New polynuclear U(IV)-U(V) complexes from U(IV) mediated uranyl(V) disproportionation.
Mougel, Victor; Pécaut, Jacques; Mazzanti, Marinella; Chemical communications (Cambridge, England) 48 (2012) 868–870; doi:10.1039/c1cc16646h

data_7112553
_publ_section_title
;
 New polynuclear U(IV)-U(V) complexes from U(IV) mediated uranyl(V)
 disproportionation.
;
_journal_issue                   6
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              868
_journal_page_last               870
_journal_paper_doi               10.1039/c1cc16646h
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C21.5 H23.5 K N3.5 O4 U'
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_chemical_name_systematic
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?
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_space_group_IT_number           14
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_cell_angle_alpha                90.00
_cell_angle_beta                 101.946(15)
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_cell_formula_units_Z            8
_cell_length_a                   22.925(4)
_cell_length_b                   14.316(3)
_cell_length_c                   14.0547(19)
_cell_measurement_reflns_used    1997
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.0273
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_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
1 omega -25.00 16.00 1.0000 300.0000
omega____ theta____ kappa____ phi______ frames
- 17.3113 102.0000 9.0000 41

2 omega 37.00 93.00 1.0000 300.0000
omega____ theta____ kappa____ phi______ frames
- 17.3113 179.0000 -180.0000 56

3 omega -74.00 35.00 1.0000 300.0000
omega____ theta____ kappa____ phi______ frames
- -19.0300 0.0000 90.0000 109

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1018
_diffrn_reflns_av_sigmaI/netI    0.1942
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12681
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    7.412
_exptl_absorpt_correction_T_max  0.9499
_exptl_absorpt_correction_T_min  0.1349
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.894
_refine_diff_density_min         -1.329
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         6438
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1720
_refine_ls_R_factor_gt           0.0932
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0702P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1986
_refine_ls_wR_factor_ref         0.2419
_reflns_number_gt                2989
_reflns_number_total             6438
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc16646h.txt
_cod_data_source_block           1
_cod_original_cell_volume        4512.5(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C21.50 H23.50 K N3.50 O4 U'
_cod_database_code               7112553