Synthesis, structure, magnetic properties and thermal behaviour of Ba–MII (MII = Mn, Co, Cu, and Zn) allylmalonates
Zorina-Tikhonova, Ekaterina N.; Matyukhina, Anna K.; Chistyakov, Aleksandr S.; Vologzhanina, Anna V.; Korlyukov, Alexander A.; Gogoleva, Natalia V.; Novikova, Veronika A.; Belova, Ekaterina V.; Ugolkova, Elena A.; Starikova, Alyona A.; Korchagin, Denis V.; Babeshkin, Konstantin A.; Efimov, Nikolay N.; Kiskin, Mikhail A.; Eremenko, Igor L.; New Journal of Chemistry 46 (2022) 21245–21256; doi:10.1039/D2NJ03751C

data_7062024
_publ_section_title
;
 Synthesis, structure, magnetic properties and thermal behaviour of
 Ba--MII (MII = Mn, Co, Cu, and Zn) allylmalonates
;
_journal_issue                   44
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              21245
_journal_page_last               21256
_journal_paper_doi               10.1039/D2NJ03751C
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         '0.08(C144 H216 Ba12 Cu12 O132)'
_chemical_formula_sum            'C12 H18 Ba Cu O11'
_chemical_formula_weight         539.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-08-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-04-20 deposited with the CCDC.	2022-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.921(4)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   12.313(2)
_cell_length_b                   24.650(4)
_cell_length_c                   17.294(3)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.32
_cell_measurement_theta_min      2.37
_cell_volume                     5170.5(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1027
_diffrn_reflns_av_unetI/netI     0.0902
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            66003
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.786
_diffrn_reflns_theta_min         1.453
_exptl_absorpt_coefficient_mu    3.559
_exptl_absorpt_correction_T_max  0.3368
_exptl_absorpt_correction_T_min  0.2002
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1519 before and 0.0880 after correction.
The Ratio of minimum to maximum transmission is 0.5944.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.078
_exptl_crystal_description       prism
_exptl_crystal_F_000             3156
_refine_diff_density_max         5.842
_refine_diff_density_min         -4.011
_refine_diff_density_rms         0.346
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         15863
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0769
_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^)+(0.0978P)^2^+60.0049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1871
_refine_ls_wR_factor_ref         0.2063
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11864
_reflns_number_total             15863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj03751c2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7062021--7062024.cif.'
_cod_original_cell_volume        5170.5(16)
_cod_database_code               7062024
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Restrained distances
 C11-C10 = C11A-C10
 1.5 with sigma of 0.02
 C12-C11 = C12A-C11A
 1.35 with sigma of 0.02
 C8-C10A = C8-C10
 1.5 with sigma of 0.02
 C11-C10 = C11A-C10A
 1.5 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O19) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uiso(C12) = Uiso(C12A)
Uiso(C11A) = Uiso(C11)
Uiso(C10) = Uiso(C10A)
3. Others
 Fixed Sof: C10(0.5) H10A(0.5) H10B(0.5) C11(0.5) H11(0.5) C12(0.5) H12A(0.5)
 H12B(0.5) C11A(0.5) H11A(0.5) C12A(0.5) H12C(0.5) H12D(0.5) C10A(0.5)
 H10C(0.5) H10D(0.5)
4.a Riding coordinates:
 O26(H26A,H26B), O27(H27A,H27B), O28(H28A,H28B), O29(H29A,H29B), O30(H30A,
 H30B), O31(H31A,H31B), O32(H32A,H32B), O33(H33A,H33B)
4.b Rotating group:
 O25(H25A,H25B)
4.c Ternary CH refined with riding coordinates:
 C2(H2), C8(H8), C14(H14), C20(H20), C26(H26), C32(H32)
4.d Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C10(H10A,H10B), C16(H16A,H16B), C22(H22A,H22B), C28(H28C,H28D),
 C34(H34A,H34B), C10A(H10C,H10D)
4.e Aromatic/amide H refined with riding coordinates:
 C5(H5), C11(H11), C17(H17), C23(H23), C29(H29), C35(H35), C11A(H11A)
4.f X=CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B), C24(H24A,H24B), C30(H30C,H30D),
 C36(H36A,H36B), C12A(H12C,H12D)
;
_shelx_res_checksum              49850
_olex2_submission_special_instructions 'No special instructions were received'