# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_H25_A
_database_code_depnum_ccdc_archive 'CCDC 1913403'
loop_
_audit_author_name
_audit_author_address
'Jack Clegg'
;The University of Queensalnd
Australia
;
_audit_update_record             
;
2019-05-01 deposited with the CCDC.	2019-09-05 downloaded from the CCDC.
;
_audit_creation_date             2019-05-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '12(H2 N0.5), 6(F3 Ni1.5 O4 S1), 3(C4 H12 N2)'
_chemical_formula_sum            'C12 H60 F18 N12 Ni9 O24 S6'
_chemical_formula_weight         1819.32
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 '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'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m'
_space_group_name_Hall           '-R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   7.3042(3)
_cell_length_b                   7.3042(3)
_cell_length_c                   25.8978(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1196.58(12)
_cell_formula_units_Z            1.00008
_cell_measurement_reflns_used    571
_cell_measurement_temperature    100(10)
_cell_measurement_theta_max      32.6860
_cell_measurement_theta_min      3.5610
_shelx_estimated_absorpt_T_max   0.653
_shelx_estimated_absorpt_T_min   0.456
_exptl_absorpt_coefficient_mu    3.881
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57270
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.15 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.525
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             918
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0778
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            5492
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.271
_diffrn_reflns_theta_min         2.359
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(10)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0465008000
_diffrn_orient_matrix_UB_12      0.0187715000
_diffrn_orient_matrix_UB_13      0.0218522000
_diffrn_orient_matrix_UB_21      -0.0189115000
_diffrn_orient_matrix_UB_22      0.0710784000
_diffrn_orient_matrix_UB_23      -0.0145776000
_diffrn_orient_matrix_UB_31      -0.1004150000
_diffrn_orient_matrix_UB_32      -0.0848329000
_diffrn_orient_matrix_UB_33      -0.0073879000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                412
_reflns_number_total             412
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.0034(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     51
_refine_ls_number_reflns         412
_refine_ls_number_restraints     74
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0268
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0396P)²+3.2754P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0693
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 H1C-N1
 0.84 with sigma of 0.02
 N1-H1D
 0.84 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N3) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.001 and sigma
for terminal atoms of 0.02
Uanis(N2) = Uanis(C1) = Uanis(C2) = Uanis(N3) = Uanis(C3) = Uanis(C4)
4. Rigid body (RIGU) restrains
 N3, N2, C1, C3, C2, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N3(0.08333) H3A(0.08333) H3B(0.08333) C1(0.08333) H1A(0.08333)
 H1B(0.08333) C3(0.08333) H3C(0.08333) H3D(0.08333) N2(0.08333) H2A(0.08333)
 H2B(0.08333) C2(0.08333) H2C(0.08333) H2D(0.08333) C4(0.08333) H4A(0.08333)
 H4B(0.08333)
6.a Free rotating group:
 C3(N2,C2)
6.b Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), C1(H1A,H1B), C3(H3C,H3D), N2(H2A,H2B), C2(H2C,H2D), C4(H4A,H4B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
N1 N 0.3333 0.6667 0.60215(17) 0.0190(8) Uani 1 6 d DS T P A 1
H1C H 0.3333 0.6667 0.5698(8) 0.023 Uiso 1 6 d DRS T P B 1
H1D H 0.2684(16) 0.537(3) 0.6108(14) 0.023 Uiso 1 2 d DRS T P C 1
F1 F 0.7373(3) 0.86864(13) 0.64340(6) 0.0142(3) Uani 1 2 d S T P D 2
S1 S 0.6667 0.3333 0.57373(4) 0.0095(3) Uani 1 6 d S T P D 2
O1 O 0.77662(15) 0.5532(3) 0.59310(7) 0.0183(4) Uani 1 2 d S T P D 2
O2 O 0.6667 0.3333 0.51763(12) 0.0166(7) Uani 1 6 d S T P D 2
Ni1 Ni 0.8333 0.6667 0.6667 0.0102(2) Uani 1 4 d S T P D 2
N3 N 0.994(12) -0.045(5) 0.5530(7) 0.0106(19) Uani 0.0833 1 d . U . E -1
H3A H 1.0513 -0.0185 0.5877 0.013 Uiso 0.0833 1 calc R . . E -1
H3B H 0.8417 -0.1374 0.5545 0.013 Uiso 0.0833 1 calc R . . E -1
C1 C 0.91(2) 0.110(19) 0.4814(17) 0.0106(19) Uani 0.0833 1 d . U . E -1
H1A H 0.9086 0.2173 0.4593 0.013 Uiso 0.0833 1 calc R . . E -1
H1B H 0.7732 0.0388 0.4990 0.013 Uiso 0.0833 1 calc R . . E -1
C3 C 1.079(8) -0.118(8) 0.5249(12) 0.0106(19) Uani 0.0833 1 d . U . E -1
H3C H 1.1022 -0.2196 0.5436 0.013 Uiso 0.0833 1 calc R . . E -1
H3D H 1.2129 -0.0066 0.5119 0.013 Uiso 0.0833 1 calc R . . E -1
N2 N 0.927(4) -0.053(10) 0.4470(8) 0.0106(19) Uani 0.0833 1 d G U . E -1
H2A H 0.8174 -0.1048 0.4209 0.013 Uiso 0.0833 1 calc R . . E -1
H2B H 1.0628 0.0168 0.4295 0.013 Uiso 0.0833 1 calc R . . E -1
C2 C 1.067(10) 0.209(7) 0.5180(16) 0.0106(19) Uani 0.0833 1 d G U . E -1
H2C H 1.0502 0.3093 0.5391 0.013 Uiso 0.0833 1 calc R . . E -1
H2D H 1.2079 0.2754 0.5032 0.013 Uiso 0.0833 1 calc R . . E -1
C4 C 0.909(6) -0.234(5) 0.4773(16) 0.0106(19) Uani 0.0833 1 d . U . E -1
H4A H 0.9467 -0.3207 0.4566 0.013 Uiso 0.0833 1 calc R . . E -1
H4B H 0.7661 -0.3215 0.4904 0.013 Uiso 0.0833 1 calc R . . E -1


_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
F1 Ni1 2.0166(7) . ?
F1 Ni1 2.0166(7) 3_675 ?
S1 O1 1.4788(19) 3_665 ?
S1 O1 1.4788(19) 2_655 ?
S1 O1 1.4788(19) . ?
S1 O2 1.453(3) . ?
O1 Ni1 2.0358(18) . ?
Ni1 F1 2.0165(7) 25_666 ?
Ni1 F1 2.0166(7) 2_765 ?
Ni1 F1 2.0166(7) 26_456 ?
Ni1 O1 2.0358(19) 25_666 ?
N3 C3 1.24(7) . ?
N3 C2 1.89(4) . ?
C1 N2 1.54(5) . ?
C1 C2 1.39(9) . ?
C3 C4 1.65(5) . ?
N2 C4 1.49(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
Ni1 F1 Ni1 129.79(8) . 3_675 ?
O1 S1 O1 109.10(8) 3_665 2_655 ?
O1 S1 O1 109.10(8) 3_665 . ?
O1 S1 O1 109.10(8) . 2_655 ?
O2 S1 O1 109.84(8) . 2_655 ?
O2 S1 O1 109.84(8) . 3_665 ?
O2 S1 O1 109.84(8) . . ?
S1 O1 Ni1 130.47(12) . . ?
F1 Ni1 F1 180.0 26_456 2_765 ?
F1 Ni1 F1 88.93(10) 25_666 2_765 ?
F1 Ni1 F1 91.07(10) . 2_765 ?
F1 Ni1 F1 91.07(10) 25_666 26_456 ?
F1 Ni1 F1 180.0 25_666 . ?
F1 Ni1 F1 88.93(10) . 26_456 ?
F1 Ni1 O1 93.23(5) . 25_666 ?
F1 Ni1 O1 86.77(5) . . ?
F1 Ni1 O1 86.77(6) 2_765 . ?
F1 Ni1 O1 86.77(6) 26_456 25_666 ?
F1 Ni1 O1 93.23(6) 26_456 . ?
F1 Ni1 O1 93.23(6) 2_765 25_666 ?
F1 Ni1 O1 93.23(5) 25_666 . ?
F1 Ni1 O1 86.77(5) 25_666 25_666 ?
O1 Ni1 O1 180.00(6) 25_666 . ?
C3 N3 C2 101(2) . . ?
C2 C1 N2 115(4) . . ?
N3 C3 C4 104(5) . . ?
C4 N2 C1 112(2) . . ?
C1 C2 N3 94(3) . . ?
N2 C4 C3 103(2) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_B
_database_code_depnum_ccdc_archive 'CCDC 1913405'
loop_
_audit_author_name
_audit_author_address
'Jack Clegg'
;The University of Queensalnd
Australia
;
_audit_update_record             
;
2019-05-01 deposited with the CCDC.	2019-09-05 downloaded from the CCDC.
;
_audit_creation_date             2019-03-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.5(F4 H8 Ni6 O28 S6), C4 H12 N2'
_chemical_formula_sum            'C4 H16 F2 N2 Ni3 O14 S3'
_chemical_formula_weight         626.50
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C6 N3H12 F6 S2 O8 Ni3'
_chemical_oxdiff_usercomment     'Kagome- HFx2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 '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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   9.9382(2)
_cell_length_b                   22.0085(6)
_cell_length_c                   7.1872(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1572.02(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13569
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.3390
_cell_measurement_theta_min      2.9600
_shelx_estimated_absorpt_T_max   0.888
_shelx_estimated_absorpt_T_min   0.711
_exptl_absorpt_coefficient_mu    4.061
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.17a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.647
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            20071
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         2.982
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -13.00  42.00   0.50    2.00    --    7.96 -95.00-143.00  110
  2  ω    -87.00   7.00   0.50    2.00    --   -9.21 -35.00 -26.00  188
  3  ω     -5.00  44.00   0.50    2.00    --    7.96 -99.00  60.00   98
  4  ω    -10.00  81.00   0.50    2.00    --    7.96  57.00 -60.00  182
  5  ω      3.00  44.00   0.50    2.00    --    7.96 -99.00  90.00   82
  6  ω    -23.00   8.00   0.50    2.00    --   -9.21 -57.00  30.00   62
  7  ω    -81.00 -47.00   0.50    2.00    --   -9.21 -57.00  30.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0008064000
_diffrn_orient_matrix_UB_12      -0.0091976000
_diffrn_orient_matrix_UB_13      0.0945208000
_diffrn_orient_matrix_UB_21      0.0663484000
_diffrn_orient_matrix_UB_22      -0.0114678000
_diffrn_orient_matrix_UB_23      -0.0093646000
_diffrn_orient_matrix_UB_31      0.0262979000
_diffrn_orient_matrix_UB_32      0.0286988000
_diffrn_orient_matrix_UB_33      0.0265782000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1907
_reflns_number_total             2006
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.17a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.17a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.17a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2006
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0220
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0341P)²+0.8473P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0609
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O8(H8A,H8B)
2.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D), C2(H2A,H2B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Ni1 Ni 0.60997(3) 0.7500 0.46270(4) 0.00585(9) Uani 1 2 d S T P . .
Ni2 Ni 0.83339(2) 0.67815(2) 0.78501(3) 0.00606(8) Uani 1 1 d . . . . .
S3 S 0.42543(6) 0.7500 0.07141(8) 0.00631(12) Uani 1 2 d S T P . .
S8 S 0.59705(4) 0.60823(2) 0.55921(6) 0.00645(10) Uani 1 1 d . . . . .
F1 F 0.43218(14) 0.7500 0.5972(2) 0.0075(3) Uani 1 2 d S T P . .
F2 F 0.70714(15) 0.7500 0.71315(19) 0.0079(3) Uani 1 2 d S T P . .
O3 O 0.29766(17) 0.7500 0.1784(2) 0.0086(3) Uani 1 2 d S T P . .
O1 O 0.54163(18) 0.7500 0.1958(2) 0.0102(3) Uani 1 2 d S T P . .
O4 O 0.43411(13) 0.69426(6) -0.04324(17) 0.0091(2) Uani 1 1 d . . . . .
O6 O 0.47484(13) 0.61149(6) 0.67941(18) 0.0109(3) Uani 1 1 d . . . . .
O2 O 0.59798(13) 0.66013(6) 0.42789(18) 0.0101(3) Uani 1 1 d . . . . .
O8 O 0.73490(14) 0.66588(6) 1.03240(18) 0.0113(3) Uani 1 1 d . . . . .
H8A H 0.6528 0.6789 1.0246 0.017 Uiso 1 1 d GR . . . .
H8B H 0.7751 0.6857 1.1207 0.017 Uiso 1 1 d GR . . . .
O7 O 0.71715(13) 0.61053(6) 0.68200(18) 0.0111(3) Uani 1 1 d . . . . .
O5 O 0.59797(12) 0.55216(6) 0.45301(17) 0.0099(3) Uani 1 1 d . . . . .
N1 N 0.53379(15) 0.56087(7) 0.0583(2) 0.0110(3) Uani 1 1 d . . . . .
H1A H 0.5160 0.5842 -0.0569 0.013 Uiso 1 1 calc R . . . .
H1B H 0.5651 0.5897 0.1548 0.013 Uiso 1 1 calc R . . . .
C1 C 0.40615(17) 0.53072(9) 0.1222(3) 0.0118(3) Uani 1 1 d . . . . .
H1C H 0.3357 0.5618 0.1424 0.014 Uiso 1 1 calc R . . . .
H1D H 0.4223 0.5096 0.2419 0.014 Uiso 1 1 calc R . . . .
C2 C 0.64125(18) 0.51456(8) 0.0217(3) 0.0117(3) Uani 1 1 d . . . . .
H2A H 0.6635 0.4930 0.1387 0.014 Uiso 1 1 calc R . . . .
H2B H 0.7236 0.5351 -0.0233 0.014 Uiso 1 1 calc R . . . .


_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 2.0140(14) . ?
Ni1 F2 2.0427(14) . ?
Ni1 O3 2.1231(18) 6_656 ?
Ni1 O1 2.0352(17) . ?
Ni1 O2 1.9972(13) . ?
Ni1 O2 1.9971(13) 7_575 ?
Ni2 F1 2.0450(9) 6_657 ?
Ni2 F2 2.0837(10) . ?
Ni2 O4 2.0364(12) 6_656 ?
Ni2 O6 2.0478(12) 6_657 ?
Ni2 O8 2.0475(13) . ?
Ni2 O7 2.0241(13) . ?
S3 O3 1.4844(18) . ?
S3 O1 1.4602(18) . ?
S3 O4 1.4804(13) 7_575 ?
S3 O4 1.4803(13) . ?
S8 O6 1.4922(13) . ?
S8 O2 1.4818(13) . ?
S8 O7 1.4853(13) . ?
S8 O5 1.4512(13) . ?
F1 Ni2 2.0450(9) 6_557 ?
F1 Ni2 2.0450(9) 4_466 ?
F2 Ni2 2.0838(10) 7_575 ?
O3 Ni1 2.1231(18) 6_556 ?
O4 Ni2 2.0365(12) 6_556 ?
O6 Ni2 2.0477(12) 6_557 ?
N1 C1 1.504(2) . ?
N1 C2 1.499(2) . ?
C1 C2 1.511(3) 5_665 ?
C2 C1 1.511(3) 5_665 ?

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 F2 89.54(6) . . ?
F1 Ni1 O3 179.85(6) . 6_656 ?
F1 Ni1 O1 99.18(7) . . ?
F2 Ni1 O3 90.32(6) . 6_656 ?
O1 Ni1 F2 171.28(7) . . ?
O1 Ni1 O3 80.97(7) . 6_656 ?
O2 Ni1 F1 90.44(4) 7_575 . ?
O2 Ni1 F1 90.44(4) . . ?
O2 Ni1 F2 97.97(4) . . ?
O2 Ni1 F2 97.97(4) 7_575 . ?
O2 Ni1 O3 89.58(4) . 6_656 ?
O2 Ni1 O3 89.58(4) 7_575 6_656 ?
O2 Ni1 O1 82.07(4) 7_575 . ?
O2 Ni1 O1 82.07(4) . . ?
O2 Ni1 O2 164.05(8) 7_575 . ?
F1 Ni2 F2 78.75(4) 6_657 . ?
F1 Ni2 O6 99.94(5) 6_657 6_657 ?
F1 Ni2 O8 88.39(5) 6_657 . ?
O4 Ni2 F1 89.01(5) 6_656 6_657 ?
O4 Ni2 F2 87.27(5) 6_656 . ?
O4 Ni2 O6 83.91(5) 6_656 6_657 ?
O4 Ni2 O8 177.31(5) 6_656 . ?
O6 Ni2 F2 171.11(6) 6_657 . ?
O8 Ni2 F2 91.57(5) . . ?
O8 Ni2 O6 97.20(6) . 6_657 ?
O7 Ni2 F1 173.72(5) . 6_657 ?
O7 Ni2 F2 97.10(5) . . ?
O7 Ni2 O4 95.53(5) . 6_656 ?
O7 Ni2 O6 84.88(5) . 6_657 ?
O7 Ni2 O8 87.01(5) . . ?
O1 S3 O3 111.07(11) . . ?
O1 S3 O4 107.14(7) . . ?
O1 S3 O4 107.13(7) . 7_575 ?
O4 S3 O3 109.76(7) . . ?
O4 S3 O3 109.76(7) 7_575 . ?
O4 S3 O4 111.93(10) . 7_575 ?
O2 S8 O6 109.68(7) . . ?
O2 S8 O7 110.32(8) . . ?
O7 S8 O6 107.97(8) . . ?
O5 S8 O6 110.52(7) . . ?
O5 S8 O2 108.69(8) . . ?
O5 S8 O7 109.66(7) . . ?
Ni1 F1 Ni2 128.31(3) . 6_557 ?
Ni1 F1 Ni2 128.31(3) . 4_466 ?
Ni2 F1 Ni2 101.31(6) 6_557 4_466 ?
Ni1 F2 Ni2 120.20(4) . . ?
Ni1 F2 Ni2 120.20(4) . 7_575 ?
Ni2 F2 Ni2 98.74(6) . 7_575 ?
S3 O3 Ni1 120.28(10) . 6_556 ?
S3 O1 Ni1 147.23(12) . . ?
S3 O4 Ni2 126.21(8) . 6_556 ?
S8 O6 Ni2 131.73(8) . 6_557 ?
S8 O2 Ni1 133.16(8) . . ?
S8 O7 Ni2 134.51(8) . . ?
C2 N1 C1 110.76(14) . . ?
N1 C1 C2 110.16(15) . 5_665 ?
N1 C2 C1 110.25(14) . 5_665 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.432
_oxdiff_exptl_absorpt_empirical_full_min 0.647

####################################################################### 
# 
# 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_H25_A-new
_database_code_depnum_ccdc_archive 'CCDC 1913404'
loop_
_audit_author_name
_audit_author_address
'Jack Clegg'
;The University of Queensalnd
Australia
;
_audit_update_record             
;
2019-05-01 deposited with the CCDC.	2019-09-05 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_REFNR01_H25_A-new           
;
PROBLEM: Ratio of reflections to parameters is < 8 for a
RESPONSE: This is a re-refinement of old data
;
_vrf_THETM01_H25_A-new           
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: This is a re-refinement of old data
;
_vrf_PLAT088_H25_A-new           
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.00 Note
RESPONSE: This is a re-refinement of old data
;
# Added during the CSD deposition process: Wednesday 01 May 2019 06:52 AM
# end Validation Reply Form

_audit_creation_date             2019-05-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '6(F3 Ni1.5 O4 S1), 12(H2 N0.5), 3(C4 H12 N2)'
_chemical_formula_sum            'C12 H60 F18 N12 Ni9 O24 S6'
_chemical_formula_weight         1819.47
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 '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'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m'
_space_group_name_Hall           '-R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   7.3166(3)
_cell_length_b                   7.3166(3)
_cell_length_c                   26.1942(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1214.38(12)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    571
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      2.33
_shelx_estimated_absorpt_T_max   0.546
_shelx_estimated_absorpt_T_min   0.436
_exptl_absorpt_coefficient_mu    3.824
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.713782
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.488
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             918
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.824
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            1673
_diffrn_reflns_point_group_measured_fraction_full 0.824
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         23.258
_diffrn_reflns_theta_min         2.333
_diffrn_ambient_temperature      130.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.824
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens CCD-diffractometer'
_diffrn_measurement_method       Ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                243
_reflns_number_total             252
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       SAINT(Siemens,1996)
_computing_data_collection       SAINT(Siemens,1996)
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.0015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         252
_refine_ls_number_restraints     74
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0204
_refine_ls_restrained_S_all      0.964
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0222P)²+4.4306P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0534
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 H1C-N1
 0.84 with sigma of 0.02
 N1-H1D
 0.84 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N3) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N2) = Uanis(C1) = Uanis(C2) = Uanis(N3) = Uanis(C3) = Uanis(C4)
4. Rigid body (RIGU) restrains
 N2, N3, C2, C3, C4, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C3(0.08333) H3A(0.08333) H3B(0.08333) N2(0.08333) H2A(0.08333)
 H2B(0.08333) N3(0.08333) H3C(0.08333) H3D(0.08333) C2(0.08333) H2C(0.08333)
 H2D(0.08333) C4(0.08333) H4A(0.08333) H4B(0.08333) C1(0.08333) H1A(0.08333)
 H1B(0.08333)
6.a Free rotating group:
 C3(N2,N3,C2,C4,C1)
6.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), N2(H2A,H2B), N3(H3C,H3D), C2(H2C,H2D), C4(H4A,H4B), C1(H1A,H1B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Ni1 Ni 0.8333 0.6667 0.6667 0.0149(3) Uani 1 4 d S T P . .
S1 S 0.6667 0.3333 0.57432(5) 0.0151(4) Uani 1 6 d S T P . .
F1 F 0.7381(4) 0.86904(18) 0.64357(8) 0.0215(5) Uani 1 2 d S T P . .
O1 O 0.7758(2) 0.5516(4) 0.59356(9) 0.0282(7) Uani 1 2 d S T P . .
O2 O 0.6667 0.3333 0.51889(16) 0.0268(12) Uani 1 6 d S T P . .
N1 N 0.3333 0.6667 0.6018(3) 0.0327(15) Uani 1 6 d DS T P A 1
H1D H 0.271(2) 0.543(4) 0.6149(15) 0.039 Uiso 1 2 d DRS T P B 1
H1C H 0.3333 0.6667 0.5696(9) 0.039 Uiso 1 6 d DRS T P C 1
C3 C 1.078(6) -0.123(6) 0.5253(12) 0.013(3) Uani 0.0833 1 d . U . D -1
H3A H 1.0711 -0.2301 0.5495 0.016 Uiso 0.0833 1 calc R . . D -1
H3B H 1.2196 -0.0516 0.5095 0.016 Uiso 0.0833 1 calc R . . D -1
N2 N 0.915(4) -0.073(6) 0.4474(12) 0.013(3) Uani 0.0833 1 d G U . D -1
H2A H 0.8017 -0.1449 0.4218 0.016 Uiso 0.0833 1 calc R . . D -1
H2B H 1.0521 -0.0042 0.4292 0.016 Uiso 0.0833 1 calc R . . D -1
N3 N 1.044(5) 0.035(6) 0.5534(12) 0.013(3) Uani 0.0833 1 d G U . D -1
H3C H 1.1543 0.1045 0.5799 0.016 Uiso 0.0833 1 calc R . . D -1
H3D H 0.9049 -0.0373 0.5706 0.016 Uiso 0.0833 1 calc R . . D -1
C2 C 1.053(5) 0.197(6) 0.5166(13) 0.013(3) Uani 0.0833 1 d G U . D -1
H2C H 1.1950 0.2733 0.5009 0.016 Uiso 0.0833 1 calc R . . D -1
H2D H 1.0285 0.3001 0.5352 0.016 Uiso 0.0833 1 calc R . . D -1
C4 C 0.910(6) -0.232(6) 0.4838(13) 0.013(3) Uani 0.0833 1 d G U . D -1
H4A H 0.9356 -0.3346 0.4651 0.016 Uiso 0.0833 1 calc R . . D -1
H4B H 0.7682 -0.3103 0.4998 0.016 Uiso 0.0833 1 calc R . . D -1
C1 C 0.887(5) 0.091(7) 0.4748(13) 0.013(3) Uani 0.0833 1 d G U . D -1
H1A H 0.7440 0.0242 0.4903 0.016 Uiso 0.0833 1 calc R . . D -1
H1B H 0.8984 0.1989 0.4502 0.016 Uiso 0.0833 1 calc R . . D -1


_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 2.0190(9) 26_456 ?
Ni1 F1 2.0189(9) 25_666 ?
Ni1 F1 2.0190(9) . ?
Ni1 F1 2.0190(9) 2_765 ?
Ni1 O1 2.049(2) 25_666 ?
Ni1 O1 2.049(2) . ?
S1 O1 1.472(3) 3_665 ?
S1 O1 1.472(3) . ?
S1 O1 1.472(3) 2_655 ?
S1 O2 1.452(4) . ?
F1 Ni1 2.0190(9) 3_675 ?
C3 N3 1.4895 . ?
C3 C4 1.5337 . ?
N2 C4 1.4872 . ?
N2 C1 1.5018 . ?
N3 C2 1.5043 . ?
C2 C1 1.5286 . ?

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 89.22(13) 26_456 . ?
F1 Ni1 F1 90.78(13) . 2_765 ?
F1 Ni1 F1 180.0 26_456 2_765 ?
F1 Ni1 F1 90.78(13) 26_456 25_666 ?
F1 Ni1 F1 180.00(10) . 25_666 ?
F1 Ni1 F1 89.22(13) 25_666 2_765 ?
F1 Ni1 O1 93.11(7) 25_666 . ?
F1 Ni1 O1 93.11(8) 26_456 . ?
F1 Ni1 O1 93.10(8) 2_765 25_666 ?
F1 Ni1 O1 93.10(7) . 25_666 ?
F1 Ni1 O1 86.90(7) . . ?
F1 Ni1 O1 86.89(7) 25_666 25_666 ?
F1 Ni1 O1 86.90(7) 2_765 . ?
F1 Ni1 O1 86.89(7) 26_456 25_666 ?
O1 Ni1 O1 180.0 25_666 . ?
O1 S1 O1 108.92(11) 2_655 . ?
O1 S1 O1 108.92(11) 3_665 . ?
O1 S1 O1 108.92(11) 3_665 2_655 ?
O2 S1 O1 110.02(11) . . ?
O2 S1 O1 110.02(11) . 3_665 ?
O2 S1 O1 110.02(11) . 2_655 ?
Ni1 F1 Ni1 129.91(11) . 3_675 ?
S1 O1 Ni1 130.86(16) . . ?
N3 C3 C4 110.7 . . ?
C4 N2 C1 111.0 . . ?
C3 N3 C2 109.5 . . ?
N3 C2 C1 110.56(6) . . ?
N2 C4 C3 110.3 . . ?
N2 C1 C2 110.6 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
