Structural Properties of Nickel Dimethylglyoxime at High Pressure: Single-Crystal X-ray Diffraction and DFT Studies
Bruce-Smith, Ian F.; Zakharov, Boris A.; Stare, Jernej; Boldyreva, Elena V.; Pulham, Colin R.; The Journal of Physical Chemistry C 118 (2014) 24705–; doi:10.1021/jp508939g

data_1517999
_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
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_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
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_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
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_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/[\s^2^(Fo^2^)+(0.1194P)^2^+2.0963P] where P=(Fo^2^+2Fc^2^)/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)
_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