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_7243038
_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            'C252 H324 Cl18 Co9 N36 O98.25'
_chemical_formula_weight         6597.92
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   24.0755(8)
_cell_length_b                   24.0755(8)
_cell_length_c                   29.5779(10)
_cell_measurement_reflns_used    4088
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.00
_cell_volume                     14847.3(9)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.992
_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  0.0300
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            64451
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.403
_diffrn_reflns_theta_min         2.066
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6846
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.115
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         6727
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1291
_refine_ls_R_factor_gt           0.1016
_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^)+(0.1514P)^2^+199.5606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2669
_refine_ls_wR_factor_ref         0.3032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5170
_reflns_number_total             6727
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra02512k2.cif
_cod_data_source_block           AC35_2_0m
_cod_original_cell_volume        14847.3(11)
_cod_database_code               7243038
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              74192