Modulation of the elasticity of single crystal, 1-D metal dimethylglyoximato complexes via solid solution effect
Sugimoto, Akira; Kusumoto, Sotaro; Nakaya, Manabu; Sekine, Yoshihiro; Lindoy, Leonard F.; Hayami, Shinya; CrystEngComm  (2022) –; doi:10.1039/D2CE00402J

data_7244978
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -39.00 -13.00   0.50    4.12    --    5.00  45.00 120.00   52
  2  \w     38.00  79.00   0.50    4.12    --  -10.00  45.00  60.00   82
  3  \w    -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       '\w 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/[\s^2^(Fo^2^)+(0.0246P)^2^+0.6638P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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
_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)
;
_shelx_res_checksum              10571
_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