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_4126659
_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         'C18 H26 Co2 N7 Na O16 P2, H2 O, 3.8(O)'
_chemical_formula_sum            'C18 H28 Co2 N7 Na O20.8 P2'
_chemical_formula_weight         878.06
_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                 94.827(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1253(9)
_cell_length_b                   16.6143(15)
_cell_length_c                   23.152(2)
_cell_measurement_reflns_used    9223
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.50
_cell_measurement_theta_min      2.639
_cell_volume                     3497.6(6)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT'
_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 0.952
_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  0.0728
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            130306
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.652
_diffrn_reflns_theta_min         0.883
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.143
_exptl_absorpt_correction_T_max  0.7330
_exptl_absorpt_correction_T_min  0.5917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1555 before and 0.1056 after correction. The Ratio of minimum to maximum transmission is 0.8072. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       block
_exptl_crystal_F_000             1786
_exptl_crystal_recrystallization_method
'Orange blocks were grown by slow diffusion of MeCN vapor into a concentrated solution of the complex in water'
_exptl_crystal_size_max          0.546
_exptl_crystal_size_mid          0.268
_exptl_crystal_size_min          0.128
_refine_diff_density_max         2.809
_refine_diff_density_min         -2.180
_refine_diff_density_rms         0.316
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         13616
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.939
_refine_ls_R_factor_all          0.1302
_refine_ls_R_factor_gt           0.1290
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3824
_refine_ls_wR_factor_ref         0.3852
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13346
_reflns_number_total             13616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08574_si_002.cif
_cod_data_source_block           aet26_p21-n
_cod_original_cell_volume        3497.7(6)
_cod_original_formula_sum        'C18 H28 Co2 N7 Na O20.80 P2'
_cod_database_code               4126659
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.574
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.646(3)
 0.354(3)
2. 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 C(H,H,H) groups, All O(H) groups, All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
O12 \\sim C18: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
O16 \\sim O16A: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
Uanis(O12) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(O16A) \\sim Ueq, Uanis(O16) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
4. Others
 Sof(O16A)=1-FVAR(1)
 Sof(O16)=FVAR(1)
 Fixed Sof: O21(0.2) O22(0.2) O23(0.2) O24(0.2)
5.a Free rotating group:
 O19(H19a,H19b)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C8(H8a,H8b), C10(H10a,H10b), C12(H12a,H12b), C13(H13a,H13b),
 C15(H15a,H15b)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5)
5.d X=CH2 refined with riding coordinates:
 N2(H2a,H2b), N3(H3a,H3b), N5(H5a,H5b), N6(H6a,H6b)
5.e Idealised Me refined as rotating group:
 C18(H18a,H18b,H18c)
5.f Idealised tetrahedral OH refined as rotating group:
 O12(H12)
;
_olex2_date_sample_completion    2017-05-01
_olex2_date_sample_data_collection 2017-04-30
_olex2_date_sample_submission    2017-04-30
_olex2_exptl_crystal_mounting_method
'Crystal was mounted in Paraton-N-oil and directly coated under the stream of cold nitrogen'
_olex2_submission_original_sample_id Na[LNO2Co2(etidronate)]
_olex2_submission_special_instructions 'No special instructions were received'