From Molecules to Frameworks: Variable Dimensionality in the UO2(CH3COO)2.2H2O/HF(aq)/Piperazine System. Syntheses, Structures, and Characterization of Zero-Dimensional (C4N2H12)UO2F4.3H2O, One-Dimensional (C4N2H12)2U2F12.H2O, Two-Dimensional (C4N2H12)2(U2O4F5)4.11H2O, and Three-Dimensional (C4N2H12)U2O4F6
Susan M. Walker; P. Shiv Halasyamani; Simon Allen; Dermot O'Hare; Journal of the American Chemical Society 121 (1999) 10513–10521; doi:10.1021/ja992145f

data_4116579
_publ_contact_author_address
;
Inorganic Chemistry Laboratory
University of Oxford
South Parks Rd.
Oxford
OX1 3QR
;
_publ_contact_author_email       'dermot.ohare@chem.ox.ac.uk '
_publ_contact_author_fax         ' 01865 272 690 '
_publ_contact_author_name        'Prof. Dermot O'Hare'
_publ_contact_author_phone       ' 01865 272 658 '
_publ_section_title
;
 From Molecules to Frameworks: Variable Dimensionality in the
 UO2(CH3COO)2.2H2O/HF(aq)/Piperazine System. Syntheses, Structures, and
 Characterization of Zero-Dimensional (C4N2H12)UO2F4.3H2O, One-Dimensional
 (C4N2H12)2U2F12.H2O, Two-Dimensional (C4N2H12)2(U2O4F5)4.11H2O, and
 Three-Dimensional (C4N2H12)U2O4F6
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10513
_journal_page_last               10521
_journal_paper_doi               10.1021/ja992145f
_journal_volume                  121
_journal_year                    1999
_chemical_compound_source        'hydrothermal synthesis'
_chemical_formula_moiety         'C4 H18 F4 N2 O5 U'
_chemical_formula_structural     'U O5 F4 N2 C4 H18'
_chemical_formula_sum            'C4 H18 F4 N2 O5 U'
_chemical_formula_weight         488.23
_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
_cell_angle_alpha                90
_cell_angle_beta                 100.17(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.503(1)
_cell_length_b                   9.847(1)
_cell_length_c                   15.009(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     1236.9(2)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_sigmaI/netI    0.043
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4944
_diffrn_reflns_theta_max         26.47
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    13.181
_exptl_absorpt_correction_T_max  0.2718
_exptl_absorpt_correction_T_min  0.1913
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
        cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.622
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.859
_refine_diff_density_min         -2.495
_refine_diff_density_rms         0.255
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.042
_refine_ls_goodness_of_fit_gt    1.048
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_restrained_S_obs      1.048
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+10.9269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.085
_refine_ls_wR_factor_gt          0.0832
_reflns_number_gt                2428
_reflns_number_total             2556
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja992145f_1.cif
_cod_data_source_block           ufo8a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+10.9269P] 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^)+(0.0424P)^2^+10.9269P] 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        1236.94(3)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4116579
_exptl_absorpt_factor_mur        1.485
_exptl_absorpt_correction_t_ave  0.2289