Selective complexation of uranium(iii) over cerium(iii) by 2,6-bis(5,6-dialkyl-1,2,4-triazin-3-yl)pyridines: 1H NMR and X-ray crystallography studies
Iveson, Peter B.; Rivière, Christelle; Nierlich, Martine; Thuéry, Pierre; Ephritikhine, Michel; Guillaneux, Denis; Madic, Charles; Chemical Communications  (2001) 1512–; doi:10.1039/b103606h

data_7114795
_publ_section_title
;
 Selective complexation of uranium(iii) over cerium(iii) by
 2,6-bis(5,6-dialkyl-1,2,4-triazin-3-yl)pyridines: 1H NMR and X-ray
 crystallography studies
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_journal_issue                   16
_journal_name_full               'Chemical Communications'
_journal_page_first              1512
_journal_paper_doi               10.1039/b103606h
_journal_year                    2001
_chemical_formula_sum            'C89 H113 I3 N25 U'
_chemical_formula_weight         2151.77
_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                80.601(4)
_cell_angle_beta                 88.755(4)
_cell_angle_gamma                83.588(5)
_cell_formula_units_Z            2
_cell_length_a                   13.4305(10)
_cell_length_b                   16.5088(12)
_cell_length_c                   21.1404(15)
_cell_measurement_reflns_used    28304
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      5.10
_cell_volume                     4595.4(6)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD software (Nonius B.V., 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 0.881
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '\f 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  0.0928
_diffrn_reflns_av_sigmaI/netI    0.1027
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28304
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         5.10
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    2.832
_exptl_absorpt_correction_T_max  0.654
_exptl_absorpt_correction_T_min  0.417
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent dark brown'
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_meas      ?
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2146
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.629
_refine_diff_density_min         -1.354
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       0.0053(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1011
_refine_ls_number_reflns         15377
_refine_ls_number_restraints     346
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.2153
_refine_ls_R_factor_gt           0.0840
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0857P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1739
_refine_ls_wR_factor_ref         0.2315
_reflns_number_gt                5985
_reflns_number_total             15377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103606h.txt
_cod_data_source_block           U(PrBTP)3I3.4C5H5N
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7114795