#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:38:41 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179196 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/35/4313502.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_4313502
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         'Ni2(H2O)6U3F16 (H2O)3'
_chemical_formula_sum            'F16 Ni2 O9 U3'
_chemical_formula_weight         1297.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           194
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   7.9863(5)
_cell_length_b                   7.9863(5)
_cell_length_c                   16.5660(10)
_cell_measurement_reflns_used    481
_cell_measurement_temperature    193
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.46
_cell_volume                     915.04(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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8754
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         na
_exptl_absorpt_coefficient_mu    28.667
_exptl_absorpt_correction_T_max  '.506007 ratio of min/max'
_exptl_absorpt_correction_T_min  '.506007 ratio of min/max'
_exptl_absorpt_correction_type   'analytical and SADABS'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    4.644
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Hexagonal Tablet'
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.278
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.958
_refine_diff_density_min         -1.105
_refine_diff_density_rms         0.254
_refine_ls_extinction_coef       0.00130(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         481
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0339P)²+7.4580P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0648
_reflns_number_gt                466
_reflns_number_total             481
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0262076si20030203_104205_2.cif
_cod_data_source_block           p63mmc
_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_database_code               4313502
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'
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 -0.50149(2) -0.49851(2) 0.7500 0.00786(18) Uani 1 4 d S . .
Ni1 Ni -0.3333 -0.6667 0.55152(8) 0.0115(3) Uani 1 6 d S . .
F1 F -0.6777(8) -0.8388(4) 0.7500 0.0163(12) Uani 1 4 d S . .
F2 F -0.3333 -0.6667 0.7500 0.0108(18) Uani 1 12 d S . .
F3 F -0.4401(7) -0.2201(3) 0.6763(2) 0.0179(8) Uani 1 2 d S . .
F4 F -0.4518(3) -0.5482(3) 0.6224(2) 0.0164(8) Uani 1 2 d S . .
O1 O -0.5855(8) -0.7927(4) 0.4852(3) 0.0182(10) Uani 1 2 d S . .
O2 O 0.0000 0.0000 0.6115(11) 0.079(6) Uani 1 6 d S . .
O3 O 0.0000 0.0000 0.7500 0.021(4) Uani 1 12 d S . .
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'
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
F4 U1 F4 144.0(2) 16_557 . ?
F4 U1 F2 72.00(11) 16_557 . ?
F4 U1 F2 72.00(11) . . ?
F4 U1 F1 81.43(6) 16_557 . ?
F4 U1 F1 81.43(6) . . ?
F2 U1 F1 61.17(12) . . ?
F4 U1 F1 81.43(6) 16_557 3_545 ?
F4 U1 F1 81.43(6) . 3_545 ?
F2 U1 F1 61.17(12) . 3_545 ?
F1 U1 F1 122.3(2) . 3_545 ?
F4 U1 F3 133.44(11) 16_557 3_445 ?
F4 U1 F3 72.85(11) . 3_445 ?
F2 U1 F3 129.44(10) . 3_445 ?
F1 U1 F3 78.66(15) . 3_445 ?
F1 U1 F3 144.03(11) 3_545 3_445 ?
F4 U1 F3 72.85(11) 16_557 18_447 ?
F4 U1 F3 133.44(11) . 18_447 ?
F2 U1 F3 129.44(10) . 18_447 ?
F1 U1 F3 78.66(15) . 18_447 ?
F1 U1 F3 144.03(11) 3_545 18_447 ?
F3 U1 F3 62.20(15) 3_445 18_447 ?
F4 U1 F3 72.85(11) 16_557 16_557 ?
F4 U1 F3 133.44(11) . 16_557 ?
F2 U1 F3 129.44(10) . 16_557 ?
F1 U1 F3 144.03(11) . 16_557 ?
F1 U1 F3 78.66(15) 3_545 16_557 ?
F3 U1 F3 101.11(19) 3_445 16_557 ?
F3 U1 F3 70.1(2) 18_447 16_557 ?
F4 U1 F3 133.44(11) 16_557 . ?
F4 U1 F3 72.85(11) . . ?
F2 U1 F3 129.44(10) . . ?
F1 U1 F3 144.03(11) . . ?
F1 U1 F3 78.66(15) 3_545 . ?
F3 U1 F3 70.1(2) 3_445 . ?
F3 U1 F3 101.11(19) 18_447 . ?
F3 U1 F3 62.20(15) 16_557 . ?
F4 U1 U1 105.53(9) 16_557 3_445 ?
F4 U1 U1 105.53(9) . 3_445 ?
F2 U1 U1 150.0 . 3_445 ?
F1 U1 U1 88.83(12) . 3_445 ?
F1 U1 U1 148.83(12) 3_545 3_445 ?
F3 U1 U1 33.15(8) 3_445 3_445 ?
F3 U1 U1 33.15(8) 18_447 3_445 ?
F3 U1 U1 74.74(11) 16_557 3_445 ?
F3 U1 U1 74.74(11) . 3_445 ?
F4 U1 U1 105.53(9) 16_557 2_455 ?
F4 U1 U1 105.53(9) . 2_455 ?
F2 U1 U1 150.0 . 2_455 ?
F1 U1 U1 148.83(12) . 2_455 ?
F1 U1 U1 88.83(12) 3_545 2_455 ?
F3 U1 U1 74.74(11) 3_445 2_455 ?
F3 U1 U1 74.74(11) 18_447 2_455 ?
F3 U1 U1 33.15(8) 16_557 2_455 ?
F3 U1 U1 33.15(8) . 2_455 ?
U1 U1 U1 60.0 3_445 2_455 ?
F4 U1 U1 74.47(9) 16_557 2_445 ?
F4 U1 U1 74.47(9) . 2_445 ?
F2 U1 U1 30.0 . 2_445 ?
F1 U1 U1 31.17(12) . 2_445 ?
F1 U1 U1 91.17(12) 3_545 2_445 ?
F3 U1 U1 105.26(11) 3_445 2_445 ?
F3 U1 U1 105.26(11) 18_447 2_445 ?
F3 U1 U1 146.85(8) 16_557 2_445 ?
F3 U1 U1 146.85(8) . 2_445 ?
U1 U1 U1 120.0 3_445 2_445 ?
U1 U1 U1 180.000(9) 2_455 2_445 ?
F4 Ni1 F4 89.48(16) 3_545 2_445 ?
F4 Ni1 F4 89.48(16) 3_545 . ?
F4 Ni1 F4 89.48(16) 2_445 . ?
F4 Ni1 O1 88.09(13) 3_545 2_445 ?
F4 Ni1 O1 88.09(13) 2_445 2_445 ?
F4 Ni1 O1 176.58(19) . 2_445 ?
F4 Ni1 O1 176.58(19) 3_545 . ?
F4 Ni1 O1 88.09(13) 2_445 . ?
F4 Ni1 O1 88.09(13) . . ?
O1 Ni1 O1 94.2(2) 2_445 . ?
F4 Ni1 O1 88.09(13) 3_545 3_545 ?
F4 Ni1 O1 176.58(19) 2_445 3_545 ?
F4 Ni1 O1 88.09(13) . 3_545 ?
O1 Ni1 O1 94.2(2) 2_445 3_545 ?
O1 Ni1 O1 94.2(2) . 3_545 ?
U1 F1 U1 117.7(2) . 2_445 ?
U1 F2 U1 120.0 2_445 3_545 ?
U1 F2 U1 120.0 2_445 . ?
U1 F2 U1 120.0 3_545 . ?
U1 F3 U1 113.70(15) 2_455 . ?
Ni1 F4 U1 143.6(2) . . ?
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 F4 2.222(4) 16_557 ?
U1 F4 2.222(4) . ?
U1 F2 2.3261(3) . ?
U1 F1 2.354(3) . ?
U1 F1 2.354(3) 3_545 ?
U1 F3 2.363(2) 3_445 ?
U1 F3 2.363(2) 18_447 ?
U1 F3 2.363(2) 16_557 ?
U1 F3 2.363(2) . ?
U1 U1 3.9574(6) 3_445 ?
U1 U1 3.9574(6) 2_455 ?
U1 U1 4.0289(6) 2_445 ?
Ni1 F4 2.017(4) 3_545 ?
Ni1 F4 2.017(4) 2_445 ?
Ni1 F4 2.017(4) . ?
Ni1 O1 2.061(5) 2_445 ?
Ni1 O1 2.061(5) . ?
Ni1 O1 2.061(5) 3_545 ?
F1 U1 2.354(3) 2_445 ?
F2 U1 2.3261(3) 2_445 ?
F2 U1 2.3261(3) 3_545 ?
F3 U1 2.363(2) 2_455 ?
