# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 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 1552232'
_audit_update_record             
;
2017-08-01 deposited with the CCDC.
2017-11-09 downloaded from the CCDC.
;
_audit_creation_date             2017-07-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.13(C68 H24 Co8 O40)'
_chemical_formula_sum            'C8.50 H3 Co O5'
_chemical_formula_weight         244.04
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Co C H O N'
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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           98
_space_group_name_H-M_alt        'I 41 2 2'
_space_group_name_Hall           'I 4bw 2bw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x+1/2, z+1/4'
'x, -y+1/2, -z+1/4'
'-x+1/2, -y+1/2, z+1/2'
'-y, -x, -z'
'y+1/2, x+1/2, -z+1/2'
'y+1/2, -x, z+3/4'
'-x+1/2, y, -z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1, z+3/4'
'x+1/2, -y+1, -z+3/4'
'-x+1, -y+1, z+1'
'-y+1/2, -x+1/2, -z+1/2'
'y+1, x+1, -z+1'
'y+1, -x+1/2, z+5/4'
'-x+1, y+1/2, -z+5/4'

_cell_length_a                   15.33411(15)
_cell_length_b                   15.33411(15)
_cell_length_c                   12.21062(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2871.14(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    6099
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.7070
_cell_measurement_theta_min      4.1920
_shelx_estimated_absorpt_T_max   0.797
_shelx_estimated_absorpt_T_min   0.732
_exptl_absorpt_coefficient_mu    1.190
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_unetI/netI     0.0106
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13428
_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         28.271
_diffrn_reflns_theta_min         3.407
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0710
_diffrn_detector_type            Eos
_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     -4.00  40.00   1.00   33.27    --   22.24 -38.00-150.00   44
  2  ω     46.00  72.00   1.00   33.27    --   22.24  57.00   0.00   26
  3  ω     -8.00  76.00   1.00   33.27    --   22.24  77.00  90.00   84
  4  ω      7.00  62.00   1.00   33.27    --   22.24 -99.00-150.00   55
  5  ω      7.00  64.00   1.00   33.27    --   22.24 -99.00 -30.00   57
  6  ω    -51.00  94.00   1.00   33.27    --   22.24   0.00 -90.00  145
  7  ω    -99.00 -74.00   1.00   33.27    --  -22.55 178.00   0.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0364265000
_diffrn_orient_matrix_UB_12      -0.0255127000
_diffrn_orient_matrix_UB_13      0.0160206000
_diffrn_orient_matrix_UB_21      -0.0278496000
_diffrn_orient_matrix_UB_22      -0.0362474000
_diffrn_orient_matrix_UB_23      0.0088348000
_diffrn_orient_matrix_UB_31      0.0061092000
_diffrn_orient_matrix_UB_32      -0.0132187000
_diffrn_orient_matrix_UB_33      -0.0551322000
_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         0.714
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                1771
_reflns_number_total             1801
_reflns_odcompleteness_completeness 99.62
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (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    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.822
_refine_diff_density_min         -1.409
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details 
;
 Flack x determined using 725 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.220(19)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.833
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         1801
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0468
_refine_ls_restrained_S_all      0.833
_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)+(0.1058P)²+25.0394P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1373
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O1) = Uanis(O3)
3. Others
 Fixed Sof: C6(0.25)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
Co1 Co 0.81234(4) 0.31234(4) 0.2500 0.0108(2) Uani 1 2 d S T P . .
O1 O 0.7114(3) 0.4038(3) 0.2483(4) 0.0334(8) Uani 1 1 d . . . . .
C4 C 0.5000 0.5000 0.0615(5) 0.0237(14) Uani 1 2 d S T P . .
C1 C 0.5000 0.5000 0.2897(5) 0.0233(13) Uani 1 2 d S T P . .
H1 H 0.5000 0.5000 0.3659 0.028 Uiso 1 2 calc RS T P . .
C2 C 0.5666(4) 0.4607(3) 0.2347(4) 0.0234(12) Uani 1 1 d . . . . .
C3 C 0.5676(4) 0.4628(3) 0.1185(4) 0.0246(12) Uani 1 1 d . . . . .
H3 H 0.6145 0.4387 0.0807 0.030 Uiso 1 1 calc R . . . .
C5 C 0.6384(3) 0.4116(3) 0.2933(4) 0.0196(10) Uani 1 1 d . . . . .
O2 O 0.6189(3) 0.3813(3) 0.3856(3) 0.0283(8) Uani 1 1 d . . . . .
O3 O 0.7352(4) 0.2500 0.1250 0.0334(8) Uani 1 2 d S T P . .
C6 C 0.6585(13) 0.2500 0.1250 0.048(6) Uani 0.5 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.089(4) . ?
Co1 O1 2.089(4) 6_545 ?
Co1 O2 2.044(3) 7_564 ?
Co1 O2 2.044(3) 8_655 ?
Co1 O3 2.154(3) 2_645 ?
Co1 O3 2.154(3) . ?
O1 C5 1.252(6) . ?
C4 C4 1.502(12) 5_665 ?
C4 C3 1.373(6) . ?
C4 C3 1.373(6) 12_554 ?
C1 C2 1.363(6) . ?
C1 C2 1.363(6) 12_554 ?
C2 C3 1.419(7) . ?
C2 C5 1.514(6) . ?
C5 O2 1.255(6) . ?
O2 Co1 2.044(3) 2_645 ?
O3 Co1 2.154(3) 3 ?
O3 C6 1.18(2) . ?

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
O1 Co1 O1 174.3(3) 6_545 . ?
O1 Co1 O3 83.33(16) . . ?
O1 Co1 O3 92.67(17) 6_545 . ?
O1 Co1 O3 92.67(17) . 2_645 ?
O1 Co1 O3 83.33(16) 6_545 2_645 ?
O2 Co1 O1 92.4(2) 7_564 6_545 ?
O2 Co1 O1 91.7(2) 7_564 . ?
O2 Co1 O1 92.4(2) 8_655 . ?
O2 Co1 O1 91.7(2) 8_655 6_545 ?
O2 Co1 O2 86.2(2) 8_655 7_564 ?
O2 Co1 O3 91.63(13) 8_655 2_645 ?
O2 Co1 O3 175.16(17) 7_564 2_645 ?
O2 Co1 O3 175.16(17) 8_655 . ?
O2 Co1 O3 91.63(13) 7_564 . ?
O3 Co1 O3 90.85(14) . 2_645 ?
C5 O1 Co1 136.2(4) . . ?
C3 C4 C4 120.4(3) 12_554 5_665 ?
C3 C4 C4 120.4(3) . 5_665 ?
C3 C4 C3 119.1(6) . 12_554 ?
C2 C1 C2 120.9(6) . 12_554 ?
C1 C2 C3 119.5(5) . . ?
C1 C2 C5 122.1(5) . . ?
C3 C2 C5 118.4(4) . . ?
C4 C3 C2 120.5(5) . . ?
O1 C5 C2 119.3(5) . . ?
O1 C5 O2 124.8(5) . . ?
O2 C5 C2 115.8(4) . . ?
C5 O2 Co1 133.0(3) . 2_645 ?
Co1 O3 Co1 113.4(3) 3 . ?
C6 O3 Co1 123.28(13) . 3 ?
C6 O3 Co1 123.29(13) . . ?
_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.250 0.250 -0.035 707.0 124.3 ?
2 -0.250 0.750 -0.433 707.0 124.3 ?

_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 1.106
_oxdiff_exptl_absorpt_empirical_full_min 0.954
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.250 0.250 -0.019 686 167 ' '
2 0.750 0.750 -0.018 686 167 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1552233'
_audit_update_record             
;
2017-08-01 deposited with the CCDC.
2017-11-09 downloaded from the CCDC.
;
_audit_creation_date             2017-07-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.25(C70 H24 Co4 Ni4 O40)'
_chemical_formula_sum            'C17.50 H6 Co Ni O10'
_chemical_formula_weight         493.86
_chemical_absolute_configuration ?
_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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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           98
_space_group_name_H-M_alt        'I 41 2 2'
_space_group_name_Hall           'I 4bw 2bw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'-x+1/2, y, -z+3/4'
'x, -y+1/2, -z+1/4'
'y+1/2, x+1/2, -z+1/2'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'
'-x+1, y+1/2, -z+5/4'
'x+1/2, -y+1, -z+3/4'
'y+1, x+1, -z+1'
'-y+1/2, -x+1/2, -z+1/2'

_cell_length_a                   15.2512(5)
_cell_length_b                   15.2512(5)
_cell_length_c                   12.1084(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2816.4(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1622
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.8950
_cell_measurement_theta_min      4.6520
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.791
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72020
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3197
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.494
_diffrn_reflns_theta_min         4.099
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0710
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -76.00  -38.00   1.0000   18.2050
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  -60.0000 38

#__ type_ start__ end____ width___ exp.time_
  2 omega  -73.00  -48.00   1.0000   18.2050
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  120.0000 25

#__ type_ start__ end____ width___ exp.time_
  3 omega   16.00   60.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   19.0000 -180.0000 44

#__ type_ start__ end____ width___ exp.time_
  4 omega  -13.00   74.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -57.0000  -90.0000 87

#__ type_ start__ end____ width___ exp.time_
  5 omega   65.00   93.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -63.0000  -30.0000 28

#__ type_ start__ end____ width___ exp.time_
  6 omega   41.00   68.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000  -30.0000 27

#__ type_ start__ end____ width___ exp.time_
  7 omega  112.00  138.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   50.0000  150.0000 26

#__ type_ start__ end____ width___ exp.time_
  8 omega  100.00  126.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
  9 omega   59.00   84.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -38.0000  150.0000 25

#__ type_ start__ end____ width___ exp.time_
 10 omega  150.00  176.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
 11 omega  103.00  165.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000    0.0000 62

#__ type_ start__ end____ width___ exp.time_
 12 omega  108.00  134.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -63.0000  -30.0000 26

#__ type_ start__ end____ width___ exp.time_
 13 omega   39.00   64.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000   30.0000 25

#__ type_ start__ end____ width___ exp.time_
 14 omega   49.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000   60.0000 37

#__ type_ start__ end____ width___ exp.time_
 15 omega  141.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   50.0000  150.0000 33

#__ type_ start__ end____ width___ exp.time_
 16 omega   49.00   74.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -38.0000 -120.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0169808000
_diffrn_orient_matrix_UB_12      0.0839219000
_diffrn_orient_matrix_UB_13      -0.0674682000
_diffrn_orient_matrix_UB_21      -0.0752812000
_diffrn_orient_matrix_UB_22      0.0246868000
_diffrn_orient_matrix_UB_23      0.0788468000
_diffrn_orient_matrix_UB_31      0.0651740000
_diffrn_orient_matrix_UB_32      0.0506798000
_diffrn_orient_matrix_UB_33      0.0734296000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.645
_reflns_Friedel_fraction_full    0.911
_reflns_Friedel_fraction_max     0.937
_reflns_number_gt                1152
_reflns_number_total             1222
_reflns_odcompleteness_completeness 96.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 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 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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         1.434
_refine_diff_density_min         -2.772
_refine_diff_density_rms         0.185
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         1222
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0944
_refine_ls_restrained_S_all      1.080
_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)+(0.1960P)²+20.8660P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2659
_refine_ls_wR_factor_ref         0.2698
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{Ni01, Co}
3. Uiso/Uaniso restraints and constraints
Uanis(Ni01) = Uanis(Co)
4. Others
 Fixed Sof: Ni01(0.25) Co(0.25) C6(0.375)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3)
;
_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 0.68902(9) 0.31098(9) 0.5000 0.0168(8) Uani 0.5 2 d S T P A 3
O1 O 0.6176(5) 0.3773(6) 0.3868(5) 0.0299(17) Uani 1 1 d . . . . .
O2 O 0.7118(4) 0.4041(4) 0.2501(6) 0.0273(16) Uani 1 1 d . . . . .
O3 O 0.7500 0.2399(9) 0.3750 0.046(3) Uani 1 2 d S T P . .
C1 C 0.5000 0.5000 0.2921(10) 0.026(3) Uani 1 2 d S T P . .
H1 H 0.5000 0.5000 0.3689 0.031 Uiso 1 2 calc RS T P . .
C4 C 0.5000 0.5000 0.0627(11) 0.033(3) Uani 1 2 d S T P . .
C2 C 0.5678(7) 0.4599(7) 0.2346(10) 0.033(3) Uani 1 1 d . . . . .
C3 C 0.5679(8) 0.4623(7) 0.1210(10) 0.037(3) Uani 1 1 d . . . . .
H3 H 0.6148 0.4380 0.0827 0.044 Uiso 1 1 calc R . . . .
C5 C 0.6391(7) 0.4113(7) 0.2952(9) 0.024(2) Uani 1 1 d . . . . .
Co Co 0.68902(9) 0.31098(9) 0.5000 0.0168(8) Uani 0.5 2 d S T P A 4
C6 C 0.7500 0.1541(16) 0.3750 0.052(7) Uani 0.75 2 d S T P A .


_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 O1 2.021(6) 8_666 ?
Ni01 O1 2.021(6) . ?
Ni01 O2 2.075(6) 3_645 ?
Ni01 O2 2.075(6) 5_655 ?
Ni01 O3 2.081(7) 3_645 ?
Ni01 O3 2.081(7) . ?
O1 C5 1.268(13) . ?
O2 Ni01 2.075(6) 4_564 ?
O2 C5 1.241(13) . ?
O2 Co 2.075(6) 4_564 ?
O3 Ni01 2.081(7) 4_564 ?
O3 Co 2.081(7) 4_564 ?
O3 C6 1.31(3) . ?
C1 H1 0.9300 . ?
C1 C2 1.388(13) . ?
C1 C2 1.388(13) 10_554 ?
C4 C4 1.52(3) 15_444 ?
C4 C3 1.379(14) 10_554 ?
C4 C3 1.379(14) . ?
C2 C3 1.376(18) . ?
C2 C5 1.507(14) . ?
C3 H3 0.9300 . ?

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
O1 Ni01 O1 85.5(4) 8_666 . ?
O1 Ni01 O2 92.9(4) . 5_655 ?
O1 Ni01 O2 89.8(4) . 3_645 ?
O1 Ni01 O2 89.8(4) 8_666 5_655 ?
O1 Ni01 O2 92.9(4) 8_666 3_645 ?
O1 Ni01 O3 175.7(2) . 3_645 ?
O1 Ni01 O3 90.5(3) . . ?
O1 Ni01 O3 175.7(2) 8_666 . ?
O1 Ni01 O3 90.5(3) 8_666 3_645 ?
O2 Ni01 O2 176.4(4) 5_655 3_645 ?
O2 Ni01 O3 85.8(3) 5_655 3_645 ?
O2 Ni01 O3 85.8(3) 3_645 . ?
O2 Ni01 O3 91.7(3) 5_655 . ?
O2 Ni01 O3 91.7(3) 3_645 3_645 ?
O3 Ni01 O3 93.6(4) 3_645 . ?
C5 O1 Ni01 131.2(7) . . ?
C5 O2 Ni01 135.5(7) . 4_564 ?
C5 O2 Co 135.5(7) . 4_564 ?
Ni01 O3 Ni01 117.2(6) . 4_564 ?
C6 O3 Ni01 121.4(3) . 4_564 ?
C6 O3 Ni01 121.4(3) . . ?
C6 O3 Co 121.4(3) . 4_564 ?
C2 C1 H1 120.1 10_554 . ?
C2 C1 H1 120.1 . . ?
C2 C1 C2 119.8(13) 10_554 . ?
C3 C4 C4 120.8(7) . 15_444 ?
C3 C4 C4 120.8(7) 10_554 15_444 ?
C3 C4 C3 118.3(14) 10_554 . ?
C1 C2 C5 120.7(11) . . ?
C3 C2 C1 119.4(10) . . ?
C3 C2 C5 119.9(10) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 C4 121.5(10) . . ?
C2 C3 H3 119.2 . . ?
O1 C5 C2 116.2(10) . . ?
O2 C5 O1 125.4(10) . . ?
O2 C5 C2 118.3(10) . . ?


_olex2_submission_special_instructions 'No special instructions were received'
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.250 0.250 -0.021 671 251 ' '
2 0.750 0.750 -0.020 671 251 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1552234'
_audit_update_record             
;
2017-08-01 deposited with the CCDC.
2017-11-09 downloaded from the CCDC.
;
_audit_creation_date             2017-07-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C68 H24 Ni8 O40)'
_chemical_formula_sum            'C17 H6 Ni2 O10'
_chemical_formula_weight         487.64
_chemical_absolute_configuration ?
_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'
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           98
_space_group_name_H-M_alt        'I 41 2 2'
_space_group_name_Hall           'I 4bw 2bw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x+1/2, z+1/4'
'-x, -y, z'
'y, -x+1/2, z+1/4'
'x, -y+1/2, -z+1/4'
'-x, y+1/2, -z+1/4'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1, z+3/4'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1, z+3/4'
'x+1/2, -y+1, -z+3/4'
'-x+1/2, y+1, -z+3/4'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'

_cell_length_a                   15.25380(10)
_cell_length_b                   15.25380(10)
_cell_length_c                   12.1148(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2818.85(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3140
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      51.948
_cell_measurement_theta_min      6.854
_shelx_estimated_absorpt_T_max   0.887
_shelx_estimated_absorpt_T_min   0.743
_exptl_absorpt_coefficient_mu    1.371
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3140
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.974
_diffrn_reflns_theta_min         3.427
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.694
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                1334
_reflns_number_total             1394
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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         0.366
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 
;
 Flack x determined using 527 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.081(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         1394
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0275
_refine_ls_restrained_S_all      1.167
_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)+(0.0381P)²+0.1483P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0757
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: C6(0.25)
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3)
;
_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 0.18910(2) 0.31090(2) 0.7500 0.01110(19) Uani 1 2 d S T P . .
O1 O 0.28746(15) 0.40423(15) 0.7503(2) 0.0231(5) Uani 1 1 d . . . . .
O3 O 0.2500 0.2401(3) 0.8750 0.0485(13) Uani 1 2 d S T P . .
C4 C 0.5000 0.5000 0.5614(4) 0.0263(11) Uani 1 2 d S T P . .
C5 C 0.5000 0.5000 0.7933(4) 0.0230(10) Uani 1 2 d S T P . .
H5 H 0.5000 0.5000 0.8700 0.028 Uiso 1 2 calc RS T P . .
C2 C 0.4319(2) 0.4598(2) 0.7356(3) 0.0237(10) Uani 1 1 d . . . . .
C1 C 0.3602(2) 0.4095(2) 0.7961(3) 0.0190(8) Uani 1 1 d . . . . .
C3 C 0.4312(3) 0.4628(2) 0.6204(3) 0.0281(11) Uani 1 1 d . . . . .
H3 H 0.3837 0.4394 0.5823 0.034 Uiso 1 1 calc R . . . .
O2 O 0.38233(19) 0.3780(2) 0.88707(19) 0.0272(6) Uani 1 1 d . . . . .
C6 C 0.2500 0.1576(8) 0.8750 0.041(3) Uani 0.5 2 d S T P . .


_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 O1 2.068(2) 16_556 ?
Ni1 O1 2.068(2) . ?
Ni1 O3 2.079(2) . ?
Ni1 O3 2.079(2) 10_544 ?
Ni1 O2 2.027(2) 10_544 ?
Ni1 O2 2.027(2) 14_546 ?
O1 C1 1.243(4) . ?
O3 Ni1 2.079(2) 4 ?
O3 C6 1.259(13) . ?
C4 C4 1.489(9) 7_556 ?
C4 C3 1.390(4) . ?
C4 C3 1.390(4) 3_665 ?
C5 C2 1.393(4) 3_665 ?
C5 C2 1.393(4) . ?
C2 C1 1.524(5) . ?
C2 C3 1.397(6) . ?
C1 O2 1.249(4) . ?
O2 Ni1 2.027(2) 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
O1 Ni1 O1 176.99(14) 16_556 . ?
O1 Ni1 O3 91.82(11) . . ?
O1 Ni1 O3 86.12(12) 16_556 . ?
O1 Ni1 O3 86.12(12) . 10_544 ?
O1 Ni1 O3 91.82(11) 16_556 10_544 ?
O3 Ni1 O3 93.81(13) 10_544 . ?
O2 Ni1 O1 92.35(13) 10_544 16_556 ?
O2 Ni1 O1 89.87(13) 14_546 16_556 ?
O2 Ni1 O1 92.35(13) 14_546 . ?
O2 Ni1 O1 89.87(13) 10_544 . ?
O2 Ni1 O3 175.36(8) 10_544 . ?
O2 Ni1 O3 90.62(10) 14_546 . ?
O2 Ni1 O3 90.62(10) 10_544 10_544 ?
O2 Ni1 O3 175.36(8) 14_546 10_544 ?
O2 Ni1 O2 84.99(13) 14_546 10_544 ?
C1 O1 Ni1 133.9(2) . . ?
Ni1 O3 Ni1 117.4(2) 4 . ?
C6 O3 Ni1 121.29(11) . . ?
C6 O3 Ni1 121.29(11) . 4 ?
C3 C4 C4 120.9(2) 3_665 7_556 ?
C3 C4 C4 120.9(2) . 7_556 ?
C3 C4 C3 118.2(4) 3_665 . ?
C2 C5 C2 119.8(5) . 3_665 ?
C5 C2 C1 121.0(4) . . ?
C5 C2 C3 119.5(3) . . ?
C3 C2 C1 119.4(3) . . ?
O1 C1 C2 117.3(3) . . ?
O1 C1 O2 127.6(3) . . ?
O2 C1 C2 115.1(3) . . ?
C4 C3 C2 121.4(3) . . ?
C1 O2 Ni1 130.1(2) . 4 ?


_olex2_submission_special_instructions 'No special instructions were received'
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.250 0.750 -0.020 671 39 ' '
2 0.750 0.250 -0.019 671 39 ' '
_platon_squeeze_details          
;
;
