Improving the potential of paraCEST through magnetic-coupling induced line sharpening.
Guo, Xin; Zhang, Lei; Hu, Jiesheng; Szilágyi, Balázs; Yu, Meng; Chen, Shizhen; Tircsó, Gyula; Zhou, Xin; Tao, Jun; Chemical science 14 (2023) 14157–14165; doi:10.1039/d3sc04770a

data_1570350
_publ_section_title
;
 Improving the potential of paraCEST through magnetic-coupling induced
 line sharpening.
;
_journal_issue                   48
_journal_name_full               'Chemical science'
_journal_page_first              14157
_journal_page_last               14165
_journal_paper_doi               10.1039/d3sc04770a
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C32 H46 N8 Ni2 O6, 2(Cl), 3(H2 O)'
_chemical_formula_sum            'C32 H52 Cl2 N8 Ni2 O9'
_chemical_formula_weight         881.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-10-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-08-30 deposited with the CCDC.	2023-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.111(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2398(4)
_cell_length_b                   15.3856(6)
_cell_length_c                   12.1399(4)
_cell_measurement_reflns_used    6897
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5660
_cell_measurement_theta_min      4.2810
_cell_volume                     1870.02(12)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25225
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.664
_diffrn_reflns_theta_min         3.555
_exptl_absorpt_coefficient_mu    1.213
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       block
_exptl_crystal_F_000             924
_refine_diff_density_max         1.770
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0564
_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^)+(0.1070P)^2^+1.6509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
_refine_ls_wR_factor_ref         0.1715
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3927
_reflns_number_total             4760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04770a2.cif
_cod_data_source_block           111
_cod_depositor_comments
'Adding full bibliography for 1570350--1570352.cif.'
_cod_database_code               1570350
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Others
 Fixed Sof: O5(0.5) HB(0.5) HC(0.5)
2.a Free rotating group:
 O4(H,HA), O5(HB,HC)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C14(H14A,H14B), C16(H16A,H16B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7)
2.d X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N4(H4A,H4B)
2.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              31178
_shelx_hkl_checksum              23715
_olex2_submission_special_instructions 'No special instructions were received'