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_7710498
_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_sum            'C116 H176 Cu8 N16 O84'
_chemical_formula_weight         3647.06
_chemical_name_systematic
bis[tris(2-hydroxy-6-methyl-1H-pyridine-3-carboxylato-k2O,O')(mu-2-hydroxy-6-methyl-1H-pyridine-3-carboxylato-k2O,O':kO'')(methanol)dicopper(II)][bis(2-hydroxy-6-methyl-1H-pyridine-3-carboxylato-k2O,O')bis(mu-2-hydroxy-6-methyl-1H-pyridine-3-carboxylato-k2O,O':kO'')dicopper(II)]bis[bis(2-hydroxy-6-methyl-1H-pyridine-3-carboxylato-k2O,O')(methanol)copper(II)]hexadecahydrate}
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-05-02 deposited with the CCDC.	2022-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.627(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.4921(14)
_cell_length_b                   9.4963(8)
_cell_length_c                   37.786(2)
_cell_measurement_reflns_used    51215
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.767
_cell_measurement_theta_min      2.211
_cell_volume                     7345.4(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker Venture'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0782
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            51215
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.767
_diffrn_reflns_theta_min         2.211
_exptl_absorpt_coefficient_mu    1.251
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS, Program for Empirical Adsorption Correction, 
Institute for Inorganic Chemistry, University of Gottingen: Germany, 
1996Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_density_method    none
_exptl_crystal_description       'trigonal antiprism'
_exptl_crystal_F_000             3776
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.900
_refine_diff_density_min         -1.651
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1021
_refine_ls_number_reflns         18810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0892P)^2^+8.0472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1628
_refine_ls_wR_factor_ref         0.1815
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12339
_reflns_number_total             18812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00838f2.cif
_cod_data_source_block           Compound4Cu
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7710498
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              5358
_shelx_hkl_checksum              58871