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_7115313
_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         'C53 H56 N3 Se2 U1,2(C4 H8 O1)'
_chemical_formula_sum            'C61 H72 N3 O2 Se2 U'
_chemical_formula_weight         1275.22
_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'
_cell_angle_alpha                90.00
_cell_angle_beta                 100.6420(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7186(2)
_cell_length_b                   26.9121(4)
_cell_length_c                   17.5708(3)
_cell_measurement_reflns_used    49413
_cell_measurement_temperature    150.00(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      1
_cell_volume                     5446.03(16)
_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 0.9910
_diffrn_measured_fraction_theta_max 0.9910
_diffrn_measurement_device_type  Nonius_KappaCCD
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite 002'
_diffrn_radiation_type           MO-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_sigmaI/netI    0.0914
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49413
_diffrn_reflns_theta_full        27.9
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         2.33
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.362
_exptl_absorpt_correction_T_max  0.4661
_exptl_absorpt_correction_T_min  0.4133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2540
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.07
_refine_diff_density_min         -1.16
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.915
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         12859
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.085
_refine_ls_R_factor_gt           0.037
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
' w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.064
_refine_ls_wR_factor_ref         0.073
_reflns_number_gt                8039
_reflns_number_total             12859
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            c4cc03355h2.cif
_cod_data_source_block           JK449
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc'
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 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        5446.03(15)
_cod_original_formula_sum        'C61 H72 N3 O2 Se2 U1'
_cod_database_code               7115313