Nitrogen-rich Compounds of the Actinoids: Dioxouranium(VI) 5,5'-Azobis[tetrazolide] Pentahydrate and Its Unusually Small Uranyl Angle
Georg Steinhauser; Gerald Giester; Christoph Wagner; Peter Weinberger; Bernhard Zachhuber; Georg Ramer; Mario Villa; Bernhard Lendl; Inorganic Chemistry 51 (2012) 6739–6745; doi:10.1021/ic300377j

data_4329486
_publ_section_title
;
 Nitrogen-rich Compounds of the Actinoids: Dioxouranium(VI)
 5,5'-Azobis[tetrazolide] Pentahydrate and Its Unusually Small Uranyl
 Angle
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6739
_journal_page_last               6745
_journal_paper_doi               10.1021/ic300377j
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C2 H10 N10 O7 U'
_chemical_formula_weight         524.23
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Steinhauser, G.'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.665(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9770(10)
_cell_length_b                   6.9420(5)
_cell_length_c                   20.740(2)
_cell_measurement_reflns_used    4195
_cell_measurement_temperature    200(2)
_cell_volume                     1283.7(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            14498
_diffrn_reflns_theta_full        30.47
_diffrn_reflns_theta_max         30.47
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    12.698
_exptl_absorpt_correction_T_max  0.08
_exptl_absorpt_correction_T_min  0.006
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Sheldrick, G., 1997'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.712
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.308
_refine_diff_density_min         -1.079
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       0.00081(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         3897
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0419
_refine_ls_wR_factor_ref         0.0453
_reflns_number_gt                3106
_reflns_number_total             3897
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300377j_si_001.cif
_cod_data_source_block           uo2zt
_cod_database_code               4329486