Synthesis and Crystal Structure of UO2Cl2(THF)3: A Simple Preparation of an Anhydrous Uranyl Reagent
Marianne P. Wilkerson; Carol J. Burns; Robert T. Paine; Brian L. Scott; Inorganic Chemistry 38 (1999) 4156–4158; doi:10.1021/ic990159g

data_4322236
_publ_section_title
;
 Synthesis and Crystal Structure of UO2Cl2(THF)3: A Simple Preparation of
 an Anhydrous Uranyl Reagent
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4156
_journal_page_last               4158
_journal_paper_doi               10.1021/ic990159g
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C12 H24 Cl2 O5 U'
_chemical_formula_weight         557.24
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.8930(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.8225(4)
_cell_length_b                   16.7914(10)
_cell_length_c                   15.6088(9)
_cell_measurement_temperature    203
_cell_volume                     1785.85(18)
_computing_cell_refinement       'SAINT 4.051(Bruker, 1996)'
_computing_data_collection       'SMART 4.210 (Bruker, 1996)'
_computing_data_reduction        'SAINT 4.051 (Bruker, 1996)'
_computing_molecular_graphics    'SHELXTL 5.1 (Bruker, 1997)'
_computing_publication_material  'SHELXTL 5.1 (Bruker, 1997)'
_computing_structure_refinement  'SHELXTL 5.1 (Bruker, 1997)'
_computing_structure_solution    'SHELXTL 5.1 (Bruker, 1997)'
_diffrn_ambient_temperature      203
_diffrn_measurement_device       'Siemens P4/CCD'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0598
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3592
_diffrn_reflns_theta_max         26.48
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    9.401
_exptl_absorpt_correction_T_max  0.20
_exptl_absorpt_correction_T_min  0.32
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.073
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.725
_refine_diff_density_min         -1.536
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       'not refined'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.799
_refine_ls_goodness_of_fit_obs   0.810
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.799
_refine_ls_restrained_S_obs      0.810
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_obs          0.0395
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1199
_refine_ls_wR_factor_obs         0.1070
_reflns_number_observed          2813
_reflns_number_total             3592
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990159g.cif
_cod_data_source_block           ccd42
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1785.9(2)
_cod_database_code               4322236