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_4106151
_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
;C32 H20 N6 O12 U, 2(C4 H12 N), 3(H2 O), C H4 O, /
3(C4 H8 O2)
;
_chemical_formula_sum            'C53 H78 N8 O22 U'
_chemical_formula_weight         1417.26
_chemical_name_common            'TAM(ophen-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                79.417(2)
_cell_angle_beta                 86.227(2)
_cell_angle_gamma                88.558(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2600(15)
_cell_length_b                   13.259(2)
_cell_length_c                   23.405(4)
_cell_measurement_reflns_used    2665
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      20.252
_cell_measurement_theta_min      3.302
_cell_volume                     2818.4(8)
_computing_cell_refinement       'SAINT v. 7.07'
_computing_data_collection       'Bruker SMART v. 5.059'
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      163(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker SMART 1000'
_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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0892
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            14330
_diffrn_reflns_theta_full        24.78
_diffrn_reflns_theta_max         24.78
_diffrn_reflns_theta_min         3.30
_exptl_absorpt_coefficient_mu    2.968
_exptl_absorpt_correction_T_max  0.9430
_exptl_absorpt_correction_T_min  0.5484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       plate
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
See Refinement special details for more detailed discussion.
;
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         9212
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0616P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1106
_reflns_number_gt                6822
_reflns_number_total             9212
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja201511u_si_002_4.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        2818.3(8)
_cod_database_code               4106151