Mixed-Valent Uranium(IV,VI) Diphosphonate: Synthesis, Structure, and Spectroscopy
Juan Diwu; Thomas E. Albrecht-Schmitt; Inorganic Chemistry 51 (2012) 4432–4434; doi:10.1021/ic300391p

data_4328995
_publ_section_title
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 Mixed-Valent Uranium(IV,VI) Diphosphonate: Synthesis, Structure, and
 Spectroscopy
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4432
_journal_page_last               4434
_journal_paper_doi               10.1021/ic300391p
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         (UO2)3U(H2O)2[CH2(PO3)2]3.(H2O)6(H3O)2
_chemical_formula_sum            'C3 H6 O34 P6 U4'
_chemical_formula_weight         1724.02
_chemical_name_common
'mixed-valent (IV, VI) uranium methylenediphosphonate'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.415(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.903(5)
_cell_length_b                   17.021(3)
_cell_length_c                   16.723(3)
_cell_measurement_reflns_used    8694
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.62
_cell_measurement_theta_min      1.44
_cell_volume                     7172(2)
_computing_cell_refinement       'SMART SAINT'
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELCIF-97 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       '0.3 wide w/ exposures'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_source         'Imus microdocused'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41446
_diffrn_reflns_theta_full        28.62
_diffrn_reflns_theta_max         28.62
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    18.382
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SHELXPREP
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.193
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             6032
_exptl_crystal_size_max          0.063
_exptl_crystal_size_mid          0.042
_exptl_crystal_size_min          0.039
_refine_diff_density_max         2.961
_refine_diff_density_min         -1.381
_refine_diff_density_rms         0.360
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         8694
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.071
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0251P)^2^+495.5570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1036
_reflns_number_gt                6756
_reflns_number_total             8694
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300391p_si_002.cif
_cod_data_source_block           UC1P2S
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_original_cell_volume        7172(3)
_cod_database_code               4328995