Isomeric Co(ii) paraCEST agents as pH responsive MRI probes.
Bond, Christopher J.; Cineus, Roy; Nazarenko, Alexander Y.; Spernyak, Joseph A.; Morrow, Janet R.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 279–284; doi:10.1039/c9dt04558a

data_7703127
_publ_section_title
;
 Isomeric Co(ii) paraCEST agents as pH responsive MRI probes.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              279
_journal_page_last               284
_journal_paper_doi               10.1039/c9dt04558a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C18 H36 Co N8 O4, 3(H2 O), C4 Co N4 S4'
_chemical_formula_sum            'C22 H42 Co2 N12 O7 S4'
_chemical_formula_weight         832.77
_chemical_name_systematic
'(2,2',2'',2'''-(1,4,8,11-Tetraazacyclotetradecane-1,4,8,11-tetrayl)tetraacetamide)-cobalt(ii) tetrathiocyanatocobaltate trihydrate.'
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-28 deposited with the CCDC.	2019-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                75.030(2)
_cell_angle_beta                 74.215(2)
_cell_angle_gamma                82.412(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0766(5)
_cell_length_b                   10.7225(6)
_cell_length_c                   17.5231(9)
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.90
_cell_measurement_theta_min      2.83
_cell_volume                     1756.18(16)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker PHOTON-100 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            76295
_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         26.623
_diffrn_reflns_theta_min         2.788
_diffrn_source                   sealedtube
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.240
_exptl_absorpt_correction_T_max  0.9109
_exptl_absorpt_correction_T_min  0.8256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0609 before and 0.0537 after correction.
The Ratio of minimum to maximum transmission is 0.9064.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ethanol'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   1
_exptl_transmission_factor_min   0.91
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7331
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0293P)^2^+1.9709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5582
_reflns_number_total             7331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04558a2.cif
_cod_data_source_block           mo_jm050817_0m
_cod_database_code               7703127
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.790
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups, All O(H,H,H) groups
2. Restrained distances
 O5-H5AA \\sim O5-H5BB \\sim O5-H5CC \\sim O6-H6AA \\sim O6-H6BB \\sim O6-H6CC
\\sim O7-H7AA \\sim O7-H7BB
 \\sim O7-H7CC
 with sigma of 0.02
3. Others
 Fixed Sof: H6BB(0.5) H6CC(0.5) H5BB(0.5) H5CC(0.5) H7BB(0.5) H7CC(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5C,H5D), C6(H6C,H6D),
 C7(H7C,H7D), C8(H8C,H8D), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B)
4.b X=CH2 refined with riding coordinates and stretchable bonds:
 N5(H5A,H5B), N6(H6A,H6B), N7(H7A,H7B), N8(H8A,H8B)
;
_shelx_res_checksum              77380
_olex2_submission_special_instructions 'No special instructions were received'