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_4106148
_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 H18 N4 O9 S U, 0.125(C H4 O)'
_chemical_formula_sum            'C20.13 H18.5 N4 O9.13 S U'
_chemical_formula_weight         732.48
_chemical_name_common            'o-phen(1,2-HOPO)2 uranyl 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                62.678(2)
_cell_angle_beta                 89.739(2)
_cell_angle_gamma                86.387(3)
_cell_formula_units_Z            4
_cell_length_a                   8.2812(13)
_cell_length_b                   17.169(3)
_cell_length_c                   18.399(3)
_cell_measurement_reflns_used    2964
_cell_measurement_temperature    176(2)
_cell_measurement_theta_max      22.748
_cell_measurement_theta_min      2.378
_cell_volume                     2318.6(7)
_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      176(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0624
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13925
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         2.21
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.151
_exptl_absorpt_correction_T_max  0.8141
_exptl_absorpt_correction_T_min  0.4343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.098
_exptl_crystal_description       plate
_exptl_crystal_F_000             1393
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.795
_refine_diff_density_min         -2.418
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         8335
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1116
_reflns_number_gt                6026
_reflns_number_total             8335
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja201511u_si_002_1.cif
_cod_data_source_block           orth1h2
_cod_original_cell_volume        2318.6(6)
_cod_original_formula_sum        'C20.13 H18.50 N4 O9.13 S U'
_cod_database_code               4106148