Mono- and dinuclear uranyl(VI) complexes with chiral Schiff base ligand
Giovanna Brancatelli; Andrea Pappalardo; Giuseppe Trusso Sfrazzetto; Anna Notti; Silvano Geremia; Inorganica Chimica Acta 396 (2013) 25–29; doi:10.1016/j.ica.2012.12.034

data_1512964
_publ_section_title
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 Mono- and dinuclear uranyl(VI) complexes with chiral Schiff base ligand
;
_journal_name_full
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Inorganica Chimica Acta
;
_journal_page_first              25
_journal_page_last               29
_journal_paper_doi               10.1016/j.ica.2012.12.034
_journal_volume                  396
_journal_year                    2013
_chemical_absolute_configuration rmad
_chemical_formula_moiety
'C86 H67 N2 O7 U, C140 H117 N4 O13 U2, 2(C4 H12 N), 1.3(C7), 1.05(C2O), 2(O)'
_chemical_formula_sum            'C245.2 H208 N8 O23.05 U3'
_chemical_formula_weight         4349.68
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6280(10)
_cell_length_b                   30.001(2)
_cell_length_c                   37.2050(10)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.5
_cell_volume                     21908.5(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7
_diffrn_reflns_av_unetI/netI     0.1031
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            40131
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    2.085
_exptl_absorpt_correction_T_min  0.6137
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             8782
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.291
_refine_diff_density_min         -1.04
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.011(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2460
_refine_ls_number_reflns         40131
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.078
_refine_ls_shift/su_mean         0.032
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0958P)^2^+1.0758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.16
_refine_ls_wR_factor_ref         0.171
_reflns_number_gt                34496
_reflns_number_total             40131
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ICA-2013-396-25-29.cif
_cod_data_source_block           uranyl-salen-pyrene
_cod_database_code               1512964