Gear Up for a pH Shift: A Responsive Iron(II) 2-Amino-6-picolyl-Appended Macrocyclic paraCEST Agent That Protonates at a Pendent Group.
Tsitovich, Pavel B.; Cox, Jordan M.; Spernyak, Joseph A.; Morrow, Janet R.; Inorganic chemistry 55 (2016) 12001–12010; doi:10.1021/acs.inorgchem.6b02159

data_4349240
_publ_section_title
;
 Gear Up for a pH Shift: A Responsive Iron(II) 2-Amino-6-picolyl-Appended
 Macrocyclic paraCEST Agent That Protonates at a Pendent Group.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12001
_journal_page_last               12010
_journal_paper_doi               10.1021/acs.inorgchem.6b02159
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C32 H45 Co N12, Cl4 Co, Cl, 2(H2 O)'
_chemical_formula_sum            'C32 H49 Cl5 Co2 N12 O2'
_chemical_formula_weight         928.94
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.7293(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7544(5)
_cell_length_b                   14.9885(6)
_cell_length_c                   23.5529(8)
_cell_measurement_reflns_used    7126
_cell_measurement_temperature    90
_cell_measurement_theta_max      26.381
_cell_measurement_theta_min      2.328
_cell_volume                     4140.8(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      90
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_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  0.0469
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31091
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.385
_diffrn_reflns_theta_min         1.611
_diffrn_source                   'microfocus rotating anode'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.170
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1038 before and 0.0459 after correction.
The Ratio of minimum to maximum transmission is 0.9532.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       prism
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.719
_refine_diff_density_min         -1.203
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         8400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0691P)^2^+11.1738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1440
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6548
_reflns_number_total             8400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02159_si_002.cif
_cod_data_source_block           jmc_041607_0m
_cod_database_code               4349240
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O1(H1C,H1D), O2(H2A,H2B)
2.b Rotating group:
 N6(H6A,H6B), N10(H10A,H10B), N12(H12A,H12B)
2.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C15(H15A,H15B), C16(H16A,
 H16B), C17(H17A,H17B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C31(H31A,H31B), C32(H32A,H32B)
2.d Aromatic/amide H refined with riding coordinates:
 N7(H7), C3(H3), C4(H4), C5(H5), C11(H11), C12(H12), C13(H13), C19(H19),
 C20(H20), C21(H21), C27(H27), C28(H28), C29(H29)
2.e X=CH2 refined with riding coordinates:
 N8(H8C,H8D)
;
_shelx_res_checksum              14991
_shelx_hkl_checksum              40793
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'