data_NI(GLU)

_publ_requested_journal           '?'
_audit_creation_method            SHELXL-97
_chemical_formula_moiety          'C5 H9 N Ni O5, H2 O'
_chemical_formula_sum             'C5 H11 N Ni O6'
_chemical_formula_weight          239.86
_chemical_melting_point           ?
_chemical_name_common             'Ni(Glu)'
_chemical_name_systematic         'Ni(Glu)'
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 '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'
 'Ni' 'Ni' 0.3393 1.1124 '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'

_symmetry_cell_setting            'Orthorhombic'
_symmetry_space_group_name_H-M    'P 21 21 21'
_symmetry_space_group_name_Hall   'P 2ac 2ab'
loop_
  _symmetry_equiv_pos_as_xyz
 'x+1/2, -y+1/2, -z'
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z+1/2'

_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_formula_units_Z             4
_cell_length_a                    7.1385(14)
_cell_length_b                    10.343(2)
_cell_length_c                    11.135(2)
_cell_measurement_reflns_used     0
_cell_measurement_temperature     100(2)
_cell_measurement_theta_max       0.0
_cell_measurement_theta_min       0.0
_cell_volume                      822.2(3)
_exptl_absorpt_coefficient_mu     2.359
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_type    ?
_exptl_absorpt_process_details    ?
_exptl_crystal_F_000              496
_exptl_crystal_colour             Green
_exptl_crystal_colour_lustre      clear
_exptl_crystal_colour_primary     green
_exptl_crystal_density_diffrn     1.938
_exptl_crystal_density_meas       0.0
_exptl_crystal_density_method     'not measured'
_exptl_crystal_description        prism
_exptl_crystal_size_max           0.1
_exptl_crystal_size_mid           0.1
_exptl_crystal_size_min           0.1
_exptl_special_details            '?'
_diffrn_ambient_temperature       100.0
_diffrn_detector_area_resol_mean  8.0
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type   'Bruker APEX-I CCD'
_diffrn_measurement_method        'ω scans'
_diffrn_radiation_monochromator   graphite
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_type            'MO K\a'
_diffrn_radiation_wavelength      0.71073
_diffrn_reflns_av_R_equivalents   0.0364
_diffrn_reflns_av_sigmaI/netI     0.0709
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_h_min        -8
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_l_max        14
_diffrn_reflns_limit_l_min        -12
_diffrn_reflns_number             4322
_diffrn_reflns_theta_full         27.92
_diffrn_reflns_theta_max          27.92
_diffrn_reflns_theta_min          2.69
_diffrn_source                    'sealed tube'
_diffrn_source_current            35.0
_diffrn_source_power              1.575
_diffrn_source_voltage            45.0
_diffrn_standards_decay_%         ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_number          ?
_reflns_number_gt                 1613
_reflns_number_total              1858
_reflns_threshold_expression      >2sigma(I)
_computing_cell_refinement        'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection        'SMART'
_computing_data_reduction         'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics     
;
 OLEX2: a complete structure solution, refinement and analysis program.
 Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material   
;
 OLEX2: a complete structure solution, refinement and analysis program.
 Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max          0.483
_refine_diff_density_min          -0.381
_refine_diff_density_rms          0.070
_refine_ls_R_factor_all           0.0305
_refine_ls_R_factor_gt            0.0257
_refine_ls_abs_structure_Flack    -0.002(13)
_refine_ls_abs_structure_details  'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_coef        ?
_refine_ls_extinction_method      none
_refine_ls_goodness_of_fit_ref    0.785
_refine_ls_hydrogen_treatment     refall
_refine_ls_matrix_type            full
_refine_ls_number_parameters      162
_refine_ls_number_reflns          1858
_refine_ls_number_restraints      0
_refine_ls_restrained_S_all       0.785
_refine_ls_shift/su_max           1.351
_refine_ls_shift/su_mean          0.008
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_wR_factor_gt           0.0363
_refine_ls_wR_factor_ref          0.0368
_refine_ls_weighting_details      
;
calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme       calc
_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.
;
_atom_sites_solution_hydrogens    geom
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
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
 Ni1 Ni 0.89196(5) 0.43441(3) 0.03909(3) 0.00911(8) Uani 1 1 d . . .
 O1 O 1.0225(2) 0.25999(16) 0.02293(17) 0.0090(4) Uani 1 1 d . . .
 O5W O 0.7983(3) 0.61793(18) 0.0307(2) 0.0170(5) Uani 1 1 d . . .
 O3 O 1.4964(2) 0.53511(17) -0.29217(15) 0.0109(4) Uani 1 1 d . . .
 C5 C 1.3490(4) 0.4773(2) -0.3286(2) 0.0118(7) Uani 1 1 d . . .
 O2 O 0.6452(2) 0.37401(15) 0.11382(15) 0.0121(4) Uani 1 1 d . . .
 O4 O 1.3188(2) 0.46597(15) -0.44100(16) 0.0131(5) Uani 1 1 d . . .
 N1 N 0.8205(4) 0.3929(2) -0.1363(2) 0.0111(6) Uani 1 1 d . . .
 C1 C 1.0408(4) 0.2187(2) -0.0832(2) 0.0090(6) Uani 1 1 d . . .
 C2 C 0.9341(4) 0.2849(2) -0.1846(2) 0.0099(7) Uani 1 1 d . . .
 C4 C 1.2178(4) 0.4239(3) -0.2345(2) 0.0127(6) Uani 1 1 d . . .
 C3 C 1.0701(4) 0.3323(3) -0.2821(3) 0.0114(7) Uani 1 1 d . . .
 O6W O 0.4618(3) 0.6493(2) -0.0763(2) 0.0140(5) Uani 1 1 d . . .
 H3B H 1.131(3) 0.249(2) -0.3217(18) 0.003(6) Uiso 1 1 d . . .
 H3A H 0.995(4) 0.371(3) -0.341(2) 0.017(8) Uiso 1 1 d . . .
 H5WA H 0.701(4) 0.634(2) 0.000(2) 0.018(10) Uiso 1 1 d . . .
 H6WA H 0.404(4) 0.614(2) -0.038(2) 0.011(9) Uiso 1 1 d . . .
 H1B H 0.809(3) 0.454(2) -0.181(2) 0.003(8) Uiso 1 1 d . . .
 H4A H 1.166(3) 0.504(2) -0.189(2) 0.020(8) Uiso 1 1 d . . .
 H1A H 0.689(4) 0.368(2) -0.120(2) 0.014(8) Uiso 1 1 d . . .
 H6WB H 0.469(5) 0.607(3) -0.137(3) 0.050(14) Uiso 1 1 d . . .
 H5WB H 0.864(5) 0.681(3) 0.047(3) 0.061(12) Uiso 1 1 d . . .
 H4B H 1.300(4) 0.377(2) -0.166(2) 0.025(8) Uiso 1 1 d . . .
 H2 H 0.858(3) 0.2233(19) -0.223(2) 0.000(6) Uiso 1 1 d . . .

loop_
  _atom_site_aniso_label
  _atom_site_aniso_U_11
  _atom_site_aniso_U_22
  _atom_site_aniso_U_33
  _atom_site_aniso_U_23
  _atom_site_aniso_U_13
  _atom_site_aniso_U_12
 Ni1 0.00831(16) 0.01018(14) 0.00883(15) -0.00008(17) 0.00005(17) -0.00032(16)
 O1 0.0096(10) 0.0108(9) 0.0067(10) 0.0001(9) -0.0010(9) 0.0032(7)
 O5W 0.0102(11) 0.0121(10) 0.0288(13) -0.0005(11) -0.0066(12) -0.0001(8)
 O3 0.0089(11) 0.0158(11) 0.0079(9) -0.0003(8) -0.0009(8) -0.0037(8)
 C5 0.0119(18) 0.0095(13) 0.0141(16) 0.0012(11) 0.0015(12) 0.0041(11)
 O2 0.0110(11) 0.0119(9) 0.0133(10) -0.0018(8) 0.0007(9) -0.0015(8)
 O4 0.0115(10) 0.0161(10) 0.0118(11) 0.0000(8) 0.0006(8) -0.0007(7)
 N1 0.0113(14) 0.0115(13) 0.0106(14) 0.0039(11) -0.0003(11) 0.0037(10)
 C1 0.0071(14) 0.0053(13) 0.0145(15) 0.0000(11) 0.0005(12) -0.0028(11)
 C2 0.0077(17) 0.0083(14) 0.0138(16) -0.0029(12) -0.0004(12) -0.0025(11)
 C4 0.0111(15) 0.0161(16) 0.0111(14) 0.0004(14) -0.0013(12) -0.0033(14)
 C3 0.0100(18) 0.0163(15) 0.0079(14) 0.0024(13) -0.0004(12) -0.0006(12)
 O6W 0.0145(12) 0.0145(11) 0.0131(13) 0.0006(10) 0.0012(10) -0.0019(9)

_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
 Ni1 O1 2.0386(17) . ?
 Ni1 O5W 2.0147(19) . ?
 Ni1 O3 2.0651(17) 2_765 ?
 Ni1 O2 2.0460(18) . ?
 Ni1 O4 2.3181(16) 2_765 ?
 Ni1 N1 2.064(2) . ?
 O1 C1 1.264(3) . ?
 O5W H5WA 0.79(3) . ?
 O5W H5WB 0.82(3) . ?
 O3 Ni1 2.0650(17) 2_764 ?
 O3 C5 1.276(3) . ?
 C5 O4 1.276(3) . ?
 C5 C4 1.510(4) . ?
 O2 C1 1.261(3) 3_455 ?
 O4 Ni1 2.3181(16) 2_764 ?
 N1 C2 1.482(3) . ?
 N1 H1B 0.81(2) . ?
 N1 H1A 0.99(3) . ?
 C1 O2 1.261(3) 3 ?
 C1 C2 1.524(4) . ?
 C2 C3 1.537(3) . ?
 C2 H2 0.94(2) . ?
 C4 C3 1.514(4) . ?
 C4 H4A 1.03(2) . ?
 C4 H4B 1.08(3) . ?
 C3 H3B 1.06(2) . ?
 C3 H3A 0.94(2) . ?
 O6W H6WA 0.70(3) . ?
 O6W H6WB 0.81(3) . ?

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
 Ni1 O5W H5WA 120.4(19) . . ?
 Ni1 O5W H5WB 123(2) . . ?
 Ni1 N1 H1B 116.9(17) . . ?
 Ni1 N1 H1A 96.3(15) . . ?
 O1 Ni1 O3 92.23(7) . 2_765 ?
 O1 Ni1 O2 99.17(7) . . ?
 O1 Ni1 O4 89.69(6) . 2_765 ?
 O1 Ni1 N1 81.11(8) . . ?
 O1 C1 C2 119.3(2) . . ?
 O5W Ni1 O1 168.94(9) . . ?
 O5W Ni1 O3 91.52(8) . 2_765 ?
 O5W Ni1 O2 91.19(8) . . ?
 O5W Ni1 O4 83.18(8) . 2_765 ?
 O5W Ni1 N1 94.01(10) . . ?
 O3 Ni1 O4 60.09(6) 2_765 2_765 ?
 O3 C5 C4 117.5(2) . . ?
 C5 O3 Ni1 95.77(16) . 2_764 ?
 C5 O4 Ni1 84.40(15) . 2_764 ?
 C5 C4 C3 114.7(2) . . ?
 C5 C4 H4A 105.5(14) . . ?
 C5 C4 H4B 108.6(14) . . ?
 O2 Ni1 O3 90.51(7) . 2_765 ?
 O2 Ni1 O4 149.74(7) . 2_765 ?
 O2 Ni1 N1 96.23(9) . . ?
 O2 C1 O1 124.8(2) 3 . ?
 O2 C1 C2 115.9(2) 3 . ?
 O4 C5 O3 119.6(2) . . ?
 O4 C5 C4 122.8(2) . . ?
 N1 Ni1 O3 171.18(9) . 2_765 ?
 N1 Ni1 O4 113.77(8) . 2_765 ?
 N1 C2 C1 110.1(2) . . ?
 N1 C2 C3 111.2(2) . . ?
 N1 C2 H2 111.3(13) . . ?
 C1 O1 Ni1 115.38(16) . . ?
 C1 O2 Ni1 129.13(17) 3_455 . ?
 C1 C2 C3 110.5(2) . . ?
 C1 C2 H2 108.7(13) . . ?
 C2 N1 Ni1 111.42(17) . . ?
 C2 N1 H1B 114.5(17) . . ?
 C2 N1 H1A 112.8(14) . . ?
 C2 C3 H3B 107.2(12) . . ?
 C2 C3 H3A 105.5(17) . . ?
 C4 C3 C2 113.1(2) . . ?
 C4 C3 H3B 111.4(12) . . ?
 C4 C3 H3A 112.0(17) . . ?
 C3 C2 H2 104.9(14) . . ?
 C3 C4 H4A 114.8(14) . . ?
 C3 C4 H4B 110.3(14) . . ?
 H3B C3 H3A 107.2(19) . . ?
 H5WA O5W H5WB 116(3) . . ?
 H6WA O6W H6WB 106(3) . . ?
 H1B N1 H1A 103(2) . . ?
 H4A C4 H4B 102.0(18) . . ?

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
 Ni1 O1 C1 O2 166.73(19) . . . 3 ?
 Ni1 O1 C1 C2 -12.0(3) . . . . ?
 Ni1 O3 C5 O4 -3.6(2) 2_764 . . . ?
 Ni1 O3 C5 C4 175.9(2) 2_764 . . . ?
 Ni1 N1 C2 C1 11.7(3) . . . . ?
 Ni1 N1 C2 C3 -111.2(2) . . . . ?
 O1 Ni1 O2 C1 -46.5(2) . . . 3_455 ?
 O1 Ni1 N1 C2 -13.81(17) . . . . ?
 O1 C1 C2 N1 -0.1(3) . . . . ?
 O1 C1 C2 C3 123.2(3) . . . . ?
 O5W Ni1 O1 C1 -49.9(5) . . . . ?
 O5W Ni1 O2 C1 129.6(2) . . . 3_455 ?
 O5W Ni1 N1 C2 156.19(18) . . . . ?
 O3 Ni1 O1 C1 -159.62(19) 2_765 . . . ?
 O3 Ni1 O2 C1 -138.8(2) 2_765 . . 3_455 ?
 O3 Ni1 N1 C2 27.5(7) 2_765 . . . ?
 O3 C5 O4 Ni1 3.2(2) . . . 2_764 ?
 O3 C5 C4 C3 -167.3(2) . . . . ?
 C5 C4 C3 C2 -177.4(2) . . . . ?
 O2 Ni1 O1 C1 109.50(19) . . . . ?
 O2 Ni1 N1 C2 -112.16(18) . . . . ?
 O2 C1 C2 N1 -178.9(2) 3 . . . ?
 O2 C1 C2 C3 -55.7(3) 3 . . . ?
 O4 Ni1 O1 C1 -99.57(19) 2_765 . . . ?
 O4 Ni1 O2 C1 -151.91(18) 2_765 . . 3_455 ?
 O4 Ni1 N1 C2 71.89(19) 2_765 . . . ?
 O4 C5 C4 C3 12.2(4) . . . . ?
 N1 Ni1 O1 C1 14.56(19) . . . . ?
 N1 Ni1 O2 C1 35.5(2) . . . 3_455 ?
 N1 C2 C3 C4 65.2(3) . . . . ?
 C1 C2 C3 C4 -57.4(3) . . . . ?
 C4 C5 O4 Ni1 -176.3(2) . . . 2_764 ?

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
 O5W H5WA O6W 0.79(3) 1.92(3) 2.701(3) 173(3) .
 O5W H5WB O6W 0.82(3) 1.92(3) 2.723(3) 165(3) 3_565
 O6W H6WA O4 0.70(3) 2.09(3) 2.776(3) 167(3) 2_665
 O6W H6WB O3 0.81(3) 1.89(3) 2.689(3) 170(3) 1_455