Combined experimental and theoretical investigation on the magnetic properties derived from the coordination of 6-methyl-2-oxonicotinate to 3d-metal ions
Razquin-Bobillo, Laura; Pajuelo-Corral, Oier; Artetxe, Beñat; Zabala-Lekuona, Andoni; Choquesillo-Lazarte, Duane; Rodríguez-Diéguez, Antonio; San Sebastian, Eider; Cepeda, Javier; Dalton Transactions  (2022) –; doi:10.1039/D2DT00838F

data_7710497
_publ_section_title
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 Combined experimental and theoretical investigation on the magnetic
 properties derived from the coordination of 6-methyl-2-oxonicotinate to
 3d-metal ions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00838F
_journal_year                    2022
_chemical_formula_moiety         'C22 H22 Mn N3 Na O10, C H4 O, H2 O'
_chemical_formula_sum            'C23 H28 Mn N3 Na O12'
_chemical_formula_weight         616.41
_chemical_name_systematic
'Poly{[bis(mu3-2-hydroxy-6-methyl-1H-pyridine-3-carboxylato-kO:k2O,O':kO')(mu-2-hydroxy-6-methyl-1H-pyridine-3-carboxylato-kO:k2O,O')manganese(II)sodium(methanol)] hydrate methanol}'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-04-13
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-05-02 deposited with the CCDC.	2022-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.946(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4049(9)
_cell_length_b                   12.2948(7)
_cell_length_c                   15.1192(10)
_cell_measurement_reflns_used    6273
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      24.98
_cell_measurement_theta_min      2.70
_cell_volume                     2667.7(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'Bruker Apex3, 2019'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1556
_diffrn_reflns_av_unetI/netI     0.0813
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24651
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        23.255
_diffrn_reflns_theta_max         23.255
_diffrn_reflns_theta_min         2.138
_diffrn_source                   'high brilliance microfocus sealed tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_T_max  0.0911
_exptl_absorpt_correction_T_min  0.0666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0923 before and 0.0778 after correction.
The Ratio of minimum to maximum transmission is 0.7311.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       'trigonal antiprism'
_exptl_crystal_F_000             1276
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         3821
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+5.4554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0950
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2642
_reflns_number_total             3821
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00838f2.cif
_cod_data_source_block           Compound1Mn
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7710497
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.955
_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:
 O1W(H1WA,H1WB)
2.b Aromatic/amide H refined with riding coordinates:
 N1B(H1B), N1C(H1C), N1A(H1A), C5B(H5B), C4A(H4A), C4B(H4B), C4C(H4C),
 C5A(H5A), C5C(H5C)
2.c Idealised Me refined as rotating group:
 C61B(H61A,H61B,H61C), C61(H61D,H61E,H61F), C61C(H61G,H61H,H61I), C2N(H2NA,
 H2NB,H2NC), C2M(H2MA,H2MB,H2MC)
2.d Idealised tetrahedral OH refined as rotating group:
 O1N(H1N), O1M(H1M)
;
_olex2_submission_special_instructions 'No special instructions were received'