Hydrothermal Preparation of Nickel(II)/Uranium(IV) Fluorides with One-, Two-, and Three-Dimensional Topologies
Amanda C. Bean; Tyler A. Sullens; Wolfgang Runde; Thomas E. Albrecht-Schmitt; Inorganic Chemistry 42 (2003) 2628–2633; doi:10.1021/ic0262076

data_4313503
_publ_contact_author
;
Prof. Thomas E. Albrecht-Schmitt 
179 Chemistry Building
Department of Chemistry
Auburn University, AL
36849
;
_publ_contact_author_email       ' albreth@auburn.edu '
_publ_contact_author_fax         ' 334 844 6959 '
_publ_contact_author_phone       ' 334 844 6948 '
_publ_section_title
;
 Hydrothermal Preparation of Nickel(II)/Uranium(IV) Fluorides with One-,
 Two-, and Three-Dimensional Topologies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2628
_journal_page_last               2633
_journal_paper_doi               10.1021/ic0262076
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         Ni(H2O)2UF6(H2O)
_chemical_formula_sum            'F6 H6 Ni O3 U'
_chemical_formula_weight         464.79
_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   'not included'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.833(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0590(10)
_cell_length_b                   6.8895(6)
_cell_length_c                   7.9351(7)
_cell_measurement_reflns_used    805
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      3.38
_cell_volume                     658.45(10)
_computing_cell_refinement       'SMART and SAINT'
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-97 (sheldrick, 1997)'
_computing_publication_material  'SHELXCIF-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'Bruker APEX'
_diffrn_measurement_method       '0.3 wide w/ exposures'
_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  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2712
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         3.38
_diffrn_standards_decay_%        na
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         na
_exptl_absorpt_coefficient_mu    27.507
_exptl_absorpt_correction_T_max  '.328435 ratio of min/ max'
_exptl_absorpt_correction_T_min  '.328435 ratio of min/ max'
_exptl_absorpt_correction_type   'analytical and SADABS (multiscan)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    4.689
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal block'
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.048
_refine_diff_density_max         3.633
_refine_diff_density_min         -4.262
_refine_diff_density_rms         0.498
_refine_ls_extinction_coef       0.0099(7)
_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_all   1.098
_refine_ls_goodness_of_fit_obs   1.098
_refine_ls_hydrogen_treatment    'not included'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         805
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_restrained_S_obs      1.098
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_obs          0.0330
_refine_ls_shift/esd_max         0.013
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+3.7635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0878
_refine_ls_wR_factor_obs         0.0878
_reflns_number_observed          803
_reflns_number_total             805
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0262076si20030203_104205_3.cif
_cod_data_source_block           abs1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'nm' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+3.7635P] 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^)+(0.0656P)^2^+3.7635P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'H6 F6 Ni O3 U'
_cod_database_code               4313503