H-Bonding and intramolecular catalysis of proton exchange affect the CEST properties of Eu<sup>III</sup> complexes with HP-DO3A-like ligands.
Baroni, Simona; Carnovale, Irene Maria; Carrera, Carla; Boccalon, Mariangela; Guidolin, Nicol; Demitri, Nicola; Lattuada, Luciano; Tedoldi, Fabio; Baranyai, Zsolt; Aime, Silvio; Chemical communications (Cambridge, England) 57 (2021) 3287–3290; doi:10.1039/d1cc00366f

data_7127978
_publ_section_title
;
 H-Bonding and intramolecular catalysis of proton exchange affect the CEST
 properties of Eu<sup>III</sup> complexes with HP-DO3A-like ligands.
;
_journal_issue                   26
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3287
_journal_page_last               3290
_journal_paper_doi               10.1039/d1cc00366f
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C23 H32 Gd N4 O10 Na, 10.5 (H2 O)'
_chemical_formula_sum            'C23 H53 Gd N4 Na O20.5'
_chemical_formula_weight         893.93
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-12-31 deposited with the CCDC.	2021-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.01(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.550(4)
_cell_length_b                   17.234(3)
_cell_length_c                   24.922(5)
_cell_measurement_reflns_used    10183
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.999
_cell_measurement_theta_min      2.039
_cell_volume                     7245(3)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'Ortep3 for Windows - Coot'
_computing_publication_material  'enCIFer - publCIF'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
;
'Huber 4-circles Kappa Goniometer, Pilatus 2M detector'
;
_diffrn_measurement_method       'Rotating crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            111879
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         2.039
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.844
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       'Thick rods'
_exptl_crystal_F_000             3664
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.215
_refine_diff_density_min         -1.468
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       0.00287(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1268
_refine_ls_number_reflns         22004
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+10.3402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0756
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21919
_reflns_number_total             22004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00366f2.cif
_cod_data_source_block           PHC
_cod_depositor_comments
'Adding full bibliography for 7127978--7127979.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C23 H53 Gd N4 Na O20.50'
_cod_database_code               7127978
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.837
_shelx_estimated_absorpt_t_max   0.913
_shelx_res_checksum              52671
_shelx_hkl_checksum              83407