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_7713235
_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_absolute_configuration ad
_chemical_formula_moiety         'C14 H32 Co N4 O2, Cl4 Co'
_chemical_formula_sum            'C14 H32 Cl4 Co2 N4 O2'
_chemical_formula_weight         548.09
_chemical_name_systematic
;
1,1?-(1,4,7,10-tetraazacyclododecane-1,7-diyl)bis(propan-2-ol)cobalt(II) tetrachloridocobaltate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dualspace
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc25w82f
_audit_creation_date             2020-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-07 deposited with the CCDC.	2023-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8000(9)
_cell_length_b                   13.7390(14)
_cell_length_c                   15.4056(15)
_cell_measurement_reflns_used    3085
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.14
_cell_measurement_theta_min      2.97
_cell_volume                     2285.9(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 10.4
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker PHOTON-100 CMOS'
_diffrn_measurement_method       ' \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.997
_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       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            42350
_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         26.364
_diffrn_reflns_theta_min         3.032
_diffrn_source                   sealedtube
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.935
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0854 before and 0.0676 after correction.
The Ratio of minimum to maximum transmission is 0.7803.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile, ethanol'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   1
_exptl_transmission_factor_min   0.78
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 1453 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.036(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         4662
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0190P)^2^+0.6666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0569
_reflns_Friedel_coverage         0.767
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3809
_reflns_number_total             4662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01572f2.cif
_cod_data_source_block           mo_jm101616_0m
_cod_database_code               7713235
_shelx_shelxl_version_number     2018/3
_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, All O(H) groups
2. Restrained distances
 O1-H1
 0.85 with sigma of 0.03
 O2-H2
 0.85 with sigma of 0.03
3.a Ternary CH refined with riding coordinates:
 N2(H2A), N4(H4), C10(H10), C13(H13)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2B,H2C), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C12(H12A,H12B)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              46739
_olex2_submission_special_instructions 'No special instructions were received'