Synthesis, Characterization, and Multielectron Reduction Chemistry of Uranium Supported by Redox-Active α-Diimine Ligands
Steven J. Kraft; Ursula J. Williams; Scott R. Daly; Eric J. Schelter; Stosh A. Kozimor; Kevin S. Boland; James M. Kikkawa; William P. Forrest; Christin N. Christensen; Daniel E. Schwarz; Phillip E. Fanwick; David L. Clark; Steve D. Conradson; Suzanne C. Bart; Inorganic Chemistry 50 (2011) 9838–9848; doi:10.1021/ic2002805

data_4326435
_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
;
 Synthesis, Characterization, and Multielectron Reduction Chemistry of
 Uranium Supported by Redox-Active \a-Diimine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9838
_journal_page_last               9848
_journal_paper_doi               10.1021/ic2002805
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C45 H59 I1 N4 U1'
_chemical_formula_sum            'C45 H59 I N4 U'
_chemical_formula_weight         1020.93
_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_type_scat_source
'International Tables for Crystallography (Vol C)'
_audit_creation_date             30-03-11
_audit_creation_method           'SHELXL and local programs'
_cell_angle_alpha                90.00
_cell_angle_beta                 94.674(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4755(15)
_cell_length_b                   11.0385(13)
_cell_length_c                   28.420(4)
_cell_measurement_reflns_used    7465
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      67
_cell_measurement_theta_min      1
_cell_volume                     4213.4(9)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_computing_data_collection       'CrystalClear(Rigaku, 2001)'
_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      150.0(2)
_diffrn_measured_fraction_theta_full 0.9790
_diffrn_measured_fraction_theta_max 0.9790
_diffrn_measurement_details
;
Data were collected on a Rigaku Rapid which has a quarter 
chi circle and a 200 degree curved image plate at a fixed 
distance of 127.4mm.  Strategy was optimized using the 
CrystalClear software.  The completeness is the best 
that can be obtained with this geometry. The missing data are not cusp 
data but mostly high angle data.
Also the use of HKL2000/SCALEPACK lowers the number 
of observed data as inconsistent equivalents are removed 
from the data set and not included in the collected total
;
_diffrn_measurement_device_type  Rigaku_Rapid_II
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'confocal optics'
_diffrn_radiation_type           CU-K\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0700
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            35507
_diffrn_reflns_theta_full        57.5
_diffrn_reflns_theta_max         67.04
_diffrn_reflns_theta_min         1.56
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.740
_exptl_absorpt_correction_T_max  0.5873
_exptl_absorpt_correction_T_min  0.5367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       needle
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.43
_refine_diff_density_min         -0.88
_refine_ls_d_res_high            0.91
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         5642
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.096
_refine_ls_R_factor_gt           0.068
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0809P)^2^+56.4355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.170
_refine_ls_wR_factor_ref         0.192
_reflns_number_gt                4130
_reflns_number_total             5642
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            ic2002805_si_003.cif
_cod_data_source_block           SKC126
_cod_original_formula_sum        'C45 H59 I1 N4 U1'
_cod_database_code               4326435