#------------------------------------------------------------------------------
#$Date: 2016-02-20 04:06:23 +0100 (Sat 20 de Feb de 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/27/2202758.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2202758
loop_
_publ_author_name
'Dai-Xi Li'
'Duan-Jun Xu'
'Yuan-Zhi Xu'
_publ_section_title
;
 Redetermination of bis(dimethylglyoximato-κ²N,N')nickel(II)
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1094
_journal_page_last               m1095
_journal_paper_doi               10.1107/S1600536803024656
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Ni (C4 H7 N2 O2)2]'
_chemical_formula_moiety         'C8 H14 N4 Ni O4'
_chemical_formula_sum            'C8 H14 N4 Ni O4'
_chemical_formula_weight         288.92
_chemical_name_systematic        ?
_space_group_IT_number           72
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2 2c'
_symmetry_space_group_name_H-M   'I b a m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.5752(17)
_cell_length_b                   10.4233(13)
_cell_length_c                   6.4744(14)
_cell_measurement_reflns_used    7201
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.3
_cell_volume                     1118.6(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-2 (Altomare et al., 1993)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_av_sigmaI/netI    0.013
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4806
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.3
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.745
_exptl_absorpt_correction_T_max  0.840
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.29
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     53
_refine_ls_number_reflns         705
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.038
_refine_ls_R_factor_gt           0.034
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0661P)²+1.2037P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.100
_refine_ls_wR_factor_ref         0.103
_reflns_number_gt                632
_reflns_number_total             705
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            na6262.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2202758
_cod_database_fobs_code          2202758
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z+1/2'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, y+1/2, -z+1'
'-x, -y, -z'
'x, y, -z'
'-x, y, z-1/2'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
loop_
_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
_atom_site_type_symbol
Ni 0.5000 0.5000 0.5000 0.0362(2) Uani d S 1 . . Ni
N1 0.50997(16) 0.6779(3) 0.5000 0.0418(6) Uani d S 1 . . N
N2 0.61203(19) 0.5078(2) 0.5000 0.0423(6) Uani d S 1 . . N
O1 0.44664(15) 0.7593(3) 0.5000 0.0537(6) Uani d S 1 . . O
O2 0.66005(15) 0.4043(2) 0.5000 0.0517(6) Uani d S 1 . . O
C1 0.6012(3) 0.8624(4) 0.5000 0.0659(11) Uani d S 1 . . C
H1A 0.5518 0.9105 0.5000 0.099 Uiso calc SR 1 . . H
H1B 0.6319 0.8835 0.3789 0.099 Uiso calc PR 0.50 . . H
H1C 0.6319 0.8835 0.6211 0.099 Uiso calc PR 0.50 . . H
C2 0.5826(2) 0.7227(3) 0.5000 0.0469(8) Uani d S 1 . . C
C3 0.6438(2) 0.6210(3) 0.5000 0.0444(7) Uani d S 1 . . C
C4 0.7321(2) 0.6426(4) 0.5000 0.0626(10) Uani d S 1 . . C
H4A 0.7595 0.5614 0.5000 0.094 Uiso calc SR 1 . . H
H4B 0.7471 0.6902 0.6211 0.094 Uiso calc PR 0.50 . . H
H4C 0.7471 0.6902 0.3789 0.094 Uiso calc PR 0.50 . . H
H2 0.6225 0.3309 0.5000 0.080 Uiso d SP 0.50 . . H
H1 0.3951 0.6915 0.5000 0.080 Uiso d SP 0.50 . . H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ni 0.0408(3) 0.0358(3) 0.0319(3) 0.0022(2) 0.000 0.000
N1 0.0506(16) 0.0395(14) 0.0353(13) 0.0038(11) 0.000 0.000
N2 0.0458(15) 0.0462(15) 0.0349(13) 0.0051(11) 0.000 0.000
O1 0.0605(15) 0.0409(13) 0.0597(15) 0.0117(11) 0.000 0.000
O2 0.0440(12) 0.0529(14) 0.0582(15) 0.0104(10) 0.000 0.000
C1 0.079(3) 0.046(2) 0.073(3) -0.0117(19) 0.000 0.000
C2 0.061(2) 0.0441(18) 0.0360(15) -0.0069(15) 0.000 0.000
C3 0.0487(17) 0.0509(18) 0.0337(14) -0.0047(15) 0.000 0.000
C4 0.049(2) 0.072(3) 0.067(2) -0.0128(18) 0.000 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N2 Ni N1 82.40(11)
C2 N1 O1 119.8(3)
C2 N1 Ni 116.3(2)
O1 N1 Ni 123.9(2)
C3 N2 O2 119.5(3)
C3 N2 Ni 116.6(2)
O2 N2 Ni 123.9(2)
N1 O1 H1 101.4
N2 O2 H2 104.4
C2 C1 H1A 109.5
C2 C1 H1B 109.5
H1A C1 H1B 109.5
C2 C1 H1C 109.5
H1A C1 H1C 109.5
H1B C1 H1C 109.5
N1 C2 C3 112.5(3)
N1 C2 C1 123.1(4)
C3 C2 C1 124.3(4)
N2 C3 C2 112.2(3)
N2 C3 C4 122.8(3)
C2 C3 C4 125.0(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
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni N2 . 1.859(3) y
Ni N1 . 1.861(3) y
N1 C2 . 1.292(5) y
N1 O1 . 1.350(4) y
N2 C3 . 1.292(4) y
N2 O2 . 1.341(4) y
O1 H1 . 1.109 ?
O2 H2 . 0.986 ?
C1 C2 . 1.489(5) ?
C1 H1A . 0.9600 ?
C1 H1B . 0.9600 ?
C1 H1C . 0.9600 ?
C2 C3 . 1.467(5) ?
C3 C4 . 1.482(5) ?
C4 H4A . 0.9600 ?
C4 H4B . 0.9600 ?
C4 H4C . 0.9600 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1 H1 O2 9_666 1.11 1.35 2.457(4) 172 y
O2 H2 O1 9_666 0.99 1.48 2.457(4) 169 y
