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_7718956
_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         'C27 H36 N6 Ni, 2(Cl O4)'
_chemical_formula_sum            'C27 H36 Cl2 N6 Ni O8'
_chemical_formula_weight         702.23
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2024-08-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-04-24 deposited with the CCDC.	2025-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.670(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.8189(7)
_cell_length_b                   11.8401(5)
_cell_length_c                   33.4481(15)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      24.90
_cell_measurement_theta_min      2.27
_cell_volume                     5866.2(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1410
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            152269
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.522
_diffrn_reflns_theta_min         1.810
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0986 before and 0.0846 after correction.
The Ratio of minimum to maximum transmission is 0.8738.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic bluish blue'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       needle
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.602
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.237
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         13477
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.237
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0883
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+40.8697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1550
_refine_ls_wR_factor_ref         0.1632
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10780
_reflns_number_total             13477
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01149c2.cif
_cod_data_source_block           NiL1a
_cod_depositor_comments
'Adding full bibliography for 7718951--7718957.cif.'
_cod_database_code               7718956
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.612
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00V(H00A,H00B), C00Z(H00C,H00D), C011(H01P,H01Q), C012(H01R,H01S), C019(H01A,
 H01B), C01D(H01D,H01E), C01E(H01V,H01X), C01H(H01F,H01G), C01J(H01Z,H),
 C01O(H01,HA), C01P(H01L,H01M), C01R(H01N,H01O), C01V(H3,HF), C020(H02A,H02B),
 C024(H02U,H02V), C025(H02C,H02D), C026(H02E,H02F), C027(H02G,H02H)
2.b Aromatic/amide H refined with riding coordinates:
 C013(H013), C014(H014), C015(H015), C017(H017), C01A(H01T), C01B(H01C),
 C01C(H01U), C01I(H01Y), C01K(H01K), C01W(H01W), C01X(H4), C01Y(H5), C01Z(H6),
 C021(H021), C028(H028), C02C(H02L), C02E(H02P), C02G(H02Q)
2.c Idealised Me refined as rotating group:
 C01M(H01H,H01I,H01J), C01S(H1,HB,HC), C01U(H2,HD,HE), C022(H02R,H02S,H02T),
 C029(H02I,H02J,H02K), C02D(H02M,H02N,H02O)
;
_shelx_res_checksum              88358
_shelx_hkl_checksum              64613
_olex2_submission_special_instructions 'No special instructions were received'