Ratiometric pH Imaging with a Co(II)2 MRI Probe via CEST Effects of Opposing pH Dependences.
Thorarinsdottir, Agnes E.; Du, Kang; Collins, James H. P.; Harris, T. David; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b08574

data_4126658
_publ_section_title
;
 Ratiometric pH Imaging with a Co(II)2 MRI Probe via CEST Effects of
 Opposing pH Dependences.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b08574
_journal_year                    2017
_chemical_formula_moiety
'C17 H25 Cl Co2 N7 Na O14 P2, 2(H2 O), 5.19(O)'
_chemical_formula_sum            'C17 H29 Cl Co2 N7 Na O21.19 P2'
_chemical_formula_weight         908.83
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.543(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1331(9)
_cell_length_b                   16.6578(17)
_cell_length_c                   22.867(2)
_cell_measurement_reflns_used    9454
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.775
_cell_measurement_theta_min      2.653
_cell_volume                     3472.3(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            106421
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.828
_diffrn_reflns_theta_min         2.163
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.230
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0716 before and 0.0472 after correction. The Ratio of minimum to maximum transmission is 0.9022. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_description       block
_exptl_crystal_F_000             1846
_exptl_crystal_recrystallization_method
'Dark orange blocks were grown by slow diffusion of MeCN vapor into a concentrated solution of the complex in water.'
_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.051
_refine_diff_density_max         1.435
_refine_diff_density_min         -1.706
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         10816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0522P)^2^+9.1265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1198
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10054
_reflns_number_total             10816
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08574_si_003.cif
_cod_data_source_block           aet27-work
_cod_original_cell_volume        3472.4(6)
_cod_database_code               4126658
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.905
_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. Uiso/Uaniso restraints and constraints
Uiso(O17) = Uiso(O17A)
3. Others
 Sof(Cl)=Sof(H17a)=1-FVAR(1)
 Sof(Cl1)=Sof(H17)=FVAR(1)
 Sof(O19A)=1-FVAR(2)
 Sof(O19)=FVAR(2)
 Sof(O20A)=1-FVAR(3)
 Sof(O20)=FVAR(3)
 Sof(O18A)=1-FVAR(4)
 Sof(O18)=FVAR(4)
 Sof(O16A)=1-FVAR(5)
 Sof(O16)=FVAR(5)
 Sof(O17A)=1-FVAR(6)
 Sof(O17)=FVAR(6)
4.a Free rotating group:
 O14(H14a,H14b), O21(H21a,H21b)
4.b Rotating group:
 O15(H15c,H15d)
4.c Ternary CH refined with riding coordinates:
 C17(H17), C17(H17a)
4.d Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C8(H8a,H8b), C10(H10a,H10b), C12(H12a,H12b), C13(H13a,H13b),
 C15(H15a,H15b)
4.e Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5)
4.f X=CH2 refined with riding coordinates:
 N2(H2a,H2b), N3(H3a,H3b), N5(H5a,H5b), N6(H6a,H6b)
;
_olex2_date_sample_completion    2017-05-22
_olex2_date_sample_data_collection 2017-05-21
_olex2_date_sample_submission    2017-05-21
_olex2_exptl_crystal_mounting_method
'The crystal was directly coated with Paratone-N oil and mounted under the stream of cold dinitrogen.'
_olex2_submission_original_sample_id AET5-135
_olex2_submission_special_instructions 'No special instructions were received'