Synthesis and characterisation of (C4N2H12)(UO2)2(PO3H)2{PO2(OH)H}2: a three dimensionally connected actinide framework
Doran, Michael; Walker, Susan M.; O’Hare, Dermot; Chemical Communications  (2001) 1988–; doi:10.1039/b106804k

data_7115022
_publ_section_title
;
 Synthesis and characterisation of (C4N2H12)(UO2)2(PO3H)2{PO2(OH)H}2: a
 three dimensionally connected actinide framework
;
_journal_issue                   19
_journal_name_full               'Chemical Communications'
_journal_page_first              1988
_journal_paper_doi               10.1039/b106804k
_journal_year                    2001
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C4 H12 N2 O8 P2 U2'
_chemical_formula_structural     'U2 O8 P2 C4 N2 H12'
_chemical_formula_sum            'C4 H18 N2 O16 P4 U2'
_chemical_formula_weight         950.14
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2001-07-26T14:56:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 106.647(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   13.758(5)
_cell_length_b                   8.180(5)
_cell_length_c                   18.037(5)
_cell_measurement_reflns_used    8604
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_measurement_wavelength     0.71073
_cell_volume                     1944.8(15)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8286
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.2
_exptl_absorpt_coefficient_mu    17.042
_exptl_absorpt_correction_T_max  0.0273
_exptl_absorpt_correction_T_min  0.0104
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.353
_refine_diff_density_min         -2.379
_refine_diff_density_rms         0.777
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1046P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1669
_reflns_number_gt                3315
_reflns_number_total             4467
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b106804k.txt
_cod_data_source_block           smw89
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7115022
_exptl_absorpt_correction_t_ave  0.0206