Stable and inert macrocyclic cobalt(II) and nickel(II) complexes with paraCEST response.
Pérez-Lourido, Paulo; Madarasi, Enikő; Antal, Fanni; Esteban-Gómez, David; Wang, Gaoji; Angelovski, Goran; Platas-Iglesias, Carlos; Tircsó, Gyula; Valencia, Laura; Dalton transactions (Cambridge, England : 2003) 51 (2022) 1580–1593; doi:10.1039/d1dt03217h

data_7709137
_publ_section_title
;
 Stable and inert macrocyclic cobalt(II) and nickel(II) complexes with
 paraCEST response.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1580
_journal_page_last               1593
_journal_paper_doi               10.1039/d1dt03217h
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C15 H24 N6 Ni O2, 2(Cl O4)'
_chemical_formula_sum            'C15 H24 Cl2 N6 Ni O10'
_chemical_formula_weight         578.01
_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     dual
_audit_creation_date             2021-09-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-07 deposited with the CCDC.	2021-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                66.997(2)
_cell_angle_beta                 78.831(2)
_cell_angle_gamma                85.433(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2809(6)
_cell_length_b                   10.4879(6)
_cell_length_c                   11.4557(7)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    116(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.55
_cell_volume                     1115.45(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      115.92
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Incoatec HeliosTM multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            43397
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.336
_diffrn_reflns_theta_min         2.264
_exptl_absorpt_coefficient_mu    1.176
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1254 before and 0.0384 after correction. The Ratio of minimum to maximum transmission is 0.8601. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.185
_refine_diff_density_max         1.554
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0364P)^2^+1.6665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0798
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5358
_reflns_number_total             5553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03217h2.cif
_cod_data_source_block           32037901_0m
_cod_depositor_comments
'Adding full bibliography for 7709136--7709139.cif.'
_cod_database_code               7709137
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.812
_shelx_estimated_absorpt_t_min   0.780
_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
2.a Ternary CH refined with riding coordinates:
 N3(H3A)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,
 H11B), C12(H12A,H12B), C14(H14A,H14B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4)
2.d X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N6(H6C,H6D)
;
_shelx_res_checksum              12963
_shelx_hkl_checksum              84927
_olex2_submission_special_instructions 'No special instructions were received'