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_7115310
_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 S2 U1,C4 H10 O1'
_chemical_formula_sum            'C57 H66 N3 O S2 U'
_chemical_formula_weight         1111.34
_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                 99.239(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8172(4)
_cell_length_b                   19.4061(7)
_cell_length_c                   24.4379(8)
_cell_measurement_reflns_used    9791
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      68
_cell_measurement_theta_min      2
_cell_volume                     5531.5(3)
_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 0.9550
_diffrn_measured_fraction_theta_max 0.9550
_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  0.0940
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            51617
_diffrn_reflns_theta_full        68.5
_diffrn_reflns_theta_max         68.50
_diffrn_reflns_theta_min         2.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.251
_exptl_absorpt_correction_T_max  0.6297
_exptl_absorpt_correction_T_min  0.4723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2244
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_platon_squeeze_details
'                                                                       '
_refine_diff_density_max         4.14
_refine_diff_density_min         -1.76
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         9730
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.069
_refine_ls_R_factor_gt           0.065
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1458P)^2^+5.7493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.186
_refine_ls_wR_factor_ref         0.194
_reflns_number_gt                8699
_reflns_number_total             9730
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            c4cc03355h2.cif
_cod_data_source_block           JK1190
_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_formula_sum        'C57 H66 N3 O1 S2 U1'
_cod_database_code               7115310