Redox-Inactive Metal Cations Modulate the Reduction Potential of the Uranyl Ion in Macrocyclic Complexes.
Kumar, Amit; Lionetti, Davide; Day, Victor; Blakemore, James D.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b11903

data_4134088
_publ_section_title
;
 Redox-Inactive Metal Cations Modulate the Reduction Potential of the
 Uranyl Ion in Macrocyclic Complexes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b11903
_journal_year                    2020
_chemical_formula_moiety         'C29 H34 F6 N4 O14 S2 U Y, C F3 O3 S'
_chemical_formula_sum            'C30 H34 F9 N4 O17 S3 U Y'
_chemical_formula_weight         1316.73
_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             2019-08-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                102.095(5)
_cell_angle_beta                 102.738(6)
_cell_angle_gamma                103.991(5)
_cell_formula_units_Z            2
_cell_length_a                   9.1814(6)
_cell_length_b                   13.6032(8)
_cell_length_c                   18.8769(12)
_cell_measurement_reflns_used    4780
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      69.826
_cell_measurement_theta_min      2.498
_cell_volume                     2143.6(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  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      199.99
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Bruker MicroStar microfocus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28130
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        66.000
_diffrn_reflns_theta_max         70.433
_diffrn_reflns_theta_min         2.498
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.767
_exptl_absorpt_correction_T_max  0.5526
_exptl_absorpt_correction_T_min  0.3888
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.040
_exptl_crystal_description       Chunk
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.025
_refine_diff_density_max         2.344
_refine_diff_density_min         -1.182
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         7605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0658P)^2^+5.3038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1326
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6180
_reflns_number_total             7605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11903_si_002.cif
_cod_data_source_block           L(salben)UO2Y
_cod_original_cell_volume        2143.6(2)
_cod_database_code               4134088
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.709
_shelx_estimated_absorpt_t_min   0.666
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C21(H21A,H21B), C13(H13A,H13B), C12(H12A,H12B), C11(H11A,
 H11B), C10(H10A,H10B), C9(H9A,H9B), C8(H8A,H8B), C24(H24A,H24B), C23(H23A,H23B)
2.b Me refined with riding coordinates:
 C25(H25A,H25B,H25C)
2.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C17(H17), C16(H16), C15(H15), C5(H5), C4(H4), C3(H3), C1(H1)
2.d Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC)
;
_olex2_submission_special_instructions 'No special instructions were received'