Paramagnetic solid-state NMR assignment and novel chemical conversion of the aldehyde group to dihydrogen ortho ester and hemiacetal moieties in copper(ii)- and cobalt(ii)-pyridinecarboxaldehyde complexes
Crespi, Ayelén F.; Sánchez, Verónica M.; Vega, Daniel; Pérez, Ana L.; Brondino, Carlos D.; Linck, Yamila Garro; Hodgkinson, Paul; Rodríguez-Castellón, Enrique; Lázaro-Martínez, Juan M.; RSC Advances 11 (2021) 20216–20231; doi:10.1039/D1RA02512K

data_7243037
_publ_section_title
;
 Paramagnetic solid-state NMR assignment and novel chemical conversion of
 the aldehyde group to dihydrogen ortho ester and hemiacetal moieties in
 copper(ii)- and cobalt(ii)-pyridinecarboxaldehyde complexes
;
_journal_issue                   33
_journal_name_full               'RSC Advances'
_journal_page_first              20216
_journal_page_last               20231
_journal_paper_doi               10.1039/D1RA02512K
_journal_volume                  11
_journal_year                    2021
_chemical_formula_sum            'C24 H20 Cl2 Co N4 O4'
_chemical_formula_weight         558.27
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-11-28 deposited with the CCDC.	2021-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.41(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7191(15)
_cell_length_b                   36.122(7)
_cell_length_c                   8.4932(17)
_cell_measurement_reflns_used    1710
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.35
_cell_measurement_theta_min      2.47
_cell_volume                     2366.1(8)
_computing_cell_refinement       'APEX3 v2018.7-2'
_computing_data_collection       'APEX3 v2018.7-2'
_computing_data_reduction        'APEX3 v2018.7-2'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_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 Quest Eco Photon detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1501
_diffrn_reflns_av_unetI/netI     0.1129
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            18330
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.724
_diffrn_reflns_theta_max         24.724
_diffrn_reflns_theta_min         2.466
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.991
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4016
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1276
_refine_ls_R_factor_gt           0.0650
_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^)+(0.0313P)^2^+6.1654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1303
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2447
_reflns_number_total             4016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra02512k2.cif
_cod_data_source_block           C5_0m
_cod_original_cell_volume        2366.0(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7243037
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              73403