"Oxidative Addition" of Halogens to Uranium(IV) Bis(amidophenolate) Complexes
Ellen M. Matson; Stacey R. Opperwall; Phillip E. Fanwick; Suzanne C. Bart; Inorganic Chemistry 52 (2013) 7295–7304; doi:10.1021/ic4009812

data_4335289
_publ_contact_author_address
;    Department of Chemistry
     Purdue University
     560 Oval Dr.
     W. Lafayette
     IN 47907-2084
     USA
;
_publ_contact_author_email       pfanwick@purdue.edu
_publ_contact_author_fax         1(765)4940239
_publ_contact_author_name        'Fanwick, Phillip E.'
_publ_contact_author_phone       1(765)4944572
_publ_section_title
;
 "Oxidative Addition" of Halogens to Uranium(IV) Bis(amidophenolate)
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7295
_journal_page_last               7304
_journal_paper_doi               10.1021/ic4009812
_journal_volume                  52
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C40 H66 I2 N2 O3 U1,C4 H8 O1'
_chemical_formula_sum            'C44 H74 I2 N2 O4 U'
_chemical_formula_weight         1186.93
_chemical_name_systematic        ' ?'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 91.360(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6672(5)
_cell_length_b                   17.3698(12)
_cell_length_c                   14.6146(8)
_cell_measurement_reflns_used    20439
_cell_measurement_temperature    150.00(2)
_cell_measurement_theta_max      68
_cell_measurement_theta_min      3
_cell_volume                     2453.4(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_data_collection       'Collect (Nonius, 1998)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_molecular_graphics
;
    ORTEP (Johnson, 1976)
    PLATON (Spek, 2003)
;
_computing_publication_material  'SHELX97(Sheldrick, 2008) and local programs'
_computing_structure_refinement  'SHELX97 (Sheldrick, 2008)'
_computing_structure_solution
;
 PATTY (DIRDIF, Beurskins, 2008)
;
_diffrn_ambient_temperature      150.00(2)
_diffrn_measured_fraction_theta_full 0.9770
_diffrn_measured_fraction_theta_max 0.9770
_diffrn_measurement_device_type  Nonius_KappaCCD
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite 002'
_diffrn_radiation_type           CU-K\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1000
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20439
_diffrn_reflns_theta_full        68.4
_diffrn_reflns_theta_max         68.42
_diffrn_reflns_theta_min         2.54
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.481
_exptl_absorpt_correction_T_max  0.4588
_exptl_absorpt_correction_T_min  0.4337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       plate
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.18
_refine_diff_density_min         -2.38
_refine_ls_abs_structure_details
'Flack H. D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.099(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         8454
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.071
_refine_ls_R_factor_gt           0.070
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'1/[\s^2^(Fo^2^)+(0.1479P)^2^+10.1685P] where P=(Fo^2^+2Fc^2^)/3 '
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.190
_refine_ls_wR_factor_ref         0.191
_reflns_Friedel_coverage         0.9229
_reflns_number_gt                8274
_reflns_number_total             8454
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            ic4009812_si_004_1.cif
_cod_data_source_block           EMM49
_cod_original_formula_sum        'C44 H74 I2 N2 O4 U1'
_cod_database_code               4335289