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_4106149
_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
'C20 H20 N6 O12 U, 4.35(C4 H8 O2), 0.15(C2 H6 O S), C H4 O, 2(C4 H12 N)'
_chemical_formula_sum            'C58.7 H83.7 N8 O21.85 S0.15 U'
_chemical_formula_weight         1493.88
_chemical_name_common            'TAM(ophen-1,2-HOPO)2, uranly complex'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.075(2)
_cell_angle_beta                 95.478(3)
_cell_angle_gamma                91.560(3)
_cell_formula_units_Z            2
_cell_length_a                   9.7996(14)
_cell_length_b                   17.047(2)
_cell_length_c                   19.030(3)
_cell_measurement_reflns_used    1648
_cell_measurement_temperature    154(2)
_cell_measurement_theta_max      18.091
_cell_measurement_theta_min      2.259
_cell_volume                     3090.9(8)
_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      154(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0501
_diffrn_reflns_av_sigmaI/netI    0.0917
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12833
_diffrn_reflns_theta_full        21.32
_diffrn_reflns_theta_max         21.32
_diffrn_reflns_theta_min         2.26
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.716
_exptl_absorpt_correction_T_max  0.9230
_exptl_absorpt_correction_T_min  0.7364
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       plate
_exptl_crystal_F_000             1522
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.386
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         6860
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0796P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1364
_reflns_number_gt                5437
_reflns_number_total             6860
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja201511u_si_002_2.cif
_cod_data_source_block           gs4053
_cod_original_cell_volume        3090.8(8)
_cod_original_formula_sum        'C58.70 H83.70 N8 O21.85 S0.15 U'
_cod_database_code               4106149