# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 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_complex1
_database_code_depnum_ccdc_archive 'CCDC 1442294'
_audit_update_record             
;
2016-01-31 deposited with the CCDC.
2016-10-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Co F H3 O5 S'
_chemical_formula_weight         193.01

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'
H H 0.0000 0.0000 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P n n a'

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

_cell_length_a                   13.1891(6)
_cell_length_b                   10.6850(6)
_cell_length_c                   6.6081(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     931.25(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1429
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      30.6

_exptl_crystal_description       block
_exptl_crystal_colour            Pink
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.753
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             760
_exptl_absorpt_coefficient_mu    4.087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.415
_exptl_absorpt_correction_T_max  0.527
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14909
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0208
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         30.56
_reflns_number_total             1429
_reflns_number_gt                1356
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0000P)²+12.5013P] 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     SHELXL
_refine_ls_extinction_coef       0.0229(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1429
_refine_ls_number_parameters     99
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0541
_refine_ls_wR_factor_ref         0.1248
_refine_ls_wR_factor_gt          0.1241
_refine_ls_goodness_of_fit_ref   1.408
_refine_ls_restrained_S_all      1.477
_refine_ls_shift/su_max          0.000
_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
Co1 Co 0.5000 0.0000 0.0000 0.0114(3) Uani 1 2 d S . .
Co2 Co 0.62689(8) 0.2500 0.2500 0.0102(3) Uani 1 2 d S . .
S1 S 0.57006(14) 0.2500 -0.2500 0.0116(4) Uani 1 2 d S . .
S2 S 0.7500 0.0000 0.0874(3) 0.0105(4) Uani 1 2 d S . .
F1 F 0.5178(3) 0.1209(4) 0.2266(7) 0.0226(8) Uani 1 1 d . . .
O1 O 0.5030(3) 0.1430(4) -0.2081(7) 0.0171(9) Uani 1 1 d . . .
O2 O 0.6352(3) 0.2770(4) -0.0752(7) 0.0168(8) Uani 1 1 d . . .
O4 O 0.7345(3) 0.1097(4) 0.2202(7) 0.0192(9) Uani 1 1 d . . .
O3 O 0.6610(3) -0.0221(4) -0.0409(6) 0.0153(8) Uani 1 1 d . . .
O1WA O 0.3552(11) 0.1836(13) 0.442(2) 0.041(4) Uani 0.48(2) 1 d PD A 2
O1WB O 0.3680(10) 0.0716(14) 0.465(2) 0.045(4) Uani 0.52(2) 1 d PD A 1
H1A H 0.402(16) 0.130(7) 0.40(5) 0.25(16) Uiso 1 1 d D . .
H2A H 0.36(3) 0.136(5) 0.549(6) 0.6(5) Uiso 1 1 d D . .
H3A H 0.319(14) 0.117(3) 0.41(5) 0.4(3) Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0117(5) 0.0093(5) 0.0131(5) 0.0008(4) -0.0013(4) -0.0016(4)
Co2 0.0094(5) 0.0098(5) 0.0113(5) -0.0010(4) 0.000 0.000
S1 0.0126(8) 0.0111(8) 0.0110(8) 0.0013(7) 0.000 0.000
S2 0.0094(7) 0.0111(8) 0.0110(7) 0.000 0.000 0.0022(6)
F1 0.0191(16) 0.0195(18) 0.029(2) -0.0083(16) 0.0060(16) -0.0085(14)
O1 0.020(2) 0.0168(19) 0.014(2) 0.0072(16) -0.0041(16) -0.0065(16)
O2 0.0177(19) 0.021(2) 0.0122(18) -0.0003(16) -0.0019(15) -0.0036(16)
O4 0.021(2) 0.0174(19) 0.019(2) -0.0073(17) -0.0037(17) 0.0088(17)
O3 0.0088(16) 0.021(2) 0.0167(19) -0.0036(16) -0.0030(14) -0.0003(15)
O1WA 0.039(7) 0.043(8) 0.042(8) -0.002(6) 0.009(6) -0.016(6)
O1WB 0.037(7) 0.060(10) 0.038(7) -0.006(6) 0.009(6) -0.007(6)

_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
Co1 F1 1.991(4) 5_655 ?
Co1 F1 1.991(4) . ?
Co1 O1 2.056(4) . ?
Co1 O1 2.056(4) 5_655 ?
Co1 O3 2.154(4) . ?
Co1 O3 2.154(4) 5_655 ?
Co2 F1 1.999(4) . ?
Co2 F1 1.999(4) 2 ?
Co2 O4 2.073(4) 2 ?
Co2 O4 2.073(4) . ?
Co2 O2 2.171(4) 2 ?
Co2 O2 2.171(4) . ?
S1 O2 1.468(4) . ?
S1 O2 1.468(4) 2_554 ?
S1 O1 1.472(4) . ?
S1 O1 1.472(4) 2_554 ?
S2 O3 1.467(4) . ?
S2 O3 1.467(4) 4_655 ?
S2 O4 1.479(4) 4_655 ?
S2 O4 1.479(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
F1 Co1 F1 180.0(2) 5_655 . ?
F1 Co1 O1 88.94(17) 5_655 . ?
F1 Co1 O1 91.06(17) . . ?
F1 Co1 O1 91.06(17) 5_655 5_655 ?
F1 Co1 O1 88.94(17) . 5_655 ?
O1 Co1 O1 180.00(17) . 5_655 ?
F1 Co1 O3 87.18(15) 5_655 . ?
F1 Co1 O3 92.82(15) . . ?
O1 Co1 O3 88.77(17) . . ?
O1 Co1 O3 91.23(17) 5_655 . ?
F1 Co1 O3 92.82(15) 5_655 5_655 ?
F1 Co1 O3 87.18(15) . 5_655 ?
O1 Co1 O3 91.23(17) . 5_655 ?
O1 Co1 O3 88.77(17) 5_655 5_655 ?
O3 Co1 O3 180.00(4) . 5_655 ?
F1 Co2 F1 88.0(2) . 2 ?
F1 Co2 O4 177.05(17) . 2 ?
F1 Co2 O4 89.21(17) 2 2 ?
F1 Co2 O4 89.21(17) . . ?
F1 Co2 O4 177.05(17) 2 . ?
O4 Co2 O4 93.6(3) 2 . ?
F1 Co2 O2 91.23(18) . 2 ?
F1 Co2 O2 92.94(17) 2 2 ?
O4 Co2 O2 88.13(17) 2 2 ?
O4 Co2 O2 87.91(17) . 2 ?
F1 Co2 O2 92.94(17) . . ?
F1 Co2 O2 91.23(18) 2 . ?
O4 Co2 O2 87.91(17) 2 . ?
O4 Co2 O2 88.13(17) . . ?
O2 Co2 O2 174.2(2) 2 . ?
O2 S1 O2 108.4(4) . 2_554 ?
O2 S1 O1 110.9(2) . . ?
O2 S1 O1 110.3(3) 2_554 . ?
O2 S1 O1 110.3(3) . 2_554 ?
O2 S1 O1 110.9(2) 2_554 2_554 ?
O1 S1 O1 106.1(4) . 2_554 ?
O3 S2 O3 109.4(4) . 4_655 ?
O3 S2 O4 109.0(3) . 4_655 ?
O3 S2 O4 111.1(2) 4_655 4_655 ?
O3 S2 O4 111.1(2) . . ?
O3 S2 O4 109.0(3) 4_655 . ?
O4 S2 O4 107.2(4) 4_655 . ?
Co1 F1 Co2 126.2(2) . . ?
S1 O1 Co1 135.6(3) . . ?
S1 O2 Co2 136.3(3) . . ?
S2 O4 Co2 136.4(3) . . ?
S2 O3 Co1 134.3(3) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        30.56
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.808
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.194
####################################################################### 
# 
# 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_complex2
_database_code_depnum_ccdc_archive 'CCDC 1442295'
_audit_update_record             
;
2016-01-31 deposited with the CCDC.
2016-10-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'F H3 Ni O5 S'
_chemical_formula_weight         192.79

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'
H H 0.0000 0.0000 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P n n a'

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

_cell_length_a                   13.0149(3)
_cell_length_b                   10.6079(3)
_cell_length_c                   6.5455(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     903.68(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1380
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      30.5

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             768
_exptl_absorpt_coefficient_mu    4.708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.390
_exptl_absorpt_correction_T_max  0.455
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15429
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.13
_diffrn_reflns_theta_max         30.49
_reflns_number_total             1380
_reflns_number_gt                1204
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0176P)²+9.7138P] 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     SHELXL
_refine_ls_extinction_coef       0.0043(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1380
_refine_ls_number_parameters     87
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0503
_refine_ls_wR_factor_ref         0.1164
_refine_ls_wR_factor_gt          0.1143
_refine_ls_goodness_of_fit_ref   1.359
_refine_ls_restrained_S_all      1.449
_refine_ls_shift/su_max          0.000
_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
Ni1 Ni 0.62670(7) 0.2500 0.2500 0.0090(2) Uani 1 2 d S . .
Ni2 Ni 0.5000 0.0000 0.0000 0.0100(2) Uani 1 2 d S . .
S1 S 0.56859(14) 0.2500 -0.2500 0.0099(3) Uani 1 2 d S . .
S2 S 0.2500 0.0000 -0.0865(3) 0.0093(3) Uani 1 2 d S . .
F1 F 0.5192(3) 0.1207(3) 0.2253(6) 0.0185(8) Uani 1 1 d . . .
O1 O 0.6348(3) 0.2778(4) -0.0730(6) 0.0148(8) Uani 1 1 d . . .
O2 O 0.4994(3) -0.1425(4) 0.2077(6) 0.0142(8) Uani 1 1 d . . .
O3 O 0.7353(3) 0.1112(4) 0.2197(6) 0.0166(9) Uani 1 1 d . . .
O4 O 0.3403(3) 0.0207(4) 0.0441(6) 0.0137(8) Uani 1 1 d . . .
O1WA O 0.3535(8) 0.1879(9) 0.4378(18) 0.037(4) Uani 0.500(18) 1 d PD A 1
O1WB O 0.3663(8) 0.0693(10) 0.4654(17) 0.040(4) Uani 0.500(18) 1 d PD A 2
H1 H 0.4028 0.1317 0.4068 0.050 Uiso 1 1 d D . .
H2 H 0.3191 0.1180 0.4003 0.050 Uiso 1 1 d D . .
H3 H 0.3567 0.1369 0.5474 0.050 Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0085(4) 0.0085(4) 0.0100(4) -0.0008(4) 0.000 0.000
Ni2 0.0103(4) 0.0074(4) 0.0124(4) 0.0011(4) -0.0011(3) -0.0010(4)
S1 0.0104(8) 0.0090(7) 0.0104(7) 0.0009(7) 0.000 0.000
S2 0.0088(7) 0.0100(7) 0.0090(7) 0.000 0.000 0.0020(6)
F1 0.0171(16) 0.0153(16) 0.023(2) -0.0044(14) 0.0040(15) -0.0058(13)
O1 0.0165(19) 0.017(2) 0.0104(17) -0.0001(15) -0.0010(15) -0.0036(15)
O2 0.0176(19) 0.0140(18) 0.011(2) 0.0068(15) -0.0039(15) -0.0066(15)
O3 0.017(2) 0.0167(18) 0.016(2) -0.0067(16) -0.0022(16) 0.0070(16)
O4 0.0095(17) 0.0170(19) 0.0145(19) -0.0019(15) -0.0034(14) -0.0010(15)
O1WA 0.037(7) 0.031(6) 0.042(7) 0.003(5) 0.007(5) -0.008(5)
O1WB 0.036(7) 0.054(8) 0.032(7) -0.003(5) 0.009(5) -0.011(6)

_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
Ni1 F1 1.966(3) . ?
Ni1 F1 1.966(3) 4 ?
Ni1 O3 2.051(4) 4 ?
Ni1 O3 2.051(4) . ?
Ni1 O1 2.138(4) . ?
Ni1 O1 2.138(4) 4 ?
Ni2 F1 1.968(4) . ?
Ni2 F1 1.968(4) 5_655 ?
Ni2 O2 2.033(4) 5_655 ?
Ni2 O2 2.033(4) . ?
Ni2 O4 2.110(4) 5_655 ?
Ni2 O4 2.110(4) . ?
S1 O2 1.470(4) 5_655 ?
S1 O2 1.470(4) 8_665 ?
S1 O1 1.474(4) . ?
S1 O1 1.474(4) 4_554 ?
S2 O4 1.470(4) . ?
S2 O4 1.470(4) 2 ?
S2 O3 1.479(4) 5_655 ?
S2 O3 1.479(4) 6 ?
O2 S1 1.470(4) 5_655 ?
O3 S2 1.479(4) 5_655 ?

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 Ni1 F1 89.3(2) . 4 ?
F1 Ni1 O3 178.07(16) . 4 ?
F1 Ni1 O3 88.93(16) 4 4 ?
F1 Ni1 O3 88.93(16) . . ?
F1 Ni1 O3 178.07(16) 4 . ?
O3 Ni1 O3 92.9(2) 4 . ?
F1 Ni1 O1 92.88(16) . . ?
F1 Ni1 O1 91.16(17) 4 . ?
O3 Ni1 O1 87.84(16) 4 . ?
O3 Ni1 O1 88.24(17) . . ?
F1 Ni1 O1 91.16(17) . 4 ?
F1 Ni1 O1 92.88(16) 4 4 ?
O3 Ni1 O1 88.24(17) 4 4 ?
O3 Ni1 O1 87.84(16) . 4 ?
O1 Ni1 O1 174.3(2) . 4 ?
F1 Ni2 F1 180.0(2) . 5_655 ?
F1 Ni2 O2 90.99(16) . 5_655 ?
F1 Ni2 O2 89.01(16) 5_655 5_655 ?
F1 Ni2 O2 89.01(16) . . ?
F1 Ni2 O2 90.99(16) 5_655 . ?
O2 Ni2 O2 180.00(15) 5_655 . ?
F1 Ni2 O4 92.59(15) . 5_655 ?
F1 Ni2 O4 87.41(15) 5_655 5_655 ?
O2 Ni2 O4 88.98(16) 5_655 5_655 ?
O2 Ni2 O4 91.02(16) . 5_655 ?
F1 Ni2 O4 87.41(15) . . ?
F1 Ni2 O4 92.59(15) 5_655 . ?
O2 Ni2 O4 91.02(16) 5_655 . ?
O2 Ni2 O4 88.98(16) . . ?
O4 Ni2 O4 180.0(2) 5_655 . ?
O2 S1 O2 105.9(4) 5_655 8_665 ?
O2 S1 O1 111.1(2) 5_655 . ?
O2 S1 O1 110.2(2) 8_665 . ?
O2 S1 O1 110.2(2) 5_655 4_554 ?
O2 S1 O1 111.1(2) 8_665 4_554 ?
O1 S1 O1 108.4(3) . 4_554 ?
O4 S2 O4 108.9(3) . 2 ?
O4 S2 O3 111.0(2) . 5_655 ?
O4 S2 O3 109.1(2) 2 5_655 ?
O4 S2 O3 109.1(2) . 6 ?
O4 S2 O3 111.0(2) 2 6 ?
O3 S2 O3 107.7(4) 5_655 6 ?
Ni1 F1 Ni2 127.27(19) . . ?
S1 O1 Ni1 136.1(3) . . ?
S1 O2 Ni2 134.8(3) 5_655 . ?
S2 O3 Ni1 136.0(3) 5_655 . ?
S2 O4 Ni2 133.8(3) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        30.49
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.899
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.178
