# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2026

####################################################################### 
# 
# 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_fbw-154_auto
_database_code_depnum_ccdc_archive 'CCDC 2517391'
loop_
_audit_author_name
_audit_author_address
'Bowen Fan'
;FUJIAN INSTITUTE OF RESEARCH ON THE STRUCTURE
China
;
_audit_update_record             
;
2025-12-19 deposited with the CCDC.	2026-03-10 downloaded from the CCDC.
;
_audit_creation_date             2025-12-08
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7317)
;
_chemical_formula_moiety         'C12 H30 Co N30, 2(Cl O4)'
_chemical_formula_sum            'C12 H30 Cl2 Co N30 O8'
_chemical_formula_weight         852.408
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00313 0.00162 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.21560 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
Cl 0.14908 0.15974 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940
47.77840 -9.55740 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
Co 0.35001 0.97719 12.28410 7.34090 4.00340 2.34880 4.27910 0.27840 13.53590
71.16920 1.01180 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.00304 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
N 0.00612 0.00332 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.52900 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
O 0.01085 0.00610 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.25080 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'

_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -y,x-y,z
3 -x+y,-x,z
4 -x,-y,-z
5 y,-x+y,-z
6 x-y,x,-z

_symmetry_Int_Tables_number      147
_cell_length_a                   11.9655(4)
_cell_length_b                   11.9655(4)
_cell_length_c                   6.8101(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     844.40(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    2980
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      30.0880
_cell_measurement_theta_min      2.0050
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.101a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pinkish pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_description       block
_exptl_crystal_F_000             438.002
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_diffrn_reflns_av_R_equivalents  0.0133
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.9980
_diffrn_reflns_Laue_measured_fraction_max 0.8108
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3570
_diffrn_reflns_point_group_measured_fraction_full 0.9980
_diffrn_reflns_point_group_measured_fraction_max 0.8108
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         30.20
_diffrn_reflns_theta_min         2.99
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9980
_diffrn_measured_fraction_theta_max 0.8108
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -10.00  29.00   0.50    1.00    --   -9.40 -99.00 -60.00   78
  2  ω    -13.00  29.00   0.50    1.00    --   -9.40 -99.00   0.00   84
  3  ω    -22.00  40.00   0.50    1.00    --   10.10 -79.00 158.00  124
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0350102000
_diffrn_orient_matrix_UB_12      0.0158052000
_diffrn_orient_matrix_UB_13      0.0677264000
_diffrn_orient_matrix_UB_21      -0.0133015000
_diffrn_orient_matrix_UB_22      -0.0548047000
_diffrn_orient_matrix_UB_23      0.0572290000
_diffrn_orient_matrix_UB_31      0.0573018000
_diffrn_orient_matrix_UB_32      0.0378368000
_diffrn_orient_matrix_UB_33      0.0546603000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              0
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              9
_reflns_limit_l_min              -9
_reflns_number_gt                1241
_reflns_number_total             1363
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-alpha (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.6124
_refine_diff_density_min         -1.0210
_refine_diff_density_rms         0.1051
_refine_ls_d_res_high            0.7064
_refine_ls_d_res_low             6.8101
_refine_ls_goodness_of_fit_ref   1.0337
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    7
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1363
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0555
_refine_ls_restrained_S_all      1.0337
_refine_ls_shift/su_max          -0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0534P)²+2.6234P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1303
_refine_ls_wR_factor_ref         0.1335
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a X=CH2 refined with riding coordinates:
 N15(H15a,H15b)
2.b Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c)
;
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Co1 Co 1.0 0.0 0.5 0.0154(2) Uani 1.000000 6 S T P
Cl1 Cl 0.6666666666666666 0.3333333333333333 0.38111(16) 0.0216(3) Uani
1.000000 3 S T P
N14 N 0.6392(2) -0.1207(2) 0.2026(4) 0.0225(5) Uani 1.000000 1 . . .
N11 N 0.8278(2) -0.0659(2) 0.3207(3) 0.0187(5) Uani 1.000000 1 . . .
N12 N 0.7658(2) -0.1918(2) 0.2602(3) 0.0210(5) Uani 1.000000 1 . . .
N13 N 0.6537(2) -0.2260(2) 0.1905(4) 0.0247(5) Uani 1.000000 1 . . .
N15 N 0.7649(2) 0.0956(2) 0.3119(4) 0.0247(5) Uani 1.000000 1 . . .
H15a H 0.7039(2) 0.1133(2) 0.2817(4) 0.0297(6) Uiso 1.000000 1 R . .
H15b H 0.8379(2) 0.1557(2) 0.3632(4) 0.0297(6) Uiso 1.000000 1 R . .
C11 C 0.7467(3) -0.0224(3) 0.2800(4) 0.0191(5) Uani 1.000000 1 . . .
O31 O 0.5844(3) 0.2045(3) 0.3204(7) 0.0781(13) Uani 1.000000 1 . . .
C12 C 0.5261(3) -0.1199(3) 0.1275(6) 0.0397(9) Uani 1.000000 1 . . .
H12a H 0.5514(5) -0.058(2) 0.019(3) 0.0595(13) Uiso 1.000000 1 GR . .
H12b H 0.4634(12) -0.2063(8) 0.080(4) 0.0595(13) Uiso 1.000000 1 GR . .
H12c H 0.4870(17) -0.095(3) 0.2327(13) 0.0595(13) Uiso 1.000000 1 GR . .
O21 O 0.6666666666666666 0.3333333333333333 0.5826(9) 0.117(3) Uani 1.000000 3
S T P


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 N11 2.176(2) 3_765 ?
Co1 N11 2.176(2) 6_546 ?
Co1 N11 2.176(2) . ?
Co1 N11 2.176(2) 5_666 ?
Co1 N11 2.176(2) 4_756 ?
Co1 N11 2.176(2) 2_645 ?
Cl1 O31 1.413(3) . ?
Cl1 O31 1.413(3) 2_655 ?
Cl1 O31 1.413(3) 3_665 ?
Cl1 O21 1.372(6) . ?
N14 N13 1.358(3) . ?
N14 C11 1.343(4) . ?
N14 C12 1.451(4) . ?
N11 N12 1.369(3) . ?
N11 C11 1.339(3) . ?
N12 N13 1.282(3) . ?
N15 H15a 0.8800 . ?
N15 H15b 0.8800 . ?
N15 C11 1.333(4) . ?
C12 H12a 0.9800 . ?
C12 H12b 0.9800 . ?
C12 H12c 0.9800 . ?

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
N11 Co1 N11 91.58(8) . 3_765 ?
N11 Co1 N11 180.0 6_546 3_765 ?
N11 Co1 N11 88.42(8) 5_666 3_765 ?
N11 Co1 N11 180.0 5_666 2_645 ?
N11 Co1 N11 88.42(8) 4_756 2_645 ?
N11 Co1 N11 91.58(8) 6_546 4_756 ?
N11 Co1 N11 88.42(8) 4_756 3_765 ?
N11 Co1 N11 91.58(8) 2_645 3_765 ?
N11 Co1 N11 88.42(8) 6_546 2_645 ?
N11 Co1 N11 88.42(8) 6_546 . ?
N11 Co1 N11 91.58(8) 6_546 5_666 ?
N11 Co1 N11 91.58(8) 2_645 . ?
N11 Co1 N11 91.58(8) 5_666 4_756 ?
N11 Co1 N11 88.42(8) 5_666 . ?
N11 Co1 N11 180.0 4_756 . ?
O31 Cl1 O31 111.81(18) 2_655 . ?
O31 Cl1 O31 111.81(19) 3_665 . ?
O31 Cl1 O31 111.81(18) 3_665 2_655 ?
O21 Cl1 O31 107.0(2) . . ?
O21 Cl1 O31 107.0(2) . 2_655 ?
O21 Cl1 O31 107.0(2) . 3_665 ?
C11 N14 N13 109.0(2) . . ?
C12 N14 N13 122.5(3) . . ?
C12 N14 C11 128.4(3) . . ?
N12 N11 Co1 117.45(16) . 2_645 ?
C11 N11 Co1 135.58(18) . 2_645 ?
C11 N11 N12 105.5(2) . . ?
N13 N12 N11 111.5(2) . . ?
N12 N13 N14 106.3(2) . . ?
H15b N15 H15a 120.0 . . ?
C11 N15 H15a 120.0 . . ?
C11 N15 H15b 120.0 . . ?
N11 C11 N14 107.7(2) . . ?
N15 C11 N14 124.7(3) . . ?
N15 C11 N11 127.6(2) . . ?
H12a C12 N14 109.5 . . ?
H12b C12 N14 109.5 . . ?
H12b C12 H12a 109.5 . . ?
H12c C12 N14 109.5 . . ?
H12c C12 H12a 109.5 . . ?
H12c C12 H12b 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
Co1 N11 N12 N13 167.1(2) . . . . ?
Co1 N11 C11 N14 -163.6(3) . . . . ?
Co1 N11 C11 N15 15.2(3) . . . . ?
Cl1 O31 Cl1 O31 135.5 . 2_655 2_655 . ?
Cl1 O31 Cl1 O31 18.0 3_665 . . 2_655 ?
Cl1 O31 Cl1 O31 153.5 2_655 . . 3_665 ?
Cl1 O31 Cl1 O31 32.8 . 3_665 3_665 . ?
Cl1 O31 Cl1 O21 -87.8 2_655 . . . ?
Cl1 O31 Cl1 O21 -99.8 3_665 . . . ?
N14 N13 N12 N11 0.4(2) . . . . ?
N14 C11 N11 N12 1.5(2) . . . . ?
N11 C11 N14 N13 -1.3(2) . . . . ?
N11 C11 N14 C12 -177.1(3) . . . . ?
N12 N11 C11 N15 -179.7(2) . . . . ?
N12 N13 N14 C11 0.6(2) . . . . ?
N12 N13 N14 C12 176.6(3) . . . . ?
N13 N14 C11 N15 179.9(2) . . . . ?
N13 N12 N11 C11 -1.2(3) . . . . ?
N15 C11 N14 C12 4.1(4) . . . . ?
O31 Cl1 O31 Cl1 0(700000000000000) . . 2_655 2_655 ?
O31 Cl1 O31 Cl1 0(600000000000000) . . 3_665 3_665 ?
O21 Cl1 O31 Cl1 0(700000000000000) . . 2_655 2_655 ?
O21 Cl1 O31 Cl1 0(600000000000000) . . 3_665 3_665 ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.389
_oxdiff_exptl_absorpt_empirical_full_min 0.826
####################################################################### 
# 
# 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_fbw-146_auto
_database_code_depnum_ccdc_archive 'CCDC 2517392'
loop_
_audit_author_name
_audit_author_address
'Bowen Fan'
;FUJIAN INSTITUTE OF RESEARCH ON THE STRUCTURE
China
;
_audit_update_record             
;
2025-12-19 deposited with the CCDC.	2026-03-10 downloaded from the CCDC.
;
_audit_creation_date             2025-12-08
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7317)
;
_chemical_formula_moiety         'C8 H24 Co N20 O2, 2(Cl O4)'
_chemical_formula_sum            'C8 H24 Cl2 Co N20 O10'
_chemical_formula_weight         690.247
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00313 0.00162 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.21560 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
Cl 0.14908 0.15974 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940
47.77840 -9.55740 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
Co 0.35001 0.97719 12.28410 7.34090 4.00340 2.34880 4.27910 0.27840 13.53590
71.16920 1.01180 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.00304 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
N 0.00612 0.00332 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.52900 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
O 0.01085 0.00610 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.25080 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z+1/2
3 -x,-y,-z
4 x,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   8.4564(3)
_cell_length_b                   10.8285(3)
_cell_length_c                   13.8488(5)
_cell_angle_alpha                90
_cell_angle_beta                 100.029(3)
_cell_angle_gamma                90
_cell_volume                     1248.75(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7359
_cell_measurement_temperature    99.97(10)
_cell_measurement_theta_max      30.3540
_cell_measurement_theta_min      2.3880
_exptl_absorpt_coefficient_mu    0.991
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.101a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.836
_exptl_crystal_description       block
_exptl_crystal_F_000             707.892
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.9991
_diffrn_reflns_Laue_measured_fraction_max 0.8017
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11040
_diffrn_reflns_point_group_measured_fraction_full 0.9991
_diffrn_reflns_point_group_measured_fraction_max 0.8017
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         2.40
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.8017
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     10.00  90.00   0.50    0.05    --   10.10   5.00 -18.00  160
  2  ω    -16.00  26.00   0.50    0.05    --   -9.40 -99.00 -90.00   84
  3  ω     16.00  44.00   0.50    0.05    --   10.10 -99.00 -60.00   56
  4  ω     38.00  63.00   0.50    0.05    --   10.10-126.00  35.21   50
  5  ω    -17.00  31.00   0.50    0.05    --   10.10 -99.00 150.00   96
  6  ω    -69.00  15.00   0.50    0.05    --   10.10  -5.00 165.00  168
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0525336000
_diffrn_orient_matrix_UB_12      0.0010994000
_diffrn_orient_matrix_UB_13      0.0347077000
_diffrn_orient_matrix_UB_21      0.0669705000
_diffrn_orient_matrix_UB_22      0.0041083000
_diffrn_orient_matrix_UB_23      0.0386267000
_diffrn_orient_matrix_UB_31      -0.0033385000
_diffrn_orient_matrix_UB_32      0.0653617000
_diffrn_orient_matrix_UB_33      -0.0030279000
_diffrn_oxdiff_digest_hkl        
;
017eb1b6b24f418beeac7735a656695415b7ba
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                2749
_reflns_number_total             3060
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-alpha (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.4721
_refine_diff_density_min         -0.4691
_refine_diff_density_rms         0.0784
_refine_ls_d_res_high            0.6995
_refine_ls_d_res_low             8.4802
_refine_ls_extinction_coef       0.0037(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0581
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    16
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3060
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0299
_refine_ls_restrained_S_all      1.0576
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0324P)²+1.0492P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0770
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O31-H31a = O31-H31b
 0.87 with sigma of 0.02
 H31a-H31b
 1.38 with sigma of 0.04
3.a Rotating group:
 N25(H25a,H25b)
3.b X=CH2 refined with riding coordinates:
 N15(H15a,H15b)
3.c Idealised Me refined as rotating group:
 C22(H22a,H22b,H22c), C12(H12a,H12b,H12c)
;
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Co1 Co 0.5 0.5 0.5 0.00929(10) Uani 1.000000 2 S T P
Cl1 Cl 0.19837(5) 0.88534(3) 0.61602(3) 0.01383(11) Uani 1.000000 1 . . .
O31 O 0.51926(14) 0.67505(10) 0.57527(9) 0.0127(2) Uani 1.000000 1 D . .
H31a H 0.584(2) 0.6829(19) 0.6292(13) 0.0190(4) Uiso 1.000000 1 DR . .
H31b H 0.4278(19) 0.6973(19) 0.5895(16) 0.0190(4) Uiso 1.000000 1 DR . .
O71 O 0.24105(15) 0.75831(11) 0.64472(10) 0.0211(3) Uani 1.000000 1 . . .
O61 O 0.02964(16) 0.89029(13) 0.57948(12) 0.0287(3) Uani 1.000000 1 . . .
O41 O 0.28734(17) 0.92231(12) 0.54125(10) 0.0242(3) Uani 1.000000 1 . . .
N24 N 0.65020(17) 0.69934(12) 0.25841(11) 0.0131(3) Uani 1.000000 1 . . .
O51 O 0.23993(19) 0.96564(13) 0.69906(11) 0.0288(3) Uani 1.000000 1 . . .
N23 N 0.64088(16) 0.57864(12) 0.23536(10) 0.0121(3) Uani 1.000000 1 . . .
N11 N 0.26595(16) 0.55160(12) 0.43364(10) 0.0126(3) Uani 1.000000 1 . . .
N21 N 0.58923(16) 0.58076(12) 0.37846(10) 0.0123(3) Uani 1.000000 1 . . .
N13 N 0.09350(17) 0.67805(13) 0.36616(11) 0.0151(3) Uani 1.000000 1 . . .
N12 N 0.24331(16) 0.66978(13) 0.40665(11) 0.0145(3) Uani 1.000000 1 . . .
N14 N 0.00978(17) 0.57237(14) 0.36326(11) 0.0165(3) Uani 1.000000 1 . . .
N22 N 0.60496(17) 0.50687(12) 0.30325(11) 0.0129(3) Uani 1.000000 1 . . .
N15 N 0.09970(18) 0.37135(14) 0.41676(12) 0.0193(3) Uani 1.000000 1 . . .
H15a H 0.00531(18) 0.33824(14) 0.39463(12) 0.0232(4) Uiso 1.000000 1 R . .
H15b H 0.17921(18) 0.32474(14) 0.44580(12) 0.0232(4) Uiso 1.000000 1 R . .
N25 N 0.62771(19) 0.79643(13) 0.40952(12) 0.0194(3) Uani 1.000000 1 . . .
H25a H 0.6159(19) 0.86535(14) 0.37448(13) 0.0233(4) Uiso 1.000000 1 GR . .
H25b H 0.5502(12) 0.7922(8) 0.4451(8) 0.0233(4) Uiso 1.000000 1 GR . .
C21 C 0.61859(19) 0.69726(15) 0.34934(13) 0.0126(3) Uani 1.000000 1 . . .
C22 C 0.6716(2) 0.53203(16) 0.14174(13) 0.0172(3) Uani 1.000000 1 . . .
H22a H 0.5897(9) 0.5639(10) 0.08870(16) 0.0258(5) Uiso 1.000000 1 GR . .
H22b H 0.7780(7) 0.5593(10) 0.1316(5) 0.0258(5) Uiso 1.000000 1 GR . .
H22c H 0.6676(16) 0.44158(17) 0.1419(4) 0.0258(5) Uiso 1.000000 1 GR . .
C11 C 0.1226(2) 0.49418(15) 0.40614(13) 0.0138(3) Uani 1.000000 1 . . .
C12 C 0.0215(2) 0.79552(17) 0.32937(15) 0.0221(4) Uani 1.000000 1 . . .
H12a H -0.0068(16) 0.8433(6) 0.3840(2) 0.0331(6) Uiso 1.000000 1 GR . .
H12b H 0.0986(7) 0.8423(6) 0.2986(10) 0.0331(6) Uiso 1.000000 1 GR . .
H12c H -0.0754(10) 0.77962(17) 0.2809(8) 0.0331(6) Uiso 1.000000 1 GR . .


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 O31 2.1557(11) 3_666 ?
Co1 O31 2.1557(11) . ?
Co1 N11 2.1072(13) . ?
Co1 N11 2.1072(13) 3_666 ?
Co1 N21 2.1470(14) . ?
Co1 N21 2.1470(14) 3_666 ?
Cl1 O71 1.4596(12) . ?
Cl1 O61 1.4294(14) . ?
Cl1 O41 1.4386(13) . ?
Cl1 O51 1.4358(14) . ?
O31 H31a 0.850(15) . ?
O31 H31b 0.865(15) . ?
N24 N23 1.3445(19) . ?
N24 C21 1.332(2) . ?
N23 N22 1.296(2) . ?
N23 C22 1.456(2) . ?
N11 N12 1.338(2) . ?
N11 C11 1.356(2) . ?
N21 N22 1.338(2) . ?
N21 C21 1.360(2) . ?
N13 N12 1.2961(19) . ?
N13 N14 1.343(2) . ?
N13 C12 1.463(2) . ?
N14 C11 1.335(2) . ?
N15 H15a 0.8800 . ?
N15 H15b 0.8800 . ?
N15 C11 1.356(2) . ?
N25 H25a 0.8863 . ?
N25 H25b 0.8864 . ?
N25 C21 1.353(2) . ?
C22 H22a 0.9800 . ?
C22 H22b 0.9800 . ?
C22 H22c 0.9800 . ?
C12 H12a 0.9800 . ?
C12 H12b 0.9800 . ?
C12 H12c 0.9800 . ?

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
O31 Co1 O31 180.0 3_666 . ?
N11 Co1 O31 92.07(5) 3_666 . ?
N11 Co1 O31 87.93(5) . . ?
N11 Co1 O31 92.07(5) . 3_666 ?
N11 Co1 O31 87.93(5) 3_666 3_666 ?
N11 Co1 N11 180.0 3_666 . ?
N21 Co1 O31 90.78(5) . . ?
N21 Co1 O31 89.22(5) . 3_666 ?
N21 Co1 O31 89.22(5) 3_666 . ?
N21 Co1 O31 90.78(5) 3_666 3_666 ?
N21 Co1 N11 88.95(5) . . ?
N21 Co1 N11 91.05(5) 3_666 . ?
N21 Co1 N11 88.95(5) 3_666 3_666 ?
N21 Co1 N11 91.05(5) . 3_666 ?
N21 Co1 N21 180.0 3_666 . ?
O61 Cl1 O71 108.42(8) . . ?
O41 Cl1 O71 108.83(8) . . ?
O41 Cl1 O61 110.47(9) . . ?
O51 Cl1 O71 109.77(9) . . ?
O51 Cl1 O61 110.54(9) . . ?
O51 Cl1 O41 108.79(9) . . ?
H31a O31 Co1 119.8(14) . . ?
H31b O31 Co1 111.1(14) . . ?
H31b O31 H31a 103.7(19) . . ?
C21 N24 N23 101.23(13) . . ?
N22 N23 N24 114.98(14) . . ?
C22 N23 N24 122.42(14) . . ?
C22 N23 N22 122.60(14) . . ?
N12 N11 Co1 116.96(10) . . ?
C11 N11 Co1 136.59(11) . . ?
C11 N11 N12 106.42(13) . . ?
N22 N21 Co1 117.56(10) . . ?
C21 N21 Co1 135.83(11) . . ?
C21 N21 N22 106.01(13) . . ?
N14 N13 N12 115.13(14) . . ?
C12 N13 N12 121.78(14) . . ?
C12 N13 N14 123.07(14) . . ?
N13 N12 N11 105.58(13) . . ?
C11 N14 N13 101.24(13) . . ?
N21 N22 N23 105.88(13) . . ?
H15b N15 H15a 120.0 . . ?
C11 N15 H15a 120.0 . . ?
C11 N15 H15b 120.0 . . ?
H25b N25 H25a 108.9 . . ?
C21 N25 H25a 110.0 . . ?
C21 N25 H25b 109.4 . . ?
N21 C21 N24 111.89(14) . . ?
N25 C21 N24 124.70(15) . . ?
N25 C21 N21 123.17(16) . . ?
H22a C22 N23 109.5 . . ?
H22b C22 N23 109.5 . . ?
H22b C22 H22a 109.5 . . ?
H22c C22 N23 109.5 . . ?
H22c C22 H22a 109.5 . . ?
H22c C22 H22b 109.5 . . ?
N14 C11 N11 111.63(14) . . ?
N15 C11 N11 123.83(16) . . ?
N15 C11 N14 124.46(16) . . ?
H12a C12 N13 109.5 . . ?
H12b C12 N13 109.5 . . ?
H12b C12 H12a 109.5 . . ?
H12c C12 N13 109.5 . . ?
H12c C12 H12a 109.5 . . ?
H12c C12 H12b 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
Co1 N11 N12 N13 178.48(12) . . . . ?
Co1 N11 C11 N14 -178.16(17) . . . . ?
Co1 N11 C11 N15 -1.18(18) . . . . ?
Co1 N21 N22 N23 172.37(11) . . . . ?
Co1 N21 C21 N24 -169.75(16) . . . . ?
Co1 N21 C21 N25 15.54(17) . . . . ?
N24 N23 N22 N21 -0.46(14) . . . . ?
N24 C21 N21 N22 0.75(15) . . . . ?
N23 N24 C21 N21 -0.95(13) . . . . ?
N23 N24 C21 N25 173.66(12) . . . . ?
N23 N22 N21 C21 -0.17(14) . . . . ?
N11 N12 N13 N14 0.03(15) . . . . ?
N11 N12 N13 C12 178.24(13) . . . . ?
N11 C11 N14 N13 0.43(16) . . . . ?
N21 N22 N23 C22 178.55(12) . . . . ?
N13 N12 N11 C11 0.24(15) . . . . ?
N13 N14 C11 N15 -176.52(12) . . . . ?
N12 N11 C11 N14 -0.44(14) . . . . ?
N12 N11 C11 N15 176.54(13) . . . . ?
N12 N13 N14 C11 -0.28(16) . . . . ?
N22 N23 N24 C21 0.88(15) . . . . ?
N22 N21 C21 N25 -173.97(13) . . . . ?
C21 N24 N23 C22 -178.13(12) . . . . ?
C11 N14 N13 C12 -178.47(14) . . . . ?


_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 1.354
_oxdiff_exptl_absorpt_empirical_full_min 0.803
loop_
_restr_distance_atom_site_label_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
_restr_distance_diff
O31 H31a 1 0.8700 0.0200 0.0200
O31 H31b 1 0.8700 0.0200 0.0051
H31a H31b 1 1.3800 0.0400 0.0313

