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_7709138
_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_absolute_configuration ad
_chemical_formula_moiety         'C23 H40 N6 Ni O2, 2(F6 P)'
_chemical_formula_sum            'C23 H40 F12 N6 Ni O2 P2'
_chemical_formula_weight         781.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-11
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9022(6)
_cell_length_b                   12.0154(4)
_cell_length_c                   16.8911(5)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.44
_cell_volume                     3227.40(19)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0310
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            48068
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.358
_diffrn_reflns_theta_min         2.412
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.803
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0724 before and 0.0445 after correction. The Ratio of minimum to maximum transmission is 0.9253. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 3462 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         8011
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0242
_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^)+(0.0302P)^2^+0.9384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0559
_refine_ls_wR_factor_ref         0.0568
_reflns_Friedel_coverage         0.924
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                7622
_reflns_number_total             8011
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03217h2.cif
_cod_data_source_block           32025901_0r
_cod_depositor_comments
'Adding full bibliography for 7709136--7709139.cif.'
_cod_database_code               7709138
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.854
_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
2.a Ternary CH refined with riding coordinates:
 N3(H3)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C7(H7A,H7B), C11(H11A,H11B), C9(H9A,H9B), C10(H10A,H10B),
 C18(H18A,H18B), C12(H12A,H12B), C6(H6A,H6B)
2.c Aromatic/amide H refined with riding coordinates:
 N5(H5), N6(H6), C3(H3A), C4(H4), C2(H2)
2.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C22(H22A,H22B,
 H22C), C21(H21A,H21B,H21C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              28648
_shelx_hkl_checksum              46299
_olex2_submission_special_instructions 'No special instructions were received'