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_7709136
_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 H26 Co N6 O3, 2(F6 P), H2 O'
_chemical_formula_sum            'C15 H28 Co F12 N6 O4 P2'
_chemical_formula_weight         705.30
_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   mixed
_atom_sites_solution_primary     iterative
_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                 99.614(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4836(7)
_cell_length_b                   19.3332(13)
_cell_length_c                   13.5320(9)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.51
_cell_volume                     2704.2(3)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.01
_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  0.0399
_diffrn_reflns_av_unetI/netI     0.0243
_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       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            52383
_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         28.355
_diffrn_reflns_theta_min         2.514
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.269
_exptl_crystal_size_mid          0.263
_exptl_crystal_size_min          0.253
_refine_diff_density_max         2.530
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         6736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0577P)^2^+7.9402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1341
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5792
_reflns_number_total             6736
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03217h2.cif
_cod_data_source_block           32018601_0m
_cod_depositor_comments
'Adding full bibliography for 7709136--7709139.cif.'
_cod_database_code               7709136
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.810
_shelx_estimated_absorpt_t_min   0.800
_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
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O2W(H2WA,H2WB)
2.b Rotating group:
 O1W(H1WA)
2.c Ternary CH refined with riding coordinates:
 N3(H3A)
2.d 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.e Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4)
2.f X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N6(H6C,H6D)
;
_shelx_res_checksum              37922
_shelx_hkl_checksum              5861
_olex2_submission_special_instructions 'No special instructions were received'