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_4124366
_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         'C43 H64 N6 O P U, C4 H8 O'
_chemical_formula_sum            'C47 H72 N6 O2 P U'
_chemical_formula_weight         1022.10
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_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
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_cell_length_b                   20.0894(10)
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_cell_measurement_temperature    100(2)
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;  
SHELXL-2014/7 (Sheldrick, 2014), 
SHELXLE Rev714 (H\"ubschle et al., 2011)
;
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_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker AXS D8 Quest CMOS diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_k_min       -30
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_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            151365
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
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_diffrn_reflns_theta_min         2.159
_diffrn_source                   'I-mu-S microsource X-ray tube'
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_exptl_absorpt_correction_T_min  0.4737
_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_description       plate
_exptl_crystal_F_000             4152
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_exptl_crystal_size_min          0.12
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_refine_diff_density_min         -2.070
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     1066
_refine_ls_number_reflns         33344
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0116P)^2^+18.2919P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0742
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29893
_reflns_number_total             33344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b06217_si_006.cif
_cod_data_source_block           Quest15mz180_0m
_cod_database_code               4124366
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              26579
_shelx_hkl_checksum              60434