#------------------------------------------------------------------------------
#$Date: 2022-05-25 01:30:41 +0300 (Wed, 25 May 2022) $
#$Revision: 275628 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/49/7244978.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_7244978
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 Ni0.599 O4 Pd0.401'
_chemical_formula_sum            'C8 H14 N4 Ni0.6 O4 Pd0.4'
_chemical_formula_weight         308.14
_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             2022-04-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-04-28 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                   10.5483(7)
_cell_length_b                   16.3439(10)
_cell_length_c                   6.3648(4)
_cell_measurement_reflns_used    1924
_cell_measurement_temperature    123
_cell_measurement_theta_max      30.5920
_cell_measurement_theta_min      2.4680
_cell_volume                     1097.29(12)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -39.00 -13.00   0.50    4.12    --    5.00  45.00 120.00   52
  2  ω     38.00  79.00   0.50    4.12    --  -10.00  45.00  60.00   82
  3  ω    -99.00   4.00   0.50    4.12    --  -10.00  45.00  60.00  206
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0426334000
_diffrn_orient_matrix_UB_12      0.0116673000
_diffrn_orient_matrix_UB_13      0.0075415000
_diffrn_orient_matrix_UB_21      0.0072843000
_diffrn_orient_matrix_UB_22      0.0661696000
_diffrn_orient_matrix_UB_23      -0.0074809000
_diffrn_orient_matrix_UB_31      -0.0035816000
_diffrn_orient_matrix_UB_32      -0.0037807000
_diffrn_orient_matrix_UB_33      -0.1108431000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2907
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.677
_diffrn_reflns_theta_min         2.298
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.748
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97068
_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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_description       needle
_exptl_crystal_F_000             629
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         802
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0246P)²+0.6638P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0554
_reflns_Friedel_coverage         0.000
_reflns_number_gt                712
_reflns_number_total             802
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ce00402j2.cif
_cod_data_source_block           Ni(x)Pd(1-x)(HDMG)2
_cod_original_formula_sum        'C8 H14 N4 Ni0.60 O4 Pd0.40'
_cod_database_code               7244978
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ni Pd C N O H'
_chemical_oxdiff_usercomment     123K
_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 99.20
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Ni01, Pd01}
3. Restrained distances
 O003-H003
 0.84 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Ni01) = Uanis(Pd01)
5. Others
 Sof(Pd01)=0.25*(1-FVAR(2))
 Sof(Ni01)=0.25*FVAR(2)
 Fixed Sof: H00A(0.5) H00B(0.5) H00C(0.5) H00D(0.5) H00E(0.5) H00F(0.5)
6.a Idealised Me refined as rotating group:
 C008(H00A,H00B,H00C), C009(H00D,H00E,H00F)
;
_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 1.114
_oxdiff_exptl_absorpt_empirical_full_min 0.933
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
Ni01 Ni 0.500000 0.500000 0.500000 0.01309(12) Uani 0.599(7) 4 d S T P A 3
O002 O 0.59212(14) 0.66406(9) 0.500000 0.0221(4) Uani 1 2 d S T P A .
O003 O 0.23950(16) 0.44627(10) 0.500000 0.0249(4) Uani 1 2 d DS T P A .
N004 N 0.48963(15) 0.61664(12) 0.500000 0.0188(4) Uani 1 2 d S T P . .
N005 N 0.31988(19) 0.51132(11) 0.500000 0.0197(4) Uani 1 2 d S T P . .
C006 C 0.2757(2) 0.58486(14) 0.500000 0.0208(4) Uani 1 2 d S T P A .
C007 C 0.3764(2) 0.64759(13) 0.500000 0.0202(4) Uani 1 2 d S T P A .
C008 C 0.3546(2) 0.73740(14) 0.500000 0.0280(5) Uani 1 2 d S T P . .
H00A H 0.415668 0.763397 0.410337 0.042 Uiso 0.5 1 calc R U P A -1
H00B H 0.363263 0.758098 0.640418 0.042 Uiso 0.5 1 calc R U P A -1
H00C H 0.270684 0.748736 0.449245 0.042 Uiso 0.5 1 calc R U P A -1
C009 C 0.1376(2) 0.60306(15) 0.500000 0.0286(5) Uani 1 2 d S T P . .
H00D H 0.123942 0.657896 0.450874 0.043 Uiso 0.5 1 calc R U P A -1
H00E H 0.104923 0.597750 0.640133 0.043 Uiso 0.5 1 calc R U P A -1
H00F H 0.094656 0.565283 0.408993 0.043 Uiso 0.5 1 calc R U P A -1
H003 H 0.288(5) 0.403(2) 0.500000 0.16(2) Uiso 1 2 d DS . P . .
Pd01 Pd 0.500000 0.500000 0.500000 0.01309(12) Uani 0.401(7) 4 d S T P A 4
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'
Pd Pd -0.9988 1.0072 '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
N004 Ni01 N004 180.00(10) 9_666 . ?
N005 Ni01 N004 98.84(7) . 9_666 ?
N005 Ni01 N004 98.85(7) 9_666 . ?
N005 Ni01 N004 81.16(7) . . ?
N005 Ni01 N004 81.16(7) 9_666 9_666 ?
N005 Ni01 N005 180.0 . 9_666 ?
N005 O003 H003 106(4) . . ?
O002 N004 Ni01 122.35(13) . . ?
O002 N004 Pd01 122.35(13) . . ?
C007 N004 Ni01 116.23(15) . . ?
C007 N004 O002 121.4(2) . . ?
C007 N004 Pd01 116.23(15) . . ?
O003 N005 Ni01 123.01(14) . . ?
O003 N005 Pd01 123.01(14) . . ?
C006 N005 Ni01 116.73(15) . . ?
C006 N005 O003 120.25(19) . . ?
C006 N005 Pd01 116.73(15) . . ?
N005 C006 C007 112.84(19) . . ?
N005 C006 C009 122.7(2) . . ?
C007 C006 C009 124.5(2) . . ?
N004 C007 C006 113.04(19) . . ?
N004 C007 C008 121.9(2) . . ?
C006 C007 C008 125.1(2) . . ?
C007 C008 H00A 109.5 . . ?
C007 C008 H00B 109.5 . . ?
C007 C008 H00C 109.5 . . ?
H00A C008 H00B 109.5 . . ?
H00A C008 H00C 109.5 . . ?
H00B C008 H00C 109.5 . . ?
C006 C009 H00D 109.5 . . ?
C006 C009 H00E 109.5 . . ?
C006 C009 H00F 109.5 . . ?
H00D C009 H00E 109.5 . . ?
H00D C009 H00F 109.5 . . ?
H00E C009 H00F 109.5 . . ?
N004 Pd01 N004 180.00(10) 9_666 . ?
N004 Pd01 Pd01 90.0 . 7_546 ?
N004 Pd01 Pd01 90.0 9_666 7_545 ?
N004 Pd01 Pd01 90.0 9_666 7_546 ?
N004 Pd01 Pd01 90.0 . 7_545 ?
N005 Pd01 N004 81.16(7) 9_666 9_666 ?
N005 Pd01 N004 98.84(7) . 9_666 ?
N005 Pd01 N004 81.16(7) . . ?
N005 Pd01 N004 98.85(7) 9_666 . ?
N005 Pd01 N005 180.0 . 9_666 ?
N005 Pd01 Pd01 90.0 . 7_546 ?
N005 Pd01 Pd01 90.0 9_666 7_545 ?
N005 Pd01 Pd01 90.0 9_666 7_546 ?
N005 Pd01 Pd01 90.0 . 7_545 ?
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
Ni01 N004 1.909(2) 9_666 ?
Ni01 N004 1.909(2) . ?
Ni01 N005 1.909(2) . ?
Ni01 N005 1.909(2) 9_666 ?
O002 N004 1.330(2) . ?
O003 N005 1.360(2) . ?
O003 H003 0.87(2) . ?
N004 C007 1.297(3) . ?
N004 Pd01 1.909(2) . ?
N005 C006 1.289(3) . ?
N005 Pd01 1.909(2) . ?
C006 C007 1.476(3) . ?
C006 C009 1.488(3) . ?
C007 C008 1.486(3) . ?
C008 H00A 0.9600 . ?
C008 H00B 0.9600 . ?
C008 H00C 0.9600 . ?
C009 H00D 0.9600 . ?
C009 H00E 0.9600 . ?
C009 H00F 0.9600 . ?
Pd01 Pd01 3.1824(2) 7_546 ?
Pd01 Pd01 3.1824(2) 7_545 ?
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
Ni01 N004 C007 C006 0.0 . . . . ?
Ni01 N004 C007 C008 180.0 . . . . ?
Ni01 N005 C006 C007 0.0 . . . . ?
Ni01 N005 C006 C009 180.0 . . . . ?
O002 N004 C007 C006 180.0 . . . . ?
O002 N004 C007 C008 0.0 . . . . ?
O003 N005 C006 C007 180.0 . . . . ?
O003 N005 C006 C009 0.0 . . . . ?
N005 C006 C007 N004 0.0 . . . . ?
N005 C006 C007 C008 180.0 . . . . ?
C009 C006 C007 N004 180.0 . . . . ?
C009 C006 C007 C008 0.0 . . . . ?
Pd01 N004 C007 C006 0.0 . . . . ?
Pd01 N004 C007 C008 180.0 . . . . ?
Pd01 N005 C006 C007 0.0 . . . . ?
Pd01 N005 C006 C009 180.0 . . . . ?
