Toward Inert Paramagnetic Ni(II)-Based Chemical Exchange Saturation Transfer MRI Agents
Caneda-Martínez, Laura; Laura, Valencia; Fernandez-Perez, Isabel; Regueiro-Figueroa, Martín; Angelovski, Goran; Brandariz, Isabel; Esteban-Gómez, David; Platas-Iglesias, Carlos; Dalton Trans.  (2017) –; doi:10.1039/C7DT02758C

data_7044397
_publ_section_title
;
 Toward Inert Paramagnetic Ni(II)-Based Chemical Exchange Saturation
 Transfer MRI Agents
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02758C
_journal_year                    2017
_chemical_formula_moiety         'C16 H22 F12 N6 Ni O3 P2'
_chemical_formula_sum            'C16 H22 F12 N6 Ni O3 P2'
_chemical_formula_weight         695.04
_chemical_name_systematic        '[Ni(H2dedpam)](PF6)2?H2O'
_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   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-07-27 deposited with the CCDC.
2017-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.100(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2296(8)
_cell_length_b                   16.2475(15)
_cell_length_c                   16.8968(15)
_cell_measurement_reflns_used    78952
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      47.910
_cell_measurement_theta_min      4.822
_cell_volume                     2533.3(4)
_computing_cell_refinement
'SAINT V7.68A (Bruker: Madison, 2009 ) in Apex2 suite.'
_computing_data_collection       'Apex2, Bruker Instrument Service v2010, 1-2'
_computing_data_reduction
'SAINT and XPREP Version 2008/2 (Sheldrick, Bruker AXS Inc.)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      102(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8 APEX'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            78952
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.259
_diffrn_reflns_theta_min         1.739
_exptl_absorpt_coefficient_mu    1.014
_exptl_absorpt_correction_T_max  0.8880
_exptl_absorpt_correction_T_min  0.6311
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS Version 2008/1 (Sheldrick, Bruker AXS Inc.)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: H2O'
_exptl_crystal_size_max          0.495
_exptl_crystal_size_mid          0.252
_exptl_crystal_size_min          0.115
_refine_diff_density_max         1.116
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5668
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0603
_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^)+(0.1106P)^2^+3.8448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1773
_refine_ls_wR_factor_ref         0.1860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4817
_reflns_number_total             5668
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02758c2.cif
_cod_data_source_block           shelx
_cod_database_code               7044397
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.634
_shelx_estimated_absorpt_t_max   0.892
_shelx_res_checksum              29238