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_7718957
_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 Zn, 2(Cl O4)'
_chemical_formula_sum            'C27 H36 Cl2 N6 O8 Zn'
_chemical_formula_weight         708.89
_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             2025-04-24
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7221)
;
_audit_update_record
;
2025-04-24 deposited with the CCDC.	2025-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.4400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.0523(3)
_cell_length_b                   12.0637(2)
_cell_length_c                   33.9291(6)
_cell_measurement_reflns_used    9367
_cell_measurement_temperature    302.00
_cell_measurement_theta_max      30.405
_cell_measurement_theta_min      2.255
_cell_volume                     6159.12(19)
_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      302.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8V'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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            279151
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.164
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.030
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.6954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0976 before and 0.0418 after correction.
The Ratio of minimum to maximum transmission is 0.9310.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       block
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.950
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         14100
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0816P)^2^+5.1861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1408
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12980
_reflns_number_total             14100
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01149c2.cif
_cod_data_source_block           ZnL1a
_cod_depositor_comments
'Adding full bibliography for 7718951--7718957.cif.'
_cod_database_code               7718957
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.010
_shelx_estimated_absorpt_t_min   0.007
_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:
 C26(H26A,H26B), C1(H1A,H1B), C13(H13A,H13B), C5(H5A,H5B), C3(H3A,H3B), C2(H2A,
 H2B), C4(H4A,H4B), C32(H32A,H32B), C28(H28A,H28B), C31(H31A,H31B), C19(H19A,
 H19B), C29(H29A,H29B), C27(H27A,H27B), C38(H38A,H38B), C30(H30A,H30B), C6(H6A,
 H6B), C53(H53A,H53B), C46(H46A,H46B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C21(H21), C23(H23), C9(H9), C10(H10), C36(H36), C22(H22), C34(H34),
 C48(H48), C17(H17), C50(H50), C35(H35), C41(H41), C49(H49), C15(H15), C16(H16),
  C43(H43), C42(H42)
2.c Idealised Me refined as rotating group:
 C01H(H01A,H01B,H01C), C39(H39A,H39B,H39C), C12(H12A,H12B,H12C), C01X(H01D,
 H01E,H01F), C52(H52A,H52B,H52C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              67212
_shelx_hkl_checksum              44016
_olex2_submission_special_instructions 'No special instructions were received'