Theoretical and experimental study of the coordination ability of 4,6-dimethylpyrimidinylhydrazone diacetylmonooxime towards Ni(ii), Mn(ii), Fe(iii) and Co(iii) ions
Lukov, Vladimir V.; Tsaturyan, Arshak A.; Tupolova, Yulia P.; Popov, Leonid D.; Shcherbakov, Igor N.; Lebedev, Vladimir E.; Askalepova, Olga I.; Lastovina, Tatiana A.; Lazarenko, Vladimir A.; Khustalev, Victor N.; Poler, Jordan C.; New Journal of Chemistry 44 (2020) 2146–2154; doi:10.1039/C9NJ05200C

data_7059272
_publ_section_title
;
 Theoretical and experimental study of the coordination ability of
 4,6-dimethylpyrimidinylhydrazone diacetylmonooxime towards Ni(ii),
 Mn(ii), Fe(iii) and Co(iii) ions
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2146
_journal_page_last               2154
_journal_paper_doi               10.1039/C9NJ05200C
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C20 H30 N10 Ni O2, 2(Cl), 1.17(H2 O)'
_chemical_formula_sum            'C20 H32.34 Cl2 N10 Ni O3.17'
_chemical_formula_weight         593.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-30 deposited with the CCDC.	2020-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                70.07(3)
_cell_angle_beta                 65.63(3)
_cell_angle_gamma                88.17(3)
_cell_formula_units_Z            2
_cell_length_a                   11.070(2)
_cell_length_b                   11.180(2)
_cell_length_c                   12.880(3)
_cell_measurement_reflns_used    500
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.161
_cell_measurement_theta_min      2.179
_cell_volume                     1354.0(7)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7927
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16940
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        28.161
_diffrn_reflns_theta_max         28.161
_diffrn_reflns_theta_min         2.179
_exptl_absorpt_coefficient_mu    1.287
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XDS (Kabsh, 2010)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       prism
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   28.161
_exptl_transmission_factor_min   2.179
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         4703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0461P)^2^+0.9720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4282
_reflns_number_total             4703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05200c2.cif
_cod_data_source_block           532
_cod_depositor_comments
'Adding full bibliography for 7059271--7059274.cif.'
_cod_original_cell_volume        1354.0(6)
_cod_database_code               7059272
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.927
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O4(H4A,H4B), O3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 N7(H7), N9(H9), C18(H18), C3(H3)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C12(H12A,H12B,H12C), C1(H1A,H1B,H1C), C10(H10A,H10B,
 H10C), C8(H8A,H8B,H8C), C20(H20A,H20B,H20C), C16(H16A,H16B,H16C), C5(H5A,H5B,
 H5C)
2.d Idealised tetrahedral OH refined as rotating group:
 O2(H2), O1(H1)
;
_shelx_res_checksum              70227
_olex2_submission_special_instructions 'No special instructions were received'