Seven-Coordinate Co(II), Fe(II) and Six-Coordinate Ni(II) Amide-Appended Macrocyclic Complexes as ParaCEST Agents in Biological Media.
Olatunde, Abiola O.; Cox, Jordan M.; Daddario, Michael D.; Spernyak, Joseph A.; Benedict, Jason B.; Morrow, Janet R.; Inorganic chemistry 53 (2014) 8311–8321; doi:10.1021/ic5006083

data_4338413
_publ_section_title
;
 Seven-Coordinate Co(II), Fe(II) and Six-Coordinate Ni(II) Amide-Appended
 Macrocyclic Complexes as ParaCEST Agents in Biological Media.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8311
_journal_page_last               8321
_journal_paper_doi               10.1021/ic5006083
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C14 H28 Fe N4 O5, 2(C F3 O3 S)'
_chemical_formula_sum            'C16 H28 F6 Fe N4 O11 S2'
_chemical_formula_weight         686.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 92.5153(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7589(6)
_cell_length_b                   9.6358(4)
_cell_length_c                   18.4079(8)
_cell_measurement_temperature    90.0
_cell_volume                     2615.34(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 microfocus rotating anode'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            37095
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         33.239
_diffrn_reflns_theta_min         2.215
_diffrn_source                   'microfocus rotating anode'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.7131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0505 before and 0.0416 after correction.
The Ratio of minimum to maximum transmission is 0.9553.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_description       plate
_exptl_crystal_F_000             1408
_exptl_crystal_preparation
'L was prepared using a previously reported procedure.7 Metal salts were complexed to L in equimolar ratio in either ethanol (CoII), or acetonitrile (NiII), stirred at room temp for over 1 hour and isolated as previously reported.7,10 Fe(CF3SO3)2 and L were added under argon to prevent the oxidation of the free FeII to FeIII in solution. [Fe(L)]2+ was isolated as a slightly yellowish tan powder.'
_exptl_crystal_recrystallization_method
'grown over several days by vapor diffusion of hexane into acetonitrile'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         10026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+1.3759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0772
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7985
_reflns_number_total             10026
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5006083_si_002.cif
_cod_data_source_block           fe(l)
_cod_depositor_comments
'Adding full bibliography for 4338412--4338414.cif.'
_cod_database_code               4338413
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1A,H1B), C13(H13A,H13B), C6(H6A,H6B), C11(H11A,H11B), C9(H9A,
 H9B), C10(H10A,H10B), C4(H4C,H4D), C7(H7A,H7B), C8(H8A,H8B), C3(H3C,H3D),
 C5(H5A,H5B)
2.b X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N4(H4A,H4B)
;
_shelx_res_checksum              10456
_shelx_hkl_checksum              50334
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'