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_4106154
_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         'C34 H24 N6 O12 U, 2(C4 H12 N), 2(C H4 O)'
_chemical_formula_sum            'C44 H56 N8 O14 U'
_chemical_formula_weight         1159.00
_chemical_name_common            'TAM(o-phen-3,2-HOPO)2 uranyl complex'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 108.948(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.970(2)
_cell_length_b                   12.5873(18)
_cell_length_c                   22.161(3)
_cell_measurement_reflns_used    4576
_cell_measurement_temperature    152(2)
_cell_measurement_theta_max      26.023
_cell_measurement_theta_min      2.444
_cell_volume                     4477.2(10)
_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      152(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12451
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         2.53
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.703
_exptl_absorpt_correction_T_max  0.8970
_exptl_absorpt_correction_T_min  0.5887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_description       rhombohedron
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.115
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4576
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0580
_reflns_number_gt                4114
_reflns_number_total             4576
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja201511u_si_002_7.cif
_cod_data_source_block           gs4019
_cod_original_cell_volume        4477.2(11)
_cod_database_code               4106154