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_1512875
_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_formula_moiety         'C54 H80 N2 O6 U, 2(C2 H3 N) '
_chemical_formula_sum            'C58 H86 N4 O6 U'
_chemical_formula_weight         1173.34
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                94.7380(10)
_cell_angle_beta                 104.7450(10)
_cell_angle_gamma                111.7950(10)
_cell_formula_units_Z            1
_cell_length_a                   9.4697(2)
_cell_length_b                   11.1762(3)
_cell_length_c                   15.0633(4)
_cell_measurement_reflns_used    4807
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.283
_cell_measurement_theta_min      0.407
_cell_volume                     1403.40(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_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    'SIR97 (Altomare, et. al. 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0663
_diffrn_reflns_av_sigmaI/netI    0.0700
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18102
_diffrn_reflns_theta_full        28.14
_diffrn_reflns_theta_max         28.14
_diffrn_reflns_theta_min         2.64
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    2.942
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_correction_T_min  0.531
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             602
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         6816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+4.6436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0922
_reflns_number_gt                6610
_reflns_number_total             6816
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            2007-3397_RS.txt
_cod_data_source_block           so117a=1
_cod_database_code               1512875
_exptl_absorpt_factor_mur        0.206
_exptl_absorpt_rmerge_before     0.0522
_exptl_absorpt_rmerge_after      0.0474