Macrocyclic transition-metal parashift complexes for MRI at clinical and pre-clinical magnetic fields.
Rogers, Nicola J.; Ashok Kumar, Chowan; Alexander, Carlson; Bowdery, Daniel; Pavlovskaya, Galina; Harvey, Peter; Dalton transactions (Cambridge, England : 2003) 54 (2025) 11036–11046; doi:10.1039/d5dt01149c

data_7718952
_publ_section_title
;
 Macrocyclic transition-metal parashift complexes for MRI at clinical and
 pre-clinical magnetic fields.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11036
_journal_page_last               11046
_journal_paper_doi               10.1039/d5dt01149c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C36 H50 Cu N8, 4(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C36 H50 Cl4 Cu N8 O17'
_chemical_formula_weight         1092.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-07-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2025-04-24 deposited with the CCDC.	2025-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                85.0880(10)
_cell_angle_beta                 83.0030(10)
_cell_angle_gamma                76.6270(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4580(2)
_cell_length_b                   12.5503(2)
_cell_length_c                   16.0052(2)
_cell_measurement_reflns_used    18105
_cell_measurement_temperature    100.05(16)
_cell_measurement_theta_max      67.0650
_cell_measurement_theta_min      2.8270
_cell_volume                     2218.55(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -28.00  23.00   0.50    0.05    --   45.38 -19.00-150.00  102
  2  \w    -30.00   8.00   0.50    0.05    --   45.38 -19.00 -90.00   76
  3  \w    -29.00  22.00   0.50    0.05    --   45.38 -19.00 -60.00  102
  4  \w    -28.00  -3.00   0.50    0.05    --   45.38 -19.00 -30.00   50
  5  \w     63.00 112.00   0.50    0.06    --  105.06-125.00 -90.00   98
  6  \w     53.00 126.00   0.50    0.06    --  105.06-144.00-111.00  146
  7  \w     66.00 104.00   0.50    0.05    --   45.38-144.00-111.00   76
  8  \w     81.00 107.00   0.50    0.06    --  105.06-126.00  56.00   52
  9  \w     32.00  57.00   0.50    0.05    --   45.38-126.00  56.00   50
 10  \w     32.00  57.00   0.50    0.06    --  105.06 -61.00 -90.00   50
 11  \w     33.00  59.00   0.50    0.06    --  105.06 -77.00-150.00   52
 12  \w     75.00 100.00   0.50    0.06    --  105.06 -77.00-150.00   50
 13  \w     42.00  67.00   0.50    0.06    --  105.06 -61.00 -60.00   50
 14  \w     45.00  92.00   0.50    0.06    --  105.06 -77.00  30.00   94
 15  \w     67.00 102.00   0.50    0.06    --  105.06 -77.00  60.00   70
 16  \w     93.00 119.00   0.50    0.06    --  105.06  45.00  90.00   52
 17  \w    131.00 168.00   0.50    0.06    --  105.06  45.00  90.00   74
 18  \w     96.00 148.00   0.50    0.06    --  105.06 126.00 133.00  104
 19  \w     63.00 109.00   0.50    0.05    --   45.38 144.00 -58.00   92
 20  \w     88.00 160.00   0.50    0.06    --  105.06  61.00 -60.00  144
 21  \w     92.00 117.00   0.50    0.06    --  105.06 144.00 -58.00   50
 22  \w   -116.00 -26.00   0.50    0.05    --  -45.38 -77.00  90.00  180
 23  \w   -161.00 -83.00   0.50    0.06    --  -97.00 -45.00 120.00  156
 24  \w   -169.00 -82.00   0.50    0.06    --  -97.00 -45.00  90.00  174
 25  \w   -111.00 -84.00   0.50    0.06    --  -97.00 -30.00-120.00   54
 26  \w   -167.00 -85.00   0.50    0.06    --  -97.00 -30.00-150.00  164
 27  \w   -169.00-120.00   0.50    0.06    --  -97.00 -30.00-120.00   98
 28  \w   -161.00-135.00   0.50    0.06    --  -97.00 -94.00-180.00   52
 29  \w   -123.00 -98.00   0.50    0.06    --  -97.00 -94.00-180.00   50
 30  \w   -139.00 -90.00   0.50    0.06    --  -97.00-144.00-111.00   98
 31  \w    -97.00 -69.00   0.50    0.05    --  -45.38-144.00-111.00   56
 32  \w   -149.00-124.00   0.50    0.06    --  -97.00-126.00  56.00   50
 33  \w    -53.00 -26.00   0.50    0.06    --  -97.00  45.00 -60.00   54
 34  \w    -72.00 -25.00   0.50    0.06    --  -97.00  61.00-180.00   94
 35  \w   -108.00 -42.00   0.50    0.06    --  -97.00  77.00 -60.00  132
 36  \w    -97.00 -56.00   0.50    0.06    --  -97.00  77.00 120.00   82
 37  \w    -50.00 -25.00   0.50    0.06    --  -97.00  45.00  90.00   50
 38  \w   -108.00 -28.00   0.50    0.06    --  -97.00 110.00 -46.70  160
 39  \w   -126.00 -88.00   0.50    0.06    --  -97.00 144.00 -58.00   76
 40  \w    -69.00 -44.00   0.50    0.05    --  -45.38 144.00 -58.00   50
 41  \w   -112.00 -80.00   0.50    0.06    --  -97.00 125.00   0.00   64
 42  \w   -108.00 -82.00   0.50    0.06    --  -97.00 125.00  90.00   52
 43  \w    -52.00 -27.00   0.50    0.06    --  -97.00 125.00  90.00   50
 44  \w   -110.00 -27.00   0.50    0.06    --  -97.00 126.00 133.00  166
 45  \w    -92.00 -27.00   0.50    0.05    --  -45.38 126.00 133.00  130
 46  \w    -76.00 -37.00   0.50    0.06    --  -97.00 125.00   0.00   78
;
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29200
_diffrn_reflns_theta_full        67.04
_diffrn_reflns_theta_max         67.04
_diffrn_reflns_theta_min         2.79
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.629
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1110
_exptl_crystal_size_max          0.602
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         7903
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+3.4240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1117
_reflns_number_gt                7148
_reflns_number_total             7903
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d5dt01149c2.cif
_cod_data_source_block           CuL2a
_cod_depositor_comments
'Adding full bibliography for 7718951--7718957.cif.'
_cod_database_code               7718952
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O006(H00L,H00M), O1(H1A,H1B)
2.b Secondary CH2 refined with riding coordinates:
 C00S(H00A,H00B), C00U(H00C,H00D), C00W(H00E,H00F), C00X(H00H,H00I), C00Z(H00J,
 H00K), C011(H01A,H01B), C016(H01C,H01D), C018(H01E,H01F), C019(H01G,H01H),
 C01B(H01I,H01J), C01C(H01K,H01L), C01L(H01W,H01X)
2.c Aromatic/amide H refined with riding coordinates:
 N00G(H00G), N00N(H00N), C010(H010), C013(H013), C015(H015), C01F(H01M),
 C01G(H01N), C01J(H01U), C01K(H01V), C01N(H01Y), C01O(H01Z), C01Q(H01),
 C01R(H0AA), C01T(H2AA)
2.d Idealised Me refined as rotating group:
 C01H(H01O,H01P,H01Q), C01I(H01R,H01S,H01T), C01S(H1AA,H,HA), C01U(H3AA,HB,HC)
;
_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
;