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_7127979
_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         'C22 H34 Gd N5 O8, 7 (H2 O)'
_chemical_formula_sum            'C22 H48 Gd N5 O15'
_chemical_formula_weight         779.90
_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
;
2021-01-01 deposited with the CCDC.	2021-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.97(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.237(4)
_cell_length_b                   17.179(3)
_cell_length_c                   23.059(5)
_cell_measurement_reflns_used    2677
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.752
_cell_measurement_theta_min      1.024
_cell_volume                     6872(3)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Elettra XRD2 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 0.991
_diffrn_measurement_device_type
;
'Arinax MD2s Goniometer, Pilatus 6M detector'
;
_diffrn_measurement_method       'Rotating crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.620
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            121338
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        21.839
_diffrn_reflns_theta_max         29.736
_diffrn_reflns_theta_min         1.024
_diffrn_source                   'Elettra Synchrotron - XRD2 BL'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.392
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       'Thick plates'
_exptl_crystal_F_000             3192
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.742
_refine_diff_density_min         -3.019
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     908
_refine_ls_number_reflns         29223
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1165P)^2^+5.7449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1849
_refine_ls_wR_factor_ref         0.2079
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19071
_reflns_number_total             29223
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00366f2.cif
_cod_data_source_block           PHN
_cod_depositor_comments
'Adding full bibliography for 7127978--7127979.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7127979
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.873
_shelx_estimated_absorpt_t_max   0.973
_shelx_res_checksum              33038
_shelx_hkl_checksum              15332
_shelx_fab_checksum              11764