Hexadentate Terephthalamide(bis-hydroxypyridinone) Ligands for Uranyl Chelation: Structural and Thermodynamic Consequences of Ligand Variation(1)
Géza Szigethy; Kenneth N. Raymond; Journal of the American Chemical Society 133 (2011) 7942–7956; doi:10.1021/ja201511u

data_4106153
_publ_section_title
;
 Hexadentate Terephthalamide(bis-hydroxypyridinone) Ligands for Uranyl
 Chelation: Structural and Thermodynamic Consequences of Ligand
 Variation(1)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7942
_journal_page_last               7956
_journal_paper_doi               10.1021/ja201511u
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C26 H24 N6 O12 U, 2(C4 H12 N), 2(C3 H6 O)'
_chemical_formula_sum            'C40 H60 N8 O14 U'
_chemical_formula_weight         1114.99
_chemical_name_common            'TAM(en-3,2-HOPO)2 uranyl complex'
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.686(3)
_cell_length_b                   17.686(3)
_cell_length_c                   14.605(3)
_cell_measurement_reflns_used    4281
_cell_measurement_temperature    144(2)
_cell_measurement_theta_max      20.544
_cell_measurement_theta_min      2.303
_cell_volume                     4568.4(14)
_computing_cell_refinement       'Saint v.7.07'
_computing_data_collection       'Bruker SMART v.6.531'
_computing_data_reduction        'Saint v.7.07'
_computing_molecular_graphics    'ORTEP-3 v.1.08, POV-Ray v3.6.1c.icl8.win32'
_computing_publication_material  'ORTEP-3 v.1.08, POV-Ray v3.6.1c.icl8.win32'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      144(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-I'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26113
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         2.30
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.626
_exptl_absorpt_correction_T_max  0.7132
_exptl_absorpt_correction_T_min  0.5614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       wedge
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.018(7)
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         4687
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0638
_reflns_number_gt                4080
_reflns_number_total             4687
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja201511u_si_002_6.cif
_cod_data_source_block           gs4058
_cod_original_cell_volume        4568.6(13)
_cod_database_code               4106153