data_global
_audit_creation_method                  'APEX2 v2010.11-3'

_publ_requested_journal                 ?

_publ_contact_author_name               ?
_publ_contact_author_address            
;
;
_publ_contact_author_email              ?
_publ_contact_author_fax                ?
_publ_contact_author_phone              ?

_publ_section_title                     
;
;
_publ_section_abstract                  
;
;
_publ_section_references                
;
;
_publ_section_comment                   
;
;

data_1
_chemical_name_systematic               ?
_chemical_name_common                   [Ni2(Hhissal)2(adi)(H2O)2].8H2O
_chemical_formula_moiety                'C32 H40 N6 Ni2 O12, 8(H2 O)'
_chemical_formula_sum                   'C32 H56 N6 Ni2 O20'
_chemical_formula_iupac                 ?
_chemical_formula_weight                962.25
_chemical_absolute_configuration        rmad

_chemical_melting_point                 ?

_space_group_crystal_system             monoclinic
_space_group_name_H-M_alt               'C 2'
_space_group_name_Hall                  'C 2y'
loop_
    _space_group_symop_operation_xyz
    'x, y, z'
    '-x, y, -z'
    'x+1/2, y+1/2, z'
    '-x+1/2, y+1/2, -z'

_cell_length_a                          20.1803(8)
_cell_length_b                          6.2496(3)
_cell_length_c                          17.1447(8)
_cell_angle_alpha                       90
_cell_angle_beta                        100.701(2)
_cell_angle_gamma                       90
_cell_volume                            2124.67(17)
_cell_formula_units_Z                   2
_cell_measurement_reflns_used           3126
_cell_measurement_theta_min             2.4179
_cell_measurement_theta_max             24.6851
_cell_measurement_temperature           296.(2)

_exptl_crystal_description              block
_exptl_crystal_colour                   'clear blue'
_exptl_crystal_size_max                 0.20
_exptl_crystal_size_mid                 0.18
_exptl_crystal_size_min                 0.15
_exptl_crystal_density_diffrn           1.504
_exptl_crystal_density_meas             ?
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    1012

_exptl_absorpt_coefficient_mu           0.971
_exptl_absorpt_correction_type          multi-scan
_exptl_absorpt_process_details          'SADABS V2008/1 (Bruker AXS)'
_exptl_absorpt_correction_T_min         0.6117
_exptl_absorpt_correction_T_max         0.7452

_exptl_special_details                  
;
; 

_diffrn_ambient_temperature             296.(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                   7998
_diffrn_reflns_av_R_equivalents         0.0311
_diffrn_reflns_av_sigmaI/netI           0.0494
_diffrn_reflns_theta_min                1.21
_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              -23
_diffrn_reflns_limit_h_max              24
_diffrn_reflns_limit_k_min              -7
_diffrn_reflns_limit_k_max              5
_diffrn_reflns_limit_l_min              -13
_diffrn_reflns_limit_l_max              20

_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                    3141
_reflns_number_gt                       2819
_reflns_threshold_expression            >2sigma(I)

_refine_ls_structure_factor_coef        Fsqd
_refine_ls_matrix_type                  full
_refine_ls_R_factor_all                 0.0510
_refine_ls_R_factor_gt                  0.0431
_refine_ls_wR_factor_gt                 0.1181
_refine_ls_wR_factor_ref                0.1306
_refine_ls_goodness_of_fit_ref          1.029
_refine_ls_restrained_S_all             1.027
_refine_ls_number_reflns                3141
_refine_ls_number_parameters            284
_refine_ls_number_restraints            19
_refine_ls_hydrogen_treatment           mixed
_refine_ls_weighting_scheme             calc
_refine_ls_weighting_details
    'calc w=1/[σ²(Fo²)+(0.0951P)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                0.689
_refine_diff_density_min                -0.407
_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          0.02(2)

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 V2011.4-1 (Bruker AXS)'
_computing_cell_refinement              'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_data_reduction               'SAINT V8.30C (Bruker AXS Inc., 2013)'
_computing_structure_solution           'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement         'SHELXL-2013 (Sheldrick, 2013)'
_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 0.25596(3) 0.74638(11) 0.80446(3) 0.02080(19) Uani d D 1 . .
    O O1 0.22051(17) 1.0609(6) 0.8026(2) 0.0232(8) Uani d . 1 . .
    O O2 0.12404(17) 1.2429(8) 0.7808(2) 0.0371(8) Uani d . 1 . .
    O O3 0.29122(18) 0.8085(6) 0.69700(19) 0.0273(9) Uani d D 1 . .
    O O4 0.34998(17) 0.8175(6) 0.8680(2) 0.0276(9) Uani d . 1 . .
    O O5 0.40733(19) 0.9210(7) 0.7753(2) 0.0339(9) Uani d . 1 . .
    O O6 0.2908(2) 0.4383(6) 0.8009(3) 0.0361(10) Uani d D 1 . .
    O O7 0.4180(2) 0.3725(9) 0.7778(3) 0.0516(12) Uiso d D 1 . .
    O O8 0.5035(3) 0.8420(12) 0.6860(4) 0.0823(19) Uiso d D 1 . .
    O O9 0.4339(5) 0.4928(17) 0.6332(5) 0.128(3) Uiso d D 1 . .
    O O10 0.4674(5) 0.1231(16) 0.5628(5) 0.125(3) Uiso d D 1 . .    
    N N1 0.1608(2) 0.6963(6) 0.7402(2) 0.0232(11) Uani d . 1 . .
    H H1 0.1466 0.566 0.7544 0.028 Uiso calc R 1 . .
    N N2 0.2121(2) 0.6685(8) 1.0312(3) 0.0323(11) Uani d . 1 . .
    H H2 0.224 0.6458 1.0813 0.039 Uiso calc R 1 . .
    N N3 0.2180(2) 0.7034(7) 0.9055(2) 0.0244(11) Uani d . 1 . .
    C C1 0.1562(3) 1.0726(9) 0.7841(3) 0.0251(12) Uani d . 1 . .
    C C2 0.1183(2) 0.8599(8) 0.7688(3) 0.0227(11) Uani d . 1 . .
    H H2A 0.0782 0.8829 0.7276 0.027 Uiso calc R 1 . .
    C C3 0.1561(3) 0.6956(9) 0.6516(3) 0.0334(15) Uani d . 1 . .
    H H3B 0.1092 0.6814 0.6262 0.04 Uiso calc R 1 . .
    H H3A 0.1802 0.5723 0.6368 0.04 Uiso calc R 1 . .
    C C4 0.1848(3) 0.8956(10) 0.6214(3) 0.0303(13) Uani d . 1 . .
    C C5 0.1436(3) 1.0326(11) 0.5681(3) 0.0395(15) Uani d . 1 . .
    H H5 0.0976 1.0054 0.5533 0.047 Uiso calc R 1 . .
    C C6 0.1724(3) 1.2101(12) 0.5378(3) 0.0430(18) Uani d . 1 . .
    H H6 0.1452 1.2999 0.5021 0.052 Uiso calc R 1 . .
    C C7 0.2399(3) 1.2550(13) 0.5595(3) 0.0383(13) Uani d . 1 . .
    H H7 0.2584 1.3739 0.5389 0.046 Uiso calc R 1 . .
    C C8 0.2801(3) 1.1191(10) 0.6129(3) 0.0356(14) Uani d . 1 . .
    H H8 0.3259 1.1481 0.6282 0.043 Uiso calc R 1 . .
    C C9 0.2531(3) 0.9439(10) 0.6429(3) 0.0297(13) Uani d D 1 . .
    C C10 0.0954(3) 0.7810(10) 0.8437(3) 0.0306(14) Uani d . 1 . .
    H H10B 0.0694 0.6511 0.8309 0.037 Uiso calc R 1 . .
    H H10A 0.0656 0.8875 0.8596 0.037 Uiso calc R 1 . .
    C C11 0.1518(2) 0.7349(12) 0.9145(3) 0.0255(10) Uani d . 1 . .
    C C12 0.1485(3) 0.7158(11) 0.9919(3) 0.0331(13) Uani d . 1 . .
    H H12 0.1103 0.7317 1.0144 0.04 Uiso calc R 1 . .
    C C13 0.2524(3) 0.6638(9) 0.9777(3) 0.0299(13) Uani d . 1 . .
    H H13 0.2985 0.6364 0.9895 0.036 Uiso calc R 1 . .
    C C14 0.4033(3) 0.8596(8) 0.8453(3) 0.0252(12) Uani d . 1 . .
    C C15 0.4686(3) 0.8468(11) 0.9061(3) 0.0354(14) Uani d . 1 . .
    H H15A 0.5057 0.821 0.8785 0.042 Uiso calc R 1 . .
    H H15B 0.4765 0.9835 0.933 0.042 Uiso calc R 1 . .
    C C16 0.4682(3) 0.6738(10) 0.9671(3) 0.0343(14) Uani d . 1 . .
    H H16A 0.4644 0.5359 0.9407 0.041 Uiso calc R 1 . .
    H H16B 0.4288 0.6921 0.9914 0.041 Uiso calc R 1 . .
    H H3 0.303(3) 0.704(6) 0.6707(16) 0.051 Uiso d D 1 . .
    H H10D 0.5031(19) 0.054(8) 0.586(3) 0.051 Uiso d D 1 . .
    H H10C 0.440(2) 0.038(7) 0.533(3) 0.051 Uiso d D 1 . .
    H H6B 0.276(3) 0.359(6) 0.835(2) 0.051 Uiso d D 1 . .
    H H6A 0.280(3) 0.387(6) 0.7541(10) 0.051 Uiso d D 1 . .
    H H7B 0.445(3) 0.448(9) 0.812(2) 0.051 Uiso d D 1 . .
    H H7A 0.415(3) 0.426(9) 0.7313(14) 0.051 Uiso d D 1 . .
    H H8B 0.539(2) 0.881(9) 0.720(3) 0.051 Uiso d D 1 . .
    H H8A 0.493(3) 0.711(4) 0.694(3) 0.051 Uiso d D 1 . .
    H H9B 0.455(2) 0.452(11) 0.597(2) 0.051 Uiso d D 1 . .
    H H9A 0.3929(13) 0.527(11) 0.613(3) 0.051 Uiso d 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 . 2.037(4) ?
    Ni1 N1 . 2.053(4) ?
    Ni1 O4 . 2.053(3) ?
    Ni1 O6 . 2.054(4) ?
    Ni1 O1 . 2.090(4) ?
    Ni1 O3 . 2.130(3) ?
    O1 C1 . 1.280(6) ?
    O2 C1 . 1.242(7) ?
    O3 C9 . 1.380(7) ?
    O3 H3 . 0.852(10) ?
    O4 C14 . 1.239(6) ?
    O5 C14 . 1.278(6) ?
    O6 H6B . 0.855(10) ?
    O6 H6A . 0.853(10) ?
    O7 H7B . 0.856(10) ?
    O7 H7A . 0.858(10) ?
    O8 H8B . 0.863(10) ?
    O8 H8A . 0.864(10) ?
    O9 H9B . 0.863(10) ?
    O9 H9A . 0.862(10) ?
    O10 H10D . 0.868(10) ?
    O10 H10C . 0.861(10) ?
    N1 C2 . 1.475(6) ?
    N1 C3 . 1.505(6) ?
    N1 H1 . 0.91 ?
    N2 C13 . 1.334(7) ?
    N2 C12 . 1.366(7) ?
    N2 H2 . 0.86 ?
    N3 C13 . 1.325(7) ?
    N3 C11 . 1.388(6) ?
    C1 C2 . 1.531(7) ?
    C2 C10 . 1.526(7) ?
    C2 H2A . 0.98 ?
    C3 C4 . 1.508(8) ?
    C3 H3B . 0.97 ?
    C3 H3A . 0.97 ?
    C4 C9 . 1.393(8) ?
    C4 C5 . 1.406(8) ?
    C5 C6 . 1.397(10) ?
    C5 H5 . 0.93 ?
    C6 C7 . 1.372(9) ?
    C6 H6 . 0.93 ?
    C7 C8 . 1.394(9) ?
    C7 H7 . 0.93 ?
    C8 C9 . 1.365(9) ?
    C8 H8 . 0.93 ?
    C10 C11 . 1.527(7) ?
    C10 H10B . 0.97 ?
    C10 H10A . 0.97 ?
    C11 C12 . 1.347(7) ?
    C12 H12 . 0.93 ?
    C13 H13 . 0.93 ?
    C14 C15 . 1.522(7) ?
    C15 C16 . 1.505(8) ?
    C15 H15A . 0.97 ?
    C15 H15B . 0.97 ?
    C16 C16 2_657 1.543(10) ?
    C16 H16A . 0.97 ?
    C16 H16B . 0.97 ?

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 N1 . . 88.51(16) ?
    N3 Ni1 O4 . . 91.92(15) ?
    N1 Ni1 O4 . . 176.27(16) ?
    N3 Ni1 O6 . . 94.95(17) ?
    N1 Ni1 O6 . . 97.61(16) ?
    O4 Ni1 O6 . . 86.04(16) ?
    N3 Ni1 O1 . . 87.41(16) ?
    N1 Ni1 O1 . . 81.48(14) ?
    O4 Ni1 O1 . . 94.84(14) ?
    O6 Ni1 O1 . . 177.45(16) ?
    N3 Ni1 O3 . . 176.25(17) ?
    N1 Ni1 O3 . . 89.63(15) ?
    O4 Ni1 O3 . . 89.73(14) ?
    O6 Ni1 O3 . . 88.53(16) ?
    O1 Ni1 O3 . . 89.09(14) ?
    C1 O1 Ni1 . . 112.7(3) ?
    C9 O3 Ni1 . . 117.3(3) ?
    C9 O3 H3 . . 107.(2) ?
    Ni1 O3 H3 . . 120.(4) ?
    C14 O4 Ni1 . . 130.6(3) ?
    Ni1 O6 H6B . . 111.(3) ?
    Ni1 O6 H6A . . 111.(3) ?
    H6B O6 H6A . . 111.(3) ?
    H7B O7 H7A . . 110.(3) ?
    H8B O8 H8A . . 111.(3) ?
    H9B O9 H9A . . 111.(3) ?
    H10D O10 H10C . . 110.(3) ?
    C2 N1 C3 . . 113.9(4) ?
    C2 N1 Ni1 . . 105.1(3) ?
    C3 N1 Ni1 . . 114.8(3) ?
    C2 N1 H1 . . 107.6 ?
    C3 N1 H1 . . 107.6 ?
    Ni1 N1 H1 . . 107.6 ?
    C13 N2 C12 . . 107.6(4) ?
    C13 N2 H2 . . 126.2 ?
    C12 N2 H2 . . 126.2 ?
    C13 N3 C11 . . 105.7(4) ?
    C13 N3 Ni1 . . 127.2(4) ?
    C11 N3 Ni1 . . 126.7(3) ?
    O2 C1 O1 . . 123.9(5) ?
    O2 C1 C2 . . 119.8(4) ?
    O1 C1 C2 . . 116.3(5) ?
    N1 C2 C10 . . 109.9(4) ?
    N1 C2 C1 . . 110.9(4) ?
    C10 C2 C1 . . 110.8(4) ?
    N1 C2 H2A . . 108.4 ?
    C10 C2 H2A . . 108.4 ?
    C1 C2 H2A . . 108.4 ?
    N1 C3 C4 . . 112.8(4) ?
    N1 C3 H3B . . 109.0 ?
    C4 C3 H3B . . 109.0 ?
    N1 C3 H3A . . 109.0 ?
    C4 C3 H3A . . 109.0 ?
    H3B C3 H3A . . 107.8 ?
    C9 C4 C5 . . 118.5(6) ?
    C9 C4 C3 . . 120.8(5) ?
    C5 C4 C3 . . 120.6(5) ?
    C6 C5 C4 . . 119.2(6) ?
    C6 C5 H5 . . 120.4 ?
    C4 C5 H5 . . 120.4 ?
    C7 C6 C5 . . 121.5(6) ?
    C7 C6 H6 . . 119.2 ?
    C5 C6 H6 . . 119.2 ?
    C6 C7 C8 . . 118.7(7) ?
    C6 C7 H7 . . 120.6 ?
    C8 C7 H7 . . 120.6 ?
    C9 C8 C7 . . 120.8(6) ?
    C9 C8 H8 . . 119.6 ?
    C7 C8 H8 . . 119.6 ?
    C8 C9 O3 . . 122.3(5) ?
    C8 C9 C4 . . 121.3(5) ?
    O3 C9 C4 . . 116.5(5) ?
    C2 C10 C11 . . 115.6(4) ?
    C2 C10 H10B . . 108.4 ?
    C11 C10 H10B . . 108.4 ?
    C2 C10 H10A . . 108.4 ?
    C11 C10 H10A . . 108.4 ?
    H10B C10 H10A . . 107.4 ?
    C12 C11 N3 . . 108.7(4) ?
    C12 C11 C10 . . 129.4(5) ?
    N3 C11 C10 . . 121.9(4) ?
    C11 C12 N2 . . 107.0(4) ?
    C11 C12 H12 . . 126.5 ?
    N2 C12 H12 . . 126.5 ?
    N3 C13 N2 . . 111.0(5) ?
    N3 C13 H13 . . 124.5 ?
    N2 C13 H13 . . 124.5 ?
    O4 C14 O5 . . 124.7(5) ?
    O4 C14 C15 . . 117.8(4) ?
    O5 C14 C15 . . 117.5(5) ?
    C16 C15 C14 . . 113.4(5) ?
    C16 C15 H15A . . 108.9 ?
    C14 C15 H15A . . 108.9 ?
    C16 C15 H15B . . 108.9 ?
    C14 C15 H15B . . 108.9 ?
    H15A C15 H15B . . 107.7 ?
    C15 C16 C16 . 2_657 113.4(4) ?
    C15 C16 H16A . . 108.9 ?
    C16 C16 H16A 2_657 . 108.9 ?
    C15 C16 H16B . . 108.9 ?
    C16 C16 H16B 2_657 . 108.9 ?
    H16A C16 H16B . . 107.7 ?
#===END
#
_vrf_PLAT420_1                   
;
PROBLEM: D-H Without Acceptor
RESPONSE: This could not be eliminated after numerous attempts; 
however, the geometrical parameters for this water molecule are correct.
;
