# 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.
# 
#  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_I
_chemical_name_systematic        ?
_chemical_name_common            '[Ni(bpta)(CH3COO)2(H2O)].H2O'
_chemical_formula_moiety         'C20 H29 N3 Ni O5, H2 O'
_chemical_formula_sum            'C20 H31 N3 Ni O6'
_chemical_formula_iupac          ?
_chemical_formula_weight         468.19

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.362(2)
_cell_length_b                   9.211(3)
_cell_length_c                   14.892(4)
_cell_angle_alpha                100.999(19)
_cell_angle_beta                 94.355(17)
_cell_angle_gamma                97.503(17)
_cell_volume                     1110.3(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3000
_cell_measurement_theta_min      2.2775
_cell_measurement_theta_max      22.8674
_cell_measurement_temperature    270.(2)

_exptl_crystal_description       'rod shaped'
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             496

_exptl_absorpt_coefficient_mu    0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_T_max  0.91

_exptl_special_details           
;
;

_diffrn_ambient_temperature      270.(2)

_diffrn_source                   ?
_diffrn_source_type              ?

_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  ?

_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            13454
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0604
_diffrn_reflns_theta_min         1.40
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_full        25.09
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17

_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.
;

_reflns_number_total             3893
_reflns_number_gt                2960
_reflns_threshold_expression     >2sigma(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.1031
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_restrained_S_all      0.974
_refine_ls_number_reflns         3893
_refine_ls_number_parameters     285
_refine_ls_number_restraints     3
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0514P)²+0.1953P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.386
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_computing_data_collection       ?
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.29902(4) 0.45987(4) 0.26800(3) 0.02811(14) Uani d . 1 . .
N N1 0.2489(3) 0.6756(3) 0.30422(16) 0.0308(6) Uani d . 1 . .
N N2 0.0390(3) 0.4326(3) 0.20710(15) 0.0264(6) Uani d . 1 . .
N N3 0.1849(3) 0.3894(3) 0.37331(16) 0.0293(6) Uani d . 1 . .
O O1 0.3398(2) 0.2507(2) 0.21494(15) 0.0419(6) Uani d . 1 . .
O O2 0.5665(3) 0.2184(3) 0.29281(18) 0.0565(7) Uani d . 1 . .
O O3 0.4024(2) 0.5349(2) 0.15844(14) 0.0381(5) Uani d . 1 . .
O O4 0.6346(3) 0.6633(3) 0.23401(16) 0.0503(6) Uani d . 1 . .
O O5 0.5214(3) 0.5050(3) 0.34799(15) 0.0401(6) Uani d D 1 . .
H H5A 0.572(4) 0.553(3) 0.315(2) 0.06 Uiso d D 1 . .
H H5B 0.553(4) 0.4229(19) 0.336(2) 0.06 Uiso d D 1 . .
O O6 0.7227(4) 0.9666(4) 0.3471(3) 0.0941(11) Uani d G 1 . .
H H6A 0.6752 1.036 0.3322 0.141 Uiso d G 1 . .
H H6B 0.6911 0.8857 0.3081 0.141 Uiso d G 1 . .
C C1 0.4527(4) 0.1777(4) 0.2291(2) 0.0385(8) Uani d . 1 . .
C C2 0.4493(5) 0.0319(4) 0.1629(3) 0.0657(12) Uani d . 1 . .
H H2A 0.4246 -0.0493 0.1939 0.099 Uiso calc R 1 . .
H H2B 0.5534 0.0281 0.1401 0.099 Uiso calc R 1 . .
H H2C 0.3679 0.0238 0.1125 0.099 Uiso calc R 1 . .
C C3 0.5335(4) 0.6226(3) 0.1633(2) 0.0346(8) Uani d . 1 . .
C C4 0.5729(4) 0.6811(4) 0.0786(2) 0.0452(9) Uani d . 1 . .
H H4A 0.606 0.6032 0.0345 0.068 Uiso calc R 1 . .
H H4B 0.6593 0.7639 0.0948 0.068 Uiso calc R 1 . .
H H4C 0.4786 0.7134 0.0524 0.068 Uiso calc R 1 . .
C C5 0.3336(4) 0.7877(4) 0.3685(2) 0.0396(8) Uani d . 1 . .
H H5 0.422 0.7678 0.4036 0.048 Uiso calc R 1 . .
C C6 0.2954(4) 0.9289(4) 0.3844(2) 0.0459(9) Uani d . 1 . .
H H6 0.3569 1.0038 0.4292 0.055 Uiso calc R 1 . .
C C7 0.1642(4) 0.9591(4) 0.3331(2) 0.0500(9) Uani d . 1 . .
H H7 0.1356 1.0547 0.3428 0.06 Uiso calc R 1 . .
C C8 0.0759(4) 0.8454(4) 0.2672(2) 0.0415(8) Uani d . 1 . .
H H8 -0.0141 0.863 0.2325 0.05 Uiso calc R 1 . .
C C9 0.1223(3) 0.7062(3) 0.2533(2) 0.0305(7) Uani d . 1 . .
C C10 0.0364(4) 0.5796(3) 0.1793(2) 0.0316(7) Uani d . 1 . .
H H10A -0.0752 0.5946 0.1669 0.038 Uiso calc R 1 . .
H H10B 0.0884 0.579 0.1232 0.038 Uiso calc R 1 . .
C C11 -0.0289(3) 0.3030(3) 0.12783(19) 0.0299(7) Uani d . 1 . .
C C12 -0.1977(4) 0.3200(4) 0.0855(2) 0.0435(9) Uani d . 1 . .
H H12A -0.1886 0.4052 0.0568 0.065 Uiso calc R 1 . .
H H12B -0.269 0.3338 0.133 0.065 Uiso calc R 1 . .
H H12C -0.2406 0.2317 0.0404 0.065 Uiso calc R 1 . .
C C13 -0.0412(4) 0.1573(3) 0.1634(2) 0.0403(8) Uani d . 1 . .
H H13A -0.0734 0.0741 0.1128 0.061 Uiso calc R 1 . .
H H13B -0.1203 0.1575 0.2069 0.061 Uiso calc R 1 . .
H H13C 0.0624 0.1486 0.1928 0.061 Uiso calc R 1 . .
C C14 0.0861(4) 0.2957(4) 0.0533(2) 0.0412(8) Uani d . 1 . .
H H14A 0.1905 0.2802 0.078 0.062 Uiso calc R 1 . .
H H14B 0.0967 0.3878 0.0316 0.062 Uiso calc R 1 . .
H H14C 0.0437 0.2144 0.0031 0.062 Uiso calc R 1 . .
C C15 -0.0573(3) 0.4310(3) 0.28742(19) 0.0295(7) Uani d . 1 . .
H H15A -0.1621 0.3705 0.2663 0.035 Uiso calc R 1 . .
H H15B -0.0761 0.5321 0.3116 0.035 Uiso calc R 1 . .
C C16 0.0220(3) 0.3714(3) 0.36379(19) 0.0287(7) Uani d . 1 . .
C C17 -0.0690(4) 0.3084(4) 0.4240(2) 0.0388(8) Uani d . 1 . .
H H17 -0.1817 0.2966 0.4158 0.047 Uiso calc R 1 . .
C C18 0.0096(4) 0.2634(4) 0.4966(2) 0.0446(9) Uani d . 1 . .
H H18 -0.0492 0.2189 0.5373 0.053 Uiso calc R 1 . .
C C19 0.1764(4) 0.2854(4) 0.5077(2) 0.0439(9) Uani d . 1 . .
H H19 0.2317 0.2587 0.5572 0.053 Uiso calc R 1 . .
C C20 0.2600(4) 0.3467(4) 0.4456(2) 0.0367(8) Uani d . 1 . .
H H20 0.3727 0.3596 0.4531 0.044 Uiso calc R 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 O1 . 2.021(2) ?
Ni1 N3 . 2.061(2) ?
Ni1 N1 . 2.063(3) ?
Ni1 O5 . 2.079(2) ?
Ni1 O3 . 2.092(2) ?
Ni1 N2 . 2.255(2) ?
N1 C5 . 1.347(4) ?
N1 C9 . 1.347(4) ?
N2 C10 . 1.491(4) ?
N2 C15 . 1.493(3) ?
N2 C11 . 1.524(4) ?
N3 C16 . 1.343(3) ?
N3 C20 . 1.353(4) ?
O1 C1 . 1.256(4) ?
O2 C1 . 1.258(4) ?
O3 C3 . 1.262(3) ?
O4 C3 . 1.262(4) ?
O5 H5A . 0.833(10) ?
O5 H5B . 0.825(10) ?
O6 H6A . 0.85 ?
O6 H6B . 0.8501 ?
C1 C2 . 1.502(5) ?
C2 H2A . 0.96 ?
C2 H2B . 0.96 ?
C2 H2C . 0.96 ?
C3 C4 . 1.506(4) ?
C4 H4A . 0.96 ?
C4 H4B . 0.96 ?
C4 H4C . 0.96 ?
C5 C6 . 1.361(4) ?
C5 H5 . 0.93 ?
C6 C7 . 1.378(5) ?
C6 H6 . 0.93 ?
C7 C8 . 1.379(5) ?
C7 H7 . 0.93 ?
C8 C9 . 1.370(4) ?
C8 H8 . 0.93 ?
C9 C10 . 1.503(4) ?
C10 H10A . 0.97 ?
C10 H10B . 0.97 ?
C11 C14 . 1.520(4) ?
C11 C13 . 1.529(4) ?
C11 C12 . 1.541(4) ?
C12 H12A . 0.96 ?
C12 H12B . 0.96 ?
C12 H12C . 0.96 ?
C13 H13A . 0.96 ?
C13 H13B . 0.96 ?
C13 H13C . 0.96 ?
C14 H14A . 0.96 ?
C14 H14B . 0.96 ?
C14 H14C . 0.96 ?
C15 C16 . 1.501(4) ?
C15 H15A . 0.97 ?
C15 H15B . 0.97 ?
C16 C17 . 1.381(4) ?
C17 C18 . 1.381(4) ?
C17 H17 . 0.93 ?
C18 C19 . 1.375(4) ?
C18 H18 . 0.93 ?
C19 C20 . 1.363(4) ?
C19 H19 . 0.93 ?
C20 H20 . 0.93 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Ni1 N3 . . 91.97(10) ?
O1 Ni1 N1 . . 172.32(9) ?
N3 Ni1 N1 . . 93.66(10) ?
O1 Ni1 O5 . . 91.05(9) ?
N3 Ni1 O5 . . 91.07(9) ?
N1 Ni1 O5 . . 94.05(9) ?
O1 Ni1 O3 . . 89.49(9) ?
N3 Ni1 O3 . . 176.74(9) ?
N1 Ni1 O3 . . 84.62(9) ?
O5 Ni1 O3 . . 91.82(8) ?
O1 Ni1 N2 . . 96.99(9) ?
N3 Ni1 N2 . . 80.63(9) ?
N1 Ni1 N2 . . 78.82(9) ?
O5 Ni1 N2 . . 168.60(8) ?
O3 Ni1 N2 . . 96.30(8) ?
C5 N1 C9 . . 118.0(3) ?
C5 N1 Ni1 . . 127.1(2) ?
C9 N1 Ni1 . . 114.72(19) ?
C10 N2 C15 . . 108.0(2) ?
C10 N2 C11 . . 111.3(2) ?
C15 N2 C11 . . 111.0(2) ?
C10 N2 Ni1 . . 100.47(15) ?
C15 N2 Ni1 . . 104.38(15) ?
C11 N2 Ni1 . . 120.61(17) ?
C16 N3 C20 . . 118.2(3) ?
C16 N3 Ni1 . . 116.44(19) ?
C20 N3 Ni1 . . 125.1(2) ?
C1 O1 Ni1 . . 133.5(2) ?
C3 O3 Ni1 . . 126.5(2) ?
Ni1 O5 H5A . . 97.(3) ?
Ni1 O5 H5B . . 101.(3) ?
H5A O5 H5B . . 103.(2) ?
H6A O6 H6B . . 109.6 ?
O1 C1 O2 . . 125.0(3) ?
O1 C1 C2 . . 116.1(3) ?
O2 C1 C2 . . 118.8(3) ?
C1 C2 H2A . . 109.5 ?
C1 C2 H2B . . 109.5 ?
H2A C2 H2B . . 109.5 ?
C1 C2 H2C . . 109.5 ?
H2A C2 H2C . . 109.5 ?
H2B C2 H2C . . 109.5 ?
O3 C3 O4 . . 124.6(3) ?
O3 C3 C4 . . 117.7(3) ?
O4 C3 C4 . . 117.8(3) ?
C3 C4 H4A . . 109.5 ?
C3 C4 H4B . . 109.5 ?
H4A C4 H4B . . 109.5 ?
C3 C4 H4C . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
N1 C5 C6 . . 122.8(3) ?
N1 C5 H5 . . 118.6 ?
C6 C5 H5 . . 118.6 ?
C5 C6 C7 . . 119.0(3) ?
C5 C6 H6 . . 120.5 ?
C7 C6 H6 . . 120.5 ?
C6 C7 C8 . . 119.0(3) ?
C6 C7 H7 . . 120.5 ?
C8 C7 H7 . . 120.5 ?
C9 C8 C7 . . 119.3(3) ?
C9 C8 H8 . . 120.3 ?
C7 C8 H8 . . 120.3 ?
N1 C9 C8 . . 121.9(3) ?
N1 C9 C10 . . 116.2(3) ?
C8 C9 C10 . . 122.0(3) ?
N2 C10 C9 . . 111.4(2) ?
N2 C10 H10A . . 109.4 ?
C9 C10 H10A . . 109.4 ?
N2 C10 H10B . . 109.4 ?
C9 C10 H10B . . 109.4 ?
H10A C10 H10B . . 108.0 ?
C14 C11 N2 . . 109.2(2) ?
C14 C11 C13 . . 108.9(3) ?
N2 C11 C13 . . 108.8(2) ?
C14 C11 C12 . . 108.6(2) ?
N2 C11 C12 . . 112.2(2) ?
C13 C11 C12 . . 109.1(2) ?
C11 C12 H12A . . 109.5 ?
C11 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C11 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
C11 C13 H13A . . 109.5 ?
C11 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C11 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
C11 C14 H14A . . 109.5 ?
C11 C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
C11 C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
N2 C15 C16 . . 114.1(2) ?
N2 C15 H15A . . 108.7 ?
C16 C15 H15A . . 108.7 ?
N2 C15 H15B . . 108.7 ?
C16 C15 H15B . . 108.7 ?
H15A C15 H15B . . 107.6 ?
N3 C16 C17 . . 122.0(3) ?
N3 C16 C15 . . 116.9(3) ?
C17 C16 C15 . . 121.1(3) ?
C16 C17 C18 . . 119.1(3) ?
C16 C17 H17 . . 120.5 ?
C18 C17 H17 . . 120.5 ?
C19 C18 C17 . . 118.9(3) ?
C19 C18 H18 . . 120.6 ?
C17 C18 H18 . . 120.6 ?
C20 C19 C18 . . 119.5(3) ?
C20 C19 H19 . . 120.3 ?
C18 C19 H19 . . 120.3 ?
N3 C20 C19 . . 122.4(3) ?
N3 C20 H20 . . 118.8 ?
C19 C20 H20 . . 118.8 ?

_database_code_depnum_ccdc_archive 'CCDC 979224'
#######################################################################
#
#                 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_1
_chemical_name_systematic        ?
_chemical_name_common            '[Ni(bpta)(H2O)2(adc)].2H2O'
_chemical_formula_moiety         'C20 H25 N3 Ni O6, 2(H2 O)'
_chemical_formula_sum            'C20 H29 N3 Ni O8'
_chemical_formula_iupac          ?
_chemical_formula_weight         498.17

_chemical_melting_point          ?

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   13.9083(6)
_cell_length_b                   17.7966(7)
_cell_length_c                   18.4094(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4556.7(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    4884
_cell_measurement_theta_min      2.2126
_cell_measurement_theta_max      24.1420
_cell_measurement_temperature    140.(2)

_exptl_crystal_description       rectangular
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2096

_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_absorpt_correction_T_min  0.6014
_exptl_absorpt_correction_T_max  0.7452

_exptl_special_details           
;
;

_diffrn_ambient_temperature      140.(2)

_diffrn_source                   'sealed tube'
_diffrn_source_type              'fine focus'

_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            24675
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_theta_min         2.16
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_full        25.06
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21

_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.
;

_reflns_number_total             4028
_reflns_number_gt                2939
_reflns_threshold_expression     >2sigma(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0880
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_refine_ls_number_reflns         4028
_refine_ls_number_parameters     316
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    undef
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0615P)²+4.7923P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.322
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_computing_data_collection       'APEX2 (Bruker)'
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Bruker AXS)'
_computing_publication_material  'SHELXTL (Bruker AXS)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.35710(2) 0.070513(18) 0.307388(18) 0.01552(12) Uani d . 1 . .
N N1 0.32236(17) -0.05183(12) 0.32634(12) 0.0176(5) Uani d . 1 . .
N N2 0.39054(16) 0.02880(12) 0.20600(12) 0.0175(5) Uani d . 1 . .
N N3 0.48074(16) 0.03270(12) 0.35642(11) 0.0161(5) Uani d . 1 . .
O O1 0.22852(15) 0.11266(11) 0.26622(11) 0.0204(5) Uani d . 1 . .
H H1A 0.228(2) 0.1452(16) 0.2319(17) 0.031 Uiso d . 1 . .
H H1B 0.208(2) 0.1365(17) 0.3008(17) 0.031 Uiso d . 1 . .
O O2 0.41877(15) 0.17497(11) 0.28648(12) 0.0233(5) Uani d . 1 . .
H H2A 0.400(2) 0.2060(17) 0.2520(17) 0.035 Uiso d . 1 . .
H H2B 0.446(2) 0.2013(18) 0.3164(17) 0.035 Uiso d . 1 . .
O O3 0.31967(13) 0.10961(10) 0.40991(10) 0.0205(5) Uani d . 1 . .
O O4 0.18008(14) 0.17101(11) 0.39385(10) 0.0262(5) Uani d . 1 . .
O O5 0.37239(15) 0.24883(11) 0.65848(11) 0.0271(5) Uani d . 1 . .
O O6 0.21517(15) 0.27715(12) 0.66189(11) 0.0329(5) Uani d . 1 . .
O O7 0.52263(17) 0.24638(13) 0.39215(13) 0.0327(6) Uani d . 1 . .
H H7A 0.517(2) 0.2474(18) 0.4412(19) 0.049 Uiso d . 1 . .
H H7B 0.579(3) 0.2362(19) 0.384(2) 0.049 Uiso d . 1 . .
O O8 0.5207(2) 0.25332(18) 0.54623(14) 0.0550(8) Uani d . 1 . .
H H8A 0.482(3) 0.250(2) 0.576(2) 0.083 Uiso d . 1 . .
H H8B 0.567(3) 0.279(2) 0.565(2) 0.083 Uiso d . 1 . .
C C1 0.3740(2) -0.09181(15) 0.26594(15) 0.0209(7) Uani d . 1 . .
H H1C 0.4381 -0.1051 0.2823 0.025 Uiso calc R 1 . .
H H1D 0.3401 -0.1381 0.2549 0.025 Uiso calc R 1 . .
C C2 0.3821(2) -0.04591(15) 0.19789(15) 0.0192(6) Uani d . 1 . .
C C3 0.3869(2) -0.07965(16) 0.12997(16) 0.0246(7) Uani d . 1 . .
H H3A 0.3808 -0.1315 0.1255 0.029 Uiso calc R 1 . .
C C4 0.4009(2) -0.03570(17) 0.06913(16) 0.0267(7) Uani d . 1 . .
H H4A 0.4025 -0.0573 0.0232 0.032 Uiso calc R 1 . .
C C5 0.4124(2) 0.04098(17) 0.07748(16) 0.0244(7) Uani d . 1 . .
H H5A 0.4239 0.0717 0.0375 0.029 Uiso calc R 1 . .
C C6 0.4066(2) 0.07093(16) 0.14654(15) 0.0214(6) Uani d . 1 . .
H H6A 0.4141 0.1225 0.1522 0.026 Uiso calc R 1 . .
C C7 0.3755(2) -0.06782(15) 0.39471(15) 0.0212(7) Uani d . 1 . .
H H7C 0.3836 -0.1217 0.3999 0.025 Uiso calc R 1 . .
H H7D 0.3381 -0.05 0.4357 0.025 Uiso calc R 1 . .
C C8 0.4723(2) -0.03080(15) 0.39549(14) 0.0184(6) Uani d . 1 . .
C C9 0.5651(2) 0.06896(16) 0.35727(15) 0.0203(6) Uani d . 1 . .
H H9 0.5712 0.1127 0.3301 0.024 Uiso calc R 1 . .
C C10 0.6431(2) 0.04431(16) 0.39660(15) 0.0223(7) Uani d . 1 . .
H H10 0.7002 0.0714 0.3969 0.027 Uiso calc R 1 . .
C C11 0.6346(2) -0.02144(16) 0.43553(15) 0.0238(7) Uani d . 1 . .
H H11 0.6866 -0.0399 0.4618 0.029 Uiso calc R 1 . .
C C12 0.5481(2) -0.05985(15) 0.43523(15) 0.0231(7) Uani d . 1 . .
H H12 0.541 -0.1043 0.4612 0.028 Uiso calc R 1 . .
C C13 0.2178(2) -0.07800(15) 0.33166(16) 0.0211(7) Uani d . 1 . .
C C14 0.1638(2) -0.02723(17) 0.38453(16) 0.0271(7) Uani d . 1 . .
H H14A 0.195 -0.0284 0.431 0.041 Uiso calc R 1 . .
H H14B 0.0988 -0.0447 0.3895 0.041 Uiso calc R 1 . .
H H14C 0.1636 0.0233 0.3663 0.041 Uiso calc R 1 . .
C C15 0.2091(2) -0.15971(16) 0.35777(18) 0.0314(8) Uani d . 1 . .
H H15A 0.2475 -0.1916 0.3273 0.047 Uiso calc R 1 . .
H H15B 0.1431 -0.1753 0.3553 0.047 Uiso calc R 1 . .
H H15C 0.2312 -0.1633 0.407 0.047 Uiso calc R 1 . .
C C16 0.1708(2) -0.07029(17) 0.25687(16) 0.0263(7) Uani d . 1 . .
H H16A 0.1833 -0.021 0.2378 0.039 Uiso calc R 1 . .
H H16B 0.1027 -0.0776 0.2613 0.039 Uiso calc R 1 . .
H H16C 0.197 -0.1074 0.2246 0.039 Uiso calc R 1 . .
C C17 0.2539(2) 0.15397(15) 0.42871(15) 0.0197(6) Uani d . 1 . .
C C18 0.2656(2) 0.18898(15) 0.50127(16) 0.0219(7) Uani d . 1 . .
C C19 0.2759(2) 0.21648(16) 0.55961(16) 0.0216(7) Uani d . 1 . .
C C20 0.2890(2) 0.25027(15) 0.63300(15) 0.0218(7) Uani d . 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 N3 . 2.055(2) ?
Ni1 N2 . 2.062(2) ?
Ni1 O3 . 2.0779(18) ?
Ni1 O1 . 2.082(2) ?
Ni1 O2 . 2.083(2) ?
Ni1 N1 . 2.257(2) ?
N1 C7 . 1.487(3) ?
N1 C1 . 1.503(4) ?
N1 C13 . 1.530(4) ?
N2 C2 . 1.343(3) ?
N2 C6 . 1.345(3) ?
N3 C9 . 1.339(3) ?
N3 C8 . 1.345(3) ?
O1 H1A . 0.86(3) ?
O1 H1B . 0.82(3) ?
O2 H2A . 0.88(3) ?
O2 H2B . 0.81(3) ?
O3 C17 . 1.257(3) ?
O4 C17 . 1.248(3) ?
O5 C20 . 1.251(3) ?
O6 C20 . 1.252(3) ?
O7 H7A . 0.91(3) ?
O7 H7B . 0.81(4) ?
O8 H8A . 0.76(4) ?
O8 H8B . 0.86(4) ?
C1 C2 . 1.500(4) ?
C1 H1C . 0.97 ?
C1 H1D . 0.97 ?
C2 C3 . 1.389(4) ?
C3 C4 . 1.380(4) ?
C3 H3A . 0.93 ?
C4 C5 . 1.383(4) ?
C4 H4A . 0.93 ?
C5 C6 . 1.381(4) ?
C5 H5A . 0.93 ?
C6 H6A . 0.93 ?
C7 C8 . 1.499(4) ?
C7 H7C . 0.97 ?
C7 H7D . 0.97 ?
C8 C12 . 1.383(4) ?
C9 C10 . 1.376(4) ?
C9 H9 . 0.93 ?
C10 C11 . 1.377(4) ?
C10 H10 . 0.93 ?
C11 C12 . 1.384(4) ?
C11 H11 . 0.93 ?
C12 H12 . 0.93 ?
C13 C14 . 1.526(4) ?
C13 C16 . 1.531(4) ?
C13 C15 . 1.536(4) ?
C14 H14A . 0.96 ?
C14 H14B . 0.96 ?
C14 H14C . 0.96 ?
C15 H15A . 0.96 ?
C15 H15B . 0.96 ?
C15 H15C . 0.96 ?
C16 H16A . 0.96 ?
C16 H16B . 0.96 ?
C16 H16C . 0.96 ?
C17 C18 . 1.483(4) ?
C18 C19 . 1.189(4) ?
C19 C20 . 1.490(4) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N3 Ni1 N2 . . 95.22(9) ?
N3 Ni1 O3 . . 85.43(8) ?
N2 Ni1 O3 . . 177.96(8) ?
N3 Ni1 O1 . . 175.13(8) ?
N2 Ni1 O1 . . 89.65(8) ?
O3 Ni1 O1 . . 89.71(8) ?
N3 Ni1 O2 . . 91.65(8) ?
N2 Ni1 O2 . . 93.50(9) ?
O3 Ni1 O2 . . 88.41(8) ?
O1 Ni1 O2 . . 87.99(8) ?
N3 Ni1 N1 . . 78.20(8) ?
N2 Ni1 N1 . . 80.85(8) ?
O3 Ni1 N1 . . 97.41(8) ?
O1 Ni1 N1 . . 102.70(8) ?
O2 Ni1 N1 . . 167.79(8) ?
C7 N1 C1 . . 107.3(2) ?
C7 N1 C13 . . 111.1(2) ?
C1 N1 C13 . . 111.0(2) ?
C7 N1 Ni1 . . 102.06(15) ?
C1 N1 Ni1 . . 103.88(16) ?
C13 N1 Ni1 . . 120.46(16) ?
C2 N2 C6 . . 118.4(2) ?
C2 N2 Ni1 . . 115.93(18) ?
C6 N2 Ni1 . . 124.98(18) ?
C9 N3 C8 . . 118.4(2) ?
C9 N3 Ni1 . . 125.47(19) ?
C8 N3 Ni1 . . 115.90(18) ?
Ni1 O1 H1A . . 121.(2) ?
Ni1 O1 H1B . . 102.(2) ?
H1A O1 H1B . . 103.(3) ?
Ni1 O2 H2A . . 125.(2) ?
Ni1 O2 H2B . . 125.(2) ?
H2A O2 H2B . . 105.(3) ?
C17 O3 Ni1 . . 129.99(18) ?
H7A O7 H7B . . 105.(3) ?
H8A O8 H8B . . 106.(4) ?
C2 C1 N1 . . 113.3(2) ?
C2 C1 H1C . . 108.9 ?
N1 C1 H1C . . 108.9 ?
C2 C1 H1D . . 108.9 ?
N1 C1 H1D . . 108.9 ?
H1C C1 H1D . . 107.7 ?
N2 C2 C3 . . 121.6(3) ?
N2 C2 C1 . . 116.9(2) ?
C3 C2 C1 . . 121.3(3) ?
C4 C3 C2 . . 119.5(3) ?
C4 C3 H3A . . 120.2 ?
C2 C3 H3A . . 120.2 ?
C3 C4 C5 . . 119.1(3) ?
C3 C4 H4A . . 120.5 ?
C5 C4 H4A . . 120.5 ?
C6 C5 C4 . . 118.5(3) ?
C6 C5 H5A . . 120.8 ?
C4 C5 H5A . . 120.8 ?
N2 C6 C5 . . 122.9(3) ?
N2 C6 H6A . . 118.5 ?
C5 C6 H6A . . 118.5 ?
N1 C7 C8 . . 111.7(2) ?
N1 C7 H7C . . 109.3 ?
C8 C7 H7C . . 109.3 ?
N1 C7 H7D . . 109.3 ?
C8 C7 H7D . . 109.3 ?
H7C C7 H7D . . 107.9 ?
N3 C8 C12 . . 122.0(3) ?
N3 C8 C7 . . 116.3(2) ?
C12 C8 C7 . . 121.7(3) ?
N3 C9 C10 . . 122.9(3) ?
N3 C9 H9 . . 118.5 ?
C10 C9 H9 . . 118.5 ?
C9 C10 C11 . . 118.5(3) ?
C9 C10 H10 . . 120.7 ?
C11 C10 H10 . . 120.7 ?
C10 C11 C12 . . 119.4(3) ?
C10 C11 H11 . . 120.3 ?
C12 C11 H11 . . 120.3 ?
C8 C12 C11 . . 118.7(3) ?
C8 C12 H12 . . 120.7 ?
C11 C12 H12 . . 120.7 ?
C14 C13 N1 . . 109.2(2) ?
C14 C13 C16 . . 108.1(2) ?
N1 C13 C16 . . 108.7(2) ?
C14 C13 C15 . . 108.8(2) ?
N1 C13 C15 . . 112.5(2) ?
C16 C13 C15 . . 109.4(2) ?
C13 C14 H14A . . 109.5 ?
C13 C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
C13 C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
C13 C15 H15A . . 109.5 ?
C13 C15 H15B . . 109.5 ?
H15A C15 H15B . . 109.5 ?
C13 C15 H15C . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
C13 C16 H16A . . 109.5 ?
C13 C16 H16B . . 109.5 ?
H16A C16 H16B . . 109.5 ?
C13 C16 H16C . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
O4 C17 O3 . . 127.6(3) ?
O4 C17 C18 . . 116.9(2) ?
O3 C17 C18 . . 115.6(3) ?
C19 C18 C17 . . 179.2(3) ?
C18 C19 C20 . . 179.5(3) ?
O5 C20 O6 . . 127.5(3) ?
O5 C20 C19 . . 116.4(3) ?
O6 C20 C19 . . 116.0(3) ?
_database_code_depnum_ccdc_archive 'CCDC 965630'
#######################################################################
#
#                 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_2
_chemical_name_systematic        ?
_chemical_name_common            '[Ni4(bpta)4(fumarate)4(H2O)4].4H2O'
_chemical_formula_moiety         'C80 H100 N12 Ni4 O20, 4(H2 O)'
_chemical_formula_sum            'C80 H108 N12 Ni4 O24'
_chemical_formula_iupac          ?
_chemical_formula_weight         1856.62

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.1706(9)
_cell_length_b                   14.6580(12)
_cell_length_c                   16.5447(16)
_cell_angle_alpha                75.264(5)
_cell_angle_beta                 83.445(6)
_cell_angle_gamma                87.664(6)
_cell_volume                     2136.6(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    2835
_cell_measurement_theta_min      2.4541
_cell_measurement_theta_max      22.9301
_cell_measurement_temperature    150.(2)

_exptl_crystal_description       rectangular
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             976

_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_absorpt_correction_T_min  0.6632
_exptl_absorpt_correction_T_max  0.7452

_exptl_special_details           
;
;

_diffrn_ambient_temperature      150.(2)

_diffrn_source                   'sealed tube'
_diffrn_source_type              'fine focus'

_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker kappa Apex2'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            16303
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_sigmaI/netI    0.1182
_diffrn_reflns_theta_min         1.28
_diffrn_reflns_theta_max         25.14
_diffrn_reflns_theta_full        25.14
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19

_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.
;

_reflns_number_total             7539
_reflns_number_gt                4333
_reflns_threshold_expression     >2sigma(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0452
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.1123
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_restrained_S_all      0.897
_refine_ls_number_reflns         7539
_refine_ls_number_parameters     549
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    undef
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0415P)²+0.0000P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.442
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_computing_data_collection       ?
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni1 1.08110(7) 0.78466(4) -0.18664(3) 0.02549(17) Uani d . 1 . .
Ni Ni2 0.36991(7) 0.68762(4) 0.31100(3) 0.02432(17) Uani d . 1 . .
N N1 0.4347(4) 0.8144(2) 0.3269(2) 0.0274(9) Uani d . 1 . .
N N2 0.1659(4) 0.7710(2) 0.2866(2) 0.0275(9) Uani d . 1 . .
N N3 0.2428(4) 0.6398(2) 0.4258(2) 0.0295(9) Uani d . 1 . .
N N4 1.2336(4) 0.8516(2) -0.1408(2) 0.0240(9) Uani d . 1 . .
N N5 1.2667(4) 0.6761(2) -0.1752(2) 0.0299(9) Uani d . 1 . .
N N6 1.1858(4) 0.8164(2) -0.3089(2) 0.0296(9) Uani d . 1 . .
O O1 0.9324(3) 0.70775(19) -0.22700(19) 0.0318(8) Uani d . 1 . .
O O2 0.2954(3) 0.57287(19) 0.27891(18) 0.0308(8) Uani d . 1 . .
O O3 0.5495(3) 0.61203(18) 0.36129(17) 0.0279(7) Uani d . 1 . .
H H3A 0.5312 0.553 0.3752 0.042 Uiso d R 1 . .
H H3B 0.6245 0.6225 0.3246 0.042 Uiso d R 1 . .
O O4 0.4890(3) 0.72496(19) 0.19513(17) 0.0283(8) Uani d . 1 . .
O O5 0.7087(4) 0.6595(2) 0.22173(19) 0.0363(8) Uani d . 1 . .
O O6 0.9723(3) 0.74584(18) -0.06896(18) 0.0298(8) Uani d . 1 . .
O O7 0.9526(3) 0.90661(17) -0.21828(17) 0.0294(8) Uani d . 1 . .
H H7A 0.8896 0.8988 -0.2501 0.044 Uiso d R 1 . .
H H7B 0.9079 0.9179 -0.1736 0.044 Uiso d R 1 . .
O O8 0.4208(4) 0.45587(19) 0.35701(19) 0.0334(8) Uani d . 1 . .
O O10 0.8128(3) 0.8658(2) -0.06883(19) 0.0367(8) Uani d . 1 . .
O O11 0.1813(4) 0.1740(2) 0.3132(2) 0.0557(11) Uani d . 1 . .
O O13 0.6509(4) 0.68005(18) 0.49135(19) 0.0454(9) Uani d G 1 . .
H H13C 0.6193 0.6583 0.4537 0.068 Uiso d G 1 . .
H H13D 0.6346 0.6391 0.5379 0.068 Uiso d G 1 . .
O O12 0.1975(6) 0.1501(2) 0.4988(3) 0.119(2) Uani d G 1 . .
H H12C 0.1784 0.1615 0.4481 0.178 Uiso d G 1 . .
H H12D 0.2321 0.1992 0.5077 0.178 Uiso d G 1 . .
C C1 0.1602(6) 0.2598(3) 0.2768(3) 0.0336(12) Uani d . 1 . .
C C3 0.2502(5) 0.3283(3) 0.3030(3) 0.0333(12) Uani d . 1 . .
H H3 0.3161 0.3036 0.3438 0.04 Uiso calc R 1 . .
C C4 0.2441(5) 0.4199(3) 0.2734(3) 0.0302(11) Uani d . 1 . .
H H4 0.1843 0.4452 0.2295 0.036 Uiso calc R 1 . .
C C5 0.3290(5) 0.4880(3) 0.3064(3) 0.0293(11) Uani d . 1 . .
C C6 0.3298(6) 0.8811(3) 0.3257(3) 0.0299(12) Uani d . 1 . .
C C7 0.1746(5) 0.8493(3) 0.3292(3) 0.0324(12) Uani d . 1 . .
H H7C 0.133 0.8276 0.3886 0.039 Uiso calc R 1 . .
H H7D 0.1143 0.9035 0.3018 0.039 Uiso calc R 1 . .
C C8 0.0511(5) 0.7053(3) 0.3382(3) 0.0396(13) Uani d . 1 . .
H H8A 0.0308 0.6577 0.308 0.048 Uiso calc R 1 . .
H H8B -0.0409 0.7411 0.3465 0.048 Uiso calc R 1 . .
C C9 0.1001(6) 0.6563(3) 0.4223(3) 0.0355(12) Uani d . 1 . .
C C10 0.2902(6) 0.5908(3) 0.4983(3) 0.0347(12) Uani d . 1 . .
H H10 0.3926 0.5792 0.5002 0.042 Uiso calc R 1 . .
C C11 0.1963(6) 0.5566(3) 0.5701(3) 0.0446(14) Uani d . 1 . .
H H11 0.2328 0.5209 0.6203 0.054 Uiso calc R 1 . .
C C12 0.0508(7) 0.5752(4) 0.5673(3) 0.0522(16) Uani d . 1 . .
H H12 -0.0161 0.5531 0.616 0.063 Uiso calc R 1 . .
C C13 -0.0001(6) 0.6262(3) 0.4935(3) 0.0487(15) Uani d . 1 . .
H H13 -0.1017 0.6405 0.4911 0.058 Uiso calc R 1 . .
C C14 0.1305(5) 0.8091(3) 0.1963(3) 0.0312(12) Uani d . 1 . .
C C15 0.2394(5) 0.8867(3) 0.1521(3) 0.0349(12) Uani d . 1 . .
H H15A 0.3397 0.8625 0.1586 0.052 Uiso calc R 1 . .
H H15B 0.2224 0.9406 0.177 0.052 Uiso calc R 1 . .
H H15C 0.2259 0.9067 0.0922 0.052 Uiso calc R 1 . .
C C16 0.1497(6) 0.7302(3) 0.1509(3) 0.0375(13) Uani d . 1 . .
H H16A 0.1331 0.7555 0.0918 0.056 Uiso calc R 1 . .
H H16B 0.0788 0.6804 0.1776 0.056 Uiso calc R 1 . .
H H16C 0.2496 0.7041 0.1541 0.056 Uiso calc R 1 . .
C C17 -0.0258(5) 0.8485(3) 0.1913(3) 0.0420(13) Uani d . 1 . .
H H17A -0.0414 0.8963 0.2236 0.063 Uiso calc R 1 . .
H H17B -0.0958 0.7973 0.2146 0.063 Uiso calc R 1 . .
H H17C -0.0405 0.8773 0.1324 0.063 Uiso calc R 1 . .
C C18 0.3630(6) 0.9734(3) 0.3247(3) 0.0357(13) Uani d . 1 . .
H H18 0.2872 1.0197 0.3242 0.043 Uiso calc R 1 . .
C C19 0.5062(6) 0.9965(3) 0.3246(3) 0.0401(14) Uani d . 1 . .
H H19 0.5308 1.0589 0.3245 0.048 Uiso calc R 1 . .
C C20 0.6143(6) 0.9287(3) 0.3245(3) 0.0396(13) Uani d . 1 . .
H H20 0.7143 0.9434 0.324 0.048 Uiso calc R 1 . .
C C21 0.5743(6) 0.8389(3) 0.3252(3) 0.0325(12) Uani d . 1 . .
H H21 0.6492 0.7923 0.3245 0.039 Uiso calc R 1 . .
C C22 0.6216(6) 0.7103(3) 0.1741(3) 0.0280(11) Uani d . 1 . .
C C23 0.6799(5) 0.7577(3) 0.0862(3) 0.0266(11) Uani d . 1 . .
H H23 0.6205 0.8048 0.0541 0.032 Uiso calc R 1 . .
C C24 0.8081(5) 0.7381(3) 0.0507(3) 0.0290(11) Uani d . 1 . .
H H24 0.866 0.6895 0.0819 0.035 Uiso calc R 1 . .
C C25 0.8677(5) 0.7878(3) -0.0357(3) 0.0276(11) Uani d . 1 . .
C C27 1.3690(5) 0.8158(3) -0.1391(3) 0.0265(11) Uani d . 1 . .
C C28 1.4798(6) 0.8573(3) -0.1114(3) 0.0362(12) Uani d . 1 . .
H H28 1.5757 0.8304 -0.1109 0.043 Uiso calc R 1 . .
C C29 1.4490(6) 0.9382(3) -0.0847(3) 0.0404(14) Uani d . 1 . .
H H29 1.5243 0.9688 -0.0671 0.049 Uiso calc R 1 . .
C C30 1.3094(6) 0.9740(3) -0.0837(3) 0.0346(12) Uani d . 1 . .
H H30 1.2854 1.0288 -0.064 0.042 Uiso calc R 1 . .
C C31 1.2046(5) 0.9291(3) -0.1117(3) 0.0304(12) Uani d . 1 . .
H H31 1.1071 0.9537 -0.1105 0.037 Uiso calc R 1 . .
C C32 1.4007(5) 0.7300(3) -0.1727(3) 0.0341(12) Uani d . 1 . .
H H32A 1.4518 0.7499 -0.2303 0.041 Uiso calc R 1 . .
H H32B 1.4681 0.6874 -0.1372 0.041 Uiso calc R 1 . .
C C33 1.2536(5) 0.5861(3) -0.1054(3) 0.0338(12) Uani d . 1 . .
C C34 1.3787(6) 0.5152(3) -0.1146(3) 0.0449(14) Uani d . 1 . .
H H34A 1.4732 0.5446 -0.1156 0.067 Uiso calc R 1 . .
H H34B 1.3756 0.4964 -0.1672 0.067 Uiso calc R 1 . .
H H34C 1.3671 0.4594 -0.067 0.067 Uiso calc R 1 . .
C C35 1.1089(6) 0.5387(3) -0.1064(3) 0.0426(14) Uani d . 1 . .
H H35A 1.0931 0.4856 -0.0566 0.064 Uiso calc R 1 . .
H H35B 1.1127 0.5155 -0.1572 0.064 Uiso calc R 1 . .
H H35C 1.0281 0.5844 -0.106 0.064 Uiso calc R 1 . .
C C36 1.2521(6) 0.6111(3) -0.0222(3) 0.0395(13) Uani d . 1 . .
H H36A 1.1688 0.6535 -0.0152 0.059 Uiso calc R 1 . .
H H36B 1.3438 0.6426 -0.021 0.059 Uiso calc R 1 . .
H H36C 1.2427 0.5535 0.0236 0.059 Uiso calc R 1 . .
C C37 1.2733(5) 0.6568(3) -0.2592(3) 0.0304(12) Uani d . 1 . .
H H37A 1.1871 0.6194 -0.2617 0.036 Uiso calc R 1 . .
H H37B 1.363 0.6194 -0.269 0.036 Uiso calc R 1 . .
C C38 1.2749(5) 0.7484(3) -0.3266(3) 0.0320(12) Uani d . 1 . .
C C39 1.1782(5) 0.8980(3) -0.3673(3) 0.0335(12) Uani d . 1 . .
H H39 1.1134 0.9462 -0.3553 0.04 Uiso calc R 1 . .
C C40 1.2613(6) 0.9145(3) -0.4447(3) 0.0431(14) Uani d . 1 . .
H H40 1.2528 0.9725 -0.4857 0.052 Uiso calc R 1 . .
C C41 1.3567(6) 0.8447(4) -0.4606(3) 0.0444(14) Uani d . 1 . .
H H41 1.418 0.8549 -0.5123 0.053 Uiso calc R 1 . .
C C42 1.3629(6) 0.7611(3) -0.4021(3) 0.0369(13) Uani d . 1 . .
H H42 1.4269 0.712 -0.4129 0.044 Uiso calc R 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 O6 . 2.037(3) ?
Ni1 N4 . 2.056(3) ?
Ni1 O1 . 2.072(3) ?
Ni1 N6 . 2.084(4) ?
Ni1 O7 . 2.086(3) ?
Ni1 N5 . 2.272(4) ?
Ni2 O4 . 2.050(3) ?
Ni2 O2 . 2.051(3) ?
Ni2 N1 . 2.061(3) ?
Ni2 O3 . 2.080(3) ?
Ni2 N3 . 2.084(4) ?
Ni2 N2 . 2.212(4) ?
N1 C21 . 1.339(5) ?
N1 C6 . 1.342(5) ?
N2 C8 . 1.491(5) ?
N2 C7 . 1.500(5) ?
N2 C14 . 1.523(5) ?
N3 C9 . 1.326(6) ?
N3 C10 . 1.340(5) ?
N4 C27 . 1.329(5) ?
N4 C31 . 1.348(5) ?
N5 C37 . 1.482(5) ?
N5 C32 . 1.498(5) ?
N5 C33 . 1.515(5) ?
N6 C38 . 1.333(5) ?
N6 C39 . 1.337(5) ?
O1 C1 2_665 1.246(5) ?
O2 C5 . 1.250(5) ?
O3 H3A . 0.8546 ?
O3 H3B . 0.8545 ?
O4 C22 . 1.251(5) ?
O5 C22 . 1.269(5) ?
O6 C25 . 1.267(5) ?
O7 H7A . 0.8539 ?
O7 H7B . 0.8539 ?
O8 C5 . 1.249(5) ?
O10 C25 . 1.248(5) ?
O11 C1 . 1.266(5) ?
O13 H13C . 0.8499 ?
O13 H13D . 0.85 ?
O12 H12C . 0.8499 ?
O12 H12D . 0.8499 ?
C1 O1 2_665 1.246(5) ?
C1 C3 . 1.500(6) ?
C3 C4 . 1.308(5) ?
C3 H3 . 0.95 ?
C4 C5 . 1.529(6) ?
C4 H4 . 0.95 ?
C6 C18 . 1.395(5) ?
C6 C7 . 1.506(6) ?
C7 H7C . 0.99 ?
C7 H7D . 0.99 ?
C8 C9 . 1.505(6) ?
C8 H8A . 0.99 ?
C8 H8B . 0.99 ?
C9 C13 . 1.395(6) ?
C10 C11 . 1.380(6) ?
C10 H10 . 0.95 ?
C11 C12 . 1.355(7) ?
C11 H11 . 0.95 ?
C12 C13 . 1.380(7) ?
C12 H12 . 0.95 ?
C13 H13 . 0.95 ?
C14 C16 . 1.526(5) ?
C14 C15 . 1.526(6) ?
C14 C17 . 1.526(6) ?
C15 H15A . 0.98 ?
C15 H15B . 0.98 ?
C15 H15C . 0.98 ?
C16 H16A . 0.98 ?
C16 H16B . 0.98 ?
C16 H16C . 0.98 ?
C17 H17A . 0.98 ?
C17 H17B . 0.98 ?
C17 H17C . 0.98 ?
C18 C19 . 1.370(6) ?
C18 H18 . 0.95 ?
C19 C20 . 1.375(7) ?
C19 H19 . 0.95 ?
C20 C21 . 1.377(6) ?
C20 H20 . 0.95 ?
C21 H21 . 0.95 ?
C22 C23 . 1.491(6) ?
C23 C24 . 1.308(6) ?
C23 H23 . 0.95 ?
C24 C25 . 1.482(6) ?
C24 H24 . 0.95 ?
C27 C28 . 1.381(6) ?
C27 C32 . 1.506(6) ?
C28 C29 . 1.375(6) ?
C28 H28 . 0.95 ?
C29 C30 . 1.363(7) ?
C29 H29 . 0.95 ?
C30 C31 . 1.371(6) ?
C30 H30 . 0.95 ?
C31 H31 . 0.95 ?
C32 H32A . 0.99 ?
C32 H32B . 0.99 ?
C33 C36 . 1.511(6) ?
C33 C35 . 1.527(6) ?
C33 C34 . 1.537(6) ?
C34 H34A . 0.98 ?
C34 H34B . 0.98 ?
C34 H34C . 0.98 ?
C35 H35A . 0.98 ?
C35 H35B . 0.98 ?
C35 H35C . 0.98 ?
C36 H36A . 0.98 ?
C36 H36B . 0.98 ?
C36 H36C . 0.98 ?
C37 C38 . 1.510(6) ?
C37 H37A . 0.99 ?
C37 H37B . 0.99 ?
C38 C42 . 1.382(6) ?
C39 C40 . 1.383(6) ?
C39 H39 . 0.95 ?
C40 C41 . 1.375(7) ?
C40 H40 . 0.95 ?
C41 C42 . 1.359(6) ?
C41 H41 . 0.95 ?
C42 H42 . 0.95 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O6 Ni1 N4 . . 89.29(12) ?
O6 Ni1 O1 . . 88.78(12) ?
N4 Ni1 O1 . . 175.69(13) ?
O6 Ni1 N6 . . 176.01(12) ?
N4 Ni1 N6 . . 94.35(14) ?
O1 Ni1 N6 . . 87.48(13) ?
O6 Ni1 O7 . . 91.99(11) ?
N4 Ni1 O7 . . 92.78(12) ?
O1 Ni1 O7 . . 91.14(11) ?
N6 Ni1 O7 . . 89.46(13) ?
O6 Ni1 N5 . . 100.68(12) ?
N4 Ni1 N5 . . 79.43(13) ?
O1 Ni1 N5 . . 97.15(12) ?
N6 Ni1 N5 . . 78.44(14) ?
O7 Ni1 N5 . . 164.96(12) ?
O4 Ni2 O2 . . 88.77(11) ?
O4 Ni2 N1 . . 86.04(12) ?
O2 Ni2 N1 . . 171.59(13) ?
O4 Ni2 O3 . . 90.22(12) ?
O2 Ni2 O3 . . 92.10(11) ?
N1 Ni2 O3 . . 94.52(13) ?
O4 Ni2 N3 . . 175.15(12) ?
O2 Ni2 N3 . . 86.39(12) ?
N1 Ni2 N3 . . 98.78(13) ?
O3 Ni2 N3 . . 89.93(14) ?
O4 Ni2 N2 . . 101.20(13) ?
O2 Ni2 N2 . . 94.00(12) ?
N1 Ni2 N2 . . 80.55(14) ?
O3 Ni2 N2 . . 167.15(12) ?
N3 Ni2 N2 . . 79.20(14) ?
C21 N1 C6 . . 118.3(4) ?
C21 N1 Ni2 . . 124.8(3) ?
C6 N1 Ni2 . . 116.1(3) ?
C8 N2 C7 . . 106.7(3) ?
C8 N2 C14 . . 111.9(3) ?
C7 N2 C14 . . 111.2(3) ?
C8 N2 Ni2 . . 102.2(3) ?
C7 N2 Ni2 . . 104.5(3) ?
C14 N2 Ni2 . . 119.2(3) ?
C9 N3 C10 . . 119.2(4) ?
C9 N3 Ni2 . . 114.0(3) ?
C10 N3 Ni2 . . 126.7(3) ?
C27 N4 C31 . . 117.9(4) ?
C27 N4 Ni1 . . 118.0(3) ?
C31 N4 Ni1 . . 124.1(3) ?
C37 N5 C32 . . 108.3(3) ?
C37 N5 C33 . . 111.7(3) ?
C32 N5 C33 . . 111.5(3) ?
C37 N5 Ni1 . . 99.4(3) ?
C32 N5 Ni1 . . 104.9(2) ?
C33 N5 Ni1 . . 120.0(3) ?
C38 N6 C39 . . 118.7(4) ?
C38 N6 Ni1 . . 114.3(3) ?
C39 N6 Ni1 . . 126.8(3) ?
C1 O1 Ni1 2_665 . 126.4(3) ?
C5 O2 Ni2 . . 127.9(3) ?
Ni2 O3 H3A . . 109.8 ?
Ni2 O3 H3B . . 109.5 ?
H3A O3 H3B . . 109.2 ?
C22 O4 Ni2 . . 129.8(3) ?
C25 O6 Ni1 . . 129.0(3) ?
Ni1 O7 H7A . . 109.6 ?
Ni1 O7 H7B . . 109.4 ?
H7A O7 H7B . . 109.3 ?
H13C O13 H13D . . 107.6 ?
H12C O12 H12D . . 109.6 ?
O1 C1 O11 2_665 . 127.1(4) ?
O1 C1 C3 2_665 . 118.0(4) ?
O11 C1 C3 . . 114.7(4) ?
C4 C3 C1 . . 124.3(4) ?
C4 C3 H3 . . 117.8 ?
C1 C3 H3 . . 117.8 ?
C3 C4 C5 . . 122.8(4) ?
C3 C4 H4 . . 118.6 ?
C5 C4 H4 . . 118.6 ?
O8 C5 O2 . . 126.6(4) ?
O8 C5 C4 . . 119.4(4) ?
O2 C5 C4 . . 114.0(4) ?
N1 C6 C18 . . 121.6(5) ?
N1 C6 C7 . . 116.1(4) ?
C18 C6 C7 . . 122.3(4) ?
N2 C7 C6 . . 112.3(4) ?
N2 C7 H7C . . 109.1 ?
C6 C7 H7C . . 109.1 ?
N2 C7 H7D . . 109.1 ?
C6 C7 H7D . . 109.1 ?
H7C C7 H7D . . 107.9 ?
N2 C8 C9 . . 110.8(4) ?
N2 C8 H8A . . 109.5 ?
C9 C8 H8A . . 109.5 ?
N2 C8 H8B . . 109.5 ?
C9 C8 H8B . . 109.5 ?
H8A C8 H8B . . 108.1 ?
N3 C9 C13 . . 120.9(5) ?
N3 C9 C8 . . 117.3(4) ?
C13 C9 C8 . . 121.7(5) ?
N3 C10 C11 . . 122.7(5) ?
N3 C10 H10 . . 118.7 ?
C11 C10 H10 . . 118.7 ?
C12 C11 C10 . . 118.3(5) ?
C12 C11 H11 . . 120.9 ?
C10 C11 H11 . . 120.9 ?
C11 C12 C13 . . 119.9(5) ?
C11 C12 H12 . . 120.0 ?
C13 C12 H12 . . 120.0 ?
C12 C13 C9 . . 118.9(5) ?
C12 C13 H13 . . 120.5 ?
C9 C13 H13 . . 120.5 ?
N2 C14 C16 . . 109.3(3) ?
N2 C14 C15 . . 108.4(3) ?
C16 C14 C15 . . 108.3(4) ?
N2 C14 C17 . . 112.4(4) ?
C16 C14 C17 . . 108.8(4) ?
C15 C14 C17 . . 109.5(4) ?
C14 C15 H15A . . 109.5 ?
C14 C15 H15B . . 109.5 ?
H15A C15 H15B . . 109.5 ?
C14 C15 H15C . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
C14 C16 H16A . . 109.5 ?
C14 C16 H16B . . 109.5 ?
H16A C16 H16B . . 109.5 ?
C14 C16 H16C . . 109.5 ?
H16A C16 H16C . . 109.5 ?
H16B C16 H16C . . 109.5 ?
C14 C17 H17A . . 109.5 ?
C14 C17 H17B . . 109.5 ?
H17A C17 H17B . . 109.5 ?
C14 C17 H17C . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 109.5 ?
C19 C18 C6 . . 119.1(5) ?
C19 C18 H18 . . 120.4 ?
C6 C18 H18 . . 120.4 ?
C18 C19 C20 . . 119.4(4) ?
C18 C19 H19 . . 120.3 ?
C20 C19 H19 . . 120.3 ?
C19 C20 C21 . . 118.6(5) ?
C19 C20 H20 . . 120.7 ?
C21 C20 H20 . . 120.7 ?
N1 C21 C20 . . 122.9(5) ?
N1 C21 H21 . . 118.5 ?
C20 C21 H21 . . 118.5 ?
O4 C22 O5 . . 125.2(4) ?
O4 C22 C23 . . 116.4(4) ?
O5 C22 C23 . . 118.4(4) ?
C24 C23 C22 . . 123.7(4) ?
C24 C23 H23 . . 118.2 ?
C22 C23 H23 . . 118.2 ?
C23 C24 C25 . . 123.5(4) ?
C23 C24 H24 . . 118.3 ?
C25 C24 H24 . . 118.3 ?
O10 C25 O6 . . 126.0(4) ?
O10 C25 C24 . . 118.5(4) ?
O6 C25 C24 . . 115.5(4) ?
N4 C27 C28 . . 122.1(4) ?
N4 C27 C32 . . 117.4(4) ?
C28 C27 C32 . . 120.4(4) ?
C29 C28 C27 . . 119.0(5) ?
C29 C28 H28 . . 120.5 ?
C27 C28 H28 . . 120.5 ?
C30 C29 C28 . . 119.5(5) ?
C30 C29 H29 . . 120.3 ?
C28 C29 H29 . . 120.3 ?
C29 C30 C31 . . 118.5(4) ?
C29 C30 H30 . . 120.7 ?
C31 C30 H30 . . 120.7 ?
N4 C31 C30 . . 122.9(5) ?
N4 C31 H31 . . 118.5 ?
C30 C31 H31 . . 118.5 ?
N5 C32 C27 . . 113.9(4) ?
N5 C32 H32A . . 108.8 ?
C27 C32 H32A . . 108.8 ?
N5 C32 H32B . . 108.8 ?
C27 C32 H32B . . 108.8 ?
H32A C32 H32B . . 107.7 ?
C36 C33 N5 . . 108.6(3) ?
C36 C33 C35 . . 108.5(4) ?
N5 C33 C35 . . 109.1(4) ?
C36 C33 C34 . . 109.8(4) ?
N5 C33 C34 . . 112.8(4) ?
C35 C33 C34 . . 107.9(4) ?
C33 C34 H34A . . 109.5 ?
C33 C34 H34B . . 109.5 ?
H34A C34 H34B . . 109.5 ?
C33 C34 H34C . . 109.5 ?
H34A C34 H34C . . 109.5 ?
H34B C34 H34C . . 109.5 ?
C33 C35 H35A . . 109.5 ?
C33 C35 H35B . . 109.5 ?
H35A C35 H35B . . 109.5 ?
C33 C35 H35C . . 109.5 ?
H35A C35 H35C . . 109.5 ?
H35B C35 H35C . . 109.5 ?
C33 C36 H36A . . 109.5 ?
C33 C36 H36B . . 109.5 ?
H36A C36 H36B . . 109.5 ?
C33 C36 H36C . . 109.5 ?
H36A C36 H36C . . 109.5 ?
H36B C36 H36C . . 109.5 ?
N5 C37 C38 . . 110.0(3) ?
N5 C37 H37A . . 109.7 ?
C38 C37 H37A . . 109.7 ?
N5 C37 H37B . . 109.7 ?
C38 C37 H37B . . 109.7 ?
H37A C37 H37B . . 108.2 ?
N6 C38 C42 . . 121.8(4) ?
N6 C38 C37 . . 115.9(4) ?
C42 C38 C37 . . 122.3(4) ?
N6 C39 C40 . . 122.3(5) ?
N6 C39 H39 . . 118.9 ?
C40 C39 H39 . . 118.9 ?
C41 C40 C39 . . 118.2(4) ?
C41 C40 H40 . . 120.9 ?
C39 C40 H40 . . 120.9 ?
C42 C41 C40 . . 119.7(5) ?
C42 C41 H41 . . 120.1 ?
C40 C41 H41 . . 120.1 ?
C41 C42 C38 . . 119.2(5) ?
C41 C42 H42 . . 120.4 ?
C38 C42 H42 . . 120.4 ?
_database_code_depnum_ccdc_archive 'CCDC 965631'
#######################################################################
#
#                 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_2
_chemical_name_systematic        ?
_chemical_name_common            '[Ni(bpta)(succinate)(H2O)2].3H2O'
_chemical_formula_moiety         'C20 H29 N3 Ni O6, 3(H2 O)'
_chemical_formula_sum            'C20 H35 N3 Ni O9'
_chemical_formula_iupac          ?
_chemical_formula_weight         520.22
_chemical_absolute_configuration ?

_chemical_melting_point          ?

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'

_cell_length_a                   14.5930(13)
_cell_length_b                   9.6778(7)
_cell_length_c                   17.2357(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2434.2(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4067
_cell_measurement_theta_min      2.3633
_cell_measurement_theta_max      23.8232
_cell_measurement_temperature    150.(2)

_exptl_crystal_description       rectangular
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104

_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_T_max  0.75

_exptl_special_details           
;
;

_diffrn_ambient_temperature      150.(2)

_diffrn_source_type              'sealed tube'

_diffrn_radiation_type           'Mo Ka'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            16582
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_sigmaI/netI    ?
_diffrn_reflns_theta_min         2.10
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_full        25.07
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20

_refine_special_details          
;
;

_reflns_number_total             4267
_reflns_number_gt                3633
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0354
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0734
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_restrained_S_all      0.968
_refine_ls_number_reflns         4267
_refine_ls_number_parameters     314
_refine_ls_number_restraints     1
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
w=1/[σ²(Fo²)+(0.0258P)²+0.5981P]
where P=(Fo²+2Fc²)/3
;

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.187
_refine_diff_density_min         -0.307
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
Flack x determined using 1500 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.010(11)

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'

_computing_data_collection       'APEX2 (Bruker)'
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Bruker AXS)'
_computing_publication_material  'SHELXTL (Bruker AXS)'


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.72592(3) 0.95930(5) 0.74560(4) 0.02524(15) Uani d . . . 1 . .
O O1 0.6082(3) 1.0446(4) 0.7902(2) 0.0359(9) Uani d . . . 1 . .
H H1A 0.613(4) 1.123(7) 0.816(4) 0.07(2) Uiso d . . . 1 . .
H H1B 0.577(5) 0.989(7) 0.812(4) 0.06(2) Uiso d . . . 1 . .
O O2 0.7932(2) 0.9945(4) 0.8522(2) 0.0320(8) Uani d . . . 1 . .
H H2A 0.764(5) 1.067(8) 0.881(5) 0.10(3) Uiso d . . . 1 . .
H H2B 0.779(4) 0.910(8) 0.878(4) 0.07(2) Uiso d . . . 1 . .
O O3 0.6822(2) 0.7696(3) 0.78419(19) 0.0334(8) Uani d . . . 1 . .
O O4 0.7528(3) 0.7450(3) 0.8982(2) 0.0458(9) Uani d . . . 1 . .
O O5 0.6029(3) 0.2795(4) 0.8716(3) 0.0524(11) Uani d . . . 1 . .
O O6 0.7408(2) 0.2374(3) 0.9196(2) 0.0424(9) Uani d . . . 1 . .
O O7 0.43635(18) 0.4126(4) 0.88937(16) 0.0656(13) Uani d . . G 1 . .
H H7B 0.3955 0.3522 0.8985 0.098 Uiso d U . G 1 . .
H H7A 0.4887 0.3742 0.8879 0.098 Uiso d U . G 1 . .
O O8 0.98256(18) 0.0997(4) 0.8702(2) 0.0669(13) Uani d . . G 1 . .
H H8A 0.973 0.1688 0.8996 0.1 Uiso d U . G 1 . .
H H8B 0.9337 0.0525 0.8661 0.1 Uiso d U . G 1 . .
O O9 0.0826(2) 0.6744(4) 0.4508(2) 0.0563(10) Uani d . . G 1 . .
H H9B 0.0793 0.6169 0.4136 0.084 Uiso d U . G 1 . .
H H9A 0.1385 0.6877 0.4393 0.084 Uiso d U . G 1 . .
N N1 0.6750(3) 0.9546(4) 0.6236(2) 0.0277(9) Uani d . . . 1 . .
N N2 0.8346(3) 0.8589(4) 0.6929(2) 0.0283(9) Uani d . . . 1 . .
N N3 0.7606(3) 1.1561(4) 0.7085(2) 0.0288(9) Uani d . . . 1 . .
C C1 0.7019(3) 0.7026(5) 0.8448(3) 0.0286(11) Uani d . . . 1 . .
C C2 0.6611(4) 0.5601(5) 0.8493(3) 0.0441(13) Uani d . . . 1 . .
H H2D 0.5936 0.5698 0.8514 0.053 Uiso calc U . R 1 . .
H H2C 0.6761 0.511 0.8005 0.053 Uiso calc U . R 1 . .
C C3 0.6901(4) 0.4713(5) 0.9155(4) 0.0462(14) Uani d . . . 1 . .
H H3C 0.6547 0.4982 0.9621 0.055 Uiso calc U . R 1 . .
H H3D 0.7557 0.489 0.9265 0.055 Uiso calc U . R 1 . .
C C4 0.6772(4) 0.3183(5) 0.9016(3) 0.0346(12) Uani d . . . 1 . .
C C6 0.5981(3) 0.8543(5) 0.6003(3) 0.0323(11) Uani d . . . 1 . .
C C7 0.6378(4) 0.7064(5) 0.6003(3) 0.0425(13) Uani d . . . 1 . .
H H24 0.6646 0.6863 0.6511 0.064 Uiso calc U . R 1 . .
H H23 0.6852 0.699 0.5602 0.064 Uiso calc U . R 1 . .
H H22 0.5887 0.6401 0.5894 0.064 Uiso calc U . R 1 . .
C C8 0.5217(3) 0.8591(5) 0.6606(3) 0.0406(13) Uani d . . . 1 . .
H H20 0.5011 0.9547 0.6673 0.061 Uiso calc U . R 1 . .
H H19 0.5448 0.8238 0.7102 0.061 Uiso calc U . R 1 . .
H H21 0.4703 0.8019 0.6432 0.061 Uiso calc U . R 1 . .
C C9 0.5589(4) 0.8871(6) 0.5205(3) 0.0441(13) Uani d . . . 1 . .
H H26 0.5158 0.8143 0.5052 0.066 Uiso calc U . R 1 . .
H H11A 0.6088 0.892 0.4825 0.066 Uiso calc U . R 1 . .
H H25 0.5269 0.976 0.5222 0.066 Uiso calc U . R 1 . .
C C10 0.6448(4) 1.1000(5) 0.6133(3) 0.0363(12) Uani d . . . 1 . .
H H10B 0.5844 1.1126 0.6385 0.044 Uiso calc U . R 1 . .
H H18 0.6374 1.1193 0.5572 0.044 Uiso calc U . R 1 . .
C C11 0.7117(3) 1.2009(5) 0.6471(3) 0.0320(11) Uani d . . . 1 . .
C C12 0.7213(4) 1.3331(6) 0.6187(4) 0.0446(14) Uani d . . . 1 . .
H H11 0.6867 1.363 0.5752 0.053 Uiso calc U . R 1 . .
C C13 0.7823(4) 1.4215(6) 0.6548(4) 0.0491(15) Uani d . . . 1 . .
H H12 0.7898 1.5132 0.6362 0.059 Uiso calc U . R 1 . .
C C14 0.8319(4) 1.3765(5) 0.7172(3) 0.0444(14) Uani d . . . 1 . .
H H13 0.8737 1.4363 0.7429 0.053 Uiso calc U . R 1 . .
C C15 0.8198(3) 1.2423(4) 0.7419(4) 0.0360(10) Uani d . . . 1 . .
H H14 0.855 1.2099 0.7846 0.043 Uiso calc U . R 1 . .
C C16 0.7592(3) 0.9333(5) 0.5756(3) 0.0335(12) Uani d . . . 1 . .
H H16B 0.7418 0.8878 0.5263 0.04 Uiso calc U . R 1 . .
H H16A 0.786 1.0245 0.5628 0.04 Uiso calc U . R 1 . .
C C17 0.8299(3) 0.8474(5) 0.6157(3) 0.0306(11) Uani d . . . 1 . .
C C18 0.8904(3) 0.7649(5) 0.5746(3) 0.0374(12) Uani d . . . 1 . .
H H17 0.8869 0.7594 0.5197 0.045 Uiso calc U . R 1 . .
C C19 0.9560(3) 0.6906(5) 0.6148(4) 0.0446(14) Uani d . . . 1 . .
H H27 0.9971 0.6316 0.5877 0.054 Uiso calc U . R 1 . .
C C20 0.9617(4) 0.7026(5) 0.6940(4) 0.0435(14) Uani d . . . 1 . .
H H28 1.0069 0.6537 0.7226 0.052 Uiso calc U . R 1 . .
C C21 0.8998(3) 0.7876(5) 0.7309(3) 0.0353(13) Uani d . . . 1 . .
H H29 0.9033 0.7963 0.7857 0.042 Uiso calc U . R 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 O3 . 2.054(3) ?
Ni1 O1 . 2.055(4) ?
Ni1 N2 . 2.070(4) ?
Ni1 N3 . 2.072(4) ?
Ni1 O2 . 2.112(3) ?
Ni1 N1 . 2.230(4) ?
O1 H1A . 0.88(7) ?
O1 H1B . 0.80(7) ?
O2 H2A . 0.95(8) ?
O2 H2B . 0.95(7) ?
O3 C1 . 1.263(6) ?
O4 C1 . 1.251(6) ?
O5 C4 . 1.259(6) ?
O6 C4 . 1.253(6) ?
O7 H7B . 0.8501 ?
O7 H7A . 0.8499 ?
O8 H8A . 0.8503 ?
O8 H8B . 0.8499 ?
O9 H9B . 0.85 ?
O9 H9A . 0.85 ?
N1 C10 . 1.485(6) ?
N1 C16 . 1.495(6) ?
N1 C6 . 1.537(6) ?
N2 C17 . 1.336(6) ?
N2 C21 . 1.346(6) ?
N3 C15 . 1.332(6) ?
N3 C11 . 1.348(6) ?
C1 C2 . 1.504(7) ?
C2 C3 . 1.491(7) ?
C2 H2D . 0.99 ?
C2 H2C . 0.99 ?
C3 C4 . 1.512(7) ?
C3 H3C . 0.99 ?
C3 H3D . 0.99 ?
C6 C9 . 1.524(7) ?
C6 C8 . 1.525(7) ?
C6 C7 . 1.544(7) ?
C7 H24 . 0.98 ?
C7 H23 . 0.98 ?
C7 H22 . 0.98 ?
C8 H20 . 0.98 ?
C8 H19 . 0.98 ?
C8 H21 . 0.98 ?
C9 H26 . 0.98 ?
C9 H11A . 0.98 ?
C9 H25 . 0.98 ?
C10 C11 . 1.498(7) ?
C10 H10B . 0.99 ?
C10 H18 . 0.99 ?
C11 C12 . 1.378(7) ?
C12 C13 . 1.382(8) ?
C12 H11 . 0.95 ?
C13 C14 . 1.368(8) ?
C13 H12 . 0.95 ?
C14 C15 . 1.379(7) ?
C14 H13 . 0.95 ?
C15 H14 . 0.95 ?
C16 C17 . 1.495(7) ?
C16 H16B . 0.99 ?
C16 H16A . 0.99 ?
C17 C18 . 1.385(7) ?
C18 C19 . 1.383(7) ?
C18 H17 . 0.95 ?
C19 C20 . 1.373(8) ?
C19 H27 . 0.95 ?
C20 C21 . 1.376(7) ?
C20 H28 . 0.95 ?
C21 H29 . 0.95 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 Ni1 O1 . . 88.75(16) ?
O3 Ni1 N2 . . 87.75(14) ?
O1 Ni1 N2 . . 173.32(16) ?
O3 Ni1 N3 . . 175.84(15) ?
O1 Ni1 N3 . . 87.16(16) ?
N2 Ni1 N3 . . 96.24(15) ?
O3 Ni1 O2 . . 90.38(14) ?
O1 Ni1 O2 . . 89.90(15) ?
N2 Ni1 O2 . . 95.81(15) ?
N3 Ni1 O2 . . 90.39(15) ?
O3 Ni1 N1 . . 100.58(13) ?
O1 Ni1 N1 . . 94.74(14) ?
N2 Ni1 N1 . . 80.32(14) ?
N3 Ni1 N1 . . 79.00(14) ?
O2 Ni1 N1 . . 168.17(14) ?
Ni1 O1 H1A . . 118.(4) ?
Ni1 O1 H1B . . 113.(5) ?
H1A O1 H1B . . 112.(6) ?
Ni1 O2 H2A . . 111.(5) ?
Ni1 O2 H2B . . 100.(4) ?
H2A O2 H2B . . 107.(6) ?
C1 O3 Ni1 . . 131.0(3) ?
H7B O7 H7A . . 109.5 ?
H8A O8 H8B . . 109.5 ?
H9B O9 H9A . . 88.7 ?
C10 N1 C16 . . 107.9(4) ?
C10 N1 C6 . . 110.5(4) ?
C16 N1 C6 . . 111.6(4) ?
C10 N1 Ni1 . . 101.1(3) ?
C16 N1 Ni1 . . 104.5(3) ?
C6 N1 Ni1 . . 120.1(3) ?
C17 N2 C21 . . 118.6(4) ?
C17 N2 Ni1 . . 115.9(3) ?
C21 N2 Ni1 . . 124.6(3) ?
C15 N3 C11 . . 118.8(4) ?
C15 N3 Ni1 . . 126.9(3) ?
C11 N3 Ni1 . . 114.1(3) ?
O4 C1 O3 . . 125.0(4) ?
O4 C1 C2 . . 119.9(4) ?
O3 C1 C2 . . 115.0(4) ?
C3 C2 C1 . . 117.1(5) ?
C3 C2 H2D . . 108.0 ?
C1 C2 H2D . . 108.0 ?
C3 C2 H2C . . 108.0 ?
C1 C2 H2C . . 108.0 ?
H2D C2 H2C . . 107.3 ?
C2 C3 C4 . . 114.0(5) ?
C2 C3 H3C . . 108.7 ?
C4 C3 H3C . . 108.7 ?
C2 C3 H3D . . 108.7 ?
C4 C3 H3D . . 108.7 ?
H3C C3 H3D . . 107.6 ?
O6 C4 O5 . . 123.6(5) ?
O6 C4 C3 . . 118.7(5) ?
O5 C4 C3 . . 117.7(5) ?
C9 C6 C8 . . 109.6(4) ?
C9 C6 N1 . . 112.2(4) ?
C8 C6 N1 . . 109.7(4) ?
C9 C6 C7 . . 109.4(4) ?
C8 C6 C7 . . 107.6(4) ?
N1 C6 C7 . . 108.2(4) ?
C6 C7 H24 . . 109.5 ?
C6 C7 H23 . . 109.5 ?
H24 C7 H23 . . 109.5 ?
C6 C7 H22 . . 109.5 ?
H24 C7 H22 . . 109.5 ?
H23 C7 H22 . . 109.5 ?
C6 C8 H20 . . 109.5 ?
C6 C8 H19 . . 109.5 ?
H20 C8 H19 . . 109.5 ?
C6 C8 H21 . . 109.5 ?
H20 C8 H21 . . 109.5 ?
H19 C8 H21 . . 109.5 ?
C6 C9 H26 . . 109.5 ?
C6 C9 H11A . . 109.5 ?
H26 C9 H11A . . 109.5 ?
C6 C9 H25 . . 109.5 ?
H26 C9 H25 . . 109.5 ?
H11A C9 H25 . . 109.5 ?
N1 C10 C11 . . 112.2(4) ?
N1 C10 H10B . . 109.2 ?
C11 C10 H10B . . 109.2 ?
N1 C10 H18 . . 109.2 ?
C11 C10 H18 . . 109.2 ?
H10B C10 H18 . . 107.9 ?
N3 C11 C12 . . 121.6(5) ?
N3 C11 C10 . . 116.2(4) ?
C12 C11 C10 . . 122.2(5) ?
C11 C12 C13 . . 118.7(5) ?
C11 C12 H11 . . 120.6 ?
C13 C12 H11 . . 120.6 ?
C14 C13 C12 . . 119.9(5) ?
C14 C13 H12 . . 120.1 ?
C12 C13 H12 . . 120.1 ?
C13 C14 C15 . . 118.3(5) ?
C13 C14 H13 . . 120.8 ?
C15 C14 H13 . . 120.8 ?
N3 C15 C14 . . 122.7(5) ?
N3 C15 H14 . . 118.7 ?
C14 C15 H14 . . 118.7 ?
C17 C16 N1 . . 112.8(4) ?
C17 C16 H16B . . 109.0 ?
N1 C16 H16B . . 109.0 ?
C17 C16 H16A . . 109.0 ?
N1 C16 H16A . . 109.0 ?
H16B C16 H16A . . 107.8 ?
N2 C17 C18 . . 121.6(5) ?
N2 C17 C16 . . 116.7(4) ?
C18 C17 C16 . . 121.6(5) ?
C19 C18 C17 . . 119.0(5) ?
C19 C18 H17 . . 120.5 ?
C17 C18 H17 . . 120.5 ?
C20 C19 C18 . . 119.7(5) ?
C20 C19 H27 . . 120.2 ?
C18 C19 H27 . . 120.2 ?
C19 C20 C21 . . 118.1(5) ?
C19 C20 H28 . . 121.0 ?
C21 C20 H28 . . 121.0 ?
N2 C21 C20 . . 123.0(5) ?
N2 C21 H29 . . 118.5 ?
C20 C21 H29 . . 118.5 ?


#===END

_database_code_depnum_ccdc_archive 'CCDC 965632'
