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_7112554
_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            'C96 H104 N16 O13 U4'
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_symmetry_space_group_name_Hall  '-P 2ac 2ab'
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_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.5621(19)
_cell_length_b                   10.9547(8)
_cell_length_c                   30.626(3)
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_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.8525
_cell_measurement_theta_min      3.3227
_cell_volume                     9247.0(13)
_computing_cell_refinement
;
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
;
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 0.890
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_details
;
1 omega 7.00 34.00 1.0000 300.0000
omega____ theta____ kappa____ phi______ frames
- 16.8425 37.0000 -150.0000 27

2 omega 17.00 74.00 1.0000 300.0000
omega____ theta____ kappa____ phi______ frames
- 16.8425 37.0000 -60.0000 57

;
_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  0.1045
_diffrn_reflns_av_sigmaI/netI    0.2274
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14335
_diffrn_reflns_theta_full        26.30
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.33
_exptl_absorpt_coefficient_mu    7.056
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_exptl_absorpt_correction_T_min  0.3175
_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            red
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5056
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.427
_refine_diff_density_min         -1.438
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         8400
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1989
_refine_ls_R_factor_gt           0.0919
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1823
_reflns_number_gt                4068
_reflns_number_total             8400
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc16646h.txt
_cod_data_source_block           2
_cod_original_cell_volume        9246.9(13)
_cod_database_code               7112554