Aminoalkylbis(phenolate) [O,N,O] donor ligands for uranyl(VI) ion coordination: Syntheses, structures, and extraction studies
Harri Sopo; Kamal Goljahanpoor; Reijo Sillanpää; Polyhedron 26 (2007) 3397–3408; doi:10.1016/j.poly.2007.03.032

data_1512878
_publ_section_title
;
 Aminoalkylbis(phenolate) [O,N,O] donor ligands for uranyl(VI) ion
 coordination: Syntheses, structures, and extraction studies
;
_journal_issue                   13
_journal_name_full               Polyhedron
_journal_page_first              3397
_journal_page_last               3408
_journal_paper_doi               10.1016/j.poly.2007.03.032
_journal_volume                  26
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C60 H88 N2 O6 U1'
_chemical_formula_sum            'C60 H88 N2 O6 U'
_chemical_formula_weight         1171.35
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 98.1970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9942(2)
_cell_length_b                   25.7977(5)
_cell_length_c                   10.8009(3)
_cell_measurement_reflns_used    17694
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      0.407
_cell_measurement_wavelength     0.71073
_cell_volume                     2756.32(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.063
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20144
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         2.06
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    2.995
_exptl_absorpt_correction_T_max  0.787
_exptl_absorpt_correction_T_min  0.603
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Sheldrick, G.M. (anon) SHELX97 Release 97-2 (1998)
I/sigma threshold for reflections     =   5.000
Delta(U)/lambda**2                    =   0.000
Highest even order spherical harmonic =       6
Highest odd  order spherical harmonic =       3
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         6474
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+8.0740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0798
_reflns_number_gt                4507
_reflns_number_total             6474
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            2007-3397_RS.txt
_cod_data_source_block           so117db2=4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1512878
_exptl_absorpt_factor_mur        0.210
_exptl_absorpt_rmerge_before     0.0412
_exptl_absorpt_rmerge_after      0.0375