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_7718953
_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 Cu N6, 2(Cl O4)'
_chemical_formula_sum            'C27 H36 Cl2 Cu N6 O8'
_chemical_formula_weight         707.06
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-05-30
_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                90.00
_cell_angle_beta                 91.6010(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.0287(3)
_cell_length_b                   11.9831(2)
_cell_length_c                   33.9757(7)
_cell_measurement_reflns_used    9594
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      28.91
_cell_measurement_theta_min      2.57
_cell_volume                     6116.3(2)
_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      300.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0142
_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       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            306170
_diffrn_reflns_theta_full        27.89
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         2.08
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_T_max  0.0096
_exptl_absorpt_correction_T_min  0.0078
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2936
_exptl_crystal_size_max          0.608
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         14604
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0688P)^2^+5.0707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1348
_reflns_number_gt                13547
_reflns_number_total             14604
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d5dt01149c2.cif
_cod_data_source_block           CuL1a
_cod_depositor_comments
'Adding full bibliography for 7718951--7718957.cif.'
_cod_database_code               7718953
_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:
 C00P(H00A,H00B), C00U(H,HA), C00Z(H00C,H00D), C013(H01A,H01B), C014(H01C,
 H01D), C016(HB,HC), C018(H01E,H01F), C01A(H01G,H01H), C01C(HD,HE), C01E(H01M,
 H01N), C01F(H01O,H01P), C01H(HG,HH), C01J(HI,HJ), C01K(H01Q,H01R), C01M(HL,HM),
  C01N(HN,HO), C01T(HQ,HR), C01X(HV,HW)
2.b Aromatic/amide H refined with riding coordinates:
 C00R(H00R), C01B(H01I), C01G(HF), C01L(HK), C01O(H01S), C01P(HP), C01Q(H01T),
 C01S(H01X), C01V(H01Y), C01W(H01Z), C01Y(HX), C01Z(HY), C020(HZ), C021(H0AA),
 C024(H024), C026(H4AA), C027(H5AA), C029(H029)
2.c Idealised Me refined as rotating group:
 C01D(H01J,H01K,H01L), C01R(H01U,H01V,H01W), C01U(HS,HT,HU), C022(H1AA,H2AA,
 H3AA), C025(H02A,H02B,H02C), C028(H6AA,H7AA,H8AA)
;
_olex2_submission_special_instructions 'No special instructions were received'