Synthesis and Characterization of Heavier Dioxouranium(VI) Dihalides
Margaret-Jane Crawford; Arkady Ellern; Konstantin Karaghiosoff; Peter Mayer; Heinrich Nöth; Max Suter; Inorganic Chemistry 43 (2004) 7120–7126; doi:10.1021/ic0354926

data_4311864
_publ_contact_author
;
      Margaret-Jane Crawford
      Institut f\"ur anorganische Chemie
      Universit\"at M\"unchen
      Butenandtstr. 5-13 (Haus D)
      81377 M\"unchen
      Bundesrepublik Deutschland
;
_publ_contact_author_email       mjc@cup.uni-muenchen.de
_publ_contact_author_fax         '089 2180 77492'
_publ_contact_author_phone       '089 2180 77503'
_publ_section_title
;
 Synthesis and Characterization of Heavier Dioxouranium(VI) Dihalides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7120
_journal_page_last               7126
_journal_paper_doi               10.1021/ic0354926
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         '[U O2 Br2 O2 H4]2'
_chemical_formula_sum            'Br4 H8 O8 U2'
_chemical_formula_weight         931.733
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 99.616(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.0568(7)
_cell_length_b                   10.5117(9)
_cell_length_c                   10.3623(12)
_cell_measurement_reflns_used    4004
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.8
_cell_volume                     650.47(12)
_computing_cell_refinement       'Stoe IPDS software (Darmstadt, Germany)'
_computing_data_collection       'Stoe IPDS software (Darmstadt, Germany)'
_computing_data_reduction        'Stoe IPDS software (Darmstadt, Germany)'
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      202(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'area detection'
_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  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5484
_diffrn_reflns_theta_full        28.06
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    37.162
_exptl_absorpt_correction_T_max  0.2193
_exptl_absorpt_correction_T_min  0.0379
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
crystal faces optimized with XShape, rev. 1.02, STOE (Darmstadt, Germany)
Absorption correction with XRed, rev 1.09, STOE (Darmstadt, Germany)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.7572(9)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.197
_refine_diff_density_min         -2.601
_refine_diff_density_rms         0.335
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         1559
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.532
_refine_ls_wR_factor_ref         0.0551
_reflns_number_gt                1263
_reflns_number_total             1559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0354926si20040705_042654_4.cif
_cod_data_source_block           i015
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'H8 Br4 O8 U2'
_cod_database_code               4311864