# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 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_s1
_database_code_depnum_ccdc_archive 'CCDC 1471374'
loop_
_audit_author_name
_audit_author_address
'Feng Xu'
;Hunan University
China
;
_audit_update_record             
;
2022-04-25 deposited with the CCDC.	2023-04-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/1
_shelx_SHELXL_version_number     2019/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H94 Cu10 Ni10 O69'
_chemical_formula_weight         2793.56

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'
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           229
_space_group_name_H-M_alt        'I m -3 m'
_space_group_name_Hall           '-I 4 2 3'

_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, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, z+1/2, -y+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z+1/2, x+1/2, y+1/2'
'z+1/2, x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z+1/2, x+1/2'
'-y+1/2, z+1/2, x+1/2'
'y+1/2, z+1/2, -x+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'z+1/2, y+1/2, x+1/2'

_cell_length_a                   17.1976(4)
_cell_length_b                   17.1976(4)
_cell_length_c                   17.1976(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5086.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1915
_cell_measurement_theta_min      2.90
_cell_measurement_theta_max      25.69

_exptl_crystal_description       block
_exptl_crystal_colour            'clear  green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_F_000             2804
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    3.938
_shelx_estimated_absorpt_T_min   0.439
_shelx_estimated_absorpt_T_max   0.506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4389
_exptl_absorpt_correction_T_max  0.5060
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7991
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_av_R_equivalents  0.1238
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.901
_diffrn_reflns_theta_max         24.991
_diffrn_reflns_theta_full        24.991
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 0.971
_reflns_number_total             469
_reflns_number_gt                434
_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    ?
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0458P)²+254.0004P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         469
_refine_ls_number_parameters     59
_refine_ls_number_restraints     198
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.1046
_refine_ls_wR_factor_ref         0.2302
_refine_ls_wR_factor_gt          0.2263
_refine_ls_goodness_of_fit_ref   1.403
_refine_ls_restrained_S_all      1.235
_refine_ls_shift/su_max          0.002
_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
Cu1 Cu 0.000000 0.1379(15) 0.1379(15) 0.0255(12) Uani 0.8502 4 d S TU P . .
Ni1 Ni 0.000000 0.137(10) 0.137(10) 0.033(5) Uani 0.1498 4 d S TU P . .
Ni2 Ni 0.16891(12) 0.16891(12) 0.16891(12) 0.0487(14) Uani 1 6 d S TU P . .
O1 O 0.043(3) 0.043(3) 0.043(3) 0.034(5) Uani 0.25 6 d S TU P . .
O1' O 0.000000 0.074(8) 0.000000 0.033(6) Uani 0.1666 8 d S TU P . .
O2 O 0.0855(4) 0.1924(6) 0.0855(4) 0.030(2) Uani 1 2 d S TU P . .
H2 H 0.076914 0.240204 0.076886 0.036 Uiso 1 2 d R U P . .
O3 O 0.2351(10) 0.000000 0.2351(10) 0.089(5) Uani 1 4 d S TU P . .
H3 H 0.258009 -0.036143 0.258198 0.107 Uiso 0.0417 2 d R U P . .
O4 O 0.2487(7) 0.1316(10) 0.2487(7) 0.084(4) Uani 1 2 d S TU P . .
H4B H 0.233115 0.156866 0.288300 0.101 Uiso 0.25 1 d R U P A 2
H4C H 0.288046 0.156866 0.233370 0.101 Uiso 0.25 1 d R U P A 2
O5 O 0.064(4) 0.334(4) 1.000000 0.076(11) Uani 0.25 2 d S TU P . .
C1 C 0.263(2) 0.065(4) 0.263(2) 0.082(6) Uani 0.5 2 d S TU P . .
C2 C 0.319(2) 0.048(3) 0.319(2) 0.093(7) Uani 0.5 2 d S TU P . .
H2B H 0.336623 0.098215 0.337463 0.140 Uiso 0.5 2 d R U P . .
H2C H 0.297633 0.020095 0.365430 0.140 Uiso 0.25 1 d R U P . .
H2D H 0.361903 0.020095 0.301160 0.140 Uiso 0.25 1 d R U P . .
C3 C 0.000000 0.356(7) 1.000000 0.079(11) Uani 0.5 8 d S TU P . .
C4 C 0.000000 0.454(6) 1.000000 0.081(11) Uani 0.5 8 d S TU P . .
H4D H -0.052480 0.472879 1.000000 0.122 Uiso 0.125 2 d R U P . .
H4E H 0.026240 0.472879 1.045450 0.122 Uiso 0.0625 1 d R U P . .
H4F H 0.026240 0.472879 0.954550 0.122 Uiso 0.0625 1 d R U P . .
C5 C 0.000000 0.000000 0.000000 0.036(6) Uani 1 48 d S TU P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O2 1.963(5) . ?
Cu1 O2 1.963(5) 5 ?
Cu1 O2 1.963(5) 52 ?
Cu1 O2 1.963(5) 54 ?
Cu1 O3 2.36(4) 9 ?
Cu1 O1 2.43(6) 52 ?
Cu1 O1 2.43(6) . ?
Cu1 Ni2 3.001(10) . ?
Cu1 Ni2 3.001(10) 52 ?
Ni1 O2 1.963(8) . ?
Ni1 O2 1.963(8) 5 ?
Ni1 O2 1.963(8) 52 ?
Ni1 O2 1.963(8) 54 ?
Ni1 O3 2.4(3) 9 ?
Ni2 O4 2.045(17) . ?
Ni2 O4 2.045(17) 9 ?
Ni2 O4 2.045(17) 5 ?
Ni2 O2 2.069(11) 9 ?
Ni2 O2 2.069(11) 5 ?
Ni2 O2 2.069(11) . ?
O1 O1' 1.18(7) 9 ?
O1 O1' 1.18(7) 5 ?
O1 O1' 1.18(7) . ?
O1 C5 1.28(8) . ?
O1 O1 1.48(9) 52 ?
O1 O1 1.48(9) 51 ?
O1 O1 1.48(9) 50 ?
O1' C5 1.28(14) . ?
O3 C1 1.31(5) 51 ?
O3 C1 1.31(5) . ?
O4 C1 1.19(6) . ?
O5 C3 1.15(7) . ?
O5 O5 1.55(10) 21_456 ?
O5 O5 1.55(10) 23_656 ?
C1 C2 1.40(7) . ?
C2 C2 1.67(12) 51 ?
C3 C4 1.70(16) . ?
C4 C4 1.6(2) 49_567 ?

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
O2 Cu1 O2 83.0(7) . 5 ?
O2 Cu1 O2 97.0(7) . 52 ?
O2 Cu1 O2 179(2) 5 52 ?
O2 Cu1 O2 179(2) . 54 ?
O2 Cu1 O2 97.0(7) 5 54 ?
O2 Cu1 O2 83.0(7) 52 54 ?
O2 Cu1 O3 89.3(11) . 9 ?
O2 Cu1 O3 89.3(11) 5 9 ?
O2 Cu1 O3 89.3(11) 52 9 ?
O2 Cu1 O3 89.3(11) 54 9 ?
O2 Cu1 O1 103.9(16) . 52 ?
O2 Cu1 O1 103.9(16) 5 52 ?
O2 Cu1 O1 77.5(14) 52 52 ?
O2 Cu1 O1 77.5(14) 54 52 ?
O3 Cu1 O1 162.3(15) 9 52 ?
O2 Cu1 O1 77.5(14) . . ?
O2 Cu1 O1 77.5(14) 5 . ?
O2 Cu1 O1 103.9(16) 52 . ?
O2 Cu1 O1 103.9(16) 54 . ?
O3 Cu1 O1 162.3(15) 9 . ?
O1 Cu1 O1 35(3) 52 . ?
O2 Cu1 Ni2 43.3(4) . . ?
O2 Cu1 Ni2 43.3(4) 5 . ?
O2 Cu1 Ni2 136.2(7) 52 . ?
O2 Cu1 Ni2 136.2(7) 54 . ?
O3 Cu1 Ni2 75.5(7) 9 . ?
O1 Cu1 Ni2 122.3(17) 52 . ?
O1 Cu1 Ni2 86.8(15) . . ?
O2 Cu1 Ni2 136.2(7) . 52 ?
O2 Cu1 Ni2 136.2(7) 5 52 ?
O2 Cu1 Ni2 43.3(4) 52 52 ?
O2 Cu1 Ni2 43.3(4) 54 52 ?
O3 Cu1 Ni2 75.5(7) 9 52 ?
O1 Cu1 Ni2 86.8(15) 52 52 ?
O1 Cu1 Ni2 122.3(17) . 52 ?
Ni2 Cu1 Ni2 150.9(13) . 52 ?
O2 Ni1 O2 83.0(7) . 5 ?
O2 Ni1 O2 97.0(8) . 52 ?
O2 Ni1 O2 177(10) 5 52 ?
O2 Ni1 O2 177(10) . 54 ?
O2 Ni1 O2 97.0(8) 5 54 ?
O2 Ni1 O2 83.0(7) 52 54 ?
O2 Ni1 O3 89(7) . 9 ?
O2 Ni1 O3 89(7) 5 9 ?
O2 Ni1 O3 89(7) 52 9 ?
O2 Ni1 O3 89(7) 54 9 ?
O4 Ni2 O4 88.3(7) . 9 ?
O4 Ni2 O4 88.3(7) . 5 ?
O4 Ni2 O4 88.3(7) 9 5 ?
O4 Ni2 O2 96.7(4) . 9 ?
O4 Ni2 O2 173.0(6) 9 9 ?
O4 Ni2 O2 96.7(4) 5 9 ?
O4 Ni2 O2 96.7(4) . 5 ?
O4 Ni2 O2 96.7(4) 9 5 ?
O4 Ni2 O2 173.0(6) 5 5 ?
O2 Ni2 O2 77.9(5) 9 5 ?
O4 Ni2 O2 173.0(6) . . ?
O4 Ni2 O2 96.7(4) 9 . ?
O4 Ni2 O2 96.7(4) 5 . ?
O2 Ni2 O2 77.9(5) 9 . ?
O2 Ni2 O2 77.9(5) 5 . ?
O4 Ni2 Cu1 135.5(3) . . ?
O4 Ni2 Cu1 86.2(8) 9 . ?
O4 Ni2 Cu1 135.5(3) 5 . ?
O2 Ni2 Cu1 86.7(7) 9 . ?
O2 Ni2 Cu1 40.6(2) 5 . ?
O2 Ni2 Cu1 40.6(2) . . ?
O4 Ni2 Cu1 135.5(3) . 9 ?
O4 Ni2 Cu1 135.5(3) 9 9 ?
O4 Ni2 Cu1 86.2(8) 5 9 ?
O2 Ni2 Cu1 40.6(2) 9 9 ?
O2 Ni2 Cu1 86.7(7) 5 9 ?
O2 Ni2 Cu1 40.6(2) . 9 ?
Cu1 Ni2 Cu1 68.0(11) . 9 ?
O4 Ni2 Cu1 86.2(8) . 5 ?
O4 Ni2 Cu1 135.5(3) 9 5 ?
O4 Ni2 Cu1 135.5(3) 5 5 ?
O2 Ni2 Cu1 40.6(2) 9 5 ?
O2 Ni2 Cu1 40.6(2) 5 5 ?
O2 Ni2 Cu1 86.7(7) . 5 ?
Cu1 Ni2 Cu1 68.0(11) . 5 ?
Cu1 Ni2 Cu1 68.0(11) 9 5 ?
O1' O1 O1' 100(9) 9 5 ?
O1' O1 O1' 100(9) 9 . ?
O1' O1 O1' 100(9) 5 . ?
O1' O1 C5 63(7) 9 . ?
O1' O1 C5 63(7) 5 . ?
O1' O1 C5 63(7) . . ?
O1' O1 O1 117(7) 9 52 ?
O1' O1 O1 51(3) 5 52 ?
O1' O1 O1 51(3) . 52 ?
C5 O1 O1 54.735(7) . 52 ?
O1' O1 O1 51(3) 9 51 ?
O1' O1 O1 51(3) 5 51 ?
O1' O1 O1 117(7) . 51 ?
C5 O1 O1 54.736(7) . 51 ?
O1 O1 O1 90.000(5) 52 51 ?
O1' O1 O1 51(3) 9 50 ?
O1' O1 O1 117(7) 5 50 ?
O1' O1 O1 51(3) . 50 ?
C5 O1 O1 54.736(8) . 50 ?
O1 O1 O1 90.000(5) 52 50 ?
O1 O1 O1 90.000(5) 51 50 ?
O1' O1 Cu1 86(5) 9 5 ?
O1' O1 Cu1 86(5) 5 5 ?
O1' O1 Cu1 170(8) . 5 ?
C5 O1 Cu1 127.0(14) . 5 ?
O1 O1 Cu1 132.3(4) 52 5 ?
O1 O1 Cu1 72.3(14) 51 5 ?
O1 O1 Cu1 132.3(4) 50 5 ?
O1' O1 Cu1 86(5) 9 9 ?
O1' O1 Cu1 170(8) 5 9 ?
O1' O1 Cu1 86(5) . 9 ?
C5 O1 Cu1 127.0(14) . 9 ?
O1 O1 Cu1 132.3(4) 52 9 ?
O1 O1 Cu1 132.3(4) 51 9 ?
O1 O1 Cu1 72.3(14) 50 9 ?
Cu1 O1 Cu1 88(2) 5 9 ?
O1' O1 Cu1 170(8) 9 . ?
O1' O1 Cu1 86(5) 5 . ?
O1' O1 Cu1 86(5) . . ?
C5 O1 Cu1 127.0(14) . . ?
O1 O1 Cu1 72.3(14) 52 . ?
O1 O1 Cu1 132.3(4) 51 . ?
O1 O1 Cu1 132.3(4) 50 . ?
Cu1 O1 Cu1 88(2) 5 . ?
Cu1 O1 Cu1 88(2) 9 . ?
O1 O1' O1 125(10) 3 . ?
O1 O1' O1 78(6) 3 52 ?
O1 O1' O1 78(6) . 52 ?
O1 O1' O1 78(6) 3 50 ?
O1 O1' O1 78(6) . 50 ?
O1 O1' O1 125(10) 52 50 ?
O1 O1' C5 63(7) 3 . ?
O1 O1' C5 63(7) . . ?
O1 O1' C5 63(7) 52 . ?
O1 O1' C5 63(7) 50 . ?
Ni1 O2 Cu1 1(9) . . ?
Ni1 O2 Cu1 117(6) . 9 ?
Cu1 O2 Cu1 117(2) . 9 ?
Ni1 O2 Ni2 96(3) . . ?
Cu1 O2 Ni2 96.2(5) . . ?
Cu1 O2 Ni2 96.2(5) 9 . ?
C1 O3 C1 119(5) 51 . ?
C1 O3 Cu1 121(3) 51 5 ?
C1 O3 Cu1 121(3) . 5 ?
C1 O4 Ni2 125(2) . . ?
C3 O5 O5 48(2) . 21_456 ?
C3 O5 O5 48(2) . 23_656 ?
O5 O5 O5 90.00(2) 21_456 23_656 ?
O4 C1 O3 133(4) . . ?
O4 C1 C2 118(5) . . ?
O3 C1 C2 109(5) . . ?
C1 C2 C2 102(4) . 51 ?
O5 C3 O5 84(4) 21_456 3_557 ?
O5 C3 O5 143(10) 21_456 23_656 ?
O5 C3 O5 84(4) 3_557 23_656 ?
O5 C3 O5 84(4) 21_456 . ?
O5 C3 O5 143(10) 3_557 . ?
O5 C3 O5 84(4) 23_656 . ?
O5 C3 C4 109(7) 21_456 . ?
O5 C3 C4 109(7) 3_557 . ?
O5 C3 C4 109(7) 23_656 . ?
O5 C3 C4 109(7) . . ?
C4 C4 C3 180.00(5) 49_567 . ?
O1 C5 O1 180(10) 49 . ?
O1 C5 O1 109.471(2) 49 52 ?
O1 C5 O1 70.529(2) . 52 ?
O1 C5 O1 70.529(2) 49 4 ?
O1 C5 O1 109.471(2) . 4 ?
O1 C5 O1 180(10) 52 4 ?
O1 C5 O1 70.529(4) 49 2 ?
O1 C5 O1 109.471(4) . 2 ?
O1 C5 O1 70.529(1) 52 2 ?
O1 C5 O1 109.471(1) 4 2 ?
O1 C5 O1 109.471(4) 49 50 ?
O1 C5 O1 70.529(4) . 50 ?
O1 C5 O1 109.471(1) 52 50 ?
O1 C5 O1 70.529(1) 4 50 ?
O1 C5 O1 180(10) 2 50 ?
O1 C5 O1 70.529(5) 49 3 ?
O1 C5 O1 109.471(4) . 3 ?
O1 C5 O1 70.5 52 3 ?
O1 C5 O1 109.5 4 3 ?
O1 C5 O1 109.5 2 3 ?
O1 C5 O1 70.5 50 3 ?
O1 C5 O1 109.471(4) 49 51 ?
O1 C5 O1 70.529(5) . 51 ?
O1 C5 O1 109.5 52 51 ?
O1 C5 O1 70.5 4 51 ?
O1 C5 O1 70.5 2 51 ?
O1 C5 O1 109.5 50 51 ?
O1 C5 O1 180(10) 3 51 ?
O1 C5 O1' 54.735(3) 49 57 ?
O1 C5 O1' 125.265(3) . 57 ?
O1 C5 O1' 54.735(3) 52 57 ?
O1 C5 O1' 125.265(3) 4 57 ?
O1 C5 O1' 54.735(3) 2 57 ?
O1 C5 O1' 125.265(3) 50 57 ?
O1 C5 O1' 54.735(3) 3 57 ?
O1 C5 O1' 125.265(3) 51 57 ?
O1 C5 O1' 125.265(3) 49 9 ?
O1 C5 O1' 54.735(3) . 9 ?
O1 C5 O1' 125.265(3) 52 9 ?
O1 C5 O1' 54.735(3) 4 9 ?
O1 C5 O1' 125.265(3) 2 9 ?
O1 C5 O1' 54.735(3) 50 9 ?
O1 C5 O1' 125.265(3) 3 9 ?
O1 C5 O1' 54.735(3) 51 9 ?
O1' C5 O1' 180.0 57 9 ?
O1 C5 O1' 54.736(4) 49 49 ?
O1 C5 O1' 125.264(3) . 49 ?
O1 C5 O1' 125.264(2) 52 49 ?
O1 C5 O1' 54.736(2) 4 49 ?
O1 C5 O1' 54.736(3) 2 49 ?
O1 C5 O1' 125.264(3) 50 49 ?
O1 C5 O1' 125.264(2) 3 49 ?
O1 C5 O1' 54.736(2) 51 49 ?
O1' C5 O1' 90.000(2) 57 49 ?
O1' C5 O1' 90.000(2) 9 49 ?
O1 C5 O1' 125.264(3) 49 5 ?
O1 C5 O1' 54.736(3) . 5 ?
O1 C5 O1' 54.736(3) 52 5 ?
O1 C5 O1' 125.264(3) 4 5 ?
O1 C5 O1' 54.736(1) 2 5 ?
O1 C5 O1' 125.264(1) 50 5 ?
O1 C5 O1' 125.264(3) 3 5 ?
O1 C5 O1' 54.736(3) 51 5 ?
O1' C5 O1' 90.000(2) 57 5 ?
O1' C5 O1' 90.000(2) 9 5 ?
O1' C5 O1' 90.000(2) 49 5 ?

_refine_diff_density_max         1.174
_refine_diff_density_min         -1.566
_refine_diff_density_rms         0.177

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1840132'
loop_
_audit_author_name
_audit_author_address
'Feng Xu'
;Hunan University
China
;
_audit_update_record             
;
2022-04-25 deposited with the CCDC.	2023-04-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/1
_shelx_SHELXL_version_number     2019/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            
'C31 H94 Co3.46 Cu11.31 Mn0.39 Ni4.15 O69 Zn0.69'
_chemical_formula_weight         2803.48

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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      cubic
_space_group_IT_number           229
_space_group_name_H-M_alt        'I m -3 m'
_space_group_name_Hall           '-I 4 2 3'

_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, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, z+1/2, -y+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z+1/2, x+1/2, y+1/2'
'z+1/2, x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z+1/2, x+1/2'
'-y+1/2, z+1/2, x+1/2'
'y+1/2, z+1/2, -x+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'z+1/2, y+1/2, x+1/2'

_cell_length_a                   17.2463(2)
_cell_length_b                   17.2463(2)
_cell_length_c                   17.2463(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5129.65(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3347
_cell_measurement_theta_min      2.89
_cell_measurement_theta_max      27.38

_exptl_crystal_description       block
_exptl_crystal_colour            'clear  green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_F_000             2800
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    3.871
_shelx_estimated_absorpt_T_min   0.321
_shelx_estimated_absorpt_T_max   0.390
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3209
_exptl_absorpt_correction_T_max  0.3897
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8659
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.362
_diffrn_reflns_theta_max         24.979
_diffrn_reflns_theta_full        24.979
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             484
_reflns_number_gt                423
_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    ?
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0739P)²+260.8606P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.0028(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         484
_refine_ls_number_parameters     56
_refine_ls_number_restraints     300
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0703
_refine_ls_wR_factor_ref         0.2003
_refine_ls_wR_factor_gt          0.1948
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      0.962
_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
Cu1 Cu 0.000000 0.13695(8) 0.13695(8) 0.0302(9) Uani 0.9424 4 d S TU P . .
Zn1 Zn 0.000000 0.13695(8) 0.13695(8) 0.0302(9) Uani 0.0576 4 d S TU P . .
Ni1 Ni 0.16941(10) 0.16941(10) 0.16941(10) 0.0451(11) Uani 0.519 6 d S TU P . .
Co1 Co 0.16941(10) 0.16941(10) 0.16941(10) 0.0451(11) Uani 0.432 6 d S TU P . .
Mn1 Mn 0.16941(10) 0.16941(10) 0.16941(10) 0.0451(11) Uani 0.049 6 d S TU P . .
O1 O 0.0439(3) 0.0439(3) 0.0439(3) 0.037(4) Uani 0.25 6 d DS TU P . .
O1' O 0.000000 0.0760(6) 0.000000 0.036(6) Uani 0.1666 8 d DS TU P . .
O2 O 0.0844(4) 0.1915(5) 0.0844(4) 0.037(2) Uani 1 2 d S TU P . .
H2 H 0.075880 0.239312 0.075951 0.045 Uiso 1 2 d R U P . .
O3 O 0.2365(7) 0.000000 0.2365(7) 0.086(4) Uani 1 4 d S TU P . .
H3 H 0.256943 -0.038370 0.258547 0.103 Uiso 0.0417 2 calc R U P A 1
O4 O 0.2484(5) 0.1332(7) 0.2484(5) 0.083(3) Uani 1 2 d S TU P . .
H4B H 0.232753 0.158508 0.288300 0.100 Uiso 0.25 1 d R U P B 2
H4C H 0.287683 0.158508 0.233370 0.100 Uiso 0.25 1 d R U P B 2
O5 O 0.0661(11) 0.3284(19) 0.000000 0.062(7) Uani 0.25 2 d DS TU P C 1
C1 C 0.2695(12) 0.073(2) 0.2695(12) 0.075(5) Uani 0.5 2 d DS TU P D 1
C2 C 0.3306(13) 0.059(3) 0.3306(13) 0.125(11) Uani 0.5 2 d DS TU P D 1
H2B H 0.337679 0.003070 0.337679 0.187 Uiso 0.25 1 calc R U P D 1
H2C H 0.379627 0.082384 0.314012 0.187 Uiso 0.25 1 calc R U P D 1
H2D H 0.314012 0.082384 0.379627 0.187 Uiso 0.25 1 calc R U P D 1
C3 C 0.000000 0.357(2) 0.000000 0.064(8) Uani 0.5 8 d DS TU P C 1
C4 C 0.000000 0.444(2) 0.000000 0.077(10) Uani 0.5 8 d DS TU P C 1
H4D H 0.000000 0.462456 0.053574 0.116 Uiso 0.0625 1 calc R U P C 1
H4E H 0.046396 0.462456 -0.026787 0.116 Uiso 0.0625 1 calc R U P C 1
H4F H -0.046396 0.462456 -0.026787 0.116 Uiso 0.0625 1 calc R U P C 1
C5 C 0.000000 0.000000 0.000000 0.030(6) Uani 1 48 d DS TU P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O2 1.956(4) . ?
Cu1 O2 1.956(4) 5 ?
Cu1 O2 1.956(4) 52 ?
Cu1 O2 1.956(4) 54 ?
Cu1 O1 2.393(6) 52 ?
Cu1 O1 2.393(6) . ?
Cu1 O3 2.429(18) 9 ?
Cu1 Ni1 3.027(2) . ?
Cu1 Ni1 3.027(2) 52 ?
Ni1 O4 2.024(13) 9 ?
Ni1 O4 2.024(13) 5 ?
Ni1 O4 2.024(13) . ?
Ni1 O2 2.107(9) . ?
Ni1 O2 2.107(9) 9 ?
Ni1 O2 2.107(9) 5 ?
O1 O1' 1.205(7) . ?
O1 O1' 1.205(7) 5 ?
O1 O1' 1.205(7) 9 ?
O1 C5 1.311(10) . ?
O1 O1 1.514(12) 52 ?
O1 O1 1.514(12) 51 ?
O1 O1 1.514(12) 50 ?
O1' C5 1.311(11) . ?
O3 C1 1.49(3) . ?
O4 C1 1.16(4) . ?
O5 C3 1.239(10) . ?
O5 O5 1.61(3) 21 ?
O5 O5 1.61(3) 23 ?
C1 C2 1.509(10) . ?
C3 C4 1.500(10) . ?
C4 C4 1.95(7) 49_565 ?

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
O2 Cu1 O2 83.8(5) . 5 ?
O2 Cu1 O2 96.2(5) . 52 ?
O2 Cu1 O2 178.5(4) 5 52 ?
O2 Cu1 O2 178.5(4) . 54 ?
O2 Cu1 O2 96.2(5) 5 54 ?
O2 Cu1 O2 83.8(5) 52 54 ?
O2 Cu1 O1 104.3(3) . 52 ?
O2 Cu1 O1 104.3(3) 5 52 ?
O2 Cu1 O1 77.1(3) 52 52 ?
O2 Cu1 O1 77.1(3) 54 52 ?
O2 Cu1 O1 77.1(3) . . ?
O2 Cu1 O1 77.1(3) 5 . ?
O2 Cu1 O1 104.3(3) 52 . ?
O2 Cu1 O1 104.3(3) 54 . ?
O1 Cu1 O1 36.9(4) 52 . ?
O2 Cu1 O3 89.3(2) . 9 ?
O2 Cu1 O3 89.3(2) 5 9 ?
O2 Cu1 O3 89.3(2) 52 9 ?
O2 Cu1 O3 89.3(2) 54 9 ?
O1 Cu1 O3 161.6(2) 52 9 ?
O1 Cu1 O3 161.6(2) . 9 ?
O2 Cu1 Ni1 43.8(3) . . ?
O2 Cu1 Ni1 43.8(3) 5 . ?
O2 Cu1 Ni1 135.7(2) 52 . ?
O2 Cu1 Ni1 135.7(2) 54 . ?
O1 Cu1 Ni1 123.6(2) 52 . ?
O1 Cu1 Ni1 86.7(2) . . ?
O3 Cu1 Ni1 74.84(5) 9 . ?
O2 Cu1 Ni1 135.7(2) . 52 ?
O2 Cu1 Ni1 135.7(2) 5 52 ?
O2 Cu1 Ni1 43.8(3) 52 52 ?
O2 Cu1 Ni1 43.8(3) 54 52 ?
O1 Cu1 Ni1 86.7(2) 52 52 ?
O1 Cu1 Ni1 123.6(2) . 52 ?
O3 Cu1 Ni1 74.84(5) 9 52 ?
Ni1 Cu1 Ni1 149.68(10) . 52 ?
O4 Ni1 O4 87.8(5) 9 5 ?
O4 Ni1 O4 87.8(5) 9 . ?
O4 Ni1 O4 87.8(5) 5 . ?
O4 Ni1 O2 97.6(3) 9 . ?
O4 Ni1 O2 97.6(3) 5 . ?
O4 Ni1 O2 172.5(4) . . ?
O4 Ni1 O2 172.5(4) 9 9 ?
O4 Ni1 O2 97.6(3) 5 9 ?
O4 Ni1 O2 97.6(3) . 9 ?
O2 Ni1 O2 76.6(4) . 9 ?
O4 Ni1 O2 97.6(3) 9 5 ?
O4 Ni1 O2 172.5(4) 5 5 ?
O4 Ni1 O2 97.6(3) . 5 ?
O2 Ni1 O2 76.6(4) . 5 ?
O2 Ni1 O2 76.6(4) 9 5 ?
O4 Ni1 Cu1 87.2(3) 9 . ?
O4 Ni1 Cu1 135.8(2) 5 . ?
O4 Ni1 Cu1 135.8(2) . . ?
O2 Ni1 Cu1 39.97(13) . . ?
O2 Ni1 Cu1 85.3(3) 9 . ?
O2 Ni1 Cu1 39.97(12) 5 . ?
O4 Ni1 Cu1 135.8(2) 9 9 ?
O4 Ni1 Cu1 87.2(3) 5 9 ?
O4 Ni1 Cu1 135.8(2) . 9 ?
O2 Ni1 Cu1 39.97(12) . 9 ?
O2 Ni1 Cu1 39.97(12) 9 9 ?
O2 Ni1 Cu1 85.3(3) 5 9 ?
Cu1 Ni1 Cu1 66.97(8) . 9 ?
O4 Ni1 Cu1 135.8(2) 9 5 ?
O4 Ni1 Cu1 135.8(2) 5 5 ?
O4 Ni1 Cu1 87.2(3) . 5 ?
O2 Ni1 Cu1 85.3(3) . 5 ?
O2 Ni1 Cu1 39.97(13) 9 5 ?
O2 Ni1 Cu1 39.97(12) 5 5 ?
Cu1 Ni1 Cu1 66.97(8) . 5 ?
Cu1 Ni1 Cu1 66.97(8) 9 5 ?
O1' O1 O1' 100.6(8) . 5 ?
O1' O1 O1' 100.6(8) . 9 ?
O1' O1 O1' 100.6(8) 5 9 ?
O1' O1 C5 62.6(6) . . ?
O1' O1 C5 62.7(6) 5 . ?
O1' O1 C5 62.7(6) 9 . ?
O1' O1 O1 51.1(3) . 52 ?
O1' O1 O1 51.1(3) 5 52 ?
O1' O1 O1 117.4(6) 9 52 ?
C5 O1 O1 54.738(1) . 52 ?
O1' O1 O1 117.4(6) . 51 ?
O1' O1 O1 51.1(3) 5 51 ?
O1' O1 O1 51.1(3) 9 51 ?
C5 O1 O1 54.738(1) . 51 ?
O1 O1 O1 90.0 52 51 ?
O1' O1 O1 51.1(3) . 50 ?
O1' O1 O1 117.4(6) 5 50 ?
O1' O1 O1 51.1(3) 9 50 ?
C5 O1 O1 54.738(1) . 50 ?
O1 O1 O1 90.0 52 50 ?
O1 O1 O1 90.004(1) 51 50 ?
O1' O1 Cu1 171.1(8) . 5 ?
O1' O1 Cu1 85.1(4) 5 5 ?
O1' O1 Cu1 85.1(4) 9 5 ?
C5 O1 Cu1 126.3(2) . 5 ?
O1 O1 Cu1 132.13(6) 52 5 ?
O1 O1 Cu1 71.6(2) 51 5 ?
O1 O1 Cu1 132.13(6) 50 5 ?
O1' O1 Cu1 85.1(4) . 9 ?
O1' O1 Cu1 171.1(8) 5 9 ?
O1' O1 Cu1 85.1(4) 9 9 ?
C5 O1 Cu1 126.3(2) . 9 ?
O1 O1 Cu1 132.13(6) 52 9 ?
O1 O1 Cu1 132.13(6) 51 9 ?
O1 O1 Cu1 71.6(2) 50 9 ?
Cu1 O1 Cu1 88.5(3) 5 9 ?
O1' O1 Cu1 85.1(4) . . ?
O1' O1 Cu1 85.1(4) 5 . ?
O1' O1 Cu1 171.1(8) 9 . ?
C5 O1 Cu1 126.3(2) . . ?
O1 O1 Cu1 71.6(2) 52 . ?
O1 O1 Cu1 132.13(6) 51 . ?
O1 O1 Cu1 132.13(6) 50 . ?
Cu1 O1 Cu1 88.5(3) 5 . ?
Cu1 O1 Cu1 88.5(3) 9 . ?
O1 O1' O1 125.2(13) . 3 ?
O1 O1' O1 77.8(5) . 52 ?
O1 O1' O1 77.8(5) 3 52 ?
O1 O1' O1 77.8(5) . 50 ?
O1 O1' O1 77.8(5) 3 50 ?
O1 O1' O1 125.2(13) 52 50 ?
O1 O1' C5 62.6(6) . . ?
O1 O1' C5 62.6(6) 3 . ?
O1 O1' C5 62.6(6) 52 . ?
O1 O1' C5 62.6(6) 50 . ?
Cu1 O2 Cu1 117.2(4) . 9 ?
Cu1 O2 Ni1 96.2(3) . . ?
Cu1 O2 Ni1 96.2(3) 9 . ?
C1 O3 Cu1 122.5(14) . 5 ?
C1 O4 Ni1 134.4(18) . . ?
C3 O5 O5 49.4(6) . 21 ?
C3 O5 O5 49.4(6) . 23 ?
O5 O5 O5 90.000(2) 21 23 ?
O4 C1 O3 121(2) . . ?
O4 C1 C2 126(4) . . ?
O3 C1 C2 113(3) . . ?
O5 C3 O5 81.2(12) 21 3 ?
O5 C3 O5 134(3) 21 23 ?
O5 C3 O5 81.2(12) 3 23 ?
O5 C3 O5 81.2(12) 21 . ?
O5 C3 O5 134(3) 3 . ?
O5 C3 O5 81.2(12) 23 . ?
O5 C3 C4 113.1(16) 21 . ?
O5 C3 C4 113.1(16) 3 . ?
O5 C3 C4 113.1(16) 23 . ?
O5 C3 C4 113.1(16) . . ?
C3 C4 C4 180.0 . 49_565 ?
O1 C5 O1 180.0(13) . 49 ?
O1 C5 O1 70.529(1) . 52 ?
O1 C5 O1 109.471(1) 49 52 ?
O1 C5 O1 109.471(1) . 4 ?
O1 C5 O1 70.529(1) 49 4 ?
O1 C5 O1 180.0(13) 52 4 ?
O1 C5 O1 70.529(1) . 51 ?
O1 C5 O1 109.471(1) 49 51 ?
O1 C5 O1 109.5 52 51 ?
O1 C5 O1 70.5 4 51 ?
O1 C5 O1 109.471(1) . 3 ?
O1 C5 O1 70.529(1) 49 3 ?
O1 C5 O1 70.5 52 3 ?
O1 C5 O1 109.5 4 3 ?
O1 C5 O1 180.0(13) 51 3 ?
O1 C5 O1 109.5 . 2 ?
O1 C5 O1 70.529(1) 49 2 ?
O1 C5 O1 70.5 52 2 ?
O1 C5 O1 109.5 4 2 ?
O1 C5 O1 70.5 51 2 ?
O1 C5 O1 109.5 3 2 ?
O1 C5 O1 70.5 . 50 ?
O1 C5 O1 109.5 49 50 ?
O1 C5 O1 109.5 52 50 ?
O1 C5 O1 70.5 4 50 ?
O1 C5 O1 109.5 51 50 ?
O1 C5 O1 70.5 3 50 ?
O1 C5 O1 180.0(13) 2 50 ?
O1 C5 O1' 54.7 . . ?
O1 C5 O1' 125.3 49 . ?
O1 C5 O1' 54.7 52 . ?
O1 C5 O1' 125.3 4 . ?
O1 C5 O1' 125.3 51 . ?
O1 C5 O1' 54.7 3 . ?
O1 C5 O1' 125.3 2 . ?
O1 C5 O1' 54.7 50 . ?
O1 C5 O1' 125.3 . 57 ?
O1 C5 O1' 54.7 49 57 ?
O1 C5 O1' 54.7 52 57 ?
O1 C5 O1' 125.3 4 57 ?
O1 C5 O1' 125.3 51 57 ?
O1 C5 O1' 54.7 3 57 ?
O1 C5 O1' 54.7 2 57 ?
O1 C5 O1' 125.3 50 57 ?
O1' C5 O1' 90.0 . 57 ?
O1 C5 O1' 125.3 . 49 ?
O1 C5 O1' 54.7 49 49 ?
O1 C5 O1' 125.3 52 49 ?
O1 C5 O1' 54.7 4 49 ?
O1 C5 O1' 54.7 51 49 ?
O1 C5 O1' 125.3 3 49 ?
O1 C5 O1' 54.7 2 49 ?
O1 C5 O1' 125.3 50 49 ?
O1' C5 O1' 180.0 . 49 ?
O1' C5 O1' 90.0 57 49 ?
O1 C5 O1' 54.7 . 5 ?
O1 C5 O1' 125.3 49 5 ?
O1 C5 O1' 54.7 52 5 ?
O1 C5 O1' 125.3 4 5 ?
O1 C5 O1' 54.7 51 5 ?
O1 C5 O1' 125.3 3 5 ?
O1 C5 O1' 54.7 2 5 ?
O1 C5 O1' 125.3 50 5 ?
O1' C5 O1' 90.0 . 5 ?
O1' C5 O1' 90.0 57 5 ?
O1' C5 O1' 90.0 49 5 ?

_refine_diff_density_max         2.534
_refine_diff_density_min         -1.871
_refine_diff_density_rms         0.218

####################################################################### 
# 
# 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_s4
_database_code_depnum_ccdc_archive 'CCDC 1840131'
loop_
_audit_author_name
_audit_author_address
'Feng Xu'
;Hunan University
China
;
_audit_update_record             
;
2022-04-25 deposited with the CCDC.	2023-04-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/1
_shelx_SHELXL_version_number     2019/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H94 Co4.90 Cu10.20 Ni4.90 O69'
_chemical_formula_weight         2795.60

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'
O O 0.0106 0.0060 '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'
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      cubic
_space_group_IT_number           229
_space_group_name_H-M_alt        'I m -3 m'
_space_group_name_Hall           '-I 4 2 3'

_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, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, z+1/2, -y+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z+1/2, x+1/2, y+1/2'
'z+1/2, x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z+1/2, x+1/2'
'-y+1/2, z+1/2, x+1/2'
'y+1/2, z+1/2, -x+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'z+1/2, y+1/2, x+1/2'

_cell_length_a                   17.2801(2)
_cell_length_b                   17.2801(2)
_cell_length_c                   17.2801(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5159.87(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1906
_cell_measurement_theta_min      2.89
_cell_measurement_theta_max      25.86

_exptl_crystal_description       block
_exptl_crystal_colour            'clear  green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_F_000             2795
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.380
_exptl_absorpt_coefficient_mu    3.781
_shelx_estimated_absorpt_T_min   0.293
_shelx_estimated_absorpt_T_max   0.328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2932
_exptl_absorpt_correction_T_max  0.3276
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6459
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.357
_diffrn_reflns_theta_max         24.990
_diffrn_reflns_theta_full        24.990
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             487
_reflns_number_gt                421
_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    ?
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1997P)²+33.7110P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         487
_refine_ls_number_parameters     55
_refine_ls_number_restraints     240
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0743
_refine_ls_wR_factor_ref         0.2613
_refine_ls_wR_factor_gt          0.2489
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.006
_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
Cu1 Cu 0.000000 0.13717(7) 0.13717(7) 0.0317(9) Uani 0.8502 4 d S TU P . .
Ni1 Ni 0.000000 0.13717(7) 0.13717(7) 0.0317(9) Uani 0.1498 4 d S TU P . .
Ni2 Ni 0.16888(8) 0.16888(8) 0.16888(8) 0.0451(10) Uani 0.3877 6 d S TU P . .
Co1 Co 0.16888(8) 0.16888(8) 0.16888(8) 0.0451(10) Uani 0.6124 6 d S TU P . .
O1 O 0.0438(15) 0.0438(15) 0.0438(15) 0.040(4) Uani 0.25 6 d S TU P . .
O1' O 0.000000 0.083(5) 0.000000 0.038(5) Uani 0.1666 8 d S TU P . .
O2 O 0.0846(3) 0.1914(4) 0.0846(3) 0.0379(16) Uani 1 2 d S TU P . .
H2 H 0.076089 0.239205 0.076081 0.045 Uiso 1 2 d R U P . .
O3 O 0.2363(6) 0.000000 0.2363(6) 0.105(5) Uani 1 4 d S TU P . .
H3 H 0.261442 -0.032028 0.262884 0.126 Uiso 0.0417 2 calc R U P . .
O4 O 0.2477(4) 0.1335(6) 0.2477(4) 0.085(3) Uani 1 2 d S TU P . .
H4B H 0.232045 0.158760 0.288300 0.102 Uiso 0.25 1 d R U P A 2
H4C H 0.286975 0.158760 0.233370 0.102 Uiso 0.25 1 d R U P A 2
O5 O 0.067(2) 0.3314(17) 0.000000 0.055(6) Uani 0.25 2 d S TU P B 1
C1 C 0.2589(13) 0.080(2) 0.2589(13) 0.083(5) Uani 0.5 2 d S TU P . .
C2 C 0.3410(15) 0.074(3) 0.3410(15) 0.115(8) Uani 0.5 2 d S TU P . .
H2B H 0.358632 0.124280 0.339826 0.173 Uiso 0.25 1 d R U P . .
H2C H 0.319642 0.046160 0.365430 0.173 Uiso 0.25 1 d R U P . .
H2D H 0.383912 0.046160 0.301160 0.173 Uiso 0.25 1 d R U P . .
C3 C 0.000000 0.358(3) 0.000000 0.062(7) Uani 0.5 8 d S TU P B 1
C4 C 0.000000 0.432(3) 0.000000 0.076(9) Uani 0.5 8 d S TU P B 1
H4D H -0.052480 0.450355 0.000000 0.114 Uiso 0.125 2 d R U P B 1
H4E H 0.026240 0.450355 0.045450 0.114 Uiso 0.0625 1 d R U P B 1
H4F H 0.026240 0.450355 -0.045450 0.114 Uiso 0.0625 1 d R U P B 1
C5 C 0.000000 0.000000 0.000000 0.031(5) Uani 1 48 d S TU P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O2 1.960(3) 54 ?
Cu1 O2 1.960(3) 5 ?
Cu1 O2 1.960(3) 52 ?
Cu1 O2 1.960(3) . ?
Cu1 O1 2.40(3) 52 ?
Cu1 O1 2.40(3) . ?
Cu1 Ni2 3.0194(18) 52 ?
Cu1 Ni2 3.0194(18) . ?
Ni2 O4 2.020(11) 9 ?
Ni2 O4 2.020(11) 5 ?
Ni2 O4 2.020(11) . ?
Ni2 O2 2.095(8) . ?
Ni2 O2 2.095(8) 9 ?
Ni2 O2 2.095(8) 5 ?
O1 O1' 1.26(5) . ?
O1 O1' 1.26(5) 9 ?
O1 O1' 1.26(5) 5 ?
O1 C5 1.31(5) . ?
O1 O1 1.51(5) 52 ?
O1 O1 1.51(5) 51 ?
O1 O1 1.51(5) 50 ?
O1' C5 1.43(8) . ?
O2 H2 0.8518 . ?
O3 C1 1.49(3) . ?
O3 H3 0.8400 . ?
O3 H3 0.8400 51 ?
O4 C1 0.96(3) . ?
O4 H4B 0.8700 . ?
O4 H4C 0.8446 . ?
O5 C3 1.24(4) . ?
O5 O5 1.63(6) 21 ?
O5 O5 1.63(6) 23 ?
C1 C2 2.01(5) . ?
C2 C2 2.57(10) 51 ?
C2 H2B 0.9127 . ?
C2 H2C 0.7443 . ?
C2 H2D 1.1240 . ?
C3 C4 1.27(8) . ?
C4 C4 2.36(12) 49_565 ?
C4 H4D 0.9618 . ?
C4 H4E 0.9619 . ?
C4 H4F 0.9619 . ?
C4 H4D 0.9619 3 ?
C4 H4D 0.9619 21 ?
C4 H4D 0.9619 23 ?
C4 H4E 0.9618 3 ?
C4 H4E 0.9618 52 ?
C4 H4E 0.9618 21 ?
C4 H4E 0.9618 70 ?
C4 H4E 0.9618 23 ?
C4 H4E 0.9618 72 ?

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
O2 Cu1 O2 96.5(4) 54 5 ?
O2 Cu1 O2 83.5(4) 54 52 ?
O2 Cu1 O2 178.8(3) 5 52 ?
O2 Cu1 O2 178.8(3) 54 . ?
O2 Cu1 O2 83.5(4) 5 . ?
O2 Cu1 O2 96.5(4) 52 . ?
O2 Cu1 O1 77.0(7) 54 52 ?
O2 Cu1 O1 104.2(7) 5 52 ?
O2 Cu1 O1 77.0(7) 52 52 ?
O2 Cu1 O1 104.2(7) . 52 ?
O2 Cu1 O1 104.2(7) 54 . ?
O2 Cu1 O1 77.0(7) 5 . ?
O2 Cu1 O1 104.2(7) 52 . ?
O2 Cu1 O1 77.0(7) . . ?
O1 Cu1 O1 36.7(18) 52 . ?
O2 Cu1 Ni2 43.6(2) 54 52 ?
O2 Cu1 Ni2 135.9(2) 5 52 ?
O2 Cu1 Ni2 43.6(2) 52 52 ?
O2 Cu1 Ni2 135.9(2) . 52 ?
O1 Cu1 Ni2 86.5(9) 52 52 ?
O1 Cu1 Ni2 123.2(9) . 52 ?
O2 Cu1 Ni2 135.9(2) 54 . ?
O2 Cu1 Ni2 43.6(2) 5 . ?
O2 Cu1 Ni2 135.9(2) 52 . ?
O2 Cu1 Ni2 43.6(2) . . ?
O1 Cu1 Ni2 123.2(9) 52 . ?
O1 Cu1 Ni2 86.5(9) . . ?
Ni2 Cu1 Ni2 150.26(8) 52 . ?
O4 Ni2 O4 87.4(4) 9 5 ?
O4 Ni2 O4 87.4(4) 9 . ?
O4 Ni2 O4 87.4(4) 5 . ?
O4 Ni2 O2 97.6(3) 9 . ?
O4 Ni2 O2 97.6(3) 5 . ?
O4 Ni2 O2 173.1(4) . . ?
O4 Ni2 O2 173.1(4) 9 9 ?
O4 Ni2 O2 97.6(3) 5 9 ?
O4 Ni2 O2 97.6(3) . 9 ?
O2 Ni2 O2 77.0(3) . 9 ?
O4 Ni2 O2 97.6(3) 9 5 ?
O4 Ni2 O2 173.1(4) 5 5 ?
O4 Ni2 O2 97.6(3) . 5 ?
O2 Ni2 O2 77.0(3) . 5 ?
O2 Ni2 O2 77.0(3) 9 5 ?
O4 Ni2 Cu1 135.94(18) 9 5 ?
O4 Ni2 Cu1 135.94(18) 5 5 ?
O4 Ni2 Cu1 87.2(3) . 5 ?
O2 Ni2 Cu1 85.8(2) . 5 ?
O2 Ni2 Cu1 40.20(10) 9 5 ?
O2 Ni2 Cu1 40.20(10) 5 5 ?
O4 Ni2 Cu1 135.94(17) 9 9 ?
O4 Ni2 Cu1 87.2(3) 5 9 ?
O4 Ni2 Cu1 135.94(18) . 9 ?
O2 Ni2 Cu1 40.20(10) . 9 ?
O2 Ni2 Cu1 40.20(10) 9 9 ?
O2 Ni2 Cu1 85.8(2) 5 9 ?
Cu1 Ni2 Cu1 67.44(7) 5 9 ?
O4 Ni2 Cu1 87.2(3) 9 . ?
O4 Ni2 Cu1 135.94(17) 5 . ?
O4 Ni2 Cu1 135.94(18) . . ?
O2 Ni2 Cu1 40.20(10) . . ?
O2 Ni2 Cu1 85.8(2) 9 . ?
O2 Ni2 Cu1 40.20(10) 5 . ?
Cu1 Ni2 Cu1 67.44(7) 5 . ?
Cu1 Ni2 Cu1 67.44(7) 9 . ?
O1' O1 O1' 106(4) . 9 ?
O1' O1 O1' 106(4) . 5 ?
O1' O1 O1' 106(4) 9 5 ?
O1' O1 C5 67(4) . . ?
O1' O1 C5 67(4) 9 . ?
O1' O1 C5 67(4) 5 . ?
O1' O1 O1 53.2(18) . 52 ?
O1' O1 O1 122(4) 9 52 ?
O1' O1 O1 53.2(18) 5 52 ?
C5 O1 O1 54.738(4) . 52 ?
O1' O1 O1 122(4) . 51 ?
O1' O1 O1 53.2(18) 9 51 ?
O1' O1 O1 53.2(18) 5 51 ?
C5 O1 O1 54.738(3) . 51 ?
O1 O1 O1 90.004(2) 52 51 ?
O1' O1 O1 53.2(18) . 50 ?
O1' O1 O1 53.2(18) 9 50 ?
O1' O1 O1 122(4) 5 50 ?
C5 O1 O1 54.738(3) . 50 ?
O1 O1 O1 90.004(2) 52 50 ?
O1 O1 O1 90.004(2) 51 50 ?
O1' O1 Cu1 82(2) . . ?
O1' O1 Cu1 166(4) 9 . ?
O1' O1 Cu1 82(2) 5 . ?
C5 O1 Cu1 126.4(9) . . ?
O1 O1 Cu1 71.6(9) 52 . ?
O1 O1 Cu1 132.2(3) 51 . ?
O1 O1 Cu1 132.2(3) 50 . ?
O1' O1 Cu1 82(2) . 9 ?
O1' O1 Cu1 82(2) 9 9 ?
O1' O1 Cu1 166(4) 5 9 ?
C5 O1 Cu1 126.4(9) . 9 ?
O1 O1 Cu1 132.2(3) 52 9 ?
O1 O1 Cu1 132.2(3) 51 9 ?
O1 O1 Cu1 71.6(9) 50 9 ?
Cu1 O1 Cu1 88.4(13) . 9 ?
O1' O1 Cu1 166(4) . 5 ?
O1' O1 Cu1 82(2) 9 5 ?
O1' O1 Cu1 82(2) 5 5 ?
C5 O1 Cu1 126.4(9) . 5 ?
O1 O1 Cu1 132.2(3) 52 5 ?
O1 O1 Cu1 71.6(9) 51 5 ?
O1 O1 Cu1 132.2(3) 50 5 ?
Cu1 O1 Cu1 88.4(13) . 5 ?
Cu1 O1 Cu1 88.4(13) 9 5 ?
O1 O1' O1 116(8) . 3 ?
O1 O1' O1 74(4) . 52 ?
O1 O1' O1 74(4) 3 52 ?
O1 O1' O1 74(4) . 50 ?
O1 O1' O1 74(4) 3 50 ?
O1 O1' O1 116(8) 52 50 ?
O1 O1' C5 58(4) . . ?
O1 O1' C5 58(4) 3 . ?
O1 O1' C5 58(4) 52 . ?
O1 O1' C5 58(4) 50 . ?
Cu1 O2 Cu1 117.5(3) 9 . ?
Cu1 O2 Ni2 96.2(2) 9 . ?
Cu1 O2 Ni2 96.2(2) . . ?
Cu1 O2 H2 114.5 9 . ?
Cu1 O2 H2 114.5 . . ?
Ni2 O2 H2 114.9 . . ?
C1 O3 H3 109.5 . . ?
C1 O3 H3 27.0(15) . 51 ?
H3 O3 H3 82.4 . 51 ?
C1 O4 Ni2 124(2) . . ?
C1 O4 H4B 112.5 . . ?
Ni2 O4 H4B 100.5 . . ?
C1 O4 H4C 113.2 . . ?
Ni2 O4 H4C 100.8 . . ?
H4B O4 H4C 103.0 . . ?
C3 O5 O5 49.1(10) . 21 ?
C3 O5 O5 49.1(10) . 23 ?
O5 O5 O5 89.998(3) 21 23 ?
O4 C1 O3 142(3) . . ?
O4 C1 C2 109(3) . . ?
O3 C1 C2 109(3) . . ?
O4 C1 H3 169(4) . 51 ?
O3 C1 H3 27.3(12) . 51 ?
C2 C1 H3 82(3) . 51 ?
C1 C2 C2 92.7(18) . 51 ?
C1 C2 H2B 100.1 . . ?
C2 C2 H2B 160.5 51 . ?
C1 C2 H2C 94.6 . . ?
C2 C2 H2C 48.9 51 . ?
H2B C2 H2C 143.0 . . ?
C1 C2 H2D 93.0 . . ?
C2 C2 H2D 64.2 51 . ?
H2B C2 H2D 100.2 . . ?
H2C C2 H2D 112.8 . . ?
C1 C2 H3 23.5(11) . 51 ?
C2 C2 H3 69.2(15) 51 51 ?
H2B C2 H3 122.8 . 51 ?
H2C C2 H3 78.8 . 51 ?
H2D C2 H3 83.3 . 51 ?
O5 C3 O5 81.8(19) 21 3 ?
O5 C3 O5 136(5) 21 23 ?
O5 C3 O5 81.8(19) 3 23 ?
O5 C3 O5 81.8(19) 21 . ?
O5 C3 O5 136(5) 3 . ?
O5 C3 O5 81.8(19) 23 . ?
O5 C3 C4 112(3) 21 . ?
O5 C3 C4 112(3) 3 . ?
O5 C3 C4 112(3) 23 . ?
O5 C3 C4 112(3) . . ?
C3 C4 C4 180.0 . 49_565 ?
C3 C4 H4D 109.5 . . ?
C4 C4 H4D 70.5 49_565 . ?
C3 C4 H4E 109.5 . . ?
C4 C4 H4E 70.5 49_565 . ?
H4D C4 H4E 109.5 . . ?
C3 C4 H4F 109.5 . . ?
C4 C4 H4F 70.5 49_565 . ?
H4D C4 H4F 109.5 . . ?
H4E C4 H4F 109.5 . . ?
C3 C4 H4D 109.463(6) . 3 ?
C4 C4 H4D 70.537(3) 49_565 3 ?
H4D C4 H4D 141.1 . 3 ?
H4E C4 H4D 56.3 . 3 ?
H4F C4 H4D 56.3 . 3 ?
C3 C4 H4D 109.463(1) . 21 ?
C4 C4 H4D 70.5 49_565 21 ?
H4D C4 H4D 83.6 . 21 ?
H4E C4 H4D 28.2 . 21 ?
H4F C4 H4D 131.2 . 21 ?
H4D C4 H4D 83.6 3 21 ?
C3 C4 H4D 109.463(1) . 23 ?
C4 C4 H4D 70.537(1) 49_565 23 ?
H4D C4 H4D 83.6 . 23 ?
H4E C4 H4D 131.2 . 23 ?
H4F C4 H4D 28.2 . 23 ?
H4D C4 H4D 83.6 3 23 ?
H4D C4 H4D 141.1 21 23 ?
C3 C4 H4E 109.464(4) . 3 ?
C4 C4 H4E 70.536(1) 49_565 3 ?
H4D C4 H4E 56.3 . 3 ?
H4E C4 H4E 141.1 . 3 ?
H4F C4 H4E 56.3 . 3 ?
H4D C4 H4E 109.5 3 3 ?
H4D C4 H4E 131.2 21 3 ?
H4D C4 H4E 28.2 23 3 ?
C3 C4 H4E 109.464(3) . 52 ?
C4 C4 H4E 70.536(1) 49_565 52 ?
H4D C4 H4E 56.3 . 52 ?
H4E C4 H4E 56.3 . 52 ?
H4F C4 H4E 141.1 . 52 ?
H4D C4 H4E 109.5 3 52 ?
H4D C4 H4E 28.2 21 52 ?
H4D C4 H4E 131.2 23 52 ?
H4E C4 H4E 109.5 3 52 ?
C3 C4 H4E 109.464(6) . 21 ?
C4 C4 H4E 70.536(2) 49_565 21 ?
H4D C4 H4E 131.2 . 21 ?
H4E C4 H4E 83.6 . 21 ?
H4F C4 H4E 28.3 . 21 ?
H4D C4 H4E 28.2 3 21 ?
H4D C4 H4E 109.5 21 21 ?
H4D C4 H4E 56.3 23 21 ?
H4E C4 H4E 83.6 3 21 ?
H4E C4 H4E 131.2 52 21 ?
C3 C4 H4E 109.464(6) . 70 ?
C4 C4 H4E 70.536(1) 49_565 70 ?
H4D C4 H4E 28.2 . 70 ?
H4E C4 H4E 131.2 . 70 ?
H4F C4 H4E 83.6 . 70 ?
H4D C4 H4E 131.2 3 70 ?
H4D C4 H4E 109.5 21 70 ?
H4D C4 H4E 56.3 23 70 ?
H4E C4 H4E 28.3 3 70 ?
H4E C4 H4E 83.6 52 70 ?
H4E C4 H4E 109.5 21 70 ?
C3 C4 H4E 109.464(6) . 23 ?
C4 C4 H4E 70.536(3) 49_565 23 ?
H4D C4 H4E 28.2 . 23 ?
H4E C4 H4E 83.6 . 23 ?
H4F C4 H4E 131.2 . 23 ?
H4D C4 H4E 131.2 3 23 ?
H4D C4 H4E 56.3 21 23 ?
H4D C4 H4E 109.5 23 23 ?
H4E C4 H4E 83.6 3 23 ?
H4E C4 H4E 28.3 52 23 ?
H4E C4 H4E 141.1 21 23 ?
H4E C4 H4E 56.3 70 23 ?
C3 C4 H4E 109.464(6) . 72 ?
C4 C4 H4E 70.536(3) 49_565 72 ?
H4D C4 H4E 131.2 . 72 ?
H4E C4 H4E 28.3 . 72 ?
H4F C4 H4E 83.6 . 72 ?
H4D C4 H4E 28.2 3 72 ?
H4D C4 H4E 56.3 21 72 ?
H4D C4 H4E 109.5 23 72 ?
H4E C4 H4E 131.2 3 72 ?
H4E C4 H4E 83.6 52 72 ?
H4E C4 H4E 56.3 21 72 ?
H4E C4 H4E 141.1 70 72 ?
H4E C4 H4E 109.5 23 72 ?
O1' C5 O1' 90.0 . 57 ?
O1' C5 O1' 90.0 . 9 ?
O1' C5 O1' 180.0 57 9 ?
O1' C5 O1' 90.000(1) . 53 ?
O1' C5 O1' 90.000(1) 57 53 ?
O1' C5 O1' 90.000(1) 9 53 ?
O1' C5 O1' 90.000(1) . 5 ?
O1' C5 O1' 90.000(1) 57 5 ?
O1' C5 O1' 90.000(1) 9 5 ?
O1' C5 O1' 180.0 53 5 ?
O1' C5 O1' 180.0 . 49 ?
O1' C5 O1' 90.000(1) 57 49 ?
O1' C5 O1' 90.000(1) 9 49 ?
O1' C5 O1' 90.0 53 49 ?
O1' C5 O1' 90.0 5 49 ?
O1' C5 O1 54.736(1) . . ?
O1' C5 O1 125.265(2) 57 . ?
O1' C5 O1 54.735(2) 9 . ?
O1' C5 O1 125.264(2) 53 . ?
O1' C5 O1 54.736(2) 5 . ?
O1' C5 O1 125.264(1) 49 . ?
O1' C5 O1 125.264(1) . 49 ?
O1' C5 O1 54.735(2) 57 49 ?
O1' C5 O1 125.265(2) 9 49 ?
O1' C5 O1 54.736(2) 53 49 ?
O1' C5 O1 125.264(2) 5 49 ?
O1' C5 O1 54.736(2) 49 49 ?
O1 C5 O1 180(6) . 49 ?
O1' C5 O1 125.264(2) . 2 ?
O1' C5 O1 54.735(2) 57 2 ?
O1' C5 O1 125.265(2) 9 2 ?
O1' C5 O1 125.264(2) 53 2 ?
O1' C5 O1 54.736(2) 5 2 ?
O1' C5 O1 54.736(2) 49 2 ?
O1 C5 O1 109.5 . 2 ?
O1 C5 O1 70.529(1) 49 2 ?
O1' C5 O1 54.736(2) . 50 ?
O1' C5 O1 125.265(2) 57 50 ?
O1' C5 O1 54.735(2) 9 50 ?
O1' C5 O1 54.736(2) 53 50 ?
O1' C5 O1 125.264(2) 5 50 ?
O1' C5 O1 125.264(2) 49 50 ?
O1 C5 O1 70.5 . 50 ?
O1 C5 O1 109.471(1) 49 50 ?
O1 C5 O1 180(6) 2 50 ?
O1' C5 O1 125.264(2) . 51 ?
O1' C5 O1 125.265(2) 57 51 ?
O1' C5 O1 54.735(2) 9 51 ?
O1' C5 O1 125.264(2) 53 51 ?
O1' C5 O1 54.736(2) 5 51 ?
O1' C5 O1 54.736(2) 49 51 ?
O1 C5 O1 70.529(1) . 51 ?
O1 C5 O1 109.471(1) 49 51 ?
O1 C5 O1 70.529(1) 2 51 ?
O1 C5 O1 109.471(1) 50 51 ?
O1' C5 O1 54.736(2) . 3 ?
O1' C5 O1 54.735(2) 57 3 ?
O1' C5 O1 125.265(2) 9 3 ?
O1' C5 O1 54.736(2) 53 3 ?
O1' C5 O1 125.264(2) 5 3 ?
O1' C5 O1 125.264(2) 49 3 ?
O1 C5 O1 109.471(1) . 3 ?
O1 C5 O1 70.529(1) 49 3 ?
O1 C5 O1 109.471(1) 2 3 ?
O1 C5 O1 70.529(1) 50 3 ?
O1 C5 O1 180(6) 51 3 ?

_refine_diff_density_max         1.107
_refine_diff_density_min         -1.727
_refine_diff_density_rms         0.229

