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_4124290
_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         'C58.29 H74.59 N4.099 O2.733 U1.366'
_chemical_formula_sum            'C41 H54 N3 O2 U'
_chemical_formula_weight         858.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 125.896(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.3976(9)
_cell_length_b                   11.7278(5)
_cell_length_c                   15.5037(6)
_cell_measurement_reflns_used    30867
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      63.432
_cell_measurement_theta_min      4.728
_cell_volume                     3888.2(4)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Crystal Clear(Rigaku 2001)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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 HKL3000/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_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.157
_diffrn_reflns_av_unetI/netI     0.1371
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30867
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        63.432
_diffrn_reflns_theta_max         63.432
_diffrn_reflns_theta_min         4.728
_diffrn_source                   'microfocus source'
_exptl_absorpt_coefficient_mu    12.021
_exptl_absorpt_correction_T_max  0.486
_exptl_absorpt_correction_T_min  0.027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       plate
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.138
_refine_diff_density_min         -2.149
_refine_diff_density_rms         0.245
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3347
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+18.6842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1492
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3073
_reflns_number_total             3347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b06217_si_005.cif
_cod_data_source_block           JK6205
_cod_depositor_comments
'Adding full bibliography for 4124290--4124292.cif.'
_cod_original_cell_volume        3888.2(3)
_cod_database_code               4124290
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.177
_shelx_estimated_absorpt_t_max   0.532
_shelx_res_checksum              69875
_shelx_hkl_checksum              82491