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_1570351
_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(C2 H3 O2), H2 O, 2(C H4 O)'
_chemical_formula_sum            'C38 H62 N8 Ni2 O13'
_chemical_formula_weight         956.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-11-04
_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                 111.493(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3815(5)
_cell_length_b                   18.3733(4)
_cell_length_c                   16.7250(5)
_cell_measurement_reflns_used    16515
_cell_measurement_temperature    99.85(10)
_cell_measurement_theta_max      30.0230
_cell_measurement_theta_min      4.0320
_cell_volume                     4398.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_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 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -63.00   5.10   0.30   12.00    --    0.10 -82.00  30.00  227
  2  \w    -40.00  29.90   0.30   12.00    --    0.10 -82.00 120.00  233
  3  \w    -62.00  -8.90   0.30   12.00    --    0.10 -57.00  30.00  177
  4  \w     36.00  89.10   0.30   12.00    --    0.10  38.00  90.00  177
  5  \w    -49.00 -22.90   0.30   12.00    --    0.10 -82.00-180.00   87
  6  \w    -65.00 -40.70   0.30   12.00    --    0.10 -77.00-120.00   81
  7  \w     45.00  78.00   0.30   12.00    --    0.10  38.00 120.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28956
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.739
_diffrn_reflns_theta_min         3.584
_exptl_absorpt_coefficient_mu    0.927
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+9.7242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0882
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5261
_reflns_number_total             5711
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04770a2.cif
_cod_data_source_block           1102-ni2-z_sq_sq
_cod_depositor_comments
'Adding full bibliography for 1570350--1570352.cif.'
_cod_database_code               1570351
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Others
 Sof(H9BC)=Sof(H9BD)=Sof(H12C)=Sof(H12D)=Sof(C10)=Sof(H10A)=Sof(H10B)=1-FVAR(1)
 Sof(H9AA)=Sof(H9AB)=Sof(H12A)=Sof(H12B)=Sof(C11)=Sof(H11A)=Sof(H11B)=FVAR(1)
 Fixed Sof: O8(0.5) H8C(0.5) H8D(0.5) O7(0.5) H7A(0.5) O6(0.5) H6(0.5)
 C20(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5)
3.a Free rotating group:
 O8(H8C,H8D)
3.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C8(H8A,H8B), C9(H9AA,H9AB), C9(H9BC,H9BD),
 C17(H17A,H17B), C12(H12A,H12B), C12(H12C,H12D), C11(H11A,H11B), C10(H10A,H10B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7)
3.d X=CH2 refined with riding coordinates:
 N4(H4A,H4B), N3(H3A,H3B)
3.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
3.f Idealised tetrahedral OH refined as rotating group:
 O7(H7A), O6(H6)
;
_shelx_res_checksum              9965
_shelx_hkl_checksum              39706
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;