#------------------------------------------------------------------------------
#$Date: 2022-05-25 01:30:41 +0300 (Wed, 25 May 2022) $
#$Revision: 275628 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/49/7244974.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_7244974
loop_
_publ_author_name
'Sugimoto, Akira'
'Kusumoto, Sotaro'
'Nakaya, Manabu'
'Sekine, Yoshihiro'
'Lindoy, Leonard F.'
'Hayami, Shinya'
_publ_section_title
;
 Modulation of the elasticity of single crystal, 1-D metal
 dimethylglyoximato complexes via solid solution effect
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00402J
_journal_year                    2022
_chemical_formula_moiety         'C8 H14 N4 Ni O4'
_chemical_formula_sum            'C8 H14 N4 Ni O4'
_chemical_formula_weight         288.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_Hall           '-I 2 2c'
_space_group_name_H-M_alt        'I b a m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-02-03 deposited with the CCDC.	2022-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.210(2)
_cell_length_b                   10.5207(16)
_cell_length_c                   6.3360(9)
_cell_measurement_reflns_used    1044
_cell_measurement_temperature    123
_cell_measurement_theta_max      28.9730
_cell_measurement_theta_min      3.8480
_cell_volume                     1080.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -83.00 -18.00   0.50   15.00    --    5.00  45.00  30.00  130
  2  ω      8.00  34.00   0.50   15.00    --   -8.90  45.00  90.00   52
  3  ω    -98.00 -19.00   0.50   15.00    --   -8.90  45.00  90.00  158
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0271527000
_diffrn_orient_matrix_UB_12      0.0528357000
_diffrn_orient_matrix_UB_13      0.0003447000
_diffrn_orient_matrix_UB_21      -0.0343603000
_diffrn_orient_matrix_UB_22      0.0418331000
_diffrn_orient_matrix_UB_23      -0.0024058000
_diffrn_orient_matrix_UB_31      -0.0006494000
_diffrn_orient_matrix_UB_32      0.0009295000
_diffrn_orient_matrix_UB_33      0.1118503000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.849
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2792
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.849
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.224
_diffrn_reflns_theta_min         2.308
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.806
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_description       needle
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1277
_refine_ls_wR_factor_ref         0.1333
_reflns_Friedel_coverage         0.000
_reflns_number_gt                637
_reflns_number_total             748
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ce00402j2.cif
_cod_data_source_block           Ni(HDMG)2
_cod_original_cell_volume        1080.6(3)
_cod_database_code               7244974
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Ni C N O'
_chemical_oxdiff_usercomment     100
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H4A(0.5) H4B(0.5) H4C(0.5) H3B(0.5) H3C(0.5) H3A(0.5)
3.a Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C3(H3B,H3C,H3A)
;
_shelx_res_file
;
    200728_sugi_ni.res created by SHELXL-2014/7

TITL 200728_sugi_ni_a.res in Ibam
REM Old TITL 200728_sugi_Ni in Iba2
REM SHELXT solution in Ibam
REM R1 0.078, Rweak 0.004, Alpha 0.070, Orientation as input
REM Formula found by SHELXT: C12 O4 Ni
CELL 0.71073 16.2102 10.5207 6.336 90 90 90
ZERR 8 0.002 0.0016 0.0009 0 0 0
LATT 2
SYMM -X,-Y,+Z
SYMM 0.5-X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H N Ni O
UNIT 32 56 16 4 16

L.S. 5 0 0
PLAN  20
list 4
fmap 2 53
acta
OMIT 2 0 0
OMIT 17 7 2
REM <olex2.extras>
REM <HklSrc "%.\\200728_sugi_Ni.hkl">
REM </olex2.extras>

WGHT    0.100000
FVAR       0.23071
NI1   4    0.500000    0.500000    0.500000    10.25000    0.01494    0.01513 =
         0.01234    0.00000    0.00000   -0.00018
O1    5    0.664037    0.406521    0.500000    10.50000    0.01662    0.02019 =
         0.02363    0.00000    0.00000    0.00493
O2    5    0.444173    0.756309    0.500000    10.50000    0.02137    0.01681 =
         0.02014    0.00000    0.00000    0.00742
N1    3    0.614537    0.508847    0.500000    10.50000    0.01627    0.01971 =
         0.01690    0.00000    0.00000    0.00134
C2    1    0.583319    0.722333    0.500000    10.50000    0.02251    0.01909 =
         0.01315    0.00000    0.00000   -0.00027
N2    3    0.509302    0.675955    0.500000    10.50000    0.01942    0.02002 =
         0.01418    0.00000    0.00000    0.00137
C4    1    0.601767    0.860285    0.500000    10.50000    0.02517    0.01914 =
         0.02462    0.00000    0.00000   -0.00284
PART -1
AFIX 137
H4A   2    0.563299    0.903553    0.590051    10.50000   -1.50000
H4B   2    0.597122    0.892815    0.358940    10.50000   -1.50000
H4C   2    0.656832    0.873859    0.551010    10.50000   -1.50000
AFIX   0
PART 0
C1    1    0.646980    0.621751    0.500000    10.50000    0.02064    0.02151 =
         0.01227    0.00000    0.00000    0.00050
C3    1    0.736813    0.643804    0.500000    10.50000    0.01738    0.02860 =
         0.02397    0.00000    0.00000   -0.00162
PART -1
AFIX 137
H3B   2    0.763021    0.583666    0.592138    10.50000   -1.50000
H3C   2    0.748043    0.728509    0.548469    10.50000   -1.50000
H3A   2    0.757858    0.633595    0.359393    10.50000   -1.50000
AFIX   0
PART 0
H1    2    0.626310    0.331383    0.500000    10.50000    0.18748
HKLF 4

REM  200728_sugi_ni_a.res in Ibam
REM R1 =  0.0480 for     637 Fo > 4sig(Fo)  and  0.0566 for all     748 data
REM     58 parameters refined using      0 restraints

END

WGHT      0.0793      0.0664

REM Highest difference peak  1.014,  deepest hole -0.651,  1-sigma level  0.138
Q1    1   0.4806  0.4336  0.5000  10.50000  0.05    1.01
Q2    1   0.4833  0.5735  0.5000  10.50000  0.05    1.00
Q3    1   0.6160  0.6731  0.5000  10.50000  0.05    0.83
Q4    1   0.4800  0.5002  0.6191  11.00000  0.05    0.79
Q5    1   0.5001  0.6034  0.6457  11.00000  0.05    0.71
Q6    1   0.6351  0.4531  0.5000  10.50000  0.05    0.70
Q7    1   0.6382  0.5540  0.5000  10.50000  0.05    0.65
Q8    1   0.5680  0.5020  0.5000  10.50000  0.05    0.57
Q9    1   0.5857  0.7970  0.5000  10.50000  0.05    0.53
Q10   1   0.4180  0.7970  0.5000  10.50000  0.05    0.45
Q11   1   0.5865  0.6009  0.5000  10.50000  0.05    0.45
Q12   1   0.5875  0.3996  0.5000  10.50000  0.05    0.44
Q13   1   0.4630  0.7237  0.5000  10.50000  0.05    0.29
Q14   1   0.4547  0.8243  0.5000  10.50000  0.05    0.28
Q15   1   0.6569  0.4987  0.6391  11.00000  0.05    0.27
Q16   1   0.7471  0.6260  0.4091  11.00000  0.05    0.27
Q17   1   0.7392  0.7177  0.5000  10.50000  0.05    0.27
Q18   1   0.5976  0.5039  0.5902  11.00000  0.05    0.27
Q19   1   0.7604  0.6914  0.3355  11.00000  0.05    0.26
Q20   1   0.7612  0.5973  0.5000  10.50000  0.05    0.26
;
_shelx_res_checksum              77099
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.913
_oxdiff_exptl_absorpt_empirical_full_min 0.444
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'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1, y+1, -z+1/2'
'x+1, -y+1, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x, -y, z+1/2'
'-x, y, z+1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.5000 0.5000 0.0141(3) Uani 1 4 d S T P . .
O1 O 0.66404(17) 0.4065(2) 0.5000 0.0201(6) Uani 1 2 d S T P . .
O2 O 0.44417(15) 0.7563(3) 0.5000 0.0194(6) Uani 1 2 d S T P . .
N1 N 0.6145(2) 0.5088(3) 0.5000 0.0176(7) Uani 1 2 d S T P . .
C2 C 0.5833(2) 0.7223(4) 0.5000 0.0183(7) Uani 1 2 d S T P . .
N2 N 0.50930(19) 0.6760(3) 0.5000 0.0179(7) Uani 1 2 d S T P . .
C4 C 0.6018(2) 0.8603(3) 0.5000 0.0230(8) Uani 1 2 d S T P . .
H4A H 0.5633 0.9036 0.5901 0.034 Uiso 0.5 1 calc GR . . A -1
H4B H 0.5971 0.8928 0.3589 0.034 Uiso 0.5 1 calc GR . . A -1
H4C H 0.6568 0.8739 0.5510 0.034 Uiso 0.5 1 calc GR . . A -1
C1 C 0.6470(2) 0.6218(4) 0.5000 0.0181(7) Uani 1 2 d S T P . .
C3 C 0.7368(2) 0.6438(4) 0.5000 0.0233(8) Uani 1 2 d S T P . .
H3B H 0.7630 0.5837 0.5921 0.035 Uiso 0.5 1 calc GR . . B -1
H3C H 0.7480 0.7285 0.5485 0.035 Uiso 0.5 1 calc GR . . B -1
H3A H 0.7579 0.6336 0.3594 0.035 Uiso 0.5 1 calc GR . . B -1
H1 H 0.626(7) 0.331(10) 0.5000 0.19(5) Uiso 1 2 d S T P . .
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 0.0149(4) 0.0151(4) 0.0123(4) 0.000 0.000 -0.0002(2)
O1 0.0166(12) 0.0202(14) 0.0236(13) 0.000 0.000 0.0049(11)
O2 0.0214(13) 0.0168(13) 0.0201(13) 0.000 0.000 0.0074(11)
N1 0.0163(16) 0.0197(16) 0.0169(15) 0.000 0.000 0.0013(11)
C2 0.0225(17) 0.0191(18) 0.0132(15) 0.000 0.000 -0.0003(16)
N2 0.0194(15) 0.0200(17) 0.0142(15) 0.000 0.000 0.0014(11)
C4 0.0252(18) 0.0191(18) 0.0246(18) 0.000 0.000 -0.0028(16)
C1 0.0206(17) 0.0215(17) 0.0123(15) 0.000 0.000 0.0005(16)
C3 0.0174(17) 0.029(2) 0.0240(19) 0.000 0.000 -0.0016(15)
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'
Ni Ni 0.3393 1.1124 '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'
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
N1 Ni1 N1 180.0 . 9_666 ?
N2 Ni1 N1 97.53(13) . 9_666 ?
N2 Ni1 N1 97.53(13) 9_666 . ?
N2 Ni1 N1 82.47(13) 9_666 9_666 ?
N2 Ni1 N1 82.47(13) . . ?
N2 Ni1 N2 180.0 9_666 . ?
O1 N1 Ni1 123.8(2) . . ?
C1 N1 Ni1 116.8(3) . . ?
C1 N1 O1 119.4(3) . . ?
N2 C2 C4 123.8(3) . . ?
N2 C2 C1 112.2(3) . . ?
C1 C2 C4 124.1(3) . . ?
O2 N2 Ni1 124.0(2) . . ?
C2 N2 Ni1 116.8(3) . . ?
C2 N2 O2 119.2(3) . . ?
N1 C1 C2 111.8(3) . . ?
N1 C1 C3 122.9(4) . . ?
C3 C1 C2 125.2(4) . . ?
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 N1 1.859(4) 9_666 ?
Ni1 N1 1.859(4) . ?
Ni1 N2 1.857(4) . ?
Ni1 N2 1.857(4) 9_666 ?
O1 N1 1.343(4) . ?
O2 N2 1.353(4) . ?
N1 C1 1.299(5) . ?
C2 N2 1.295(5) . ?
C2 C4 1.482(5) . ?
C2 C1 1.478(6) . ?
C1 C3 1.475(5) . ?
