Hydrothermal Synthesis and Characterization of [(UO2)2F8(H2O)2Zn2(4,4'-bpy)2].(4,4'-bpy), a Mixed-Metal Uranyl Aquofluoride with a Pillared Layer Structure
Chih-Min Wang; Chia-Hsien Liao; Hsien-Ming Kao; Kwang-Hwa Lii; Inorganic Chemistry 44 (2005) 6294–6298; doi:10.1021/ic0507060

data_4309535
_publ_section_title
;
Hydrothermal Synthesis and Characterization of
[(UO2)2F8(H2O)2Zn2(4,4'-bpy)2].(4,4'-bpy), a Mixed-Metal Uranyl
Aquofluoride with a Pillared Layer Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6294
_journal_page_last               6298
_journal_paper_doi               10.1021/ic0507060
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         '[(UO2)2F8(H2O)2Zn2(4,4'-bpy)2].(4,4'-bpy)'
_chemical_formula_sum            'C30 H28 F8 N6 O6 U2 Zn2'
_chemical_formula_weight         1327.38
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.899(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4630(5)
_cell_length_b                   22.3836(12)
_cell_length_c                   16.7534(8)
_cell_measurement_temperature    293(2)
_cell_volume                     3546.7(3)
_computing_molecular_graphics    Diamond
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega 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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50499
_diffrn_reflns_theta_full        31.92
_diffrn_reflns_theta_max         31.92
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    10.535
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.440
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS program'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.282
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       0.000040(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.841
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         10974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.841
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0192
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0113P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0324
_refine_ls_wR_factor_ref         0.0336
_reflns_number_gt                7413
_reflns_number_total             10974
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0507060si20050610_073030.cif
_cod_data_source_block           i6607_0m
_cod_database_code               4309535