Uranyl sequestration: synthesis and structural characterization of uranyl complexes with a tetradentate methylterephthalamide ligand
Chengbao Ni; David K. Shuh; Kenneth N. Raymond; Chem.Commun. 47 (2011) 6392–; doi:10.1039/c1cc11329a

data_7106459
_publ_section_title
;
 Uranyl sequestration: synthesis and structural characterization of uranyl
 complexes with a tetradentate methylterephthalamide ligand
;
_journal_name_full               Chem.Commun.
_journal_page_first              6392
_journal_paper_doi               10.1039/c1cc11329a
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety
'C49.5 H64.5 O25.5 N8 U2 K4, 2(C4 H12 N) 2.5 (C H4 O), 1.5 (H2 O)'
_chemical_formula_sum            'C60 H101.5 K4 N10 O29.5 U2'
_chemical_formula_weight         2066.45
_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                105.053(2)
_cell_angle_beta                 94.779(2)
_cell_angle_gamma                102.429(2)
_cell_formula_units_Z            2
_cell_length_a                   9.9029(11)
_cell_length_b                   18.940(2)
_cell_length_c                   22.970(3)
_cell_measurement_reflns_used    9717
_cell_measurement_temperature    149(2)
_cell_measurement_theta_max      50.35
_cell_measurement_theta_min      2.44
_cell_volume                     4018.4(8)
_computing_cell_refinement       'SAINT (7.60A) (Bruker, 2008)'
_computing_data_collection       'Apex2 (2009-7) (Bruker, 2009)'
_computing_data_reduction        'SAINT (7.60A) (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      149(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            61989
_diffrn_reflns_theta_full        25.38
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_min         0.93
_exptl_absorpt_coefficient_mu    4.302
_exptl_absorpt_correction_T_max  0.711
_exptl_absorpt_correction_T_min  0.553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/2 (Sheldrick, 2008)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rod
_exptl_crystal_F_000             2085
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.223
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1065
_refine_ls_number_reflns         14601
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0221P)^2^+7.9502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0602
_reflns_number_gt                12984
_reflns_number_total             14601
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc11329a.txt
_cod_data_source_block           Monomer
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7106459