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_7112556
_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            'C128 H147 N14 O16 U5'
_chemical_formula_weight         3327.75
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
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_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
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_cell_formula_units_Z            4
_cell_length_a                   16.8481(5)
_cell_length_b                   31.3059(14)
_cell_length_c                   24.9946(10)
_cell_measurement_reflns_used    8610
_cell_measurement_temperature    150(2)
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_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
1 omega -33.00 51.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 25.2489 -37.0000 90.0000 84

2 omega -93.00 -1.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -27.1239 -77.0000 30.0000 92

3 omega -80.00 -32.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -27.1239 179.0000 150.0000 48

;
_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  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0928
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            44348
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    6.387
_exptl_absorpt_correction_T_max  0.4953
_exptl_absorpt_correction_T_min  0.2228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'long block'
_exptl_crystal_F_000             6404
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         3.103
_refine_diff_density_min         -3.148
_refine_diff_density_rms         0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1459
_refine_ls_number_reflns         21558
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.1425
_refine_ls_R_factor_gt           0.1038
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0863P)^2^+470.6426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2539
_refine_ls_wR_factor_ref         0.2766
_reflns_number_gt                14486
_reflns_number_total             21558
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc16646h.txt
_cod_data_source_block           4
_cod_original_cell_volume        12766.7(8)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7112556