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_7703126
_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, 2(C N S)'
_chemical_formula_sum            'C20 H36 Co N10 O4 S2'
_chemical_formula_weight         603.64
_chemical_name_systematic
'(2,2',2'',2'''-(1,4,8,11-Tetraazacyclotetradecane-1,4,8,11-tetrayl)tetraacetamide)-cobalt(ii) dithiocyanate.'
_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             2018-02-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-08-28 deposited with the CCDC.	2019-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.610(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7005(6)
_cell_length_b                   12.9672(11)
_cell_length_c                   11.9397(11)
_cell_measurement_reflns_used    1977
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.04
_cell_measurement_theta_min      3.05
_cell_volume                     1303.49(19)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       APEX2
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker PHOTON-100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            56834
_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         32.067
_diffrn_reflns_theta_min         2.885
_diffrn_source                   sealedtube
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.867
_exptl_absorpt_correction_T_max  0.9163
_exptl_absorpt_correction_T_min  0.8162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0527 before and 0.0486 after correction.
The Ratio of minimum to maximum transmission is 0.8908.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       block
_exptl_crystal_F_000             634
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ethanol'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   1
_exptl_transmission_factor_min   0.89
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         4540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0413P)^2^+0.4690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3978
_reflns_number_total             4540
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04558a2.cif
_cod_data_source_block           mo_jm042517_0m
_cod_database_code               7703126
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C009(H00E,H00F), C00B(H00G,H00H), C00C(H00I,H00J), C00D(H00K,H00L), C00F(H00M,
 H00N), C00G(H00O,H00P), C00H(H00Q,H00R)
;
_shelx_res_checksum              78893
_olex2_submission_special_instructions 'No special instructions were received'