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_4134083
_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         'C27 H33 Ba F6 N3 O12 S2'
_chemical_formula_sum            'C27 H33 Ba F6 N3 O12 S2'
_chemical_formula_weight         907.02
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   difmap
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.9261(6)
_cell_length_b                   17.1581(9)
_cell_length_c                   37.691(2)
_cell_measurement_reflns_used    9239
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      68.509
_cell_measurement_theta_min      4.678
_cell_volume                     7066.0(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2'
_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)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      199.99
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker Platinum 135 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  0.0614
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            39237
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        66.000
_diffrn_reflns_theta_max         68.503
_diffrn_reflns_theta_min         4.678
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.704
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.4050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1297 before and 0.0817 after correction. The Ratio of minimum to maximum transmission is 0.5378. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_description       Square
_exptl_crystal_F_000             3632
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         6423
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0510P)^2^+7.9915P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1008
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5820
_reflns_number_total             6423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11903_si_002.cif
_cod_data_source_block           L(salben)Ba
_cod_original_cell_volume        7065.9(7)
_cod_database_code               4134083
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.740
_shelx_estimated_absorpt_t_min   0.326
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'