#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/35/4313501.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4313501
loop_
_publ_author_name
'Amanda C. Bean'
'Tyler A. Sullens'
'Wolfgang Runde'
'Thomas E. Albrecht-Schmitt'
_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)4UF6 (H2O)2.5'
_chemical_formula_sum            'F6 H13 Ni O6.5 U'
_chemical_formula_weight         527.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   'not included'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.3383(8)
_cell_length_b                   15.6867(8)
_cell_length_c                   8.0282(4)
_cell_measurement_reflns_used    1245
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      1.92
_cell_volume                     1805.71(16)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  '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  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9078
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         na
_exptl_absorpt_coefficient_mu    20.113
_exptl_absorpt_correction_T_max  '.519431 ratio of min/max'
_exptl_absorpt_correction_T_min  '.519431 ratio of min/max'
_exptl_absorpt_correction_type   'analytical and SADABS (multiscan)'
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    3.883
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.032
_refine_diff_density_max         2.007
_refine_diff_density_min         -1.809
_refine_diff_density_rms         0.255
_refine_ls_extinction_coef       0.00013(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         1245
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0408P)²+21.5163P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0692
_reflns_number_gt                1159
_reflns_number_total             1245
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0262076si20030203_104205_1.cif
_cod_data_source_block           niuf4w
_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 
;
_cod_original_formula_sum        'H13 F6 Ni O6.50 U'
_cod_database_code               4313501
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.5000 0.129032(13) -0.00324(2) 0.00753(12) Uani 1 2 d S . .
Ni1 Ni 0.25783(5) 0.16054(5) -0.2500 0.00977(19) Uani 1 2 d S . .
F1 F 0.35193(18) 0.16476(16) -0.0658(3) 0.0128(5) Uani 1 1 d . . .
F2 F 0.5000 0.2104(3) -0.2500 0.0139(10) Uani 1 4 d S . .
F3 F 0.5000 0.2649(2) 0.0739(4) 0.0137(7) Uani 1 2 d S . .
F4 F 0.5931(3) 0.0000 0.0000 0.0107(8) Uani 1 2 d S . .
F5 F 0.5000 0.0542(3) -0.2500 0.0140(10) Uani 1 4 d S . .
F6 F 0.4124(3) 0.1280(2) 0.2500 0.0108(7) Uani 1 2 d S . .
O1 O 0.2769(3) 0.0296(3) -0.2500 0.0147(9) Uani 1 2 d S . .
O2 O 0.1606(2) 0.1536(2) -0.0622(4) 0.0159(6) Uani 1 1 d . . .
O3 O 0.2555(3) 0.2932(3) -0.2500 0.0128(8) Uani 1 2 d S . .
O4 O 0.5000 0.386(2) -0.2500 0.216(15) Uiso 1 4 d S . .
O5 O 0.0878(7) 0.0074(5) 0.0620(12) 0.035(2) Uiso 0.50 1 d P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F3 U1 F1 79.82(7) . . ?
F3 U1 F1 79.82(7) . 12_655 ?
F1 U1 F1 140.96(13) . 12_655 ?
F3 U1 F5 136.85(14) . . ?
F1 U1 F5 86.28(7) . . ?
F1 U1 F5 86.28(7) 12_655 . ?
F3 U1 F2 73.38(14) . . ?
F1 U1 F2 71.20(7) . . ?
F1 U1 F2 71.20(7) 12_655 . ?
F5 U1 F2 63.46(16) . . ?
F3 U1 F6 76.65(11) . 3_655 ?
F1 U1 F6 133.37(10) . 3_655 ?
F1 U1 F6 72.30(10) 12_655 3_655 ?
F5 U1 F6 136.76(11) . 3_655 ?
F2 U1 F6 135.94(10) . 3_655 ?
F3 U1 F6 76.65(11) . . ?
F1 U1 F6 72.30(10) . . ?
F1 U1 F6 133.37(10) 12_655 . ?
F5 U1 F6 136.76(11) . . ?
F2 U1 F6 135.94(10) . . ?
F6 U1 F6 63.41(15) 3_655 . ?
F3 U1 F4 142.99(8) . 9_655 ?
F1 U1 F4 72.00(11) . 9_655 ?
F1 U1 F4 136.81(10) 12_655 9_655 ?
F5 U1 F4 65.40(9) . 9_655 ?
F2 U1 F4 117.47(9) . 9_655 ?
F6 U1 F4 105.95(9) 3_655 9_655 ?
F6 U1 F4 72.30(9) . 9_655 ?
F3 U1 F4 142.99(8) . . ?
F1 U1 F4 136.81(10) . . ?
F1 U1 F4 72.00(11) 12_655 . ?
F5 U1 F4 65.40(9) . . ?
F2 U1 F4 117.47(9) . . ?
F6 U1 F4 72.30(9) 3_655 . ?
F6 U1 F4 105.95(9) . . ?
F4 U1 F4 66.83(17) 9_655 . ?
F3 U1 U1 106.19(9) . 10 ?
F1 U1 U1 77.12(7) . 10 ?
F1 U1 U1 77.12(7) 12_655 10 ?
F5 U1 U1 30.66(11) . 10 ?
F2 U1 U1 32.81(11) . 10 ?
F6 U1 U1 148.29(8) 3_655 10 ?
F6 U1 U1 148.29(8) . 10 ?
F4 U1 U1 90.614(4) 9_655 10 ?
F4 U1 U1 90.614(4) . 10 ?
F3 U1 U1 163.07(9) . 9_655 ?
F1 U1 U1 104.58(6) . 9_655 ?
F1 U1 U1 104.58(6) 12_655 9_655 ?
F5 U1 U1 60.08(11) . 9_655 ?
F2 U1 U1 123.54(11) . 9_655 ?
F6 U1 U1 88.99(8) 3_655 9_655 ?
F6 U1 U1 88.99(8) . 9_655 ?
F4 U1 U1 33.41(9) 9_655 9_655 ?
F4 U1 U1 33.41(9) . 9_655 ?
U1 U1 U1 90.735(5) 10 9_655 ?
F3 U1 U1 73.81(9) . 10_556 ?
F1 U1 U1 102.88(7) . 10_556 ?
F1 U1 U1 102.88(7) 12_655 10_556 ?
F5 U1 U1 149.34(11) . 10_556 ?
F2 U1 U1 147.19(11) . 10_556 ?
F6 U1 U1 31.71(8) 3_655 10_556 ?
F6 U1 U1 31.71(8) . 10_556 ?
F4 U1 U1 89.386(4) 9_655 10_556 ?
F4 U1 U1 89.386(4) . 10_556 ?
U1 U1 U1 180.000(6) 10 10_556 ?
U1 U1 U1 89.265(5) 9_655 10_556 ?
F1 Ni1 F1 95.17(15) . 10 ?
F1 Ni1 O2 178.80(12) . 10 ?
F1 Ni1 O2 85.24(12) 10 10 ?
F1 Ni1 O2 85.24(12) . . ?
F1 Ni1 O2 178.80(12) 10 . ?
O2 Ni1 O2 94.31(19) 10 . ?
F1 Ni1 O1 86.78(11) . . ?
F1 Ni1 O1 86.78(11) 10 . ?
O2 Ni1 O1 92.12(13) 10 . ?
O2 Ni1 O1 92.12(13) . . ?
F1 Ni1 O3 88.72(12) . . ?
F1 Ni1 O3 88.72(12) 10 . ?
O2 Ni1 O3 92.41(13) 10 . ?
O2 Ni1 O3 92.41(13) . . ?
O1 Ni1 O3 173.33(19) . . ?
Ni1 F1 U1 142.31(13) . . ?
U1 F2 U1 114.4(2) 10 . ?
U1 F4 U1 113.17(17) 9_655 . ?
U1 F5 U1 118.7(2) . 10 ?
U1 F6 U1 116.58(15) 10_556 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 F3 2.220(4) . ?
U1 F1 2.252(3) . ?
U1 F1 2.252(3) 12_655 ?
U1 F5 2.303(3) . ?
U1 F2 2.357(3) . ?
U1 F6 2.390(2) 3_655 ?
U1 F6 2.390(2) . ?
U1 F4 2.425(2) 9_655 ?
U1 F4 2.425(2) . ?
U1 U1 3.9621(4) 10 ?
U1 U1 4.0485(5) 9_655 ?
U1 U1 4.0661(4) 10_556 ?
Ni1 F1 2.003(3) . ?
Ni1 F1 2.003(3) 10 ?
Ni1 O2 2.056(3) 10 ?
Ni1 O2 2.056(3) . ?
Ni1 O1 2.072(5) . ?
Ni1 O3 2.081(4) . ?
F2 U1 2.357(3) 10 ?
F4 U1 2.425(2) 9_655 ?
F5 U1 2.303(3) 10 ?
F6 U1 2.390(2) 10_556 ?
O5 O5 1.02(2) 4 ?
