# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_14on
_database_code_depnum_ccdc_archive 'CCDC 1515458'
_audit_update_record             
;
2016-11-07 deposited with the CCDC.
2016-12-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(F5U), CoH12O6, 2(H2O)'
_chemical_formula_sum            'Co F10 H16 O8 U2'
_chemical_formula_weight         869.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.0745(4)
_cell_length_b                   7.0979(3)
_cell_length_c                   8.8499(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.1040(10)
_cell_angle_gamma                90.00
_cell_volume                     693.87(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    6537
_cell_measurement_theta_min      2.3072
_cell_measurement_theta_max      28.2888

_exptl_crystal_description       Plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.160
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             762
_exptl_absorpt_coefficient_mu    24.614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0837
_exptl_absorpt_correction_T_max  0.6388
_exptl_absorpt_process_details   'SADABS Version 2014/4 (Bruker, 2014)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      294(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8989
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         28.29
_reflns_number_total             1728
_reflns_number_gt                1697
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART Version 5.631 (Bruker, 2001)'
_computing_cell_refinement       'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    various
_computing_publication_material  various

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0301P)²+0.1112P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1728
_refine_ls_number_parameters     129
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0210
_refine_ls_wR_factor_ref         0.0527
_refine_ls_wR_factor_gt          0.0524
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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 0.454141(11) 0.154566(17) 0.322826(13) 0.01774(7) Uani 1 1 d . . .
Co1 Co 1.0000 -0.5000 0.0000 0.02427(15) Uani 1 2 d S . .
O1 O 1.0255(3) -0.7733(5) -0.0746(4) 0.0354(7) Uani 1 1 d . . .
O2 O 0.8377(3) -0.4713(5) -0.1332(4) 0.0323(6) Uani 1 1 d . . .
O3 O 1.1069(3) -0.3825(5) -0.1657(4) 0.0292(6) Uani 1 1 d . . .
O4 O 0.7863(3) 0.0666(5) 0.0361(4) 0.0342(7) Uani 1 1 d . . .
F1 F 0.2542(2) 0.1655(3) 0.2868(3) 0.0292(5) Uani 1 1 d . . .
F2 F 0.6118(2) 0.1408(3) -0.2070(3) 0.0237(5) Uani 1 1 d . . .
F3 F 0.4314(2) 0.2045(3) 0.0610(2) 0.0259(4) Uani 1 1 d . . .
F4 F 0.6014(2) -0.0294(3) 0.2145(2) 0.0227(4) Uani 1 1 d . . .
F5 F 0.6116(2) 0.4372(3) 0.0002(2) 0.0232(4) Uani 1 1 d . . .
H1A H 0.992(8) -0.802(12) -0.150(9) 0.07(2) Uiso 1 1 d D . .
H1B H 1.083(8) -0.828(9) -0.048(9) 0.07(3) Uiso 1 1 d D . .
H2A H 0.812(7) -0.368(8) -0.190(8) 0.043(18) Uiso 1 1 d D . .
H2B H 0.779(7) -0.495(8) -0.093(7) 0.054(19) Uiso 1 1 d D . .
H3A H 1.144(7) -0.290(8) -0.149(8) 0.05(2) Uiso 1 1 d D . .
H3B H 1.159(6) -0.462(7) -0.198(7) 0.042(15) Uiso 1 1 d D . .
H4A H 0.758(6) 0.055(9) -0.060(7) 0.053(18) Uiso 1 1 d D . .
H4B H 0.734(7) 0.053(10) 0.084(7) 0.06(2) Uiso 1 1 d D . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 F1 2.215(3) . ?
U1 F2 2.301(2) 4_566 ?
U1 F3 2.340(2) . ?
U1 F4 2.343(2) 2_655 ?
U1 F4 2.347(2) . ?
U1 F5 2.351(2) 2_645 ?
U1 F5 2.353(2) 4_566 ?
U1 F3 2.363(2) 4_566 ?
U1 F2 2.423(2) 3_655 ?
U1 U1 3.9018(3) 3_656 ?
U1 U1 3.93391(17) 2_655 ?
U1 U1 3.93391(16) 2_645 ?
Co1 O1 2.075(3) 3_745 ?
Co1 O1 2.075(3) . ?
Co1 O2 2.088(3) . ?
Co1 O2 2.088(3) 3_745 ?
Co1 O3 2.120(3) 3_745 ?
Co1 O3 2.120(3) . ?
O1 H1A 0.77(9) . ?
O1 H1B 0.77(9) . ?
O2 H2A 0.92(6) . ?
O2 H2B 0.78(7) . ?
O3 H3A 0.78(7) . ?
O3 H3B 0.87(6) . ?
O4 H4A 0.89(6) . ?
O4 H4B 0.75(7) . ?
F2 U1 2.301(2) 4_565 ?
F2 U1 2.423(2) 3_655 ?
F3 U1 2.363(2) 4_565 ?
F4 U1 2.343(2) 2_645 ?
F5 U1 2.351(2) 2_655 ?
F5 U1 2.353(2) 4_565 ?

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
F1 U1 F2 136.05(8) . 4_566 ?
F1 U1 F3 79.43(9) . . ?
F2 U1 F3 79.59(9) 4_566 . ?
F1 U1 F4 72.33(8) . 2_655 ?
F2 U1 F4 64.74(8) 4_566 2_655 ?
F3 U1 F4 72.96(8) . 2_655 ?
F1 U1 F4 132.63(8) . . ?
F2 U1 F4 75.47(8) 4_566 . ?
F3 U1 F4 73.04(8) . . ?
F4 U1 F4 131.16(5) 2_655 . ?
F1 U1 F5 76.42(8) . 2_645 ?
F2 U1 F5 139.85(8) 4_566 2_645 ?
F3 U1 F5 137.98(8) . 2_645 ?
F4 U1 F5 129.15(8) 2_655 2_645 ?
F4 U1 F5 99.47(7) . 2_645 ?
F1 U1 F5 142.28(9) . 4_566 ?
F2 U1 F5 73.69(8) 4_566 4_566 ?
F3 U1 F5 136.43(8) . 4_566 ?
F4 U1 F5 122.25(8) 2_655 4_566 ?
F4 U1 F5 67.36(7) . 4_566 ?
F5 U1 F5 67.90(9) 2_645 4_566 ?
F1 U1 F3 86.82(9) . 4_566 ?
F2 U1 F3 88.01(9) 4_566 4_566 ?
F3 U1 F3 143.96(4) . 4_566 ?
F4 U1 F3 71.14(8) 2_655 4_566 ?
F4 U1 F3 136.17(8) . 4_566 ?
F5 U1 F3 68.01(8) 2_645 4_566 ?
F5 U1 F3 69.10(8) 4_566 4_566 ?
F1 U1 F2 72.65(8) . 3_655 ?
F2 U1 F2 134.89(4) 4_566 3_655 ?
F3 U1 F2 72.81(9) . 3_655 ?
F4 U1 F2 134.47(8) 2_655 3_655 ?
F4 U1 F2 62.81(8) . 3_655 ?
F5 U1 F2 67.41(8) 2_645 3_655 ?
F5 U1 F2 103.24(8) 4_566 3_655 ?
F3 U1 F2 134.07(9) 4_566 3_655 ?
F1 U1 U1 109.60(7) . 3_656 ?
F2 U1 U1 106.93(6) 4_566 3_656 ?
F3 U1 U1 152.19(6) . 3_656 ?
F4 U1 U1 134.60(5) 2_655 3_656 ?
F4 U1 U1 82.36(5) . 3_656 ?
F5 U1 U1 33.96(5) 2_645 3_656 ?
F5 U1 U1 33.93(5) 4_566 3_656 ?
F3 U1 U1 63.85(6) 4_566 3_656 ?
F2 U1 U1 84.65(6) 3_655 3_656 ?
F1 U1 U1 101.53(5) . 2_655 ?
F2 U1 U1 34.61(6) 4_566 2_655 ?
F3 U1 U1 63.30(6) . 2_655 ?
F4 U1 U1 33.03(5) 2_655 2_655 ?
F4 U1 U1 99.48(5) . 2_655 ?
F5 U1 U1 155.48(5) 2_645 2_655 ?
F5 U1 U1 105.78(5) 4_566 2_655 ?
F3 U1 U1 87.53(6) 4_566 2_655 ?
F2 U1 U1 135.97(6) 3_655 2_655 ?
U1 U1 U1 135.414(6) 3_656 2_655 ?
F1 U1 U1 105.27(6) . 2_645 ?
F2 U1 U1 108.43(6) 4_566 2_645 ?
F3 U1 U1 79.88(6) . 2_645 ?
F4 U1 U1 152.74(5) 2_655 2_645 ?
F4 U1 U1 32.97(5) . 2_645 ?
F5 U1 U1 74.09(5) 2_645 2_645 ?
F5 U1 U1 76.84(5) 4_566 2_645 ?
F3 U1 U1 136.11(6) 4_566 2_645 ?
F2 U1 U1 32.64(6) 3_655 2_645 ?
U1 U1 U1 72.396(4) 3_656 2_645 ?
U1 U1 U1 128.882(6) 2_655 2_645 ?
O1 Co1 O1 180.0(3) 3_745 . ?
O1 Co1 O2 87.56(15) 3_745 . ?
O1 Co1 O2 92.44(15) . . ?
O1 Co1 O2 92.44(15) 3_745 3_745 ?
O1 Co1 O2 87.56(15) . 3_745 ?
O2 Co1 O2 180.00(10) . 3_745 ?
O1 Co1 O3 92.99(14) 3_745 3_745 ?
O1 Co1 O3 87.01(14) . 3_745 ?
O2 Co1 O3 85.88(14) . 3_745 ?
O2 Co1 O3 94.12(14) 3_745 3_745 ?
O1 Co1 O3 87.01(14) 3_745 . ?
O1 Co1 O3 92.99(14) . . ?
O2 Co1 O3 94.12(14) . . ?
O2 Co1 O3 85.88(14) 3_745 . ?
O3 Co1 O3 180.00(14) 3_745 . ?
Co1 O1 H1A 117(6) . . ?
Co1 O1 H1B 120(5) . . ?
H1A O1 H1B 118(7) . . ?
Co1 O2 H2A 127(4) . . ?
Co1 O2 H2B 116(5) . . ?
H2A O2 H2B 100(5) . . ?
Co1 O3 H3A 121(5) . . ?
Co1 O3 H3B 113(4) . . ?
H3A O3 H3B 105(6) . . ?
H4A O4 H4B 107(6) . . ?
U1 F2 U1 112.75(10) 4_565 3_655 ?
U1 F3 U1 159.54(12) . 4_565 ?
U1 F4 U1 114.00(9) 2_645 . ?
U1 F5 U1 112.10(9) 2_655 4_565 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1A O3 0.77(9) 1.98(10) 2.747(5) 174(8) 2_744
O1 H1B O4 0.77(9) 2.22(8) 2.948(5) 157(7) 3_745
O2 H2A F1 0.92(6) 1.80(6) 2.720(4) 173(6) 3_655
O4 H4A F1 0.89(6) 2.54(6) 3.301(4) 144(5) 3_655
O2 H2B F5 0.78(7) 2.13(7) 2.917(4) 176(7) 1_545
O3 H3A O4 0.78(7) 2.00(6) 2.747(5) 160(7) 3_755
O3 H3B F1 0.87(6) 1.80(6) 2.641(4) 162(5) 4_655
O4 H4A F2 0.89(6) 2.09(7) 2.837(4) 141(5) .
O4 H4B F4 0.75(7) 2.02(7) 2.758(4) 170(7) .

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        28.29
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.314
_refine_diff_density_min         -1.410
_refine_diff_density_rms         0.234
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_15on
_database_code_depnum_ccdc_archive 'CCDC 1515454'
_audit_update_record             
;
2016-11-07 deposited with the CCDC.
2016-12-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'F6 H6 Mn O3 U'
_chemical_formula_sum            'F6 H6 Mn O3 U'
_chemical_formula_weight         461.02

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   12.366(4)
_cell_length_b                   6.975(2)
_cell_length_c                   8.081(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.201(6)
_cell_angle_gamma                90.00
_cell_volume                     695.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    3372
_cell_measurement_theta_min      3.2999
_cell_measurement_theta_max      28.2733

_exptl_crystal_description       rod
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    4.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             804
_exptl_absorpt_coefficient_mu    25.134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1524
_exptl_absorpt_correction_T_max  0.3139
_exptl_absorpt_process_details   'SADABS Version 2014/4 (Bruker, 2014)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      294(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4427
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.30
_diffrn_reflns_theta_max         28.30
_reflns_number_total             872
_reflns_number_gt                862
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART Version 5.631 (Bruker, 2001)'
_computing_cell_refinement       'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    various
_computing_publication_material  various

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0204P)²+0.1830P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         872
_refine_ls_number_parameters     65
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0154
_refine_ls_R_factor_gt           0.0152
_refine_ls_wR_factor_ref         0.0372
_refine_ls_wR_factor_gt          0.0371
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.01863(2) 0.7500 0.01960(7) Uani 1 2 d S . .
Mn1 Mn 0.2500 0.2500 0.0000 0.02296(16) Uani 1 2 d S . .
F1 F 0.38348(17) 0.2123(3) 0.1677(3) 0.0300(5) Uani 1 1 d . . .
F2 F 0.33538(17) 0.1481(3) -0.2000(3) 0.0302(5) Uani 1 1 d . . .
F3 F 0.43394(17) 0.1343(3) 0.4952(2) 0.0297(5) Uani 1 1 d . . .
O1 O 0.3167(3) 0.5320(5) -0.0607(5) 0.0375(7) Uani 1 1 d . . .
O2 O 0.5000 0.3893(6) 0.7500 0.0450(11) Uani 1 2 d S . .
H1A H 0.285(6) 0.580(11) -0.143(9) 0.07(2) Uiso 1 1 d . . .
H1B H 0.360(6) 0.606(11) -0.025(8) 0.08(2) Uiso 1 1 d . . .
H2 H 0.445(6) 0.466(7) 0.776(9) 0.051(18) Uiso 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 F1 2.238(2) 6_556 ?
U1 F1 2.238(2) 5_656 ?
U1 F2 2.284(2) 2_655 ?
U1 F2 2.284(2) 1_556 ?
U1 F3 2.318(2) 2_656 ?
U1 F3 2.318(2) . ?
U1 F3 2.431(2) 5_656 ?
U1 F3 2.431(2) 6_556 ?
U1 O2 2.585(5) . ?
U1 U1 4.0488(14) 5_656 ?
U1 U1 4.0488(14) 5_657 ?
Mn1 F1 2.093(2) . ?
Mn1 F1 2.093(2) 7 ?
Mn1 F2 2.103(2) . ?
Mn1 F2 2.103(2) 7 ?
Mn1 O1 2.199(3) . ?
Mn1 O1 2.199(3) 7 ?
F1 U1 2.238(2) 5_656 ?
F2 U1 2.284(2) 1_554 ?
F3 U1 2.431(2) 5_656 ?
O1 H1A 0.82(7) . ?
O1 H1B 0.78(8) . ?
O2 H2 0.90(6) . ?

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
F1 U1 F1 87.91(12) 6_556 5_656 ?
F1 U1 F2 142.92(8) 6_556 2_655 ?
F1 U1 F2 76.80(9) 5_656 2_655 ?
F1 U1 F2 76.80(9) 6_556 1_556 ?
F1 U1 F2 142.92(8) 5_656 1_556 ?
F2 U1 F2 133.40(12) 2_655 1_556 ?
F1 U1 F3 134.75(7) 6_556 2_656 ?
F1 U1 F3 78.30(8) 5_656 2_656 ?
F2 U1 F3 75.28(8) 2_655 2_656 ?
F2 U1 F3 88.78(8) 1_556 2_656 ?
F1 U1 F3 78.30(8) 6_556 . ?
F1 U1 F3 134.75(7) 5_656 . ?
F2 U1 F3 88.78(8) 2_655 . ?
F2 U1 F3 75.28(8) 1_556 . ?
F3 U1 F3 139.26(11) 2_656 . ?
F1 U1 F3 71.46(8) 6_556 5_656 ?
F1 U1 F3 71.72(7) 5_656 5_656 ?
F2 U1 F3 71.70(8) 2_655 5_656 ?
F2 U1 F3 131.38(7) 1_556 5_656 ?
F3 U1 F3 139.37(10) 2_656 5_656 ?
F3 U1 F3 63.03(9) . 5_656 ?
F1 U1 F3 71.72(7) 6_556 6_556 ?
F1 U1 F3 71.46(8) 5_656 6_556 ?
F2 U1 F3 131.38(7) 2_655 6_556 ?
F2 U1 F3 71.70(8) 1_556 6_556 ?
F3 U1 F3 63.03(9) 2_656 6_556 ?
F3 U1 F3 139.37(10) . 6_556 ?
F3 U1 F3 127.96(11) 5_656 6_556 ?
F1 U1 O2 136.04(6) 6_556 . ?
F1 U1 O2 136.04(6) 5_656 . ?
F2 U1 O2 66.70(6) 2_655 . ?
F2 U1 O2 66.70(6) 1_556 . ?
F3 U1 O2 69.63(6) 2_656 . ?
F3 U1 O2 69.63(6) . . ?
F3 U1 O2 116.02(5) 5_656 . ?
F3 U1 O2 116.02(5) 6_556 . ?
F1 U1 U1 72.12(5) 6_556 5_656 ?
F1 U1 U1 102.39(5) 5_656 5_656 ?
F2 U1 U1 78.42(5) 2_655 5_656 ?
F2 U1 U1 104.56(5) 1_556 5_656 ?
F3 U1 U1 152.80(5) 2_656 5_656 ?
F3 U1 U1 32.36(5) . 5_656 ?
F3 U1 U1 30.67(5) 5_656 5_656 ?
F3 U1 U1 143.49(5) 6_556 5_656 ?
O2 U1 U1 93.680(5) . 5_656 ?
F1 U1 U1 102.39(5) 6_556 5_657 ?
F1 U1 U1 72.12(5) 5_656 5_657 ?
F2 U1 U1 104.56(5) 2_655 5_657 ?
F2 U1 U1 78.42(5) 1_556 5_657 ?
F3 U1 U1 32.36(5) 2_656 5_657 ?
F3 U1 U1 152.80(5) . 5_657 ?
F3 U1 U1 143.49(5) 5_656 5_657 ?
F3 U1 U1 30.67(5) 6_556 5_657 ?
O2 U1 U1 93.680(5) . 5_657 ?
U1 U1 U1 172.639(9) 5_656 5_657 ?
F1 Mn1 F1 180.00(14) . 7 ?
F1 Mn1 F2 92.49(9) . . ?
F1 Mn1 F2 87.51(9) 7 . ?
F1 Mn1 F2 87.51(9) . 7 ?
F1 Mn1 F2 92.49(9) 7 7 ?
F2 Mn1 F2 180.00(16) . 7 ?
F1 Mn1 O1 87.97(12) . . ?
F1 Mn1 O1 92.03(12) 7 . ?
F2 Mn1 O1 85.43(12) . . ?
F2 Mn1 O1 94.57(12) 7 . ?
F1 Mn1 O1 92.03(12) . 7 ?
F1 Mn1 O1 87.97(12) 7 7 ?
F2 Mn1 O1 94.57(12) . 7 ?
F2 Mn1 O1 85.43(12) 7 7 ?
O1 Mn1 O1 180.0 . 7 ?
Mn1 F1 U1 138.98(11) . 5_656 ?
Mn1 F2 U1 139.48(10) . 1_554 ?
U1 F3 U1 116.97(9) . 5_656 ?
Mn1 O1 H1A 112(5) . . ?
Mn1 O1 H1B 139(5) . . ?
H1A O1 H1B 108(7) . . ?
U1 O2 H2 126(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1A F2 0.82(7) 1.96(7) 2.743(4) 159(7) 4_554
O1 H1A F1 0.82(7) 2.48(7) 2.981(4) 121(6) 6_565
O1 H1B F3 0.78(8) 2.04(8) 2.766(4) 155(7) 6_565
O2 H2 O1 0.90(6) 2.16(7) 2.976(4) 149(6) 1_556
O2 H2 F1 0.90(6) 2.51(6) 3.184(5) 132(5) 6_566

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        28.30
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.817
_refine_diff_density_min         -1.245
_refine_diff_density_rms         0.160
_exptl_crystal_recrystallization_method 'Hydrothermal Growth'
_exptl_crystal_preparation       ', Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jwj1026a
_database_code_depnum_ccdc_archive 'CCDC 1515455'
_audit_update_record             
;
2016-11-07 deposited with the CCDC.
2016-12-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'F6 H6 O3 U Zn'
_chemical_formula_sum            'F6 H6 O3 U Zn'
_chemical_formula_weight         471.45

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'
Zn Zn 0.2839 1.4301 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   12.1137(7)
_cell_length_b                   6.9186(4)
_cell_length_c                   7.9813(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.9113(15)
_cell_angle_gamma                90
_cell_volume                     668.05(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9915
_cell_measurement_theta_min      3.368
_cell_measurement_theta_max      32.596

_exptl_crystal_description       needle
_exptl_crystal_colour            'light green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    4.687
_exptl_crystal_F_000             824
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    27.884
_shelx_estimated_absorpt_T_min   0.167
_shelx_estimated_absorpt_T_max   0.402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0313
_exptl_absorpt_correction_T_max  0.0725
_exptl_absorpt_process_details   'SADABS Version 2014/4 (Bruker, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean 10.4
_diffrn_reflns_number            14520
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.368
_diffrn_reflns_theta_max         32.606
_diffrn_reflns_theta_full        32.605
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1221
_reflns_number_gt                1211
_reflns_threshold_expression     'I > 2σ(I)'

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEXII v2014.9-0 (Bruker, 2014)'
_computing_cell_refinement       'SAINT Version 8.34a (Bruker, 2014)'
_computing_data_reduction        'SAINT Version 8.34a (Bruker, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    various
_computing_publication_material  various
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0002P)²+1.4014P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.01040(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1221
_refine_ls_number_parameters     66
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0102
_refine_ls_R_factor_gt           0.0100
_refine_ls_wR_factor_ref         0.0235
_refine_ls_wR_factor_gt          0.0235
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_restrained_S_all      1.130
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.0000 0.01807(2) 0.2500 0.00802(4) Uani 1 2 d S T P . .
Zn1 Zn 0.2500 0.2500 0.0000 0.00939(6) Uani 1 2 d S . P . .
F1 F 0.16988(9) 0.14466(17) 0.19745(14) 0.0126(2) Uani 1 1 d . . . . .
F2 F 0.38076(10) 0.28654(17) 0.16174(14) 0.0124(2) Uani 1 1 d . . . . .
F3 F 0.06857(10) 0.13579(17) 0.50601(14) 0.0132(2) Uani 1 1 d . . . . .
O1 O 0.18212(14) 0.5185(2) 0.0658(2) 0.0141(3) Uani 1 1 d . . . . .
H1A H 0.215(3) 0.571(5) 0.137(5) 0.025(8) Uiso 1 1 d . . . . .
H1B H 0.157(3) 0.604(6) 0.008(5) 0.041(10) Uiso 1 1 d . . . . .
O2 O 0.0000 0.3846(3) 0.2500 0.0226(5) Uani 1 2 d S T P . .
H2 H 0.044(4) 0.456(6) 0.209(6) 0.040(11) Uiso 1 1 d . . . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 F2 2.2461(11) 3_445 ?
U1 F2 2.2461(11) 4_545 ?
U1 F1 2.2947(11) 2 ?
U1 F1 2.2947(11) . ?
U1 F3 2.3143(11) 2 ?
U1 F3 2.3143(11) . ?
U1 F3 2.4040(12) 6 ?
U1 F3 2.4040(12) 5_556 ?
U1 O2 2.536(2) . ?
U1 U1 3.9985(2) 5 ?
U1 U1 3.9985(2) 5_556 ?
Zn1 F2 2.0079(11) . ?
Zn1 F2 2.0079(11) 7 ?
Zn1 F1 2.0278(11) . ?
Zn1 F1 2.0278(11) 7 ?
Zn1 O1 2.1090(15) . ?
Zn1 O1 2.1090(15) 7 ?
F2 U1 2.2462(11) 3 ?
F3 U1 2.4041(12) 5_556 ?

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
F2 U1 F2 89.01(6) 3_445 4_545 ?
F2 U1 F1 76.18(4) 3_445 2 ?
F2 U1 F1 141.56(4) 4_545 2 ?
F2 U1 F1 141.56(4) 3_445 . ?
F2 U1 F1 76.18(4) 4_545 . ?
F1 U1 F1 135.12(6) 2 . ?
F2 U1 F3 77.16(4) 3_445 2 ?
F2 U1 F3 136.40(4) 4_545 2 ?
F1 U1 F3 75.05(4) 2 2 ?
F1 U1 F3 89.39(4) . 2 ?
F2 U1 F3 136.40(4) 3_445 . ?
F2 U1 F3 77.16(4) 4_545 . ?
F1 U1 F3 89.39(4) 2 . ?
F1 U1 F3 75.05(4) . . ?
F3 U1 F3 138.79(6) 2 . ?
F2 U1 F3 70.93(4) 3_445 6 ?
F2 U1 F3 72.25(4) 4_545 6 ?
F1 U1 F3 131.84(4) 2 6 ?
F1 U1 F3 70.79(4) . 6 ?
F3 U1 F3 64.15(5) 2 6 ?
F3 U1 F3 138.39(5) . 6 ?
F2 U1 F3 72.25(4) 3_445 5_556 ?
F2 U1 F3 70.93(4) 4_545 5_556 ?
F1 U1 F3 70.79(4) 2 5_556 ?
F1 U1 F3 131.84(4) . 5_556 ?
F3 U1 F3 138.40(5) 2 5_556 ?
F3 U1 F3 64.15(5) . 5_556 ?
F3 U1 F3 127.44(6) 6 5_556 ?
F2 U1 O2 135.49(3) 3_445 . ?
F2 U1 O2 135.49(3) 4_545 . ?
F1 U1 O2 67.56(3) 2 . ?
F1 U1 O2 67.56(3) . . ?
F3 U1 O2 69.40(3) 2 . ?
F3 U1 O2 69.39(3) . . ?
F3 U1 O2 116.28(3) 6 . ?
F3 U1 O2 116.28(3) 5_556 . ?
F2 U1 U1 71.03(3) 3_445 5 ?
F2 U1 U1 103.64(3) 4_545 5 ?
F1 U1 U1 104.58(3) 2 5 ?
F1 U1 U1 78.23(3) . 5 ?
F3 U1 U1 32.76(3) 2 5 ?
F3 U1 U1 152.25(3) . 5 ?
F3 U1 U1 31.39(3) 6 5 ?
F3 U1 U1 142.96(3) 5_556 5 ?
O2 U1 U1 93.586(3) . 5 ?
F2 U1 U1 103.64(3) 3_445 5_556 ?
F2 U1 U1 71.03(3) 4_545 5_556 ?
F1 U1 U1 78.23(3) 2 5_556 ?
F1 U1 U1 104.58(3) . 5_556 ?
F3 U1 U1 152.25(3) 2 5_556 ?
F3 U1 U1 32.76(3) . 5_556 ?
F3 U1 U1 142.96(3) 6 5_556 ?
F3 U1 U1 31.39(3) 5_556 5_556 ?
O2 U1 U1 93.586(2) . 5_556 ?
U1 U1 U1 172.829(5) 5 5_556 ?
F2 Zn1 F2 180.0 . 7 ?
F2 Zn1 F1 86.49(5) . . ?
F2 Zn1 F1 93.51(5) 7 . ?
F2 Zn1 F1 93.51(5) . 7 ?
F2 Zn1 F1 86.49(5) 7 7 ?
F1 Zn1 F1 180.0 . 7 ?
F2 Zn1 O1 91.93(6) . . ?
F2 Zn1 O1 88.07(6) 7 . ?
F1 Zn1 O1 85.12(6) . . ?
F1 Zn1 O1 94.88(6) 7 . ?
F2 Zn1 O1 88.07(6) . 7 ?
F2 Zn1 O1 91.93(6) 7 7 ?
F1 Zn1 O1 94.88(6) . 7 ?
F1 Zn1 O1 85.12(6) 7 7 ?
O1 Zn1 O1 180.0 . 7 ?
Zn1 F1 U1 138.44(6) . . ?
Zn1 F2 U1 139.92(6) . 3 ?
U1 F3 U1 115.85(5) . 5_556 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1A F1 0.77(4) 1.94(4) 2.683(2) 163(4) 4
O1 H1A F2 0.77(4) 2.52(3) 2.986(2) 121(3) 4
O1 H1B F3 0.80(4) 2.09(4) 2.7881(19) 145(4) 6_565
O2 H2 O1 0.81(4) 2.11(4) 2.8662(19) 154(4) .

_refine_diff_density_max         1.281
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.133



_exptl_crystal_recrystallization_method 'Hydrothermal Growth'
_exptl_crystal_preparation       ', Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jwj1015c_1
_database_code_depnum_ccdc_archive 'CCDC 1515456'
_audit_update_record             
;
2016-11-07 deposited with the CCDC.
2016-12-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(F5 U), H12 O6 Zn, 2(H2 O)'
_chemical_formula_sum            'F10 H16 O8 U2 Zn'
_chemical_formula_weight         875.56

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'
Zn Zn 0.2839 1.4301 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.0116(5)
_cell_length_b                   7.0571(3)
_cell_length_c                   8.8476(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.2424(13)
_cell_angle_gamma                90
_cell_volume                     685.66(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9956
_cell_measurement_theta_min      3.432
_cell_measurement_theta_max      30.051

_exptl_crystal_description       'rhombic plate'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    4.241
_exptl_crystal_F_000             768
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    25.448
_shelx_estimated_absorpt_T_min   0.235
_shelx_estimated_absorpt_T_max   0.429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0312
_exptl_absorpt_correction_T_max  0.0846
_exptl_absorpt_process_details   'SADABS Version 2014/4 (Bruker, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean 10.4
_diffrn_reflns_number            28820
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.432
_diffrn_reflns_theta_max         30.065
_diffrn_reflns_theta_full        30.065
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2015
_reflns_number_gt                1941
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEXII v2014.9-0 (Bruker, 2014)'
_computing_cell_refinement       'SAINT Version 8.34a (Bruker, 2014)'
_computing_data_reduction        'SAINT Version 8.34a (Bruker, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    various
_computing_publication_material  various
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0123P)²+0.8800P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00702(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2015
_refine_ls_number_parameters     130
_refine_ls_number_restraints     29
_refine_ls_R_factor_all          0.0130
_refine_ls_R_factor_gt           0.0118
_refine_ls_wR_factor_ref         0.0277
_refine_ls_wR_factor_gt          0.0272
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.04621(2) 0.34530(2) 0.17665(2) 0.00694(4) Uani 1 1 d . . . . .
Zn1 Zn 0.5000 0.0000 0.5000 0.00906(8) Uani 1 2 d S . P . .
F1 F 0.24666(14) 0.33436(18) 0.21432(17) 0.0123(3) Uani 1 1 d . . . . .
F2 F 0.11341(13) 0.64071(18) 0.29301(16) 0.0100(3) Uani 1 1 d . . . . .
F3 F 0.10178(12) 0.02816(19) 0.21385(15) 0.0094(3) Uani 1 1 d . . . . .
F4 F 0.06847(13) 0.2952(2) 0.43882(15) 0.0108(3) Uani 1 1 d . . . . .
F5 F 0.11303(12) 0.56302(19) -0.00022(15) 0.0100(3) Uani 1 1 d . . . . .
O1 O 0.33768(16) 0.0243(3) 0.3656(2) 0.0126(3) Uani 1 1 d D . . . .
H1A H 0.278(2) -0.007(5) 0.401(4) 0.025(10) Uiso 1 1 d D . . . .
H1B H 0.322(4) 0.116(4) 0.318(4) 0.028(10) Uiso 1 1 d D . . . .
O2 O 0.47346(17) 0.2752(3) 0.5740(2) 0.0137(3) Uani 1 1 d D . . . .
H2A H 0.512(3) 0.314(5) 0.645(3) 0.025(10) Uiso 1 1 d D . . . .
H2B H 0.418(3) 0.344(4) 0.555(4) 0.022(10) Uiso 1 1 d D . . . .
O3 O 0.60499(17) 0.1176(3) 0.3336(2) 0.0118(3) Uani 1 1 d D . . . .
H3A H 0.653(3) 0.042(4) 0.310(4) 0.033(11) Uiso 1 1 d D . . . .
H3B H 0.642(4) 0.209(5) 0.354(6) 0.056(14) Uiso 1 1 d D . . . .
O4 O 0.28726(16) 0.5680(3) 0.5376(2) 0.0134(3) Uani 1 1 d D . . . .
H4A H 0.249(3) 0.593(5) 0.461(2) 0.023(9) Uiso 1 1 d D . . . .
H4B H 0.232(3) 0.550(5) 0.588(3) 0.029(10) Uiso 1 1 d D . . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 F1 2.2092(15) . ?
U1 F2 2.3055(14) 2_545 ?
U1 F3 2.3371(13) . ?
U1 F4 2.3412(13) . ?
U1 F3 2.3437(13) 2 ?
U1 F5 2.3498(13) . ?
U1 F5 2.3506(13) 3_565 ?
U1 F4 2.3553(13) 4_565 ?
U1 F2 2.4168(13) . ?
U1 U1 3.88633(19) 3_565 ?
U1 U1 3.91997(16) 2_545 ?
U1 U1 3.92000(16) 2 ?
Zn1 O2 2.0767(18) . ?
Zn1 O2 2.0767(18) 3_656 ?
Zn1 O1 2.0796(18) . ?
Zn1 O1 2.0796(18) 3_656 ?
Zn1 O3 2.1085(18) . ?
Zn1 O3 2.1085(18) 3_656 ?
F2 U1 2.3056(14) 2 ?
F3 U1 2.3437(13) 2_545 ?
F4 U1 2.3553(13) 4_566 ?
F5 U1 2.3506(13) 3_565 ?
O1 H1A 0.785(18) . ?
O1 H1B 0.783(19) . ?
O2 H2A 0.785(19) . ?
O2 H2B 0.784(18) . ?
O3 H3A 0.791(19) . ?
O3 H3B 0.780(19) . ?
O4 H4A 0.789(18) . ?
O4 H4B 0.793(18) . ?

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
F1 U1 F2 136.25(5) . 2_545 ?
F1 U1 F3 72.36(5) . . ?
F2 U1 F3 65.03(5) 2_545 . ?
F1 U1 F4 79.34(5) . . ?
F2 U1 F4 79.34(5) 2_545 . ?
F3 U1 F4 73.07(5) . . ?
F1 U1 F3 132.41(5) . 2 ?
F2 U1 F3 74.77(5) 2_545 2 ?
F3 U1 F3 130.68(3) . 2 ?
F4 U1 F3 72.46(5) . 2 ?
F1 U1 F5 76.39(5) . . ?
F2 U1 F5 139.99(5) 2_545 . ?
F3 U1 F5 128.93(5) . . ?
F4 U1 F5 138.04(5) . . ?
F3 U1 F5 100.19(5) 2 . ?
F1 U1 F5 142.92(5) . 3_565 ?
F2 U1 F5 73.26(5) 2_545 3_565 ?
F3 U1 F5 122.12(5) . 3_565 ?
F4 U1 F5 135.87(5) . 3_565 ?
F3 U1 F5 67.40(5) 2 3_565 ?
F5 U1 F5 68.45(5) . 3_565 ?
F1 U1 F4 87.20(5) . 4_565 ?
F2 U1 F4 88.34(5) 2_545 4_565 ?
F3 U1 F4 71.29(5) . 4_565 ?
F4 U1 F4 144.23(2) . 4_565 ?
F3 U1 F4 136.27(5) 2 4_565 ?
F5 U1 F4 67.78(5) . 4_565 ?
F5 U1 F4 69.17(5) 3_565 4_565 ?
F1 U1 F2 72.23(5) . . ?
F2 U1 F2 134.64(2) 2_545 . ?
F3 U1 F2 134.22(5) . . ?
F4 U1 F2 72.66(5) . . ?
F3 U1 F2 63.21(5) 2 . ?
F5 U1 F2 67.58(5) . . ?
F5 U1 F2 103.61(5) 3_565 . ?
F4 U1 F2 134.02(5) 4_565 . ?
F1 U1 U1 109.89(4) . 3_565 ?
F2 U1 U1 106.79(4) 2_545 3_565 ?
F3 U1 U1 134.55(3) . 3_565 ?
F4 U1 U1 152.10(3) . 3_565 ?
F3 U1 U1 82.79(3) 2 3_565 ?
F5 U1 U1 34.23(3) . 3_565 ?
F5 U1 U1 34.22(3) 3_565 3_565 ?
F4 U1 U1 63.66(3) 4_565 3_565 ?
F2 U1 U1 84.93(3) . 3_565 ?
F1 U1 U1 101.51(3) . 2_545 ?
F2 U1 U1 34.81(3) 2_545 2_545 ?
F3 U1 U1 33.18(3) . 2_545 ?
F4 U1 U1 63.05(4) . 2_545 ?
F3 U1 U1 98.82(3) 2 2_545 ?
F5 U1 U1 155.62(3) . 2_545 ?
F5 U1 U1 105.57(3) 3_565 2_545 ?
F4 U1 U1 87.91(3) 4_565 2_545 ?
F2 U1 U1 135.58(3) . 2_545 ?
U1 U1 U1 135.486(4) 3_565 2_545 ?
F1 U1 U1 105.22(3) . 2 ?
F2 U1 U1 107.84(3) 2_545 2 ?
F3 U1 U1 152.51(3) . 2 ?
F4 U1 U1 79.55(3) . 2 ?
F3 U1 U1 33.08(3) 2 2 ?
F5 U1 U1 74.56(3) . 2 ?
F5 U1 U1 76.88(3) 3_565 2 ?
F4 U1 U1 136.18(3) 4_565 2 ?
F2 U1 U1 33.00(3) . 2 ?
U1 U1 U1 72.641(4) 3_565 2 ?
U1 U1 U1 128.354(5) 2_545 2 ?
O2 Zn1 O2 180.0 . 3_656 ?
O2 Zn1 O1 88.17(7) . . ?
O2 Zn1 O1 91.83(7) 3_656 . ?
O2 Zn1 O1 91.83(7) . 3_656 ?
O2 Zn1 O1 88.17(7) 3_656 3_656 ?
O1 Zn1 O1 180.00(10) . 3_656 ?
O2 Zn1 O3 87.10(7) . . ?
O2 Zn1 O3 92.90(7) 3_656 . ?
O1 Zn1 O3 93.47(7) . . ?
O1 Zn1 O3 86.53(7) 3_656 . ?
O2 Zn1 O3 92.90(7) . 3_656 ?
O2 Zn1 O3 87.10(7) 3_656 3_656 ?
O1 Zn1 O3 86.53(7) . 3_656 ?
O1 Zn1 O3 93.47(7) 3_656 3_656 ?
O3 Zn1 O3 180.0 . 3_656 ?
U1 F2 U1 112.20(6) 2 . ?
U1 F3 U1 113.74(5) . 2_545 ?
U1 F4 U1 159.81(7) . 4_566 ?
U1 F5 U1 111.55(5) . 3_565 ?
Zn1 O1 H1A 117(3) . . ?
Zn1 O1 H1B 121(3) . . ?
H1A O1 H1B 107(4) . . ?
Zn1 O2 H2A 120(3) . . ?
Zn1 O2 H2B 129(3) . . ?
H2A O2 H2B 109(4) . . ?
Zn1 O3 H3A 109(3) . . ?
Zn1 O3 H3B 118(4) . . ?
H3A O3 H3B 105(5) . . ?
H4A O4 H4B 98(3) . . ?


loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1A F3 0.785(18) 2.47(3) 2.834(2) 110(3) .
O1 H1A F5 0.785(18) 2.106(19) 2.889(2) 174(4) 4_566
O1 H1B F1 0.783(19) 1.95(2) 2.717(2) 167(4) .
O2 H2A O3 0.785(19) 1.949(19) 2.730(3) 173(4) 4_566
O2 H2B O4 0.784(18) 2.140(19) 2.912(3) 168(4) .
O3 H3A F1 0.791(19) 1.86(2) 2.635(2) 168(4) 2_645
O3 H3B O4 0.780(19) 1.97(2) 2.726(3) 163(5) 3_666
O4 H4A F2 0.789(18) 2.06(2) 2.828(2) 166(4) .
O4 H4B F3 0.793(18) 1.957(19) 2.745(2) 172(4) 4_566

_refine_diff_density_max         1.099
_refine_diff_density_min         -1.106
_refine_diff_density_rms         0.135



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jbf1186d
_database_code_depnum_ccdc_archive 'CCDC 1515457'
_audit_update_record             
;
2016-11-07 deposited with the CCDC.
2016-12-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(F5 U), H12 Ni O6, 2(H2 O)'
_chemical_formula_sum            'F10 H16 Ni O8 U2'
_chemical_formula_weight         868.90

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.9605(7)
_cell_length_b                   7.0441(4)
_cell_length_c                   8.8514(6)
_cell_angle_alpha                90
_cell_angle_beta                 94.532(2)
_cell_angle_gamma                90
_cell_volume                     681.25(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9001
_cell_measurement_theta_min      3.441
_cell_measurement_theta_max      39.014

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    4.236
_exptl_crystal_F_000             764
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    25.234
_shelx_estimated_absorpt_T_min   0.237
_shelx_estimated_absorpt_T_max   0.432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0376
_exptl_absorpt_correction_T_max  0.1158
_exptl_absorpt_process_details   'SADABS Version 2014/4 (Bruker, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean 10.4
_diffrn_reflns_number            40599
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.441
_diffrn_reflns_theta_max         37.782
_diffrn_reflns_theta_full        37.780
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3655
_reflns_number_gt                3456
_reflns_threshold_expression     'I > 2σ(I)'

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEXII v2014.9-0 (Bruker, 2014)'
_computing_cell_refinement       'SAINT Version 8.34a (Bruker, 2014)'
_computing_data_reduction        'SAINT Version 8.34a (Bruker, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    various
_computing_publication_material  various
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0042P)²+0.7012P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00492(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3655
_refine_ls_number_parameters     130
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.0175
_refine_ls_R_factor_gt           0.0150
_refine_ls_wR_factor_ref         0.0276
_refine_ls_wR_factor_gt          0.0272
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      1.121
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.04681(2) 0.34525(2) 0.17671(2) 0.00548(2) Uani 1 1 d . . . . .
Ni1 Ni 0.5000 0.0000 0.5000 0.00713(5) Uani 1 2 d S . P . .
F1 F 0.24811(10) 0.33473(15) 0.21597(13) 0.01077(19) Uani 1 1 d . . . . .
F2 F 0.11382(10) 0.64101(14) 0.29334(12) 0.00892(18) Uani 1 1 d . . . . .
F3 F 0.10266(9) 0.02797(15) 0.21431(12) 0.00832(18) Uani 1 1 d . . . . .
F4 F 0.06922(10) 0.29517(16) 0.43905(12) 0.00959(18) Uani 1 1 d . . . . .
F5 F 0.11361(9) 0.56357(15) 0.00004(12) 0.00841(18) Uani 1 1 d . . . . .
O1 O 0.33924(12) 0.0225(2) 0.36624(16) 0.0109(2) Uani 1 1 d D . . . .
H1A H 0.279(2) -0.013(4) 0.398(3) 0.032(9) Uiso 1 1 d D . . . .
H1B H 0.323(3) 0.120(3) 0.326(4) 0.036(10) Uiso 1 1 d D . . . .
O2 O 0.47413(13) 0.2710(2) 0.57354(16) 0.0120(2) Uani 1 1 d D . . . .
H2A H 0.512(3) 0.306(4) 0.648(2) 0.026(8) Uiso 1 1 d D . . . .
H2B H 0.414(2) 0.334(4) 0.559(4) 0.025(8) Uiso 1 1 d D . . . .
O3 O 0.60213(13) 0.11689(19) 0.33603(16) 0.0100(2) Uani 1 1 d D . . . .
H3A H 0.650(2) 0.040(3) 0.313(3) 0.023(8) Uiso 1 1 d D . . . .
H3B H 0.634(3) 0.214(3) 0.355(4) 0.043(10) Uiso 1 1 d D . . . .
O4 O 0.28818(12) 0.5676(2) 0.53810(16) 0.0116(2) Uani 1 1 d D . . . .
H4A H 0.251(3) 0.591(4) 0.460(2) 0.021(7) Uiso 1 1 d D . . . .
H4B H 0.233(2) 0.548(4) 0.587(3) 0.018(7) Uiso 1 1 d D . . . .


_geom_special_details            
; 
All O-H distances restrained to be similar (SHELX SADI) with esd 0.02 A 
  
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 F1 2.2075(11) . ?
U1 F2 2.3052(11) 2_545 ?
U1 F3 2.3341(10) . ?
U1 F4 2.3424(11) . ?
U1 F5 2.3489(10) 3_565 ?
U1 F3 2.3497(10) 2 ?
U1 F5 2.3511(10) . ?
U1 F4 2.3549(11) 4_565 ?
U1 F2 2.4136(10) . ?
U1 U1 3.8840(2) 3_565 ?
U1 U1 3.91809(18) 2 ?
U1 U1 3.91813(19) 2_545 ?
Ni1 O2 2.0442(14) . ?
Ni1 O2 2.0442(14) 3_656 ?
Ni1 O1 2.0498(13) . ?
Ni1 O1 2.0498(13) 3_656 ?
Ni1 O3 2.0722(14) . ?
Ni1 O3 2.0722(14) 3_656 ?
F2 U1 2.3051(11) 2 ?
F3 U1 2.3497(10) 2_545 ?
F4 U1 2.3549(11) 4_566 ?
F5 U1 2.3489(10) 3_565 ?
O1 H1A 0.782(17) . ?
O1 H1B 0.788(17) . ?
O2 H2A 0.791(17) . ?
O2 H2B 0.791(17) . ?
O3 H3A 0.792(17) . ?
O3 H3B 0.783(17) . ?
O4 H4A 0.795(17) . ?
O4 H4B 0.784(16) . ?

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
F1 U1 F2 136.38(4) . 2_545 ?
F1 U1 F3 72.41(4) . . ?
F2 U1 F3 65.17(4) 2_545 . ?
F1 U1 F4 79.26(4) . . ?
F2 U1 F4 79.23(4) 2_545 . ?
F3 U1 F4 73.06(4) . . ?
F1 U1 F5 143.16(4) . 3_565 ?
F2 U1 F5 73.07(4) 2_545 3_565 ?
F3 U1 F5 122.06(4) . 3_565 ?
F4 U1 F5 135.71(4) . 3_565 ?
F1 U1 F3 132.41(4) . 2 ?
F2 U1 F3 74.40(4) 2_545 2 ?
F3 U1 F3 130.50(3) . 2 ?
F4 U1 F3 72.39(4) . 2 ?
F5 U1 F3 67.30(4) 3_565 2 ?
F1 U1 F5 76.51(4) . . ?
F2 U1 F5 139.96(4) 2_545 . ?
F3 U1 F5 128.99(4) . . ?
F4 U1 F5 138.08(4) . . ?
F5 U1 F5 68.54(4) 3_565 . ?
F3 U1 F5 100.29(4) 2 . ?
F1 U1 F4 87.31(4) . 4_565 ?
F2 U1 F4 88.57(4) 2_545 4_565 ?
F3 U1 F4 71.37(4) . 4_565 ?
F4 U1 F4 144.306(19) . 4_565 ?
F5 U1 F4 69.22(4) 3_565 4_565 ?
F3 U1 F4 136.23(4) 2 4_565 ?
F5 U1 F4 67.71(4) . 4_565 ?
F1 U1 F2 72.25(4) . . ?
F2 U1 F2 134.338(19) 2_545 . ?
F3 U1 F2 134.26(4) . . ?
F4 U1 F2 72.63(4) . . ?
F5 U1 F2 103.61(4) 3_565 . ?
F3 U1 F2 63.26(4) 2 . ?
F5 U1 F2 67.64(4) . . ?
F4 U1 F2 134.02(4) 4_565 . ?
F1 U1 U1 110.05(3) . 3_565 ?
F2 U1 U1 106.70(3) 2_545 3_565 ?
F3 U1 U1 134.58(3) . 3_565 ?
F4 U1 U1 152.05(3) . 3_565 ?
F5 U1 U1 34.29(3) 3_565 3_565 ?
F3 U1 U1 82.81(3) 2 3_565 ?
F5 U1 U1 34.25(3) . 3_565 ?
F4 U1 U1 63.63(3) 4_565 3_565 ?
F2 U1 U1 84.96(3) . 3_565 ?
F1 U1 U1 105.23(3) . 2 ?
F2 U1 U1 107.49(3) 2_545 2 ?
F3 U1 U1 152.39(3) . 2 ?
F4 U1 U1 79.44(3) . 2 ?
F5 U1 U1 76.87(3) 3_565 2 ?
F3 U1 U1 33.10(3) 2 2 ?
F5 U1 U1 74.68(3) . 2 ?
F4 U1 U1 136.21(3) 4_565 2 ?
F2 U1 U1 32.99(3) . 2 ?
U1 U1 U1 72.703(4) 3_565 2 ?
F1 U1 U1 101.67(3) . 2_545 ?
F2 U1 U1 34.76(3) 2_545 2_545 ?
F3 U1 U1 33.35(3) . 2_545 ?
F4 U1 U1 63.00(3) . 2_545 ?
F5 U1 U1 105.34(3) 3_565 2_545 ?
F3 U1 U1 98.46(3) 2 2_545 ?
F5 U1 U1 155.74(3) . 2_545 ?
F4 U1 U1 88.09(3) 4_565 2_545 ?
F2 U1 U1 135.49(3) . 2_545 ?
U1 U1 U1 135.386(3) 3_565 2_545 ?
U1 U1 U1 128.032(5) 2 2_545 ?
O2 Ni1 O2 180.0 . 3_656 ?
O2 Ni1 O1 88.70(6) . . ?
O2 Ni1 O1 91.30(6) 3_656 . ?
O2 Ni1 O1 91.30(6) . 3_656 ?
O2 Ni1 O1 88.70(6) 3_656 3_656 ?
O1 Ni1 O1 180.00(8) . 3_656 ?
O2 Ni1 O3 87.03(5) . . ?
O2 Ni1 O3 92.97(5) 3_656 . ?
O1 Ni1 O3 92.98(6) . . ?
O1 Ni1 O3 87.02(6) 3_656 . ?
O2 Ni1 O3 92.97(5) . 3_656 ?
O2 Ni1 O3 87.03(5) 3_656 3_656 ?
O1 Ni1 O3 87.02(6) . 3_656 ?
O1 Ni1 O3 92.98(6) 3_656 3_656 ?
O3 Ni1 O3 180.0 . 3_656 ?
U1 F2 U1 112.24(4) 2 . ?
U1 F3 U1 113.55(4) . 2_545 ?
U1 F4 U1 159.83(5) . 4_566 ?
U1 F5 U1 111.46(4) 3_565 . ?
Ni1 O1 H1A 119(2) . . ?
Ni1 O1 H1B 119(3) . . ?
H1A O1 H1B 106(3) . . ?
Ni1 O2 H2A 119(2) . . ?
Ni1 O2 H2B 127(2) . . ?
H2A O2 H2B 109(3) . . ?
Ni1 O3 H3A 108(2) . . ?
Ni1 O3 H3B 117(3) . . ?
H3A O3 H3B 111(4) . . ?
H4A O4 H4B 99(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1A F3 0.782(17) 2.44(3) 2.8254(17) 112(3) .
O1 H1A F5 0.782(17) 2.116(18) 2.8894(17) 170(3) 4_566
O1 H1B F1 0.788(17) 1.946(19) 2.7193(18) 167(4) .
O2 H2A O3 0.791(17) 1.944(17) 2.734(2) 177(3) 4_566
O2 H2B O4 0.791(17) 2.150(18) 2.918(2) 164(3) .
O3 H3A F1 0.792(17) 1.857(17) 2.6412(17) 170(3) 2_645
O3 H3B O4 0.783(17) 1.96(2) 2.723(2) 163(4) 3_666
O4 H4A F2 0.795(17) 2.048(19) 2.8211(18) 164(3) .
O4 H4B F3 0.784(16) 1.961(17) 2.7426(17) 174(3) 4_566

_refine_diff_density_max         1.382
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.183



