Synthesis, Characterization, and Stoichiometric U-O Bond Scission in Uranyl Species Supported by Pyridine(diimine) Ligand Radicals.
Kiernicki, John J.; Cladis, Dennis P.; Fanwick, Phillip E.; Zeller, Matthias; Bart, Suzanne C.; Journal of the American Chemical Society 137 (2015) 11115–11125; doi:10.1021/jacs.5b06217

data_4124365
_publ_section_title
;
 Synthesis, Characterization, and Stoichiometric U-O Bond Scission in
 Uranyl Species Supported by Pyridine(diimine) Ligand Radicals.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11115
_journal_page_last               11125
_journal_paper_doi               10.1021/jacs.5b06217
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C33 H47 I2 N3 O2 Si2 U1,2(C6 H6)'
_chemical_formula_sum            'C45 H59 I2 N3 O2 Si2 U'
_chemical_formula_weight         1222.00
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   39.1960(5)
_cell_length_b                   21.6988(3)
_cell_length_c                   11.8286(2)
_cell_measurement_reflns_used    37889
_cell_measurement_temperature    150.00(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1
_cell_volume                     10060.3(3)
_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
;
 Direct methods (SIR2011, Burla et al., in press)
;
_diffrn_ambient_temperature      150.00(2)
_diffrn_measured_fraction_theta_full 0.9750
_diffrn_measured_fraction_theta_max 0.9750
_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  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            37889
_diffrn_reflns_theta_full        22.5
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.537
_exptl_absorpt_correction_T_max  0.3366
_exptl_absorpt_correction_T_min  0.3013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4736
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         3.28
_refine_diff_density_min         -2.68
_refine_ls_d_res_high            0.93
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         6634
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.079
_refine_ls_R_factor_gt           0.065
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'1/[\s^2^(Fo^2^)+(0.0993P)^2^+68.5477P] where P=(Fo^2^+2Fc^2^)/3 '
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.165
_refine_ls_wR_factor_ref         0.175
_reflns_number_gt                5461
_reflns_number_total             6634
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            ja5b06217_si_003.cif
_cod_data_source_block           JK3150
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z 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        'C45 H59 I2 N3 O2 Si2 U1'
_cod_database_code               4124365