# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_cubane
_database_code_depnum_ccdc_archive 'CCDC 2195963'
loop_
_audit_author_name
_audit_author_address
'Malaya Kumar Sahoo'
;National Institute of Science Education and Research, Bhubaneswar
India
;
_audit_update_record             
;
2022-08-10 deposited with the CCDC.	2023-07-14 downloaded from the CCDC.
;
_audit_creation_date             2022-08-10
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        'CobaltFluorocubane 1D MOF'
_chemical_formula_moiety         'C12 H16 Co4 F4 N8 O12 S3, 2(C2 H8 N)'
_chemical_formula_sum            'C16 H32 Co4 F4 N10 O12 S3'
_chemical_formula_weight         964.41
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C32 H56 Co10 F24 N12 O8 S12 '
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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   18.8453(8)
_cell_length_b                   8.0828(3)
_cell_length_c                   11.4284(5)
_cell_angle_alpha                90
_cell_angle_beta                 104.375(4)
_cell_angle_gamma                90
_cell_volume                     1686.30(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    15689
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.5900
_cell_measurement_theta_min      3.6480
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.210
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark pink'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             972
_exptl_crystal_preparation       'solvothermal,Magnetic properties'
_exptl_crystal_recrystallization_method NA
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.3
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0935
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17206
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.713
_diffrn_reflns_theta_min         3.465
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -63.00   7.00   0.50   15.72    --    3.67 -35.00 -44.00  140
  2  ω      1.00  71.00   0.50   15.72    --    3.67  35.00 112.00  140
  3  ω     -7.00  63.00   0.50   15.72    --   -3.98  35.00 112.00  140
  4  ω    -71.00  -1.00   0.50   15.72    --   -3.98 -35.00 -44.00  140
  5  ω    -66.00   9.00   0.50   15.72    --    3.67 -19.00-150.00  150
  6  ω    -19.00  68.00   0.50   15.72    --    3.67  77.00 -90.00  174
  7  ω    -20.00  40.00   0.50   15.72    --    3.67 -99.00-180.00  120
  8  ω     -9.00  18.00   0.50   15.72    --   -3.98 -99.00-150.00   54
  9  ω    -20.00  26.00   0.50   15.72    --   -3.98 -99.00  90.00   92
 10  ω     27.00  53.00   0.50   15.72    --   -3.98  19.00-180.00   52
 11  ω     -6.00  61.00   0.50   15.72    --   -3.98  38.00-150.00  134
 12  ω    -19.00  30.00   0.50   15.72    --   -3.98 -99.00 120.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0328086000
_diffrn_orient_matrix_UB_12      0.0328303000
_diffrn_orient_matrix_UB_13      -0.0103932000
_diffrn_orient_matrix_UB_21      0.0118743000
_diffrn_orient_matrix_UB_22      0.0221317000
_diffrn_orient_matrix_UB_23      0.0618507000
_diffrn_orient_matrix_UB_31      0.0170911000
_diffrn_orient_matrix_UB_32      -0.0783092000
_diffrn_orient_matrix_UB_33      0.0131109000
_diffrn_oxdiff_ac3_digest_frames 
;
019b5856969ae961831a891b104466ae5b000262d93
;
_diffrn_oxdiff_ac3_digest_hkl    
;
01ce2236316288af4933002790b6a73339f838
;
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                3455
_reflns_number_total             3548
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.262
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.184
_refine_ls_abs_structure_details 
;
 Flack x determined using 1493 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3548
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0620
_refine_ls_restrained_S_all      1.125
_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)+(0.0711P)²+31.2156P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1795
_refine_ls_wR_factor_ref         0.1801
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C1(H1), C2(H2A), C3(H3), C5(H5), C4(H4), C6(H6), N4(H4A)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_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
Co2 Co -0.08610(8) -0.33617(17) -0.03820(13) 0.0204(4) Uani 1 1 d . . . . .
Co1 Co -0.00566(8) -0.62233(17) -0.14024(13) 0.0215(4) Uani 1 1 d . . . . .
S2 S 0.000000 -0.9803(5) 0.000000 0.0220(8) Uani 1 2 d S T P . .
S1 S -0.15079(18) -0.4712(5) -0.3123(3) 0.0321(7) Uani 1 1 d . . . . .
F2 F 0.0013(4) -0.3618(9) -0.1197(6) 0.0211(16) Uani 1 1 d . . . . .
F1 F -0.0740(4) -0.5932(9) -0.0205(7) 0.0261(17) Uani 1 1 d . . . . .
O6 O 0.0009(6) -0.8756(11) -0.1061(9) 0.033(2) Uani 1 1 d . . . . .
O1 O -0.1011(5) -0.6123(13) -0.2718(9) 0.038(2) Uani 1 1 d . . . . .
O5 O -0.0661(5) -0.0807(10) -0.0306(9) 0.028(2) Uani 1 1 d . . . . .
O2 O -0.1539(5) -0.3614(14) -0.2108(8) 0.039(2) Uani 1 1 d . . . . .
N1 N 0.0612(7) -0.6396(16) -0.2560(10) 0.036(3) Uani 1 1 d . . . . .
N3 N -0.1686(6) -0.3059(15) 0.0458(11) 0.033(3) Uani 1 1 d . . . . .
O4 O -0.1232(11) -0.3778(16) -0.3991(13) 0.076(5) Uani 1 1 d . . . . .
O3 O -0.2236(8) -0.537(2) -0.3639(13) 0.070(4) Uani 1 1 d . . . . .
N2 N 0.1139(11) -0.576(2) -0.3996(15) 0.066(5) Uani 1 1 d . . . . .
H2 H 0.123738 -0.523245 -0.459157 0.080 Uiso 1 1 calc R . . . .
C1 C 0.1161(10) -0.751(2) -0.2549(18) 0.052(4) Uani 1 1 d . . . . .
H1 H 0.128718 -0.839262 -0.201756 0.063 Uiso 1 1 calc R . . . .
C2 C 0.1491(12) -0.711(3) -0.344(2) 0.071(7) Uani 1 1 d . . . . .
H2A H 0.188021 -0.766078 -0.363632 0.086 Uiso 1 1 calc R . . . .
C3 C 0.0614(11) -0.538(2) -0.3455(15) 0.053(4) Uani 1 1 d . . . . .
H3 H 0.028907 -0.450237 -0.368035 0.063 Uiso 1 1 calc R . . . .
C5 C -0.2272(10) -0.219(2) 0.1789(16) 0.053(4) Uani 1 1 d . . . . .
H5 H -0.236523 -0.177976 0.249796 0.063 Uiso 1 1 calc R . . A .
C4 C -0.1638(10) -0.231(3) 0.1526(17) 0.055(4) Uani 1 1 d . . . . .
H4 H -0.120145 -0.192832 0.202280 0.066 Uiso 1 1 calc R . . . .
C6 C -0.2363(11) -0.353(6) 0.014(3) 0.138(18) Uani 1 1 d . . . . .
H6 H -0.255110 -0.429738 -0.046237 0.165 Uiso 1 1 calc R . . A .
C7 C -0.1776(11) 0.020(3) -0.350(2) 0.064(5) Uani 1 1 d . . . . .
H7A H -0.201551 -0.024529 -0.427724 0.097 Uiso 1 1 calc GR . . . .
H7B H -0.176786 0.138139 -0.354216 0.097 Uiso 1 1 calc GR . . . .
H7C H -0.203621 -0.013935 -0.291642 0.097 Uiso 1 1 calc GR . . . .
N5 N -0.1031(10) -0.042(2) -0.3142(14) 0.057(4) Uani 1 1 d . . . . .
H5A H -0.081391 -0.003035 -0.241371 0.068 Uiso 1 1 calc R . . . .
H5B H -0.104092 -0.152190 -0.309019 0.068 Uiso 1 1 calc R . . . .
N4 N -0.2756(10) -0.277(5) 0.082(2) 0.156(17) Uani 1 1 d . . . A -1
H4A H -0.322507 -0.267149 0.066059 0.188 Uiso 1 1 calc R . . A -1
C8 C -0.0606(19) 0.004(4) -0.398(3) 0.104(11) Uani 1 1 d . . . . .
H8A H -0.078811 -0.053512 -0.473169 0.157 Uiso 1 1 calc GR . . . .
H8B H -0.010167 -0.025028 -0.365143 0.157 Uiso 1 1 calc GR . . . .
H8C H -0.064487 0.121069 -0.412100 0.157 Uiso 1 1 calc GR . . . .


_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
Co2 F2 2.094(7) . ?
Co2 F2 2.103(7) 2 ?
Co2 F1 2.095(8) . ?
Co2 O5 2.097(9) . ?
Co2 O2 2.078(9) . ?
Co2 N3 2.035(11) . ?
Co1 F2 2.119(7) . ?
Co1 F1 2.112(7) . ?
Co1 F1 2.077(8) 2 ?
Co1 O6 2.082(9) . ?
Co1 O1 2.039(9) . ?
Co1 N1 2.045(11) . ?
S2 O6 1.482(10) 2 ?
S2 O6 1.482(10) . ?
S2 O5 1.455(10) 2_545 ?
S2 O5 1.455(10) 1_545 ?
S1 O1 1.476(11) . ?
S1 O2 1.473(10) . ?
S1 O4 1.441(12) . ?
S1 O3 1.453(15) . ?
F2 Co2 2.103(7) 2 ?
F1 Co1 2.077(8) 2 ?
O5 S2 1.455(10) 1_565 ?
N1 C1 1.37(2) . ?
N1 C3 1.31(2) . ?
N3 C4 1.34(2) . ?
N3 C6 1.29(2) . ?
N2 C2 1.35(3) . ?
N2 C3 1.32(2) . ?
C1 C2 1.36(3) . ?
C5 C4 1.31(2) . ?
C5 N4 1.33(3) . ?
C6 N4 1.35(3) . ?
C7 N5 1.45(3) . ?
N5 C8 1.44(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
F2 Co2 F2 81.8(3) . 2 ?
F2 Co2 F1 82.3(3) . . ?
F2 Co2 O5 87.9(3) . . ?
F1 Co2 F2 77.2(3) . 2 ?
F1 Co2 O5 163.5(3) . . ?
O5 Co2 F2 88.3(3) . 2 ?
O2 Co2 F2 86.2(3) . . ?
O2 Co2 F2 164.3(3) . 2 ?
O2 Co2 F1 91.2(4) . . ?
O2 Co2 O5 101.4(4) . . ?
N3 Co2 F2 96.6(4) . 2 ?
N3 Co2 F2 177.9(4) . . ?
N3 Co2 F1 98.7(4) . . ?
N3 Co2 O5 90.7(4) . . ?
N3 Co2 O2 95.6(4) . . ?
F1 Co1 F2 81.3(3) . . ?
F1 Co1 F2 77.2(3) 2 . ?
F1 Co1 F1 80.6(3) 2 . ?
F1 Co1 O6 87.1(4) 2 . ?
O6 Co1 F2 163.2(3) . . ?
O6 Co1 F1 90.3(3) . . ?
O1 Co1 F2 93.5(4) . . ?
O1 Co1 F1 84.6(4) . . ?
O1 Co1 F1 163.5(3) . 2 ?
O1 Co1 O6 100.2(4) . . ?
O1 Co1 N1 95.6(4) . . ?
N1 Co1 F2 96.2(4) . . ?
N1 Co1 F1 177.5(4) . . ?
N1 Co1 F1 98.9(4) . 2 ?
N1 Co1 O6 92.1(5) . . ?
O6 S2 O6 110.3(7) . 2 ?
O5 S2 O6 109.4(5) 2_545 . ?
O5 S2 O6 107.8(5) 1_545 . ?
O5 S2 O6 107.8(5) 2_545 2 ?
O5 S2 O6 109.4(5) 1_545 2 ?
O5 S2 O5 112.2(7) 1_545 2_545 ?
O2 S1 O1 111.4(6) . . ?
O4 S1 O1 108.2(8) . . ?
O4 S1 O2 108.5(7) . . ?
O4 S1 O3 112.3(10) . . ?
O3 S1 O1 107.8(8) . . ?
O3 S1 O2 108.8(7) . . ?
Co2 F2 Co2 97.0(3) . 2 ?
Co2 F2 Co1 101.9(3) 2 . ?
Co2 F2 Co1 96.5(3) . . ?
Co2 F1 Co1 96.7(3) . . ?
Co1 F1 Co2 103.6(3) 2 . ?
Co1 F1 Co1 97.9(3) 2 . ?
S2 O6 Co1 134.6(6) . . ?
S1 O1 Co1 129.6(6) . . ?
S2 O5 Co2 133.9(6) 1_565 . ?
S1 O2 Co2 132.2(6) . . ?
C1 N1 Co1 128.7(11) . . ?
C3 N1 Co1 125.6(12) . . ?
C3 N1 C1 105.6(14) . . ?
C4 N3 Co2 126.5(11) . . ?
C6 N3 Co2 130.5(13) . . ?
C6 N3 C4 102.9(16) . . ?
C3 N2 C2 107.7(16) . . ?
C2 C1 N1 108.9(18) . . ?
N2 C2 C1 106.2(17) . . ?
N1 C3 N2 111.5(18) . . ?
C4 C5 N4 104.9(16) . . ?
C5 C4 N3 112.7(17) . . ?
N3 C6 N4 110(2) . . ?
C8 N5 C7 112(2) . . ?
C5 N4 C6 106.1(17) . . ?

_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 1.566
_oxdiff_exptl_absorpt_empirical_full_min 0.831
_chemical_properties_physical    Moisture-sensitive
