Co(II) complexes of tetraazamacrocycles appended with amide or hydroxypropyl groups as paraCEST agents
Raymond, Jaclyn; Abozeid, Samira M.; Sokolow, Gregory Evan; Bond, Christopher J.; Yap, Constance E.; Nazarenko, Alexander Y.; Morrow, Janet; Dalton Transactions  (2023) –; doi:10.1039/D3DT01572F

data_7713236
_publ_section_title
;
 Co(II) complexes of tetraazamacrocycles appended with amide or
 hydroxypropyl groups as paraCEST agents
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01572F
_journal_year                    2023
_chemical_formula_moiety         'C28 H42 Co N6 O2, 2(Cl), 6(H2 O)'
_chemical_formula_sum            'C28 H54 Cl2 Co N6 O8'
_chemical_formula_weight         732.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-10
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-05-10 deposited with the CCDC.	2023-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.926(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9214(7)
_cell_length_b                   22.7525(13)
_cell_length_c                   14.3494(9)
_cell_measurement_reflns_used    9164
_cell_measurement_temperature    113.65
_cell_measurement_theta_max      30.596
_cell_measurement_theta_min      2.852
_cell_volume                     3539.7(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      113.65
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            85756
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.609
_diffrn_reflns_theta_min         2.852
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0644 before and 0.0508 after correction.
The Ratio of minimum to maximum transmission is 0.9044.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       block
_exptl_crystal_F_000             1556
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.0026(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         10903
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+2.6938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9481
_reflns_number_total             10903
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01572f2.cif
_cod_data_source_block           4
_cod_database_code               7713236
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.889
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Sof(O4B)=Sof(H4BA)=Sof(H4BB)=1-FVAR(1)
 Sof(O4A)=Sof(H4AA)=Sof(H4AB)=FVAR(1)
3.a Free rotating group:
 O8(H8C,H8D), O7(H7C,H7D), O3(H3C,H3D), O4A(H4AA,H4AB), O6(H6E,H6F), O5(H5E,
 H5F), O4B(H4BA,H4BB)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C18(H18A,H18B), C5(H5C,H5D), C20(H20A,H20B), C3(H3A,
 H3B), C11(H11A,H11B), C27(H27A,H27B), C6(H6C,H6D), C9(H9A,H9B), C7(H7A,H7B),
 C10(H10A,H10B), C4(H4A,H4B), C8(H8A,H8B)
3.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C26(H26), C17(H17), C13(H13), C23(H23), C25(H25), C24(H24),
 C14(H14), C16(H16), C15(H15)
3.d X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N6(H6A,H6B)
;
_shelx_res_checksum              49407
_olex2_submission_special_instructions 'No special instructions were received'