1 95.89(7) . . ?
N2 O4 Ni1 93.94(8) . . ?
N12 O13 Ni2 91.71(12) . . ?
N12 O14 Ni2 97.16(12) . . ?
N1 Ni1 N5 94.52(6) . . ?
N1 Ni1 N3 88.85(6) . . ?
N5 Ni1 N3 170.77(4) . . ?
N1 Ni1 N4 100.52(5) . . ?
N5 Ni1 N4 93.30(5) . . ?
N3 Ni1 N4 94.53(5) . . ?
N1 Ni1 O3 99.90(5) . . ?
N5 Ni1 O3 87.07(5) . . ?
N3 Ni1 O3 83.88(5) . . ?
N4 Ni1 O3 159.48(4) . . ?
N1 Ni1 O4 157.84(4) . . ?
N5 Ni1 O4 85.25(6) . . ?
N3 Ni1 O4 88.40(6) . . ?
N4 Ni1 O4 101.61(4) . . ?
O3 Ni1 O4 57.94(4) . . ?
N13 Ni2 N13 168.60(6) . 4_565 ?
N13 Ni2 O14 92.74(3) . . ?
N13 Ni2 O14 92.74(3) 4_565 . ?
N13 Ni2 N14 94.78(3) . . ?
N13 Ni2 N14 94.78(3) 4_565 . ?
O14 Ni2 N14 94.26(7) . . ?
N13 Ni2 N11 86.10(3) . . ?
N13 Ni2 N11 86.10(3) 4_565 . ?
O14 Ni2 N11 165.52(6) . . ?
N14 Ni2 N11 100.22(7) . . ?
N13 Ni2 O13 87.18(3) . . ?
N13 Ni2 O13 87.18(3) 4_565 . ?
O14 Ni2 O13 58.44(7) . . ?
N14 Ni2 O13 152.70(6) . . ?
N11 Ni2 O13 107.08(7) . . ?
O1 N1 O2 118.01(11) . . ?
O1 N1 Ni1 124.32(9) . . ?
O2 N1 Ni1 117.66(9) . . ?
O11 N11 O11 116.81(16) 4_565 . ?
O11 N11 Ni2 121.59(8) 4_565 . ?
O11 N11 Ni2 121.59(8) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 C1 C2 C3 -70.75(14) . . . . ?
C1 C2 C3 N4 70.07(15) . . . . ?
N4 C4 C5 C6 -70.07(15) . . . . ?
C4 C5 C6 N5 69.20(14) . . . . ?
N13 C11 C12 C13 67.84(15) . . . . ?
C11 C12 C13 N14 -73.06(16) . . . . ?
C2 C1 N3 Ni1 57.32(13) . . . . ?
C2 C3 N4 C7 67.10(14) . . . . ?
C2 C3 N4 C4 -176.31(11) . . . . ?
C2 C3 N4 Ni1 -50.53(13) . . . . ?
C5 C4 N4 C7 -65.13(14) . . . . ?
C5 C4 N4 C3 178.50(11) . . . . ?
C5 C4 N4 Ni1 52.76(13) . . . . ?
C5 C6 N5 Ni1 -57.50(13) . . . . ?
C12 C11 N13 Ni2 -55.34(13) . . . . ?
C12 C13 N14 C17 -67.54(15) . . . . ?
C12 C13 N14 C13 175.93(8) . . . 4_565 ?
C12 C13 N14 Ni2 55.70(14) . . . . ?
O4 N2 O3 Ni1 0.13(11) . . . . ?
O3 N2 O4 Ni1 -0.13(10) . . . . ?
O14 N12 O13 Ni2 0.000(1) . . . . ?
O13 N12 O14 Ni2 0.000(1) . . . . ?
C6 N5 Ni1 N1 -62.92(10) . . . . ?
C6 N5 Ni1 N3 -174.1(2) . . . . ?
C6 N5 Ni1 N4 37.91(10) . . . . ?
C6 N5 Ni1 O3 -162.64(9) . . . . ?
C6 N5 Ni1 O4 139.30(10) . . . . ?
C1 N3 Ni1 N1 63.93(9) . . . . ?
C1 N3 Ni1 N5 175.5(2) . . . . ?
C1 N3 Ni1 N4 -36.53(9) . . . . ?
C1 N3 Ni1 O3 164.02(9) . . . . ?
C1 N3 Ni1 O4 -138.06(9) . . . . ?
C7 N4 Ni1 N1 -178.01(8) . . . . ?
C3 N4 Ni1 N1 -58.48(10) . . . . ?
C4 N4 Ni1 N1 62.02(9) . . . . ?
C7 N4 Ni1 N5 86.77(9) . . . . ?
C3 N4 Ni1 N5 -153.70(9) . . . . ?
C4 N4 Ni1 N5 -33.20(9) . . . . ?
C7 N4 Ni1 N3 -88.34(9) . . . . ?
C3 N4 Ni1 N3 31.19(9) . . . . ?
C4 N4 Ni1 N3 151.69(9) . . . . ?
C7 N4 Ni1 O3 -3.70(16) . . . . ?
C3 N4 Ni1 O3 115.84(12) . . . . ?
C4 N4 Ni1 O3 -123.66(12) . . . . ?
C7 N4 Ni1 O4 0.95(8) . . . . ?
C3 N4 Ni1 O4 120.49(9) . . . . ?
C4 N4 Ni1 O4 -119.02(9) . . . . ?
N2 O3 Ni1 N1 179.61(7) . . . . ?
N2 O3 Ni1 N5 -86.31(8) . . . . ?
N2 O3 Ni1 N3 91.86(8) . . . . ?
N2 O3 Ni1 N4 5.29(15) . . . . ?
N2 O3 Ni1 O4 -0.08(7) . . . . ?
N2 O4 Ni1 N1 -0.70(14) . . . . ?
N2 O4 Ni1 N5 89.61(8) . . . . ?
N2 O4 Ni1 N3 -83.70(8) . . . . ?
N2 O4 Ni1 N4 -178.00(7) . . . . ?
N2 O4 Ni1 O3 0.08(7) . . . . ?
C11 N13 Ni2 N13 -174.5(3) . . . 4_565 ?
C11 N13 Ni2 O14 -55.89(10) . . . . ?
C11 N13 Ni2 N14 38.63(11) . . . . ?
C11 N13 Ni2 N11 138.57(10) . . . . ?
C11 N13 Ni2 O13 -114.09(11) . . . . ?
N12 O14 Ni2 N13 -85.00(3) . . . . ?
N12 O14 Ni2 N13 85.00(3) . . . 4_565 ?
N12 O14 Ni2 N14 180.0 . . . . ?
N12 O14 Ni2 N11 0.000(1) . . . . ?
N12 O14 Ni2 O13 0.0 . . . . ?
C17 N14 Ni2 N13 86.89(3) . . . . ?
C13 N14 Ni2 N13 -151.19(9) 4_565 . . . ?
C13 N14 Ni2 N13 -35.03(9) . . . . ?
C17 N14 Ni2 N13 -86.89(3) . . . 4_565 ?
C13 N14 Ni2 N13 35.03(9) 4_565 . . 4_565 ?
C13 N14 Ni2 N13 151.19(9) . . . 4_565 ?
C17 N14 Ni2 O14 180.0 . . . . ?
C13 N14 Ni2 O14 -58.08(8) 4_565 . . . ?
C13 N14 Ni2 O14 58.08(8) . . . . ?
C17 N14 Ni2 N11 0.0 . . . . ?
C13 N14 Ni2 N11 121.92(8) 4_565 . . . ?
C13 N14 Ni2 N11 -121.92(8) . . . . ?
C17 N14 Ni2 O13 180.000(1) . . . . ?
C13 N14 Ni2 O13 -58.08(8) 4_565 . . . ?
C13 N14 Ni2 O13 58.08(8) . . . . ?
N12 O13 Ni2 N13 94.95(3) . . . . ?
N12 O13 Ni2 N13 -94.95(3) . . . 4_565 ?
N12 O13 Ni2 O14 0.000(1) . . . . ?
N12 O13 Ni2 N14 0.000(1) . . . . ?
N12 O13 Ni2 N11 180.000(1) . . . . ?
N5 Ni1 N1 O1 57.08(11) . . . . ?
N3 Ni1 N1 O1 -131.52(10) . . . . ?
N4 Ni1 N1 O1 -37.13(11) . . . . ?
O3 Ni1 N1 O1 144.89(10) . . . . ?
O4 Ni1 N1 O1 145.57(10) . . . . ?
N5 Ni1 N1 O2 -122.07(10) . . . . ?
N3 Ni1 N1 O2 49.32(10) . . . . ?
N4 Ni1 N1 O2 143.72(9) . . . . ?
O3 Ni1 N1 O2 -34.26(10) . . . . ?
O4 Ni1 N1 O2 -33.59(16) . . . . ?
N13 Ni2 N11 O11 -3.57(13) . . . 4_565 ?
N13 Ni2 N11 O11 -175.24(13) 4_565 . . 4_565 ?
O14 Ni2 N11 O11 -89.41(13) . . . 4_565 ?
N14 Ni2 N11 O11 90.59(13) . . . 4_565 ?
O13 Ni2 N11 O11 -89.41(13) . . . 4_565 ?
N13 Ni2 N11 O11 175.24(13) . . . . ?
N13 Ni2 N11 O11 3.57(13) 4_565 . . . ?
O14 Ni2 N11 O11 89.41(13) . . . . ?
N14 Ni2 N11 O11 -90.59(13) . . . . ?
O13 Ni2 N11 O11 89.41(13) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 H5C O3 0.92 2.19 3.0132(16) 148.2 3_557
N5 H5D O11 0.92 2.19 3.0588(16) 156.8 4_565
N13 H13D O11 0.92 2.16 2.8225(18) 127.7 4_565

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.065

_database_code_depnum_ccdc_archive 'CCDC 994149'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex7_150K
_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;
Dinitro-(3,3-diamino-N-methyldipropylamine)nickel(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H19 N5 Ni O4'
_chemical_formula_sum            'C7 H19 N5 Ni O4'
_chemical_formula_weight         295.98

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'
O O 0.0106 0.0060 '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'


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

_cell_length_a                   7.146(5)
_cell_length_b                   23.684(5)
_cell_length_c                   10.944(5)
_cell_angle_alpha                90.000
_cell_angle_beta                 103.455(5)
_cell_angle_gamma                90.000
_cell_volume                     1801.4(16)
_cell_formula_units_Z            6
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6451
_cell_measurement_theta_min      2.9252
_cell_measurement_theta_max      30.4392

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/m

_exptl_crystal_description       Block
_exptl_crystal_colour            Violet
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936

_exptl_absorpt_coefficient_mu    1.629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.80464
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13177
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.93
_diffrn_reflns_theta_max         30.51
_reflns_number_total             5626
_reflns_number_gt                4834
_reflns_threshold_expression     >2sigma(I)


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'POV-RAY for Windows, 3.62 (Cason, 2009)'
_computing_publication_material  'WinGX, 1.80.05 (Farrugia, 1999)'


_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 > 2sigma(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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0289P)²+0.4008P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5626
_refine_ls_number_parameters     242
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0252
_refine_ls_wR_factor_ref         0.0624
_refine_ls_wR_factor_gt          0.0585
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.28150(19) 0.01868(6) 0.61648(12) 0.0208(3) Uani 1 1 d . . .
H1A H 0.1630 -0.0027 0.5790 0.025 Uiso 1 1 calc R . .
H1B H 0.3912 -0.0007 0.5934 0.025 Uiso 1 1 calc R . .
C2 C 0.2644(2) 0.07795(6) 0.56400(13) 0.0231(3) Uani 1 1 d . . .
H2A H 0.2727 0.0763 0.4750 0.028 Uiso 1 1 calc R . .
H2B H 0.3752 0.1004 0.6104 0.028 Uiso 1 1 calc R . .
C3 C 0.0797(2) 0.10833(6) 0.57105(12) 0.0230(3) Uani 1 1 d . . .
H3A H 0.0690 0.1426 0.5182 0.028 Uiso 1 1 calc R . .
H3B H -0.0299 0.0835 0.5330 0.028 Uiso 1 1 calc R . .
C4 C -0.1399(2) 0.15060(6) 0.67534(12) 0.0230(3) Uani 1 1 d . . .
H4A H -0.2328 0.1221 0.6315 0.028 Uiso 1 1 calc R . .
H4B H -0.1455 0.1830 0.6175 0.028 Uiso 1 1 calc R . .
C5 C -0.2066(2) 0.17074(6) 0.78975(14) 0.0245(3) Uani 1 1 d . . .
H5A H -0.1070 0.1960 0.8396 0.029 Uiso 1 1 calc R . .
H5B H -0.3255 0.1932 0.7612 0.029 Uiso 1 1 calc R . .
C6 C -0.24593(19) 0.12363(6) 0.87397(14) 0.0238(3) Uani 1 1 d . . .
H6A H -0.3105 0.1393 0.9373 0.029 Uiso 1 1 calc R . .
H6B H -0.3334 0.0956 0.8230 0.029 Uiso 1 1 calc R . .
C7 C 0.2013(2) 0.16968(6) 0.74825(13) 0.0236(3) Uani 1 1 d . . .
H7A H 0.3309 0.1537 0.7607 0.035 Uiso 1 1 calc R . .
H7B H 0.1813 0.1834 0.8288 0.035 Uiso 1 1 calc R . .
H7C H 0.1871 0.2011 0.6886 0.035 Uiso 1 1 calc R . .
C11 C 0.5302(2) 0.12731(6) 1.31875(13) 0.0226(3) Uani 1 1 d . . .
H11A H 0.4932 0.0871 1.3055 0.027 Uiso 1 1 calc R . .
H11B H 0.5885 0.1329 1.4093 0.027 Uiso 1 1 calc R . .
C12 C 0.6752(2) 0.14199(6) 1.24314(14) 0.0254(3) Uani 1 1 d . . .
H12A H 0.6112 0.1396 1.1528 0.031 Uiso 1 1 calc R . .
H12B H 0.7789 0.1133 1.2602 0.031 Uiso 1 1 calc R . .
C13 C 0.76588(19) 0.20003(6) 1.26944(13) 0.0221(3) Uani 1 1 d . . .
H13A H 0.8111 0.2043 1.3616 0.027 Uiso 1 1 calc R . .
H13B H 0.8809 0.2013 1.2336 0.027 Uiso 1 1 calc R . .
C17 C 0.6013(3) 0.2500 1.08151(17) 0.0249(4) Uani 1 2 d S . .
H17A H 0.5255 0.2835 1.0491 0.037 Uiso 0.50 1 calc PR . .
H17B H 0.5283 0.2160 1.0492 0.037 Uiso 0.50 1 calc PR . .
H17C H 0.7225 0.2505 1.0542 0.037 Uiso 1 2 calc SR . .
N2 N 0.36369(18) 0.05091(5) 1.04523(11) 0.0246(2) Uani 1 1 d . . .
N3 N 0.31083(15) 0.01915(5) 0.75464(10) 0.0188(2) Uani 1 1 d . . .
H3C H 0.4285 0.0355 0.7876 0.023 Uiso 1 1 calc R . .
H3D H 0.3185 -0.0178 0.7815 0.023 Uiso 1 1 calc R . .
N4 N 0.05708(15) 0.12561(4) 0.69803(10) 0.0173(2) Uani 1 1 d . . .
N5 N -0.06618(16) 0.09554(5) 0.93808(10) 0.0198(2) Uani 1 1 d . . .
H5C H -0.0980 0.0676 0.9879 0.024 Uiso 1 1 calc R . .
H5D H 0.0065 0.1216 0.9910 0.024 Uiso 1 1 calc R . .
N12 N 0.3810(3) 0.2500 1.52099(18) 0.0359(4) Uani 1 2 d S . .
N13 N 0.35796(17) 0.16311(5) 1.28078(12) 0.0238(2) Uani 1 1 d . . .
H13C H 0.2759 0.1537 1.3311 0.029 Uiso 1 1 calc R . .
H13D H 0.2975 0.1532 1.2000 0.029 Uiso 1 1 calc R . .
N14 N 0.6429(2) 0.2500 1.22069(14) 0.0158(3) Uani 1 2 d S . .
O3 O 0.24274(15) 0.01313(4) 0.99852(9) 0.0239(2) Uani 1 1 d . . .
O4 O 0.34744(14) 0.09440(4) 0.97649(9) 0.0230(2) Uani 1 1 d . . .
O13 O 0.2267(2) 0.2500 1.43619(15) 0.0327(3) Uani 1 2 d S . .
O14 O 0.5296(2) 0.2500 1.47629(13) 0.0267(3) Uani 1 2 d S . .
Ni1 Ni 0.10882(2) 0.059718(6) 0.833062(14) 0.01453(5) Uani 1 1 d . . .
Ni2 Ni 0.38704(3) 0.2500 1.28547(2) 0.01441(5) Uani 1 2 d S . .
N1 N -0.09302(16) 0.00151(5) 0.74657(10) 0.0198(2) Uani 1 1 d . . .
O1 O -0.25642(15) 0.01377(4) 0.68408(10) 0.0293(2) Uani 1 1 d . . .
O2 O -0.04863(16) -0.04964(4) 0.75928(11) 0.0295(2) Uani 1 1 d . . .
N11 N 0.1785(2) 0.2500 1.11185(14) 0.0181(3) Uani 1 2 d S . .
O11 O 0.11311(18) 0.29435(5) 1.05931(11) 0.0388(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N3 1.4774(17) . ?
C1 C2 1.5108(19) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.521(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N4 1.4930(18) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.4933(19) . ?
C4 C5 1.517(2) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.515(2) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N5 1.4714(19) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 N4 1.4798(17) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C11 N13 1.4726(18) . ?
C11 C12 1.510(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.518(2) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N14 1.4966(16) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C17 N14 1.483(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
N2 O4 1.2646(15) . ?
N2 O3 1.2664(16) . ?
N3 Ni1 2.0785(14) . ?
N3 H3C 0.9200 . ?
N3 H3D 0.9200 . ?
N4 Ni1 2.1216(12) . ?
N5 Ni1 2.0672(13) . ?
N5 H5C 0.9200 . ?
N5 H5D 0.9200 . ?
N12 O13 1.265(3) . ?
N12 O14 1.268(2) . ?
N13 Ni2 2.0678(12) . ?
N13 H13C 0.9200 . ?
N13 H13D 0.9200 . ?
N14 C13 1.4966(16) 4_565 ?
N14 Ni2 2.1091(19) . ?
O3 Ni1 2.1462(12) . ?
O4 Ni1 2.1910(13) . ?
O13 Ni2 2.2166(17) . ?
O14 Ni2 2.0997(16) . ?
Ni1 N1 2.0595(13) . ?
Ni2 N13 2.0678(12) 4_565 ?
Ni2 N11 2.1246(18) . ?
N1 O1 1.2425(16) . ?
N1 O2 1.2519(15) . ?
N11 O11 1.2358(13) 4_565 ?
N11 O11 1.2358(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 C1 C2 111.21(11) . . ?
N3 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N3 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
C1 C2 C3 114.48(12) . . ?
C1 C2 H2A 108.6 . . ?
C3 C2 H2A 108.6 . . ?
C1 C2 H2B 108.6 . . ?
C3 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
N4 C3 C2 117.38(11) . . ?
N4 C3 H3A 108.0 . . ?
C2 C3 H3A 108.0 . . ?
N4 C3 H3B 108.0 . . ?
C2 C3 H3B 108.0 . . ?
H3A C3 H3B 107.2 . . ?
N4 C4 C5 116.91(11) . . ?
N4 C4 H4A 108.1 . . ?
C5 C4 H4A 108.1 . . ?
N4 C4 H4B 108.1 . . ?
C5 C4 H4B 108.1 . . ?
H4A C4 H4B 107.3 . . ?
C6 C5 C4 114.15(12) . . ?
C6 C5 H5A 108.7 . . ?
C4 C5 H5A 108.7 . . ?
C6 C5 H5B 108.7 . . ?
C4 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
N5 C6 C5 110.98(11) . . ?
N5 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
N5 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N13 C11 C12 110.37(12) . . ?
N13 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
N13 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
C11 C12 C13 114.94(12) . . ?
C11 C12 H12A 108.5 . . ?
C13 C12 H12A 108.5 . . ?
C11 C12 H12B 108.5 . . ?
C13 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?
N14 C13 C12 117.33(12) . . ?
N14 C13 H13A 108.0 . . ?
C12 C13 H13A 108.0 . . ?
N14 C13 H13B 108.0 . . ?
C12 C13 H13B 108.0 . . ?
H13A C13 H13B 107.2 . . ?
N14 C17 H17A 109.5 . . ?
N14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O4 N2 O3 112.07(11) . . ?
C1 N3 Ni1 118.64(8) . . ?
C1 N3 H3C 107.7 . . ?
Ni1 N3 H3C 107.7 . . ?
C1 N3 H3D 107.7 . . ?
Ni1 N3 H3D 107.7 . . ?
H3C N3 H3D 107.1 . . ?
C7 N4 C3 108.80(11) . . ?
C7 N4 C4 109.27(11) . . ?
C3 N4 C4 104.81(10) . . ?
C7 N4 Ni1 105.47(8) . . ?
C3 N4 Ni1 114.06(8) . . ?
C4 N4 Ni1 114.34(8) . . ?
C6 N5 Ni1 119.63(9) . . ?
C6 N5 H5C 107.4 . . ?
Ni1 N5 H5C 107.4 . . ?
C6 N5 H5D 107.4 . . ?
Ni1 N5 H5D 107.4 . . ?
H5C N5 H5D 106.9 . . ?
O13 N12 O14 112.46(17) . . ?
C11 N13 Ni2 119.57(9) . . ?
C11 N13 H13C 107.4 . . ?
Ni2 N13 H13C 107.4 . . ?
C11 N13 H13D 107.4 . . ?
Ni2 N13 H13D 107.4 . . ?
H13C N13 H13D 107.0 . . ?
C17 N14 C13 109.09(10) . 4_565 ?
C17 N14 C13 109.09(9) . . ?
C13 N14 C13 104.53(14) 4_565 . ?
C17 N14 Ni2 111.28(11) . . ?
C13 N14 Ni2 111.30(8) 4_565 . ?
C13 N14 Ni2 111.30(8) . . ?
N2 O3 Ni1 96.07(8) . . ?
N2 O4 Ni1 93.98(8) . . ?
N12 O13 Ni2 91.86(12) . . ?
N12 O14 Ni2 97.33(13) . . ?
N1 Ni1 N5 94.63(6) . . ?
N1 Ni1 N3 88.87(6) . . ?
N5 Ni1 N3 170.90(4) . . ?
N1 Ni1 N4 100.50(5) . . ?
N5 Ni1 N4 93.18(5) . . ?
N3 Ni1 N4 94.45(5) . . ?
N1 Ni1 O3 99.83(5) . . ?
N5 Ni1 O3 87.17(5) . . ?
N3 Ni1 O3 83.95(5) . . ?
N4 Ni1 O3 159.57(4) . . ?
N1 Ni1 O4 157.71(4) . . ?
N5 Ni1 O4 85.32(6) . . ?
N3 Ni1 O4 88.26(6) . . ?
N4 Ni1 O4 101.76(4) . . ?
O3 Ni1 O4 57.88(4) . . ?
N13 Ni2 N13 168.78(7) . 4_565 ?
N13 Ni2 O14 92.72(4) . . ?
N13 Ni2 O14 92.72(4) 4_565 . ?
N13 Ni2 N14 94.68(3) . . ?
N13 Ni2 N14 94.68(3) 4_565 . ?
O14 Ni2 N14 94.38(7) . . ?
N13 Ni2 N11 86.12(4) . . ?
N13 Ni2 N11 86.12(4) 4_565 . ?
O14 Ni2 N11 165.14(6) . . ?
N14 Ni2 N11 100.48(7) . . ?
N13 Ni2 O13 87.25(4) . . ?
N13 Ni2 O13 87.25(4) 4_565 . ?
O14 Ni2 O13 58.34(7) . . ?
N14 Ni2 O13 152.72(6) . . ?
N11 Ni2 O13 106.80(8) . . ?
O1 N1 O2 117.95(11) . . ?
O1 N1 Ni1 124.36(9) . . ?
O2 N1 Ni1 117.68(9) . . ?
O11 N11 O11 116.42(16) 4_565 . ?
O11 N11 Ni2 121.78(8) 4_565 . ?
O11 N11 Ni2 121.78(8) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 C1 C2 C3 -70.21(15) . . . . ?
C1 C2 C3 N4 70.24(16) . . . . ?
N4 C4 C5 C6 -70.09(16) . . . . ?
C4 C5 C6 N5 69.22(15) . . . . ?
N13 C11 C12 C13 67.68(16) . . . . ?
C11 C12 C13 N14 -72.88(17) . . . . ?
C2 C1 N3 Ni1 56.77(13) . . . . ?
C2 C3 N4 C7 66.64(15) . . . . ?
C2 C3 N4 C4 -176.58(12) . . . . ?
C2 C3 N4 Ni1 -50.78(14) . . . . ?
C5 C4 N4 C7 -65.25(15) . . . . ?
C5 C4 N4 C3 178.28(12) . . . . ?
C5 C4 N4 Ni1 52.66(14) . . . . ?
C5 C6 N5 Ni1 -57.60(14) . . . . ?
C12 C11 N13 Ni2 -55.21(14) . . . . ?
C12 C13 N14 C17 -67.61(16) . . . . ?
C12 C13 N14 C13 175.82(8) . . . 4_565 ?
C12 C13 N14 Ni2 55.56(14) . . . . ?
O4 N2 O3 Ni1 0.00(11) . . . . ?
O3 N2 O4 Ni1 0.00(11) . . . . ?
O14 N12 O13 Ni2 0.000(1) . . . . ?
O13 N12 O14 Ni2 0.000(1) . . . . ?
C6 N5 Ni1 N1 -62.74(10) . . . . ?
C6 N5 Ni1 N3 -175.1(2) . . . . ?
C6 N5 Ni1 N4 38.07(10) . . . . ?
C6 N5 Ni1 O3 -162.39(10) . . . . ?
C6 N5 Ni1 O4 139.62(10) . . . . ?
C1 N3 Ni1 N1 64.10(10) . . . . ?
C1 N3 Ni1 N5 176.8(2) . . . . ?
C1 N3 Ni1 N4 -36.35(10) . . . . ?
C1 N3 Ni1 O3 164.11(10) . . . . ?
C1 N3 Ni1 O4 -138.01(10) . . . . ?
C7 N4 Ni1 N1 -177.78(8) . . . . ?
C3 N4 Ni1 N1 -58.45(10) . . . . ?
C4 N4 Ni1 N1 62.16(10) . . . . ?
C7 N4 Ni1 N5 86.91(9) . . . . ?
C3 N4 Ni1 N5 -153.76(9) . . . . ?
C4 N4 Ni1 N5 -33.15(9) . . . . ?
C7 N4 Ni1 N3 -88.11(10) . . . . ?
C3 N4 Ni1 N3 31.22(9) . . . . ?
C4 N4 Ni1 N3 151.83(9) . . . . ?
C7 N4 Ni1 O3 -3.51(16) . . . . ?
C3 N4 Ni1 O3 115.82(13) . . . . ?
C4 N4 Ni1 O3 -123.57(12) . . . . ?
C7 N4 Ni1 O4 1.03(9) . . . . ?
C3 N4 Ni1 O4 120.36(9) . . . . ?
C4 N4 Ni1 O4 -119.03(9) . . . . ?
N2 O3 Ni1 N1 179.53(8) . . . . ?
N2 O3 Ni1 N5 -86.25(9) . . . . ?
N2 O3 Ni1 N3 91.75(9) . . . . ?
N2 O3 Ni1 N4 5.25(16) . . . . ?
N2 O3 Ni1 O4 0.00(7) . . . . ?
N2 O4 Ni1 N1 -1.21(15) . . . . ?
N2 O4 Ni1 N5 89.59(8) . . . . ?
N2 O4 Ni1 N3 -83.95(8) . . . . ?
N2 O4 Ni1 N4 -178.13(7) . . . . ?
N2 O4 Ni1 O3 0.00(7) . . . . ?
C11 N13 Ni2 N13 -175.0(3) . . . 4_565 ?
C11 N13 Ni2 O14 -56.12(11) . . . . ?
C11 N13 Ni2 N14 38.50(11) . . . . ?
C11 N13 Ni2 N11 138.72(11) . . . . ?
C11 N13 Ni2 O13 -114.23(11) . . . . ?
N12 O14 Ni2 N13 -85.09(3) . . . . ?
N12 O14 Ni2 N13 85.09(3) . . . 4_565 ?
N12 O14 Ni2 N14 180.0 . . . . ?
N12 O14 Ni2 N11 0.000(2) . . . . ?
N12 O14 Ni2 O13 0.0 . . . . ?
C17 N14 Ni2 N13 86.91(4) . . . . ?
C13 N14 Ni2 N13 -151.18(9) 4_565 . . . ?
C13 N14 Ni2 N13 -35.01(10) . . . . ?
C17 N14 Ni2 N13 -86.91(4) . . . 4_565 ?
C13 N14 Ni2 N13 35.01(9) 4_565 . . 4_565 ?
C13 N14 Ni2 N13 151.18(9) . . . 4_565 ?
C17 N14 Ni2 O14 180.0 . . . . ?
C13 N14 Ni2 O14 -58.09(9) 4_565 . . . ?
C13 N14 Ni2 O14 58.09(9) . . . . ?
C17 N14 Ni2 N11 0.0 . . . . ?
C13 N14 Ni2 N11 121.91(9) 4_565 . . . ?
C13 N14 Ni2 N11 -121.91(9) . . . . ?
C17 N14 Ni2 O13 180.000(1) . . . . ?
C13 N14 Ni2 O13 -58.09(9) 4_565 . . . ?
C13 N14 Ni2 O13 58.09(9) . . . . ?
N12 O13 Ni2 N13 94.89(3) . . . . ?
N12 O13 Ni2 N13 -94.89(3) . . . 4_565 ?
N12 O13 Ni2 O14 0.000(1) . . . . ?
N12 O13 Ni2 N14 0.000(1) . . . . ?
N12 O13 Ni2 N11 180.000(1) . . . . ?
N5 Ni1 N1 O1 57.00(11) . . . . ?
N3 Ni1 N1 O1 -131.42(11) . . . . ?
N4 Ni1 N1 O1 -37.11(11) . . . . ?
O3 Ni1 N1 O1 144.92(10) . . . . ?
O4 Ni1 N1 O1 145.96(11) . . . . ?
N5 Ni1 N1 O2 -122.05(10) . . . . ?
N3 Ni1 N1 O2 49.53(10) . . . . ?
N4 Ni1 N1 O2 143.85(10) . . . . ?
O3 Ni1 N1 O2 -34.12(10) . . . . ?
O4 Ni1 N1 O2 -33.08(17) . . . . ?
N13 Ni2 N11 O11 -3.28(13) . . . 4_565 ?
N13 Ni2 N11 O11 -175.18(14) 4_565 . . 4_565 ?
O14 Ni2 N11 O11 -89.23(13) . . . 4_565 ?
N14 Ni2 N11 O11 90.77(13) . . . 4_565 ?
O13 Ni2 N11 O11 -89.23(13) . . . 4_565 ?
N13 Ni2 N11 O11 175.18(14) . . . . ?
N13 Ni2 N11 O11 3.28(13) 4_565 . . . ?
O14 Ni2 N11 O11 89.23(13) . . . . ?
N14 Ni2 N11 O11 -90.77(13) . . . . ?
O13 Ni2 N11 O11 89.23(13) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 H5C O3 0.92 2.19 3.0174(16) 148.5 3_557
N5 H5D O11 0.92 2.20 3.0677(16) 157.2 4_565
N13 H13D O11 0.92 2.17 2.8245(19) 127.5 4_565

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.061

_database_code_depnum_ccdc_archive 'CCDC 994150'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex7_200K
_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;
Dinitro-(3,3-diamino-N-methyldipropylamine)nickel(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H19 N5 Ni O4'
_chemical_formula_sum            'C7 H19 N5 Ni O4'
_chemical_formula_weight         295.98

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'
O O 0.0106 0.0060 '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'


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

_cell_length_a                   7.170(5)
_cell_length_b                   23.690(5)
_cell_length_c                   10.982(5)
_cell_angle_alpha                90.000
_cell_angle_beta                 103.569(5)
_cell_angle_gamma                90.000
_cell_volume                     1813.3(16)
_cell_formula_units_Z            6
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    6788
_cell_measurement_theta_min      2.9167
_cell_measurement_theta_max      30.4391

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/m

_exptl_crystal_description       Block
_exptl_crystal_colour            Violet
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936

_exptl_absorpt_coefficient_mu    1.618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.77669
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13287
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.92
_diffrn_reflns_theta_max         30.51
_reflns_number_total             5666
_reflns_number_gt                4791
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'POV-RAY for Windows, 3.62 (Cason, 2009)'
_computing_publication_material  'WinGX, 1.80.05 (Farrugia, 1999)'


_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 > 2sigma(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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0268P)²+0.2824P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5666
_refine_ls_number_parameters     254
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0249
_refine_ls_wR_factor_ref         0.0614
_refine_ls_wR_factor_gt          0.0569
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2829(2) 0.01927(6) 0.61770(12) 0.0277(3) Uani 1 1 d . . .
H1A H 0.1654 -0.0022 0.5795 0.033 Uiso 1 1 calc R . .
H1B H 0.3931 0.0002 0.5953 0.033 Uiso 1 1 calc R . .
C2 C 0.2654(2) 0.07844(6) 0.56595(13) 0.0308(3) Uani 1 1 d . . .
H2A H 0.2747 0.0770 0.4775 0.037 Uiso 1 1 calc R . .
H2B H 0.3752 0.1010 0.6129 0.037 Uiso 1 1 calc R . .
C3 C 0.0805(2) 0.10847(6) 0.57205(12) 0.0297(3) Uani 1 1 d . . .
H3A H 0.0694 0.1427 0.5192 0.036 Uiso 1 1 calc R . .
H3B H -0.0281 0.0834 0.5340 0.036 Uiso 1 1 calc R . .
C4 C -0.1392(2) 0.15057(6) 0.67528(13) 0.0303(3) Uani 1 1 d . . .
H4A H -0.2315 0.1220 0.6313 0.036 Uiso 1 1 calc R . .
H4B H -0.1448 0.1830 0.6177 0.036 Uiso 1 1 calc R . .
C5 C -0.2065(2) 0.17058(6) 0.78927(14) 0.0322(3) Uani 1 1 d . . .
H5A H -0.1079 0.1960 0.8392 0.039 Uiso 1 1 calc R . .
H5B H -0.3256 0.1929 0.7606 0.039 Uiso 1 1 calc R . .
C6 C -0.2448(2) 0.12341(6) 0.87272(14) 0.0315(3) Uani 1 1 d . . .
H6A H -0.3097 0.1389 0.9357 0.038 Uiso 1 1 calc R . .
H6B H -0.3317 0.0954 0.8216 0.038 Uiso 1 1 calc R . .
C7 C 0.2008(2) 0.16987(6) 0.74897(14) 0.0303(3) Uani 1 1 d . . .
H7A H 0.3301 0.1539 0.7622 0.045 Uiso 1 1 calc R . .
H7B H 0.1799 0.1837 0.8288 0.045 Uiso 1 1 calc R . .
H7C H 0.1872 0.2012 0.6893 0.045 Uiso 1 1 calc R . .
C11 C 0.5293(2) 0.12746(6) 1.31830(14) 0.0298(3) Uani 1 1 d . . .
H11A H 0.4925 0.0873 1.3051 0.036 Uiso 1 1 calc R . .
H11B H 0.5873 0.1331 1.4086 0.036 Uiso 1 1 calc R . .
C12 C 0.6740(2) 0.14210(6) 1.24331(15) 0.0335(3) Uani 1 1 d . . .
H12A H 0.6103 0.1397 1.1531 0.040 Uiso 1 1 calc R . .
H12B H 0.7774 0.1134 1.2605 0.040 Uiso 1 1 calc R . .
C13 C 0.76425(19) 0.20007(6) 1.26957(14) 0.0283(3) Uani 1 1 d . . .
H13A H 0.8090 0.2044 1.3615 0.034 Uiso 1 1 calc R . .
H13B H 0.8791 0.2013 1.2342 0.034 Uiso 1 1 calc R . .
C17 C 0.6001(3) 0.2500 1.08226(18) 0.0330(4) Uani 1 2 d S . .
H17A H 0.5244 0.2835 1.0499 0.050 Uiso 0.50 1 calc PR . .
H17B H 0.5274 0.2160 1.0500 0.050 Uiso 0.50 1 calc PR . .
H17C H 0.7209 0.2505 1.0551 0.050 Uiso 1 2 calc SR . .
N2 N 0.36248(18) 0.05059(6) 1.04479(11) 0.0326(3) Uani 1 1 d . . .
N3 N 0.31050(16) 0.01946(5) 0.75499(10) 0.0246(2) Uani 1 1 d . A .
H3C H 0.4278 0.0357 0.7886 0.030 Uiso 1 1 calc R . .
H3D H 0.3178 -0.0175 0.7813 0.030 Uiso 1 1 calc R . .
N4 N 0.05757(16) 0.12575(4) 0.69854(10) 0.0222(2) Uani 1 1 d . A .
N5 N -0.06605(16) 0.09538(5) 0.93709(11) 0.0256(2) Uani 1 1 d . A .
H5C H -0.0980 0.0674 0.9865 0.031 Uiso 1 1 calc R . .
H5D H 0.0063 0.1214 0.9901 0.031 Uiso 1 1 calc R . .
N12 N 0.3798(3) 0.2500 1.51952(18) 0.0454(5) Uani 1 2 d S . .
N13 N 0.35789(17) 0.16314(5) 1.28011(12) 0.0304(3) Uani 1 1 d . . .
H13C H 0.2759 0.1537 1.3300 0.036 Uiso 1 1 calc R . .
H13D H 0.2978 0.1532 1.1994 0.036 Uiso 1 1 calc R . .
N14 N 0.6415(2) 0.2500 1.22048(14) 0.0210(3) Uani 1 2 d S . .
O3 O 0.24149(15) 0.01306(4) 0.99756(9) 0.0315(2) Uani 1 1 d . A .
O4 O 0.34701(14) 0.09404(4) 0.97688(9) 0.0299(2) Uani 1 1 d . A .
O13 O 0.2264(2) 0.2500 1.43469(16) 0.0421(4) Uani 1 2 d S . .
O14 O 0.5278(2) 0.2500 1.47570(13) 0.0347(3) Uani 1 2 d S . .
Ni1 Ni 0.10854(2) 0.059752(6) 0.832637(14) 0.01888(5) Uani 1 1 d . . .
Ni2 Ni 0.38653(3) 0.2500 1.28482(2) 0.01865(6) Uani 1 2 d S . .
N1 N -0.09197(19) 0.00151(6) 0.74597(12) 0.0249(3) Uani 0.961(4) 1 d PD A 1
O1 O -0.25468(19) 0.01339(5) 0.68374(11) 0.0385(4) Uani 0.961(4) 1 d PD A 1
O2 O -0.0484(3) -0.04985(10) 0.7579(2) 0.0394(5) Uani 0.961(4) 1 d PD A 1
N1A N -0.171(4) -0.0328(10) 0.711(3) 0.028(8) Uiso 0.039(4) 1 d PD A 2
O1A O -0.149(4) 0.0218(9) 0.708(2) 0.013(5) Uiso 0.039(4) 1 d PD A 2
O2A O -0.015(6) -0.052(2) 0.784(4) 0.013(5) Uiso 0.039(4) 1 d PD A 2
N11 N 0.1778(2) 0.2500 1.11182(14) 0.0230(3) Uani 1 2 d S . .
O11 O 0.11181(18) 0.29423(5) 1.06009(12) 0.0502(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N3 1.4739(18) . ?
C1 C2 1.507(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.520(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N4 1.4938(18) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.4940(19) . ?
C4 C5 1.519(2) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.511(2) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N5 1.4692(19) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 N4 1.4789(17) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C11 N13 1.4695(19) . ?
C11 C12 1.509(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.516(2) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N14 1.4972(16) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C17 N14 1.477(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
N2 O4 1.2606(16) . ?
N2 O3 1.2653(17) . ?
N3 Ni1 2.0772(14) . ?
N3 H3C 0.9200 . ?
N3 H3D 0.9200 . ?
N4 Ni1 2.1199(12) . ?
N5 Ni1 2.0662(13) . ?
N5 H5C 0.9200 . ?
N5 H5D 0.9200 . ?
N12 O13 1.263(3) . ?
N12 O14 1.264(3) . ?
N13 Ni2 2.0675(12) . ?
N13 H13C 0.9200 . ?
N13 H13D 0.9200 . ?
N14 C13 1.4972(16) 4_565 ?
N14 Ni2 2.1092(19) . ?
O3 Ni1 2.1454(12) . ?
O4 Ni1 2.1959(13) . ?
O13 Ni2 2.2165(17) . ?
O14 Ni2 2.1034(17) . ?
Ni1 N1 2.0577(14) . ?
Ni1 O1A 2.22(3) . ?
Ni2 N13 2.0675(12) 4_565 ?
Ni2 N11 2.1251(18) . ?
N1 O1 1.238(2) . ?
N1 O2 1.256(3) . ?
N1A O2A 1.292(19) . ?
N1A O1A 1.304(18) . ?
N11 O11 1.2321(13) 4_565 ?
N11 O11 1.2321(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 C1 C2 111.25(11) . . ?
N3 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N3 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
C1 C2 C3 114.52(12) . . ?
C1 C2 H2A 108.6 . . ?
C3 C2 H2A 108.6 . . ?
C1 C2 H2B 108.6 . . ?
C3 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
N4 C3 C2 117.18(11) . . ?
N4 C3 H3A 108.0 . . ?
C2 C3 H3A 108.0 . . ?
N4 C3 H3B 108.0 . . ?
C2 C3 H3B 108.0 . . ?
H3A C3 H3B 107.2 . . ?
N4 C4 C5 116.86(11) . . ?
N4 C4 H4A 108.1 . . ?
C5 C4 H4A 108.1 . . ?
N4 C4 H4B 108.1 . . ?
C5 C4 H4B 108.1 . . ?
H4A C4 H4B 107.3 . . ?
C6 C5 C4 114.03(12) . . ?
C6 C5 H5A 108.7 . . ?
C4 C5 H5A 108.7 . . ?
C6 C5 H5B 108.7 . . ?
C4 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
N5 C6 C5 111.35(12) . . ?
N5 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
N5 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N13 C11 C12 110.39(12) . . ?
N13 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
N13 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
C11 C12 C13 114.94(12) . . ?
C11 C12 H12A 108.5 . . ?
C13 C12 H12A 108.5 . . ?
C11 C12 H12B 108.5 . . ?
C13 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?
N14 C13 C12 117.29(12) . . ?
N14 C13 H13A 108.0 . . ?
C12 C13 H13A 108.0 . . ?
N14 C13 H13B 108.0 . . ?
C12 C13 H13B 108.0 . . ?
H13A C13 H13B 107.2 . . ?
N14 C17 H17A 109.5 . . ?
N14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O4 N2 O3 112.00(11) . . ?
C1 N3 Ni1 118.83(8) . . ?
C1 N3 H3C 107.6 . . ?
Ni1 N3 H3C 107.6 . . ?
C1 N3 H3D 107.6 . . ?
Ni1 N3 H3D 107.6 . . ?
H3C N3 H3D 107.0 . . ?
C7 N4 C3 108.88(11) . . ?
C7 N4 C4 109.30(11) . . ?
C3 N4 C4 104.75(10) . . ?
C7 N4 Ni1 105.65(8) . . ?
C3 N4 Ni1 113.91(8) . . ?
C4 N4 Ni1 114.27(8) . . ?
C6 N5 Ni1 119.43(10) . . ?
C6 N5 H5C 107.5 . . ?
Ni1 N5 H5C 107.5 . . ?
C6 N5 H5D 107.5 . . ?
Ni1 N5 H5D 107.5 . . ?
H5C N5 H5D 107.0 . . ?
O13 N12 O14 112.49(17) . . ?
C11 N13 Ni2 119.59(9) . . ?
C11 N13 H13C 107.4 . . ?
Ni2 N13 H13C 107.4 . . ?
C11 N13 H13D 107.4 . . ?
Ni2 N13 H13D 107.4 . . ?
H13C N13 H13D 107.0 . . ?
C17 N14 C13 109.25(10) . 4_565 ?
C17 N14 C13 109.25(10) . . ?
C13 N14 C13 104.39(14) 4_565 . ?
C17 N14 Ni2 111.29(12) . . ?
C13 N14 Ni2 111.21(9) 4_565 . ?
C13 N14 Ni2 111.21(9) . . ?
N2 O3 Ni1 96.30(8) . . ?
N2 O4 Ni1 94.03(8) . . ?
N12 O13 Ni2 92.00(13) . . ?
N12 O14 Ni2 97.36(13) . . ?
N1 Ni1 N5 94.71(6) . . ?
N1 Ni1 N3 88.89(6) . . ?
N5 Ni1 N3 170.81(4) . . ?
N1 Ni1 N4 100.68(5) . . ?
N5 Ni1 N4 93.23(5) . . ?
N3 Ni1 N4 94.41(5) . . ?
N1 Ni1 O3 99.71(5) . . ?
N5 Ni1 O3 87.07(5) . . ?
N3 Ni1 O3 83.98(5) . . ?
N4 Ni1 O3 159.52(4) . . ?
N1 Ni1 O4 157.37(5) . . ?
N5 Ni1 O4 85.36(6) . . ?
N3 Ni1 O4 88.07(6) . . ?
N4 Ni1 O4 101.92(4) . . ?
O3 Ni1 O4 57.67(4) . . ?
N1 Ni1 O1A 18.4(6) . . ?
N5 Ni1 O1A 89.0(6) . . ?
N3 Ni1 O1A 96.9(6) . . ?
N4 Ni1 O1A 83.5(6) . . ?
O3 Ni1 O1A 116.9(6) . . ?
O4 Ni1 O1A 172.3(6) . . ?
N13 Ni2 N13 168.92(7) . 4_565 ?
N13 Ni2 O14 92.68(4) . . ?
N13 Ni2 O14 92.68(4) 4_565 . ?
N13 Ni2 N14 94.61(4) . . ?
N13 Ni2 N14 94.61(4) 4_565 . ?
O14 Ni2 N14 94.66(7) . . ?
N13 Ni2 N11 86.14(4) . . ?
N13 Ni2 N11 86.14(4) 4_565 . ?
O14 Ni2 N11 164.70(6) . . ?
N14 Ni2 N11 100.64(7) . . ?
N13 Ni2 O13 87.30(4) . . ?
N13 Ni2 O13 87.30(4) 4_565 . ?
O14 Ni2 O13 58.14(7) . . ?
N14 Ni2 O13 152.80(6) . . ?
N11 Ni2 O13 106.56(8) . . ?
O1 N1 O2 117.20(14) . . ?
O1 N1 Ni1 124.64(11) . . ?
O2 N1 Ni1 118.15(13) . . ?
O2A N1A O1A 106(4) . . ?
N1A O1A Ni1 118(2) . . ?
O11 N11 O11 116.51(17) 4_565 . ?
O11 N11 Ni2 121.72(8) 4_565 . ?
O11 N11 Ni2 121.72(8) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 C1 C2 C3 -70.15(16) . . . . ?
C1 C2 C3 N4 70.67(17) . . . . ?
N4 C4 C5 C6 -69.88(17) . . . . ?
C4 C5 C6 N5 69.15(16) . . . . ?
N13 C11 C12 C13 67.70(16) . . . . ?
C11 C12 C13 N14 -72.94(18) . . . . ?
C2 C1 N3 Ni1 56.41(14) . . . . ?
C2 C3 N4 C7 66.42(15) . . . . ?
C2 C3 N4 C4 -176.76(12) . . . . ?
C2 C3 N4 Ni1 -51.20(15) . . . . ?
C5 C4 N4 C7 -65.33(15) . . . . ?
C5 C4 N4 C3 178.13(12) . . . . ?
C5 C4 N4 Ni1 52.80(15) . . . . ?
C5 C6 N5 Ni1 -57.70(14) . . . . ?
C12 C11 N13 Ni2 -55.28(15) . . . . ?
C12 C13 N14 C17 -67.53(16) . . . . ?
C12 C13 N14 C13 175.72(8) . . . 4_565 ?
C12 C13 N14 Ni2 55.71(15) . . . . ?
O4 N2 O3 Ni1 0.05(12) . . . . ?
O3 N2 O4 Ni1 -0.05(11) . . . . ?
O14 N12 O13 Ni2 0.000(1) . . . . ?
O13 N12 O14 Ni2 0.000(2) . . . . ?
C6 N5 Ni1 N1 -62.86(11) . . . . ?
C6 N5 Ni1 N3 -175.7(2) . . . . ?
C6 N5 Ni1 N4 38.14(10) . . . . ?
C6 N5 Ni1 O3 -162.37(10) . . . . ?
C6 N5 Ni1 O4 139.84(10) . . . . ?
C6 N5 Ni1 O1A -45.3(6) . . . . ?
C1 N3 Ni1 N1 64.48(11) . . . . ?
C1 N3 Ni1 N5 177.7(2) . . . . ?
C1 N3 Ni1 N4 -36.14(10) . . . . ?
C1 N3 Ni1 O3 164.37(10) . . . . ?
C1 N3 Ni1 O4 -137.95(10) . . . . ?
C1 N3 Ni1 O1A 47.9(6) . . . . ?
C7 N4 Ni1 N1 -177.80(9) . . . . ?
C3 N4 Ni1 N1 -58.35(10) . . . . ?
C4 N4 Ni1 N1 62.00(10) . . . . ?
C7 N4 Ni1 N5 86.78(10) . . . . ?
C3 N4 Ni1 N5 -153.76(9) . . . . ?
C4 N4 Ni1 N5 -33.41(9) . . . . ?
C7 N4 Ni1 N3 -88.10(10) . . . . ?
C3 N4 Ni1 N3 31.36(10) . . . . ?
C4 N4 Ni1 N3 151.71(9) . . . . ?
C7 N4 Ni1 O3 -3.50(17) . . . . ?
C3 N4 Ni1 O3 115.96(13) . . . . ?
C4 N4 Ni1 O3 -123.69(13) . . . . ?
C7 N4 Ni1 O4 0.85(9) . . . . ?
C3 N4 Ni1 O4 120.31(10) . . . . ?
C4 N4 Ni1 O4 -119.34(9) . . . . ?
C7 N4 Ni1 O1A 175.4(6) . . . . ?
C3 N4 Ni1 O1A -65.2(6) . . . . ?
C4 N4 Ni1 O1A 55.2(6) . . . . ?
N2 O3 Ni1 N1 179.33(8) . . . . ?
N2 O3 Ni1 N5 -86.39(9) . . . . ?
N2 O3 Ni1 N3 91.49(9) . . . . ?
N2 O3 Ni1 N4 5.01(16) . . . . ?
N2 O3 Ni1 O4 -0.03(7) . . . . ?
N2 O3 Ni1 O1A -173.8(7) . . . . ?
N2 O4 Ni1 N1 -1.60(15) . . . . ?
N2 O4 Ni1 N5 89.51(8) . . . . ?
N2 O4 Ni1 N3 -84.07(8) . . . . ?
N2 O4 Ni1 N4 -178.17(8) . . . . ?
N2 O4 Ni1 O3 0.03(7) . . . . ?
N2 O4 Ni1 O1A 47(5) . . . . ?
C11 N13 Ni2 N13 -175.1(3) . . . 4_565 ?
C11 N13 Ni2 O14 -56.25(11) . . . . ?
C11 N13 Ni2 N14 38.64(12) . . . . ?
C11 N13 Ni2 N11 139.02(11) . . . . ?
C11 N13 Ni2 O13 -114.17(12) . . . . ?
N12 O14 Ni2 N13 -85.15(4) . . . . ?
N12 O14 Ni2 N13 85.15(4) . . . 4_565 ?
N12 O14 Ni2 N14 180.0 . . . . ?
N12 O14 Ni2 N11 0.000(1) . . . . ?
N12 O14 Ni2 O13 0.0 . . . . ?
C17 N14 Ni2 N13 86.93(4) . . . . ?
C13 N14 Ni2 N13 -151.01(9) 4_565 . . . ?
C13 N14 Ni2 N13 -35.13(10) . . . . ?
C17 N14 Ni2 N13 -86.93(4) . . . 4_565 ?
C13 N14 Ni2 N13 35.13(10) 4_565 . . 4_565 ?
C13 N14 Ni2 N13 151.01(9) . . . 4_565 ?
C17 N14 Ni2 O14 180.0 . . . . ?
C13 N14 Ni2 O14 -57.94(9) 4_565 . . . ?
C13 N14 Ni2 O14 57.94(9) . . . . ?
C17 N14 Ni2 N11 0.0 . . . . ?
C13 N14 Ni2 N11 122.06(9) 4_565 . . . ?
C13 N14 Ni2 N11 -122.06(9) . . . . ?
C17 N14 Ni2 O13 180.000(1) . . . . ?
C13 N14 Ni2 O13 -57.94(9) 4_565 . . . ?
C13 N14 Ni2 O13 57.94(9) . . . . ?
N12 O13 Ni2 N13 94.84(4) . . . . ?
N12 O13 Ni2 N13 -94.84(4) . . . 4_565 ?
N12 O13 Ni2 O14 0.000(1) . . . . ?
N12 O13 Ni2 N14 0.000(1) . . . . ?
N12 O13 Ni2 N11 180.000(1) . . . . ?
N5 Ni1 N1 O1 56.87(12) . . . . ?
N3 Ni1 N1 O1 -131.60(12) . . . . ?
N4 Ni1 N1 O1 -37.32(12) . . . . ?
O3 Ni1 N1 O1 144.70(12) . . . . ?
O4 Ni1 N1 O1 146.09(12) . . . . ?
O1A Ni1 N1 O1 -15.5(18) . . . . ?
N5 Ni1 N1 O2 -122.13(16) . . . . ?
N3 Ni1 N1 O2 49.40(16) . . . . ?
N4 Ni1 N1 O2 143.68(16) . . . . ?
O3 Ni1 N1 O2 -34.30(16) . . . . ?
O4 Ni1 N1 O2 -32.9(2) . . . . ?
O1A Ni1 N1 O2 165.5(19) . . . . ?
O2A N1A O1A Ni1 -6(4) . . . . ?
N1 Ni1 O1A N1A -2.2(16) . . . . ?
N5 Ni1 O1A N1A -110(2) . . . . ?
N3 Ni1 O1A N1A 62(2) . . . . ?
N4 Ni1 O1A N1A 156(2) . . . . ?
O3 Ni1 O1A N1A -24(2) . . . . ?
O4 Ni1 O1A N1A -68(5) . . . . ?
N13 Ni2 N11 O11 -2.78(14) . . . 4_565 ?
N13 Ni2 N11 O11 -174.82(14) 4_565 . . 4_565 ?
O14 Ni2 N11 O11 -88.80(14) . . . 4_565 ?
N14 Ni2 N11 O11 91.20(14) . . . 4_565 ?
O13 Ni2 N11 O11 -88.80(14) . . . 4_565 ?
N13 Ni2 N11 O11 174.82(14) . . . . ?
N13 Ni2 N11 O11 2.78(14) 4_565 . . . ?
O14 Ni2 N11 O11 88.80(14) . . . . ?
N14 Ni2 N11 O11 -91.20(14) . . . . ?
O13 Ni2 N11 O11 88.80(14) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3D O2A 0.92 2.53 2.96(5) 109.0 .
N5 H5C O3 0.92 2.19 3.0200(16) 149.4 3_557
N5 H5C O2A 0.92 2.49 3.16(4) 129.6 3_557
N5 H5D O11 0.92 2.21 3.0792(17) 157.3 4_565
N13 H13D O11 0.92 2.17 2.8233(19) 127.2 4_565

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.057

_database_code_depnum_ccdc_archive 'CCDC 994151'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex7_250K
_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;
Dinitro-(3,3-diamino-N-methyldipropylamine)nickel(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H19 N5 Ni O4'
_chemical_formula_sum            'C7 H19 N5 Ni O4'
_chemical_formula_weight         295.98

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'
O O 0.0106 0.0060 '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'


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

_cell_length_a                   7.202(5)
_cell_length_b                   23.718(5)
_cell_length_c                   11.025(5)
_cell_angle_alpha                90.000
_cell_angle_beta                 103.746(5)
_cell_angle_gamma                90.000
_cell_volume                     1829.3(16)
_cell_formula_units_Z            6
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    5592
_cell_measurement_theta_min      2.9060
_cell_measurement_theta_max      30.4401

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/m

_exptl_crystal_description       Block
_exptl_crystal_colour            Violet
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936

_exptl_absorpt_coefficient_mu    1.604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.80518
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13418
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         30.51
_reflns_number_total             5719
_reflns_number_gt                4613
_reflns_threshold_expression     >2sigma(I)


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'POV-RAY for Windows, 3.62 (Cason, 2009)'
_computing_publication_material  'WinGX, 1.80.05 (Farrugia, 1999)'


_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 > 2sigma(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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0294P)²+0.2512P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5719
_refine_ls_number_parameters     255
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0278
_refine_ls_wR_factor_ref         0.0666
_refine_ls_wR_factor_gt          0.0609
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2856(2) 0.01994(7) 0.61887(14) 0.0371(3) Uani 1 1 d . . .
H1A H 0.1705 -0.0014 0.5796 0.044 Uiso 1 1 calc R . .
H1B H 0.3955 0.0014 0.5978 0.044 Uiso 1 1 calc R . .
C2 C 0.2681(3) 0.07913(7) 0.56847(16) 0.0404(4) Uani 1 1 d . . .
H2A H 0.2785 0.0781 0.4815 0.048 Uiso 1 1 calc R . .
H2B H 0.3756 0.1014 0.6160 0.048 Uiso 1 1 calc R . .
C3 C 0.0832(3) 0.10871(7) 0.57358(14) 0.0383(4) Uani 1 1 d . . .
H3A H 0.0716 0.1425 0.5213 0.046 Uiso 1 1 calc R . .
H3B H -0.0232 0.0837 0.5357 0.046 Uiso 1 1 calc R . .
C4 C -0.1371(2) 0.15057(7) 0.67519(15) 0.0387(4) Uani 1 1 d . . .
H4A H -0.2276 0.1223 0.6312 0.046 Uiso 1 1 calc R . .
H4B H -0.1425 0.1827 0.6187 0.046 Uiso 1 1 calc R . .
C5 C -0.2053(2) 0.17025(7) 0.78787(16) 0.0412(4) Uani 1 1 d . . .
H5A H -0.1085 0.1954 0.8376 0.049 Uiso 1 1 calc R . .
H5B H -0.3228 0.1922 0.7590 0.049 Uiso 1 1 calc R . .
C6 C -0.2439(2) 0.12314(7) 0.87094(16) 0.0398(4) Uani 1 1 d . . .
H6A H -0.3080 0.1385 0.9328 0.048 Uiso 1 1 calc R . .
H6B H -0.3295 0.0954 0.8203 0.048 Uiso 1 1 calc R . .
C7 C 0.2006(2) 0.17018(6) 0.74991(15) 0.0389(4) Uani 1 1 d . . .
H7A H 0.3284 0.1546 0.7633 0.058 Uiso 1 1 calc R . .
H7B H 0.1797 0.1837 0.8287 0.058 Uiso 1 1 calc R . .
H7C H 0.1868 0.2012 0.6912 0.058 Uiso 1 1 calc R . .
C11 C 0.5294(2) 0.12776(7) 1.31744(16) 0.0381(4) Uani 1 1 d . . .
H11A H 0.4935 0.0880 1.3045 0.046 Uiso 1 1 calc R . .
H11B H 0.5865 0.1334 1.4066 0.046 Uiso 1 1 calc R . .
C12 C 0.6726(3) 0.14240(7) 1.24337(18) 0.0439(4) Uani 1 1 d . . .
H12A H 0.6097 0.1399 1.1544 0.053 Uiso 1 1 calc R . .
H12B H 0.7748 0.1141 1.2607 0.053 Uiso 1 1 calc R . .
C13 C 0.7621(2) 0.20024(7) 1.26882(16) 0.0379(4) Uani 1 1 d . . .
H13A H 0.8070 0.2046 1.3595 0.045 Uiso 1 1 calc R . .
H13B H 0.8750 0.2013 1.2338 0.045 Uiso 1 1 calc R . .
C17 C 0.5990(3) 0.2500 1.0823(2) 0.0438(6) Uani 1 2 d S . .
H17A H 0.5242 0.2831 1.0502 0.066 Uiso 0.50 1 calc PR . .
H17B H 0.5274 0.2163 1.0503 0.066 Uiso 0.50 1 calc PR . .
H17C H 0.7181 0.2506 1.0557 0.066 Uiso 1 2 calc SR . .
N2 N 0.3611(2) 0.05024(6) 1.04418(13) 0.0419(3) Uani 1 1 d . . .
N3 N 0.31013(18) 0.01961(5) 0.75558(11) 0.0318(3) Uani 1 1 d . A .
H3C H 0.4259 0.0353 0.7901 0.038 Uiso 1 1 calc R . .
H3D H 0.3160 -0.0170 0.7807 0.038 Uiso 1 1 calc R . .
N4 N 0.05881(17) 0.12598(5) 0.69901(11) 0.0283(2) Uani 1 1 d . A .
N5 N -0.06622(18) 0.09534(5) 0.93517(12) 0.0323(3) Uani 1 1 d . A .
H5C H -0.0976 0.0677 0.9839 0.039 Uiso 1 1 calc R . .
H5D H 0.0048 0.1211 0.9875 0.039 Uiso 1 1 calc R . .
N12 N 0.3782(4) 0.2500 1.5172(2) 0.0571(6) Uani 1 2 d S . .
N13 N 0.35836(19) 0.16319(5) 1.27900(14) 0.0378(3) Uani 1 1 d . . .
H13C H 0.2776 0.1538 1.3280 0.045 Uiso 1 1 calc R . .
H13D H 0.2993 0.1533 1.1994 0.045 Uiso 1 1 calc R . .
N14 N 0.6404(2) 0.2500 1.21990(15) 0.0272(3) Uani 1 2 d S . .
O3 O 0.24061(18) 0.01288(5) 0.99684(11) 0.0403(3) Uani 1 1 d . A .
O4 O 0.34617(16) 0.09362(5) 0.97675(11) 0.0389(3) Uani 1 1 d . A .
O13 O 0.2260(3) 0.2500 1.43260(18) 0.0529(5) Uani 1 2 d S . .
O14 O 0.5262(2) 0.2500 1.47435(15) 0.0437(4) Uani 1 2 d S . .
Ni1 Ni 0.10840(2) 0.059817(7) 0.832031(16) 0.02419(5) Uani 1 1 d . . .
Ni2 Ni 0.38605(3) 0.2500 1.28363(2) 0.02386(6) Uani 1 2 d S . .
N1 N -0.0900(2) 0.00145(7) 0.74529(15) 0.0311(4) Uani 0.878(4) 1 d PD A 1
O1 O -0.2523(2) 0.01307(6) 0.68262(14) 0.0494(5) Uani 0.878(4) 1 d PD A 1
O2 O -0.0484(4) -0.04984(14) 0.7553(3) 0.0522(7) Uani 0.878(4) 1 d PD A 1
N1A N -0.166(2) -0.0309(5) 0.7114(12) 0.048(4) Uiso 0.122(4) 1 d PD A 2
O1A O -0.136(2) 0.0229(5) 0.7150(12) 0.045(4) Uiso 0.122(4) 1 d PD A 2
O2A O -0.023(3) -0.0547(10) 0.7834(16) 0.027(3) Uiso 0.122(4) 1 d PD A 2
N11 N 0.1763(2) 0.2500 1.11147(16) 0.0301(4) Uani 1 2 d S . .
O11 O 0.1104(2) 0.29391(6) 1.06016(13) 0.0631(4) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N3 1.475(2) . ?
C1 C2 1.504(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C2 C3 1.518(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C3 N4 1.492(2) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 N4 1.491(2) . ?
C4 C5 1.514(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 C6 1.512(2) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 N5 1.464(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 N4 1.4780(19) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
C11 N13 1.468(2) . ?
C11 C12 1.501(2) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 C13 1.513(2) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 N14 1.4927(18) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C17 N14 1.475(3) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 H17C 0.9700 . ?
N2 O4 1.2588(18) . ?
N2 O3 1.2629(19) . ?
N3 Ni1 2.0766(15) . ?
N3 H3C 0.9100 . ?
N3 H3D 0.9100 . ?
N4 Ni1 2.1194(12) . ?
N5 Ni1 2.0650(15) . ?
N5 H5C 0.9100 . ?
N5 H5D 0.9100 . ?
N12 O13 1.259(3) . ?
N12 O14 1.264(3) . ?
N13 Ni2 2.0680(13) . ?
N13 H13C 0.9100 . ?
N13 H13D 0.9100 . ?
N14 C13 1.4927(19) 4_565 ?
N14 Ni2 2.112(2) . ?
O3 Ni1 2.1506(13) . ?
O4 Ni1 2.1960(14) . ?
O13 Ni2 2.2193(19) . ?
O14 Ni2 2.1051(18) . ?
Ni1 N1 2.0550(16) . ?
Ni1 O1A 2.111(14) . ?
Ni2 N13 2.0680(13) 4_565 ?
Ni2 N11 2.127(2) . ?
N1 O1 1.239(2) . ?
N1 O2 1.251(3) . ?
N1A O2A 1.273(15) . ?
N1A O1A 1.292(15) . ?
N11 O11 1.2257(15) 4_565 ?
N11 O11 1.2257(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 C1 C2 111.19(13) . . ?
N3 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N3 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
C1 C2 C3 114.49(14) . . ?
C1 C2 H2A 108.6 . . ?
C3 C2 H2A 108.6 . . ?
C1 C2 H2B 108.6 . . ?
C3 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
N4 C3 C2 117.30(13) . . ?
N4 C3 H3A 108.0 . . ?
C2 C3 H3A 108.0 . . ?
N4 C3 H3B 108.0 . . ?
C2 C3 H3B 108.0 . . ?
H3A C3 H3B 107.2 . . ?
N4 C4 C5 116.99(13) . . ?
N4 C4 H4A 108.0 . . ?
C5 C4 H4A 108.0 . . ?
N4 C4 H4B 108.0 . . ?
C5 C4 H4B 108.0 . . ?
H4A C4 H4B 107.3 . . ?
C6 C5 C4 114.31(14) . . ?
C6 C5 H5A 108.7 . . ?
C4 C5 H5A 108.7 . . ?
C6 C5 H5B 108.7 . . ?
C4 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
N5 C6 C5 111.11(14) . . ?
N5 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
N5 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N13 C11 C12 110.39(14) . . ?
N13 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
N13 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
C11 C12 C13 115.25(14) . . ?
C11 C12 H12A 108.5 . . ?
C13 C12 H12A 108.5 . . ?
C11 C12 H12B 108.5 . . ?
C13 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?
N14 C13 C12 117.51(14) . . ?
N14 C13 H13A 107.9 . . ?
C12 C13 H13A 107.9 . . ?
N14 C13 H13B 107.9 . . ?
C12 C13 H13B 107.9 . . ?
H13A C13 H13B 107.2 . . ?
N14 C17 H17A 109.5 . . ?
N14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O4 N2 O3 112.06(12) . . ?
C1 N3 Ni1 119.12(10) . . ?
C1 N3 H3C 107.5 . . ?
Ni1 N3 H3C 107.5 . . ?
C1 N3 H3D 107.5 . . ?
Ni1 N3 H3D 107.5 . . ?
H3C N3 H3D 107.0 . . ?
C7 N4 C4 109.20(13) . . ?
C7 N4 C3 108.90(12) . . ?
C4 N4 C3 105.00(12) . . ?
C7 N4 Ni1 105.95(9) . . ?
C4 N4 Ni1 114.10(10) . . ?
C3 N4 Ni1 113.61(9) . . ?
C6 N5 Ni1 119.62(11) . . ?
C6 N5 H5C 107.4 . . ?
Ni1 N5 H5C 107.4 . . ?
C6 N5 H5D 107.4 . . ?
Ni1 N5 H5D 107.4 . . ?
H5C N5 H5D 106.9 . . ?
O13 N12 O14 112.7(2) . . ?
C11 N13 Ni2 119.57(10) . . ?
C11 N13 H13C 107.4 . . ?
Ni2 N13 H13C 107.4 . . ?
C11 N13 H13D 107.4 . . ?
Ni2 N13 H13D 107.4 . . ?
H13C N13 H13D 107.0 . . ?
C17 N14 C13 109.23(11) . 4_565 ?
C17 N14 C13 109.23(11) . . ?
C13 N14 C13 104.50(16) 4_565 . ?
C17 N14 Ni2 111.28(13) . . ?
C13 N14 Ni2 111.18(10) 4_565 . ?
C13 N14 Ni2 111.18(10) . . ?
N2 O3 Ni1 96.25(9) . . ?
N2 O4 Ni1 94.19(9) . . ?
N12 O13 Ni2 91.96(15) . . ?
N12 O14 Ni2 97.27(15) . . ?
N1 Ni1 N5 94.82(7) . . ?
N1 Ni1 N3 88.73(7) . . ?
N5 Ni1 N3 170.83(5) . . ?
N1 Ni1 O1A 18.0(3) . . ?
N5 Ni1 O1A 88.7(4) . . ?
N3 Ni1 O1A 97.1(4) . . ?
N1 Ni1 N4 101.10(6) . . ?
N5 Ni1 N4 93.12(5) . . ?
N3 Ni1 N4 94.49(5) . . ?
O1A Ni1 N4 84.5(3) . . ?
N1 Ni1 O3 99.43(7) . . ?
N5 Ni1 O3 87.21(6) . . ?
N3 Ni1 O3 83.87(5) . . ?
O1A Ni1 O3 116.1(3) . . ?
N4 Ni1 O3 159.36(5) . . ?
N1 Ni1 O4 156.92(6) . . ?
N5 Ni1 O4 85.57(7) . . ?
N3 Ni1 O4 87.85(6) . . ?
O1A Ni1 O4 171.5(4) . . ?
N4 Ni1 O4 101.92(5) . . ?
O3 Ni1 O4 57.51(5) . . ?
N13 Ni2 N13 169.25(8) . 4_565 ?
N13 Ni2 O14 92.59(4) . . ?
N13 Ni2 O14 92.59(4) 4_565 . ?
N13 Ni2 N14 94.47(4) . . ?
N13 Ni2 N14 94.47(4) 4_565 . ?
O14 Ni2 N14 94.85(8) . . ?
N13 Ni2 N11 86.22(4) . . ?
N13 Ni2 N11 86.22(4) 4_565 . ?
O14 Ni2 N11 164.12(7) . . ?
N14 Ni2 N11 101.04(8) . . ?
N13 Ni2 O13 87.38(4) . . ?
N13 Ni2 O13 87.38(4) 4_565 . ?
O14 Ni2 O13 58.05(8) . . ?
N14 Ni2 O13 152.89(7) . . ?
N11 Ni2 O13 106.07(9) . . ?
O1 N1 O2 116.1(2) . . ?
O1 N1 Ni1 124.68(15) . . ?
O2 N1 Ni1 119.23(19) . . ?
O2A N1A O1A 108.5(18) . . ?
N1A O1A Ni1 122.3(12) . . ?
O11 N11 O11 116.37(19) 4_565 . ?
O11 N11 Ni2 121.80(9) 4_565 . ?
O11 N11 Ni2 121.80(9) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 C1 C2 C3 -69.86(18) . . . . ?
C1 C2 C3 N4 71.37(19) . . . . ?
N4 C4 C5 C6 -69.8(2) . . . . ?
C4 C5 C6 N5 68.84(18) . . . . ?
N13 C11 C12 C13 67.63(19) . . . . ?
C11 C12 C13 N14 -72.7(2) . . . . ?
C2 C1 N3 Ni1 55.64(17) . . . . ?
C5 C4 N4 C7 -65.43(18) . . . . ?
C5 C4 N4 C3 177.93(14) . . . . ?
C5 C4 N4 Ni1 52.90(17) . . . . ?
C2 C3 N4 C7 66.16(18) . . . . ?
C2 C3 N4 C4 -176.99(14) . . . . ?
C2 C3 N4 Ni1 -51.66(17) . . . . ?
C5 C6 N5 Ni1 -57.65(16) . . . . ?
C12 C11 N13 Ni2 -55.34(17) . . . . ?
C12 C13 N14 C17 -67.84(19) . . . . ?
C12 C13 N14 C13 175.38(9) . . . 4_565 ?
C12 C13 N14 Ni2 55.35(17) . . . . ?
O4 N2 O3 Ni1 0.01(14) . . . . ?
O3 N2 O4 Ni1 -0.01(13) . . . . ?
O14 N12 O13 Ni2 0.000(1) . . . . ?
O13 N12 O14 Ni2 0.000(2) . . . . ?
C6 N5 Ni1 N1 -62.91(12) . . . . ?
C6 N5 Ni1 N3 -175.5(3) . . . . ?
C6 N5 Ni1 O1A -45.9(4) . . . . ?
C6 N5 Ni1 N4 38.52(12) . . . . ?
C6 N5 Ni1 O3 -162.14(12) . . . . ?
C6 N5 Ni1 O4 140.24(12) . . . . ?
C1 N3 Ni1 N1 65.47(12) . . . . ?
C1 N3 Ni1 N5 178(10) . . . . ?
C1 N3 Ni1 O1A 49.5(4) . . . . ?
C1 N3 Ni1 N4 -35.57(12) . . . . ?
C1 N3 Ni1 O3 165.10(12) . . . . ?
C1 N3 Ni1 O4 -137.36(12) . . . . ?
C7 N4 Ni1 N1 -177.88(10) . . . . ?
C4 N4 Ni1 N1 61.95(11) . . . . ?
C3 N4 Ni1 N1 -58.37(12) . . . . ?
C7 N4 Ni1 N5 86.58(11) . . . . ?
C4 N4 Ni1 N5 -33.59(10) . . . . ?
C3 N4 Ni1 N5 -153.91(11) . . . . ?
C7 N4 Ni1 N3 -88.29(11) . . . . ?
C4 N4 Ni1 N3 151.54(10) . . . . ?
C3 N4 Ni1 N3 31.22(11) . . . . ?
C7 N4 Ni1 O1A 174.9(4) . . . . ?
C4 N4 Ni1 O1A 54.8(4) . . . . ?
C3 N4 Ni1 O1A -65.5(4) . . . . ?
C7 N4 Ni1 O3 -3.76(19) . . . . ?
C4 N4 Ni1 O3 -123.93(14) . . . . ?
C3 N4 Ni1 O3 115.75(15) . . . . ?
C7 N4 Ni1 O4 0.46(10) . . . . ?
C4 N4 Ni1 O4 -119.71(10) . . . . ?
C3 N4 Ni1 O4 119.97(11) . . . . ?
N2 O3 Ni1 N1 179.04(10) . . . . ?
N2 O3 Ni1 N5 -86.53(10) . . . . ?
N2 O3 Ni1 N3 91.35(10) . . . . ?
N2 O3 Ni1 O1A -173.7(4) . . . . ?
N2 O3 Ni1 N4 4.89(18) . . . . ?
N2 O3 Ni1 O4 -0.01(9) . . . . ?
N2 O4 Ni1 N1 -2.40(18) . . . . ?
N2 O4 Ni1 N5 89.51(10) . . . . ?
N2 O4 Ni1 N3 -84.09(10) . . . . ?
N2 O4 Ni1 O1A 42(2) . . . . ?
N2 O4 Ni1 N4 -178.23(9) . . . . ?
N2 O4 Ni1 O3 0.01(9) . . . . ?
C11 N13 Ni2 N13 -175.1(4) . . . 4_565 ?
C11 N13 Ni2 O14 -56.40(13) . . . . ?
C11 N13 Ni2 N14 38.68(13) . . . . ?
C11 N13 Ni2 N11 139.47(13) . . . . ?
C11 N13 Ni2 O13 -114.23(13) . . . . ?
N12 O14 Ni2 N13 -85.29(4) . . . . ?
N12 O14 Ni2 N13 85.29(4) . . . 4_565 ?
N12 O14 Ni2 N14 180.000(1) . . . . ?
N12 O14 Ni2 N11 0.000(2) . . . . ?
N12 O14 Ni2 O13 0.000(1) . . . . ?
C17 N14 Ni2 N13 87.01(4) . . . . ?
C13 N14 Ni2 N13 -150.98(10) 4_565 . . . ?
C13 N14 Ni2 N13 -35.00(11) . . . . ?
C17 N14 Ni2 N13 -87.01(4) . . . 4_565 ?
C13 N14 Ni2 N13 35.00(11) 4_565 . . 4_565 ?
C13 N14 Ni2 N13 150.98(11) . . . 4_565 ?
C17 N14 Ni2 O14 180.0 . . . . ?
C13 N14 Ni2 O14 -57.99(10) 4_565 . . . ?
C13 N14 Ni2 O14 57.99(10) . . . . ?
C17 N14 Ni2 N11 0.0 . . . . ?
C13 N14 Ni2 N11 122.01(10) 4_565 . . . ?
C13 N14 Ni2 N11 -122.01(10) . . . . ?
C17 N14 Ni2 O13 180.000(2) . . . . ?
C13 N14 Ni2 O13 -57.99(10) 4_565 . . . ?
C13 N14 Ni2 O13 57.99(10) . . . . ?
N12 O13 Ni2 N13 94.70(4) . . . . ?
N12 O13 Ni2 N13 -94.70(4) . . . 4_565 ?
N12 O13 Ni2 O14 0.000(1) . . . . ?
N12 O13 Ni2 N14 0.000(2) . . . . ?
N12 O13 Ni2 N11 180.000(1) . . . . ?
N5 Ni1 N1 O1 56.80(15) . . . . ?
N3 Ni1 N1 O1 -131.66(15) . . . . ?
O1A Ni1 N1 O1 -13.6(11) . . . . ?
N4 Ni1 N1 O1 -37.34(15) . . . . ?
O3 Ni1 N1 O1 144.76(15) . . . . ?
O4 Ni1 N1 O1 146.81(15) . . . . ?
N5 Ni1 N1 O2 -122.8(2) . . . . ?
N3 Ni1 N1 O2 48.7(2) . . . . ?
O1A Ni1 N1 O2 166.8(12) . . . . ?
N4 Ni1 N1 O2 143.1(2) . . . . ?
O3 Ni1 N1 O2 -34.8(2) . . . . ?
O4 Ni1 N1 O2 -32.8(3) . . . . ?
O2A N1A O1A Ni1 -2.7(18) . . . . ?
N1 Ni1 O1A N1A -1.8(8) . . . . ?
N5 Ni1 O1A N1A -111.9(12) . . . . ?
N3 Ni1 O1A N1A 61.0(12) . . . . ?
N4 Ni1 O1A N1A 154.8(12) . . . . ?
O3 Ni1 O1A N1A -25.7(13) . . . . ?
O4 Ni1 O1A N1A -65(3) . . . . ?
N13 Ni2 N11 O11 -2.67(16) . . . 4_565 ?
N13 Ni2 N11 O11 -175.02(16) 4_565 . . 4_565 ?
O14 Ni2 N11 O11 -88.84(16) . . . 4_565 ?
N14 Ni2 N11 O11 91.16(16) . . . 4_565 ?
O13 Ni2 N11 O11 -88.84(16) . . . 4_565 ?
N13 Ni2 N11 O11 175.02(16) . . . . ?
N13 Ni2 N11 O11 2.67(16) 4_565 . . . ?
O14 Ni2 N11 O11 88.84(16) . . . . ?
N14 Ni2 N11 O11 -91.16(16) . . . . ?
O13 Ni2 N11 O11 88.84(16) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3D O2A 0.91 2.61 3.05(2) 110.8 .
N5 H5C O3 0.91 2.20 3.0292(18) 150.4 3_557
N5 H5C O2A 0.91 2.52 3.166(17) 127.8 3_557
N5 H5D O11 0.91 2.23 3.0956(19) 157.7 4_565
N13 H13D O11 0.91 2.19 2.828(2) 126.9 4_565

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.055

_database_code_depnum_ccdc_archive 'CCDC 994152'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex7_298K
_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;
Dinitro-(3,3-diamino-N-methyldipropylamine)nickel(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H19 N5 Ni O4'
_chemical_formula_sum            'C7 H19 N5 Ni O4'
_chemical_formula_weight         295.98

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'
O O 0.0106 0.0060 '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'


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

_cell_length_a                   7.235(5)
_cell_length_b                   23.768(5)
_cell_length_c                   11.072(5)
_cell_angle_alpha                90.000
_cell_angle_beta                 103.920(5)
_cell_angle_gamma                90.000
_cell_volume                     1848.0(16)
_cell_formula_units_Z            6
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4894
_cell_measurement_theta_min      2.8948
_cell_measurement_theta_max      30.4400

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/m

_exptl_crystal_description       Block
_exptl_crystal_colour            Violet
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936

_exptl_absorpt_coefficient_mu    1.588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.77383
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13528
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.90
_diffrn_reflns_theta_max         30.51
_reflns_number_total             5760
_reflns_number_gt                4467
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'POV-RAY for Windows, 3.62 (Cason, 2009)'
_computing_publication_material  'WinGX, 1.80.05 (Farrugia, 1999)'

_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 > 2sigma(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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0306P)²+0.1689P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5760
_refine_ls_number_parameters     255
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0305
_refine_ls_wR_factor_ref         0.0724
_refine_ls_wR_factor_gt          0.0650
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2898(3) 0.02060(8) 0.62074(16) 0.0465(4) Uani 1 1 d . . .
H1A H 0.1776 -0.0007 0.5802 0.056 Uiso 1 1 calc R . .
H1B H 0.3997 0.0027 0.6014 0.056 Uiso 1 1 calc R . .
C2 C 0.2723(3) 0.07991(8) 0.57118(18) 0.0509(5) Uani 1 1 d . . .
H2A H 0.2840 0.0792 0.4857 0.061 Uiso 1 1 calc R . .
H2B H 0.3775 0.1019 0.6191 0.061 Uiso 1 1 calc R . .
C3 C 0.0875(3) 0.10904(8) 0.57498(15) 0.0474(4) Uani 1 1 d . . .
H3A H 0.0762 0.1425 0.5235 0.057 Uiso 1 1 calc R . .
H3B H -0.0167 0.0842 0.5369 0.057 Uiso 1 1 calc R . .
C4 C -0.1344(3) 0.15042(8) 0.67464(16) 0.0473(4) Uani 1 1 d . . .
H4A H -0.2230 0.1224 0.6306 0.057 Uiso 1 1 calc R . .
H4B H -0.1396 0.1823 0.6192 0.057 Uiso 1 1 calc R . .
C5 C -0.2040(3) 0.16975(8) 0.78603(19) 0.0510(5) Uani 1 1 d . . .
H5A H -0.1095 0.1948 0.8355 0.061 Uiso 1 1 calc R . .
H5B H -0.3202 0.1912 0.7568 0.061 Uiso 1 1 calc R . .
C6 C -0.2424(3) 0.12284(8) 0.86822(18) 0.0485(4) Uani 1 1 d . . .
H6A H -0.3065 0.1379 0.9287 0.058 Uiso 1 1 calc R . .
H6B H -0.3262 0.0954 0.8179 0.058 Uiso 1 1 calc R . .
C7 C 0.2013(3) 0.17031(7) 0.75116(18) 0.0491(4) Uani 1 1 d . . .
H7A H 0.3273 0.1548 0.7678 0.074 Uiso 1 1 calc R . .
H7B H 0.1768 0.1844 0.8271 0.074 Uiso 1 1 calc R . .
H7C H 0.1908 0.2005 0.6922 0.074 Uiso 1 1 calc R . .
C11 C 0.5299(3) 0.12824(8) 1.31662(18) 0.0494(4) Uani 1 1 d . . .
H11A H 0.4950 0.0889 1.3040 0.059 Uiso 1 1 calc R . .
H11B H 0.5858 0.1340 1.4046 0.059 Uiso 1 1 calc R . .
C12 C 0.6720(3) 0.14285(8) 1.2436(2) 0.0573(5) Uani 1 1 d . . .
H12A H 0.6102 0.1402 1.1557 0.069 Uiso 1 1 calc R . .
H12B H 0.7730 0.1150 1.2612 0.069 Uiso 1 1 calc R . .
C13 C 0.7605(2) 0.20043(8) 1.26857(19) 0.0489(4) Uani 1 1 d . . .
H13A H 0.8045 0.2049 1.3580 0.059 Uiso 1 1 calc R . .
H13B H 0.8719 0.2015 1.2344 0.059 Uiso 1 1 calc R . .
C17 C 0.5970(4) 0.2500 1.0818(2) 0.0569(7) Uani 1 2 d S . .
H17A H 0.5231 0.2827 1.0502 0.085 Uiso 0.50 1 calc PR . .
H17B H 0.5264 0.2167 1.0503 0.085 Uiso 0.50 1 calc PR . .
H17C H 0.7142 0.2506 1.0557 0.085 Uiso 1 2 calc SR . .
N2 N 0.3595(2) 0.04995(7) 1.04355(14) 0.0521(4) Uani 1 1 d . . .
N3 N 0.3102(2) 0.01973(6) 0.75602(13) 0.0408(3) Uani 1 1 d . A .
H3C H 0.4244 0.0348 0.7918 0.049 Uiso 1 1 calc R . .
H3D H 0.3141 -0.0166 0.7797 0.049 Uiso 1 1 calc R . .
N4 N 0.06104(19) 0.12612(5) 0.69947(12) 0.0355(3) Uani 1 1 d . A .
N5 N -0.0656(2) 0.09518(6) 0.93333(13) 0.0393(3) Uani 1 1 d . A .
H5C H -0.0968 0.0678 0.9811 0.047 Uiso 1 1 calc R . .
H5D H 0.0040 0.1206 0.9852 0.047 Uiso 1 1 calc R . .
N12 N 0.3772(5) 0.2500 1.5147(2) 0.0694(8) Uani 1 2 d S . .
N13 N 0.3592(2) 0.16336(6) 1.27749(15) 0.0458(4) Uani 1 1 d . . .
H13C H 0.2794 0.1541 1.3254 0.055 Uiso 1 1 calc R . .
H13D H 0.3015 0.1536 1.1989 0.055 Uiso 1 1 calc R . .
N14 N 0.6386(3) 0.2500 1.21892(17) 0.0358(4) Uani 1 2 d S . .
O3 O 0.2397(2) 0.01270(5) 0.99617(12) 0.0503(3) Uani 1 1 d . A .
O4 O 0.34568(17) 0.09313(5) 0.97688(12) 0.0480(3) Uani 1 1 d . A .
O13 O 0.2265(3) 0.2500 1.4302(2) 0.0654(6) Uani 1 2 d S . .
O14 O 0.5247(3) 0.2500 1.47279(16) 0.0538(5) Uani 1 2 d S . .
Ni1 Ni 0.10881(3) 0.059890(8) 0.831342(17) 0.03006(6) Uani 1 1 d . . .
Ni2 Ni 0.38576(4) 0.2500 1.28198(2) 0.02974(7) Uani 1 2 d S . .
N1 N -0.0872(3) 0.00141(10) 0.7439(2) 0.0389(6) Uani 0.777(5) 1 d PD A 1
O1 O -0.2493(3) 0.01283(8) 0.68170(18) 0.0624(7) Uani 0.777(5) 1 d PD A 1
O2 O -0.0469(7) -0.04996(18) 0.7520(5) 0.0673(10) Uani 0.777(5) 1 d PD A 1
N1A N -0.1640(13) -0.0303(4) 0.7113(8) 0.057(3) Uiso 0.223(5) 1 d PD A 2
O1A O -0.1310(14) 0.0222(3) 0.7164(8) 0.055(3) Uiso 0.223(5) 1 d PD A 2
O2A O -0.026(2) -0.0558(7) 0.7826(13) 0.046(3) Uiso 0.223(5) 1 d PD A 2
N11 N 0.1755(3) 0.2500 1.11059(18) 0.0371(4) Uani 1 2 d S . .
O11 O 0.1090(2) 0.29365(6) 1.06020(15) 0.0754(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N3 1.469(2) . ?
C1 C2 1.507(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.515(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N4 1.493(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N4 1.491(2) . ?
C4 C5 1.511(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.507(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N5 1.465(2) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N4 1.477(2) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C11 N13 1.467(2) . ?
C11 C12 1.494(3) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.508(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N14 1.495(2) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C17 N14 1.475(3) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
N2 O4 1.254(2) . ?
N2 O3 1.262(2) . ?
N3 Ni1 2.0771(16) . ?
N3 H3C 0.9000 . ?
N3 H3D 0.9000 . ?
N4 Ni1 2.1180(14) . ?
N5 Ni1 2.0631(16) . ?
N5 H5C 0.9000 . ?
N5 H5D 0.9000 . ?
N12 O13 1.254(3) . ?
N12 O14 1.262(3) . ?
N13 Ni2 2.0678(14) . ?
N13 H13C 0.9000 . ?
N13 H13D 0.9000 . ?
N14 C13 1.495(2) 4_565 ?
N14 Ni2 2.109(2) . ?
O3 Ni1 2.1573(14) . ?
O4 Ni1 2.1975(15) . ?
O13 Ni2 2.221(2) . ?
O14 Ni2 2.110(2) . ?
Ni1 N1 2.054(2) . ?
Ni1 O1A 2.091(10) . ?
Ni2 N13 2.0678(14) 4_565 ?
Ni2 N11 2.127(2) . ?
N1 O1 1.239(3) . ?
N1 O2 1.253(5) . ?
N1A O2A 1.267(13) . ?
N1A O1A 1.269(12) . ?
N11 O11 1.2206(16) 4_565 ?
N11 O11 1.2206(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 C1 C2 111.31(15) . . ?
N3 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N3 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
C1 C2 C3 114.50(16) . . ?
C1 C2 H2A 108.6 . . ?
C3 C2 H2A 108.6 . . ?
C1 C2 H2B 108.6 . . ?
C3 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
N4 C3 C2 117.37(15) . . ?
N4 C3 H3A 108.0 . . ?
C2 C3 H3A 108.0 . . ?
N4 C3 H3B 108.0 . . ?
C2 C3 H3B 108.0 . . ?
H3A C3 H3B 107.2 . . ?
N4 C4 C5 117.04(14) . . ?
N4 C4 H4A 108.0 . . ?
C5 C4 H4A 108.0 . . ?
N4 C4 H4B 108.0 . . ?
C5 C4 H4B 108.0 . . ?
H4A C4 H4B 107.3 . . ?
C6 C5 C4 114.45(16) . . ?
C6 C5 H5A 108.6 . . ?
C4 C5 H5A 108.6 . . ?
C6 C5 H5B 108.6 . . ?
C4 C5 H5B 108.6 . . ?
H5A C5 H5B 107.6 . . ?
N5 C6 C5 111.29(15) . . ?
N5 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
N5 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N13 C11 C12 110.37(16) . . ?
N13 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
N13 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
C11 C12 C13 115.39(17) . . ?
C11 C12 H12A 108.4 . . ?
C13 C12 H12A 108.4 . . ?
C11 C12 H12B 108.4 . . ?
C13 C12 H12B 108.4 . . ?
H12A C12 H12B 107.5 . . ?
N14 C13 C12 117.45(16) . . ?
N14 C13 H13A 107.9 . . ?
C12 C13 H13A 107.9 . . ?
N14 C13 H13B 107.9 . . ?
C12 C13 H13B 107.9 . . ?
H13A C13 H13B 107.2 . . ?
N14 C17 H17A 109.5 . . ?
N14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O4 N2 O3 112.32(14) . . ?
C1 N3 Ni1 119.64(11) . . ?
C1 N3 H3C 107.4 . . ?
Ni1 N3 H3C 107.4 . . ?
C1 N3 H3D 107.4 . . ?
Ni1 N3 H3D 107.4 . . ?
H3C N3 H3D 106.9 . . ?
C7 N4 C4 109.19(14) . . ?
C7 N4 C3 108.82(14) . . ?
C4 N4 C3 105.17(13) . . ?
C7 N4 Ni1 106.17(10) . . ?
C4 N4 Ni1 113.92(11) . . ?
C3 N4 Ni1 113.49(10) . . ?
C6 N5 Ni1 119.34(12) . . ?
C6 N5 H5C 107.5 . . ?
Ni1 N5 H5C 107.5 . . ?
C6 N5 H5D 107.5 . . ?
Ni1 N5 H5D 107.5 . . ?
H5C N5 H5D 107.0 . . ?
O13 N12 O14 112.7(2) . . ?
C11 N13 Ni2 119.52(12) . . ?
C11 N13 H13C 107.4 . . ?
Ni2 N13 H13C 107.4 . . ?
C11 N13 H13D 107.4 . . ?
Ni2 N13 H13D 107.4 . . ?
H13C N13 H13D 107.0 . . ?
C17 N14 C13 109.57(13) . 4_565 ?
C17 N14 C13 109.57(13) . . ?
C13 N14 C13 104.02(19) 4_565 . ?
C17 N14 Ni2 111.23(15) . . ?
C13 N14 Ni2 111.11(11) 4_565 . ?
C13 N14 Ni2 111.11(11) . . ?
N2 O3 Ni1 96.02(10) . . ?
N2 O4 Ni1 94.32(10) . . ?
N12 O13 Ni2 92.19(16) . . ?
N12 O14 Ni2 97.30(17) . . ?
N1 Ni1 N5 95.12(8) . . ?
N1 Ni1 N3 88.35(8) . . ?
N5 Ni1 N3 170.78(6) . . ?
N1 Ni1 O1A 17.3(2) . . ?
N5 Ni1 O1A 88.9(2) . . ?
N3 Ni1 O1A 96.8(2) . . ?
N1 Ni1 N4 101.44(8) . . ?
N5 Ni1 N4 93.17(6) . . ?
N3 Ni1 N4 94.51(6) . . ?
O1A Ni1 N4 85.7(2) . . ?
N1 Ni1 O3 99.19(8) . . ?
N5 Ni1 O3 87.14(6) . . ?
N3 Ni1 O3 83.87(6) . . ?
O1A Ni1 O3 115.0(2) . . ?
N4 Ni1 O3 159.26(5) . . ?
N1 Ni1 O4 156.49(8) . . ?
N5 Ni1 O4 85.66(7) . . ?
N3 Ni1 O4 87.77(7) . . ?
O1A Ni1 O4 170.8(2) . . ?
N4 Ni1 O4 101.98(5) . . ?
O3 Ni1 O4 57.34(5) . . ?
N13 Ni2 N13 169.64(8) 4_565 . ?
N13 Ni2 N14 94.31(4) 4_565 . ?
N13 Ni2 N14 94.31(4) . . ?
N13 Ni2 O14 92.48(4) 4_565 . ?
N13 Ni2 O14 92.48(4) . . ?
N14 Ni2 O14 95.12(8) . . ?
N13 Ni2 N11 86.34(4) 4_565 . ?
N13 Ni2 N11 86.34(4) . . ?
N14 Ni2 N11 101.28(8) . . ?
O14 Ni2 N11 163.60(8) . . ?
N13 Ni2 O13 87.48(5) 4_565 . ?
N13 Ni2 O13 87.48(5) . . ?
N14 Ni2 O13 152.90(8) . . ?
O14 Ni2 O13 57.78(9) . . ?
N11 Ni2 O13 105.82(9) . . ?
O1 N1 O2 115.2(3) . . ?
O1 N1 Ni1 124.6(2) . . ?
O2 N1 Ni1 120.2(3) . . ?
O2A N1A O1A 109.4(12) . . ?
N1A O1A Ni1 124.6(8) . . ?
O11 N11 O11 116.4(2) 4_565 . ?
O11 N11 Ni2 121.76(10) 4_565 . ?
O11 N11 Ni2 121.76(11) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 C1 C2 C3 -69.3(2) . . . . ?
C1 C2 C3 N4 71.7(2) . . . . ?
N4 C4 C5 C6 -69.7(2) . . . . ?
C4 C5 C6 N5 68.7(2) . . . . ?
N13 C11 C12 C13 67.7(2) . . . . ?
C11 C12 C13 N14 -72.8(2) . . . . ?
C2 C1 N3 Ni1 54.60(19) . . . . ?
C5 C4 N4 C7 -65.5(2) . . . . ?
C5 C4 N4 C3 177.90(16) . . . . ?
C5 C4 N4 Ni1 53.02(19) . . . . ?
C2 C3 N4 C7 66.1(2) . . . . ?
C2 C3 N4 C4 -177.06(16) . . . . ?
C2 C3 N4 Ni1 -51.91(19) . . . . ?
C5 C6 N5 Ni1 -57.73(18) . . . . ?
C12 C11 N13 Ni2 -55.5(2) . . . . ?
C12 C13 N14 C17 -67.8(2) . . . . ?
C12 C13 N14 C13 175.12(11) . . . 4_565 ?
C12 C13 N14 Ni2 55.5(2) . . . . ?
O4 N2 O3 Ni1 -0.02(16) . . . . ?
O3 N2 O4 Ni1 0.02(15) . . . . ?
O14 N12 O13 Ni2 0.000(2) . . . . ?
O13 N12 O14 Ni2 0.000(2) . . . . ?
C6 N5 Ni1 N1 -63.00(14) . . . . ?
C6 N5 Ni1 N3 -174.8(3) . . . . ?
C6 N5 Ni1 O1A -46.8(3) . . . . ?
C6 N5 Ni1 N4 38.80(13) . . . . ?
C6 N5 Ni1 O3 -161.97(13) . . . . ?
C6 N5 Ni1 O4 140.58(13) . . . . ?
C1 N3 Ni1 N1 66.58(14) . . . . ?
C1 N3 Ni1 N5 179(11) . . . . ?
C1 N3 Ni1 O1A 51.4(3) . . . . ?
C1 N3 Ni1 N4 -34.77(13) . . . . ?
C1 N3 Ni1 O3 166.00(14) . . . . ?
C1 N3 Ni1 O4 -136.61(13) . . . . ?
C7 N4 Ni1 N1 -177.89(12) . . . . ?
C4 N4 Ni1 N1 61.91(13) . . . . ?
C3 N4 Ni1 N1 -58.40(13) . . . . ?
C7 N4 Ni1 N5 86.23(12) . . . . ?
C4 N4 Ni1 N5 -33.97(11) . . . . ?
C3 N4 Ni1 N5 -154.28(12) . . . . ?
C7 N4 Ni1 N3 -88.66(12) . . . . ?
C4 N4 Ni1 N3 151.14(11) . . . . ?
C3 N4 Ni1 N3 30.83(12) . . . . ?
C7 N4 Ni1 O1A 174.8(3) . . . . ?
C4 N4 Ni1 O1A 54.6(3) . . . . ?
C3 N4 Ni1 O1A -65.7(3) . . . . ?
C7 N4 Ni1 O3 -4.1(2) . . . . ?
C4 N4 Ni1 O3 -124.26(16) . . . . ?
C3 N4 Ni1 O3 115.43(16) . . . . ?
C7 N4 Ni1 O4 0.00(12) . . . . ?
C4 N4 Ni1 O4 -120.19(11) . . . . ?
C3 N4 Ni1 O4 119.49(12) . . . . ?
N2 O3 Ni1 N1 178.61(11) . . . . ?
N2 O3 Ni1 N5 -86.66(11) . . . . ?
N2 O3 Ni1 N3 91.29(12) . . . . ?
N2 O3 Ni1 O1A -174.1(3) . . . . ?
N2 O3 Ni1 N4 4.7(2) . . . . ?
N2 O3 Ni1 O4 0.01(10) . . . . ?
N2 O4 Ni1 N1 -3.5(2) . . . . ?
N2 O4 Ni1 N5 89.37(11) . . . . ?
N2 O4 Ni1 N3 -84.16(11) . . . . ?
N2 O4 Ni1 O1A 35.7(14) . . . . ?
N2 O4 Ni1 N4 -178.30(10) . . . . ?
N2 O4 Ni1 O3 -0.01(10) . . . . ?
C11 N13 Ni2 N13 -174.9(4) . . . 4_565 ?
C11 N13 Ni2 N14 38.96(15) . . . . ?
C11 N13 Ni2 O14 -56.37(15) . . . . ?
C11 N13 Ni2 N11 140.01(15) . . . . ?
C11 N13 Ni2 O13 -113.96(15) . . . . ?
C17 N14 Ni2 N13 -87.12(4) . . . 4_565 ?
C13 N14 Ni2 N13 35.23(13) 4_565 . . 4_565 ?
C13 N14 Ni2 N13 150.53(12) . . . 4_565 ?
C17 N14 Ni2 N13 87.12(4) . . . . ?
C13 N14 Ni2 N13 -150.53(12) 4_565 . . . ?
C13 N14 Ni2 N13 -35.23(13) . . . . ?
C17 N14 Ni2 O14 180.000(1) . . . . ?
C13 N14 Ni2 O14 -57.65(11) 4_565 . . . ?
C13 N14 Ni2 O14 57.65(12) . . . . ?
C17 N14 Ni2 N11 0.0 . . . . ?
C13 N14 Ni2 N11 122.35(11) 4_565 . . . ?
C13 N14 Ni2 N11 -122.35(12) . . . . ?
C17 N14 Ni2 O13 180.000(2) . . . . ?
C13 N14 Ni2 O13 -57.65(11) 4_565 . . . ?
C13 N14 Ni2 O13 57.65(12) . . . . ?
N12 O14 Ni2 N13 85.45(4) . . . 4_565 ?
N12 O14 Ni2 N13 -85.45(4) . . . . ?
N12 O14 Ni2 N14 180.000(1) . . . . ?
N12 O14 Ni2 N11 0.000(2) . . . . ?
N12 O14 Ni2 O13 0.000(1) . . . . ?
N12 O13 Ni2 N13 -94.53(4) . . . 4_565 ?
N12 O13 Ni2 N13 94.53(4) . . . . ?
N12 O13 Ni2 N14 0.000(2) . . . . ?
N12 O13 Ni2 O14 0.000(2) . . . . ?
N12 O13 Ni2 N11 180.000(2) . . . . ?
N5 Ni1 N1 O1 56.1(2) . . . . ?
N3 Ni1 N1 O1 -132.5(2) . . . . ?
O1A Ni1 N1 O1 -13.1(8) . . . . ?
N4 Ni1 N1 O1 -38.2(2) . . . . ?
O3 Ni1 N1 O1 144.02(19) . . . . ?
O4 Ni1 N1 O1 146.97(18) . . . . ?
N5 Ni1 N1 O2 -123.4(3) . . . . ?
N3 Ni1 N1 O2 48.0(3) . . . . ?
O1A Ni1 N1 O2 167.3(10) . . . . ?
N4 Ni1 N1 O2 142.3(3) . . . . ?
O3 Ni1 N1 O2 -35.5(3) . . . . ?
O4 Ni1 N1 O2 -32.6(4) . . . . ?
O2A N1A O1A Ni1 -2.5(13) . . . . ?
N1 Ni1 O1A N1A -0.2(6) . . . . ?
N5 Ni1 O1A N1A -111.6(8) . . . . ?
N3 Ni1 O1A N1A 61.1(8) . . . . ?
N4 Ni1 O1A N1A 155.2(8) . . . . ?
O3 Ni1 O1A N1A -25.3(9) . . . . ?
O4 Ni1 O1A N1A -58.1(19) . . . . ?
N13 Ni2 N11 O11 -174.69(18) 4_565 . . 4_565 ?
N13 Ni2 N11 O11 -2.03(18) . . . 4_565 ?
N14 Ni2 N11 O11 91.64(17) . . . 4_565 ?
O14 Ni2 N11 O11 -88.36(17) . . . 4_565 ?
O13 Ni2 N11 O11 -88.36(17) . . . 4_565 ?
N13 Ni2 N11 O11 2.03(18) 4_565 . . . ?
N13 Ni2 N11 O11 174.69(18) . . . . ?
N14 Ni2 N11 O11 -91.64(17) . . . . ?
O14 Ni2 N11 O11 88.36(17) . . . . ?
O13 Ni2 N11 O11 88.36(17) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3D O2A 0.90 2.64 3.096(18) 112.2 .
N5 H5C O3 0.90 2.22 3.040(2) 151.6 3_557
N5 H5C O2A 0.90 2.57 3.194(13) 127.1 3_557
N5 H5D O11 0.90 2.26 3.114(2) 158.0 4_565
N13 H13D O11 0.90 2.20 2.831(2) 126.5 4_565

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.054

_database_code_depnum_ccdc_archive 'CCDC 994153'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex7_110K
_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;
Dinitro-(3,3-diamino-N-methyldipropylamine)nickel(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H19 N5 Ni O4'
_chemical_formula_sum            'C7 H19 N5 Ni O4'
_chemical_formula_weight         295.98


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'
O O 0.0106 0.0060 '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'


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

_cell_length_a                   7.104(5)
_cell_length_b                   23.968(5)
_cell_length_c                   10.941(5)
_cell_angle_alpha                90.000
_cell_angle_beta                 103.958(5)
_cell_angle_gamma                90.000
_cell_volume                     1807.9(16)
_cell_formula_units_Z            6
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    8101
_cell_measurement_theta_min      3.0576
_cell_measurement_theta_max      29.0585

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)

_exptl_crystal_description       Block
_exptl_crystal_colour            Violet
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936

_exptl_absorpt_coefficient_mu    1.623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.64551
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13240
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0481
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         29.23
_reflns_number_total             7592
_reflns_number_gt                6595
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'POV-RAY for Windows, 3.62 (Cason, 2009)'
_computing_publication_material  'WinGX, 1.80.05 (Farrugia, 1999)'

_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 > 2sigma(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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0409P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.498(12)
_refine_ls_number_reflns         7592
_refine_ls_number_parameters     500
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0732
_refine_ls_wR_factor_gt          0.0710
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      1.002
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3210(6) -0.15512(17) -0.3655(3) 0.0251(8) Uani 1 1 d . . .
H1A H 0.2077 -0.1757 -0.4157 0.030 Uiso 1 1 calc R . .
H1B H 0.4398 -0.1728 -0.3798 0.030 Uiso 1 1 calc R . .
C2 C 0.3116(6) -0.09554(17) -0.4091(3) 0.0249(8) Uani 1 1 d . . .
H2A H 0.3362 -0.0944 -0.4944 0.030 Uiso 1 1 calc R . .
H2B H 0.4162 -0.0742 -0.3521 0.030 Uiso 1 1 calc R . .
C3 C 0.1184(5) -0.06718(16) -0.4133(3) 0.0224(8) Uani 1 1 d . . .
H3A H 0.1098 -0.0333 -0.4661 0.027 Uiso 1 1 calc R . .
H3B H 0.0132 -0.0926 -0.4559 0.027 Uiso 1 1 calc R . .
C4 C -0.1203(5) -0.02763(18) -0.3205(3) 0.0216(9) Uani 1 1 d . . .
H4A H -0.2082 -0.0565 -0.3676 0.026 Uiso 1 1 calc R . .
H4B H -0.1241 0.0045 -0.3779 0.026 Uiso 1 1 calc R . .
C5 C -0.2004(5) -0.00882(18) -0.2122(3) 0.0243(9) Uani 1 1 d . . .
H5A H -0.3236 0.0113 -0.2464 0.029 Uiso 1 1 calc R . .
H5B H -0.1082 0.0180 -0.1610 0.029 Uiso 1 1 calc R . .
C6 C -0.2378(5) -0.05486(17) -0.1272(3) 0.0211(8) Uani 1 1 d . . .
H6A H -0.3079 -0.0394 -0.0668 0.025 Uiso 1 1 calc R . .
H6B H -0.3217 -0.0835 -0.1785 0.025 Uiso 1 1 calc R . .
C7 C 0.2177(5) -0.00535(16) -0.2348(3) 0.0220(8) Uani 1 1 d . . .
H7A H 0.2098 0.0246 -0.2968 0.033 Uiso 1 1 calc R . .
H7B H 0.3502 -0.0201 -0.2117 0.033 Uiso 1 1 calc R . .
H7C H 0.1832 0.0094 -0.1595 0.033 Uiso 1 1 calc R . .
C11 C 0.5502(6) -0.04883(18) 0.3263(3) 0.0259(9) Uani 1 1 d . . .
H11A H 0.5206 -0.0892 0.3186 0.031 Uiso 1 1 calc R . .
H11B H 0.6049 -0.0402 0.4164 0.031 Uiso 1 1 calc R . .
C12 C 0.6969(6) -0.03430(17) 0.2509(4) 0.0291(9) Uani 1 1 d . . .
H12A H 0.8062 -0.0610 0.2732 0.035 Uiso 1 1 calc R . .
H12B H 0.6349 -0.0393 0.1603 0.035 Uiso 1 1 calc R . .
C13 C 0.7769(5) 0.02393(17) 0.2704(4) 0.0212(8) Uani 1 1 d . . .
H13A H 0.8925 0.0259 0.2351 0.025 Uiso 1 1 calc R . .
H13B H 0.8214 0.0305 0.3622 0.025 Uiso 1 1 calc R . .
C14 C 0.7559(5) 0.12253(17) 0.2532(4) 0.0227(8) Uani 1 1 d . . .
H14A H 0.8680 0.1221 0.2143 0.027 Uiso 1 1 calc R . .
H14B H 0.8082 0.1211 0.3456 0.027 Uiso 1 1 calc R . .
C15 C 0.6529(7) 0.17704(17) 0.2218(4) 0.0332(10) Uani 1 1 d . . .
H15A H 0.5758 0.1757 0.1334 0.040 Uiso 1 1 calc R . .
H15B H 0.7508 0.2070 0.2278 0.040 Uiso 1 1 calc R . .
C16 C 0.5202(6) 0.19192(17) 0.3054(3) 0.0232(8) Uani 1 1 d . . .
H16A H 0.5912 0.1885 0.3948 0.028 Uiso 1 1 calc R . .
H16B H 0.4769 0.2311 0.2900 0.028 Uiso 1 1 calc R . .
C17 C 0.5936(4) 0.0657(2) 0.0758(3) 0.0272(8) Uani 1 1 d . . .
H17A H 0.5056 0.0960 0.0383 0.041 Uiso 1 1 calc R . .
H17B H 0.5303 0.0297 0.0514 0.041 Uiso 1 1 calc R . .
H17C H 0.7126 0.0680 0.0456 0.041 Uiso 1 1 calc R . .
C21 C -0.2598(5) 0.19829(18) -0.1452(4) 0.0259(9) Uani 1 1 d . . .
H21A H -0.3461 0.2256 -0.1992 0.031 Uiso 1 1 calc R . .
H21B H -0.3283 0.1834 -0.0834 0.031 Uiso 1 1 calc R . .
C22 C -0.2156(6) 0.15109(17) -0.2256(4) 0.0247(9) Uani 1 1 d . . .
H22A H -0.3348 0.1287 -0.2563 0.030 Uiso 1 1 calc R . .
H22B H -0.1169 0.1265 -0.1726 0.030 Uiso 1 1 calc R . .
C23 C -0.1417(6) 0.17044(17) -0.3390(3) 0.0233(9) Uani 1 1 d . . .
H23A H -0.1444 0.1381 -0.3958 0.028 Uiso 1 1 calc R . .
H23B H -0.2333 0.1986 -0.3857 0.028 Uiso 1 1 calc R . .
C24 C 0.0889(6) 0.21083(17) -0.4348(3) 0.0254(8) Uani 1 1 d . . .
H24A H -0.0191 0.2355 -0.4771 0.030 Uiso 1 1 calc R . .
H24B H 0.0814 0.1766 -0.4865 0.030 Uiso 1 1 calc R . .
C25 C 0.2784(5) 0.24024(17) -0.4345(3) 0.0254(8) Uani 1 1 d . . .
H25A H 0.3006 0.2384 -0.5204 0.030 Uiso 1 1 calc R . .
H25B H 0.3859 0.2200 -0.3773 0.030 Uiso 1 1 calc R . .
C26 C 0.2847(6) 0.30110(18) -0.3938(3) 0.0293(9) Uani 1 1 d . . .
H26A H 0.4017 0.3192 -0.4098 0.035 Uiso 1 1 calc R . .
H26B H 0.1694 0.3209 -0.4439 0.035 Uiso 1 1 calc R . .
C27 C 0.1990(5) 0.15115(17) -0.2540(4) 0.0241(8) Uani 1 1 d . . .
H27A H 0.1938 0.1208 -0.3146 0.036 Uiso 1 1 calc R . .
H27B H 0.1673 0.1366 -0.1777 0.036 Uiso 1 1 calc R . .
H27C H 0.3297 0.1672 -0.2323 0.036 Uiso 1 1 calc R . .
N2 N 0.3713(5) -0.12779(15) 0.0572(3) 0.0252(7) Uani 1 1 d . . .
N3 N 0.3224(5) -0.15907(14) -0.2306(3) 0.0210(7) Uani 1 1 d . A .
H3C H 0.4431 -0.1478 -0.1858 0.025 Uiso 1 1 calc R . .
H3D H 0.3111 -0.1963 -0.2128 0.025 Uiso 1 1 calc R . .
N4 N 0.0814(4) -0.05067(13) -0.2896(2) 0.0171(6) Uani 1 1 d . A .
N5 N -0.0574(4) -0.08114(14) -0.0572(3) 0.0208(7) Uani 1 1 d . A .
H5C H -0.0897 -0.1085 -0.0067 0.025 Uiso 1 1 calc R . .
H5D H 0.0133 -0.0546 -0.0047 0.025 Uiso 1 1 calc R . .
N12 N 0.3874(4) 0.0692(2) 0.5193(2) 0.0334(6) Uani 1 1 d . . .
N13 N 0.3731(5) -0.01674(14) 0.2795(3) 0.0244(7) Uani 1 1 d . B .
H13C H 0.2859 -0.0271 0.3253 0.029 Uiso 1 1 calc R . .
H13D H 0.3214 -0.0274 0.1975 0.029 Uiso 1 1 calc R . .
N14 N 0.6422(3) 0.07105(16) 0.21432(19) 0.0152(4) Uani 1 1 d . B .
N15 N 0.3508(5) 0.15480(15) 0.2799(3) 0.0267(7) Uani 1 1 d . B .
H15C H 0.2754 0.1640 0.2017 0.032 Uiso 1 1 calc R . .
H15D H 0.2797 0.1632 0.3375 0.032 Uiso 1 1 calc R . .
N22 N 0.3449(5) 0.27522(16) 0.0310(3) 0.0330(9) Uani 1 1 d . . .
N23 N -0.0800(4) 0.22636(13) -0.0779(3) 0.0204(7) Uani 1 1 d . C .
H23C H -0.0062 0.2007 -0.0245 0.024 Uiso 1 1 calc R . .
H23D H -0.1135 0.2539 -0.0286 0.024 Uiso 1 1 calc R . .
N24 N 0.0572(4) 0.19481(13) -0.3102(3) 0.0188(6) Uani 1 1 d . C .
N25 N 0.2885(5) 0.30546(14) -0.2589(3) 0.0233(7) Uani 1 1 d . C .
H25C H 0.2746 0.3426 -0.2419 0.028 Uiso 1 1 calc R . .
H25D H 0.4107 0.2951 -0.2147 0.028 Uiso 1 1 calc R . .
O3 O 0.3588(4) -0.08466(11) -0.0118(2) 0.0227(6) Uani 1 1 d . A .
O4 O 0.2485(4) -0.16447(11) 0.0092(2) 0.0253(6) Uani 1 1 d . A .
O13 O 0.2333(3) 0.06745(18) 0.4350(2) 0.0341(6) Uani 1 1 d . B .
O14 O 0.5361(3) 0.07127(15) 0.47354(17) 0.0253(4) Uani 1 1 d . B .
O23 O 0.2183(4) 0.31149(13) -0.0171(2) 0.0306(7) Uani 1 1 d . C .
O24 O 0.3346(4) 0.23280(12) -0.0379(2) 0.0260(6) Uani 1 1 d . C .
Ni1 Ni 0.12096(6) -0.116461(15) -0.15866(4) 0.01634(10) Uani 1 1 d . . .
Ni2 Ni 0.38970(4) 0.06934(2) 0.28302(3) 0.01629(9) Uani 1 1 d . . .
Ni3 Ni 0.09270(6) 0.261770(16) -0.18280(4) 0.01764(10) Uani 1 1 d . . .
N1 N -0.068(4) -0.1733(12) -0.257(3) 0.028(5) Uiso 0.120(8) 1 d PD A 1
O1 O -0.229(4) -0.1602(14) -0.310(3) 0.049(5) Uiso 0.120(8) 1 d PD A 1
O2 O -0.039(5) -0.2240(10) -0.250(3) 0.018(4) Uiso 0.120(8) 1 d PD A 1
N1A N -0.1478(6) -0.20704(15) -0.2777(3) 0.0252(10) Uani 0.880(8) 1 d PD A 2
O1A O -0.1143(5) -0.15421(13) -0.2719(3) 0.0231(9) Uani 0.880(8) 1 d PD A 2
O2A O -0.0162(5) -0.23616(17) -0.2109(4) 0.0318(9) Uani 0.880(8) 1 d PD A 2
N11 N 0.1757(5) 0.0713(3) 0.1074(4) 0.0210(10) Uani 0.680(8) 1 d PD B 3
O11 O 0.1081(9) 0.1155(2) 0.0519(5) 0.0328(14) Uani 0.680(8) 1 d PD B 3
O12 O 0.1103(7) 0.02739(19) 0.0580(4) 0.0345(14) Uani 0.680(8) 1 d PD B 3
N11A N 0.0860(10) 0.0757(4) 0.0277(7) 0.013(2) Uiso 0.320(8) 1 d PD B 4
O11A O 0.1741(12) 0.0464(4) 0.1250(8) 0.019(2) Uiso 0.320(8) 1 d PD B 4
O12A O 0.1445(19) 0.1267(5) 0.0342(13) 0.031(3) Uiso 0.320(8) 1 d PD B 4
N21 N -0.109(4) 0.3224(12) -0.271(3) 0.028(5) Uiso 0.129(8) 1 d PD C 5
O22 O -0.092(4) 0.3729(11) -0.285(2) 0.018(4) Uiso 0.129(8) 1 d PD C 5
O21 O -0.262(4) 0.3055(12) -0.330(2) 0.049(5) Uiso 0.129(8) 1 d PD C 5
N21A N -0.1860(6) 0.34959(17) -0.3044(3) 0.0277(11) Uani 0.871(8) 1 d PD C 6
O21A O -0.1467(5) 0.29748(14) -0.2970(3) 0.0255(9) Uani 0.871(8) 1 d PD C 6
O22A O -0.0524(5) 0.37999(17) -0.2397(4) 0.0341(10) Uani 0.871(8) 1 d PD C 6


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N3 1.476(4) . ?
C1 C2 1.502(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.523(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N4 1.493(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.496(5) . ?
C4 C5 1.502(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.508(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N5 1.467(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 N4 1.482(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C11 N13 1.458(5) . ?
C11 C12 1.518(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.503(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N14 1.512(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 N14 1.480(5) . ?
C14 C15 1.496(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.507(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 N15 1.468(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 N14 1.477(3) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C21 N23 1.473(5) . ?
C21 C22 1.512(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.531(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 N24 1.491(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 N24 1.484(5) . ?
C24 C25 1.519(5) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.523(6) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 N25 1.473(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 N24 1.480(5) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
N2 O4 1.260(4) . ?
N2 O3 1.271(4) . ?
N3 Ni1 2.063(3) . ?
N3 H3C 0.9200 . ?
N3 H3D 0.9200 . ?
N4 Ni1 2.103(3) . ?
N5 Ni1 2.058(3) . ?
N5 H5C 0.9200 . ?
N5 H5D 0.9200 . ?
N12 O13 1.250(3) . ?
N12 O14 1.274(3) . ?
N13 Ni2 2.066(3) . ?
N13 H13C 0.9200 . ?
N13 H13D 0.9200 . ?
N14 Ni2 2.106(2) . ?
N15 Ni2 2.066(4) . ?
N15 H15C 0.9200 . ?
N15 H15D 0.9200 . ?
N22 O24 1.257(4) . ?
N22 O23 1.270(5) . ?
N23 Ni3 2.055(3) . ?
N23 H23C 0.9200 . ?
N23 H23D 0.9200 . ?
N24 Ni3 2.101(3) . ?
N25 Ni3 2.069(3) . ?
N25 H25C 0.9200 . ?
N25 H25D 0.9200 . ?
O3 Ni1 2.169(3) . ?
O4 Ni1 2.171(3) . ?
O13 Ni2 2.212(2) . ?
O14 Ni2 2.094(2) . ?
O23 Ni3 2.173(3) . ?
O24 Ni3 2.153(3) . ?
Ni1 N1 2.03(3) . ?
Ni1 O1A 2.036(3) . ?
Ni2 O11A 2.088(9) . ?
Ni2 N11 2.144(4) . ?
Ni3 O21A 2.040(3) . ?
Ni3 N21 2.10(3) . ?
N1 O1 1.198(10) . ?
N1 O2 1.231(19) . ?
N1A O2A 1.251(5) . ?
N1A O1A 1.287(4) . ?
N11 O12 1.223(6) . ?
N11 O11 1.257(7) . ?
N11A O12A 1.286(9) . ?
N11A O11A 1.303(8) . ?
N21 O21 1.192(10) . ?
N21 O22 1.231(19) . ?
N21A O22A 1.269(5) . ?
N21A O21A 1.278(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 C1 C2 111.6(3) . . ?
N3 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N3 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
C1 C2 C3 113.9(3) . . ?
C1 C2 H2A 108.8 . . ?
C3 C2 H2A 108.8 . . ?
C1 C2 H2B 108.8 . . ?
C3 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
N4 C3 C2 116.5(3) . . ?
N4 C3 H3A 108.2 . . ?
C2 C3 H3A 108.2 . . ?
N4 C3 H3B 108.2 . . ?
C2 C3 H3B 108.2 . . ?
H3A C3 H3B 107.3 . . ?
N4 C4 C5 117.2(3) . . ?
N4 C4 H4A 108.0 . . ?
C5 C4 H4A 108.0 . . ?
N4 C4 H4B 108.0 . . ?
C5 C4 H4B 108.0 . . ?
H4A C4 H4B 107.3 . . ?
C4 C5 C6 115.1(4) . . ?
C4 C5 H5A 108.5 . . ?
C6 C5 H5A 108.5 . . ?
C4 C5 H5B 108.5 . . ?
C6 C5 H5B 108.5 . . ?
H5A C5 H5B 107.5 . . ?
N5 C6 C5 112.0(3) . . ?
N5 C6 H6A 109.2 . . ?
C5 C6 H6A 109.2 . . ?
N5 C6 H6B 109.2 . . ?
C5 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N13 C11 C12 109.6(3) . . ?
N13 C11 H11A 109.7 . . ?
C12 C11 H11A 109.7 . . ?
N13 C11 H11B 109.7 . . ?
C12 C11 H11B 109.7 . . ?
H11A C11 H11B 108.2 . . ?
C13 C12 C11 114.9(3) . . ?
C13 C12 H12A 108.5 . . ?
C11 C12 H12A 108.5 . . ?
C13 C12 H12B 108.5 . . ?
C11 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?
C12 C13 N14 117.1(3) . . ?
C12 C13 H13A 108.0 . . ?
N14 C13 H13A 108.0 . . ?
C12 C13 H13B 108.0 . . ?
N14 C13 H13B 108.0 . . ?
H13A C13 H13B 107.3 . . ?
N14 C14 C15 117.3(3) . . ?
N14 C14 H14A 108.0 . . ?
C15 C14 H14A 108.0 . . ?
N14 C14 H14B 108.0 . . ?
C15 C14 H14B 108.0 . . ?
H14A C14 H14B 107.2 . . ?
C14 C15 C16 114.2(3) . . ?
C14 C15 H15A 108.7 . . ?
C16 C15 H15A 108.7 . . ?
C14 C15 H15B 108.7 . . ?
C16 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
N15 C16 C15 110.2(3) . . ?
N15 C16 H16A 109.6 . . ?
C15 C16 H16A 109.6 . . ?
N15 C16 H16B 109.6 . . ?
C15 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
N14 C17 H17A 109.5 . . ?
N14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N23 C21 C22 110.9(3) . . ?
N23 C21 H21A 109.5 . . ?
C22 C21 H21A 109.5 . . ?
N23 C21 H21B 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 108.1 . . ?
C21 C22 C23 113.9(4) . . ?
C21 C22 H22A 108.8 . . ?
C23 C22 H22A 108.8 . . ?
C21 C22 H22B 108.8 . . ?
C23 C22 H22B 108.8 . . ?
H22A C22 H22B 107.7 . . ?
N24 C23 C22 116.2(3) . . ?
N24 C23 H23A 108.2 . . ?
C22 C23 H23A 108.2 . . ?
N24 C23 H23B 108.2 . . ?
C22 C23 H23B 108.2 . . ?
H23A C23 H23B 107.4 . . ?
N24 C24 C25 116.7(3) . . ?
N24 C24 H24A 108.1 . . ?
C25 C24 H24A 108.1 . . ?
N24 C24 H24B 108.1 . . ?
C25 C24 H24B 108.1 . . ?
H24A C24 H24B 107.3 . . ?
C24 C25 C26 114.1(3) . . ?
C24 C25 H25A 108.7 . . ?
C26 C25 H25A 108.7 . . ?
C24 C25 H25B 108.7 . . ?
C26 C25 H25B 108.7 . . ?
H25A C25 H25B 107.6 . . ?
N25 C26 C25 110.7(3) . . ?
N25 C26 H26A 109.5 . . ?
C25 C26 H26A 109.5 . . ?
N25 C26 H26B 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 108.1 . . ?
N24 C27 H27A 109.5 . . ?
N24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O4 N2 O3 112.2(3) . . ?
C1 N3 Ni1 120.8(2) . . ?
C1 N3 H3C 107.1 . . ?
Ni1 N3 H3C 107.1 . . ?
C1 N3 H3D 107.1 . . ?
Ni1 N3 H3D 107.1 . . ?
H3C N3 H3D 106.8 . . ?
C7 N4 C3 108.7(3) . . ?
C7 N4 C4 108.5(3) . . ?
C3 N4 C4 105.1(2) . . ?
C7 N4 Ni1 107.9(2) . . ?
C3 N4 Ni1 113.3(2) . . ?
C4 N4 Ni1 113.2(2) . . ?
C6 N5 Ni1 118.0(2) . . ?
C6 N5 H5C 107.8 . . ?
Ni1 N5 H5C 107.8 . . ?
C6 N5 H5D 107.8 . . ?
Ni1 N5 H5D 107.8 . . ?
H5C N5 H5D 107.2 . . ?
O13 N12 O14 111.9(2) . . ?
C11 N13 Ni2 118.6(2) . . ?
C11 N13 H13C 107.7 . . ?
Ni2 N13 H13C 107.7 . . ?
C11 N13 H13D 107.7 . . ?
Ni2 N13 H13D 107.7 . . ?
H13C N13 H13D 107.1 . . ?
C17 N14 C14 110.1(3) . . ?
C17 N14 C13 108.7(3) . . ?
C14 N14 C13 104.9(2) . . ?
C17 N14 Ni2 110.88(16) . . ?
C14 N14 Ni2 111.5(2) . . ?
C13 N14 Ni2 110.5(2) . . ?
C16 N15 Ni2 119.8(3) . . ?
C16 N15 H15C 107.4 . . ?
Ni2 N15 H15C 107.4 . . ?
C16 N15 H15D 107.4 . . ?
Ni2 N15 H15D 107.4 . . ?
H15C N15 H15D 106.9 . . ?
O24 N22 O23 111.8(3) . . ?
C21 N23 Ni3 118.2(2) . . ?
C21 N23 H23C 107.8 . . ?
Ni3 N23 H23C 107.8 . . ?
C21 N23 H23D 107.8 . . ?
Ni3 N23 H23D 107.8 . . ?
H23C N23 H23D 107.1 . . ?
C27 N24 C24 109.0(3) . . ?
C27 N24 C23 109.0(3) . . ?
C24 N24 C23 104.7(3) . . ?
C27 N24 Ni3 107.7(2) . . ?
C24 N24 Ni3 113.0(2) . . ?
C23 N24 Ni3 113.3(2) . . ?
C26 N25 Ni3 121.0(3) . . ?
C26 N25 H25C 107.1 . . ?
Ni3 N25 H25C 107.1 . . ?
C26 N25 H25D 107.1 . . ?
Ni3 N25 H25D 107.1 . . ?
H25C N25 H25D 106.8 . . ?
N2 O3 Ni1 94.9(2) . . ?
N2 O4 Ni1 95.1(2) . . ?
N12 O13 Ni2 92.54(15) . . ?
N12 O14 Ni2 97.47(17) . . ?
N22 O23 Ni3 94.5(2) . . ?
N22 O24 Ni3 95.8(2) . . ?
N1 Ni1 O1A 16.0(7) . . ?
N1 Ni1 N5 98.6(9) . . ?
O1A Ni1 N5 89.39(14) . . ?
N1 Ni1 N3 83.9(9) . . ?
O1A Ni1 N3 95.21(15) . . ?
N5 Ni1 N3 169.72(12) . . ?
N1 Ni1 N4 100.3(9) . . ?
O1A Ni1 N4 87.90(12) . . ?
N5 Ni1 N4 93.47(12) . . ?
N3 Ni1 N4 95.88(12) . . ?
N1 Ni1 O3 157.8(8) . . ?
O1A Ni1 O3 169.99(12) . . ?
N5 Ni1 O3 85.80(12) . . ?
N3 Ni1 O3 88.19(12) . . ?
N4 Ni1 O3 101.14(11) . . ?
N1 Ni1 O4 100.4(9) . . ?
O1A Ni1 O4 113.13(12) . . ?
N5 Ni1 O4 86.97(11) . . ?
N3 Ni1 O4 82.77(11) . . ?
N4 Ni1 O4 158.97(11) . . ?
O3 Ni1 O4 57.89(10) . . ?
N15 Ni2 N13 169.35(10) . . ?
N15 Ni2 O11A 100.3(2) . . ?
N13 Ni2 O11A 72.2(2) . . ?
N15 Ni2 O14 91.54(13) . . ?
N13 Ni2 O14 93.05(13) . . ?
O11A Ni2 O14 156.8(2) . . ?
N15 Ni2 N14 95.56(14) . . ?
N13 Ni2 N14 93.58(14) . . ?
O11A Ni2 N14 103.2(2) . . ?
O14 Ni2 N14 95.36(8) . . ?
N15 Ni2 N11 84.27(19) . . ?
N13 Ni2 N11 88.88(19) . . ?
O11A Ni2 N11 17.0(2) . . ?
O14 Ni2 N11 165.12(10) . . ?
N14 Ni2 N11 99.24(11) . . ?
N15 Ni2 O13 86.75(14) . . ?
N13 Ni2 O13 87.53(14) . . ?
O11A Ni2 O13 102.5(2) . . ?
O14 Ni2 O13 58.06(8) . . ?
N14 Ni2 O13 153.41(9) . . ?
N11 Ni2 O13 107.34(11) . . ?
O21A Ni3 N23 89.61(14) . . ?
O21A Ni3 N25 94.79(15) . . ?
N23 Ni3 N25 169.58(12) . . ?
O21A Ni3 N24 88.01(12) . . ?
N23 Ni3 N24 93.60(12) . . ?
N25 Ni3 N24 95.98(13) . . ?
O21A Ni3 N21 19.0(6) . . ?
N23 Ni3 N21 96.2(7) . . ?
N25 Ni3 N21 85.2(7) . . ?
N24 Ni3 N21 105.3(8) . . ?
O21A Ni3 O24 170.36(11) . . ?
N23 Ni3 O24 86.19(12) . . ?
N25 Ni3 O24 87.99(12) . . ?
N24 Ni3 O24 100.90(11) . . ?
N21 Ni3 O24 153.5(7) . . ?
O21A Ni3 O23 113.24(13) . . ?
N23 Ni3 O23 86.63(11) . . ?
N25 Ni3 O23 82.96(12) . . ?
N24 Ni3 O23 158.74(12) . . ?
N21 Ni3 O23 95.8(8) . . ?
O24 Ni3 O23 57.88(11) . . ?
O1 N1 O2 115(3) . . ?
O1 N1 Ni1 121(2) . . ?
O2 N1 Ni1 123(2) . . ?
O2A N1A O1A 114.6(4) . . ?
N1A O1A Ni1 125.6(3) . . ?
O12 N11 O11 116.9(4) . . ?
O12 N11 Ni2 119.3(4) . . ?
O11 N11 Ni2 123.9(4) . . ?
O12A N11A O11A 112.5(10) . . ?
N11A O11A Ni2 130.2(7) . . ?
O21 N21 O22 112(3) . . ?
O21 N21 Ni3 116(3) . . ?
O22 N21 Ni3 131(2) . . ?
O22A N21A O21A 113.8(4) . . ?
N21A O21A Ni3 125.9(3) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 C1 C2 C3 -69.2(4) . . . . ?
C1 C2 C3 N4 75.0(4) . . . . ?
N4 C4 C5 C6 -68.0(4) . . . . ?
C4 C5 C6 N5 67.2(4) . . . . ?
N13 C11 C12 C13 68.2(4) . . . . ?
C11 C12 C13 N14 -72.0(4) . . . . ?
N14 C14 C15 C16 76.1(5) . . . . ?
C14 C15 C16 N15 -69.9(5) . . . . ?
N23 C21 C22 C23 -69.2(4) . . . . ?
C21 C22 C23 N24 70.4(4) . . . . ?
N24 C24 C25 C26 -75.5(4) . . . . ?
C24 C25 C26 N25 68.9(4) . . . . ?
C2 C1 N3 Ni1 49.4(4) . . . . ?
C2 C3 N4 C7 67.5(4) . . . . ?
C2 C3 N4 C4 -176.4(3) . . . . ?
C2 C3 N4 Ni1 -52.3(4) . . . . ?
C5 C4 N4 C7 -65.5(4) . . . . ?
C5 C4 N4 C3 178.3(3) . . . . ?
C5 C4 N4 Ni1 54.2(4) . . . . ?
C5 C6 N5 Ni1 -58.3(4) . . . . ?
C12 C11 N13 Ni2 -59.2(4) . . . . ?
C15 C14 N14 C17 69.0(4) . . . . ?
C15 C14 N14 C13 -174.2(4) . . . . ?
C15 C14 N14 Ni2 -54.5(4) . . . . ?
C12 C13 N14 C17 -64.8(4) . . . . ?
C12 C13 N14 C14 177.5(3) . . . . ?
C12 C13 N14 Ni2 57.2(4) . . . . ?
C15 C16 N15 Ni2 52.3(4) . . . . ?
C22 C21 N23 Ni3 59.4(4) . . . . ?
C25 C24 N24 C27 -66.8(4) . . . . ?
C25 C24 N24 C23 176.7(3) . . . . ?
C25 C24 N24 Ni3 52.9(4) . . . . ?
C22 C23 N24 C27 64.7(4) . . . . ?
C22 C23 N24 C24 -178.8(3) . . . . ?
C22 C23 N24 Ni3 -55.2(4) . . . . ?
C25 C26 N25 Ni3 -49.2(4) . . . . ?
O4 N2 O3 Ni1 0.0(3) . . . . ?
O3 N2 O4 Ni1 0.0(3) . . . . ?
O14 N12 O13 Ni2 0.3(4) . . . . ?
O13 N12 O14 Ni2 -0.3(4) . . . . ?
O24 N22 O23 Ni3 0.9(3) . . . . ?
O23 N22 O24 Ni3 -0.9(3) . . . . ?
C6 N5 Ni1 N1 -59.7(9) . . . . ?
C6 N5 Ni1 O1A -46.6(3) . . . . ?
C6 N5 Ni1 N3 -163.4(6) . . . . ?
C6 N5 Ni1 N4 41.3(3) . . . . ?
C6 N5 Ni1 O3 142.2(3) . . . . ?
C6 N5 Ni1 O4 -159.8(3) . . . . ?
C1 N3 Ni1 N1 71.0(9) . . . . ?
C1 N3 Ni1 O1A 59.6(3) . . . . ?
C1 N3 Ni1 N5 175.9(6) . . . . ?
C1 N3 Ni1 N4 -28.8(3) . . . . ?
C1 N3 Ni1 O3 -129.8(3) . . . . ?
C1 N3 Ni1 O4 172.3(3) . . . . ?
C7 N4 Ni1 N1 -177.3(9) . . . . ?
C3 N4 Ni1 N1 -57.0(9) . . . . ?
C4 N4 Ni1 N1 62.6(9) . . . . ?
C7 N4 Ni1 O1A 172.5(2) . . . . ?
C3 N4 Ni1 O1A -67.1(2) . . . . ?
C4 N4 Ni1 O1A 52.4(3) . . . . ?
C7 N4 Ni1 N5 83.3(2) . . . . ?
C3 N4 Ni1 N5 -156.4(2) . . . . ?
C4 N4 Ni1 N5 -36.8(2) . . . . ?
C7 N4 Ni1 N3 -92.4(2) . . . . ?
C3 N4 Ni1 N3 27.9(2) . . . . ?
C4 N4 Ni1 N3 147.5(2) . . . . ?
C7 N4 Ni1 O3 -3.1(2) . . . . ?
C3 N4 Ni1 O3 117.2(2) . . . . ?
C4 N4 Ni1 O3 -123.2(2) . . . . ?
C7 N4 Ni1 O4 -7.3(4) . . . . ?
C3 N4 Ni1 O4 113.0(3) . . . . ?
C4 N4 Ni1 O4 -127.4(3) . . . . ?
N2 O3 Ni1 N1 -14(3) . . . . ?
N2 O3 Ni1 O1A 27.5(8) . . . . ?
N2 O3 Ni1 N5 89.1(2) . . . . ?
N2 O3 Ni1 N3 -82.6(2) . . . . ?
N2 O3 Ni1 N4 -178.2(2) . . . . ?
N2 O3 Ni1 O4 0.01(19) . . . . ?
N2 O4 Ni1 N1 174.8(9) . . . . ?
N2 O4 Ni1 O1A -175.0(2) . . . . ?
N2 O4 Ni1 N5 -87.0(2) . . . . ?
N2 O4 Ni1 N3 92.4(2) . . . . ?
N2 O4 Ni1 N4 4.8(4) . . . . ?
N2 O4 Ni1 O3 -0.01(19) . . . . ?
C16 N15 Ni2 N13 177.8(5) . . . . ?
C16 N15 Ni2 O11A -137.8(3) . . . . ?
C16 N15 Ni2 O14 62.3(3) . . . . ?
C16 N15 Ni2 N14 -33.3(3) . . . . ?
C16 N15 Ni2 N11 -132.0(3) . . . . ?
C16 N15 Ni2 O13 120.2(3) . . . . ?
C11 N13 Ni2 N15 -167.1(5) . . . . ?
C11 N13 Ni2 O11A 146.5(4) . . . . ?
C11 N13 Ni2 O14 -51.7(3) . . . . ?
C11 N13 Ni2 N14 43.9(3) . . . . ?
C11 N13 Ni2 N11 143.0(3) . . . . ?
C11 N13 Ni2 O13 -109.5(3) . . . . ?
N12 O14 Ni2 N15 85.4(3) . . . . ?
N12 O14 Ni2 N13 -85.0(3) . . . . ?
N12 O14 Ni2 O11A -35.8(7) . . . . ?
N12 O14 Ni2 N14 -178.9(3) . . . . ?
N12 O14 Ni2 N11 12.2(9) . . . . ?
N12 O14 Ni2 O13 0.2(3) . . . . ?
C17 N14 Ni2 N15 -92.3(3) . . . . ?
C14 N14 Ni2 N15 30.8(2) . . . . ?
C13 N14 Ni2 N15 147.1(2) . . . . ?
C17 N14 Ni2 N13 82.3(3) . . . . ?
C14 N14 Ni2 N13 -154.7(2) . . . . ?
C13 N14 Ni2 N13 -38.4(2) . . . . ?
C17 N14 Ni2 O11A 9.7(4) . . . . ?
C14 N14 Ni2 O11A 132.8(3) . . . . ?
C13 N14 Ni2 O11A -110.9(3) . . . . ?
C17 N14 Ni2 O14 175.7(3) . . . . ?
C14 N14 Ni2 O14 -61.3(2) . . . . ?
C13 N14 Ni2 O14 55.0(3) . . . . ?
C17 N14 Ni2 N11 -7.2(4) . . . . ?
C14 N14 Ni2 N11 115.8(3) . . . . ?
C13 N14 Ni2 N11 -127.8(3) . . . . ?
C17 N14 Ni2 O13 173.9(3) . . . . ?
C14 N14 Ni2 O13 -63.1(4) . . . . ?
C13 N14 Ni2 O13 53.2(5) . . . . ?
N12 O13 Ni2 N15 -94.1(3) . . . . ?
N12 O13 Ni2 N13 94.9(3) . . . . ?
N12 O13 Ni2 O11A 166.1(4) . . . . ?
N12 O13 Ni2 O14 -0.2(3) . . . . ?
N12 O13 Ni2 N14 1.9(5) . . . . ?
N12 O13 Ni2 N11 -177.0(3) . . . . ?
C21 N23 Ni3 O21A 46.6(3) . . . . ?
C21 N23 Ni3 N25 161.8(6) . . . . ?
C21 N23 Ni3 N24 -41.3(3) . . . . ?
C21 N23 Ni3 N21 64.5(8) . . . . ?
C21 N23 Ni3 O24 -142.0(3) . . . . ?
C21 N23 Ni3 O23 160.0(3) . . . . ?
C26 N25 Ni3 O21A -59.2(3) . . . . ?
C26 N25 Ni3 N23 -173.9(6) . . . . ?
C26 N25 Ni3 N24 29.3(3) . . . . ?
C26 N25 Ni3 N21 -75.6(8) . . . . ?
C26 N25 Ni3 O24 130.1(3) . . . . ?
C26 N25 Ni3 O23 -172.0(3) . . . . ?
C27 N24 Ni3 O21A -173.1(2) . . . . ?
C24 N24 Ni3 O21A 66.4(2) . . . . ?
C23 N24 Ni3 O21A -52.5(3) . . . . ?
C27 N24 Ni3 N23 -83.6(2) . . . . ?
C24 N24 Ni3 N23 155.9(2) . . . . ?
C23 N24 Ni3 N23 37.0(3) . . . . ?
C27 N24 Ni3 N25 92.3(2) . . . . ?
C24 N24 Ni3 N25 -28.2(2) . . . . ?
C23 N24 Ni3 N25 -147.1(3) . . . . ?
C27 N24 Ni3 N21 178.9(8) . . . . ?
C24 N24 Ni3 N21 58.4(8) . . . . ?
C23 N24 Ni3 N21 -60.4(8) . . . . ?
C27 N24 Ni3 O24 3.2(2) . . . . ?
C24 N24 Ni3 O24 -117.3(2) . . . . ?
C23 N24 Ni3 O24 123.8(2) . . . . ?
C27 N24 Ni3 O23 6.3(5) . . . . ?
C24 N24 Ni3 O23 -114.2(3) . . . . ?
C23 N24 Ni3 O23 127.0(3) . . . . ?
N22 O24 Ni3 O21A -23.5(9) . . . . ?
N22 O24 Ni3 N23 -87.9(2) . . . . ?
N22 O24 Ni3 N25 83.5(2) . . . . ?
N22 O24 Ni3 N24 179.2(2) . . . . ?
N22 O24 Ni3 N21 8.4(17) . . . . ?
N22 O24 Ni3 O23 0.6(2) . . . . ?
N22 O23 Ni3 O21A 175.2(2) . . . . ?
N22 O23 Ni3 N23 87.1(2) . . . . ?
N22 O23 Ni3 N25 -92.6(2) . . . . ?
N22 O23 Ni3 N24 -4.2(4) . . . . ?
N22 O23 Ni3 N21 -177.0(8) . . . . ?
N22 O23 Ni3 O24 -0.5(2) . . . . ?
O1A Ni1 N1 O1 -7(2) . . . . ?
N5 Ni1 N1 O1 48(3) . . . . ?
N3 Ni1 N1 O1 -142(3) . . . . ?
N4 Ni1 N1 O1 -47(3) . . . . ?
O3 Ni1 N1 O1 148(2) . . . . ?
O4 Ni1 N1 O1 137(3) . . . . ?
O1A Ni1 N1 O2 -175(7) . . . . ?
N5 Ni1 N1 O2 -119(3) . . . . ?
N3 Ni1 N1 O2 51(3) . . . . ?
N4 Ni1 N1 O2 146(3) . . . . ?
O3 Ni1 N1 O2 -19(5) . . . . ?
O4 Ni1 N1 O2 -31(3) . . . . ?
O2A N1A O1A Ni1 -3.6(5) . . . . ?
N1 Ni1 O1A N1A 13(4) . . . . ?
N5 Ni1 O1A N1A -112.1(4) . . . . ?
N3 Ni1 O1A N1A 58.7(4) . . . . ?
N4 Ni1 O1A N1A 154.4(4) . . . . ?
O3 Ni1 O1A N1A -50.9(10) . . . . ?
O4 Ni1 O1A N1A -25.7(4) . . . . ?
N15 Ni2 N11 O12 -172.2(4) . . . . ?
N13 Ni2 N11 O12 -0.4(3) . . . . ?
O11A Ni2 N11 O12 -11.8(9) . . . . ?
O14 Ni2 N11 O12 -98.1(8) . . . . ?
N14 Ni2 N11 O12 93.0(4) . . . . ?
O13 Ni2 N11 O12 -87.5(4) . . . . ?
N15 Ni2 N11 O11 6.1(5) . . . . ?
N13 Ni2 N11 O11 177.9(5) . . . . ?
O11A Ni2 N11 O11 166.5(12) . . . . ?
O14 Ni2 N11 O11 80.2(9) . . . . ?
N14 Ni2 N11 O11 -88.7(5) . . . . ?
O13 Ni2 N11 O11 90.8(5) . . . . ?
O12A N11A O11A Ni2 -0.5(12) . . . . ?
N15 Ni2 O11A N11A 21.2(8) . . . . ?
N13 Ni2 O11A N11A -166.6(9) . . . . ?
O14 Ni2 O11A N11A 140.9(6) . . . . ?
N14 Ni2 O11A N11A -77.1(8) . . . . ?
N11 Ni2 O11A N11A 1.4(5) . . . . ?
O13 Ni2 O11A N11A 110.1(8) . . . . ?
O21A Ni3 N21 O21 12.3(17) . . . . ?
N23 Ni3 N21 O21 -58(3) . . . . ?
N25 Ni3 N21 O21 132(3) . . . . ?
N24 Ni3 N21 O21 37(3) . . . . ?
O24 Ni3 N21 O21 -151.9(18) . . . . ?
O23 Ni3 N21 O21 -145(2) . . . . ?
O21A Ni3 N21 O22 -158(5) . . . . ?
N23 Ni3 N21 O22 131(3) . . . . ?
N25 Ni3 N21 O22 -38(3) . . . . ?
N24 Ni3 N21 O22 -133(3) . . . . ?
O24 Ni3 N21 O22 38(4) . . . . ?
O23 Ni3 N21 O22 44(3) . . . . ?
O22A N21A O21A Ni3 5.3(6) . . . . ?
N23 Ni3 O21A N21A 111.1(4) . . . . ?
N25 Ni3 O21A N21A -59.4(4) . . . . ?
N24 Ni3 O21A N21A -155.2(4) . . . . ?
N21 Ni3 O21A N21A 1(2) . . . . ?
O24 Ni3 O21A N21A 47.0(10) . . . . ?
O23 Ni3 O21A N21A 25.0(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3C N22 0.92 2.70 3.217(5) 116.1 2_645
N3 H3D O2 0.92 2.51 2.96(3) 110.8 .
N3 H3D O2A 0.92 2.52 3.082(5) 119.8 .
N5 H5C O23 0.92 2.17 3.006(4) 151.1 2_545
N5 H5C O22A 0.92 2.66 3.287(6) 126.5 2_545
N5 H5D O12 0.92 2.14 3.008(5) 156.8 .
N13 H13D O12 0.92 2.28 2.880(5) 122.4 .
N15 H15C O12A 0.92 2.05 2.815(15) 139.8 .
N15 H15C O11 0.92 2.12 2.830(6) 132.7 .
N23 H23C O12A 0.92 2.09 2.969(14) 158.8 .
N23 H23C O11 0.92 2.28 3.154(6) 158.2 .
N23 H23D O4 0.92 2.21 3.046(4) 150.6 2
N23 H23D O2A 0.92 2.57 3.196(5) 125.8 2
N25 H25C O22A 0.92 2.50 3.057(5) 119.7 .
N25 H25C O22 0.92 2.64 3.11(3) 112.4 .

_diffrn_measured_fraction_theta_max 0.905
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.076

_database_code_depnum_ccdc_archive 'CCDC 994154'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex7_115K
_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;
Dinitro-(3,3-diamino-N-methyldipropylamine)nickel(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H19 N5 Ni O4'
_chemical_formula_sum            'C7 H19 N5 Ni O4'
_chemical_formula_weight         295.98

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'
O O 0.0106 0.0060 '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'


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

_cell_length_a                   7.103(5)
_cell_length_b                   23.963(5)
_cell_length_c                   10.942(5)
_cell_angle_alpha                90.000
_cell_angle_beta                 103.964(5)
_cell_angle_gamma                90.000
_cell_volume                     1807.4(16)
_cell_formula_units_Z            6
_cell_measurement_temperature    115(2)
_cell_measurement_reflns_used    7822
_cell_measurement_theta_min      3.0575
_cell_measurement_theta_max      29.0636

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)

_exptl_crystal_description       Block
_exptl_crystal_colour            Violet
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936

_exptl_absorpt_coefficient_mu    1.623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.69214
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      115(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13194
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         29.24
_reflns_number_total             7580
_reflns_number_gt                6510
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'POV-RAY for Windows, 3.62 (Cason, 2009)'
_computing_publication_material  'WinGX, 1.80.05 (Farrugia, 1999)'


_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 > 2sigma(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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0419P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.504(13)
_refine_ls_number_reflns         7580
_refine_ls_number_parameters     500
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0327
_refine_ls_wR_factor_ref         0.0742
_refine_ls_wR_factor_gt          0.0719
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_restrained_S_all      0.991
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3188(6) -0.15521(18) -0.3665(3) 0.0258(9) Uani 1 1 d . . .
H1A H 0.2051 -0.1758 -0.4163 0.031 Uiso 1 1 calc R . .
H1B H 0.4372 -0.1730 -0.3812 0.031 Uiso 1 1 calc R . .
C2 C 0.3097(6) -0.09557(18) -0.4105(4) 0.0252(9) Uani 1 1 d . . .
H2A H 0.3341 -0.0946 -0.4959 0.030 Uiso 1 1 calc R . .
H2B H 0.4147 -0.0743 -0.3537 0.030 Uiso 1 1 calc R . .
C3 C 0.1162(6) -0.06672(18) -0.4148(3) 0.0231(9) Uani 1 1 d . . .
H3A H 0.1086 -0.0327 -0.4670 0.028 Uiso 1 1 calc R . .
H3B H 0.0103 -0.0919 -0.4577 0.028 Uiso 1 1 calc R . .
C4 C -0.1220(6) -0.02769(19) -0.3208(3) 0.0222(9) Uani 1 1 d . . .
H4A H -0.2098 -0.0567 -0.3674 0.027 Uiso 1 1 calc R . .
H4B H -0.1269 0.0044 -0.3785 0.027 Uiso 1 1 calc R . .
C5 C -0.2014(6) -0.0089(2) -0.2127(4) 0.0247(9) Uani 1 1 d . . .
H5A H -0.3248 0.0112 -0.2467 0.030 Uiso 1 1 calc R . .
H5B H -0.1092 0.0180 -0.1615 0.030 Uiso 1 1 calc R . .
C6 C -0.2383(5) -0.05504(19) -0.1279(3) 0.0213(9) Uani 1 1 d . . .
H6A H -0.3091 -0.0397 -0.0679 0.026 Uiso 1 1 calc R . .
H6B H -0.3216 -0.0837 -0.1795 0.026 Uiso 1 1 calc R . .
C7 C 0.2162(6) -0.00541(18) -0.2356(4) 0.0227(9) Uani 1 1 d . . .
H7A H 0.2078 0.0247 -0.2972 0.034 Uiso 1 1 calc R . .
H7B H 0.3488 -0.0201 -0.2131 0.034 Uiso 1 1 calc R . .
H7C H 0.1822 0.0091 -0.1600 0.034 Uiso 1 1 calc R . .
C11 C 0.5490(6) -0.04857(19) 0.3252(4) 0.0264(9) Uani 1 1 d . . .
H11A H 0.5186 -0.0889 0.3172 0.032 Uiso 1 1 calc R . .
H11B H 0.6050 -0.0402 0.4152 0.032 Uiso 1 1 calc R . .
C12 C 0.6940(7) -0.03420(19) 0.2491(4) 0.0298(10) Uani 1 1 d . . .
H12A H 0.8023 -0.0613 0.2702 0.036 Uiso 1 1 calc R . .
H12B H 0.6303 -0.0388 0.1587 0.036 Uiso 1 1 calc R . .
C13 C 0.7766(6) 0.02382(17) 0.2691(4) 0.0205(9) Uani 1 1 d . . .
H13A H 0.8913 0.0255 0.2327 0.025 Uiso 1 1 calc R . .
H13B H 0.8230 0.0301 0.3609 0.025 Uiso 1 1 calc R . .
C14 C 0.7573(6) 0.12212(19) 0.2546(4) 0.0231(9) Uani 1 1 d . . .
H14A H 0.8699 0.1215 0.2161 0.028 Uiso 1 1 calc R . .
H14B H 0.8091 0.1201 0.3470 0.028 Uiso 1 1 calc R . .
C15 C 0.6569(7) 0.17760(19) 0.2244(4) 0.0332(11) Uani 1 1 d . . .
H15A H 0.5816 0.1772 0.1355 0.040 Uiso 1 1 calc R . .
H15B H 0.7566 0.2072 0.2327 0.040 Uiso 1 1 calc R . .
C16 C 0.5222(6) 0.19228(19) 0.3071(4) 0.0238(9) Uani 1 1 d . . .
H16A H 0.5917 0.1884 0.3967 0.029 Uiso 1 1 calc R . .
H16B H 0.4797 0.2316 0.2922 0.029 Uiso 1 1 calc R . .
C17 C 0.5941(4) 0.0669(3) 0.0757(3) 0.0281(8) Uani 1 1 d . . .
H17A H 0.5143 0.0989 0.0391 0.042 Uiso 1 1 calc R . .
H17B H 0.5219 0.0323 0.0498 0.042 Uiso 1 1 calc R . .
H17C H 0.7138 0.0666 0.0462 0.042 Uiso 1 1 calc R . .
C21 C -0.2594(6) 0.19795(19) -0.1436(4) 0.0253(9) Uani 1 1 d . . .
H21A H -0.3471 0.2252 -0.1971 0.030 Uiso 1 1 calc R . .
H21B H -0.3265 0.1828 -0.0813 0.030 Uiso 1 1 calc R . .
C22 C -0.2146(6) 0.15100(18) -0.2246(4) 0.0247(9) Uani 1 1 d . . .
H22A H -0.3338 0.1286 -0.2555 0.030 Uiso 1 1 calc R . .
H22B H -0.1161 0.1263 -0.1716 0.030 Uiso 1 1 calc R . .
C23 C -0.1402(6) 0.17009(19) -0.3378(4) 0.0233(9) Uani 1 1 d . . .
H23A H -0.1418 0.1376 -0.3939 0.028 Uiso 1 1 calc R . .
H23B H -0.2323 0.1980 -0.3852 0.028 Uiso 1 1 calc R . .
C24 C 0.0896(6) 0.21104(18) -0.4335(3) 0.0256(9) Uani 1 1 d . . .
H24A H -0.0182 0.2358 -0.4755 0.031 Uiso 1 1 calc R . .
H24B H 0.0814 0.1769 -0.4856 0.031 Uiso 1 1 calc R . .
C25 C 0.2794(6) 0.24029(19) -0.4334(4) 0.0264(9) Uani 1 1 d . . .
H25A H 0.3015 0.2384 -0.5193 0.032 Uiso 1 1 calc R . .
H25B H 0.3868 0.2200 -0.3762 0.032 Uiso 1 1 calc R . .
C26 C 0.2859(7) 0.30122(19) -0.3925(4) 0.0290(10) Uani 1 1 d . . .
H26A H 0.4026 0.3194 -0.4088 0.035 Uiso 1 1 calc R . .
H26B H 0.1702 0.3210 -0.4423 0.035 Uiso 1 1 calc R . .
C27 C 0.2002(6) 0.15129(19) -0.2530(4) 0.0250(9) Uani 1 1 d . . .
H27A H 0.1957 0.1210 -0.3139 0.038 Uiso 1 1 calc R . .
H27B H 0.1687 0.1365 -0.1769 0.038 Uiso 1 1 calc R . .
H27C H 0.3307 0.1675 -0.2312 0.038 Uiso 1 1 calc R . .
N2 N 0.3701(5) -0.12798(16) 0.0558(3) 0.0250(8) Uani 1 1 d . . .
N3 N 0.3211(5) -0.15919(15) -0.2322(3) 0.0214(7) Uani 1 1 d . A .
H3C H 0.4419 -0.1479 -0.1876 0.026 Uiso 1 1 calc R . .
H3D H 0.3100 -0.1964 -0.2143 0.026 Uiso 1 1 calc R . .
N4 N 0.0801(4) -0.05048(14) -0.2907(3) 0.0168(6) Uani 1 1 d . A .
N5 N -0.0592(5) -0.08115(15) -0.0577(3) 0.0216(7) Uani 1 1 d . A .
H5C H -0.0917 -0.1085 -0.0074 0.026 Uiso 1 1 calc R . .
H5D H 0.0115 -0.0546 -0.0053 0.026 Uiso 1 1 calc R . .
N12 N 0.3872(4) 0.0696(2) 0.5191(2) 0.0332(6) Uani 1 1 d . . .
N13 N 0.3715(5) -0.01611(15) 0.2796(3) 0.0239(7) Uani 1 1 d . B .
H13C H 0.2854 -0.0263 0.3263 0.029 Uiso 1 1 calc R . .
H13D H 0.3182 -0.0267 0.1978 0.029 Uiso 1 1 calc R . .
N14 N 0.6426(3) 0.07132(18) 0.21443(19) 0.0155(4) Uani 1 1 d . B .
N15 N 0.3518(5) 0.15527(16) 0.2795(3) 0.0272(8) Uani 1 1 d . B .
H15C H 0.2784 0.1645 0.2008 0.033 Uiso 1 1 calc R . .
H15D H 0.2787 0.1637 0.3359 0.033 Uiso 1 1 calc R . .
N22 N 0.3467(5) 0.27486(17) 0.0325(3) 0.0326(9) Uani 1 1 d . . .
N23 N -0.0783(5) 0.22641(14) -0.0770(3) 0.0206(7) Uani 1 1 d . C .
H23C H -0.0042 0.2009 -0.0233 0.025 Uiso 1 1 calc R . .
H23D H -0.1117 0.2540 -0.0278 0.025 Uiso 1 1 calc R . .
N24 N 0.0577(4) 0.19480(14) -0.3091(3) 0.0192(7) Uani 1 1 d . C .
N25 N 0.2905(5) 0.30535(15) -0.2567(3) 0.0231(7) Uani 1 1 d . C .
H25C H 0.2772 0.3425 -0.2392 0.028 Uiso 1 1 calc R . .
H25D H 0.4126 0.2948 -0.2128 0.028 Uiso 1 1 calc R . .
O3 O 0.3566(4) -0.08481(12) -0.0136(2) 0.0236(6) Uani 1 1 d . A .
O4 O 0.2473(4) -0.16446(12) 0.0078(2) 0.0259(7) Uani 1 1 d . A .
O13 O 0.2329(3) 0.0681(2) 0.4344(2) 0.0347(6) Uani 1 1 d . B .
O14 O 0.5363(3) 0.07125(17) 0.47362(17) 0.0247(4) Uani 1 1 d . B .
O23 O 0.2203(5) 0.31125(13) -0.0156(3) 0.0295(7) Uani 1 1 d . C .
O24 O 0.3362(4) 0.23240(13) -0.0362(2) 0.0263(6) Uani 1 1 d . C .
Ni1 Ni 0.11937(6) -0.116547(16) -0.16002(4) 0.01654(11) Uani 1 1 d . . .
Ni2 Ni 0.38967(4) 0.06969(3) 0.28294(3) 0.01599(8) Uani 1 1 d . . .
Ni3 Ni 0.09422(6) 0.261667(16) -0.18123(4) 0.01791(11) Uani 1 1 d . . .
N1 N -0.071(4) -0.1716(11) -0.254(3) 0.026(4) Uiso 0.144(8) 1 d PD A 1
O1 O -0.232(4) -0.1603(11) -0.313(2) 0.044(4) Uiso 0.144(8) 1 d PD A 1
O2 O -0.050(5) -0.2223(10) -0.242(3) 0.024(5) Uiso 0.144(8) 1 d PD A 1
N1A N -0.1504(7) -0.20670(17) -0.2795(4) 0.0247(11) Uani 0.856(8) 1 d PD A 2
O1A O -0.1164(5) -0.15393(15) -0.2737(3) 0.0241(10) Uani 0.856(8) 1 d PD A 2
O2A O -0.0176(6) -0.2363(2) -0.2136(4) 0.0335(12) Uani 0.856(8) 1 d PD A 2
N11 N 0.1760(5) 0.0720(3) 0.1073(3) 0.0195(10) Uani 0.704(8) 1 d PD B 3
O11 O 0.1078(9) 0.1154(2) 0.0528(5) 0.0339(14) Uani 0.704(8) 1 d PD B 3
O12 O 0.1112(7) 0.02735(19) 0.0579(4) 0.0336(14) Uani 0.704(8) 1 d PD B 3
N11A N 0.0859(11) 0.0753(5) 0.0272(7) 0.016(2) Uiso 0.296(8) 1 d PD B 4
O11A O 0.1732(13) 0.0466(4) 0.1248(9) 0.017(3) Uiso 0.296(8) 1 d PD B 4
O12A O 0.144(2) 0.1267(5) 0.0336(15) 0.032(4) Uiso 0.296(8) 1 d PD B 4
N21 N -0.106(3) 0.3243(12) -0.270(2) 0.026(4) Uiso 0.145(8) 1 d PD C 5
O22 O -0.082(5) 0.3745(12) -0.280(2) 0.024(5) Uiso 0.145(8) 1 d PD C 5
O21 O -0.259(3) 0.3064(11) -0.327(2) 0.044(4) Uiso 0.145(8) 1 d PD C 5
N21A N -0.1846(6) 0.34983(18) -0.3030(4) 0.0283(12) Uani 0.855(8) 1 d PD C 6
O21A O -0.1450(6) 0.29762(15) -0.2949(3) 0.0261(10) Uani 0.855(8) 1 d PD C 6
O22A O -0.0505(6) 0.37953(19) -0.2372(5) 0.0339(11) Uani 0.855(8) 1 d PD C 6


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N3 1.468(5) . ?
C1 C2 1.505(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.529(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N4 1.493(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.496(5) . ?
C4 C5 1.498(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.507(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N5 1.459(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 N4 1.478(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C11 N13 1.463(5) . ?
C11 C12 1.511(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.505(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N14 1.512(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 N14 1.472(6) . ?
C14 C15 1.507(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.509(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 N15 1.472(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 N14 1.477(3) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C21 N23 1.483(5) . ?
C21 C22 1.513(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.529(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 N24 1.487(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 N24 1.486(5) . ?
C24 C25 1.519(6) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.525(6) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 N25 1.482(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 N24 1.479(5) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
N2 O4 1.257(5) . ?
N2 O3 1.273(4) . ?
N3 Ni1 2.066(4) . ?
N3 H3C 0.9200 . ?
N3 H3D 0.9200 . ?
N4 Ni1 2.106(3) . ?
N5 Ni1 2.066(3) . ?
N5 H5C 0.9200 . ?
N5 H5D 0.9200 . ?
N12 O13 1.254(3) . ?
N12 O14 1.274(3) . ?
N13 Ni2 2.060(4) . ?
N13 H13C 0.9200 . ?
N13 H13D 0.9200 . ?
N14 Ni2 2.107(2) . ?
N15 Ni2 2.067(4) . ?
N15 H15C 0.9200 . ?
N15 H15D 0.9200 . ?
N22 O24 1.257(5) . ?
N22 O23 1.271(5) . ?
N23 Ni3 2.047(4) . ?
N23 H23C 0.9200 . ?
N23 H23D 0.9200 . ?
N24 Ni3 2.102(3) . ?
N25 Ni3 2.068(4) . ?
N25 H25C 0.9200 . ?
N25 H25D 0.9200 . ?
O3 Ni1 2.164(3) . ?
O4 Ni1 2.170(3) . ?
O13 Ni2 2.208(2) . ?
O14 Ni2 2.095(2) . ?
O23 Ni3 2.171(3) . ?
O24 Ni3 2.156(3) . ?
Ni1 N1 1.99(3) . ?
Ni1 O1A 2.037(3) . ?
Ni2 O11A 2.093(10) . ?
Ni2 N11 2.143(4) . ?
Ni3 O21A 2.039(4) . ?
Ni3 N21 2.13(3) . ?
N1 O1 1.199(10) . ?
N1 O2 1.226(19) . ?
N1A O2A 1.259(6) . ?
N1A O1A 1.286(5) . ?
N11 O12 1.236(6) . ?
N11 O11 1.240(7) . ?
N11A O11A 1.295(8) . ?
N11A O12A 1.296(9) . ?
N21 O21 1.195(10) . ?
N21 O22 1.222(19) . ?
N21A O22A 1.265(6) . ?
N21A O21A 1.281(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 C1 C2 111.8(3) . . ?
N3 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N3 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 107.9 . . ?
C1 C2 C3 114.1(4) . . ?
C1 C2 H2A 108.7 . . ?
C3 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
C3 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
N4 C3 C2 116.1(3) . . ?
N4 C3 H3A 108.3 . . ?
C2 C3 H3A 108.3 . . ?
N4 C3 H3B 108.3 . . ?
C2 C3 H3B 108.3 . . ?
H3A C3 H3B 107.4 . . ?
N4 C4 C5 117.4(3) . . ?
N4 C4 H4A 107.9 . . ?
C5 C4 H4A 107.9 . . ?
N4 C4 H4B 107.9 . . ?
C5 C4 H4B 107.9 . . ?
H4A C4 H4B 107.2 . . ?
C4 C5 C6 114.8(4) . . ?
C4 C5 H5A 108.6 . . ?
C6 C5 H5A 108.6 . . ?
C4 C5 H5B 108.6 . . ?
C6 C5 H5B 108.6 . . ?
H5A C5 H5B 107.5 . . ?
N5 C6 C5 112.4(3) . . ?
N5 C6 H6A 109.1 . . ?
C5 C6 H6A 109.1 . . ?
N5 C6 H6B 109.1 . . ?
C5 C6 H6B 109.1 . . ?
H6A C6 H6B 107.9 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N13 C11 C12 109.7(4) . . ?
N13 C11 H11A 109.7 . . ?
C12 C11 H11A 109.7 . . ?
N13 C11 H11B 109.7 . . ?
C12 C11 H11B 109.7 . . ?
H11A C11 H11B 108.2 . . ?
C13 C12 C11 115.1(4) . . ?
C13 C12 H12A 108.5 . . ?
C11 C12 H12A 108.5 . . ?
C13 C12 H12B 108.5 . . ?
C11 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?
C12 C13 N14 116.9(3) . . ?
C12 C13 H13A 108.1 . . ?
N14 C13 H13A 108.1 . . ?
C12 C13 H13B 108.1 . . ?
N14 C13 H13B 108.1 . . ?
H13A C13 H13B 107.3 . . ?
N14 C14 C15 117.7(4) . . ?
N14 C14 H14A 107.9 . . ?
C15 C14 H14A 107.9 . . ?
N14 C14 H14B 107.9 . . ?
C15 C14 H14B 107.9 . . ?
H14A C14 H14B 107.2 . . ?
C14 C15 C16 114.1(4) . . ?
C14 C15 H15A 108.7 . . ?
C16 C15 H15A 108.7 . . ?
C14 C15 H15B 108.7 . . ?
C16 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
N15 C16 C15 110.2(4) . . ?
N15 C16 H16A 109.6 . . ?
C15 C16 H16A 109.6 . . ?
N15 C16 H16B 109.6 . . ?
C15 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
N14 C17 H17A 109.5 . . ?
N14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N23 C21 C22 110.5(3) . . ?
N23 C21 H21A 109.6 . . ?
C22 C21 H21A 109.6 . . ?
N23 C21 H21B 109.6 . . ?
C22 C21 H21B 109.6 . . ?
H21A C21 H21B 108.1 . . ?
C21 C22 C23 114.5(4) . . ?
C21 C22 H22A 108.6 . . ?
C23 C22 H22A 108.6 . . ?
C21 C22 H22B 108.6 . . ?
C23 C22 H22B 108.6 . . ?
H22A C22 H22B 107.6 . . ?
N24 C23 C22 116.2(3) . . ?
N24 C23 H23A 108.2 . . ?
C22 C23 H23A 108.2 . . ?
N24 C23 H23B 108.2 . . ?
C22 C23 H23B 108.2 . . ?
H23A C23 H23B 107.4 . . ?
N24 C24 C25 116.9(3) . . ?
N24 C24 H24A 108.1 . . ?
C25 C24 H24A 108.1 . . ?
N24 C24 H24B 108.1 . . ?
C25 C24 H24B 108.1 . . ?
H24A C24 H24B 107.3 . . ?
C24 C25 C26 113.9(4) . . ?
C24 C25 H25A 108.8 . . ?
C26 C25 H25A 108.8 . . ?
C24 C25 H25B 108.8 . . ?
C26 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
N25 C26 C25 110.5(3) . . ?
N25 C26 H26A 109.5 . . ?
C25 C26 H26A 109.5 . . ?
N25 C26 H26B 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 108.1 . . ?
N24 C27 H27A 109.5 . . ?
N24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O4 N2 O3 111.8(3) . . ?
C1 N3 Ni1 120.6(3) . . ?
C1 N3 H3C 107.2 . . ?
Ni1 N3 H3C 107.2 . . ?
C1 N3 H3D 107.2 . . ?
Ni1 N3 H3D 107.2 . . ?
H3C N3 H3D 106.8 . . ?
C7 N4 C3 108.8(3) . . ?
C7 N4 C4 108.7(3) . . ?
C3 N4 C4 105.1(3) . . ?
C7 N4 Ni1 107.8(2) . . ?
C3 N4 Ni1 113.4(2) . . ?
C4 N4 Ni1 112.8(2) . . ?
C6 N5 Ni1 117.5(2) . . ?
C6 N5 H5C 107.9 . . ?
Ni1 N5 H5C 107.9 . . ?
C6 N5 H5D 107.9 . . ?
Ni1 N5 H5D 107.9 . . ?
H5C N5 H5D 107.2 . . ?
O13 N12 O14 111.9(2) . . ?
C11 N13 Ni2 118.7(3) . . ?
C11 N13 H13C 107.6 . . ?
Ni2 N13 H13C 107.6 . . ?
C11 N13 H13D 107.6 . . ?
Ni2 N13 H13D 107.6 . . ?
H13C N13 H13D 107.1 . . ?
C14 N14 C17 109.9(3) . . ?
C14 N14 C13 104.7(2) . . ?
C17 N14 C13 108.7(3) . . ?
C14 N14 Ni2 111.6(2) . . ?
C17 N14 Ni2 110.91(16) . . ?
C13 N14 Ni2 110.8(2) . . ?
C16 N15 Ni2 119.8(3) . . ?
C16 N15 H15C 107.4 . . ?
Ni2 N15 H15C 107.4 . . ?
C16 N15 H15D 107.4 . . ?
Ni2 N15 H15D 107.4 . . ?
H15C N15 H15D 106.9 . . ?
O24 N22 O23 111.9(3) . . ?
C21 N23 Ni3 118.7(3) . . ?
C21 N23 H23C 107.6 . . ?
Ni3 N23 H23C 107.6 . . ?
C21 N23 H23D 107.6 . . ?
Ni3 N23 H23D 107.6 . . ?
H23C N23 H23D 107.1 . . ?
C27 N24 C24 108.9(3) . . ?
C27 N24 C23 108.9(3) . . ?
C24 N24 C23 104.8(3) . . ?
C27 N24 Ni3 107.4(2) . . ?
C24 N24 Ni3 112.9(3) . . ?
C23 N24 Ni3 113.8(2) . . ?
C26 N25 Ni3 120.8(3) . . ?
C26 N25 H25C 107.1 . . ?
Ni3 N25 H25C 107.1 . . ?
C26 N25 H25D 107.1 . . ?
Ni3 N25 H25D 107.1 . . ?
H25C N25 H25D 106.8 . . ?
N2 O3 Ni1 95.1(2) . . ?
N2 O4 Ni1 95.3(2) . . ?
N12 O13 Ni2 92.60(15) . . ?
N12 O14 Ni2 97.38(16) . . ?
N22 O23 Ni3 94.5(2) . . ?
N22 O24 Ni3 95.7(2) . . ?
N1 Ni1 O1A 15.5(6) . . ?
N1 Ni1 N5 97.0(8) . . ?
O1A Ni1 N5 89.40(16) . . ?
N1 Ni1 N3 85.6(8) . . ?
O1A Ni1 N3 95.32(16) . . ?
N5 Ni1 N3 169.63(13) . . ?
N1 Ni1 N4 100.8(8) . . ?
O1A Ni1 N4 87.79(13) . . ?
N5 Ni1 N4 93.50(13) . . ?
N3 Ni1 N4 95.90(13) . . ?
N1 Ni1 O3 157.9(7) . . ?
O1A Ni1 O3 170.19(13) . . ?
N5 Ni1 O3 85.70(13) . . ?
N3 Ni1 O3 88.22(13) . . ?
N4 Ni1 O3 100.97(11) . . ?
N1 Ni1 O4 100.3(7) . . ?
O1A Ni1 O4 113.49(13) . . ?
N5 Ni1 O4 86.85(12) . . ?
N3 Ni1 O4 82.80(12) . . ?
N4 Ni1 O4 158.72(12) . . ?
O3 Ni1 O4 57.81(11) . . ?
N13 Ni2 N15 169.25(10) . . ?
N13 Ni2 O11A 72.0(3) . . ?
N15 Ni2 O11A 100.4(3) . . ?
N13 Ni2 O14 92.83(14) . . ?
N15 Ni2 O14 91.82(14) . . ?
O11A Ni2 O14 156.6(3) . . ?
N13 Ni2 N14 93.86(16) . . ?
N15 Ni2 N14 95.36(16) . . ?
O11A Ni2 N14 103.3(3) . . ?
O14 Ni2 N14 95.31(8) . . ?
N13 Ni2 N11 88.96(19) . . ?
N15 Ni2 N11 84.11(19) . . ?
O11A Ni2 N11 17.3(2) . . ?
O14 Ni2 N11 165.20(10) . . ?
N14 Ni2 N11 99.24(11) . . ?
N13 Ni2 O13 87.45(15) . . ?
N15 Ni2 O13 86.78(16) . . ?
O11A Ni2 O13 102.3(3) . . ?
O14 Ni2 O13 58.16(8) . . ?
N14 Ni2 O13 153.46(9) . . ?
N11 Ni2 O13 107.29(11) . . ?
O21A Ni3 N23 89.52(15) . . ?
O21A Ni3 N25 94.89(16) . . ?
N23 Ni3 N25 169.48(13) . . ?
O21A Ni3 N24 88.01(13) . . ?
N23 Ni3 N24 93.54(14) . . ?
N25 Ni3 N24 96.15(14) . . ?
O21A Ni3 N21 19.8(6) . . ?
N23 Ni3 N21 97.0(7) . . ?
N25 Ni3 N21 84.3(6) . . ?
N24 Ni3 N21 105.8(7) . . ?
O21A Ni3 O24 170.27(13) . . ?
N23 Ni3 O24 86.21(12) . . ?
N25 Ni3 O24 87.93(13) . . ?
N24 Ni3 O24 100.97(12) . . ?
N21 Ni3 O24 152.8(7) . . ?
O21A Ni3 O23 113.16(14) . . ?
N23 Ni3 O23 86.72(12) . . ?
N25 Ni3 O23 82.77(12) . . ?
N24 Ni3 O23 158.83(13) . . ?
N21 Ni3 O23 95.2(7) . . ?
O24 Ni3 O23 57.90(12) . . ?
O1 N1 O2 111(3) . . ?
O1 N1 Ni1 125(2) . . ?
O2 N1 Ni1 124(2) . . ?
O2A N1A O1A 114.8(4) . . ?
N1A O1A Ni1 125.4(3) . . ?
O12 N11 O11 117.1(4) . . ?
O12 N11 Ni2 118.6(4) . . ?
O11 N11 Ni2 124.3(4) . . ?
O11A N11A O12A 112.2(11) . . ?
N11A O11A Ni2 130.7(8) . . ?
O21 N21 O22 116(3) . . ?
O21 N21 Ni3 114(2) . . ?
O22 N21 Ni3 130(2) . . ?
O22A N21A O21A 112.8(5) . . ?
N21A O21A Ni3 126.3(3) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 C1 C2 C3 -69.3(4) . . . . ?
C1 C2 C3 N4 74.4(4) . . . . ?
N4 C4 C5 C6 -68.4(5) . . . . ?
C4 C5 C6 N5 67.6(4) . . . . ?
N13 C11 C12 C13 68.6(5) . . . . ?
C11 C12 C13 N14 -72.0(5) . . . . ?
N14 C14 C15 C16 75.4(5) . . . . ?
C14 C15 C16 N15 -69.1(5) . . . . ?
N23 C21 C22 C23 -68.5(4) . . . . ?
C21 C22 C23 N24 69.8(5) . . . . ?
N24 C24 C25 C26 -75.7(5) . . . . ?
C24 C25 C26 N25 69.1(5) . . . . ?
C2 C1 N3 Ni1 49.7(4) . . . . ?
C2 C3 N4 C7 68.0(4) . . . . ?
C2 C3 N4 C4 -175.7(3) . . . . ?
C2 C3 N4 Ni1 -52.0(4) . . . . ?
C5 C4 N4 C7 -64.9(5) . . . . ?
C5 C4 N4 C3 178.7(4) . . . . ?
C5 C4 N4 Ni1 54.6(4) . . . . ?
C5 C6 N5 Ni1 -58.5(4) . . . . ?
C12 C11 N13 Ni2 -58.9(4) . . . . ?
C15 C14 N14 C17 68.7(4) . . . . ?
C15 C14 N14 C13 -174.6(4) . . . . ?
C15 C14 N14 Ni2 -54.7(4) . . . . ?
C12 C13 N14 C14 176.7(4) . . . . ?
C12 C13 N14 C17 -65.8(4) . . . . ?
C12 C13 N14 Ni2 56.3(4) . . . . ?
C15 C16 N15 Ni2 52.9(4) . . . . ?
C22 C21 N23 Ni3 58.7(4) . . . . ?
C25 C24 N24 C27 -66.2(4) . . . . ?
C25 C24 N24 C23 177.3(4) . . . . ?
C25 C24 N24 Ni3 53.0(4) . . . . ?
C22 C23 N24 C27 65.3(4) . . . . ?
C22 C23 N24 C24 -178.2(4) . . . . ?
C22 C23 N24 Ni3 -54.4(4) . . . . ?
C25 C26 N25 Ni3 -49.5(5) . . . . ?
O4 N2 O3 Ni1 -0.2(3) . . . . ?
O3 N2 O4 Ni1 0.2(3) . . . . ?
O14 N12 O13 Ni2 0.1(5) . . . . ?
O13 N12 O14 Ni2 -0.2(5) . . . . ?
O24 N22 O23 Ni3 0.9(3) . . . . ?
O23 N22 O24 Ni3 -0.9(3) . . . . ?
C6 N5 Ni1 N1 -59.9(8) . . . . ?
C6 N5 Ni1 O1A -46.4(3) . . . . ?
C6 N5 Ni1 N3 -163.6(7) . . . . ?
C6 N5 Ni1 N4 41.4(3) . . . . ?
C6 N5 Ni1 O3 142.1(3) . . . . ?
C6 N5 Ni1 O4 -159.9(3) . . . . ?
C1 N3 Ni1 N1 71.3(8) . . . . ?
C1 N3 Ni1 O1A 59.2(3) . . . . ?
C1 N3 Ni1 N5 176.0(7) . . . . ?
C1 N3 Ni1 N4 -29.1(3) . . . . ?
C1 N3 Ni1 O3 -129.9(3) . . . . ?
C1 N3 Ni1 O4 172.3(3) . . . . ?
C7 N4 Ni1 N1 -179.0(9) . . . . ?
C3 N4 Ni1 N1 -58.5(9) . . . . ?
C4 N4 Ni1 N1 60.9(9) . . . . ?
C7 N4 Ni1 O1A 172.4(3) . . . . ?
C3 N4 Ni1 O1A -67.0(3) . . . . ?
C4 N4 Ni1 O1A 52.4(3) . . . . ?
C7 N4 Ni1 N5 83.2(3) . . . . ?
C3 N4 Ni1 N5 -156.3(2) . . . . ?
C4 N4 Ni1 N5 -36.9(3) . . . . ?
C7 N4 Ni1 N3 -92.4(3) . . . . ?
C3 N4 Ni1 N3 28.1(2) . . . . ?
C4 N4 Ni1 N3 147.5(2) . . . . ?
C7 N4 Ni1 O3 -3.1(3) . . . . ?
C3 N4 Ni1 O3 117.5(2) . . . . ?
C4 N4 Ni1 O3 -123.2(2) . . . . ?
C7 N4 Ni1 O4 -7.1(5) . . . . ?
C3 N4 Ni1 O4 113.4(4) . . . . ?
C4 N4 Ni1 O4 -127.2(3) . . . . ?
N2 O3 Ni1 N1 -9(2) . . . . ?
N2 O3 Ni1 O1A 28.9(9) . . . . ?
N2 O3 Ni1 N5 89.1(2) . . . . ?
N2 O3 Ni1 N3 -82.5(2) . . . . ?
N2 O3 Ni1 N4 -178.1(2) . . . . ?
N2 O3 Ni1 O4 0.1(2) . . . . ?
N2 O4 Ni1 N1 176.5(9) . . . . ?
N2 O4 Ni1 O1A -175.0(2) . . . . ?
N2 O4 Ni1 N5 -87.0(2) . . . . ?
N2 O4 Ni1 N3 92.3(2) . . . . ?
N2 O4 Ni1 N4 4.5(5) . . . . ?
N2 O4 Ni1 O3 -0.1(2) . . . . ?
C11 N13 Ni2 N15 -168.0(5) . . . . ?
C11 N13 Ni2 O11A 145.8(4) . . . . ?
C11 N13 Ni2 O14 -52.5(3) . . . . ?
C11 N13 Ni2 N14 43.1(3) . . . . ?
C11 N13 Ni2 N11 142.2(3) . . . . ?
C11 N13 Ni2 O13 -110.4(3) . . . . ?
C16 N15 Ni2 N13 176.9(5) . . . . ?
C16 N15 Ni2 O11A -138.9(4) . . . . ?
C16 N15 Ni2 O14 61.2(3) . . . . ?
C16 N15 Ni2 N14 -34.3(3) . . . . ?
C16 N15 Ni2 N11 -133.0(3) . . . . ?
C16 N15 Ni2 O13 119.2(3) . . . . ?
N12 O14 Ni2 N13 -85.1(3) . . . . ?
N12 O14 Ni2 N15 85.2(3) . . . . ?
N12 O14 Ni2 O11A -36.6(8) . . . . ?
N12 O14 Ni2 N14 -179.3(3) . . . . ?
N12 O14 Ni2 N11 11.5(9) . . . . ?
N12 O14 Ni2 O13 0.1(3) . . . . ?
C14 N14 Ni2 N13 -154.0(2) . . . . ?
C17 N14 Ni2 N13 83.1(4) . . . . ?
C13 N14 Ni2 N13 -37.7(3) . . . . ?
C14 N14 Ni2 N15 31.6(2) . . . . ?
C17 N14 Ni2 N15 -91.3(4) . . . . ?
C13 N14 Ni2 N15 147.8(3) . . . . ?
C14 N14 Ni2 O11A 133.6(3) . . . . ?
C17 N14 Ni2 O11A 10.7(4) . . . . ?
C13 N14 Ni2 O11A -110.2(3) . . . . ?
C14 N14 Ni2 O14 -60.7(3) . . . . ?
C17 N14 Ni2 O14 176.3(3) . . . . ?
C13 N14 Ni2 O14 55.5(3) . . . . ?
C14 N14 Ni2 N11 116.5(3) . . . . ?
C17 N14 Ni2 N11 -6.4(4) . . . . ?
C13 N14 Ni2 N11 -127.3(3) . . . . ?
C14 N14 Ni2 O13 -62.0(5) . . . . ?
C17 N14 Ni2 O13 175.1(4) . . . . ?
C13 N14 Ni2 O13 54.3(5) . . . . ?
N12 O13 Ni2 N13 94.8(3) . . . . ?
N12 O13 Ni2 N15 -94.2(3) . . . . ?
N12 O13 Ni2 O11A 165.8(4) . . . . ?
N12 O13 Ni2 O14 -0.1(3) . . . . ?
N12 O13 Ni2 N14 1.3(6) . . . . ?
N12 O13 Ni2 N11 -177.1(4) . . . . ?
C21 N23 Ni3 O21A 47.0(3) . . . . ?
C21 N23 Ni3 N25 161.9(7) . . . . ?
C21 N23 Ni3 N24 -41.0(3) . . . . ?
C21 N23 Ni3 N21 65.4(7) . . . . ?
C21 N23 Ni3 O24 -141.8(3) . . . . ?
C21 N23 Ni3 O23 160.2(3) . . . . ?
C26 N25 Ni3 O21A -59.0(3) . . . . ?
C26 N25 Ni3 N23 -173.5(6) . . . . ?
C26 N25 Ni3 N24 29.5(3) . . . . ?
C26 N25 Ni3 N21 -75.8(8) . . . . ?
C26 N25 Ni3 O24 130.4(3) . . . . ?
C26 N25 Ni3 O23 -171.7(3) . . . . ?
C27 N24 Ni3 O21A -173.5(3) . . . . ?
C24 N24 Ni3 O21A 66.5(3) . . . . ?
C23 N24 Ni3 O21A -52.8(3) . . . . ?
C27 N24 Ni3 N23 -84.1(3) . . . . ?
C24 N24 Ni3 N23 155.9(2) . . . . ?
C23 N24 Ni3 N23 36.6(3) . . . . ?
C27 N24 Ni3 N25 91.8(3) . . . . ?
C24 N24 Ni3 N25 -28.2(3) . . . . ?
C23 N24 Ni3 N25 -147.5(3) . . . . ?
C27 N24 Ni3 N21 177.6(7) . . . . ?
C24 N24 Ni3 N21 57.6(7) . . . . ?
C23 N24 Ni3 N21 -61.7(7) . . . . ?
C27 N24 Ni3 O24 2.8(3) . . . . ?
C24 N24 Ni3 O24 -117.3(2) . . . . ?
C23 N24 Ni3 O24 123.4(3) . . . . ?
C27 N24 Ni3 O23 6.0(5) . . . . ?
C24 N24 Ni3 O23 -114.1(4) . . . . ?
C23 N24 Ni3 O23 126.6(3) . . . . ?
N22 O24 Ni3 O21A -23.8(9) . . . . ?
N22 O24 Ni3 N23 -87.9(2) . . . . ?
N22 O24 Ni3 N25 83.3(2) . . . . ?
N22 O24 Ni3 N24 179.2(2) . . . . ?
N22 O24 Ni3 N21 10.0(15) . . . . ?
N22 O24 Ni3 O23 0.6(2) . . . . ?
N22 O23 Ni3 O21A 175.1(2) . . . . ?
N22 O23 Ni3 N23 87.0(2) . . . . ?
N22 O23 Ni3 N25 -92.7(3) . . . . ?
N22 O23 Ni3 N24 -4.3(5) . . . . ?
N22 O23 Ni3 N21 -176.2(7) . . . . ?
N22 O23 Ni3 O24 -0.6(2) . . . . ?
O1A Ni1 N1 O1 -8.7(19) . . . . ?
N5 Ni1 N1 O1 53(3) . . . . ?
N3 Ni1 N1 O1 -137(3) . . . . ?
N4 Ni1 N1 O1 -42(3) . . . . ?
O3 Ni1 N1 O1 148.3(19) . . . . ?
O4 Ni1 N1 O1 141(3) . . . . ?
O1A Ni1 N1 O2 -177(6) . . . . ?
N5 Ni1 N1 O2 -116(3) . . . . ?
N3 Ni1 N1 O2 54(3) . . . . ?
N4 Ni1 N1 O2 149(3) . . . . ?
O3 Ni1 N1 O2 -20(5) . . . . ?
O4 Ni1 N1 O2 -28(3) . . . . ?
O2A N1A O1A Ni1 -4.5(6) . . . . ?
N1 Ni1 O1A N1A 8(3) . . . . ?
N5 Ni1 O1A N1A -111.9(4) . . . . ?
N3 Ni1 O1A N1A 58.8(4) . . . . ?
N4 Ni1 O1A N1A 154.5(4) . . . . ?
O3 Ni1 O1A N1A -52.0(11) . . . . ?
O4 Ni1 O1A N1A -25.6(4) . . . . ?
N13 Ni2 N11 O12 -0.9(3) . . . . ?
N15 Ni2 N11 O12 -172.6(3) . . . . ?
O11A Ni2 N11 O12 -12.3(9) . . . . ?
O14 Ni2 N11 O12 -98.0(8) . . . . ?
N14 Ni2 N11 O12 92.9(4) . . . . ?
O13 Ni2 N11 O12 -87.9(4) . . . . ?
N13 Ni2 N11 O11 176.9(5) . . . . ?
N15 Ni2 N11 O11 5.1(5) . . . . ?
O11A Ni2 N11 O11 165.5(12) . . . . ?
O14 Ni2 N11 O11 79.8(9) . . . . ?
N14 Ni2 N11 O11 -89.3(5) . . . . ?
O13 Ni2 N11 O11 89.9(5) . . . . ?
O12A N11A O11A Ni2 -1.5(13) . . . . ?
N13 Ni2 O11A N11A -166.2(9) . . . . ?
N15 Ni2 O11A N11A 21.7(9) . . . . ?
O14 Ni2 O11A N11A 141.9(7) . . . . ?
N14 Ni2 O11A N11A -76.4(9) . . . . ?
N11 Ni2 O11A N11A 1.8(5) . . . . ?
O13 Ni2 O11A N11A 110.6(8) . . . . ?
O21A Ni3 N21 O21 12.0(15) . . . . ?
N23 Ni3 N21 O21 -57(2) . . . . ?
N25 Ni3 N21 O21 134(2) . . . . ?
N24 Ni3 N21 O21 39(2) . . . . ?
O24 Ni3 N21 O21 -152.0(15) . . . . ?
O23 Ni3 N21 O21 -144(2) . . . . ?
O21A Ni3 N21 O22 -161(5) . . . . ?
N23 Ni3 N21 O22 130(3) . . . . ?
N25 Ni3 N21 O22 -40(3) . . . . ?
N24 Ni3 N21 O22 -134(3) . . . . ?
O24 Ni3 N21 O22 35(4) . . . . ?
O23 Ni3 N21 O22 43(3) . . . . ?
O22A N21A O21A Ni3 4.5(6) . . . . ?
N23 Ni3 O21A N21A 111.5(4) . . . . ?
N25 Ni3 O21A N21A -59.0(4) . . . . ?
N24 Ni3 O21A N21A -155.0(4) . . . . ?
N21 Ni3 O21A N21A -1(2) . . . . ?
O24 Ni3 O21A N21A 47.6(10) . . . . ?
O23 Ni3 O21A N21A 25.3(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3C N22 0.92 2.71 3.217(5) 115.8 2_645
N3 H3D O2 0.92 2.58 3.02(3) 110.0 .
N3 H3D O2A 0.92 2.52 3.079(6) 119.7 .
N5 H5C O23 0.92 2.17 3.008(5) 150.9 2_545
N5 H5C O22A 0.92 2.64 3.270(6) 126.5 2_545
N5 H5D O12 0.92 2.15 3.015(6) 157.1 .
N13 H13D O12 0.92 2.26 2.868(5) 123.3 .
N15 H15C O12A 0.92 2.06 2.823(16) 139.7 .
N15 H15C O11 0.92 2.13 2.827(6) 132.0 .
N23 H23C O12A 0.92 2.08 2.955(15) 158.1 .
N23 H23C O11 0.92 2.28 3.151(6) 157.7 .
N23 H23D O4 0.92 2.21 3.048(4) 150.8 2
N23 H23D O2A 0.92 2.59 3.214(6) 125.7 2
N25 H25C O22A 0.92 2.50 3.053(6) 119.2 .
N25 H25C O22 0.92 2.60 3.08(3) 113.3 .

_diffrn_measured_fraction_theta_max 0.904
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.077

_database_code_depnum_ccdc_archive 'CCDC 994155'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex7_120K
_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;
Dinitro-(3,3-diamino-N-methyldipropylamine)nickel(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H19 N5 Ni O4'
_chemical_formula_sum            'C7 H19 N5 Ni O4'
_chemical_formula_weight         295.98

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'
O O 0.0106 0.0060 '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'


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

_cell_length_a                   7.101(5)
_cell_length_b                   23.928(5)
_cell_length_c                   10.936(5)
_cell_angle_alpha                90.000
_cell_angle_beta                 103.958(5)
_cell_angle_gamma                90.000
_cell_volume                     1803.3(16)
_cell_formula_units_Z            6
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    6907
_cell_measurement_theta_min      3.0579
_cell_measurement_theta_max      29.0601

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)

_exptl_crystal_description       Block
_exptl_crystal_colour            Violet
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936

_exptl_absorpt_coefficient_mu    1.627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.76309
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12927
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0523
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.11
_diffrn_reflns_theta_max         29.25
_reflns_number_total             7549
_reflns_number_gt                6258
_reflns_threshold_expression     >2sigma(I)


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'POV-RAY for Windows, 3.62 (Cason, 2009)'
_computing_publication_material  'WinGX, 1.80.05 (Farrugia, 1999)'


_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 > 2sigma(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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0663P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.50(2)
_refine_ls_number_reflns         7549
_refine_ls_number_parameters     500
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0404
_refine_ls_wR_factor_ref         0.1034
_refine_ls_wR_factor_gt          0.0988
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_restrained_S_all      0.986
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3079(11) -0.1546(3) -0.3732(6) 0.0261(14) Uani 1 1 d . . .
H1A H 0.1920 -0.1747 -0.4217 0.031 Uiso 1 1 calc R . .
H1B H 0.4240 -0.1731 -0.3898 0.031 Uiso 1 1 calc R . .
C2 C 0.3010(10) -0.0960(3) -0.4177(6) 0.0248(14) Uani 1 1 d . . .
H2A H 0.3232 -0.0955 -0.5037 0.030 Uiso 1 1 calc R . .
H2B H 0.4078 -0.0748 -0.3621 0.030 Uiso 1 1 calc R . .
C3 C 0.1078(9) -0.0664(3) -0.4203(5) 0.0251(15) Uani 1 1 d . . .
H3A H 0.1011 -0.0320 -0.4717 0.030 Uiso 1 1 calc R . .
H3B H 0.0006 -0.0911 -0.4635 0.030 Uiso 1 1 calc R . .
C4 C -0.1279(10) -0.0270(3) -0.3227(5) 0.0231(15) Uani 1 1 d . . .
H4A H -0.1326 0.0054 -0.3797 0.028 Uiso 1 1 calc R . .
H4B H -0.2174 -0.0556 -0.3696 0.028 Uiso 1 1 calc R . .
C5 C -0.2035(10) -0.0087(3) -0.2151(6) 0.0271(16) Uani 1 1 d . . .
H5A H -0.3261 0.0119 -0.2481 0.033 Uiso 1 1 calc R . .
H5B H -0.1095 0.0178 -0.1641 0.033 Uiso 1 1 calc R . .
C6 C -0.2415(8) -0.0543(3) -0.1299(5) 0.0196(13) Uani 1 1 d . . .
H6A H -0.3098 -0.0382 -0.0692 0.023 Uiso 1 1 calc R . .
H6B H -0.3280 -0.0825 -0.1810 0.023 Uiso 1 1 calc R . .
C7 C 0.2116(10) -0.0050(3) -0.2402(6) 0.0233(14) Uani 1 1 d . . .
H7A H 0.2036 0.0249 -0.3024 0.035 Uiso 1 1 calc R . .
H7B H 0.3440 -0.0200 -0.2177 0.035 Uiso 1 1 calc R . .
H7C H 0.1782 0.0098 -0.1647 0.035 Uiso 1 1 calc R . .
C11 C 0.5411(10) -0.0485(3) 0.3221(6) 0.0249(15) Uani 1 1 d . . .
H11A H 0.5080 -0.0887 0.3130 0.030 Uiso 1 1 calc R . .
H11B H 0.5999 -0.0408 0.4121 0.030 Uiso 1 1 calc R . .
C12 C 0.6850(11) -0.0338(3) 0.2427(6) 0.0275(16) Uani 1 1 d . . .
H12A H 0.7908 -0.0618 0.2596 0.033 Uiso 1 1 calc R . .
H12B H 0.6174 -0.0367 0.1525 0.033 Uiso 1 1 calc R . .
C13 C 0.7732(9) 0.0236(3) 0.2666(6) 0.0207(14) Uani 1 1 d . . .
H13A H 0.8200 0.0288 0.3588 0.025 Uiso 1 1 calc R . .
H13B H 0.8879 0.0252 0.2302 0.025 Uiso 1 1 calc R . .
C14 C 0.7622(10) 0.1222(3) 0.2601(6) 0.0231(15) Uani 1 1 d . . .
H14A H 0.8768 0.1213 0.2235 0.028 Uiso 1 1 calc R . .
H14B H 0.8108 0.1190 0.3527 0.028 Uiso 1 1 calc R . .
C15 C 0.6677(12) 0.1789(3) 0.2320(8) 0.0358(19) Uani 1 1 d . . .
H15A H 0.7704 0.2078 0.2454 0.043 Uiso 1 1 calc R . .
H15B H 0.5974 0.1801 0.1421 0.043 Uiso 1 1 calc R . .
C16 C 0.5294(10) 0.1929(3) 0.3105(5) 0.0224(14) Uani 1 1 d . . .
H16A H 0.5947 0.1881 0.4007 0.027 Uiso 1 1 calc R . .
H16B H 0.4896 0.2325 0.2968 0.027 Uiso 1 1 calc R . .
C17 C 0.5958(5) 0.0689(5) 0.0763(3) 0.0282(9) Uani 1 1 d . . .
H17A H 0.5249 0.1027 0.0412 0.042 Uiso 1 1 calc R . .
H17B H 0.5151 0.0360 0.0479 0.042 Uiso 1 1 calc R . .
H17C H 0.7160 0.0663 0.0475 0.042 Uiso 1 1 calc R . .
C21 C -0.2572(9) 0.1988(3) -0.1403(6) 0.0264(15) Uani 1 1 d . . .
H21A H -0.3415 0.2265 -0.1948 0.032 Uiso 1 1 calc R . .
H21B H -0.3273 0.1844 -0.0788 0.032 Uiso 1 1 calc R . .
C22 C -0.2121(9) 0.1509(3) -0.2204(6) 0.0215(14) Uani 1 1 d . . .
H22A H -0.3313 0.1285 -0.2511 0.026 Uiso 1 1 calc R . .
H22B H -0.1135 0.1264 -0.1668 0.026 Uiso 1 1 calc R . .
C23 C -0.1369(10) 0.1701(3) -0.3344(5) 0.0219(14) Uani 1 1 d . . .
H23A H -0.1383 0.1375 -0.3904 0.026 Uiso 1 1 calc R . .
H23B H -0.2289 0.1980 -0.3820 0.026 Uiso 1 1 calc R . .
C24 C 0.0925(10) 0.2115(3) -0.4288(6) 0.0257(15) Uani 1 1 d . . .
H24A H -0.0147 0.2367 -0.4697 0.031 Uiso 1 1 calc R . .
H24B H 0.0825 0.1776 -0.4817 0.031 Uiso 1 1 calc R . .
C25 C 0.2806(10) 0.2400(3) -0.4292(6) 0.0289(15) Uani 1 1 d . . .
H25A H 0.3009 0.2384 -0.5155 0.035 Uiso 1 1 calc R . .
H25B H 0.3877 0.2190 -0.3733 0.035 Uiso 1 1 calc R . .
C26 C 0.2931(12) 0.3016(3) -0.3861(6) 0.0308(16) Uani 1 1 d . . .
H26A H 0.4120 0.3189 -0.4014 0.037 Uiso 1 1 calc R . .
H26B H 0.1797 0.3225 -0.4355 0.037 Uiso 1 1 calc R . .
C27 C 0.2046(10) 0.1522(3) -0.2489(6) 0.0242(14) Uani 1 1 d . . .
H27A H 0.1920 0.1200 -0.3057 0.036 Uiso 1 1 calc R . .
H27B H 0.1816 0.1403 -0.1680 0.036 Uiso 1 1 calc R . .
H27C H 0.3356 0.1678 -0.2354 0.036 Uiso 1 1 calc R . .
N2 N 0.3654(8) -0.1286(3) 0.0502(4) 0.0243(12) Uani 1 1 d . . .
N3 N 0.3147(8) -0.1589(2) -0.2374(5) 0.0210(11) Uani 1 1 d . A .
H3C H 0.4358 -0.1471 -0.1940 0.025 Uiso 1 1 calc R . .
H3D H 0.3055 -0.1961 -0.2193 0.025 Uiso 1 1 calc R . .
N4 N 0.0737(7) -0.0505(2) -0.2948(4) 0.0198(11) Uani 1 1 d . A .
N5 N -0.0648(7) -0.0817(2) -0.0606(5) 0.0205(12) Uani 1 1 d . A .
H5C H -0.0996 -0.1095 -0.0122 0.025 Uiso 1 1 calc R . .
H5D H 0.0070 -0.0559 -0.0063 0.025 Uiso 1 1 calc R . .
N12 N 0.3856(5) 0.0704(4) 0.5182(3) 0.0332(7) Uani 1 1 d . . .
N13 N 0.3671(8) -0.0150(3) 0.2790(5) 0.0258(12) Uani 1 1 d . B .
H13C H 0.2818 -0.0248 0.3266 0.031 Uiso 1 1 calc R . .
H13D H 0.3112 -0.0254 0.1973 0.031 Uiso 1 1 calc R . .
N14 N 0.6432(3) 0.0717(3) 0.2152(2) 0.0162(5) Uani 1 1 d . B .
N15 N 0.3554(8) 0.1568(2) 0.2784(5) 0.0243(12) Uani 1 1 d . B .
H15C H 0.2868 0.1663 0.1986 0.029 Uiso 1 1 calc R . .
H15D H 0.2788 0.1657 0.3325 0.029 Uiso 1 1 calc R . .
N22 N 0.3528(9) 0.2735(3) 0.0389(5) 0.0323(15) Uani 1 1 d . . .
N23 N -0.0735(8) 0.2260(2) -0.0725(5) 0.0201(12) Uani 1 1 d . C .
H23C H -0.0007 0.1997 -0.0204 0.024 Uiso 1 1 calc R . .
H23D H -0.1046 0.2534 -0.0216 0.024 Uiso 1 1 calc R . .
N24 N 0.0616(7) 0.1949(2) -0.3053(4) 0.0171(10) Uani 1 1 d . C .
N25 N 0.2971(9) 0.3049(2) -0.2521(5) 0.0255(13) Uani 1 1 d . C .
H25C H 0.2854 0.3421 -0.2337 0.031 Uiso 1 1 calc R . .
H25D H 0.4189 0.2938 -0.2087 0.031 Uiso 1 1 calc R . .
O3 O 0.3514(7) -0.0849(2) -0.0185(4) 0.0268(11) Uani 1 1 d . A .
O4 O 0.2428(7) -0.1650(2) 0.0035(4) 0.0263(11) Uani 1 1 d . A .
O13 O 0.2314(4) 0.0700(3) 0.4337(2) 0.0333(6) Uani 1 1 d . B .
O14 O 0.5350(3) 0.0718(3) 0.4736(2) 0.0256(5) Uani 1 1 d . B .
O23 O 0.2274(7) 0.3101(2) -0.0103(4) 0.0281(11) Uani 1 1 d . C .
O24 O 0.3415(6) 0.23120(19) -0.0300(4) 0.0240(10) Uani 1 1 d . C .
Ni1 Ni 0.11391(10) -0.11677(2) -0.16434(6) 0.01630(17) Uani 1 1 d . . .
Ni2 Ni 0.38959(5) 0.07086(5) 0.28270(3) 0.01520(10) Uani 1 1 d . . .
Ni3 Ni 0.09978(10) 0.26148(2) -0.17588(6) 0.01734(17) Uani 1 1 d . . .
N1 N -0.080(3) -0.1721(9) -0.254(2) 0.026(3) Uiso 0.241(11) 1 d PD A 1
O1 O -0.242(3) -0.1652(10) -0.315(2) 0.041(3) Uiso 0.241(11) 1 d PD A 1
O2 O -0.049(4) -0.2240(8) -0.241(2) 0.020(3) Uiso 0.241(11) 1 d PD A 1
N1A N -0.1583(11) -0.2065(2) -0.2847(7) 0.0259(18) Uani 0.759(11) 1 d PD A 2
O1A O -0.1220(9) -0.1533(2) -0.2776(5) 0.0208(15) Uani 0.759(11) 1 d PD A 2
O2A O -0.0236(11) -0.2369(4) -0.2189(8) 0.035(2) Uani 0.759(11) 1 d PD A 2
N11 N 0.1773(5) 0.0719(3) 0.1081(3) 0.0194(9) Uani 0.841(9) 1 d PD B 3
O11 O 0.1076(11) 0.1157(3) 0.0545(6) 0.0324(16) Uani 0.841(9) 1 d PD B 3
O12 O 0.1144(10) 0.0276(3) 0.0569(5) 0.0368(18) Uani 0.841(9) 1 d PD B 3
N11A N 0.086(2) 0.0762(9) 0.0291(13) 0.008(4) Uiso 0.159(9) 1 d PD B 4
O11A O 0.172(3) 0.0466(8) 0.1264(17) 0.014(5) Uiso 0.159(9) 1 d PD B 4
O12A O 0.148(4) 0.1274(9) 0.030(2) 0.019(6) Uiso 0.159(9) 1 d PD B 4
N21 N -0.099(3) 0.3238(8) -0.2650(19) 0.026(3) Uiso 0.266(12) 1 d PD C 5
O22 O -0.063(3) 0.3739(8) -0.2700(16) 0.020(3) Uiso 0.266(12) 1 d PD C 5
O21 O -0.250(3) 0.3053(9) -0.3216(19) 0.041(3) Uiso 0.266(12) 1 d PD C 5
N21A N -0.1800(11) 0.3502(3) -0.2971(6) 0.0243(19) Uani 0.734(12) 1 d PD C 6
O21A O -0.1412(9) 0.2975(2) -0.2909(6) 0.0243(17) Uani 0.734(12) 1 d PD C 6
O22A O -0.0443(10) 0.3786(3) -0.2287(7) 0.0291(17) Uani 0.734(12) 1 d PD C 6


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N3 1.477(8) . ?
C1 C2 1.481(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.538(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N4 1.500(8) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.472(10) . ?
C4 N4 1.499(9) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.500(9) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N5 1.456(8) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 N4 1.488(8) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C11 N13 1.452(8) . ?
C11 C12 1.533(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.507(9) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N14 1.497(9) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 N14 1.488(9) . ?
C14 C15 1.512(10) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.490(11) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 N15 1.480(8) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 N14 1.476(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C21 N23 1.487(7) . ?
C21 C22 1.523(10) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.539(10) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 N24 1.492(8) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 N24 1.474(8) . ?
C24 C25 1.501(10) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.543(10) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 N25 1.460(9) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 N24 1.467(8) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
N2 O4 1.250(8) . ?
N2 O3 1.277(7) . ?
N3 Ni1 2.058(6) . ?
N3 H3C 0.9200 . ?
N3 H3D 0.9200 . ?
N4 Ni1 2.107(5) . ?
N5 Ni1 2.072(6) . ?
N5 H5C 0.9200 . ?
N5 H5D 0.9200 . ?
N12 O13 1.251(4) . ?
N12 O14 1.271(4) . ?
N13 Ni2 2.061(6) . ?
N13 H13C 0.9200 . ?
N13 H13D 0.9200 . ?
N14 Ni2 2.105(3) . ?
N15 Ni2 2.069(6) . ?
N15 H15C 0.9200 . ?
N15 H15D 0.9200 . ?
N22 O24 1.253(8) . ?
N22 O23 1.273(8) . ?
N23 Ni3 2.045(6) . ?
N23 H23C 0.9200 . ?
N23 H23D 0.9200 . ?
N24 Ni3 2.104(5) . ?
N25 Ni3 2.074(6) . ?
N25 H25C 0.9200 . ?
N25 H25D 0.9200 . ?
O3 Ni1 2.161(4) . ?
O4 Ni1 2.174(4) . ?
O13 Ni2 2.210(2) . ?
O14 Ni2 2.094(2) . ?
O23 Ni3 2.159(4) . ?
O24 Ni3 2.167(4) . ?
Ni1 N1 1.99(2) . ?
Ni1 O1A 2.026(5) . ?
Ni2 O11A 2.091(19) . ?
Ni2 N11 2.128(4) . ?
Ni3 O21A 2.053(5) . ?
Ni3 N21 2.12(2) . ?
N1 O1 1.198(10) . ?
N1 O2 1.263(18) . ?
N1A O2A 1.277(8) . ?
N1A O1A 1.295(7) . ?
N11 O12 1.230(7) . ?
N11 O11 1.245(7) . ?
N11A O12A 1.301(10) . ?
N11A O11A 1.302(10) . ?
N21 O21 1.189(10) . ?
N21 O22 1.229(17) . ?
N21A O22A 1.265(7) . ?
N21A O21A 1.289(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 C1 C2 112.8(5) . . ?
N3 C1 H1A 109.0 . . ?
C2 C1 H1A 109.0 . . ?
N3 C1 H1B 109.0 . . ?
C2 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C1 C2 C3 113.6(6) . . ?
C1 C2 H2A 108.8 . . ?
C3 C2 H2A 108.8 . . ?
C1 C2 H2B 108.8 . . ?
C3 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
N4 C3 C2 116.1(5) . . ?
N4 C3 H3A 108.3 . . ?
C2 C3 H3A 108.3 . . ?
N4 C3 H3B 108.3 . . ?
C2 C3 H3B 108.3 . . ?
H3A C3 H3B 107.4 . . ?
C5 C4 N4 117.6(5) . . ?
C5 C4 H4A 107.9 . . ?
N4 C4 H4A 107.9 . . ?
C5 C4 H4B 107.9 . . ?
N4 C4 H4B 107.9 . . ?
H4A C4 H4B 107.2 . . ?
C4 C5 C6 115.8(6) . . ?
C4 C5 H5A 108.3 . . ?
C6 C5 H5A 108.3 . . ?
C4 C5 H5B 108.3 . . ?
C6 C5 H5B 108.3 . . ?
H5A C5 H5B 107.4 . . ?
N5 C6 C5 112.9(5) . . ?
N5 C6 H6A 109.0 . . ?
C5 C6 H6A 109.0 . . ?
N5 C6 H6B 109.0 . . ?
C5 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N13 C11 C12 108.7(6) . . ?
N13 C11 H11A 110.0 . . ?
C12 C11 H11A 110.0 . . ?
N13 C11 H11B 110.0 . . ?
C12 C11 H11B 110.0 . . ?
H11A C11 H11B 108.3 . . ?
C13 C12 C11 114.7(5) . . ?
C13 C12 H12A 108.6 . . ?
C11 C12 H12A 108.6 . . ?
C13 C12 H12B 108.6 . . ?
C11 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
N14 C13 C12 116.3(5) . . ?
N14 C13 H13A 108.2 . . ?
C12 C13 H13A 108.2 . . ?
N14 C13 H13B 108.2 . . ?
C12 C13 H13B 108.2 . . ?
H13A C13 H13B 107.4 . . ?
N14 C14 C15 118.2(6) . . ?
N14 C14 H14A 107.8 . . ?
C15 C14 H14A 107.8 . . ?
N14 C14 H14B 107.8 . . ?
C15 C14 H14B 107.8 . . ?
H14A C14 H14B 107.1 . . ?
C16 C15 C14 114.0(6) . . ?
C16 C15 H15A 108.7 . . ?
C14 C15 H15A 108.7 . . ?
C16 C15 H15B 108.7 . . ?
C14 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
N15 C16 C15 111.1(6) . . ?
N15 C16 H16A 109.4 . . ?
C15 C16 H16A 109.4 . . ?
N15 C16 H16B 109.4 . . ?
C15 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
N14 C17 H17A 109.5 . . ?
N14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N23 C21 C22 109.6(5) . . ?
N23 C21 H21A 109.7 . . ?
C22 C21 H21A 109.7 . . ?
N23 C21 H21B 109.7 . . ?
C22 C21 H21B 109.7 . . ?
H21A C21 H21B 108.2 . . ?
C21 C22 C23 113.8(6) . . ?
C21 C22 H22A 108.8 . . ?
C23 C22 H22A 108.8 . . ?
C21 C22 H22B 108.8 . . ?
C23 C22 H22B 108.8 . . ?
H22A C22 H22B 107.7 . . ?
N24 C23 C22 116.1(5) . . ?
N24 C23 H23A 108.3 . . ?
C22 C23 H23A 108.3 . . ?
N24 C23 H23B 108.3 . . ?
C22 C23 H23B 108.3 . . ?
H23A C23 H23B 107.4 . . ?
N24 C24 C25 117.0(5) . . ?
N24 C24 H24A 108.0 . . ?
C25 C24 H24A 108.0 . . ?
N24 C24 H24B 108.0 . . ?
C25 C24 H24B 108.0 . . ?
H24A C24 H24B 107.3 . . ?
C24 C25 C26 114.8(6) . . ?
C24 C25 H25A 108.6 . . ?
C26 C25 H25A 108.6 . . ?
C24 C25 H25B 108.6 . . ?
C26 C25 H25B 108.6 . . ?
H25A C25 H25B 107.6 . . ?
N25 C26 C25 110.1(6) . . ?
N25 C26 H26A 109.6 . . ?
C25 C26 H26A 109.6 . . ?
N25 C26 H26B 109.6 . . ?
C25 C26 H26B 109.6 . . ?
H26A C26 H26B 108.2 . . ?
N24 C27 H27A 109.5 . . ?
N24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O4 N2 O3 112.5(4) . . ?
C1 N3 Ni1 119.9(4) . . ?
C1 N3 H3C 107.3 . . ?
Ni1 N3 H3C 107.3 . . ?
C1 N3 H3D 107.3 . . ?
Ni1 N3 H3D 107.3 . . ?
H3C N3 H3D 106.9 . . ?
C7 N4 C4 108.2(5) . . ?
C7 N4 C3 108.4(5) . . ?
C4 N4 C3 105.4(4) . . ?
C7 N4 Ni1 108.0(3) . . ?
C4 N4 Ni1 112.8(4) . . ?
C3 N4 Ni1 113.8(4) . . ?
C6 N5 Ni1 117.5(4) . . ?
C6 N5 H5C 107.9 . . ?
Ni1 N5 H5C 107.9 . . ?
C6 N5 H5D 107.9 . . ?
Ni1 N5 H5D 107.9 . . ?
H5C N5 H5D 107.2 . . ?
O13 N12 O14 112.3(3) . . ?
C11 N13 Ni2 119.2(4) . . ?
C11 N13 H13C 107.5 . . ?
Ni2 N13 H13C 107.5 . . ?
C11 N13 H13D 107.5 . . ?
Ni2 N13 H13D 107.5 . . ?
H13C N13 H13D 107.0 . . ?
C17 N14 C14 110.3(6) . . ?
C17 N14 C13 108.6(6) . . ?
C14 N14 C13 104.5(3) . . ?
C17 N14 Ni2 111.01(19) . . ?
C14 N14 Ni2 111.0(4) . . ?
C13 N14 Ni2 111.3(4) . . ?
C16 N15 Ni2 119.3(4) . . ?
C16 N15 H15C 107.5 . . ?
Ni2 N15 H15C 107.5 . . ?
C16 N15 H15D 107.5 . . ?
Ni2 N15 H15D 107.5 . . ?
H15C N15 H15D 107.0 . . ?
O24 N22 O23 111.4(5) . . ?
C21 N23 Ni3 118.6(4) . . ?
C21 N23 H23C 107.7 . . ?
Ni3 N23 H23C 107.7 . . ?
C21 N23 H23D 107.7 . . ?
Ni3 N23 H23D 107.7 . . ?
H23C N23 H23D 107.1 . . ?
C27 N24 C24 109.4(5) . . ?
C27 N24 C23 109.5(5) . . ?
C24 N24 C23 104.7(4) . . ?
C27 N24 Ni3 106.3(4) . . ?
C24 N24 Ni3 112.9(4) . . ?
C23 N24 Ni3 114.0(4) . . ?
C26 N25 Ni3 121.7(4) . . ?
C26 N25 H25C 106.9 . . ?
Ni3 N25 H25C 106.9 . . ?
C26 N25 H25D 106.9 . . ?
Ni3 N25 H25D 106.9 . . ?
H25C N25 H25D 106.7 . . ?
N2 O3 Ni1 94.7(4) . . ?
N2 O4 Ni1 94.9(3) . . ?
N12 O13 Ni2 92.29(18) . . ?
N12 O14 Ni2 97.2(2) . . ?
N22 O23 Ni3 95.3(4) . . ?
N22 O24 Ni3 95.6(4) . . ?
N1 Ni1 O1A 16.2(5) . . ?
N1 Ni1 N3 86.9(7) . . ?
O1A Ni1 N3 95.7(3) . . ?
N1 Ni1 N5 95.5(7) . . ?
O1A Ni1 N5 89.1(2) . . ?
N3 Ni1 N5 169.6(2) . . ?
N1 Ni1 N4 101.8(7) . . ?
O1A Ni1 N4 87.4(2) . . ?
N3 Ni1 N4 95.7(2) . . ?
N5 Ni1 N4 93.7(2) . . ?
N1 Ni1 O3 157.2(6) . . ?
O1A Ni1 O3 170.5(2) . . ?
N3 Ni1 O3 88.2(2) . . ?
N5 Ni1 O3 85.7(2) . . ?
N4 Ni1 O3 100.86(19) . . ?
N1 Ni1 O4 99.3(6) . . ?
O1A Ni1 O4 113.9(2) . . ?
N3 Ni1 O4 83.0(2) . . ?
N5 Ni1 O4 86.6(2) . . ?
N4 Ni1 O4 158.8(2) . . ?
O3 Ni1 O4 57.95(18) . . ?
N13 Ni2 N15 169.15(12) . . ?
N13 Ni2 O11A 70.6(5) . . ?
N15 Ni2 O11A 101.4(5) . . ?
N13 Ni2 O14 92.7(2) . . ?
N15 Ni2 O14 92.2(2) . . ?
O11A Ni2 O14 155.2(5) . . ?
N13 Ni2 N14 94.1(3) . . ?
N15 Ni2 N14 95.0(3) . . ?
O11A Ni2 N14 104.0(5) . . ?
O14 Ni2 N14 95.25(10) . . ?
N13 Ni2 N11 87.6(2) . . ?
N15 Ni2 N11 85.1(2) . . ?
O11A Ni2 N11 17.4(5) . . ?
O14 Ni2 N11 165.12(11) . . ?
N14 Ni2 N11 99.56(12) . . ?
N13 Ni2 O13 87.4(3) . . ?
N15 Ni2 O13 87.1(3) . . ?
O11A Ni2 O13 101.5(5) . . ?
O14 Ni2 O13 58.16(10) . . ?
N14 Ni2 O13 153.40(10) . . ?
N11 Ni2 O13 107.03(12) . . ?
N23 Ni3 O21A 89.4(3) . . ?
N23 Ni3 N25 170.0(2) . . ?
O21A Ni3 N25 95.0(3) . . ?
N23 Ni3 N24 93.5(2) . . ?
O21A Ni3 N24 87.3(2) . . ?
N25 Ni3 N24 95.6(2) . . ?
N23 Ni3 N21 97.1(6) . . ?
O21A Ni3 N21 19.9(4) . . ?
N25 Ni3 N21 84.4(5) . . ?
N24 Ni3 N21 105.0(6) . . ?
N23 Ni3 O23 86.9(2) . . ?
O21A Ni3 O23 114.0(2) . . ?
N25 Ni3 O23 83.1(2) . . ?
N24 Ni3 O23 158.7(2) . . ?
N21 Ni3 O23 96.0(5) . . ?
N23 Ni3 O24 85.97(19) . . ?
O21A Ni3 O24 170.6(2) . . ?
N25 Ni3 O24 88.4(2) . . ?
N24 Ni3 O24 101.10(18) . . ?
N21 Ni3 O24 153.4(5) . . ?
O23 Ni3 O24 57.68(19) . . ?
O1 N1 O2 108(3) . . ?
O1 N1 Ni1 129.9(19) . . ?
O2 N1 Ni1 121.4(18) . . ?
O2A N1A O1A 114.5(7) . . ?
N1A O1A Ni1 125.7(5) . . ?
O12 N11 O11 116.8(4) . . ?
O12 N11 Ni2 120.0(5) . . ?
O11 N11 Ni2 123.2(5) . . ?
O12A N11A O11A 114(2) . . ?
N11A O11A Ni2 128.8(16) . . ?
O21 N21 O22 120(2) . . ?
O21 N21 Ni3 113.4(17) . . ?
O22 N21 Ni3 125.9(15) . . ?
O22A N21A O21A 111.8(7) . . ?
N21A O21A Ni3 125.4(5) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 C1 C2 C3 -69.8(7) . . . . ?
C1 C2 C3 N4 73.2(7) . . . . ?
N4 C4 C5 C6 -68.3(8) . . . . ?
C4 C5 C6 N5 67.2(7) . . . . ?
N13 C11 C12 C13 69.9(7) . . . . ?
C11 C12 C13 N14 -73.6(7) . . . . ?
N14 C14 C15 C16 74.2(7) . . . . ?
C14 C15 C16 N15 -68.1(8) . . . . ?
N23 C21 C22 C23 -69.9(6) . . . . ?
C21 C22 C23 N24 70.0(7) . . . . ?
N24 C24 C25 C26 -75.5(7) . . . . ?
C24 C25 C26 N25 67.9(8) . . . . ?
C2 C1 N3 Ni1 51.3(7) . . . . ?
C5 C4 N4 C7 -65.5(8) . . . . ?
C5 C4 N4 C3 178.7(6) . . . . ?
C5 C4 N4 Ni1 53.9(7) . . . . ?
C2 C3 N4 C7 68.8(7) . . . . ?
C2 C3 N4 C4 -175.6(6) . . . . ?
C2 C3 N4 Ni1 -51.5(7) . . . . ?
C5 C6 N5 Ni1 -56.5(7) . . . . ?
C12 C11 N13 Ni2 -58.4(6) . . . . ?
C15 C14 N14 C17 67.8(7) . . . . ?
C15 C14 N14 C13 -175.7(7) . . . . ?
C15 C14 N14 Ni2 -55.7(6) . . . . ?
C12 C13 N14 C17 -66.2(6) . . . . ?
C12 C13 N14 C14 176.1(6) . . . . ?
C12 C13 N14 Ni2 56.3(6) . . . . ?
C15 C16 N15 Ni2 54.1(7) . . . . ?
C22 C21 N23 Ni3 60.7(6) . . . . ?
C25 C24 N24 C27 -64.7(7) . . . . ?
C25 C24 N24 C23 177.9(6) . . . . ?
C25 C24 N24 Ni3 53.4(7) . . . . ?
C22 C23 N24 C27 65.2(7) . . . . ?
C22 C23 N24 C24 -177.6(6) . . . . ?
C22 C23 N24 Ni3 -53.8(7) . . . . ?
C25 C26 N25 Ni3 -48.4(8) . . . . ?
O4 N2 O3 Ni1 -0.8(6) . . . . ?
O3 N2 O4 Ni1 0.8(6) . . . . ?
O14 N12 O13 Ni2 0.9(8) . . . . ?
O13 N12 O14 Ni2 -1.0(9) . . . . ?
O24 N22 O23 Ni3 1.1(6) . . . . ?
O23 N22 O24 Ni3 -1.1(6) . . . . ?
C1 N3 Ni1 N1 71.8(8) . . . . ?
C1 N3 Ni1 O1A 58.1(5) . . . . ?
C1 N3 Ni1 N5 175.4(11) . . . . ?
C1 N3 Ni1 N4 -29.8(5) . . . . ?
C1 N3 Ni1 O3 -130.5(5) . . . . ?
C1 N3 Ni1 O4 171.5(5) . . . . ?
C6 N5 Ni1 N1 -62.5(8) . . . . ?
C6 N5 Ni1 O1A -47.6(5) . . . . ?
C6 N5 Ni1 N3 -165.4(11) . . . . ?
C6 N5 Ni1 N4 39.7(5) . . . . ?
C6 N5 Ni1 O3 140.3(5) . . . . ?
C6 N5 Ni1 O4 -161.6(5) . . . . ?
C7 N4 Ni1 N1 -179.9(8) . . . . ?
C4 N4 Ni1 N1 60.6(8) . . . . ?
C3 N4 Ni1 N1 -59.4(8) . . . . ?
C7 N4 Ni1 O1A 172.6(5) . . . . ?
C4 N4 Ni1 O1A 53.1(4) . . . . ?
C3 N4 Ni1 O1A -66.9(4) . . . . ?
C7 N4 Ni1 N3 -91.9(4) . . . . ?
C4 N4 Ni1 N3 148.6(4) . . . . ?
C3 N4 Ni1 N3 28.6(4) . . . . ?
C7 N4 Ni1 N5 83.7(4) . . . . ?
C4 N4 Ni1 N5 -35.8(4) . . . . ?
C3 N4 Ni1 N5 -155.8(4) . . . . ?
C7 N4 Ni1 O3 -2.6(4) . . . . ?
C4 N4 Ni1 O3 -122.1(4) . . . . ?
C3 N4 Ni1 O3 117.8(4) . . . . ?
C7 N4 Ni1 O4 -6.6(8) . . . . ?
C4 N4 Ni1 O4 -126.1(6) . . . . ?
C3 N4 Ni1 O4 113.9(6) . . . . ?
N2 O3 Ni1 N1 -5(2) . . . . ?
N2 O3 Ni1 O1A 32.2(16) . . . . ?
N2 O3 Ni1 N3 -82.4(4) . . . . ?
N2 O3 Ni1 N5 89.2(4) . . . . ?
N2 O3 Ni1 N4 -177.8(4) . . . . ?
N2 O3 Ni1 O4 0.5(3) . . . . ?
N2 O4 Ni1 N1 177.4(8) . . . . ?
N2 O4 Ni1 O1A -175.1(4) . . . . ?
N2 O4 Ni1 N3 91.7(4) . . . . ?
N2 O4 Ni1 N5 -87.6(4) . . . . ?
N2 O4 Ni1 N4 4.0(8) . . . . ?
N2 O4 Ni1 O3 -0.5(4) . . . . ?
C11 N13 Ni2 N15 -170.7(7) . . . . ?
C11 N13 Ni2 O11A 145.3(7) . . . . ?
C11 N13 Ni2 O14 -53.6(5) . . . . ?
C11 N13 Ni2 N14 41.9(5) . . . . ?
C11 N13 Ni2 N11 141.3(5) . . . . ?
C11 N13 Ni2 O13 -111.5(5) . . . . ?
C16 N15 Ni2 N13 176.5(6) . . . . ?
C16 N15 Ni2 O11A -141.6(7) . . . . ?
C16 N15 Ni2 O14 59.3(5) . . . . ?
C16 N15 Ni2 N14 -36.2(5) . . . . ?
C16 N15 Ni2 N11 -135.3(5) . . . . ?
C16 N15 Ni2 O13 117.3(5) . . . . ?
N12 O14 Ni2 N13 -84.6(6) . . . . ?
N12 O14 Ni2 N15 85.7(6) . . . . ?
N12 O14 Ni2 O11A -38.0(14) . . . . ?
N12 O14 Ni2 N14 -179.0(6) . . . . ?
N12 O14 Ni2 N11 6.4(14) . . . . ?
N12 O14 Ni2 O13 0.6(5) . . . . ?
C17 N14 Ni2 N13 84.5(6) . . . . ?
C14 N14 Ni2 N13 -152.4(4) . . . . ?
C13 N14 Ni2 N13 -36.5(4) . . . . ?
C17 N14 Ni2 N15 -89.6(6) . . . . ?
C14 N14 Ni2 N15 33.4(4) . . . . ?
C13 N14 Ni2 N15 149.3(4) . . . . ?
C17 N14 Ni2 O11A 13.5(8) . . . . ?
C14 N14 Ni2 O11A 136.5(6) . . . . ?
C13 N14 Ni2 O11A -107.6(6) . . . . ?
C17 N14 Ni2 O14 177.7(6) . . . . ?
C14 N14 Ni2 O14 -59.3(4) . . . . ?
C13 N14 Ni2 O14 56.6(4) . . . . ?
C17 N14 Ni2 N11 -3.8(7) . . . . ?
C14 N14 Ni2 N11 119.3(4) . . . . ?
C13 N14 Ni2 N11 -124.8(4) . . . . ?
C17 N14 Ni2 O13 176.9(7) . . . . ?
C14 N14 Ni2 O13 -60.0(9) . . . . ?
C13 N14 Ni2 O13 55.9(9) . . . . ?
N12 O13 Ni2 N13 94.2(6) . . . . ?
N12 O13 Ni2 N15 -95.1(6) . . . . ?
N12 O13 Ni2 O11A 163.9(7) . . . . ?
N12 O13 Ni2 O14 -0.6(5) . . . . ?
N12 O13 Ni2 N14 0.3(10) . . . . ?
N12 O13 Ni2 N11 -179.0(6) . . . . ?
C21 N23 Ni3 O21A 45.2(5) . . . . ?
C21 N23 Ni3 N25 161.5(12) . . . . ?
C21 N23 Ni3 N24 -42.0(5) . . . . ?
C21 N23 Ni3 N21 63.6(7) . . . . ?
C21 N23 Ni3 O23 159.3(5) . . . . ?
C21 N23 Ni3 O24 -142.9(5) . . . . ?
C26 N25 Ni3 N23 -173.8(11) . . . . ?
C26 N25 Ni3 O21A -58.0(5) . . . . ?
C26 N25 Ni3 N24 29.8(5) . . . . ?
C26 N25 Ni3 N21 -74.8(7) . . . . ?
C26 N25 Ni3 O23 -171.6(5) . . . . ?
C26 N25 Ni3 O24 130.8(5) . . . . ?
C27 N24 Ni3 N23 -84.6(4) . . . . ?
C24 N24 Ni3 N23 155.5(4) . . . . ?
C23 N24 Ni3 N23 36.2(4) . . . . ?
C27 N24 Ni3 O21A -173.8(5) . . . . ?
C24 N24 Ni3 O21A 66.3(4) . . . . ?
C23 N24 Ni3 O21A -53.0(4) . . . . ?
C27 N24 Ni3 N25 91.5(4) . . . . ?
C24 N24 Ni3 N25 -28.5(4) . . . . ?
C23 N24 Ni3 N25 -147.8(4) . . . . ?
C27 N24 Ni3 N21 177.1(6) . . . . ?
C24 N24 Ni3 N21 57.2(7) . . . . ?
C23 N24 Ni3 N21 -62.1(7) . . . . ?
C27 N24 Ni3 O23 6.0(8) . . . . ?
C24 N24 Ni3 O23 -113.9(6) . . . . ?
C23 N24 Ni3 O23 126.8(6) . . . . ?
C27 N24 Ni3 O24 2.0(4) . . . . ?
C24 N24 Ni3 O24 -117.9(4) . . . . ?
C23 N24 Ni3 O24 122.8(4) . . . . ?
N22 O23 Ni3 N23 86.4(4) . . . . ?
N22 O23 Ni3 O21A 174.4(4) . . . . ?
N22 O23 Ni3 N25 -93.2(4) . . . . ?
N22 O23 Ni3 N24 -5.3(8) . . . . ?
N22 O23 Ni3 N21 -176.7(7) . . . . ?
N22 O23 Ni3 O24 -0.7(4) . . . . ?
N22 O24 Ni3 N23 -88.2(4) . . . . ?
N22 O24 Ni3 O21A -27.8(16) . . . . ?
N22 O24 Ni3 N25 83.6(4) . . . . ?
N22 O24 Ni3 N24 179.0(4) . . . . ?
N22 O24 Ni3 N21 9.7(13) . . . . ?
N22 O24 Ni3 O23 0.7(4) . . . . ?
O1A Ni1 N1 O1 -12.7(18) . . . . ?
N3 Ni1 N1 O1 -136(3) . . . . ?
N5 Ni1 N1 O1 55(3) . . . . ?
N4 Ni1 N1 O1 -40(3) . . . . ?
O3 Ni1 N1 O1 146.5(19) . . . . ?
O4 Ni1 N1 O1 142(3) . . . . ?
O1A Ni1 N1 O2 175(5) . . . . ?
N3 Ni1 N1 O2 52(2) . . . . ?
N5 Ni1 N1 O2 -118(2) . . . . ?
N4 Ni1 N1 O2 147(2) . . . . ?
O3 Ni1 N1 O2 -26(4) . . . . ?
O4 Ni1 N1 O2 -31(2) . . . . ?
O2A N1A O1A Ni1 -4.8(12) . . . . ?
N1 Ni1 O1A N1A 2(3) . . . . ?
N3 Ni1 O1A N1A 59.2(7) . . . . ?
N5 Ni1 O1A N1A -111.6(7) . . . . ?
N4 Ni1 O1A N1A 154.6(7) . . . . ?
O3 Ni1 O1A N1A -54.8(19) . . . . ?
O4 Ni1 O1A N1A -25.7(8) . . . . ?
N13 Ni2 N11 O12 -2.9(5) . . . . ?
N15 Ni2 N11 O12 -174.8(5) . . . . ?
O11A Ni2 N11 O12 -15.6(18) . . . . ?
O14 Ni2 N11 O12 -94.6(12) . . . . ?
N14 Ni2 N11 O12 90.9(5) . . . . ?
O13 Ni2 N11 O12 -89.4(5) . . . . ?
N13 Ni2 N11 O11 175.4(6) . . . . ?
N15 Ni2 N11 O11 3.5(5) . . . . ?
O11A Ni2 N11 O11 163(2) . . . . ?
O14 Ni2 N11 O11 83.7(12) . . . . ?
N14 Ni2 N11 O11 -90.8(6) . . . . ?
O13 Ni2 N11 O11 88.9(6) . . . . ?
O12A N11A O11A Ni2 1(3) . . . . ?
N13 Ni2 O11A N11A -166.5(19) . . . . ?
N15 Ni2 O11A N11A 21.2(18) . . . . ?
O14 Ni2 O11A N11A 143.2(14) . . . . ?
N14 Ni2 O11A N11A -77.0(18) . . . . ?
N11 Ni2 O11A N11A 0.1(9) . . . . ?
O13 Ni2 O11A N11A 110.5(17) . . . . ?
N23 Ni3 N21 O21 -56.3(18) . . . . ?
O21A Ni3 N21 O21 11.5(14) . . . . ?
N25 Ni3 N21 O21 133.6(18) . . . . ?
N24 Ni3 N21 O21 39.3(19) . . . . ?
O23 Ni3 N21 O21 -144.0(18) . . . . ?
O24 Ni3 N21 O21 -151.6(13) . . . . ?
N23 Ni3 N21 O22 129.6(19) . . . . ?
O21A Ni3 N21 O22 -163(4) . . . . ?
N25 Ni3 N21 O22 -40.5(19) . . . . ?
N24 Ni3 N21 O22 -134.8(19) . . . . ?
O23 Ni3 N21 O22 42(2) . . . . ?
O24 Ni3 N21 O22 34(3) . . . . ?
O22A N21A O21A Ni3 4.2(11) . . . . ?
N23 Ni3 O21A N21A 111.0(7) . . . . ?
N25 Ni3 O21A N21A -60.1(7) . . . . ?
N24 Ni3 O21A N21A -155.5(7) . . . . ?
N21 Ni3 O21A N21A -2.2(18) . . . . ?
O23 Ni3 O21A N21A 24.6(8) . . . . ?
O24 Ni3 O21A N21A 50.8(19) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3C N22 0.92 2.74 3.230(8) 114.3 2_645
N3 H3D O2 0.92 2.56 3.01(3) 110.6 .
N3 H3D O2A 0.92 2.53 3.089(10) 119.2 .
N5 H5C O23 0.92 2.17 3.011(7) 152.2 2_545
N5 H5C O22A 0.92 2.60 3.215(9) 124.6 2_545
N5 H5D O12 0.92 2.19 3.053(8) 155.7 .
N13 H13D O12 0.92 2.21 2.839(7) 125.0 .
N15 H15C O12A 0.92 2.08 2.84(3) 139.0 .
N15 H15C O11 0.92 2.14 2.825(8) 129.9 .
N23 H23C O12A 0.92 2.04 2.91(3) 158.3 .
N23 H23C O11 0.92 2.24 3.113(8) 159.2 .
N23 H23D O4 0.92 2.22 3.042(7) 149.0 2
N23 H23D O2A 0.92 2.58 3.218(10) 127.1 2
N25 H25C O22A 0.92 2.51 3.058(10) 118.3 .
N25 H25C O22 0.92 2.53 3.01(2) 113.1 .

_diffrn_measured_fraction_theta_max 0.905
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.099

_database_code_depnum_ccdc_archive 'CCDC 994156'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex7_125K
_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;
Dinitro-(3,3-diamino-N-methyldipropylamine)nickel(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H19 N5 Ni O4'
_chemical_formula_sum            'C7 H19 N5 Ni O4'
_chemical_formula_weight         295.98


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'
O O 0.0106 0.0060 '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'


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

_cell_length_a                   7.096(5)
_cell_length_b                   23.843(5)
_cell_length_c                   10.917(5)
_cell_angle_alpha                90.000
_cell_angle_beta                 103.788(5)
_cell_angle_gamma                90.000
_cell_volume                     1793.8(16)
_cell_formula_units_Z            6
_cell_measurement_temperature    125(2)
_cell_measurement_reflns_used    4124
_cell_measurement_theta_min      3.0551
_cell_measurement_theta_max      29.0650

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/m

_exptl_crystal_description       Block
_exptl_crystal_colour            Violet
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936

_exptl_absorpt_coefficient_mu    1.636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.77921
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      125(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12300
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.12
_diffrn_reflns_theta_max         29.26
_reflns_number_total             4497
_reflns_number_gt                3651
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'POV-RAY for Windows, 3.62 (Cason, 2009)'
_computing_publication_material  'WinGX, 1.80.05 (Farrugia, 1999)'


_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 > 2sigma(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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0524P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4497
_refine_ls_number_parameters     241
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0359
_refine_ls_wR_factor_ref         0.0911
_refine_ls_wR_factor_gt          0.0871
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2924(4) 0.02058(10) 0.6186(2) 0.0226(5) Uani 1 1 d . . .
H1A H 0.1750 -0.0002 0.5747 0.027 Uiso 1 1 calc R . .
H1B H 0.4066 0.0020 0.5992 0.027 Uiso 1 1 calc R . .
C2 C 0.2799(3) 0.08020(11) 0.5708(2) 0.0240(5) Uani 1 1 d . . .
H2A H 0.2955 0.0800 0.4830 0.029 Uiso 1 1 calc R . .
H2B H 0.3893 0.1019 0.6226 0.029 Uiso 1 1 calc R . .
C3 C 0.0923(3) 0.10987(10) 0.5731(2) 0.0223(5) Uani 1 1 d . . .
H3A H 0.0834 0.1440 0.5205 0.027 Uiso 1 1 calc R . .
H3B H -0.0166 0.0851 0.5325 0.027 Uiso 1 1 calc R . .
C4 C -0.1353(3) 0.15131(10) 0.6728(2) 0.0204(5) Uani 1 1 d . . .
H4A H -0.2275 0.1230 0.6265 0.025 Uiso 1 1 calc R . .
H4B H -0.1389 0.1838 0.6157 0.025 Uiso 1 1 calc R . .
C5 C -0.2078(3) 0.17060(10) 0.7851(2) 0.0211(5) Uani 1 1 d . . .
H5A H -0.3283 0.1925 0.7543 0.025 Uiso 1 1 calc R . .
H5B H -0.1099 0.1960 0.8366 0.025 Uiso 1 1 calc R . .
C6 C -0.2487(3) 0.12384(10) 0.8684(2) 0.0198(4) Uani 1 1 d . . .
H6A H -0.3155 0.1394 0.9309 0.024 Uiso 1 1 calc R . .
H6B H -0.3362 0.0961 0.8163 0.024 Uiso 1 1 calc R . .
C7 C 0.2059(3) 0.17064(10) 0.7523(2) 0.0214(5) Uani 1 1 d . . .
H7A H 0.3375 0.1555 0.7646 0.032 Uiso 1 1 calc R . .
H7B H 0.1847 0.1830 0.8336 0.032 Uiso 1 1 calc R . .
H7C H 0.1899 0.2026 0.6943 0.032 Uiso 1 1 calc R . .
C11 C 0.5335(3) 0.12846(10) 1.3164(2) 0.0205(4) Uani 1 1 d . . .
H11A H 0.4962 0.0885 1.3033 0.025 Uiso 1 1 calc R . .
H11B H 0.5938 0.1341 1.4071 0.025 Uiso 1 1 calc R . .
C12 C 0.6772(4) 0.14303(10) 1.2400(2) 0.0240(5) Uani 1 1 d . . .
H12A H 0.6111 0.1406 1.1494 0.029 Uiso 1 1 calc R . .
H12B H 0.7820 0.1146 1.2567 0.029 Uiso 1 1 calc R . .
C13 C 0.7680(3) 0.20053(10) 1.2658(2) 0.0204(5) Uani 1 1 d . . .
H13A H 0.8145 0.2048 1.3583 0.024 Uiso 1 1 calc R . .
H13B H 0.8835 0.2017 1.2299 0.024 Uiso 1 1 calc R . .
C17 C 0.6000(5) 0.2500 1.0779(3) 0.0250(7) Uani 1 2 d S . .
H17A H 0.7209 0.2535 1.0499 0.038 Uiso 0.50 1 calc PR . .
H17B H 0.5148 0.2817 1.0456 0.038 Uiso 0.50 1 calc PR . .
H17C H 0.5350 0.2148 1.0460 0.038 Uiso 0.50 1 calc PR . .
N2 N 0.3607(3) 0.04979(9) 1.04517(18) 0.0234(4) Uani 1 1 d . . .
N3 N 0.3091(3) 0.01873(8) 0.75519(17) 0.0194(4) Uani 1 1 d . A .
H3C H 0.4297 0.0325 0.7941 0.023 Uiso 1 1 calc R . .
H3D H 0.3071 -0.0184 0.7778 0.023 Uiso 1 1 calc R . .
N4 N 0.0635(3) 0.12668(8) 0.69889(16) 0.0161(4) Uani 1 1 d . A .
N5 N -0.0689(3) 0.09581(8) 0.93497(17) 0.0165(4) Uani 1 1 d . A .
H5C H -0.1023 0.0680 0.9842 0.020 Uiso 1 1 calc R . .
H5D H 0.0040 0.1216 0.9889 0.020 Uiso 1 1 calc R . .
N11 N 0.1788(4) 0.2500 1.1091(2) 0.0158(5) Uani 1 2 d S . .
N12 N 0.3843(5) 0.2500 1.5186(3) 0.0299(7) Uani 1 2 d S . .
N13 N 0.3603(3) 0.16378(8) 1.27894(19) 0.0201(4) Uani 1 1 d . . .
H13C H 0.2788 0.1545 1.3299 0.024 Uiso 1 1 calc R . .
H13D H 0.2980 0.1539 1.1980 0.024 Uiso 1 1 calc R . .
N14 N 0.6444(3) 0.2500 1.2170(2) 0.0139(5) Uani 1 2 d S . .
O3 O 0.2387(2) 0.01298(7) 0.99817(15) 0.0226(3) Uani 1 1 d . A .
O4 O 0.3467(2) 0.09311(7) 0.97634(15) 0.0206(3) Uani 1 1 d . A .
O11 O 0.1126(3) 0.29406(8) 1.05621(17) 0.0318(4) Uani 1 1 d . . .
O13 O 0.2291(3) 0.2500 1.4337(2) 0.0272(5) Uani 1 2 d S . .
O14 O 0.5330(3) 0.2500 1.4744(2) 0.0231(5) Uani 1 2 d S . .
Ni1 Ni 0.10764(4) 0.060510(11) 0.83118(2) 0.01298(9) Uani 1 1 d . . .
Ni2 Ni 0.38904(5) 0.2500 1.28308(3) 0.01168(10) Uani 1 2 d S . .
N1 N -0.0904(5) 0.00154(15) 0.7442(3) 0.0176(8) Uiso 0.573(6) 1 d PD A 1
O1 O -0.2535(5) 0.01380(14) 0.6820(3) 0.0288(10) Uiso 0.573(6) 1 d PD A 1
O2 O -0.0474(6) -0.05017(17) 0.7499(4) 0.0261(11) Uiso 0.573(6) 1 d PD A 1
N1A N -0.1732(7) -0.02841(19) 0.7095(4) 0.0225(14) Uiso 0.427(6) 1 d PD A 2
O1A O -0.1338(6) 0.02489(17) 0.7163(4) 0.0200(11) Uiso 0.427(6) 1 d PD A 2
O2A O -0.0371(7) -0.0558(2) 0.7808(5) 0.0213(13) Uiso 0.427(6) 1 d PD A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N3 1.468(3) . ?
C1 C2 1.510(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.513(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N4 1.491(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.492(3) . ?
C4 C5 1.510(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.510(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N5 1.470(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 N4 1.476(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C11 N13 1.465(3) . ?
C11 C12 1.504(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.513(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N14 1.490(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C17 N14 1.475(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
N2 O3 1.253(3) . ?
N2 O4 1.267(3) . ?
N3 Ni1 2.071(2) . ?
N3 H3C 0.9200 . ?
N3 H3D 0.9200 . ?
N4 Ni1 2.1112(18) . ?
N5 Ni1 2.0585(19) . ?
N5 H5C 0.9200 . ?
N5 H5D 0.9200 . ?
N11 O11 1.236(2) 4_565 ?
N11 O11 1.236(2) . ?
N11 Ni2 2.118(3) . ?
N12 O13 1.258(4) . ?
N12 O14 1.261(4) . ?
N13 Ni2 2.0653(19) . ?
N13 H13C 0.9200 . ?
N13 H13D 0.9200 . ?
N14 C13 1.490(3) 4_565 ?
N14 Ni2 2.104(3) . ?
O3 Ni1 2.1597(18) . ?
O4 Ni1 2.1706(18) . ?
O13 Ni2 2.210(2) . ?
O14 Ni2 2.095(2) . ?
Ni1 O1A 2.051(4) . ?
Ni1 N1 2.054(3) . ?
Ni2 N13 2.0653(19) 4_565 ?
N1 O1 1.230(5) . ?
N1 O2 1.268(5) . ?
N1A O2A 1.268(6) . ?
N1A O1A 1.299(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 C1 C2 111.32(19) . . ?
N3 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N3 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
C1 C2 C3 114.43(19) . . ?
C1 C2 H2A 108.7 . . ?
C3 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
C3 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
N4 C3 C2 117.07(19) . . ?
N4 C3 H3A 108.0 . . ?
C2 C3 H3A 108.0 . . ?
N4 C3 H3B 108.0 . . ?
C2 C3 H3B 108.0 . . ?
H3A C3 H3B 107.3 . . ?
N4 C4 C5 117.04(18) . . ?
N4 C4 H4A 108.0 . . ?
C5 C4 H4A 108.0 . . ?
N4 C4 H4B 108.0 . . ?
C5 C4 H4B 108.0 . . ?
H4A C4 H4B 107.3 . . ?
C4 C5 C6 114.58(19) . . ?
C4 C5 H5A 108.6 . . ?
C6 C5 H5A 108.6 . . ?
C4 C5 H5B 108.6 . . ?
C6 C5 H5B 108.6 . . ?
H5A C5 H5B 107.6 . . ?
N5 C6 C5 111.37(18) . . ?
N5 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
N5 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N13 C11 C12 110.30(19) . . ?
N13 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
N13 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
C11 C12 C13 114.89(19) . . ?
C11 C12 H12A 108.5 . . ?
C13 C12 H12A 108.5 . . ?
C11 C12 H12B 108.5 . . ?
C13 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?
N14 C13 C12 117.54(19) . . ?
N14 C13 H13A 107.9 . . ?
C12 C13 H13A 107.9 . . ?
N14 C13 H13B 107.9 . . ?
C12 C13 H13B 107.9 . . ?
H13A C13 H13B 107.2 . . ?
N14 C17 H17A 109.5 . . ?
N14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O3 N2 O4 112.27(19) . . ?
C1 N3 Ni1 119.73(14) . . ?
C1 N3 H3C 107.4 . . ?
Ni1 N3 H3C 107.4 . . ?
C1 N3 H3D 107.4 . . ?
Ni1 N3 H3D 107.4 . . ?
H3C N3 H3D 106.9 . . ?
C7 N4 C3 108.92(17) . . ?
C7 N4 C4 108.84(18) . . ?
C3 N4 C4 105.10(16) . . ?
C7 N4 Ni1 106.53(13) . . ?
C3 N4 Ni1 113.51(14) . . ?
C4 N4 Ni1 113.84(13) . . ?
C6 N5 Ni1 118.97(14) . . ?
C6 N5 H5C 107.6 . . ?
Ni1 N5 H5C 107.6 . . ?
C6 N5 H5D 107.6 . . ?
Ni1 N5 H5D 107.6 . . ?
H5C N5 H5D 107.0 . . ?
O11 N11 O11 116.4(3) 4_565 . ?
O11 N11 Ni2 121.79(13) 4_565 . ?
O11 N11 Ni2 121.79(13) . . ?
O13 N12 O14 112.6(3) . . ?
C11 N13 Ni2 119.62(15) . . ?
C11 N13 H13C 107.4 . . ?
Ni2 N13 H13C 107.4 . . ?
C11 N13 H13D 107.4 . . ?
Ni2 N13 H13D 107.4 . . ?
H13C N13 H13D 106.9 . . ?
C17 N14 C13 109.35(15) . 4_565 ?
C17 N14 C13 109.35(15) . . ?
C13 N14 C13 104.6(2) 4_565 . ?
C17 N14 Ni2 111.27(18) . . ?
C13 N14 Ni2 111.01(13) 4_565 . ?
C13 N14 Ni2 111.01(13) . . ?
N2 O3 Ni1 95.43(13) . . ?
N2 O4 Ni1 94.49(13) . . ?
N12 O13 Ni2 91.91(17) . . ?
N12 O14 Ni2 97.3(2) . . ?
O1A Ni1 N1 18.88(12) . . ?
O1A Ni1 N5 88.67(12) . . ?
N1 Ni1 N5 95.48(11) . . ?
O1A Ni1 N3 96.41(13) . . ?
N1 Ni1 N3 86.96(11) . . ?
N5 Ni1 N3 170.31(7) . . ?
O1A Ni1 N4 85.70(13) . . ?
N1 Ni1 N4 102.81(12) . . ?
N5 Ni1 N4 93.47(7) . . ?
N3 Ni1 N4 95.13(7) . . ?
O1A Ni1 O3 115.34(13) . . ?
N1 Ni1 O3 98.09(11) . . ?
N5 Ni1 O3 86.91(7) . . ?
N3 Ni1 O3 83.47(7) . . ?
N4 Ni1 O3 158.96(7) . . ?
O1A Ni1 O4 171.29(11) . . ?
N1 Ni1 O4 155.84(11) . . ?
N5 Ni1 O4 85.63(8) . . ?
N3 Ni1 O4 88.32(8) . . ?
N4 Ni1 O4 101.21(7) . . ?
O3 Ni1 O4 57.81(7) . . ?
N13 Ni2 N13 169.01(10) 4_565 . ?
N13 Ni2 O14 92.52(6) 4_565 . ?
N13 Ni2 O14 92.52(6) . . ?
N13 Ni2 N14 94.65(5) 4_565 . ?
N13 Ni2 N14 94.65(5) . . ?
O14 Ni2 N14 94.97(10) . . ?
N13 Ni2 N11 86.31(6) 4_565 . ?
N13 Ni2 N11 86.31(6) . . ?
O14 Ni2 N11 165.09(9) . . ?
N14 Ni2 N11 99.94(10) . . ?
N13 Ni2 O13 87.18(5) 4_565 . ?
N13 Ni2 O13 87.18(5) . . ?
O14 Ni2 O13 58.19(10) . . ?
N14 Ni2 O13 153.16(10) . . ?
N11 Ni2 O13 106.90(10) . . ?
O1 N1 O2 116.2(4) . . ?
O1 N1 Ni1 122.9(3) . . ?
O2 N1 Ni1 120.9(3) . . ?
O2A N1A O1A 110.3(5) . . ?
N1A O1A Ni1 125.2(4) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 C1 C2 C3 -69.7(3) . . . . ?
C1 C2 C3 N4 72.5(3) . . . . ?
N4 C4 C5 C6 -69.3(3) . . . . ?
C4 C5 C6 N5 68.3(2) . . . . ?
N13 C11 C12 C13 67.7(3) . . . . ?
C11 C12 C13 N14 -73.2(3) . . . . ?
C2 C1 N3 Ni1 53.3(2) . . . . ?
C2 C3 N4 C7 66.9(3) . . . . ?
C2 C3 N4 C4 -176.6(2) . . . . ?
C2 C3 N4 Ni1 -51.6(2) . . . . ?
C5 C4 N4 C7 -65.4(2) . . . . ?
C5 C4 N4 C3 178.0(2) . . . . ?
C5 C4 N4 Ni1 53.2(2) . . . . ?
C5 C6 N5 Ni1 -57.7(2) . . . . ?
C12 C11 N13 Ni2 -55.2(2) . . . . ?
C12 C13 N14 C17 -67.3(3) . . . . ?
C12 C13 N14 C13 175.63(12) . . . 4_565 ?
C12 C13 N14 Ni2 55.8(2) . . . . ?
O4 N2 O3 Ni1 0.08(18) . . . . ?
O3 N2 O4 Ni1 -0.07(17) . . . . ?
O14 N12 O13 Ni2 0.000(2) . . . . ?
O13 N12 O14 Ni2 0.000(2) . . . . ?
C6 N5 Ni1 O1A -46.41(19) . . . . ?
C6 N5 Ni1 N1 -64.03(19) . . . . ?
C6 N5 Ni1 N3 -168.3(4) . . . . ?
C6 N5 Ni1 N4 39.20(16) . . . . ?
C6 N5 Ni1 O3 -161.87(16) . . . . ?
C6 N5 Ni1 O4 140.20(16) . . . . ?
C1 N3 Ni1 O1A 53.1(2) . . . . ?
C1 N3 Ni1 N1 69.51(19) . . . . ?
C1 N3 Ni1 N5 174.4(4) . . . . ?
C1 N3 Ni1 N4 -33.09(18) . . . . ?
C1 N3 Ni1 O3 168.02(18) . . . . ?
C1 N3 Ni1 O4 -134.20(17) . . . . ?
C7 N4 Ni1 O1A 173.82(17) . . . . ?
C3 N4 Ni1 O1A -66.32(18) . . . . ?
C4 N4 Ni1 O1A 53.87(18) . . . . ?
C7 N4 Ni1 N1 -178.16(15) . . . . ?
C3 N4 Ni1 N1 -58.30(17) . . . . ?
C4 N4 Ni1 N1 61.89(18) . . . . ?
C7 N4 Ni1 N5 85.42(15) . . . . ?
C3 N4 Ni1 N5 -154.72(15) . . . . ?
C4 N4 Ni1 N5 -34.53(15) . . . . ?
C7 N4 Ni1 N3 -90.12(15) . . . . ?
C3 N4 Ni1 N3 29.74(15) . . . . ?
C4 N4 Ni1 N3 149.93(15) . . . . ?
C7 N4 Ni1 O3 -5.0(3) . . . . ?
C3 N4 Ni1 O3 114.9(2) . . . . ?
C4 N4 Ni1 O3 -124.94(19) . . . . ?
C7 N4 Ni1 O4 -0.81(14) . . . . ?
C3 N4 Ni1 O4 119.05(15) . . . . ?
C4 N4 Ni1 O4 -120.77(15) . . . . ?
N2 O3 Ni1 O1A -173.90(16) . . . . ?
N2 O3 Ni1 N1 178.07(15) . . . . ?
N2 O3 Ni1 N5 -86.83(13) . . . . ?
N2 O3 Ni1 N3 92.09(14) . . . . ?
N2 O3 Ni1 N4 4.8(2) . . . . ?
N2 O3 Ni1 O4 -0.05(11) . . . . ?
N2 O4 Ni1 O1A 39.8(8) . . . . ?
N2 O4 Ni1 N1 -4.5(3) . . . . ?
N2 O4 Ni1 N5 89.14(13) . . . . ?
N2 O4 Ni1 N3 -83.29(13) . . . . ?
N2 O4 Ni1 N4 -178.18(12) . . . . ?
N2 O4 Ni1 O3 0.05(11) . . . . ?
C11 N13 Ni2 N13 -173.9(5) . . . 4_565 ?
C11 N13 Ni2 O14 -56.67(17) . . . . ?
C11 N13 Ni2 N14 38.52(18) . . . . ?
C11 N13 Ni2 N11 138.22(17) . . . . ?
C11 N13 Ni2 O13 -114.64(18) . . . . ?
N12 O14 Ni2 N13 85.11(5) . . . 4_565 ?
N12 O14 Ni2 N13 -85.11(5) . . . . ?
N12 O14 Ni2 N14 180.000(1) . . . . ?
N12 O14 Ni2 N11 0.000(2) . . . . ?
N12 O14 Ni2 O13 0.000(1) . . . . ?
C17 N14 Ni2 N13 -87.06(6) . . . 4_565 ?
C13 N14 Ni2 N13 34.98(16) 4_565 . . 4_565 ?
C13 N14 Ni2 N13 150.90(15) . . . 4_565 ?
C17 N14 Ni2 N13 87.06(6) . . . . ?
C13 N14 Ni2 N13 -150.90(15) 4_565 . . . ?
C13 N14 Ni2 N13 -34.98(16) . . . . ?
C17 N14 Ni2 O14 180.000(1) . . . . ?
C13 N14 Ni2 O14 -57.96(15) 4_565 . . . ?
C13 N14 Ni2 O14 57.96(15) . . . . ?
C17 N14 Ni2 N11 0.000(1) . . . . ?
C13 N14 Ni2 N11 122.04(15) 4_565 . . . ?
C13 N14 Ni2 N11 -122.04(15) . . . . ?
C17 N14 Ni2 O13 180.000(2) . . . . ?
C13 N14 Ni2 O13 -57.96(15) 4_565 . . . ?
C13 N14 Ni2 O13 57.96(15) . . . . ?
O11 N11 Ni2 N13 -175.2(2) 4_565 . . 4_565 ?
O11 N11 Ni2 N13 3.3(2) . . . 4_565 ?
O11 N11 Ni2 N13 -3.3(2) 4_565 . . . ?
O11 N11 Ni2 N13 175.2(2) . . . . ?
O11 N11 Ni2 O14 -89.2(2) 4_565 . . . ?
O11 N11 Ni2 O14 89.2(2) . . . . ?
O11 N11 Ni2 N14 90.8(2) 4_565 . . . ?
O11 N11 Ni2 N14 -90.8(2) . . . . ?
O11 N11 Ni2 O13 -89.2(2) 4_565 . . . ?
O11 N11 Ni2 O13 89.2(2) . . . . ?
N12 O13 Ni2 N13 -94.72(5) . . . 4_565 ?
N12 O13 Ni2 N13 94.72(5) . . . . ?
N12 O13 Ni2 O14 0.000(2) . . . . ?
N12 O13 Ni2 N14 0.000(2) . . . . ?
N12 O13 Ni2 N11 180.000(2) . . . . ?
O1A Ni1 N1 O1 -12.9(4) . . . . ?
N5 Ni1 N1 O1 56.5(3) . . . . ?
N3 Ni1 N1 O1 -132.9(3) . . . . ?
N4 Ni1 N1 O1 -38.4(3) . . . . ?
O3 Ni1 N1 O1 144.1(3) . . . . ?
O4 Ni1 N1 O1 148.0(2) . . . . ?
O1A Ni1 N1 O2 165.4(7) . . . . ?
N5 Ni1 N1 O2 -125.2(3) . . . . ?
N3 Ni1 N1 O2 45.4(3) . . . . ?
N4 Ni1 N1 O2 140.0(3) . . . . ?
O3 Ni1 N1 O2 -37.6(3) . . . . ?
O4 Ni1 N1 O2 -33.7(5) . . . . ?
O2A N1A O1A Ni1 -2.4(6) . . . . ?
N1 Ni1 O1A N1A 0.2(4) . . . . ?
N5 Ni1 O1A N1A -111.1(4) . . . . ?
N3 Ni1 O1A N1A 60.6(4) . . . . ?
N4 Ni1 O1A N1A 155.3(4) . . . . ?
O3 Ni1 O1A N1A -25.2(4) . . . . ?
O4 Ni1 O1A N1A -61.9(10) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3D O2A 0.92 2.61 3.098(6) 114.0 .
N5 H5C O3 0.92 2.19 3.022(3) 150.4 3_557
N5 H5C O2A 0.92 2.54 3.161(6) 125.5 3_557
N5 H5D O11 0.92 2.22 3.081(3) 156.4 4_565
N13 H13D O11 0.92 2.17 2.824(3) 127.6 4_565

_diffrn_measured_fraction_theta_max 0.900
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.089

_database_code_depnum_ccdc_archive 'CCDC 994157'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex7_130K
_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;
Dinitro-(3,3-diamino-N-methyldipropylamine)nickel(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H19 N5 Ni O4'
_chemical_formula_sum            'C7 H19 N5 Ni O4'
_chemical_formula_weight         295.98


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'
O O 0.0106 0.0060 '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'


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

_cell_length_a                   7.102(5)
_cell_length_b                   23.707(5)
_cell_length_c                   10.910(5)
_cell_angle_alpha                90.000
_cell_angle_beta                 103.541(5)
_cell_angle_gamma                90.000
_cell_volume                     1785.8(15)
_cell_formula_units_Z            6
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    4367
_cell_measurement_theta_min      3.0510
_cell_measurement_theta_max      29.3664

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/m

_exptl_crystal_description       Block
_exptl_crystal_colour            Violet
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936

_exptl_absorpt_coefficient_mu    1.643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.77444
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12180
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.24
_diffrn_reflns_theta_max         29.23
_reflns_number_total             4482
_reflns_number_gt                3684
_reflns_threshold_expression     >2sigma(I)


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'POV-RAY for Windows, 3.62 (Cason, 2009)'
_computing_publication_material  'WinGX, 1.80.05 (Farrugia, 1999)'


_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 > 2sigma(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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0586P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4482
_refine_ls_number_parameters     256
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0352
_refine_ls_wR_factor_ref         0.0931
_refine_ls_wR_factor_gt          0.0896
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2835(3) 0.01892(10) 0.61667(19) 0.0173(4) Uani 1 1 d . . .
H1A H 0.1645 -0.0024 0.5778 0.021 Uiso 1 1 calc R . .
H1B H 0.3945 -0.0003 0.5942 0.021 Uiso 1 1 calc R . .
C2 C 0.2672(3) 0.07829(10) 0.5650(2) 0.0205(5) Uani 1 1 d . . .
H2A H 0.3784 0.1005 0.6127 0.025 Uiso 1 1 calc R . .
H2B H 0.2770 0.0769 0.4760 0.025 Uiso 1 1 calc R . .
C3 C 0.0825(3) 0.10853(10) 0.5710(2) 0.0196(5) Uani 1 1 d . . .
H3A H 0.0727 0.1428 0.5181 0.024 Uiso 1 1 calc R . .
H3B H -0.0277 0.0838 0.5321 0.024 Uiso 1 1 calc R . .
C4 C -0.1394(3) 0.15068(10) 0.6745(2) 0.0185(4) Uani 1 1 d . . .
H4A H -0.2328 0.1222 0.6299 0.022 Uiso 1 1 calc R . .
H4B H -0.1445 0.1832 0.6168 0.022 Uiso 1 1 calc R . .
C5 C -0.2073(3) 0.17057(10) 0.7889(2) 0.0201(5) Uani 1 1 d . . .
H5A H -0.1075 0.1959 0.8391 0.024 Uiso 1 1 calc R . .
H5B H -0.3272 0.1930 0.7600 0.024 Uiso 1 1 calc R . .
C6 C -0.2467(3) 0.12381(10) 0.8728(2) 0.0195(5) Uani 1 1 d . . .
H6A H -0.3118 0.1395 0.9362 0.023 Uiso 1 1 calc R . .
H6B H -0.3350 0.0959 0.8214 0.023 Uiso 1 1 calc R . .
C7 C 0.2022(3) 0.16971(9) 0.7489(2) 0.0189(4) Uani 1 1 d . . .
H7A H 0.3329 0.1540 0.7616 0.028 Uiso 1 1 calc R . .
H7B H 0.1816 0.1832 0.8297 0.028 Uiso 1 1 calc R . .
H7C H 0.1876 0.2012 0.6893 0.028 Uiso 1 1 calc R . .
C11 C 0.5314(3) 0.12752(10) 1.3183(2) 0.0182(4) Uani 1 1 d . . .
H11A H 0.4938 0.0874 1.3047 0.022 Uiso 1 1 calc R . .
H11B H 0.5908 0.1330 1.4091 0.022 Uiso 1 1 calc R . .
C12 C 0.6762(3) 0.14223(10) 1.2422(2) 0.0208(5) Uani 1 1 d . . .
H12A H 0.6113 0.1399 1.1516 0.025 Uiso 1 1 calc R . .
H12B H 0.7809 0.1137 1.2592 0.025 Uiso 1 1 calc R . .
C13 C 0.7663(3) 0.20010(10) 1.2686(2) 0.0182(4) Uani 1 1 d . . .
H13A H 0.8111 0.2044 1.3611 0.022 Uiso 1 1 calc R . .
H13B H 0.8826 0.2013 1.2333 0.022 Uiso 1 1 calc R . .
C17 C 0.6014(5) 0.2500 1.0806(3) 0.0210(7) Uani 1 2 d S . .
H17A H 0.7212 0.2430 1.0531 0.032 Uiso 0.50 1 calc PR . .
H17B H 0.5480 0.2867 1.0487 0.032 Uiso 0.50 1 calc PR . .
H17C H 0.5071 0.2203 1.0477 0.032 Uiso 0.50 1 calc PR . .
N2 N 0.3635(3) 0.05077(9) 1.04541(18) 0.0209(4) Uani 1 1 d . . .
N3 N 0.3107(3) 0.01897(8) 0.75487(16) 0.0154(4) Uani 1 1 d . A .
H3C H 0.4297 0.0348 0.7890 0.018 Uiso 1 1 calc R . .
H3D H 0.3163 -0.0180 0.7811 0.018 Uiso 1 1 calc R . .
N4 N 0.0585(3) 0.12574(7) 0.69816(16) 0.0131(3) Uani 1 1 d . A .
N5 N -0.0670(3) 0.09560(8) 0.93740(17) 0.0156(4) Uani 1 1 d . A .
H5C H -0.0998 0.0676 0.9870 0.019 Uiso 1 1 calc R . .
H5D H 0.0063 0.1215 0.9909 0.019 Uiso 1 1 calc R . .
N11 N 0.1793(3) 0.2500 1.1112(2) 0.0138(5) Uani 1 2 d S . .
N12 N 0.3814(5) 0.2500 1.5203(3) 0.0292(7) Uani 1 2 d S . .
N13 N 0.3588(3) 0.16334(8) 1.28079(19) 0.0188(4) Uani 1 1 d . . .
H13C H 0.2768 0.1541 1.3317 0.023 Uiso 1 1 calc R . .
H13D H 0.2970 0.1534 1.1998 0.023 Uiso 1 1 calc R . .
N14 N 0.6435(3) 0.2500 1.2194(2) 0.0122(5) Uani 1 2 d S . .
O3 O 0.2424(2) 0.01323(7) 0.99869(15) 0.0194(3) Uani 1 1 d . A .
O4 O 0.3473(2) 0.09405(7) 0.97657(14) 0.0185(3) Uani 1 1 d . A .
O11 O 0.1134(3) 0.29446(8) 1.05839(17) 0.0317(4) Uani 1 1 d . . .
O13 O 0.2277(3) 0.2500 1.4360(2) 0.0268(5) Uani 1 2 d S . .
O14 O 0.5310(3) 0.2500 1.4758(2) 0.0227(5) Uani 1 2 d S . .
Ni1 Ni 0.10868(4) 0.059876(11) 0.83272(2) 0.01121(9) Uani 1 1 d . . .
Ni2 Ni 0.38781(5) 0.2500 1.28500(3) 0.01083(10) Uani 1 2 d S . .
N1 N -0.0926(3) 0.00151(11) 0.7464(2) 0.0165(5) Uani 0.922(6) 1 d PD A 1
O1 O -0.2559(3) 0.01378(8) 0.68384(18) 0.0244(6) Uani 0.922(6) 1 d PD A 1
O2 O -0.0487(5) -0.04926(14) 0.7590(4) 0.0244(7) Uani 0.922(6) 1 d PD A 1
N1A N -0.182(4) -0.0311(8) 0.710(2) 0.021(7) Uiso 0.078(6) 1 d PD A 2
O1A O -0.137(4) 0.0223(8) 0.716(2) 0.014(6) Uiso 0.078(6) 1 d PD A 2
O2A O -0.037(5) -0.0609(16) 0.771(4) 0.015(9) Uiso 0.078(6) 1 d PD A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N3 1.475(3) . ?
C1 C2 1.510(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.509(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N4 1.494(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.491(3) . ?
C4 C5 1.515(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.505(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N5 1.467(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 N4 1.473(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C11 N13 1.469(3) . ?
C11 C12 1.506(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.513(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N14 1.493(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C17 N14 1.473(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
N2 O3 1.260(3) . ?
N2 O4 1.261(3) . ?
N3 Ni1 2.0712(19) . ?
N3 H3C 0.9200 . ?
N3 H3D 0.9200 . ?
N4 Ni1 2.1154(18) . ?
N5 Ni1 2.0606(19) . ?
N5 H5C 0.9200 . ?
N5 H5D 0.9200 . ?
N11 O11 1.239(2) 4_565 ?
N11 O11 1.239(2) . ?
N11 Ni2 2.115(3) . ?
N12 O13 1.252(4) . ?
N12 O14 1.268(4) . ?
N13 Ni2 2.0643(19) . ?
N13 H13C 0.9200 . ?
N13 H13D 0.9200 . ?
N14 C13 1.493(3) 4_565 ?
N14 Ni2 2.102(3) . ?
O3 Ni1 2.1443(17) . ?
O4 Ni1 2.1784(18) . ?
O13 Ni2 2.210(2) . ?
O14 Ni2 2.092(2) . ?
Ni1 N1 2.053(2) . ?
Ni1 O1A 2.10(2) . ?
Ni2 N13 2.0643(19) 4_565 ?
N1 O1 1.235(3) . ?
N1 O2 1.243(4) . ?
N1A O2A 1.298(10) . ?
N1A O1A 1.304(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 C1 C2 111.16(18) . . ?
N3 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N3 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
C3 C2 C1 114.70(19) . . ?
C3 C2 H2A 108.6 . . ?
C1 C2 H2A 108.6 . . ?
C3 C2 H2B 108.6 . . ?
C1 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
N4 C3 C2 117.32(18) . . ?
N4 C3 H3A 108.0 . . ?
C2 C3 H3A 108.0 . . ?
N4 C3 H3B 108.0 . . ?
C2 C3 H3B 108.0 . . ?
H3A C3 H3B 107.2 . . ?
N4 C4 C5 116.74(18) . . ?
N4 C4 H4A 108.1 . . ?
C5 C4 H4A 108.1 . . ?
N4 C4 H4B 108.1 . . ?
C5 C4 H4B 108.1 . . ?
H4A C4 H4B 107.3 . . ?
C6 C5 C4 114.35(19) . . ?
C6 C5 H5A 108.7 . . ?
C4 C5 H5A 108.7 . . ?
C6 C5 H5B 108.7 . . ?
C4 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
N5 C6 C5 111.30(18) . . ?
N5 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
N5 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N13 C11 C12 110.25(18) . . ?
N13 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
N13 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
C11 C12 C13 114.73(19) . . ?
C11 C12 H12A 108.6 . . ?
C13 C12 H12A 108.6 . . ?
C11 C12 H12B 108.6 . . ?
C13 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
N14 C13 C12 117.71(19) . . ?
N14 C13 H13A 107.9 . . ?
C12 C13 H13A 107.9 . . ?
N14 C13 H13B 107.9 . . ?
C12 C13 H13B 107.9 . . ?
H13A C13 H13B 107.2 . . ?
N14 C17 H17A 109.5 . . ?
N14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O3 N2 O4 112.05(18) . . ?
C1 N3 Ni1 118.83(13) . . ?
C1 N3 H3C 107.6 . . ?
Ni1 N3 H3C 107.6 . . ?
C1 N3 H3D 107.6 . . ?
Ni1 N3 H3D 107.6 . . ?
H3C N3 H3D 107.0 . . ?
C7 N4 C4 109.05(17) . . ?
C7 N4 C3 108.83(17) . . ?
C4 N4 C3 104.81(16) . . ?
C7 N4 Ni1 105.78(13) . . ?
C4 N4 Ni1 114.33(13) . . ?
C3 N4 Ni1 113.93(13) . . ?
C6 N5 Ni1 119.52(14) . . ?
C6 N5 H5C 107.4 . . ?
Ni1 N5 H5C 107.4 . . ?
C6 N5 H5D 107.4 . . ?
Ni1 N5 H5D 107.4 . . ?
H5C N5 H5D 107.0 . . ?
O11 N11 O11 116.6(3) 4_565 . ?
O11 N11 Ni2 121.71(14) 4_565 . ?
O11 N11 Ni2 121.71(14) . . ?
O13 N12 O14 112.6(3) . . ?
C11 N13 Ni2 119.78(14) . . ?
C11 N13 H13C 107.4 . . ?
Ni2 N13 H13C 107.4 . . ?
C11 N13 H13D 107.4 . . ?
Ni2 N13 H13D 107.4 . . ?
H13C N13 H13D 106.9 . . ?
C17 N14 C13 109.29(15) . 4_565 ?
C17 N14 C13 109.29(15) . . ?
C13 N14 C13 104.8(2) 4_565 . ?
C17 N14 Ni2 111.50(18) . . ?
C13 N14 Ni2 110.86(13) 4_565 . ?
C13 N14 Ni2 110.86(13) . . ?
N2 O3 Ni1 95.89(13) . . ?
N2 O4 Ni1 94.22(13) . . ?
N12 O13 Ni2 92.01(18) . . ?
N12 O14 Ni2 97.2(2) . . ?
N1 Ni1 N5 94.83(9) . . ?
N1 Ni1 N3 88.35(9) . . ?
N5 Ni1 N3 170.80(7) . . ?
N1 Ni1 O1A 17.5(6) . . ?
N5 Ni1 O1A 89.1(6) . . ?
N3 Ni1 O1A 96.3(6) . . ?
N1 Ni1 N4 101.13(9) . . ?
N5 Ni1 N4 93.19(7) . . ?
N3 Ni1 N4 94.67(7) . . ?
O1A Ni1 N4 85.0(6) . . ?
N1 Ni1 O3 99.37(9) . . ?
N5 Ni1 O3 87.12(7) . . ?
N3 Ni1 O3 83.83(7) . . ?
O1A Ni1 O3 115.6(6) . . ?
N4 Ni1 O3 159.40(7) . . ?
N1 Ni1 O4 157.19(9) . . ?
N5 Ni1 O4 85.28(8) . . ?
N3 Ni1 O4 88.45(8) . . ?
O1A Ni1 O4 171.5(6) . . ?
N4 Ni1 O4 101.64(7) . . ?
O3 Ni1 O4 57.83(6) . . ?
N13 Ni2 N13 168.85(10) . 4_565 ?
N13 Ni2 O14 92.57(6) . . ?
N13 Ni2 O14 92.57(6) 4_565 . ?
N13 Ni2 N14 94.71(5) . . ?
N13 Ni2 N14 94.71(5) 4_565 . ?
O14 Ni2 N14 94.66(10) . . ?
N13 Ni2 N11 86.26(6) . . ?
N13 Ni2 N11 86.26(6) 4_565 . ?
O14 Ni2 N11 165.31(9) . . ?
N14 Ni2 N11 100.03(10) . . ?
N13 Ni2 O13 87.16(5) . . ?
N13 Ni2 O13 87.16(5) 4_565 . ?
O14 Ni2 O13 58.23(10) . . ?
N14 Ni2 O13 152.89(10) . . ?
N11 Ni2 O13 107.08(10) . . ?
O1 N1 O2 117.9(3) . . ?
O1 N1 Ni1 123.9(2) . . ?
O2 N1 Ni1 118.2(2) . . ?
O2A N1A O1A 110(3) . . ?
N1A O1A Ni1 127(2) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 C1 C2 C3 -70.1(3) . . . . ?
C1 C2 C3 N4 70.6(3) . . . . ?
N4 C4 C5 C6 -69.8(3) . . . . ?
C4 C5 C6 N5 69.0(2) . . . . ?
N13 C11 C12 C13 67.4(3) . . . . ?
C11 C12 C13 N14 -73.4(3) . . . . ?
C2 C1 N3 Ni1 56.0(2) . . . . ?
C5 C4 N4 C7 -65.4(2) . . . . ?
C5 C4 N4 C3 178.17(19) . . . . ?
C5 C4 N4 Ni1 52.7(2) . . . . ?
C2 C3 N4 C7 67.0(3) . . . . ?
C2 C3 N4 C4 -176.4(2) . . . . ?
C2 C3 N4 Ni1 -50.7(2) . . . . ?
C5 C6 N5 Ni1 -57.4(2) . . . . ?
C12 C11 N13 Ni2 -54.9(2) . . . . ?
C12 C13 N14 C17 -67.2(3) . . . . ?
C12 C13 N14 C13 175.77(12) . . . 4_565 ?
C12 C13 N14 Ni2 56.1(2) . . . . ?
O4 N2 O3 Ni1 0.07(17) . . . . ?
O3 N2 O4 Ni1 -0.07(17) . . . . ?
O14 N12 O13 Ni2 0.000(2) . . . . ?
O13 N12 O14 Ni2 0.000(2) . . . . ?
C6 N5 Ni1 N1 -63.37(18) . . . . ?
C6 N5 Ni1 N3 -173.3(4) . . . . ?
C6 N5 Ni1 O1A -46.8(6) . . . . ?
C6 N5 Ni1 N4 38.09(17) . . . . ?
C6 N5 Ni1 O3 -162.54(16) . . . . ?
C6 N5 Ni1 O4 139.52(16) . . . . ?
C1 N3 Ni1 N1 65.29(17) . . . . ?
C1 N3 Ni1 N5 175.7(4) . . . . ?
C1 N3 Ni1 O1A 49.7(6) . . . . ?
C1 N3 Ni1 N4 -35.75(16) . . . . ?
C1 N3 Ni1 O3 164.89(16) . . . . ?
C1 N3 Ni1 O4 -137.30(16) . . . . ?
C7 N4 Ni1 N1 -177.92(13) . . . . ?
C4 N4 Ni1 N1 62.08(16) . . . . ?
C3 N4 Ni1 N1 -58.42(16) . . . . ?
C7 N4 Ni1 N5 86.52(14) . . . . ?
C4 N4 Ni1 N5 -33.48(15) . . . . ?
C3 N4 Ni1 N5 -153.98(15) . . . . ?
C7 N4 Ni1 N3 -88.69(14) . . . . ?
C4 N4 Ni1 N3 151.31(15) . . . . ?
C3 N4 Ni1 N3 30.81(15) . . . . ?
C7 N4 Ni1 O1A 175.3(6) . . . . ?
C4 N4 Ni1 O1A 55.3(6) . . . . ?
C3 N4 Ni1 O1A -65.2(6) . . . . ?
C7 N4 Ni1 O3 -3.8(3) . . . . ?
C4 N4 Ni1 O3 -123.79(19) . . . . ?
C3 N4 Ni1 O3 115.7(2) . . . . ?
C7 N4 Ni1 O4 0.69(14) . . . . ?
C4 N4 Ni1 O4 -119.31(14) . . . . ?
C3 N4 Ni1 O4 120.19(15) . . . . ?
N2 O3 Ni1 N1 179.31(13) . . . . ?
N2 O3 Ni1 N5 -86.27(13) . . . . ?
N2 O3 Ni1 N3 92.01(13) . . . . ?
N2 O3 Ni1 O1A -173.9(7) . . . . ?
N2 O3 Ni1 N4 5.1(2) . . . . ?
N2 O3 Ni1 O4 -0.04(11) . . . . ?
N2 O4 Ni1 N1 -1.6(2) . . . . ?
N2 O4 Ni1 N5 89.61(12) . . . . ?
N2 O4 Ni1 N3 -83.65(12) . . . . ?
N2 O4 Ni1 O1A 41(4) . . . . ?
N2 O4 Ni1 N4 -178.10(12) . . . . ?
N2 O4 Ni1 O3 0.04(11) . . . . ?
C11 N13 Ni2 N13 -173.9(5) . . . 4_565 ?
C11 N13 Ni2 O14 -56.45(17) . . . . ?
C11 N13 Ni2 N14 38.44(18) . . . . ?
C11 N13 Ni2 N11 138.21(17) . . . . ?
C11 N13 Ni2 O13 -114.45(17) . . . . ?
N12 O14 Ni2 N13 -85.06(5) . . . . ?
N12 O14 Ni2 N13 85.06(5) . . . 4_565 ?
N12 O14 Ni2 N14 180.000(2) . . . . ?
N12 O14 Ni2 N11 0.000(2) . . . . ?
N12 O14 Ni2 O13 0.000(1) . . . . ?
C17 N14 Ni2 N13 87.02(6) . . . . ?
C13 N14 Ni2 N13 -150.97(15) 4_565 . . . ?
C13 N14 Ni2 N13 -34.98(16) . . . . ?
C17 N14 Ni2 N13 -87.02(6) . . . 4_565 ?
C13 N14 Ni2 N13 34.98(16) 4_565 . . 4_565 ?
C13 N14 Ni2 N13 150.97(15) . . . 4_565 ?
C17 N14 Ni2 O14 180.000(1) . . . . ?
C13 N14 Ni2 O14 -57.99(14) 4_565 . . . ?
C13 N14 Ni2 O14 57.99(15) . . . . ?
C17 N14 Ni2 N11 0.000(1) . . . . ?
C13 N14 Ni2 N11 122.01(14) 4_565 . . . ?
C13 N14 Ni2 N11 -122.01(15) . . . . ?
C17 N14 Ni2 O13 180.000(2) . . . . ?
C13 N14 Ni2 O13 -57.99(14) 4_565 . . . ?
C13 N14 Ni2 O13 57.99(15) . . . . ?
O11 N11 Ni2 N13 -3.3(2) 4_565 . . . ?
O11 N11 Ni2 N13 175.0(2) . . . . ?
O11 N11 Ni2 N13 -175.0(2) 4_565 . . 4_565 ?
O11 N11 Ni2 N13 3.3(2) . . . 4_565 ?
O11 N11 Ni2 O14 -89.2(2) 4_565 . . . ?
O11 N11 Ni2 O14 89.2(2) . . . . ?
O11 N11 Ni2 N14 90.8(2) 4_565 . . . ?
O11 N11 Ni2 N14 -90.8(2) . . . . ?
O11 N11 Ni2 O13 -89.2(2) 4_565 . . . ?
O11 N11 Ni2 O13 89.2(2) . . . . ?
N12 O13 Ni2 N13 94.80(5) . . . . ?
N12 O13 Ni2 N13 -94.80(5) . . . 4_565 ?
N12 O13 Ni2 O14 0.000(2) . . . . ?
N12 O13 Ni2 N14 0.000(2) . . . . ?
N12 O13 Ni2 N11 180.000(2) . . . . ?
N5 Ni1 N1 O1 57.1(2) . . . . ?
N3 Ni1 N1 O1 -131.58(19) . . . . ?
O1A Ni1 N1 O1 -14(2) . . . . ?
N4 Ni1 N1 O1 -37.14(19) . . . . ?
O3 Ni1 N1 O1 144.95(18) . . . . ?
O4 Ni1 N1 O1 146.37(19) . . . . ?
N5 Ni1 N1 O2 -122.0(3) . . . . ?
N3 Ni1 N1 O2 49.3(3) . . . . ?
O1A Ni1 N1 O2 167(2) . . . . ?
N4 Ni1 N1 O2 143.7(3) . . . . ?
O3 Ni1 N1 O2 -34.2(3) . . . . ?
O4 Ni1 N1 O2 -32.8(4) . . . . ?
O2A N1A O1A Ni1 -11(4) . . . . ?
N1 Ni1 O1A N1A 0.1(14) . . . . ?
N5 Ni1 O1A N1A -109(2) . . . . ?
N3 Ni1 O1A N1A 63(2) . . . . ?
N4 Ni1 O1A N1A 158(2) . . . . ?
O3 Ni1 O1A N1A -23(2) . . . . ?
O4 Ni1 O1A N1A -61(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3D O2A 0.92 2.68 3.15(5) 112.1 .
N5 H5C O3 0.92 2.19 3.017(2) 149.1 3_557
N5 H5C O2A 0.92 2.59 3.20(4) 123.8 3_557
N5 H5D O11 0.92 2.20 3.064(3) 156.6 4_565
N13 H13D O11 0.92 2.16 2.819(3) 127.7 4_565

_diffrn_measured_fraction_theta_max 0.904
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.096

_database_code_depnum_ccdc_archive 'CCDC 994158'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_complex7_135K
_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;
Dinitro-(3,3-diamino-N-methyldipropylamine)nickel(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H19 N5 Ni O4'
_chemical_formula_sum            'C7 H19 N5 Ni O4'
_chemical_formula_weight         295.98

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'
O O 0.0106 0.0060 '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'


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

_cell_length_a                   7.108(5)
_cell_length_b                   23.656(5)
_cell_length_c                   10.909(5)
_cell_angle_alpha                90.000
_cell_angle_beta                 103.439(5)
_cell_angle_gamma                90.000
_cell_volume                     1784.1(15)
_cell_formula_units_Z            6
_cell_measurement_temperature    135(2)
_cell_measurement_reflns_used    4348
_cell_measurement_theta_min      3.0490
_cell_measurement_theta_max      29.0170


_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/m

_exptl_crystal_description       Block
_exptl_crystal_colour            Violet
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936

_exptl_absorpt_coefficient_mu    1.645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.77566
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      135(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12216
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0446
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.24
_diffrn_reflns_theta_max         29.20
_reflns_number_total             4479
_reflns_number_gt                3690
_reflns_threshold_expression     >2sigma(I)


_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'POV-RAY for Windows, 3.62 (Cason, 2009)'
_computing_publication_material  'WinGX, 1.80.05 (Farrugia, 1999)'


_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 > 2sigma(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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0471P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4479
_refine_ls_number_parameters     267
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0304
_refine_ls_wR_factor_ref         0.0790
_refine_ls_wR_factor_gt          0.0757
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2811(3) 0.01858(8) 0.61630(17) 0.0166(4) Uani 1 1 d . . .
H1A H 0.1618 -0.0028 0.5789 0.020 Uiso 1 1 calc R . .
H1B H 0.3911 -0.0009 0.5930 0.020 Uiso 1 1 calc R . .
C2 C 0.2643(3) 0.07791(9) 0.56373(18) 0.0190(4) Uani 1 1 d . . .
H2A H 0.2730 0.0763 0.4745 0.023 Uiso 1 1 calc R . .
H2B H 0.3756 0.1004 0.6105 0.023 Uiso 1 1 calc R . .
C3 C 0.0792(3) 0.10824(8) 0.57050(17) 0.0188(4) Uani 1 1 d . . .
H3A H 0.0686 0.1426 0.5174 0.023 Uiso 1 1 calc R . .
H3B H -0.0309 0.0834 0.5325 0.023 Uiso 1 1 calc R . .
C4 C -0.1407(3) 0.15059(8) 0.67492(18) 0.0183(4) Uani 1 1 d . . .
H4A H -0.2341 0.1220 0.6309 0.022 Uiso 1 1 calc R . .
H4B H -0.1461 0.1831 0.6170 0.022 Uiso 1 1 calc R . .
C5 C -0.2073(3) 0.17067(8) 0.78997(19) 0.0205(4) Uani 1 1 d . . .
H5A H -0.1072 0.1960 0.8398 0.025 Uiso 1 1 calc R . .
H5B H -0.3270 0.1932 0.7616 0.025 Uiso 1 1 calc R . .
C6 C -0.2461(3) 0.12366(9) 0.87428(19) 0.0197(4) Uani 1 1 d . . .
H6A H -0.3108 0.1393 0.9380 0.024 Uiso 1 1 calc R . .
H6B H -0.3342 0.0956 0.8233 0.024 Uiso 1 1 calc R . .
C7 C 0.2013(3) 0.16967(8) 0.74833(18) 0.0184(4) Uani 1 1 d . . .
H7A H 0.3316 0.1537 0.7616 0.028 Uiso 1 1 calc R . .
H7B H 0.1803 0.1836 0.8287 0.028 Uiso 1 1 calc R . .
H7C H 0.1877 0.2010 0.6881 0.028 Uiso 1 1 calc R . .
C11 C 0.5306(3) 0.12727(8) 1.31903(18) 0.0183(4) Uani 1 1 d . . .
H11A H 0.4930 0.0870 1.3054 0.022 Uiso 1 1 calc R . .
H11B H 0.5893 0.1327 1.4098 0.022 Uiso 1 1 calc R . .
C12 C 0.6760(3) 0.14204(8) 1.2431(2) 0.0205(4) Uani 1 1 d . . .
H12A H 0.6117 0.1397 1.1525 0.025 Uiso 1 1 calc R . .
H12B H 0.7805 0.1134 1.2602 0.025 Uiso 1 1 calc R . .
C13 C 0.7661(3) 0.19998(8) 1.26953(19) 0.0173(4) Uani 1 1 d . . .
H13A H 0.8106 0.2043 1.3620 0.021 Uiso 1 1 calc R . .
H13B H 0.8824 0.2012 1.2342 0.021 Uiso 1 1 calc R . .
C17 C 0.6013(4) 0.2500 1.0813(2) 0.0205(6) Uani 1 2 d S . .
H17A H 0.7207 0.2424 1.0538 0.031 Uiso 0.50 1 calc PR . .
H17B H 0.5499 0.2870 1.0495 0.031 Uiso 0.50 1 calc PR . .
H17C H 0.5058 0.2206 1.0484 0.031 Uiso 0.50 1 calc PR . .
N2 N 0.3644(2) 0.05092(7) 1.04522(15) 0.0205(4) Uani 1 1 d . . .
N3 N 0.3109(2) 0.01916(8) 0.75428(15) 0.0149(3) Uani 1 1 d . . .
N4 N 0.0571(2) 0.12559(6) 0.69813(14) 0.0131(3) Uani 1 1 d . . .
N5 N -0.0661(2) 0.09566(7) 0.93802(16) 0.0159(3) Uani 1 1 d . . .
N11 N 0.1790(3) 0.2500 1.1118(2) 0.0139(4) Uani 1 2 d S . .
N12 N 0.3808(4) 0.2500 1.5211(2) 0.0298(6) Uani 1 2 d S . .
N13 N 0.3586(2) 0.16311(7) 1.28135(19) 0.0193(4) Uani 1 1 d . . .
N14 N 0.6430(3) 0.2500 1.2201(2) 0.0118(4) Uani 1 2 d S . .
O3 O 0.2429(2) 0.01325(6) 0.99871(13) 0.0191(3) Uani 1 1 d . . .
O4 O 0.34768(19) 0.09438(6) 0.97674(13) 0.0185(3) Uani 1 1 d . . .
O11 O 0.1133(2) 0.29449(7) 1.05915(15) 0.0329(4) Uani 1 1 d . . .
O13 O 0.2271(3) 0.2500 1.4366(2) 0.0275(5) Uani 1 2 d S . .
O14 O 0.5304(3) 0.2500 1.47635(18) 0.0223(4) Uani 1 2 d S . .
Ni1 Ni 0.10888(3) 0.059706(9) 0.83311(2) 0.01112(8) Uani 1 1 d . . .
Ni2 Ni 0.38727(4) 0.2500 1.28563(3) 0.01089(9) Uani 1 2 d S . .
N1 N -0.0930(2) 0.00155(7) 0.74673(15) 0.0153(3) Uani 1 1 d . . .
O1 O -0.2569(2) 0.01389(6) 0.68406(14) 0.0244(3) Uani 1 1 d . . .
O2 O -0.0486(2) -0.04951(6) 0.75950(15) 0.0243(3) Uani 1 1 d . . .
H5C H -0.092(4) 0.0701(13) 0.977(3) 0.038(8) Uiso 1 1 d . . .
H3C H 0.304(3) -0.0130(11) 0.785(2) 0.022(6) Uiso 1 1 d . . .
H5D H 0.002(4) 0.1196(11) 0.991(2) 0.022(6) Uiso 1 1 d . . .
H3D H 0.425(4) 0.0300(11) 0.788(2) 0.028(6) Uiso 1 1 d . . .
H13C H 0.275(4) 0.1521(11) 1.322(3) 0.036(7) Uiso 1 1 d . . .
H13D H 0.305(4) 0.1564(11) 1.206(3) 0.030(7) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N3 1.471(2) . ?
C1 C2 1.510(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.515(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N4 1.495(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.491(2) . ?
C4 C5 1.517(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.509(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N5 1.465(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 N4 1.475(2) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C11 N13 1.466(3) . ?
C11 C12 1.508(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.512(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N14 1.496(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C17 N14 1.474(3) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
N2 O4 1.260(2) . ?
N2 O3 1.262(2) . ?
N3 Ni1 2.0727(17) . ?
N3 H3C 0.84(3) . ?
N3 H3D 0.85(3) . ?
N4 Ni1 2.1169(16) . ?
N5 Ni1 2.0596(17) . ?
N5 H5C 0.79(3) . ?
N5 H5D 0.87(3) . ?
N11 O11 1.2373(19) 4_565 ?
N11 O11 1.2373(19) . ?
N11 Ni2 2.117(2) . ?
N12 O13 1.255(4) . ?
N12 O14 1.269(3) . ?
N13 Ni2 2.0651(18) . ?
N13 H13C 0.86(3) . ?
N13 H13D 0.84(3) . ?
N14 C13 1.496(2) 4_565 ?
N14 Ni2 2.102(2) . ?
O3 Ni1 2.1398(15) . ?
O4 Ni1 2.1847(16) . ?
O13 Ni2 2.209(2) . ?
O14 Ni2 2.093(2) . ?
Ni1 N1 2.0521(17) . ?
Ni2 N13 2.0651(18) 4_565 ?
N1 O1 1.241(2) . ?
N1 O2 1.248(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 C1 C2 111.08(16) . . ?
N3 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N3 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
C1 C2 C3 114.49(16) . . ?
C1 C2 H2A 108.6 . . ?
C3 C2 H2A 108.6 . . ?
C1 C2 H2B 108.6 . . ?
C3 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
N4 C3 C2 117.13(16) . . ?
N4 C3 H3A 108.0 . . ?
C2 C3 H3A 108.0 . . ?
N4 C3 H3B 108.0 . . ?
C2 C3 H3B 108.0 . . ?
H3A C3 H3B 107.3 . . ?
N4 C4 C5 116.54(16) . . ?
N4 C4 H4A 108.2 . . ?
C5 C4 H4A 108.2 . . ?
N4 C4 H4B 108.2 . . ?
C5 C4 H4B 108.2 . . ?
H4A C4 H4B 107.3 . . ?
C6 C5 C4 114.20(16) . . ?
C6 C5 H5A 108.7 . . ?
C4 C5 H5A 108.7 . . ?
C6 C5 H5B 108.7 . . ?
C4 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
N5 C6 C5 111.06(16) . . ?
N5 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
N5 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N13 C11 C12 110.21(16) . . ?
N13 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
N13 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
C11 C12 C13 114.80(16) . . ?
C11 C12 H12A 108.6 . . ?
C13 C12 H12A 108.6 . . ?
C11 C12 H12B 108.6 . . ?
C13 C12 H12B 108.6 . . ?
H12A C12 H12B 107.5 . . ?
N14 C13 C12 117.54(17) . . ?
N14 C13 H13A 107.9 . . ?
C12 C13 H13A 107.9 . . ?
N14 C13 H13B 107.9 . . ?
C12 C13 H13B 107.9 . . ?
H13A C13 H13B 107.2 . . ?
N14 C17 H17A 109.5 . . ?
N14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O4 N2 O3 112.10(16) . . ?
C1 N3 Ni1 118.70(12) . . ?
C1 N3 H3C 112.8(16) . . ?
Ni1 N3 H3C 98.6(15) . . ?
C1 N3 H3D 110.3(16) . . ?
Ni1 N3 H3D 111.3(16) . . ?
H3C N3 H3D 104(2) . . ?
C7 N4 C4 109.20(15) . . ?
C7 N4 C3 108.99(14) . . ?
C4 N4 C3 104.47(14) . . ?
C7 N4 Ni1 105.58(12) . . ?
C4 N4 Ni1 114.50(11) . . ?
C3 N4 Ni1 114.01(12) . . ?
C6 N5 Ni1 119.78(13) . . ?
C6 N5 H5C 108(2) . . ?
Ni1 N5 H5C 103(2) . . ?
C6 N5 H5D 108.1(17) . . ?
Ni1 N5 H5D 108.6(15) . . ?
H5C N5 H5D 108(3) . . ?
O11 N11 O11 116.6(2) 4_565 . ?
O11 N11 Ni2 121.71(12) 4_565 . ?
O11 N11 Ni2 121.71(12) . . ?
O13 N12 O14 112.4(2) . . ?
C11 N13 Ni2 119.87(13) . . ?
C11 N13 H13C 107.9(18) . . ?
Ni2 N13 H13C 111.5(18) . . ?
C11 N13 H13D 109.0(18) . . ?
Ni2 N13 H13D 103.3(18) . . ?
H13C N13 H13D 104(2) . . ?
C17 N14 C13 109.34(13) . 4_565 ?
C17 N14 C13 109.34(13) . . ?
C13 N14 C13 104.6(2) 4_565 . ?
C17 N14 Ni2 111.48(16) . . ?
C13 N14 Ni2 110.93(11) 4_565 . ?
C13 N14 Ni2 110.93(11) . . ?
N2 O3 Ni1 96.06(11) . . ?
N2 O4 Ni1 93.97(11) . . ?
N12 O13 Ni2 92.08(15) . . ?
N12 O14 Ni2 97.19(18) . . ?
N1 Ni1 N5 94.81(8) . . ?
N1 Ni1 N3 88.70(8) . . ?
N5 Ni1 N3 171.04(7) . . ?
N1 Ni1 N4 100.61(7) . . ?
N5 Ni1 N4 93.02(7) . . ?
N3 Ni1 N4 94.44(6) . . ?
N1 Ni1 O3 99.78(6) . . ?
N5 Ni1 O3 87.17(7) . . ?
N3 Ni1 O3 84.10(6) . . ?
N4 Ni1 O3 159.51(6) . . ?
N1 Ni1 O4 157.65(6) . . ?
N5 Ni1 O4 85.14(8) . . ?
N3 Ni1 O4 88.48(7) . . ?
N4 Ni1 O4 101.71(6) . . ?
O3 Ni1 O4 57.87(5) . . ?
N13 Ni2 N13 168.99(10) 4_565 . ?
N13 Ni2 O14 92.58(6) 4_565 . ?
N13 Ni2 O14 92.58(6) . . ?
N13 Ni2 N14 94.64(5) 4_565 . ?
N13 Ni2 N14 94.64(5) . . ?
O14 Ni2 N14 94.52(9) . . ?
N13 Ni2 N11 86.27(6) 4_565 . ?
N13 Ni2 N11 86.27(6) . . ?
O14 Ni2 N11 165.38(8) . . ?
N14 Ni2 N11 100.09(9) . . ?
N13 Ni2 O13 87.23(5) 4_565 . ?
N13 Ni2 O13 87.23(5) . . ?
O14 Ni2 O13 58.30(9) . . ?
N14 Ni2 O13 152.83(9) . . ?
N11 Ni2 O13 107.08(9) . . ?
O1 N1 O2 118.03(16) . . ?
O1 N1 Ni1 124.20(13) . . ?
O2 N1 Ni1 117.76(13) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 C1 C2 C3 -70.5(2) . . . . ?
C1 C2 C3 N4 70.4(2) . . . . ?
N4 C4 C5 C6 -69.9(2) . . . . ?
C4 C5 C6 N5 69.2(2) . . . . ?
N13 C11 C12 C13 67.4(2) . . . . ?
C11 C12 C13 N14 -73.3(2) . . . . ?
C2 C1 N3 Ni1 56.93(19) . . . . ?
C5 C4 N4 C7 -65.4(2) . . . . ?
C5 C4 N4 C3 178.14(16) . . . . ?
C5 C4 N4 Ni1 52.73(19) . . . . ?
C2 C3 N4 C7 66.8(2) . . . . ?
C2 C3 N4 C4 -176.60(16) . . . . ?
C2 C3 N4 Ni1 -50.9(2) . . . . ?
C5 C6 N5 Ni1 -57.7(2) . . . . ?
C12 C11 N13 Ni2 -55.0(2) . . . . ?
C12 C13 N14 C17 -67.2(2) . . . . ?
C12 C13 N14 C13 175.76(10) . . . 4_565 ?
C12 C13 N14 Ni2 56.1(2) . . . . ?
O4 N2 O3 Ni1 0.39(15) . . . . ?
O3 N2 O4 Ni1 -0.38(14) . . . . ?
O14 N12 O13 Ni2 0.000(1) . . . . ?
O13 N12 O14 Ni2 0.000(2) . . . . ?
C6 N5 Ni1 N1 -62.68(15) . . . . ?
C6 N5 Ni1 N3 -175.5(4) . . . . ?
C6 N5 Ni1 N4 38.24(15) . . . . ?
C6 N5 Ni1 O3 -162.27(15) . . . . ?
C6 N5 Ni1 O4 139.75(15) . . . . ?
C1 N3 Ni1 N1 64.00(15) . . . . ?
C1 N3 Ni1 N5 177.2(4) . . . . ?
C1 N3 Ni1 N4 -36.55(15) . . . . ?
C1 N3 Ni1 O3 163.97(15) . . . . ?
C1 N3 Ni1 O4 -138.18(14) . . . . ?
C7 N4 Ni1 N1 -177.81(11) . . . . ?
C4 N4 Ni1 N1 62.03(13) . . . . ?
C3 N4 Ni1 N1 -58.21(13) . . . . ?
C7 N4 Ni1 N5 86.72(12) . . . . ?
C4 N4 Ni1 N5 -33.44(13) . . . . ?
C3 N4 Ni1 N5 -153.67(13) . . . . ?
C7 N4 Ni1 N3 -88.31(12) . . . . ?
C4 N4 Ni1 N3 151.54(13) . . . . ?
C3 N4 Ni1 N3 31.30(13) . . . . ?
C7 N4 Ni1 O3 -3.3(2) . . . . ?
C4 N4 Ni1 O3 -123.43(16) . . . . ?
C3 N4 Ni1 O3 116.33(17) . . . . ?
C7 N4 Ni1 O4 1.06(12) . . . . ?
C4 N4 Ni1 O4 -119.10(13) . . . . ?
C3 N4 Ni1 O4 120.66(13) . . . . ?
N2 O3 Ni1 N1 179.32(10) . . . . ?
N2 O3 Ni1 N5 -86.28(12) . . . . ?
N2 O3 Ni1 N3 91.67(12) . . . . ?
N2 O3 Ni1 N4 4.8(2) . . . . ?
N2 O3 Ni1 O4 -0.25(9) . . . . ?
N2 O4 Ni1 N1 -0.88(19) . . . . ?
N2 O4 Ni1 N5 89.96(11) . . . . ?
N2 O4 Ni1 N3 -83.74(11) . . . . ?
N2 O4 Ni1 N4 -177.96(10) . . . . ?
N2 O4 Ni1 O3 0.25(9) . . . . ?
C11 N13 Ni2 N13 -174.1(5) . . . 4_565 ?
C11 N13 Ni2 O14 -56.17(16) . . . . ?
C11 N13 Ni2 N14 38.59(17) . . . . ?
C11 N13 Ni2 N11 138.43(16) . . . . ?
C11 N13 Ni2 O13 -114.24(16) . . . . ?
N12 O14 Ni2 N13 85.14(5) . . . 4_565 ?
N12 O14 Ni2 N13 -85.14(5) . . . . ?
N12 O14 Ni2 N14 180.000(1) . . . . ?
N12 O14 Ni2 N11 0.000(2) . . . . ?
N12 O14 Ni2 O13 0.000(1) . . . . ?
C17 N14 Ni2 N13 -87.03(6) . . . 4_565 ?
C13 N14 Ni2 N13 35.08(14) 4_565 . . 4_565 ?
C13 N14 Ni2 N13 150.86(13) . . . 4_565 ?
C17 N14 Ni2 N13 87.03(6) . . . . ?
C13 N14 Ni2 N13 -150.86(13) 4_565 . . . ?
C13 N14 Ni2 N13 -35.08(14) . . . . ?
C17 N14 Ni2 O14 180.000(1) . . . . ?
C13 N14 Ni2 O14 -57.89(13) 4_565 . . . ?
C13 N14 Ni2 O14 57.89(13) . . . . ?
C17 N14 Ni2 N11 0.000(1) . . . . ?
C13 N14 Ni2 N11 122.11(13) 4_565 . . . ?
C13 N14 Ni2 N11 -122.11(13) . . . . ?
C17 N14 Ni2 O13 180.000(2) . . . . ?
C13 N14 Ni2 O13 -57.89(13) 4_565 . . . ?
C13 N14 Ni2 O13 57.89(13) . . . . ?
O11 N11 Ni2 N13 -175.04(18) 4_565 . . 4_565 ?
O11 N11 Ni2 N13 3.16(17) . . . 4_565 ?
O11 N11 Ni2 N13 -3.16(17) 4_565 . . . ?
O11 N11 Ni2 N13 175.04(18) . . . . ?
O11 N11 Ni2 O14 -89.10(17) 4_565 . . . ?
O11 N11 Ni2 O14 89.10(17) . . . . ?
O11 N11 Ni2 N14 90.90(17) 4_565 . . . ?
O11 N11 Ni2 N14 -90.90(17) . . . . ?
O11 N11 Ni2 O13 -89.10(17) 4_565 . . . ?
O11 N11 Ni2 O13 89.10(17) . . . . ?
N12 O13 Ni2 N13 -94.76(5) . . . 4_565 ?
N12 O13 Ni2 N13 94.76(5) . . . . ?
N12 O13 Ni2 O14 0.000(2) . . . . ?
N12 O13 Ni2 N14 0.000(2) . . . . ?
N12 O13 Ni2 N11 180.000(2) . . . . ?
N5 Ni1 N1 O1 56.98(14) . . . . ?
N3 Ni1 N1 O1 -131.27(14) . . . . ?
N4 Ni1 N1 O1 -37.00(14) . . . . ?
O3 Ni1 N1 O1 144.94(13) . . . . ?
O4 Ni1 N1 O1 145.90(14) . . . . ?
N5 Ni1 N1 O2 -122.09(13) . . . . ?
N3 Ni1 N1 O2 49.66(13) . . . . ?
N4 Ni1 N1 O2 143.93(13) . . . . ?
O3 Ni1 N1 O2 -34.13(13) . . . . ?
O4 Ni1 N1 O2 -33.2(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 H5C O3 0.79(3) 2.29(3) 3.016(2) 154(3) 3_557
N3 H3C O2 0.84(3) 2.61(2) 3.040(3) 113.7(19) .
N5 H5D O11 0.87(3) 2.24(3) 3.056(2) 155(2) 4_565
N13 H13D O11 0.84(3) 2.18(3) 2.821(3) 133(2) 4_565

_diffrn_measured_fraction_theta_max 0.906
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.090

_database_code_depnum_ccdc_archive 'CCDC 994159'
