# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_6_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2329613'
loop_
_audit_author_name
_audit_author_address
'Vasiliev Alexander'
;Kirensky Institute of Physics, Federal Research Center KSC SB RAS
Russia
;
_audit_update_record             
;
2024-01-30 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'B4 Co1.76 Ni4.24 O12'
_chemical_formula_sum            'B4 Co1.76 Ni4.24 O12'
_chemical_formula_weight         587.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 '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'
Ni Ni 0.3393 1.1124 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_H-M_alt        'P n n m'
_space_group_name_Hall           '-P 2 2n'

_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.
;

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

_cell_length_a                   4.4917(6)
_cell_length_b                   5.4314(8)
_cell_length_c                   8.3789(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     204.41(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2438
_cell_measurement_theta_min      3.75
_cell_measurement_theta_max      38.72

_exptl_crystal_description       shapeless
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    4.775
_exptl_crystal_F_000             282.2
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_exptl_absorpt_coefficient_mu    13.136
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.094
_exptl_absorpt_correction_T_max  0.141
_exptl_absorpt_process_details   
;
 Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker PHOTON-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3844
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.472
_diffrn_reflns_theta_max         37.996
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             584
_reflns_number_gt                525
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0387P)²+0.1986P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.271(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         584
_refine_ls_number_parameters     34
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.0838
_refine_ls_wR_factor_gt          0.0783
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_restrained_S_all      1.164
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.000000 0.500000 0.81521(4) 0.00514(14) Uani 0.66(13) 2 d S T P . .
Co1 Co 0.000000 0.500000 0.81521(4) 0.00514(14) Uani 0.34(13) 2 d S T P . .
Ni2 Ni 0.500000 0.500000 0.500000 0.00516(16) Uani 0.80(15) 4 d S T P . .
Co2 Co 0.500000 0.500000 0.500000 0.00516(16) Uani 0.20(15) 4 d S T P . .
O1 O 0.2014(2) 0.29748(19) 0.63965(14) 0.0065(3) Uani 1 1 d . . . . .
O2 O 0.7476(3) 0.1771(3) 0.500000 0.0061(3) Uani 1 2 d S T P . .
B B 1.0428(5) 0.2458(4) 0.500000 0.0062(4) Uani 1 2 d S T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.00661(19) 0.00518(19) 0.00365(19) 0.000 0.000 0.00018(6)
Co1 0.00661(19) 0.00518(19) 0.00365(19) 0.000 0.000 0.00018(6)
Ni2 0.0052(2) 0.0044(2) 0.0059(2) 0.000 0.000 -0.00032(9)
Co2 0.0052(2) 0.0044(2) 0.0059(2) 0.000 0.000 -0.00032(9)
O1 0.0071(4) 0.0076(4) 0.0048(4) -0.0008(3) 0.0004(3) 0.0001(3)
O2 0.0062(5) 0.0069(6) 0.0051(6) 0.000 0.000 -0.0006(4)
B 0.0068(7) 0.0064(8) 0.0054(8) 0.000 0.000 -0.0004(6)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.0475(11) . ?
Ni1 O1 2.0475(11) 2_565 ?
Ni1 O2 2.1352(10) 7_566 ?
Ni1 O2 2.1352(10) 3_556 ?
Ni1 O1 2.1337(11) 3_556 ?
Ni1 O1 2.1337(11) 4_456 ?
Ni2 O2 2.0767(15) . ?
Ni2 O2 2.0767(15) 5_666 ?
Ni2 O1 2.0923(11) 6_556 ?
Ni2 O1 2.0923(11) 2_665 ?
Ni2 O1 2.0923(11) 5_666 ?
Ni2 O1 2.0924(11) . ?
Ni2 B 2.475(2) 5_766 ?
Ni2 B 2.475(2) 1_455 ?
O1 B 1.3984(17) 1_455 ?
O2 B 1.378(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
O1 Ni1 O1 88.15(7) . 2_565 ?
O1 Ni1 O2 92.80(5) . 7_566 ?
O1 Ni1 O2 173.26(5) 2_565 7_566 ?
O1 Ni1 O2 173.26(5) . 3_556 ?
O1 Ni1 O2 92.80(5) 2_565 3_556 ?
O2 Ni1 O2 87.04(6) 7_566 3_556 ?
O1 Ni1 O1 104.86(3) . 3_556 ?
O1 Ni1 O1 89.90(3) 2_565 3_556 ?
O2 Ni1 O1 83.41(5) 7_566 3_556 ?
O2 Ni1 O1 81.82(5) 3_556 3_556 ?
O1 Ni1 O1 89.90(3) . 4_456 ?
O1 Ni1 O1 104.86(3) 2_565 4_456 ?
O2 Ni1 O1 81.82(5) 7_566 4_456 ?
O2 Ni1 O1 83.41(5) 3_556 4_456 ?
O1 Ni1 O1 159.58(6) 3_556 4_456 ?
O2 Ni2 O2 180.0 . 5_666 ?
O2 Ni2 O1 84.22(4) . 6_556 ?
O2 Ni2 O1 95.78(4) 5_666 6_556 ?
O2 Ni2 O1 95.78(4) . 2_665 ?
O2 Ni2 O1 84.22(4) 5_666 2_665 ?
O1 Ni2 O1 180.0 6_556 2_665 ?
O2 Ni2 O1 95.78(4) . 5_666 ?
O2 Ni2 O1 84.22(4) 5_666 5_666 ?
O1 Ni2 O1 112.00(6) 6_556 5_666 ?
O1 Ni2 O1 68.00(6) 2_665 5_666 ?
O2 Ni2 O1 84.22(4) . . ?
O2 Ni2 O1 95.78(4) 5_666 . ?
O1 Ni2 O1 68.01(6) 6_556 . ?
O1 Ni2 O1 111.99(6) 2_665 . ?
O1 Ni2 O1 180.0 5_666 . ?
O2 Ni2 B 91.54(7) . 5_766 ?
O2 Ni2 B 88.46(7) 5_666 5_766 ?
O1 Ni2 B 145.62(3) 6_556 5_766 ?
O1 Ni2 B 34.38(3) 2_665 5_766 ?
O1 Ni2 B 34.38(3) 5_666 5_766 ?
O1 Ni2 B 145.62(3) . 5_766 ?
O2 Ni2 B 88.46(7) . 1_455 ?
O2 Ni2 B 91.54(7) 5_666 1_455 ?
O1 Ni2 B 34.38(3) 6_556 1_455 ?
O1 Ni2 B 145.62(3) 2_665 1_455 ?
O1 Ni2 B 145.62(3) 5_666 1_455 ?
O1 Ni2 B 34.38(3) . 1_455 ?
B Ni2 B 180.0 5_766 1_455 ?
B O1 Ni1 118.95(11) 1_455 . ?
B O1 Ni2 87.95(10) 1_455 . ?
Ni1 O1 Ni2 113.74(5) . . ?
B O1 Ni1 108.45(11) 1_455 3_546 ?
Ni1 O1 Ni1 123.86(6) . 3_546 ?
Ni2 O1 Ni1 95.41(4) . 3_546 ?
B O2 Ni2 106.67(13) . . ?
B O2 Ni1 128.56(6) . 7_665 ?
Ni2 O2 Ni1 95.83(5) . 7_665 ?
B O2 Ni1 128.56(6) . 3_546 ?
Ni2 O2 Ni1 95.83(5) . 3_546 ?
Ni1 O2 Ni1 92.96(6) 7_665 3_546 ?
O2 B O1 123.01(9) . 1_655 ?
O2 B O1 123.01(9) . 6_656 ?
O1 B O1 113.60(18) 1_655 6_656 ?
O2 B Ni2 161.79(16) . 1_655 ?
O1 B Ni2 57.67(9) 1_655 1_655 ?
O1 B Ni2 57.67(9) 6_656 1_655 ?

_refine_diff_density_max         1.502
_refine_diff_density_min         -1.147
_refine_diff_density_rms         0.305

_shelx_res_file                  
;

TITL 6_0m_a.res in Pnnm
    6_0m_a.res
    created by SHELXL-2018/3 at 13:20:29 on 30-Jan-2024
REM Old TITL 6_0m in Pnnm

REM SHELXT solution in Pnnm
REM R1 0.156,  Rweak 0.001,  Alpha 0.054,  Orientation as input
REM Formula found by SHELXT:  O2 Co

CELL  0.71073   4.4917   5.4314   8.3789   90.000   90.000   90.000
ZERR    1.000   0.0006   0.0008   0.0012    0.000    0.000    0.000
LATT  1
SYMM -X, -Y, Z
SYMM 1/2-X, 1/2+Y, 1/2-Z
SYMM 1/2+X, 1/2-Y, 1/2-Z
SFAC B O NI Co
UNIT 2 6 2 1
TEMP 23.000
omit -2 76
acta
EADP Ni1 Co1
EXYZ Ni1 Co1
EADP Ni2 Co2
EXYZ Ni2 Co2
L.S. 10
BOND $H
LIST 6
FMAP 2
PLAN 20
WGHT    0.038700    0.198600
EXTI    0.270578
FVAR       1.01680   0.65686   0.80270
NI1   3    0.000000    0.500000    0.815215    20.50000    0.00661    0.00518 =
         0.00365    0.00000    0.00000    0.00018
CO1   4    0.000000    0.500000    0.815215   -20.50000    0.00661    0.00518 =
         0.00365    0.00000    0.00000    0.00018
NI2   3    0.500000    0.500000    0.500000    30.25000    0.00520    0.00439 =
         0.00589    0.00000    0.00000   -0.00032
CO2   4    0.500000    0.500000    0.500000   -30.25000    0.00520    0.00439 =
         0.00589    0.00000    0.00000   -0.00032
O1    2    0.201401    0.297480    0.639651    11.00000    0.00711    0.00762 =
         0.00482   -0.00076    0.00043    0.00015
O2    2    0.747564    0.177091    0.500000    10.50000    0.00616    0.00693 =
         0.00514    0.00000    0.00000   -0.00060
B     1    1.042821    0.245769    0.500000    10.50000    0.00681    0.00636 =
         0.00539    0.00000    0.00000   -0.00041
HKLF 4




REM  6_0m_a.res in Pnnm
REM wR2 = 0.0838, GooF = S = 1.164, Restrained GooF = 1.164 for all data
REM R1 = 0.0288 for 525 Fo > 4sig(Fo) and 0.0321 for all 584 data
REM 34 parameters refined using 0 restraints

END

WGHT      0.0419      0.2599

REM Highest difference peak  1.502,  deepest hole -1.147,  1-sigma level  0.305
Q1    1   0.3544  0.5029  0.5000  10.50000  0.05    1.50
Q2    1   0.3916  0.4405  0.5000  10.50000  0.05    1.43
Q3    1  -0.1604  0.5044  0.8134  11.00000  0.05    1.39
Q4    1   0.5000  0.5000  0.4301  10.50000  0.05    1.27
Q5    1  -0.1099  0.5701  0.8133  11.00000  0.05    1.24
Q6    1   0.9421  0.2228  0.5000  10.50000  0.05    0.94
Q7    1   0.3576  0.4313  0.6004  11.00000  0.05    0.89
Q8    1  -0.1551  0.4837  0.8843  11.00000  0.05    0.83
Q9    1  -0.1452  0.4476  0.7287  11.00000  0.05    0.82
Q10   1  -0.1538  0.5424  0.7310  11.00000  0.05    0.74
Q11   1   0.0000  0.5000  0.7597  10.50000  0.05    0.74
Q12   1   0.1289  0.2222  0.6259  11.00000  0.05    0.74
Q13   1   1.1260  0.2690  0.4576  11.00000  0.05    0.72
Q14   1   0.7440  0.0362  0.5511  11.00000  0.05    0.72
Q15   1   0.8665  0.2852  0.5421  11.00000  0.05    0.71
Q16   1   0.2897  0.4858  0.6939  11.00000  0.05    0.68
Q17   1   0.8535  0.0416  0.5000  10.50000  0.05    0.67
Q18   1   0.0023  0.2915  0.6633  11.00000  0.05    0.67
Q19   1  -0.1506  0.5645  0.8982  11.00000  0.05    0.65
Q20   1   1.0050  0.2749  0.4172  11.00000  0.05    0.65
;
_shelx_res_checksum              98448

_exptl_crystal_preparation       'Magnetic properties'
