"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_4335290
_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_formula_moiety         'C56 H86 N2 O4 U1, 8/3(C4 H8 O1), 2/3(C5 H12)'
_chemical_formula_sum            'C70 H111.33333 N2 O6.66667 U'
_chemical_formula_weight         1329.74
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                70.95
_cell_angle_beta                 73.10
_cell_angle_gamma                83.34
_cell_formula_units_Z            3
_cell_length_a                   14.6626(6)
_cell_length_b                   16.6809(5)
_cell_length_c                   22.7494(6)
_cell_measurement_reflns_used    18408
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      70
_cell_measurement_theta_min      2
_cell_volume                     5030.9(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 0.9580
_diffrn_measured_fraction_theta_max 0.9580
_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  0.0890
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            99463
_diffrn_reflns_theta_full        70.3
_diffrn_reflns_theta_max         70.29
_diffrn_reflns_theta_min         2.80
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.200
_exptl_absorpt_correction_T_max  0.6492
_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    1.317
_exptl_crystal_description       needle
_exptl_crystal_F_000             2084
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.80
_refine_diff_density_min         -1.42
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1096
_refine_ls_number_reflns         18398
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.052
_refine_ls_R_factor_gt           0.051
_refine_ls_shift/su_max          0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1126P)^2^+5.1474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.143
_refine_ls_wR_factor_ref         0.144
_reflns_number_gt                17721
_reflns_number_total             18398
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            ic4009812_si_004_2.cif
_cod_data_source_block           EMM64
_cod_depositor_comments
;

2021-10-24
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel

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_moiety     '3(C56 H86 N2 O4 U1),8(C4 H8 O1),2(C5 H12)'
_cod_original_formula_sum        'C210 H346 N6 O20 U3'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     3989.22
_cod_database_code               4335290