A Cu(II)2 Paramagnetic Chemical Exchange Saturation Transfer Contrast Agent Enabled by Magnetic Exchange Coupling.
Du, Kang; Harris, T. David; Journal of the American Chemical Society 138 (2016) 7804–7807; doi:10.1021/jacs.6b03060

data_4130412
_publ_section_title
;
 A Cu(II)2 Paramagnetic Chemical Exchange Saturation Transfer Contrast
 Agent Enabled by Magnetic Exchange Coupling.
;
_journal_issue                   25
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7804
_journal_page_last               7807
_journal_paper_doi               10.1021/jacs.6b03060
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety
'C17 H23 Cu2 K N6 O15.5 P2, C17 H25 Cu2 N6 O12 P2, N O3, 2.5(O1)'
_chemical_formula_sum            'C34 H62 Cu4 K N13 O33 P4'
_chemical_formula_weight         1598.10
_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   geom
_audit_creation_date             2016-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                106.880(4)
_cell_angle_beta                 91.828(4)
_cell_angle_gamma                90.151(4)
_cell_formula_units_Z            2
_cell_length_a                   10.4003(9)
_cell_length_b                   16.0666(13)
_cell_length_c                   21.6870(18)
_cell_measurement_reflns_used    9807
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.54
_cell_volume                     3465.7(5)
_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  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.04
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            54176
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.972
_diffrn_reflns_theta_min         1.401
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.452
_exptl_absorpt_correction_T_max  27.90
_exptl_absorpt_correction_T_min  2.54
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear brownish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       plate
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.077
_refine_diff_density_max         2.481
_refine_diff_density_min         -2.570
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     791
_refine_ls_number_reflns         16420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0705
_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^)+(0.1265P)^2^+11.9577P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2074
_refine_ls_wR_factor_ref         0.2169
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12964
_reflns_number_total             16420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b03060_si_002.cif
_cod_data_source_block           H[LCu2(P2O7)]
_cod_database_code               4130412
_shelx_estimated_absorpt_t_max   0.896
_shelx_estimated_absorpt_t_min   0.761
_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 C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uiso(O2AA) = Uiso(O4AA)
Uiso(O1) = Uiso(O3AA)
Uiso(O0AA) = Uiso(O0AB)
3. Others
 Sof(O4AA)=1-FVAR(1)
 Sof(O2AA)=FVAR(1)
 Sof(O6AB)=1-FVAR(2)
 Sof(O6AA)=FVAR(2)
 Sof(O0AB)=1-FVAR(3)
 Sof(O0AA)=FVAR(3)
 Sof(O1A)=1-FVAR(4)
 Sof(O1)=FVAR(4)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C5(H5C,H5D), C13(H13A,H13B), C16(H16A,H16B),
 C19(H19A,H19B), C21(H21A,H21B), C22(H22A,H22B), C30(H30A,H30B), C31(H31A,H31B),
  C33(H33A,H33B)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10), C24(H24), C27(H27)
4.c X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N3(H3A,H3B), N5(H5A,H5B), N6(H6A,H6B), N7(H7A,H7B), N8(H8A,H8B),
 N11(H11A,H11B), N12(H12A,H12B)
4.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              81043
_shelx_hkl_checksum              37444
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'