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_1570352
_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 H44 Ga N8 Ni O6, Br, C H4 O'
_chemical_formula_sum            'C33 H48 Br Ga N8 Ni O7'
_chemical_formula_weight         877.13
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-02-08
_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                 103.741(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.4737(12)
_cell_length_b                   14.7532(5)
_cell_length_c                   20.5922(8)
_cell_measurement_reflns_used    15592
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.4240
_cell_measurement_theta_min      3.7260
_cell_volume                     8697.9(6)
_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      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.913
_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     15.00  41.00   0.50   68.00    --    0.10  59.00-142.00   52
  2  \w    -28.00  -2.00   0.50   68.00    --    0.10 -59.00  77.00   52
  3  \w    -27.00   6.00   0.50   68.00    --    0.10 -82.00  60.00   66
  4  \w    -77.00 -50.00   0.50   68.00    --    0.10 -38.00 -60.00   54
  5  \w    -26.00   1.00   0.50   68.00    --    0.10 -82.00  30.00   54
  6  \w    -16.00  78.00   0.50   68.00    --    0.10  38.00-180.00  188
  7  \w    -13.00  65.00   0.50   68.00    --    0.10  38.00  90.00  156
  8  \w      6.00  31.00   0.50   68.00    --    0.10 -82.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_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  0.0484
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            58238
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.621
_diffrn_reflns_theta_min         3.525
_exptl_absorpt_coefficient_mu    2.020
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71947
_exptl_absorpt_correction_type   none
_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    1.340
_exptl_crystal_description       block
_exptl_crystal_F_000             3616
_refine_diff_density_max         0.756
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         11178
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+29.5569P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1254
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8612
_reflns_number_total             11178
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04770a2.cif
_cod_data_source_block           1122-ga-93-exp_1589_sq
_cod_depositor_comments
'Adding full bibliography for 1570350--1570352.cif.'
_cod_database_code               1570352
_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 N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Sof(Br2)=1-FVAR(1)
 Sof(Br1)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C12(H12A,H12B), C11(H11A,H11B), C10(H10A,H10B), C28(H28A,
 H28B), C9(H9A,H9B), C8(H8A,H8B), C20(H20A,H20B), C25(H25A,H25B), C24(H24A,
 H24B), C32(H32A,H32B), C23(H23A,H23B), C21(H21A,H21B), C22(H22A,H22B)
3.b Aromatic/amide H refined with riding coordinates:
 N8(H8), N5(H5), C7(H7), C14(H14), C17(H17), C3(H3)
3.c X=CH2 refined with riding coordinates:
 N7(H7A,H7B), N6(H6A,H6B)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C16(H16A,H16B,H16C), C33(H33A,H33B,H33C)
3.e Idealised tetrahedral OH refined as rotating group:
 O7(H7C)
;
_shelx_res_checksum              69225
_shelx_hkl_checksum              46714
_shelx_fab_checksum              99033
_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
;