# 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_mb-001-03
_database_code_depnum_ccdc_archive 'CCDC 2409307'
loop_
_audit_author_name
_audit_author_address
'Luca Carrella'
;Department of Chemistry, Johannes Gutenberg University of Mainz
Germany
;
_audit_update_record             
;
2024-12-11 deposited with the CCDC.	2026-02-05 downloaded from the CCDC.
;
_audit_creation_date             2023-08-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C96 H129.75 Co5 N9 O16, 0.25(C4 H9)'
_chemical_formula_sum            'C44 H52 Cu2 N4 O8'
_chemical_formula_weight         891.97
_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'
Cu Cu 0.3201 1.2651 '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'

_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      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   16.7781(8)
_cell_length_b                   17.5851(8)
_cell_length_c                   6.8233(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2013.18(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    61996
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.20
_cell_measurement_theta_min      2.32
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.116
_exptl_absorpt_correction_T_max  0.9583
_exptl_absorpt_correction_T_min  0.6966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             932
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0175
0 1 0 0.0175
-1 -1 2 0.0180
1 1 -2 0.0180
1 -3 0 0.1285
-1 3 0 0.1285

_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_exptl_crystal_size_rad          0.100
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.864
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            17977
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.864
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.465
_diffrn_reflns_theta_min         2.316
_diffrn_ambient_temperature      120
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.864
_diffrn_measurement_details      
;
 1783 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  180
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Axo Mo'
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_target            Cu
_diffrn_source_type              'I\mS Incoatec'
_diffrn_source_voltage           60
_reflns_d_resolution_high        0.662
_reflns_d_resolution_low         8.793
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_limit_h_max              21
_reflns_limit_h_min              -24
_reflns_limit_k_max              26
_reflns_limit_k_min              -22
_reflns_limit_l_max              7
_reflns_limit_l_min              -9
_reflns_number_gt                2413
_reflns_number_total             3150
_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       
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection       
;
X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)
;
_computing_data_reduction        
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.1, Darmstadt 2022
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.158
_refine_diff_density_min         -1.162
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         3150
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0573
_refine_ls_restrained_S_all      1.096
_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)+(0.0843P)²+3.3531P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1539
_refine_ls_wR_factor_ref         0.1674
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C8(H8)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C)
;
_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
Cu1 Cu 0.500000 0.51015(2) 0.750000 0.01875(15) Uani 1 2 d S T P . .
O1 O 0.57715(11) 0.58657(11) 0.6964(3) 0.0219(4) Uani 1 1 d . . . . .
O2 O 0.63625(14) 0.74525(12) 0.4900(3) 0.0323(5) Uani 1 1 d . . . . .
N1 N 0.57108(13) 0.42829(12) 0.6750(3) 0.0214(4) Uani 1 1 d . . . . .
C1 C 0.53163(16) 0.35382(14) 0.6694(4) 0.0241(5) Uani 1 1 d . . . . .
H1A H 0.570876 0.312757 0.692670 0.029 Uiso 1 1 calc R U . . .
H1B H 0.506526 0.345491 0.539899 0.029 Uiso 1 1 calc R U . . .
C2 C 0.64555(15) 0.43422(15) 0.6326(4) 0.0224(5) Uani 1 1 d . . . . .
H2 H 0.673820 0.388583 0.605812 0.027 Uiso 1 1 calc R U . . .
C3 C 0.68971(15) 0.50478(15) 0.6225(4) 0.0213(5) Uani 1 1 d . . . . .
C4 C 0.65281(15) 0.57719(15) 0.6547(3) 0.0212(5) Uani 1 1 d . . . . .
C5 C 0.70347(15) 0.64218(16) 0.6430(4) 0.0233(5) Uani 1 1 d . . . . .
C6 C 0.78395(16) 0.63439(17) 0.6003(4) 0.0270(5) Uani 1 1 d . . . . .
H6 H 0.816159 0.678777 0.595005 0.032 Uiso 1 1 calc R U . . .
C7 C 0.81969(15) 0.56337(18) 0.5645(4) 0.0273(6) Uani 1 1 d . . . . .
C8 C 0.77131(16) 0.50052(17) 0.5765(4) 0.0252(5) Uani 1 1 d . . . . .
H8 H 0.794017 0.451907 0.552592 0.030 Uiso 1 1 calc R U . . .
C9 C 0.90750(17) 0.5567(2) 0.5134(5) 0.0353(7) Uani 1 1 d . . . . .
H9A H 0.939531 0.579743 0.617867 0.053 Uiso 1 1 calc R U . . .
H9B H 0.917852 0.583187 0.389639 0.053 Uiso 1 1 calc R U . . .
H9C H 0.921781 0.502943 0.499851 0.053 Uiso 1 1 calc R U . . .
C10 C 0.66773(17) 0.71930(16) 0.6732(4) 0.0270(5) Uani 1 1 d . . . . .
H10A H 0.624699 0.716584 0.772176 0.032 Uiso 1 1 calc R U . . .
H10B H 0.708911 0.755119 0.720903 0.032 Uiso 1 1 calc R U . . .
C11 C 0.5847(2) 0.80826(19) 0.5135(5) 0.0409(8) Uani 1 1 d . . . . .
H11A H 0.567642 0.826497 0.384432 0.061 Uiso 1 1 calc R U . . .
H11B H 0.612904 0.849065 0.582521 0.061 Uiso 1 1 calc R U . . .
H11C H 0.537943 0.792862 0.589765 0.061 Uiso 1 1 calc R U . . .


_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
Cu1 O1 1.9013(19) 3_656 ?
Cu1 O1 1.9013(19) . ?
Cu1 N1 1.938(2) 3_656 ?
Cu1 N1 1.938(2) . ?
O1 C4 1.312(3) . ?
O2 C10 1.432(3) . ?
O2 C11 1.414(4) . ?
N1 C1 1.468(3) . ?
N1 C2 1.287(3) . ?
C1 C1 1.528(5) 3_656 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2 0.9500 . ?
C2 C3 1.447(4) . ?
C3 C4 1.433(4) . ?
C3 C8 1.407(4) . ?
C4 C5 1.426(4) . ?
C5 C6 1.388(4) . ?
C5 C10 1.497(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.407(4) . ?
C7 C8 1.374(4) . ?
C7 C9 1.518(4) . ?
C8 H8 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 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
O1 Cu1 O1 90.05(11) 3_656 . ?
O1 Cu1 N1 174.06(8) 3_656 . ?
O1 Cu1 N1 93.17(9) . . ?
O1 Cu1 N1 93.17(9) 3_656 3_656 ?
O1 Cu1 N1 174.06(8) . 3_656 ?
N1 Cu1 N1 84.07(13) . 3_656 ?
C4 O1 Cu1 127.73(17) . . ?
C11 O2 C10 112.1(2) . . ?
C1 N1 Cu1 113.08(16) . . ?
C2 N1 Cu1 126.63(18) . . ?
C2 N1 C1 120.3(2) . . ?
N1 C1 C1 107.14(16) . 3_656 ?
N1 C1 H1A 110.3 . . ?
N1 C1 H1B 110.3 . . ?
C1 C1 H1A 110.3 3_656 . ?
C1 C1 H1B 110.3 3_656 . ?
H1A C1 H1B 108.5 . . ?
N1 C2 H2 117.4 . . ?
N1 C2 C3 125.3(2) . . ?
C3 C2 H2 117.4 . . ?
C4 C3 C2 122.3(2) . . ?
C8 C3 C2 117.6(2) . . ?
C8 C3 C4 120.1(2) . . ?
O1 C4 C3 124.3(2) . . ?
O1 C4 C5 119.2(2) . . ?
C5 C4 C3 116.5(2) . . ?
C4 C5 C10 118.7(2) . . ?
C6 C5 C4 120.8(3) . . ?
C6 C5 C10 120.5(2) . . ?
C5 C6 H6 118.7 . . ?
C5 C6 C7 122.6(3) . . ?
C7 C6 H6 118.7 . . ?
C6 C7 C9 121.5(3) . . ?
C8 C7 C6 116.9(2) . . ?
C8 C7 C9 121.7(3) . . ?
C3 C8 H8 118.5 . . ?
C7 C8 C3 123.1(3) . . ?
C7 C8 H8 118.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O2 C10 C5 108.5(2) . . ?
O2 C10 H10A 110.0 . . ?
O2 C10 H10B 110.0 . . ?
C5 C10 H10A 110.0 . . ?
C5 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
O2 C11 H11A 109.5 . . ?
O2 C11 H11B 109.5 . . ?
O2 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 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
Cu1 O1 C4 C3 6.6(4) . . . . ?
Cu1 O1 C4 C5 -172.20(17) . . . . ?
Cu1 N1 C1 C1 -33.5(3) . . . 3_656 ?
Cu1 N1 C2 C3 -3.7(4) . . . . ?
O1 C4 C5 C6 179.6(2) . . . . ?
O1 C4 C5 C10 -1.8(4) . . . . ?
N1 C2 C3 C4 -1.8(4) . . . . ?
N1 C2 C3 C8 179.2(3) . . . . ?
C1 N1 C2 C3 176.4(2) . . . . ?
C2 N1 C1 C1 146.4(3) . . . 3_656 ?
C2 C3 C4 O1 0.3(4) . . . . ?
C2 C3 C4 C5 179.2(2) . . . . ?
C2 C3 C8 C7 -179.3(3) . . . . ?
C3 C4 C5 C6 0.7(4) . . . . ?
C3 C4 C5 C10 179.3(2) . . . . ?
C4 C3 C8 C7 1.6(4) . . . . ?
C4 C5 C6 C7 0.6(4) . . . . ?
C4 C5 C10 O2 -85.3(3) . . . . ?
C5 C6 C7 C8 -1.0(4) . . . . ?
C5 C6 C7 C9 178.6(3) . . . . ?
C6 C5 C10 O2 93.2(3) . . . . ?
C6 C7 C8 C3 -0.2(4) . . . . ?
C8 C3 C4 O1 179.4(2) . . . . ?
C8 C3 C4 C5 -1.8(4) . . . . ?
C9 C7 C8 C3 -179.7(3) . . . . ?
C10 C5 C6 C7 -177.9(2) . . . . ?
C11 O2 C10 C5 165.5(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_STOE_detector_distance          '60.0 mm'
_STOE_detector_pixelsize_x       '0.075 mm'
_STOE_detector_pixelsize_y       '0.075 mm'
_STOE_detector_size_x            '8.0 cm'
_STOE_detector_size_y            '7.7 cm'
_STOE_evaluation_integration_A   12.0
_STOE_evaluation_integration_B   0.9
_STOE_evaluation_integration_EMS 0.032
_STOE_evaluation_LANA_BIS_l_even_max -
_STOE_evaluation_LANA_BIS_l_odd_max -
_STOE_evaluation_LANA_BOS_l_even_max 4
_STOE_evaluation_LANA_BOS_l_odd_max 1
_STOE_evaluation_LANA_completeness 86.2
_STOE_evaluation_LANA_DXS_max_order 1
_STOE_evaluation_LANA_DYS_max_order 1
_STOE_evaluation_LANA_FS_max_order 4
_STOE_evaluation_LANA_max_2theta_available 65.0
_STOE_evaluation_LANA_max_2theta_desired 65.0
_STOE_evaluation_LANA_mean_redundancy 5.7
_STOE_evaluation_LANA_number_refls_after_OR 17977
_STOE_evaluation_LANA_number_refls_outliers 6060
_STOE_evaluation_LANA_number_refls_total 24037
_STOE_evaluation_LANA_number_refls_unique 3150
_STOE_evaluation_LANA_number_refls_written 17977
_STOE_evaluation_LANA_OR_c1      0.035
_STOE_evaluation_LANA_OR_c2      0
_STOE_evaluation_LANA_OR_c3      0
_STOE_evaluation_LANA_OR_c4      0.7
_STOE_evaluation_LANA_point_group mmm
_STOE_evaluation_LANA_table      
;
#----------------------------------------------------------------------------
2Theta           7.6   14.4   21.2   28.0   34.8   41.6   48.4   55.2   62.0
#----------------------------------------------------------------------------
<Resolution>    4.70   2.77   1.93   1.46   1.18   1.00   0.87   0.77   0.70
N(total)         327   1431   2717   3059   4360   4623   3769   3135    616
<Redundancy>    12.6   15.8   14.1    9.2    8.6    6.9    4.4    3.3    1.4
Complet. [%%]   100.0  100.0  100.0  100.0  100.0  100.0  100.0   98.0   45.5
<I/sigma>      297.8  158.7   76.5   61.7   32.9   19.8   11.7    6.5    3.8
R(int)         0.057  0.046  0.064  0.067  0.059  0.066  0.057  0.083  0.112
#----------------------------------------------------------------------------
;
_STOE_measurement_identifier     MB-001-03
_STOE_measurement_max_exposure_per_frame '60.0 s'
_STOE_measurement_mean_exposure_per_frame '60.0 s'
_STOE_measurement_min_exposure_per_frame '60.0 s'
_STOE_measurement_total_exposure_time '29.7 h'
_STOE_measurement_total_frame_number 1783
_STOE_measurement_total_run_number 4
_STOE_measurement_tube_power     '49.8 W'
####################################################################### 
# 
# 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_xb-585-02
_database_code_depnum_ccdc_archive 'CCDC 2409308'
loop_
_audit_author_name
_audit_author_address
'Luca Carrella'
;Department of Chemistry, Johannes Gutenberg University of Mainz
Germany
;
_audit_update_record             
;
2024-12-11 deposited with the CCDC.	2026-02-05 downloaded from the CCDC.
;
_audit_creation_date             2023-07-18
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C22 H26 N2 Ni O4)'
_chemical_formula_sum            'C44 H52 N4 Ni2 O8'
_chemical_formula_weight         882.31
_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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.3770(12)
_cell_length_b                   12.7547(7)
_cell_length_c                   6.7212(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.890(4)
_cell_angle_gamma                90
_cell_volume                     1996.74(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    29751
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.32
_cell_measurement_theta_min      3.07
_shelx_estimated_absorpt_T_max   0.961
_shelx_estimated_absorpt_T_min   0.661
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_T_max  0.9554
_exptl_absorpt_correction_T_min  0.6792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_exptl_crystal_size_rad          0.060
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            19606
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.709
_diffrn_reflns_theta_min         3.072
_diffrn_ambient_temperature      120
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_details      
;
 1561 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  180
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Axo Mo'
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_voltage           60
_reflns_d_resolution_high        0.658
_reflns_d_resolution_low         6.697
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_limit_h_max              33
_reflns_limit_h_min              -35
_reflns_limit_k_max              19
_reflns_limit_k_min              -19
_reflns_limit_l_max              10
_reflns_limit_l_min              -9
_reflns_number_gt                2530
_reflns_number_total             3317
_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       
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection       
;
X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)
;
_computing_data_reduction        
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.1, Darmstadt 2022
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.324
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         3317
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0483
_refine_ls_restrained_S_all      1.106
_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)+(0.0969P)²+0.6080P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1458
_refine_ls_wR_factor_ref         0.1534
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C)
;
_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
Ni1 Ni 0.500000 0.51926(3) 0.750000 0.02715(14) Uani 1 2 d S T P . .
O1 O 0.55264(6) 0.62625(12) 0.7315(2) 0.0300(3) Uani 1 1 d . . . . .
O2 O 0.59521(9) 0.83709(16) 0.5357(3) 0.0537(5) Uani 1 1 d . . . . .
N1 N 0.55299(8) 0.41417(14) 0.7248(2) 0.0318(4) Uani 1 1 d . . . . .
C1 C 0.52652(11) 0.30885(17) 0.6933(3) 0.0370(5) Uani 1 1 d . . . . .
H1A H 0.553517 0.253428 0.744691 0.044 Uiso 1 1 calc R U . . .
H1B H 0.516170 0.296232 0.549386 0.044 Uiso 1 1 calc R U . . .
C2 C 0.60842(10) 0.42321(18) 0.7288(3) 0.0345(5) Uani 1 1 d . . . . .
H2 H 0.630363 0.360795 0.722340 0.041 Uiso 1 1 calc R U . . .
C3 C 0.63875(10) 0.52109(18) 0.7424(3) 0.0321(4) Uani 1 1 d . . . . .
C4 C 0.69966(10) 0.5204(2) 0.7510(3) 0.0388(5) Uani 1 1 d . . . . .
H4 H 0.719012 0.454902 0.751686 0.047 Uiso 1 1 calc R U . . .
C5 C 0.73133(10) 0.6099(2) 0.7584(3) 0.0438(6) Uani 1 1 d . . . . .
C6 C 0.70181(10) 0.7048(2) 0.7542(3) 0.0408(5) Uani 1 1 d . . . . .
H6 H 0.723320 0.768048 0.757689 0.049 Uiso 1 1 calc R U . . .
C7 C 0.64223(9) 0.71116(19) 0.7453(3) 0.0348(4) Uani 1 1 d . . . . .
C8 C 0.60910(9) 0.61787(18) 0.7386(3) 0.0304(4) Uani 1 1 d . . . . .
C9 C 0.79685(11) 0.6082(3) 0.7631(4) 0.0589(8) Uani 1 1 d . . . . .
H9A H 0.810586 0.535936 0.781580 0.088 Uiso 1 1 calc R U . . .
H9B H 0.813246 0.651682 0.873815 0.088 Uiso 1 1 calc R U . . .
H9C H 0.808699 0.635722 0.636825 0.088 Uiso 1 1 calc R U . . .
C10 C 0.61251(10) 0.81455(19) 0.7385(3) 0.0390(5) Uani 1 1 d . . . . .
H10A H 0.578610 0.811802 0.817174 0.047 Uiso 1 1 calc R U . . .
H10B H 0.638796 0.869732 0.795570 0.047 Uiso 1 1 calc R U . . .
C11 C 0.55894(14) 0.9259(3) 0.5187(5) 0.0647(8) Uani 1 1 d . . . . .
H11A H 0.577764 0.984800 0.591357 0.097 Uiso 1 1 calc R U . . .
H11B H 0.522690 0.909783 0.575337 0.097 Uiso 1 1 calc R U . . .
H11C H 0.551225 0.944612 0.377532 0.097 Uiso 1 1 calc R U . . .


_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 1.8488(15) 2_656 ?
Ni1 O1 1.8487(15) . ?
Ni1 N1 1.8427(18) 2_656 ?
Ni1 N1 1.8426(18) . ?
O1 C8 1.321(2) . ?
O2 C10 1.418(3) . ?
O2 C11 1.413(3) . ?
N1 C1 1.487(3) . ?
N1 C2 1.299(3) . ?
C1 C1 1.510(5) 2_656 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2 0.9500 . ?
C2 C3 1.435(3) . ?
C3 C4 1.420(3) . ?
C3 C8 1.415(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.360(4) . ?
C5 C6 1.392(4) . ?
C5 C9 1.530(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.391(3) . ?
C7 C8 1.418(3) . ?
C7 C10 1.489(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 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
O1 Ni1 O1 84.86(9) . 2_656 ?
N1 Ni1 O1 94.25(8) 2_656 2_656 ?
N1 Ni1 O1 94.26(8) . . ?
N1 Ni1 O1 178.39(7) . 2_656 ?
N1 Ni1 O1 178.39(7) 2_656 . ?
N1 Ni1 N1 86.66(12) . 2_656 ?
C8 O1 Ni1 127.34(14) . . ?
C11 O2 C10 111.1(2) . . ?
C1 N1 Ni1 113.30(15) . . ?
C2 N1 Ni1 127.65(16) . . ?
C2 N1 C1 119.04(19) . . ?
N1 C1 C1 106.12(12) . 2_656 ?
N1 C1 H1A 110.5 . . ?
N1 C1 H1B 110.5 . . ?
C1 C1 H1A 110.5 2_656 . ?
C1 C1 H1B 110.5 2_656 . ?
H1A C1 H1B 108.7 . . ?
N1 C2 H2 117.8 . . ?
N1 C2 C3 124.4(2) . . ?
C3 C2 H2 117.8 . . ?
C4 C3 C2 119.0(2) . . ?
C8 C3 C2 121.3(2) . . ?
C8 C3 C4 119.6(2) . . ?
C3 C4 H4 118.8 . . ?
C5 C4 C3 122.5(2) . . ?
C5 C4 H4 118.8 . . ?
C4 C5 C6 117.5(2) . . ?
C4 C5 C9 122.0(3) . . ?
C6 C5 C9 120.5(3) . . ?
C5 C6 H6 118.5 . . ?
C7 C6 C5 123.0(2) . . ?
C7 C6 H6 118.5 . . ?
C6 C7 C8 119.6(2) . . ?
C6 C7 C10 121.1(2) . . ?
C8 C7 C10 119.31(19) . . ?
O1 C8 C3 123.9(2) . . ?
O1 C8 C7 118.33(19) . . ?
C3 C8 C7 117.8(2) . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O2 C10 C7 107.64(19) . . ?
O2 C10 H10A 110.2 . . ?
O2 C10 H10B 110.2 . . ?
C7 C10 H10A 110.2 . . ?
C7 C10 H10B 110.2 . . ?
H10A C10 H10B 108.5 . . ?
O2 C11 H11A 109.5 . . ?
O2 C11 H11B 109.5 . . ?
O2 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 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
Ni1 O1 C8 C3 6.6(3) . . . . ?
Ni1 O1 C8 C7 -172.65(13) . . . . ?
Ni1 N1 C1 C1 -32.6(2) . . . 2_656 ?
Ni1 N1 C2 C3 -4.0(3) . . . . ?
O1 Ni1 O1 C8 170.23(19) 2_656 . . . ?
O1 Ni1 N1 C1 -169.09(13) . . . . ?
O1 Ni1 N1 C2 9.83(18) . . . . ?
N1 Ni1 O1 C8 -11.12(17) . . . . ?
N1 Ni1 N1 C1 12.24(10) 2_656 . . . ?
N1 Ni1 N1 C2 -168.8(2) 2_656 . . . ?
N1 C2 C3 C4 178.3(2) . . . . ?
N1 C2 C3 C8 -4.5(3) . . . . ?
C1 N1 C2 C3 174.91(18) . . . . ?
C2 N1 C1 C1 148.4(2) . . . 2_656 ?
C2 C3 C4 C5 178.1(2) . . . . ?
C2 C3 C8 O1 3.1(3) . . . . ?
C2 C3 C8 C7 -177.69(17) . . . . ?
C3 C4 C5 C6 -0.9(3) . . . . ?
C3 C4 C5 C9 -178.7(2) . . . . ?
C4 C3 C8 O1 -179.71(18) . . . . ?
C4 C3 C8 C7 -0.5(3) . . . . ?
C4 C5 C6 C7 0.7(3) . . . . ?
C5 C6 C7 C8 -0.4(3) . . . . ?
C5 C6 C7 C10 -179.2(2) . . . . ?
C6 C7 C8 O1 179.56(18) . . . . ?
C6 C7 C8 C3 0.3(3) . . . . ?
C6 C7 C10 O2 97.0(2) . . . . ?
C8 C3 C4 C5 0.8(3) . . . . ?
C8 C7 C10 O2 -81.8(2) . . . . ?
C9 C5 C6 C7 178.5(2) . . . . ?
C10 C7 C8 O1 -1.6(3) . . . . ?
C10 C7 C8 C3 179.09(18) . . . . ?
C11 O2 C10 C7 170.9(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_STOE_detector_distance          '60.0 mm'
_STOE_detector_pixelsize_x       '0.075 mm'
_STOE_detector_pixelsize_y       '0.075 mm'
_STOE_detector_size_x            '8.0 cm'
_STOE_detector_size_y            '7.7 cm'
_STOE_evaluation_integration_A   12.5
_STOE_evaluation_integration_B   0.4
_STOE_evaluation_integration_EMS 0.017
_STOE_evaluation_LANA_BIS_l_even_max -
_STOE_evaluation_LANA_BIS_l_odd_max -
_STOE_evaluation_LANA_BOS_l_even_max 4
_STOE_evaluation_LANA_BOS_l_odd_max 1
_STOE_evaluation_LANA_completeness 90.1
_STOE_evaluation_LANA_DXS_max_order 1
_STOE_evaluation_LANA_DYS_max_order 1
_STOE_evaluation_LANA_FS_max_order 3
_STOE_evaluation_LANA_max_2theta_available 65.5
_STOE_evaluation_LANA_max_2theta_desired 65.5
_STOE_evaluation_LANA_mean_redundancy 5.9
_STOE_evaluation_LANA_number_refls_after_OR 20194
_STOE_evaluation_LANA_number_refls_outliers 5655
_STOE_evaluation_LANA_number_refls_total 25849
_STOE_evaluation_LANA_number_refls_unique 3447
_STOE_evaluation_LANA_number_refls_written 20194
_STOE_evaluation_LANA_OR_c1      0.035
_STOE_evaluation_LANA_OR_c2      0
_STOE_evaluation_LANA_OR_c3      0
_STOE_evaluation_LANA_OR_c4      0.7
_STOE_evaluation_LANA_point_group 2/m
_STOE_evaluation_LANA_table      
;
#----------------------------------------------------------------------------
2Theta           8.6   15.4   22.2   29.0   35.8   42.6   49.4   56.2   63.0
#----------------------------------------------------------------------------
<Resolution>    4.52   2.62   1.86   1.40   1.15   0.98   0.85   0.76   0.70
N(total)         599   1525   2404   2754   4228   4731   4614   4262    732
<Redundancy>    14.9   13.0   10.5    7.1    8.1    6.9    5.5    4.5    1.5
Complet. [%%]   100.0  100.0  100.0  100.0  100.0  100.0  100.0   99.2   55.7
<I/sigma>      146.9  113.1   59.4   42.7   22.1   12.1    6.3    3.1    1.7
R(int)         0.029  0.029  0.034  0.039  0.042  0.056  0.081  0.122  0.184
#----------------------------------------------------------------------------
;
_STOE_measurement_identifier     XB-585-02
_STOE_measurement_max_exposure_per_frame '45.0 s'
_STOE_measurement_mean_exposure_per_frame '45.0 s'
_STOE_measurement_min_exposure_per_frame '45.0 s'
_STOE_measurement_total_exposure_time '19.5 h'
_STOE_measurement_total_frame_number 1561
_STOE_measurement_total_run_number 7
_STOE_measurement_tube_power     '49.8 W'
