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_7710500
_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         'C28 H38 Co2 N4 Na2 O19, 2(N O3)'
_chemical_formula_sum            'C28 H38 Co2 N6 Na2 O25'
_chemical_formula_weight         1022.48
_chemical_name_systematic
'Poly{[hexaaqua(mu-aqua)bis(mu3-2-hydroxy-6-methyl-1H-pyridine-3-carboxylato-kO:k2O,O':kO')bis(mu-2-hydroxy-6-methyl-1H-pyridine-3-carboxylato-k2O,O':k2O',O'')dicobalt(II)dipotassium] nitrate}'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 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                 91.342(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5130(7)
_cell_length_b                   18.4330(7)
_cell_length_c                   15.8418(7)
_cell_measurement_reflns_used    42213
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.748
_cell_measurement_theta_min      2.210
_cell_volume                     3944.9(3)
_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)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41953
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.579
_diffrn_reflns_theta_min         2.210
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.966
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
;
_exptl_crystal_colour            'light pink'
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_description       cubic
_exptl_crystal_F_000             2096
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.551
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         5039
_refine_ls_number_restraints     194
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0410P)^2^+22.8782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4551
_reflns_number_total             5039
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00838f2.cif
_cod_data_source_block           compound2Co
_cod_original_sg_symbol_H-M      I2/a
_cod_database_code               7710500
_shelx_shelxl_version_number     2019/1
_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. Restrained distances
 N2-O3 = N2-O5
 1.25 with sigma of 0.02
 N2-O4
 1.24 with sigma of 0.02
 N1-O1 = N1-O6
 1.25 with sigma of 0.02
 N1-O2
 1.24 with sigma of 0.02
 Na3A-H4WA \\sim Na3A-H4WB
 with sigma of 0.02
 Na3A-H4WC \\sim Na3A-H4WD
 with sigma of 0.02
 N2-O3 \\sim N2-O4 \\sim N2-O5
 with sigma of 0.02
 O3-O4 \\sim O4-O5 \\sim O5-O3
 with sigma of 0.04
 O1-O2 \\sim O2-O6 \\sim O6-O1
 with sigma of 0.04
 N1-O1 \\sim N1-O2 \\sim N1-O6
 with sigma of 0.001
 N2-O5 \\sim N2A-O5A
 with sigma of 0.02
 O3-O4 \\sim O3A-O4A
 with sigma of 0.04
 O3-O5 \\sim O3A-O5A
 with sigma of 0.04
 N2-O4 \\sim N2A-O4A
 with sigma of 0.02
 O4-O5 \\sim O4A-O5A
 with sigma of 0.04
 N2-O3 \\sim N2A-O3A
 with sigma of 0.02
 H2WA-H2WB \\sim H2WC-H2WD
 with sigma of 0.04
 Co2-H2WB \\sim Co2-H2WD
 with sigma of 0.04
 Co2-H2WA \\sim Co2-H2WC
 with sigma of 0.04
 Co2-O2WA \\sim Co2-O2WB
 with sigma of 0.02
 O2WA-H2WA \\sim O2WB-H2WC
 with sigma of 0.02
 O2WA-H2WB \\sim O2WB-H2WD
 with sigma of 0.02
3. Restrained planarity
 N2, O3, O4, O5
 with sigma of 0.1
 N1, O1, O2, O6
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N2 \\sim O3 \\sim O4 \\sim O5: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N1 \\sim O1 \\sim O2 \\sim O6: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(O5A) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(O4A) \\sim Ueq, Uanis(O3A)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Na3B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 N1, O1, O2, O6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4, N2, O3, O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2A, O4A, O5A, O3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2, O3, O4, O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O2WB)=Sof(H2WC)=Sof(H2WD)=1-FVAR(1)
 Sof(O2WA)=Sof(H2WA)=Sof(H2WB)=FVAR(1)
 Sof(Na3B)=1-FVAR(2)
 Sof(Na3A)=FVAR(2)
 Fixed Sof: H3WA(0.5) H3WB(0.5) O4WA(0.5) H4WA(0.5) H4WB(0.5) O4WB(0.5)
 H4WC(0.5) H4WD(0.5) N2(0.1) O3(0.1) O4(0.1) O5(0.1) N1(0.5) O1(0.5) O2(0.5)
 O6(0.5) N2A(0.4) O4A(0.4) O5A(0.4) O3A(0.4)
7.a Riding coordinates:
 O4WA(H4WA,H4WB), O4WB(H4WC,H4WD)
7.b Rotating group:
 O1W(H1WA,H1WB), O2WA(H2WA,H2WB), O3W(H3WA,H3WB), O2WB(H2WC,H2WD)
7.c Aromatic/amide H refined with riding coordinates:
 N1A(H1A), C4A(H4A), C5A(H5A), N1B(H1B), C4B(H4B), C5B(H5B)
7.d Idealised Me refined as rotating group:
 C61A(H61A,H61B,H61C), C61B(H61D,H61E,H61F)
;
_olex2_submission_special_instructions 'No special instructions were received'