# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1528290'
_audit_update_record             
;
2017-01-18 deposited with the CCDC.
2017-06-19 downloaded from the CCDC.
;
_audit_creation_date             2015-12-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C44 H8 F20 N4 Ni'
_chemical_formula_sum            'C44 H8 F20 N4 Ni'
_chemical_formula_weight         1031.25
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'c44 h12 f20 n4 ni'
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'

_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      tetragonal
_space_group_IT_number           122
_space_group_name_H-M_alt        'I -4 2 d'
_space_group_name_Hall           'I -4 2bw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x, -y+1/2, -z+1/4'
'-x, y+1/2, -z+1/4'
'-y, -x+1/2, z+1/4'
'y, x+1/2, z+1/4'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1, -z+3/4'
'-x+1/2, y+1, -z+3/4'
'-y+1/2, -x+1, z+3/4'
'y+1/2, x+1, z+3/4'

_cell_length_a                   15.4001(2)
_cell_length_b                   15.4001(2)
_cell_length_c                   15.3253(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3634.59(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14251
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      29.5140
_cell_measurement_theta_min      3.7170
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.885
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31387
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.257
_diffrn_reflns_theta_min         3.243
_diffrn_ambient_temperature      180.01(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega    6.00   75.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628 -132.0000   34.1141 69

#__ type_ start__ end____ width___ exp.time_
  2 omega    3.00   72.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628 -127.0000  159.9459 69

#__ type_ start__ end____ width___ exp.time_
  3 omega  -13.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628   38.0000  -90.0000 102

#__ type_ start__ end____ width___ exp.time_
  4 omega   -5.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628   38.0000 -180.0000 94

#__ type_ start__ end____ width___ exp.time_
  5 omega  -13.00   87.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628   38.0000    0.0000 100

#__ type_ start__ end____ width___ exp.time_
  6 omega  -22.00   83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628    0.0000  120.0000 105

#__ type_ start__ end____ width___ exp.time_
  7 omega   21.00   88.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       13.4628 -151.0000  -54.0000 67

#__ type_ start__ end____ width___ exp.time_
  8 omega  -17.00   27.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5566  -99.0000    0.0000 44
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0384704000
_diffrn_orient_matrix_UB_12      0.0218481000
_diffrn_orient_matrix_UB_13      -0.0129723000
_diffrn_orient_matrix_UB_21      -0.0248559000
_diffrn_orient_matrix_UB_22      0.0370866000
_diffrn_orient_matrix_UB_23      -0.0113836000
_diffrn_orient_matrix_UB_31      0.0049447000
_diffrn_orient_matrix_UB_32      0.0163889000
_diffrn_orient_matrix_UB_33      0.0429346000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.788
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.948
_reflns_number_gt                2380
_reflns_number_total             2633
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 
;
 Flack x determined using 983 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2633
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0353
_refine_ls_restrained_S_all      1.098
_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)+(0.0426P)²+4.1840P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0933
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C11(H11)
;
_atom_sites_solution_hydrogens   geom
_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 0.5000 0.5000 0.0000 0.01819(16) Uani 1 4 d S T P . .
F15 F 0.6620(2) 0.07800(17) -0.24395(18) 0.0586(7) Uani 1 1 d . . . . .
C9 C 0.5506(2) 0.29127(19) -0.0371(2) 0.0225(6) Uani 1 1 d . . . . .
C10 C 0.4637(2) 0.3130(2) -0.0271(2) 0.0235(6) Uani 1 1 d . . . . .
C3 C 0.6044(2) 0.1793(2) -0.1437(2) 0.0281(6) Uani 1 1 d . . . . .
C5 C 0.6267(3) 0.0317(2) -0.1028(3) 0.0359(8) Uani 1 1 d . . . . .
F17 F 0.6519(2) -0.04919(14) -0.12217(19) 0.0543(7) Uani 1 1 d . . . . .
C8 C 0.34801(19) 0.38321(19) 0.0162(2) 0.0237(6) Uani 1 1 d . . . . .
C6 C 0.5974(2) 0.0498(2) -0.0198(2) 0.0313(7) Uani 1 1 d . . . . .
C4 C 0.6313(3) 0.0960(2) -0.1645(2) 0.0352(8) Uani 1 1 d . . . . .
C12 C 0.3216(2) 0.2940(2) 0.0034(3) 0.0395(9) Uani 1 1 d . . . . .
H12 H 0.2663 0.2696 0.0160 0.047 Uiso 1 1 calc R . . . .
C11 C 0.3928(2) 0.2512(2) -0.0309(3) 0.0358(8) Uani 1 1 d . . . . .
H11 H 0.3948 0.1935 -0.0525 0.043 Uiso 1 1 calc R . . . .
F18 F 0.59285(17) -0.01281(15) 0.03947(15) 0.0467(6) Uani 1 1 d . . . . .
F14 F 0.60799(16) 0.24040(14) -0.20551(15) 0.0389(5) Uani 1 1 d . . . . .
N13 N 0.43447(14) 0.39354(15) -0.00188(17) 0.0200(4) Uani 1 1 d . . . . .
F16 F 0.54375(18) 0.15015(15) 0.08021(15) 0.0452(6) Uani 1 1 d . . . . .
C7 C 0.5714(2) 0.1338(2) -0.0003(2) 0.0289(6) Uani 1 1 d . . . . .
C2 C 0.57430(19) 0.20032(19) -0.0610(2) 0.0238(6) Uani 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
Ni1 N13 1.925(2) 3_665 ?
Ni1 N13 1.925(2) . ?
Ni1 N13 1.925(2) 4_655 ?
Ni1 N13 1.925(2) 2_565 ?
F15 C4 1.335(4) . ?
C9 C10 1.388(4) . ?
C9 C8 1.381(4) 4_655 ?
C9 C2 1.493(4) . ?
C10 C11 1.450(4) . ?
C10 N13 1.374(4) . ?
C3 C4 1.386(5) . ?
C3 F14 1.337(4) . ?
C3 C2 1.387(5) . ?
C5 F17 1.338(4) . ?
C5 C6 1.378(5) . ?
C5 C4 1.371(6) . ?
C8 C9 1.381(4) 2_565 ?
C8 C12 1.447(4) . ?
C8 N13 1.369(4) . ?
C6 F18 1.327(4) . ?
C6 C7 1.387(4) . ?
C12 C11 1.383(5) . ?
F16 C7 1.329(4) . ?
C7 C2 1.385(5) . ?

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
N13 Ni1 N13 90.013(3) 3_665 4_655 ?
N13 Ni1 N13 90.013(3) 3_665 2_565 ?
N13 Ni1 N13 178.28(16) 3_665 . ?
N13 Ni1 N13 90.013(2) 4_655 . ?
N13 Ni1 N13 178.29(16) 4_655 2_565 ?
N13 Ni1 N13 90.012(3) 2_565 . ?
C10 C9 C2 119.3(3) . . ?
C8 C9 C10 122.2(3) 4_655 . ?
C8 C9 C2 118.0(3) 4_655 . ?
C9 C10 C11 124.3(3) . . ?
N13 C10 C9 124.4(3) . . ?
N13 C10 C11 110.9(3) . . ?
C4 C3 C2 121.8(3) . . ?
F14 C3 C4 118.4(3) . . ?
F14 C3 C2 119.8(3) . . ?
F17 C5 C6 119.2(3) . . ?
F17 C5 C4 120.3(4) . . ?
C4 C5 C6 120.5(3) . . ?
C9 C8 C12 123.7(3) 2_565 . ?
N13 C8 C9 125.2(3) . 2_565 ?
N13 C8 C12 110.9(3) . . ?
C5 C6 C7 118.9(3) . . ?
F18 C6 C5 120.2(3) . . ?
F18 C6 C7 120.9(3) . . ?
F15 C4 C3 120.6(3) . . ?
F15 C4 C5 119.9(3) . . ?
C5 C4 C3 119.6(3) . . ?
C11 C12 C8 106.3(3) . . ?
C12 C11 C10 105.6(3) . . ?
C10 N13 Ni1 126.91(19) . . ?
C8 N13 Ni1 127.28(19) . . ?
C8 N13 C10 105.7(2) . . ?
F16 C7 C6 118.0(3) . . ?
F16 C7 C2 119.6(3) . . ?
C2 C7 C6 122.3(3) . . ?
C3 C2 C9 121.7(3) . . ?
C7 C2 C9 121.4(3) . . ?
C7 C2 C3 116.9(3) . . ?

_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_170604
_database_code_depnum_ccdc_archive 'CCDC 1554445'
_audit_update_record             
;
2017-06-06 deposited with the CCDC.
2017-06-19 downloaded from the CCDC.
;
_audit_creation_date             2017-06-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C43 H3 F20 N4 Ni O2'
_chemical_formula_sum            'C43 H3 F20 N4 Ni O2'
_chemical_formula_weight         1046.20
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ni1 F20 C20 N4 O3 Cl3 H20'
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'

_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      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   15.3093(2)
_cell_length_b                   15.3093(2)
_cell_length_c                   15.8346(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3711.23(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    18724
_cell_measurement_temperature    180.0(2)
_cell_measurement_theta_max      30.1280
_cell_measurement_theta_min      3.7100
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.673
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.16b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.872
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2052
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0088
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34090
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         3.702
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -33.00  28.00   0.50    2.00    --   -1.70 -82.00  90.00  122
  2  ω    -73.00 -10.00   0.50    2.00    --   -1.70 -19.00  60.00  126
  3  ω    -80.00 -54.00   0.50    2.00    --   -1.70 -37.00-180.00   52
  4  ω    -33.00  30.00   0.50    2.00    --   -1.70 -82.00-120.00  126
  5  ω     -3.00  28.00   0.50    2.00    --   -1.70 -77.00 -30.00   62
  6  ω     -9.00  16.00   0.50    2.00    --   -1.70 -37.00-180.00   50
  7  ω     19.00  88.00   0.50    2.00    --   -1.70  37.00  30.00  138
  8  ω    -46.00  26.00   0.50    2.00    --    1.90 -77.00 -60.00  144
  9  ω    -85.00 -54.00   0.50    2.00    --    1.90 -57.00 -90.00   62
 10  ω    -32.00   9.00   0.50    2.00    --    1.90 -57.00   0.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0174669000
_diffrn_orient_matrix_UB_12      0.0301507000
_diffrn_orient_matrix_UB_13      0.0295089000
_diffrn_orient_matrix_UB_21      -0.0419913000
_diffrn_orient_matrix_UB_22      -0.0187450000
_diffrn_orient_matrix_UB_23      -0.0053444000
_diffrn_orient_matrix_UB_31      0.0087747000
_diffrn_orient_matrix_UB_32      -0.0298071000
_diffrn_orient_matrix_UB_33      0.0332593000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2051
_reflns_number_total             2127
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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 1.171.39.16b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_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         0.601
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2127
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0366
_refine_ls_restrained_S_all      1.048
_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)+(0.0622P)²+4.8393P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1064
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{C00H, O0AA}
3. Uiso/Uaniso restraints and constraints
Uanis(C00H) = Uanis(O0AA)
4. Others
 Fixed Sof: C00H(0.75) H00H(0.75) O1(0.25) O0AA(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C00H(H00H)
;
_atom_sites_solution_hydrogens   geom
_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
Ni01 Ni 0.500000 1.250000 0.375000 0.02458(15) Uani 1 4 d S T P . .
F002 F 0.54320(10) 0.89673(9) 0.45149(8) 0.0521(4) Uani 1 1 d . . . . .
F003 F 0.65520(11) 0.69835(8) 0.25395(11) 0.0611(4) Uani 1 1 d . . . . .
F004 F 0.59677(11) 0.73351(8) 0.41183(9) 0.0552(4) Uani 1 1 d . . . . .
F005 F 0.60570(10) 0.98908(8) 0.17511(8) 0.0502(3) Uani 1 1 d . . . . .
F006 F 0.65883(14) 0.82617(10) 0.13576(9) 0.0705(5) Uani 1 1 d . . . . .
N007 N 0.43317(9) 1.14385(10) 0.37170(9) 0.0265(3) Uani 1 1 d . . . . .
C008 C 0.46243(11) 1.06238(11) 0.34921(12) 0.0304(4) Uani 1 1 d . . . . .
C009 C 0.34647(11) 1.13370(11) 0.39145(12) 0.0298(4) Uani 1 1 d . . . . .
C00A C 0.54921(11) 1.03934(11) 0.33860(11) 0.0282(3) Uani 1 1 d . . . . .
C00B C 0.57026(14) 0.88048(12) 0.37283(12) 0.0342(4) Uani 1 1 d . . . . .
C00C C 0.57250(11) 0.94791(11) 0.31453(11) 0.0289(3) Uani 1 1 d . . . . .
C00D C 0.62709(14) 0.77854(12) 0.27334(14) 0.0404(4) Uani 1 1 d . . . . .
C00E C 0.60177(13) 0.92695(12) 0.23466(12) 0.0341(4) Uani 1 1 d . . . . .
C00F C 0.59732(14) 0.79663(12) 0.35304(14) 0.0380(4) Uani 1 1 d . . . . .
C00G C 0.62913(15) 0.84375(13) 0.21318(14) 0.0425(5) Uani 1 1 d . . . . .
C00H C 0.39318(14) 1.00053(13) 0.34884(17) 0.0520(5) Uani 0.75 1 d . . . A 1
H00H H 0.395709 0.942066 0.328885 0.062 Uiso 0.75 1 calc R . . A 1
C00I C 0.32030(14) 1.04287(14) 0.38379(16) 0.0460(5) Uani 1 1 d . . . . .
O1 O 0.2654(5) 1.0021(5) 0.4001(8) 0.079(3) Uani 0.25 1 d . . . A .
O0AA O 0.39318(14) 1.00053(13) 0.34884(17) 0.0520(5) Uani 0.25 1 d . . . A 2


_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
Ni01 N007 1.9210(15) 6_574 ?
Ni01 N007 1.9210(15) 16_766 ?
Ni01 N007 1.9210(15) 11_576 ?
Ni01 N007 1.9210(15) . ?
F002 C00B 1.336(2) . ?
F003 C00D 1.337(2) . ?
F004 C00F 1.342(2) . ?
F005 C00E 1.341(2) . ?
F006 C00G 1.335(2) . ?
N007 C008 1.372(2) . ?
N007 C009 1.373(2) . ?
C008 C00A 1.385(2) . ?
C008 C00H 1.421(3) . ?
C008 O0AA 1.421(3) . ?
C009 C00A 1.386(2) 11_576 ?
C009 C00I 1.452(3) . ?
C00A C00C 1.494(2) . ?
C00B C00C 1.385(3) . ?
C00B C00F 1.385(3) . ?
C00C C00E 1.380(3) . ?
C00D C00F 1.370(3) . ?
C00D C00G 1.380(3) . ?
C00E C00G 1.383(3) . ?
C00H H00H 0.9500 . ?
C00H C00I 1.404(3) . ?
C00I O1 1.078(8) . ?
C00I O0AA 1.404(3) . ?

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
N007 Ni01 N007 90.042(3) 6_574 16_766 ?
N007 Ni01 N007 176.88(8) 6_574 . ?
N007 Ni01 N007 90.044(3) 11_576 . ?
N007 Ni01 N007 176.88(8) 16_766 11_576 ?
N007 Ni01 N007 90.042(2) 6_574 11_576 ?
N007 Ni01 N007 90.041(2) 16_766 . ?
C008 N007 Ni01 127.02(12) . . ?
C008 N007 C009 105.77(14) . . ?
C009 N007 Ni01 127.21(12) . . ?
N007 C008 C00A 125.18(16) . . ?
N007 C008 C00H 111.29(16) . . ?
N007 C008 O0AA 111.29(16) . . ?
C00A C008 C00H 123.05(16) . . ?
C00A C008 O0AA 123.05(16) . . ?
N007 C009 C00A 125.34(16) . 11_576 ?
N007 C009 C00I 110.87(16) . . ?
C00A C009 C00I 123.69(17) 11_576 . ?
C008 C00A C009 121.52(16) . 16_766 ?
C008 C00A C00C 119.91(15) . . ?
C009 C00A C00C 118.20(15) 16_766 . ?
F002 C00B C00C 119.35(17) . . ?
F002 C00B C00F 118.44(17) . . ?
C00F C00B C00C 122.19(18) . . ?
C00B C00C C00A 121.49(16) . . ?
C00E C00C C00A 121.96(16) . . ?
C00E C00C C00B 116.46(16) . . ?
F003 C00D C00F 120.29(19) . . ?
F003 C00D C00G 119.9(2) . . ?
C00F C00D C00G 119.80(17) . . ?
F005 C00E C00C 119.62(16) . . ?
F005 C00E C00G 117.82(18) . . ?
C00C C00E C00G 122.55(18) . . ?
F004 C00F C00B 120.6(2) . . ?
F004 C00F C00D 119.71(18) . . ?
C00D C00F C00B 119.69(18) . . ?
F006 C00G C00D 119.71(18) . . ?
F006 C00G C00E 120.97(19) . . ?
C00D C00G C00E 119.30(19) . . ?
C008 C00H H00H 126.8 . . ?
C00I C00H C008 106.47(17) . . ?
C00I C00H H00H 126.8 . . ?
C00H C00I C009 104.82(17) . . ?
O1 C00I C009 138.6(5) . . ?
O1 C00I C00H 116.5(5) . . ?
O1 C00I O0AA 116.5(5) . . ?
O0AA C00I C009 104.82(17) . . ?
C00I O0AA C008 106.47(17) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni01 N007 C008 C00A 11.7(3) . . . . ?
Ni01 N007 C008 C00H -176.12(15) . . . . ?
Ni01 N007 C008 O0AA -176.12(15) . . . . ?
Ni01 N007 C009 C00A 5.3(3) . . . 11_576 ?
Ni01 N007 C009 C00I -178.14(14) . . . . ?
F002 C00B C00C C00A 2.8(3) . . . . ?
F002 C00B C00C C00E 179.47(17) . . . . ?
F002 C00B C00F F004 -0.4(3) . . . . ?
F002 C00B C00F C00D -178.67(18) . . . . ?
F003 C00D C00F F004 0.2(3) . . . . ?
F003 C00D C00F C00B 178.52(19) . . . . ?
F003 C00D C00G F006 0.3(3) . . . . ?
F003 C00D C00G C00E -178.49(19) . . . . ?
F005 C00E C00G F006 0.3(3) . . . . ?
F005 C00E C00G C00D 179.11(19) . . . . ?
N007 C008 C00A C009 6.6(3) . . . 16_766 ?
N007 C008 C00A C00C 179.56(17) . . . . ?
N007 C008 C00H C00I -8.3(3) . . . . ?
N007 C008 O0AA C00I -8.3(3) . . . . ?
N007 C009 C00I C00H -6.7(3) . . . . ?
N007 C009 C00I O1 168.8(10) . . . . ?
N007 C009 C00I O0AA -6.7(3) . . . . ?
C008 N007 C009 C00A -174.79(18) . . . 11_576 ?
C008 N007 C009 C00I 1.7(2) . . . . ?
C008 C00A C00C C00B -76.3(2) . . . . ?
C008 C00A C00C C00E 107.3(2) . . . . ?
C008 C00H C00I C009 8.7(3) . . . . ?
C008 C00H C00I O1 -168.0(8) . . . . ?
C009 N007 C008 C00A -168.21(18) . . . . ?
C009 N007 C008 C00H 4.0(2) . . . . ?
C009 N007 C008 O0AA 4.0(2) . . . . ?
C009 C00A C00C C00B 96.9(2) 16_766 . . . ?
C009 C00A C00C C00E -79.6(2) 16_766 . . . ?
C009 C00I O0AA C008 8.7(3) . . . . ?
C00A C008 C00H C00I 164.1(2) . . . . ?
C00A C008 O0AA C00I 164.1(2) . . . . ?
C00A C009 C00I C00H 169.9(2) 11_576 . . . ?
C00A C009 C00I O1 -14.6(11) 11_576 . . . ?
C00A C009 C00I O0AA 169.9(2) 11_576 . . . ?
C00A C00C C00E F005 -3.3(3) . . . . ?
C00A C00C C00E C00G 175.53(19) . . . . ?
C00B C00C C00E F005 -179.94(17) . . . . ?
C00B C00C C00E C00G -1.1(3) . . . . ?
C00C C00B C00F F004 177.95(18) . . . . ?
C00C C00B C00F C00D -0.3(3) . . . . ?
C00C C00E C00G F006 -178.6(2) . . . . ?
C00C C00E C00G C00D 0.2(3) . . . . ?
C00F C00B C00C C00A -175.51(18) . . . . ?
C00F C00B C00C C00E 1.1(3) . . . . ?
C00F C00D C00G F006 179.5(2) . . . . ?
C00F C00D C00G C00E 0.6(3) . . . . ?
C00G C00D C00F F004 -178.9(2) . . . . ?
C00G C00D C00F C00B -0.6(3) . . . . ?
C00H C008 C00A C009 -164.7(2) . . . 16_766 ?
C00H C008 C00A C00C 8.2(3) . . . . ?
O1 C00I O0AA C008 -168.0(8) . . . . ?
O0AA C008 C00A C009 -164.7(2) . . . 16_766 ?
O0AA C008 C00A C00C 8.2(3) . . . . ?

_shelx_SHELXL_version_number     2016/6

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.253
_oxdiff_exptl_absorpt_empirical_full_min 0.856
####################################################################### 
# 
# 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_170604
_database_code_depnum_ccdc_archive 'CCDC 1554494'
_audit_update_record             
;
2017-06-06 deposited with the CCDC.
2017-06-19 downloaded from the CCDC.
;
_audit_creation_date             2017-06-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C43 H5 F20 N4 Ni O2'
_chemical_formula_sum            'C43 H5 F20 N4 Ni O2'
_chemical_formula_weight         1048.22
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ni1 C20 F20 O3 N4 H10 Cl3'
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'

_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           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, 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'
'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'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -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'
'-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'

_cell_length_a                   20.0377(5)
_cell_length_b                   20.0377(5)
_cell_length_c                   24.6135(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     8558.5(5)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    11621
_cell_measurement_temperature    179.9(4)
_cell_measurement_theta_max      28.8500
_cell_measurement_theta_min      4.0650
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.656
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94302
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.16b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4635
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            30789
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.478
_diffrn_reflns_theta_min         3.520
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.9(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -31.00  27.00   0.50    2.00    --   -2.00 -82.00 -30.00  116
  2  ω    -17.00  38.00   0.50    2.00    --   -2.00  37.00 150.00  110
  3  ω     54.00  81.00   0.50    2.00    --   -2.00  37.00 150.00   54
  4  ω    -19.00   7.00   0.50    2.00    --   -2.00  37.00   0.00   52
  5  ω     45.00  72.00   0.50    2.00    --   -2.00  37.00   0.00   54
  6  ω    -56.00 -29.00   0.50    2.00    --    2.20 -37.00   0.00   54
  7  ω    -15.00  55.00   0.50    2.00    --    2.20  37.00 -60.00  140
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0338485333
_diffrn_orient_matrix_UB_12      0.0304469667
_diffrn_orient_matrix_UB_13      -0.0118178333
_diffrn_orient_matrix_UB_21      -0.0193539333
_diffrn_orient_matrix_UB_22      0.0210500333
_diffrn_orient_matrix_UB_23      -0.0042212667
_diffrn_orient_matrix_UB_31      0.0122425333
_diffrn_orient_matrix_UB_32      0.0172917667
_diffrn_orient_matrix_UB_33      0.0259623667
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3677
_reflns_number_total             4340
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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 1.171.39.16b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_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         0.360
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         4340
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0634
_refine_ls_restrained_S_all      1.162
_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)+(0.0257P)²+49.0360P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1418
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Shared sites
{C1, O1A}
{C2, O2A}
3. Restrained distances
 O2-C2
 1.32 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C1) = Uanis(O1A)
Uanis(C2) = Uanis(O2A)
5. Others
 Fixed Sof: C1(0.75) O2A(0.25) O1(0.25) H1(0.25) O1A(0.25) C2(0.75) O2(0.25)
 H2(0.25)
6.a Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00U(H00U)
6.b Tetrahedral OH refined with riding coordinates:
 O2(H2)
6.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_atom_sites_solution_hydrogens   geom
_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
Ni01 Ni 0.166667 0.333333 0.333333 0.04058(18) Uani 1 2 d S T P . .
F002 F 0.07724(14) 0.51628(15) 0.43283(11) 0.0702(7) Uani 1 1 d . . . . .
F003 F 0.64460(14) 0.71591(17) 0.24617(13) 0.0994(11) Uani 1 1 d . . . . .
F004 F 0.48265(15) 0.4785(2) 0.33105(14) 0.0887(9) Uani 1 1 d . . . . .
N005 N 0.09118(16) 0.31660(16) 0.38948(12) 0.0439(6) Uani 1 1 d . . . . .
N006 N 0.23669(15) 0.43497(16) 0.36280(13) 0.0440(7) Uani 1 1 d . . . . .
F007 F 0.37721(16) 0.61263(16) 0.24110(18) 0.1069(12) Uani 1 1 d . . . . .
F008 F 0.52033(18) 0.72573(16) 0.21520(17) 0.1106(12) Uani 1 1 d . . . . .
F009 F 0.07251(19) 0.6062(2) 0.51123(17) 0.1148(13) Uani 1 1 d . . . . .
F00A F 0.62628(15) 0.5934(2) 0.30456(15) 0.1097(12) Uani 1 1 d . . . . .
C00B C 0.0981(2) 0.3654(2) 0.43157(14) 0.0448(8) Uani 1 1 d . . . . .
F00C F 0.1453(3) 0.6216(2) 0.60652(15) 0.1324(16) Uani 1 1 d . . . . .
C1 C 0.2908(2) 0.5449(2) 0.41662(19) 0.0665(11) Uani 0.75 1 d . . . A 1
F00E F 0.2346(3) 0.4596(2) 0.54204(15) 0.1290(15) Uani 1 1 d . . . . .
C00F C 0.1606(2) 0.4383(2) 0.43974(15) 0.0454(8) Uani 1 1 d . . . . .
C00G C 0.22521(19) 0.4694(2) 0.40694(16) 0.0471(8) Uani 1 1 d . . . . .
C00H C 0.0311(2) 0.3317(2) 0.46554(16) 0.0537(9) Uani 1 1 d . . . . .
H00H H 0.022814 0.354379 0.496832 0.064 Uiso 1 1 calc R . . . .
C00I C 0.1154(2) 0.5241(2) 0.47883(17) 0.0517(9) Uani 1 1 d . . . . .
O2A O 0.34193(19) 0.5536(2) 0.37833(17) 0.0631(11) Uani 0.25 1 d . . . A 1
C00K C 0.3088(2) 0.4880(2) 0.34394(17) 0.0526(9) Uani 1 1 d . . . . .
C00L C 0.0194(2) 0.2526(2) 0.39794(16) 0.0486(8) Uani 1 1 d . . . . .
C00M C 0.1565(2) 0.4859(2) 0.48492(16) 0.0510(9) Uani 1 1 d . . . . .
C00N C 0.4908(2) 0.5394(3) 0.3032(2) 0.0666(12) Uani 1 1 d . . . . .
C00O C 0.4264(2) 0.5433(2) 0.2873(2) 0.0610(11) Uani 1 1 d . . . . .
C00P C 0.1118(3) 0.5694(3) 0.5190(2) 0.0692(12) Uani 1 1 d . . . . .
C00Q C 0.5642(2) 0.5975(3) 0.2895(2) 0.0760(14) Uani 1 1 d . . . . .
C00R C 0.34703(19) 0.4796(2) 0.30103(18) 0.0533(9) Uani 1 1 d . . . . .
C00S C 0.4376(2) 0.6068(2) 0.2579(2) 0.0762(14) Uani 1 1 d . . . . .
F00T F 0.2290(4) 0.5495(3) 0.62126(15) 0.172(2) Uani 1 1 d . . . . .
C00U C -0.0176(2) 0.2621(2) 0.44479(17) 0.0570(9) Uani 1 1 d . . . . .
H00U H -0.067111 0.226080 0.458463 0.068 Uiso 1 1 calc R . . . .
C00V C 0.5736(2) 0.6596(3) 0.2603(2) 0.0757(15) Uani 1 1 d . . . . .
C00W C 0.5111(3) 0.6654(2) 0.2441(2) 0.0799(15) Uani 1 1 d . . . . .
C00X C 0.1487(4) 0.5774(3) 0.5667(2) 0.0858(17) Uani 1 1 d . . . . .
C00Y C 0.1906(4) 0.5407(3) 0.5751(2) 0.101(2) Uani 1 1 d . . . . .
C00Z C 0.1937(3) 0.4952(3) 0.5342(2) 0.0824(15) Uani 1 1 d . . . . .
O1 O 0.3078(4) 0.5852(4) 0.4613(3) 0.0320(17) Uani 0.25 1 d . . . A 1
H1 H 0.342029 0.630857 0.454853 0.048 Uiso 0.25 1 calc GR . . A 1
O1A O 0.2908(2) 0.5449(2) 0.41662(19) 0.0665(11) Uani 0.25 1 d . . . A 2
C2 C 0.34193(19) 0.5536(2) 0.37833(17) 0.0631(11) Uani 0.75 1 d D . . A 2
O2 O 0.3957(9) 0.6217(9) 0.3664(7) 0.115(6) Uani 0.25 1 d D U . A 2
H2 H 0.409498 0.622581 0.334020 0.172 Uiso 0.25 1 calc R . . A 2


_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
Ni01 N005 1.950(3) . ?
Ni01 N005 1.950(3) 16 ?
Ni01 N006 1.945(3) 16 ?
Ni01 N006 1.945(3) . ?
F002 C00I 1.331(5) . ?
F003 C00V 1.347(5) . ?
F004 C00N 1.335(6) . ?
N005 C00B 1.383(4) . ?
N005 C00L 1.382(4) . ?
N006 C00G 1.367(5) . ?
N006 C00K 1.378(5) . ?
F007 C00S 1.338(5) . ?
F008 C00W 1.332(6) . ?
F009 C00P 1.335(6) . ?
F00A C00Q 1.338(6) . ?
C00B C00F 1.383(5) . ?
C00B C00H 1.431(5) . ?
F00C C00X 1.344(5) . ?
C1 C00G 1.443(5) . ?
C1 O2A 1.338(5) . ?
C1 O1 1.304(8) . ?
F00E C00Z 1.342(6) . ?
C00F C00G 1.382(5) . ?
C00F C00M 1.494(5) . ?
C00G O1A 1.443(5) . ?
C00H H00H 0.9500 . ?
C00H C00U 1.341(5) . ?
C00I C00M 1.385(5) . ?
C00I C00P 1.368(6) . ?
O2A C00K 1.420(5) . ?
C00K C00R 1.363(5) . ?
C00K C2 1.420(5) . ?
C00L C00R 1.388(5) 16 ?
C00L C00U 1.434(5) . ?
C00M C00Z 1.387(6) . ?
C00N C00O 1.389(6) . ?
C00N C00Q 1.386(6) . ?
C00O C00R 1.498(5) . ?
C00O C00S 1.381(7) . ?
C00P C00X 1.354(8) . ?
C00Q C00V 1.366(8) . ?
C00S C00W 1.391(6) . ?
F00T C00Y 1.333(6) . ?
C00U H00U 0.9500 . ?
C00V C00W 1.374(7) . ?
C00X C00Y 1.381(9) . ?
C00Y C00Z 1.380(7) . ?
O1 H1 0.8400 . ?
O1A C2 1.338(5) . ?
C2 O2 1.280(14) . ?
O2 H2 0.8400 . ?

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
N005 Ni01 N005 180.00(13) 16 . ?
N006 Ni01 N005 90.41(12) 16 16 ?
N006 Ni01 N005 89.59(12) 16 . ?
N006 Ni01 N005 90.41(12) . . ?
N006 Ni01 N005 89.59(12) . 16 ?
N006 Ni01 N006 180.0 16 . ?
C00B N005 Ni01 127.9(2) . . ?
C00L N005 Ni01 128.6(2) . . ?
C00L N005 C00B 103.4(3) . . ?
C00G N006 Ni01 127.6(2) . . ?
C00G N006 C00K 104.8(3) . . ?
C00K N006 Ni01 127.7(2) . . ?
N005 C00B C00H 111.4(3) . . ?
C00F C00B N005 125.0(3) . . ?
C00F C00B C00H 123.6(3) . . ?
O2A C1 C00G 104.9(3) . . ?
O1 C1 C00G 127.4(5) . . ?
O1 C1 O2A 124.5(4) . . ?
C00B C00F C00M 118.2(3) . . ?
C00G C00F C00B 122.8(3) . . ?
C00G C00F C00M 119.0(3) . . ?
N006 C00G C1 111.5(3) . . ?
N006 C00G C00F 126.3(3) . . ?
N006 C00G O1A 111.5(3) . . ?
C00F C00G C1 122.2(3) . . ?
C00F C00G O1A 122.2(3) . . ?
C00B C00H H00H 126.5 . . ?
C00U C00H C00B 106.9(3) . . ?
C00U C00H H00H 126.5 . . ?
F002 C00I C00M 119.5(3) . . ?
F002 C00I C00P 118.4(4) . . ?
C00P C00I C00M 122.1(4) . . ?
C1 O2A C00K 109.0(3) . . ?
N006 C00K O2A 109.7(3) . . ?
N006 C00K C2 109.7(3) . . ?
C00R C00K N006 127.1(3) . . ?
C00R C00K O2A 123.1(3) . . ?
C00R C00K C2 123.1(3) . . ?
N005 C00L C00R 125.1(3) . 16 ?
N005 C00L C00U 111.4(3) . . ?
C00R C00L C00U 123.5(3) 16 . ?
C00I C00M C00F 120.7(3) . . ?
C00I C00M C00Z 116.7(4) . . ?
C00Z C00M C00F 122.7(4) . . ?
F004 C00N C00O 120.2(4) . . ?
F004 C00N C00Q 119.1(4) . . ?
C00Q C00N C00O 120.7(5) . . ?
C00N C00O C00R 120.5(4) . . ?
C00S C00O C00N 118.2(4) . . ?
C00S C00O C00R 121.2(4) . . ?
F009 C00P C00I 120.2(5) . . ?
F009 C00P C00X 119.8(4) . . ?
C00X C00P C00I 120.0(5) . . ?
F00A C00Q C00N 120.6(6) . . ?
F00A C00Q C00V 119.5(5) . . ?
C00V C00Q C00N 119.9(5) . . ?
C00K C00R C00L 121.9(3) . 16 ?
C00K C00R C00O 119.5(3) . . ?
C00L C00R C00O 118.6(3) 16 . ?
F007 C00S C00O 120.3(4) . . ?
F007 C00S C00W 118.2(5) . . ?
C00O C00S C00W 121.5(5) . . ?
C00H C00U C00L 106.7(4) . . ?
C00H C00U H00U 126.6 . . ?
C00L C00U H00U 126.6 . . ?
F003 C00V C00Q 120.3(5) . . ?
F003 C00V C00W 118.7(6) . . ?
C00Q C00V C00W 121.0(4) . . ?
F008 C00W C00S 120.3(5) . . ?
F008 C00W C00V 120.9(4) . . ?
C00V C00W C00S 118.8(5) . . ?
F00C C00X C00P 120.4(6) . . ?
F00C C00X C00Y 119.1(6) . . ?
C00P C00X C00Y 120.5(4) . . ?
F00T C00Y C00X 121.4(6) . . ?
F00T C00Y C00Z 119.7(6) . . ?
C00Z C00Y C00X 118.9(5) . . ?
F00E C00Z C00M 118.9(4) . . ?
F00E C00Z C00Y 119.2(5) . . ?
C00Y C00Z C00M 121.9(5) . . ?
C1 O1 H1 109.5 . . ?
C2 O1A C00G 104.9(3) . . ?
O1A C2 C00K 109.0(3) . . ?
O2 C2 C00K 127.2(8) . . ?
O2 C2 O1A 118.9(8) . . ?
C2 O2 H2 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni01 N005 C00B C00F 3.1(5) . . . . ?
Ni01 N005 C00B C00H -178.2(2) . . . . ?
Ni01 N005 C00L C00R -1.9(5) . . . 16 ?
Ni01 N005 C00L C00U 178.3(3) . . . . ?
Ni01 N006 C00G C1 179.4(3) . . . . ?
Ni01 N006 C00G C00F -0.1(5) . . . . ?
Ni01 N006 C00G O1A 179.4(3) . . . . ?
Ni01 N006 C00K O2A -177.7(3) . . . . ?
Ni01 N006 C00K C00R -1.4(6) . . . . ?
Ni01 N006 C00K C2 -177.7(3) . . . . ?
F002 C00I C00M C00F 2.1(6) . . . . ?
F002 C00I C00M C00Z -178.7(4) . . . . ?
F002 C00I C00P F009 -1.8(6) . . . . ?
F002 C00I C00P C00X 178.7(4) . . . . ?
F003 C00V C00W F008 -0.5(7) . . . . ?
F003 C00V C00W C00S 179.0(4) . . . . ?
F004 C00N C00O C00R 0.1(6) . . . . ?
F004 C00N C00O C00S -179.0(4) . . . . ?
F004 C00N C00Q F00A -1.1(7) . . . . ?
F004 C00N C00Q C00V 179.0(4) . . . . ?
N005 C00B C00F C00G -2.4(6) . . . . ?
N005 C00B C00F C00M 175.6(3) . . . . ?
N005 C00B C00H C00U -0.1(4) . . . . ?
N005 C00L C00U C00H -0.2(5) . . . . ?
N006 C00G O1A C2 -1.6(5) . . . . ?
N006 C00K C00R C00L 2.8(7) . . . 16 ?
N006 C00K C00R C00O -178.6(4) . . . . ?
N006 C00K C2 O1A -3.2(5) . . . . ?
N006 C00K C2 O2 -157.9(11) . . . . ?
F007 C00S C00W F008 0.4(8) . . . . ?
F007 C00S C00W C00V -179.0(5) . . . . ?
F009 C00P C00X F00C 0.8(8) . . . . ?
F009 C00P C00X C00Y -179.1(5) . . . . ?
F00A C00Q C00V F003 0.9(7) . . . . ?
F00A C00Q C00V C00W 179.8(4) . . . . ?
C00B N005 C00L C00R 180.0(4) . . . 16 ?
C00B N005 C00L C00U 0.2(4) . . . . ?
C00B C00F C00G N006 0.8(6) . . . . ?
C00B C00F C00G C1 -178.6(4) . . . . ?
C00B C00F C00G O1A -178.6(4) . . . . ?
C00B C00F C00M C00I -78.7(5) . . . . ?
C00B C00F C00M C00Z 102.1(5) . . . . ?
C00B C00H C00U C00L 0.2(4) . . . . ?
F00C C00X C00Y F00T -1.6(10) . . . . ?
F00C C00X C00Y C00Z 179.7(5) . . . . ?
C1 O2A C00K N006 -3.2(5) . . . . ?
C1 O2A C00K C00R -179.7(4) . . . . ?
C00F C00B C00H C00U 178.6(4) . . . . ?
C00F C00G O1A C2 177.9(4) . . . . ?
C00F C00M C00Z F00E -0.5(8) . . . . ?
C00F C00M C00Z C00Y 178.7(5) . . . . ?
C00G N006 C00K O2A 2.1(4) . . . . ?
C00G N006 C00K C00R 178.4(4) . . . . ?
C00G N006 C00K C2 2.1(4) . . . . ?
C00G C1 O2A C00K 2.8(5) . . . . ?
C00G C00F C00M C00I 99.4(4) . . . . ?
C00G C00F C00M C00Z -79.8(5) . . . . ?
C00G O1A C2 C00K 2.8(5) . . . . ?
C00G O1A C2 O2 159.9(11) . . . . ?
C00H C00B C00F C00G 179.0(3) . . . . ?
C00H C00B C00F C00M -2.9(5) . . . . ?
C00I C00M C00Z F00E -179.7(5) . . . . ?
C00I C00M C00Z C00Y -0.6(8) . . . . ?
C00I C00P C00X F00C -179.8(4) . . . . ?
C00I C00P C00X C00Y 0.4(8) . . . . ?
O2A C1 C00G N006 -1.6(5) . . . . ?
O2A C1 C00G C00F 177.9(4) . . . . ?
O2A C00K C00R C00L 178.6(4) . . . 16 ?
O2A C00K C00R C00O -2.8(6) . . . . ?
C00K N006 C00G C1 -0.4(4) . . . . ?
C00K N006 C00G C00F -179.9(4) . . . . ?
C00K N006 C00G O1A -0.4(4) . . . . ?
C00L N005 C00B C00F -178.8(3) . . . . ?
C00L N005 C00B C00H 0.0(4) . . . . ?
C00M C00F C00G N006 -177.2(3) . . . . ?
C00M C00F C00G C1 3.4(5) . . . . ?
C00M C00F C00G O1A 3.4(5) . . . . ?
C00M C00I C00P F009 179.0(4) . . . . ?
C00M C00I C00P C00X -0.5(7) . . . . ?
C00N C00O C00R C00K 100.2(5) . . . . ?
C00N C00O C00R C00L -81.2(5) . . . 16 ?
C00N C00O C00S F007 179.3(4) . . . . ?
C00N C00O C00S C00W 0.4(7) . . . . ?
C00N C00Q C00V F003 -179.2(4) . . . . ?
C00N C00Q C00V C00W -0.3(7) . . . . ?
C00O C00N C00Q F00A -179.5(4) . . . . ?
C00O C00N C00Q C00V 0.6(7) . . . . ?
C00O C00S C00W F008 179.3(5) . . . . ?
C00O C00S C00W C00V -0.1(8) . . . . ?
C00P C00I C00M C00F -178.7(4) . . . . ?
C00P C00I C00M C00Z 0.5(6) . . . . ?
C00P C00X C00Y F00T 178.2(6) . . . . ?
C00P C00X C00Y C00Z -0.4(9) . . . . ?
C00Q C00N C00O C00R 178.5(4) . . . . ?
C00Q C00N C00O C00S -0.6(7) . . . . ?
C00Q C00V C00W F008 -179.4(4) . . . . ?
C00Q C00V C00W C00S 0.1(7) . . . . ?
C00R C00K C2 O1A -179.7(4) . . . . ?
C00R C00K C2 O2 25.6(13) . . . . ?
C00R C00L C00U C00H 179.9(4) 16 . . . ?
C00R C00O C00S F007 0.2(7) . . . . ?
C00R C00O C00S C00W -178.7(4) . . . . ?
C00S C00O C00R C00K -80.7(6) . . . . ?
C00S C00O C00R C00L 97.9(5) . . . 16 ?
F00T C00Y C00Z F00E 1.0(10) . . . . ?
F00T C00Y C00Z C00M -178.1(6) . . . . ?
C00X C00Y C00Z F00E 179.7(6) . . . . ?
C00X C00Y C00Z C00M 0.5(10) . . . . ?
O1 C1 C00G N006 -161.7(6) . . . . ?
O1 C1 C00G C00F 17.8(8) . . . . ?
O1 C1 O2A C00K 163.7(6) . . . . ?
C2 C00K C00R C00L 178.6(4) . . . 16 ?
C2 C00K C00R C00O -2.8(6) . . . . ?

_shelx_SHELXL_version_number     2016/6

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.150
_oxdiff_exptl_absorpt_empirical_full_min 0.914
