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_7710499
_publ_section_title
;
 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         'C14 H12 Cu N2 O6, 6(H2 O)'
_chemical_formula_sum            'C14 H24 Cu N2 O12'
_chemical_formula_weight         475.89
_chemical_name_systematic
'catena[bis(mu-2-hydroxy-6-methyl-1H-pyridine-3-carboxylato-k2O,O':kO'')copper(II)] hexahydrate}'
_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             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                 98.595(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.1194(4)
_cell_length_b                   21.9576(16)
_cell_length_c                   8.6216(6)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.472
_cell_measurement_theta_min      2.561
_cell_volume                     958.27(12)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0827
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            15093
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         2.563
_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    1.207
_exptl_absorpt_correction_T_max  0.0982
_exptl_absorpt_correction_T_min  0.0617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1285 before and 0.0789 after correction.
The Ratio of minimum to maximum transmission is 0.6283.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_description       needle
_exptl_crystal_F_000             494
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0357P)^2^+2.5559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1085
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1389
_reflns_number_total             1683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00838f2.cif
_cod_data_source_block           Compound5Cu
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7710499
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.869
_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,H) groups
2.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
2.b Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C5A(H5A), N1A(H1A)
2.c Idealised Me refined as rotating group:
 C61A(H61A,H61B,H61C)
;
_olex2_submission_special_instructions 'No special instructions were received'