Utility of a redox-active pyridine(diimine) chelate in facilitating two electron oxidative addition chemistry at uranium
John J. Kiernicki; Phillip E. Fanwick; Suzanne C. Bart; Chem.Commun. 50 (2014) 8189–; doi:10.1039/C4cc03355H

data_7115312
_publ_section_title
;
 Utility of a redox-active pyridine(diimine) chelate in facilitating two
 electron oxidative addition chemistry at uranium
;
_journal_name_full               Chem.Commun.
_journal_page_first              8189
_journal_paper_doi               10.1039/C4cc03355H
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C47 H51 Cl1 N3 Se1 U1,0.5(C3 H6 O1)'
_chemical_formula_sum            'C47 H51 Cl N3 O0.12 Se U'
_chemical_formula_weight         1012.35
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 101.179(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   42.342(2)
_cell_length_b                   8.3362(4)
_cell_length_c                   24.4297(12)
_cell_measurement_reflns_used    42978
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      67.877
_cell_measurement_theta_min      3.688
_cell_volume                     8459.4(7)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Crystal Clear(Rigaku 2001)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'DIRDIF/PATTY (Burskens, et. al,. 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.964
_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_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            42978
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.877
_diffrn_reflns_theta_min         3.688
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    12.630
_exptl_absorpt_correction_T_max  0.685
_exptl_absorpt_correction_T_min  0.037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       plate
_exptl_crystal_F_000             3984
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.980
_refine_diff_density_min         -1.375
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         7389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0074P)^2^+261.2250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1038
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5742
_reflns_number_total             7389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc03355h2.cif
_cod_data_source_block           JK5150
_cod_original_cell_volume        8459.5(7)
_cod_database_code               7115312
_shelx_estimated_absorpt_t_min   0.571
_shelx_estimated_absorpt_t_max   0.703
_shelxl_version_number           2014-3
_shelx_res_checksum              26055