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_7059274
_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 Mn N10 O2, 2(Cl O4), 0.75(H2 O)'
_chemical_formula_sum            'C20 H31.5 Cl2 Mn N10 O10.75'
_chemical_formula_weight         709.89
_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             2019-08-29
_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                94.90(3)
_cell_angle_beta                 91.49(3)
_cell_angle_gamma                96.56(3)
_cell_formula_units_Z            4
_cell_length_a                   12.890(3)
_cell_length_b                   15.010(3)
_cell_length_c                   15.150(3)
_cell_measurement_reflns_used    700
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.493
_cell_measurement_theta_min      1.35
_cell_volume                     2899.5(11)
_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    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.978
_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  0.0429
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28426
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        28.400
_diffrn_reflns_theta_max         30.990
_diffrn_reflns_theta_min         1.506
_exptl_absorpt_coefficient_mu    0.966
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XDS (Kabsh, 2010)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_description       prism
_exptl_crystal_F_000             1466
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     870
_refine_ls_number_reflns         13037
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0666P)^2^+2.6176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1359
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11068
_reflns_number_total             13037
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05200c2.cif
_cod_data_source_block           53tup
_cod_depositor_comments
'Adding full bibliography for 7059271--7059274.cif.'
_cod_original_cell_volume        2899.5(10)
_cod_original_formula_sum        'C20 H31.50 Cl2 Mn N10 O10.75'
_cod_database_code               7059274
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.944
_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. Restrained distances
 Cl4-O17 \\sim Cl4-O18 \\sim Cl4-O19 \\sim Cl4-O20
 with sigma of 0.05
 Cl4-O18 \\sim Cl4-O20
 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
Uanis(O18) \\sim Ueq, Uanis(O18A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O18) = Uanis(O18A)
4. Others
 Fixed Sof: Cl4A(0.5) Cl4(0.5) O19(0.5) O18(0.5) O18A(0.5) O17A(0.5) O20A(0.5)
 O20(0.5) O25(0.5) H25D(0.5) H25E(0.5) O17(0.5) O19A(0.5) O27(0.5) H27D(0.5)
 H27E(0.5) O26(0.5) H26A(0.5) H26B(0.5)
5.a Free rotating group:
 O25(H25D,H25E), O27(H27D,H27E), O26(H26A,H26B)
5.b Aromatic/amide H refined with riding coordinates:
 N18(H18), N20(H20), N8(H8), N10(H10), C9(H9), C29(H29), C3(H3A), C23(H23)
5.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C27(H27A,H27B,H27C), C40(H40A,H40B,H40C), C31(H31A,H31B,
 H31C), C37(H37A,H37B,H37C), C33(H33A,H33B,H33C), C7(H7A,H7B,H7C), C25(H25A,
 H25B,H25C), C20(H20A,H20B,H20C), C36(H36A,H36B,H36C), C16(H16A,H16B,H16C),
 C1(H1A,H1B,H1C), C17(H17A,H17B,H17C), C11(H11A,H11B,H11C), C5(H5A,H5B,H5C),
 C21(H21A,H21B,H21C)
5.d Idealised tetrahedral OH refined as rotating group:
 O4(H4), O3(H3), O1(H1), O2(H2)
;
_shelx_res_checksum              70533
_olex2_submission_special_instructions 'No special instructions were received'