#------------------------------------------------------------------------------
#$Date: 2016-02-18 16:37:37 +0100 (jue 18 de feb de 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/79/1517999.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1517999
loop_
_publ_author_name
'Bruce-Smith, Ian F.'
'Zakharov, Boris A.'
'Stare, Jernej'
'Boldyreva, Elena V.'
'Pulham, Colin R.'
_publ_section_title
;
 Structural Properties of Nickel Dimethylglyoxime at High Pressure:
 Single-Crystal X-ray Diffraction and DFT Studies
;
_journal_issue                   42
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              24705
_journal_paper_doi               10.1021/jp508939g
_journal_volume                  118
_journal_year                    2014
_chemical_formula_moiety         'C8 H14 N4 Ni O4'
_chemical_formula_sum            'C8 H14 N4 Ni O4'
_chemical_formula_weight         288.94
_chemical_name_common            'Nickel Dimethylglyoxime'
_chemical_name_systematic
; 
Nickel Dimethylglyoxime
;
_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                   16.3688(17)
_cell_length_b                   10.0853(15)
_cell_length_c                   6.1843(4)
_cell_measurement_reflns_used    870
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4310
_cell_measurement_theta_min      2.4810
_cell_volume                     1020.9(2)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction, 2010)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction, 2010)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_pressure         1200000
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3457
_diffrn_measured_fraction_theta_full 0.644
_diffrn_measured_fraction_theta_max 0.644
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1100
_diffrn_reflns_av_sigmaI/netI    0.0751
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2987
_diffrn_reflns_theta_full        28.18
_diffrn_reflns_theta_max         28.18
_diffrn_reflns_theta_min         2.49
_diffrn_source_current           30
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.912
_exptl_absorpt_correction_T_max  0.464
_exptl_absorpt_correction_T_min  0.384
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'Absorb-7 (Angel, 2013)'
_exptl_crystal_colour            'Red to purple'
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needles
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.044
_refine_diff_density_max         1.144
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.229
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     55
_refine_ls_number_reflns         445
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.229
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0610
_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)+(0.1194P)²+2.0963P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1648
_refine_ls_wR_factor_ref         0.2308
_reflns_number_gt                319
_reflns_number_total             445
_reflns_threshold_expression     >2sigma(I)
_iucr_refine_instructions_details
;
TITL
CELL  0.71073 16.36883 10.08530  6.18430 90.00000 90.00000 90.00000
ZERR 4  0.00166  0.00146  0.00037  0.00000  0.00000  0.00000
LATT 2
SYMM -X, -Y, Z
SYMM X, -Y, -Z+ 0.50000
SYMM -X, Y, -Z+ 0.50000
SFAC C H N O NI 
UNIT 32 56 16 16 4 
PLAN 30
FMAP 2 
L.S. 100
EQIV $1 -X, -Y+1, -Z+1
HTAB O1 O2_$1
BOND
BOND $H
CONF
ACTA
FVAR  1.04577 
WGHT  0.11940   2.09630 
NI1   5 0.000000 0.500000 0.500000  10.250000 0.023310 0.022960 =
        0.024100 0.000000 0.000000 -0.001160 
O1    4 -0.052235 0.228239 0.500000  10.500000 0.039540 0.009540 =
        0.042390 0.000000 0.000000 -0.011750 
H5    2 -0.092213 0.227838 0.500000  10.500000 -1.200000 
O2    4 0.162181 0.599085 0.500000  10.500000 0.026710 0.033480 =
        0.035760 0.000000 0.000000 -0.012830 
N1    3 0.009574 0.320180 0.500000  10.500000 0.032540 0.052910 =
        0.023590 0.000000 0.000000 -0.007020 
N2    3 0.112875 0.493445 0.500000  10.500000 0.014470 0.061040 =
        0.023890 0.000000 0.000000 -0.002290 
C1    1 0.083760 0.263819 0.500000  10.500000 0.033480 0.032450 =
        0.023420 0.000000 0.000000 0.003750 
C2    1 0.147018 0.379869 0.500000  10.500000 0.037450 0.027530 =
        0.024800 0.000000 0.000000 0.007020 
C3    1 0.103519 0.128850 0.500000  10.500000 0.043080 0.029170 =
        0.052150 0.000000 0.000000 -0.000810 
AFIX 33
H3A   2 0.081166 0.087617 0.373213  10.500000 -1.500000 
H3B   2 0.081114 0.087597 0.626705  10.500000 -1.500000 
H3C   2 0.161834 0.118726 0.500082  10.500000 -1.500000 
AFIX 0
C4    1 0.234276 0.353896 0.500000  10.500000 0.020920 0.054190 =
        0.042780 0.000000 0.000000 0.003670 
AFIX 33
H4A   2 0.258492 0.392311 0.626744  10.500000 -1.500000 
H4B   2 0.258491 0.392306 0.373251  10.500000 -1.500000 
H4C   2 0.243530 0.259901 0.500004  10.500000 -1.500000 
HKLF 4
REM
REM R1    0.0618 FOR    319 FO > 4SIG(FO)  AND  0.1031 FOR ALL    445 DATA
REM     55 PARAMETERS REFINED USING      0 RESTRAINTS
REM HIGHEST DIFFERENCE PEAK  1.147,  DEEPEST HOLE -0.859,  1-SIGMA LEVEL  0.230
END
;
_cod_data_source_file            jp508939g_si_001.cif
_cod_data_source_block           1.2GPa
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Gaussian'
changed to 'gaussian' according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 1517996--1518005.cif.
;
_cod_original_cell_volume        1020.93(19)
_cod_original_sg_symbol_H-M      Ibam
_cod_database_code               1517999
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_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
Ni1 Ni 0.0000 0.5000 0.5000 0.0235(9) Uani 1 4 d S
O1 O -0.0522(4) 0.2282(10) 0.5000 0.031(2) Uani 1 2 d S
H5 H -0.092(7) 0.228(15) 0.5000 0.037 Uiso 1 2 d S
O2 O 0.1622(5) 0.5991(9) 0.5000 0.032(2) Uani 1 2 d S
N1 N 0.0095(6) 0.3202(13) 0.5000 0.036(3) Uani 1 2 d S
N2 N 0.1129(6) 0.4935(11) 0.5000 0.033(3) Uani 1 2 d S
C1 C 0.0837(7) 0.2638(15) 0.5000 0.030(3) Uani 1 2 d S
C2 C 0.1470(7) 0.3798(15) 0.5000 0.030(3) Uani 1 2 d S
C3 C 0.1036(8) 0.1288(15) 0.5000 0.042(3) Uani 1 2 d S
H3A H 0.0812 0.0875 0.3732 0.063 Uiso 0.50 1 calc PR
H3B H 0.0812 0.0875 0.6267 0.063 Uiso 0.50 1 calc PR
H3C H 0.1619 0.1187 0.5001 0.063 Uiso 1 2 calc SR
C4 C 0.2342(6) 0.3537(14) 0.5000 0.040(3) Uani 1 2 d S
H4A H 0.2585 0.3921 0.6267 0.060 Uiso 0.50 1 calc PR
H4B H 0.2585 0.3921 0.3732 0.060 Uiso 0.50 1 calc PR
H4C H 0.2435 0.2597 0.5000 0.060 Uiso 1 2 calc SR
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 0.0234(14) 0.023(2) 0.0242(11) 0.000 0.000 -0.0011(7)
O1 0.040(6) 0.009(7) 0.043(4) 0.000 0.000 -0.012(4)
O2 0.027(5) 0.033(8) 0.036(4) 0.000 0.000 -0.013(3)
N1 0.033(8) 0.053(12) 0.023(4) 0.000 0.000 -0.007(4)
N2 0.015(7) 0.061(12) 0.024(4) 0.000 0.000 -0.002(5)
C1 0.034(8) 0.033(12) 0.023(5) 0.000 0.000 0.004(5)
C2 0.038(9) 0.027(13) 0.025(5) 0.000 0.000 0.007(5)
C3 0.044(9) 0.029(12) 0.053(7) 0.000 0.000 0.000(5)
C4 0.021(8) 0.054(12) 0.043(6) 0.000 0.000 0.004(5)
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Ni1 N1 180.000(1) 9_566 .
N1 Ni1 N2 83.0(5) 9_566 9_566
N1 Ni1 N2 97.0(5) . 9_566
N1 Ni1 N2 97.0(5) 9_566 .
N1 Ni1 N2 83.0(5) . .
N2 Ni1 N2 180.000(1) 9_566 .
N1 O1 H5 138(10) . .
C1 N1 O1 112.3(12) . .
C1 N1 Ni1 120.0(9) . .
O1 N1 Ni1 127.6(9) . .
C2 N2 O2 116.9(12) . .
C2 N2 Ni1 118.0(9) . .
O2 N2 Ni1 125.1(9) . .
N1 C1 C3 128.5(12) . .
N1 C1 C2 106.4(12) . .
C3 C1 C2 125.1(11) . .
N2 C2 C4 126.4(13) . .
N2 C2 C1 112.5(12) . .
C4 C2 C1 121.1(12) . .
C1 C3 H3A 109.5 . .
C1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C2 C4 H4A 109.5 . .
C2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C2 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_distance
_geom_bond_site_symmetry_2
Ni1 N1 1.820(13) 9_566
Ni1 N1 1.820(13) .
Ni1 N2 1.850(10) 9_566
Ni1 N2 1.850(10) .
O1 N1 1.372(13) .
O1 H5 0.65(11) .
O2 N2 1.336(13) .
N1 C1 1.341(16) .
N2 C2 1.275(16) .
C1 C3 1.400(19) .
C1 C2 1.563(18) .
C2 C4 1.452(15) .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
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_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H5 O2 0.65(11) 2.09(14) 2.504(13) 123(16) 9_566
