Oxidation Chemistry of Uranium(III) Complexes of Tpa: Synthesis and Structural Studies of Oxo, Hydroxo, and Alkoxo Complexes of Uranium(IV)
Lydia Karmazin; Marinella Mazzanti; Jacques Pécaut; Inorganic Chemistry 42 (2003) 5900–5908; doi:10.1021/ic0343004

data_4314237
_publ_section_title
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 Oxidation Chemistry of Uranium(III) Complexes of Tpa: Synthesis and
 Structural Studies of Oxo, Hydroxo, and Alkoxo Complexes of Uranium(IV)
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5900
_journal_page_last               5908
_journal_paper_doi               10.1021/ic0343004
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C19 H21 I3 N4 O U'
_chemical_formula_weight         940.13
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.0020(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4172(5)
_cell_length_b                   17.4441(8)
_cell_length_c                   12.9559(6)
_cell_measurement_temperature    293(2)
_cell_volume                     2353.97(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.856
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11747
_diffrn_reflns_theta_full        28.83
_diffrn_reflns_theta_max         28.83
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    10.847
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.750
_refine_diff_density_min         -1.629
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         5283
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.374
_refine_ls_shift/su_mean         0.039
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0688
_reflns_number_gt                4088
_reflns_number_total             5283
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0343004si20030702_093145_5.cif
_cod_data_source_block           complex5,[U(tpa)(OMe)I3]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4314237