# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_csp-ni-sk-02
_database_code_depnum_ccdc_archive 'CCDC 2226393'
loop_
_audit_author_name
_audit_author_address
'Chandra Sekhar Purohit'
;NISER Bhubaneswar
India
;
_audit_update_record             
;
2022-12-14 deposited with the CCDC.	2023-02-20 downloaded from the CCDC.
;
_audit_creation_date             2022-01-04
_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(C13 H14 N4 Ni O), C H4 O'
_chemical_formula_sum            'C27 H32 N8 Ni2 O3'
_chemical_formula_weight         634.02
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C54 H66 N16 Ni4 O6 '
_chemical_oxdiff_usercomment     'DARK PINK CUBOID'
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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6002(3)
_cell_length_b                   11.8988(4)
_cell_length_c                   13.1563(4)
_cell_angle_alpha                94.616(3)
_cell_angle_beta                 108.689(3)
_cell_angle_gamma                104.652(3)
_cell_volume                     1355.75(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11205
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.1080
_cell_measurement_theta_min      3.4890
_shelx_estimated_absorpt_T_max   0.847
_shelx_estimated_absorpt_T_min   0.698
_exptl_absorpt_coefficient_mu    1.435
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark pink'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plank
_exptl_crystal_F_000             660
_exptl_crystal_preparation       'As per the reaction scheme'
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.801
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24462
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.801
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.480
_diffrn_reflns_theta_min         3.321
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9967
_diffrn_measured_fraction_theta_max 0.8021
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -15.00  41.00   0.50    3.00    --    3.51-101.00 168.00  112
  2  ω    -15.00  33.00   0.50    3.00    --   -4.14-101.00 168.00   96
  3  ω      0.00  70.00   0.50    3.00    --    3.51  37.00 -60.00  140
  4  ω    -42.00  27.00   0.50    3.00    --    3.51 -77.00 120.00  138
  5  ω    -36.00  -5.00   0.50    3.00    --    3.51 -77.00 -30.00   62
  6  ω     -7.00  58.00   0.50    3.00    --    3.51  57.00 -90.00  130
  7  ω    -26.00  12.00   0.50    3.00    --   -4.14 -77.00  90.00   76
  8  ω    -10.00  19.00   0.50    3.00    --   -4.14 -99.00 -90.00   58
  9  ω    -14.00  13.00   0.50    3.00    --   -4.14  77.00  60.00   54
 10  ω    -40.00  19.00   0.50    3.00    --   -4.14 -77.00 -30.00  118
 11  ω     -6.00  50.00   0.50    3.00    --   -4.14  37.00 -90.00  112
 12  ω    -22.00   4.00   0.50    3.00    --   -4.14  77.00 -30.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0114752000
_diffrn_orient_matrix_UB_12      -0.0334583000
_diffrn_orient_matrix_UB_13      -0.0420928000
_diffrn_orient_matrix_UB_21      -0.0749574000
_diffrn_orient_matrix_UB_22      -0.0039704000
_diffrn_orient_matrix_UB_23      -0.0356710000
_diffrn_orient_matrix_UB_31      0.0302327000
_diffrn_orient_matrix_UB_32      0.0527533000
_diffrn_orient_matrix_UB_33      -0.0172888000
_diffrn_oxdiff_digest_frames     
;
01b8b549f67ba7851dbe397dacfc18e7e401148149e
;
_diffrn_oxdiff_digest_hkl        
;
01549ae8b597d021b2ca5bfd36049be12bc0ba
;
_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              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5089
_reflns_number_total             6616
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         6616
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0398
_refine_ls_restrained_S_all      1.045
_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)+(0.0402P)²+0.2715P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0935
_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, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C11(H11), C29(H29)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C30(H30A,H30B), C10(H10A,H10B), C28(H28A,H28B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C14(H14), C25(H25), C26(H26), C32(H32), C38(H38), C36(H36), C20(H20),
 C24(H24), C19(H19), C37(H37), C5(H5), C23(H23), C7(H7), C18(H18), C6(H6)
2.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C)
2.e Idealised tetrahedral OH refined as rotating group:
 O15(H15), O33(H33), O39(H39)
;
_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 0.16142(3) 0.59457(3) 0.10036(2) 0.01476(9) Uani 1 1 d . . . . .
Ni2 Ni 0.54161(3) 0.86842(3) 0.55683(2) 0.01448(9) Uani 1 1 d . . . . .
O15 O 0.6011(2) 0.69302(15) 0.35797(14) 0.0235(4) Uani 1 1 d . . . . .
H15 H 0.513560 0.644675 0.325343 0.035 Uiso 1 1 calc R U . . .
O33 O 0.3778(2) 0.48530(16) 0.31386(15) 0.0289(4) Uani 1 1 d . . . . .
H33 H 0.354842 0.464491 0.367367 0.043 Uiso 1 1 calc R U . . .
N9 N 0.4090(2) 0.83259(17) 0.40822(15) 0.0174(4) Uani 1 1 d . . . . .
N21 N 0.2514(2) 0.71347(17) 0.03344(15) 0.0161(4) Uani 1 1 d . . . . .
N34 N 0.0135(2) 0.66099(17) 0.12491(15) 0.0173(4) Uani 1 1 d . . . . .
N13 N 0.7237(2) 0.89606(17) 0.52189(15) 0.0162(4) Uani 1 1 d . . . . .
N27 N 0.3272(2) 0.53439(17) 0.09740(15) 0.0179(4) Uani 1 1 d . . . . .
O39 O 0.2636(2) 0.40817(18) 0.46710(16) 0.0358(5) Uani 1 1 d . . . . .
H39 H 0.302621 0.368221 0.511775 0.054 Uiso 1 1 calc R U . . .
N31 N 0.0779(2) 0.47287(17) 0.16764(16) 0.0191(4) Uani 1 1 d . . . . .
N16 N 0.6803(2) 0.90369(17) 0.70287(15) 0.0182(4) Uani 1 1 d . . . . .
N3 N 0.3556(2) 0.82846(18) 0.58496(17) 0.0198(4) Uani 1 1 d . . . . .
C17 C 0.8286(3) 0.9138(2) 0.70841(19) 0.0186(5) Uani 1 1 d . . . . .
C4 C 0.2277(3) 0.8005(2) 0.4908(2) 0.0212(5) Uani 1 1 d . . . . .
C8 C 0.2638(3) 0.8035(2) 0.3947(2) 0.0204(5) Uani 1 1 d . . . . .
H8 H 0.186202 0.785148 0.324361 0.025 Uiso 1 1 calc R U . . .
C14 C 0.8475(3) 0.9105(2) 0.60616(19) 0.0186(5) Uani 1 1 d . . . . .
H14 H 0.944881 0.918442 0.599326 0.022 Uiso 1 1 calc R U . . .
C25 C 0.2323(3) 0.8116(2) -0.00659(19) 0.0205(5) Uani 1 1 d . . . . .
H25 H 0.147397 0.840934 -0.011749 0.025 Uiso 1 1 calc R U . . .
C22 C 0.3888(3) 0.7032(2) 0.02735(19) 0.0190(5) Uani 1 1 d . . . . .
C12 C 0.7372(3) 0.8969(2) 0.41444(19) 0.0190(5) Uani 1 1 d . . . . .
H12A H 0.833804 0.879941 0.416482 0.023 Uiso 1 1 calc R U . . .
H12B H 0.742250 0.976217 0.395287 0.023 Uiso 1 1 calc R U . . .
C26 C 0.4259(3) 0.6034(2) 0.06480(19) 0.0194(5) Uani 1 1 d . . . . .
H26 H 0.518446 0.587376 0.066158 0.023 Uiso 1 1 calc R U . . .
C11 C 0.6018(3) 0.8059(2) 0.32817(19) 0.0195(5) Uani 1 1 d . . . . .
H11 H 0.620926 0.806249 0.257813 0.023 Uiso 1 1 calc R U . . .
C32 C -0.0320(3) 0.4891(2) 0.19843(19) 0.0209(5) Uani 1 1 d . . . . .
H32 H -0.082508 0.434040 0.233149 0.025 Uiso 1 1 calc R U . . .
C35 C -0.0725(3) 0.5935(2) 0.17742(19) 0.0209(5) Uani 1 1 d . . . . .
C38 C -0.0256(3) 0.7626(2) 0.1217(2) 0.0234(5) Uani 1 1 d . . . . .
H38 H 0.016274 0.826509 0.090886 0.028 Uiso 1 1 calc R U . . .
C30 C 0.1263(3) 0.3674(2) 0.1871(2) 0.0233(5) Uani 1 1 d . . . . .
H30A H 0.076640 0.307539 0.119532 0.028 Uiso 1 1 calc R U . . .
H30B H 0.091277 0.334105 0.244340 0.028 Uiso 1 1 calc R U . . .
C10 C 0.4525(3) 0.8353(2) 0.31138(19) 0.0230(5) Uani 1 1 d . . . . .
H10A H 0.463067 0.914847 0.291839 0.028 Uiso 1 1 calc R U . . .
H10B H 0.369383 0.778051 0.249676 0.028 Uiso 1 1 calc R U . . .
C28 C 0.3574(3) 0.4259(2) 0.1315(2) 0.0247(6) Uani 1 1 d . . . . .
H28A H 0.469580 0.436720 0.156067 0.030 Uiso 1 1 calc R U . . .
H28B H 0.306551 0.360417 0.068236 0.030 Uiso 1 1 calc R U . . .
C36 C -0.1654(3) 0.6527(2) 0.2057(2) 0.0254(6) Uani 1 1 d . . . . .
H36 H -0.235118 0.625500 0.242049 0.030 Uiso 1 1 calc R U . . .
C20 C 0.6837(3) 0.9141(2) 0.80727(19) 0.0236(5) Uani 1 1 d . . . . .
H20 H 0.597203 0.911430 0.828283 0.028 Uiso 1 1 calc R U . . .
C24 C 0.3544(3) 0.8641(2) -0.0394(2) 0.0250(6) Uani 1 1 d . . . . .
H24 H 0.366155 0.933116 -0.071368 0.030 Uiso 1 1 calc R U . . .
C19 C 0.8322(3) 0.9291(2) 0.8790(2) 0.0270(6) Uani 1 1 d . . . . .
H19 H 0.864329 0.938040 0.956212 0.032 Uiso 1 1 calc R U . . .
C37 C -0.1356(3) 0.7603(2) 0.1698(2) 0.0269(6) Uani 1 1 d . . . . .
H37 H -0.181899 0.820861 0.176860 0.032 Uiso 1 1 calc R U . . .
C5 C 0.0936(3) 0.7655(2) 0.5145(2) 0.0284(6) Uani 1 1 d . . . . .
H5 H -0.009203 0.741737 0.464175 0.034 Uiso 1 1 calc R U . . .
C23 C 0.4556(3) 0.7963(2) -0.0163(2) 0.0259(6) Uani 1 1 d . . . . .
H23 H 0.550828 0.810445 -0.027956 0.031 Uiso 1 1 calc R U . . .
C7 C 0.3013(3) 0.8098(3) 0.6679(2) 0.0294(6) Uani 1 1 d . . . . .
H7 H 0.363460 0.820731 0.742601 0.035 Uiso 1 1 calc R U . . .
C18 C 0.9247(3) 0.9287(2) 0.8168(2) 0.0245(6) Uani 1 1 d . . . . .
H18 H 1.031833 0.936901 0.842681 0.029 Uiso 1 1 calc R U . . .
C29 C 0.3000(3) 0.3932(2) 0.2225(2) 0.0262(6) Uani 1 1 d . . . . .
H29 H 0.326590 0.320172 0.243288 0.031 Uiso 1 1 calc R U . . .
C6 C 0.1411(3) 0.7723(2) 0.6267(3) 0.0314(7) Uani 1 1 d . . . . .
H6 H 0.075856 0.754575 0.668099 0.038 Uiso 1 1 calc R U . . .
C40 C 0.2358(4) 0.5029(3) 0.5238(3) 0.0446(8) Uani 1 1 d . . . . .
H40A H 0.209906 0.558243 0.474762 0.067 Uiso 1 1 calc R U . . .
H40B H 0.328441 0.543998 0.586863 0.067 Uiso 1 1 calc R U . . .
H40C H 0.150099 0.471324 0.548580 0.067 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 N21 1.8952(18) . ?
Ni1 N34 1.888(2) . ?
Ni1 N27 1.913(2) . ?
Ni1 N31 1.8967(19) . ?
Ni2 N9 1.9030(19) . ?
Ni2 N13 1.904(2) . ?
Ni2 N16 1.8944(19) . ?
Ni2 N3 1.891(2) . ?
O15 H15 0.8400 . ?
O15 C11 1.428(3) . ?
O33 H33 0.8400 . ?
O33 C29 1.416(3) . ?
N9 C8 1.297(3) . ?
N9 C10 1.463(3) . ?
N21 C25 1.349(3) . ?
N21 C22 1.382(3) . ?
N34 C35 1.387(3) . ?
N34 C38 1.354(3) . ?
N13 C14 1.300(3) . ?
N13 C12 1.461(3) . ?
N27 C26 1.296(3) . ?
N27 C28 1.467(3) . ?
O39 H39 0.8400 . ?
O39 C40 1.429(4) . ?
N31 C32 1.296(3) . ?
N31 C30 1.458(3) . ?
N16 C17 1.376(3) . ?
N16 C20 1.358(3) . ?
N3 C4 1.380(3) . ?
N3 C7 1.363(3) . ?
C17 C14 1.412(3) . ?
C17 C18 1.396(3) . ?
C4 C8 1.415(4) . ?
C4 C5 1.391(4) . ?
C8 H8 0.9500 . ?
C14 H14 0.9500 . ?
C25 H25 0.9500 . ?
C25 C24 1.396(3) . ?
C22 C26 1.406(3) . ?
C22 C23 1.396(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C11 1.515(3) . ?
C26 H26 0.9500 . ?
C11 H11 1.0000 . ?
C11 C10 1.513(4) . ?
C32 H32 0.9500 . ?
C32 C35 1.415(4) . ?
C35 C36 1.384(4) . ?
C38 H38 0.9500 . ?
C38 C37 1.391(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C29 1.521(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.509(4) . ?
C36 H36 0.9500 . ?
C36 C37 1.394(4) . ?
C20 H20 0.9500 . ?
C20 C19 1.392(4) . ?
C24 H24 0.9500 . ?
C24 C23 1.391(4) . ?
C19 H19 0.9500 . ?
C19 C18 1.388(4) . ?
C37 H37 0.9500 . ?
C5 H5 0.9500 . ?
C5 C6 1.388(4) . ?
C23 H23 0.9500 . ?
C7 H7 0.9500 . ?
C7 C6 1.393(4) . ?
C18 H18 0.9500 . ?
C29 H29 1.0000 . ?
C6 H6 0.9500 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 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
N21 Ni1 N27 83.74(8) . . ?
N21 Ni1 N31 177.70(9) . . ?
N34 Ni1 N21 98.47(8) . . ?
N34 Ni1 N27 171.80(8) . . ?
N34 Ni1 N31 83.79(9) . . ?
N31 Ni1 N27 93.97(9) . . ?
N9 Ni2 N13 93.62(8) . . ?
N16 Ni2 N9 177.67(9) . . ?
N16 Ni2 N13 84.10(9) . . ?
N3 Ni2 N9 83.98(9) . . ?
N3 Ni2 N13 175.35(9) . . ?
N3 Ni2 N16 98.26(9) . . ?
C11 O15 H15 109.5 . . ?
C29 O33 H33 109.5 . . ?
C8 N9 Ni2 113.95(17) . . ?
C8 N9 C10 118.3(2) . . ?
C10 N9 Ni2 127.77(16) . . ?
C25 N21 Ni1 141.64(17) . . ?
C25 N21 C22 106.11(19) . . ?
C22 N21 Ni1 112.12(16) . . ?
C35 N34 Ni1 112.79(16) . . ?
C38 N34 Ni1 140.58(17) . . ?
C38 N34 C35 105.8(2) . . ?
C14 N13 Ni2 113.31(16) . . ?
C14 N13 C12 118.6(2) . . ?
C12 N13 Ni2 128.03(16) . . ?
C26 N27 Ni1 113.44(17) . . ?
C26 N27 C28 118.2(2) . . ?
C28 N27 Ni1 128.29(16) . . ?
C40 O39 H39 109.5 . . ?
C32 N31 Ni1 114.38(17) . . ?
C32 N31 C30 119.3(2) . . ?
C30 N31 Ni1 126.36(16) . . ?
C17 N16 Ni2 111.76(15) . . ?
C20 N16 Ni2 141.64(19) . . ?
C20 N16 C17 106.3(2) . . ?
C4 N3 Ni2 112.37(16) . . ?
C7 N3 Ni2 141.32(19) . . ?
C7 N3 C4 106.1(2) . . ?
N16 C17 C14 113.9(2) . . ?
N16 C17 C18 110.1(2) . . ?
C18 C17 C14 136.0(2) . . ?
N3 C4 C8 113.5(2) . . ?
N3 C4 C5 110.5(2) . . ?
C5 C4 C8 135.6(3) . . ?
N9 C8 C4 116.1(2) . . ?
N9 C8 H8 121.9 . . ?
C4 C8 H8 121.9 . . ?
N13 C14 C17 116.2(2) . . ?
N13 C14 H14 121.9 . . ?
C17 C14 H14 121.9 . . ?
N21 C25 H25 124.7 . . ?
N21 C25 C24 110.7(2) . . ?
C24 C25 H25 124.7 . . ?
N21 C22 C26 113.7(2) . . ?
N21 C22 C23 110.3(2) . . ?
C23 C22 C26 136.0(2) . . ?
N13 C12 H12A 109.4 . . ?
N13 C12 H12B 109.4 . . ?
N13 C12 C11 111.18(19) . . ?
H12A C12 H12B 108.0 . . ?
C11 C12 H12A 109.4 . . ?
C11 C12 H12B 109.4 . . ?
N27 C26 C22 116.5(2) . . ?
N27 C26 H26 121.8 . . ?
C22 C26 H26 121.8 . . ?
O15 C11 C12 107.38(19) . . ?
O15 C11 H11 107.6 . . ?
O15 C11 C10 114.3(2) . . ?
C12 C11 H11 107.6 . . ?
C10 C11 C12 112.0(2) . . ?
C10 C11 H11 107.6 . . ?
N31 C32 H32 121.9 . . ?
N31 C32 C35 116.2(2) . . ?
C35 C32 H32 121.9 . . ?
N34 C35 C32 112.8(2) . . ?
C36 C35 N34 110.6(2) . . ?
C36 C35 C32 136.2(2) . . ?
N34 C38 H38 124.8 . . ?
N34 C38 C37 110.4(2) . . ?
C37 C38 H38 124.8 . . ?
N31 C30 H30A 109.2 . . ?
N31 C30 H30B 109.2 . . ?
N31 C30 C29 112.2(2) . . ?
H30A C30 H30B 107.9 . . ?
C29 C30 H30A 109.2 . . ?
C29 C30 H30B 109.2 . . ?
N9 C10 C11 112.6(2) . . ?
N9 C10 H10A 109.1 . . ?
N9 C10 H10B 109.1 . . ?
C11 C10 H10A 109.1 . . ?
C11 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
N27 C28 H28A 109.2 . . ?
N27 C28 H28B 109.2 . . ?
N27 C28 C29 112.1(2) . . ?
H28A C28 H28B 107.9 . . ?
C29 C28 H28A 109.2 . . ?
C29 C28 H28B 109.2 . . ?
C35 C36 H36 127.0 . . ?
C35 C36 C37 105.9(2) . . ?
C37 C36 H36 127.0 . . ?
N16 C20 H20 124.9 . . ?
N16 C20 C19 110.2(2) . . ?
C19 C20 H20 124.9 . . ?
C25 C24 H24 126.5 . . ?
C23 C24 C25 107.0(2) . . ?
C23 C24 H24 126.5 . . ?
C20 C19 H19 126.4 . . ?
C18 C19 C20 107.2(2) . . ?
C18 C19 H19 126.4 . . ?
C38 C37 C36 107.3(2) . . ?
C38 C37 H37 126.4 . . ?
C36 C37 H37 126.4 . . ?
C4 C5 H5 127.1 . . ?
C6 C5 C4 105.8(2) . . ?
C6 C5 H5 127.1 . . ?
C22 C23 H23 127.0 . . ?
C24 C23 C22 105.9(2) . . ?
C24 C23 H23 127.0 . . ?
N3 C7 H7 125.1 . . ?
N3 C7 C6 109.7(3) . . ?
C6 C7 H7 125.1 . . ?
C17 C18 H18 126.9 . . ?
C19 C18 C17 106.2(2) . . ?
C19 C18 H18 126.9 . . ?
O33 C29 C30 111.7(2) . . ?
O33 C29 C28 108.7(2) . . ?
O33 C29 H29 108.2 . . ?
C30 C29 H29 108.2 . . ?
C28 C29 C30 111.7(2) . . ?
C28 C29 H29 108.2 . . ?
C5 C6 C7 107.8(2) . . ?
C5 C6 H6 126.1 . . ?
C7 C6 H6 126.1 . . ?
O39 C40 H40A 109.5 . . ?
O39 C40 H40B 109.5 . . ?
O39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 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 N21 C25 C24 175.8(2) . . . . ?
Ni1 N21 C22 C26 4.1(3) . . . . ?
Ni1 N21 C22 C23 -176.44(17) . . . . ?
Ni1 N34 C35 C32 -1.3(3) . . . . ?
Ni1 N34 C35 C36 172.53(17) . . . . ?
Ni1 N34 C38 C37 -169.0(2) . . . . ?
Ni1 N27 C26 C22 -6.0(3) . . . . ?
Ni1 N27 C28 C29 -30.3(3) . . . . ?
Ni1 N31 C32 C35 0.1(3) . . . . ?
Ni1 N31 C30 C29 39.3(3) . . . . ?
Ni2 N9 C8 C4 -1.3(3) . . . . ?
Ni2 N9 C10 C11 30.9(3) . . . . ?
Ni2 N13 C14 C17 -5.3(3) . . . . ?
Ni2 N13 C12 C11 -35.3(3) . . . . ?
Ni2 N16 C17 C14 7.4(2) . . . . ?
Ni2 N16 C17 C18 -174.44(16) . . . . ?
Ni2 N16 C20 C19 172.3(2) . . . . ?
Ni2 N3 C4 C8 2.3(3) . . . . ?
Ni2 N3 C4 C5 176.73(17) . . . . ?
Ni2 N3 C7 C6 -175.3(2) . . . . ?
O15 C11 C10 N9 58.2(3) . . . . ?
N9 Ni2 N3 C4 -2.37(17) . . . . ?
N9 Ni2 N3 C7 171.8(3) . . . . ?
N21 Ni1 N34 C35 -178.55(15) . . . . ?
N21 Ni1 N34 C38 -10.7(3) . . . . ?
N21 C25 C24 C23 -1.3(3) . . . . ?
N21 C22 C26 N27 1.3(3) . . . . ?
N21 C22 C23 C24 -1.1(3) . . . . ?
N34 Ni1 N21 C25 -8.7(3) . . . . ?
N34 Ni1 N21 C22 166.34(16) . . . . ?
N34 Ni1 N31 C32 -0.63(17) . . . . ?
N34 Ni1 N31 C30 179.8(2) . . . . ?
N34 C35 C36 C37 -0.2(3) . . . . ?
N34 C38 C37 C36 0.6(3) . . . . ?
N13 Ni2 N16 C17 -8.12(16) . . . . ?
N13 Ni2 N16 C20 179.0(3) . . . . ?
N13 C12 C11 O15 -60.2(2) . . . . ?
N13 C12 C11 C10 66.0(3) . . . . ?
N27 Ni1 N21 C25 179.3(3) . . . . ?
N27 Ni1 N21 C22 -5.70(16) . . . . ?
N27 Ni1 N31 C32 171.45(17) . . . . ?
N27 Ni1 N31 C30 -8.2(2) . . . . ?
N27 C28 C29 O33 -61.1(3) . . . . ?
N27 C28 C29 C30 62.6(3) . . . . ?
N31 Ni1 N34 C35 1.06(16) . . . . ?
N31 Ni1 N34 C38 168.9(3) . . . . ?
N31 C32 C35 N34 0.8(3) . . . . ?
N31 C32 C35 C36 -170.8(3) . . . . ?
N31 C30 C29 O33 54.1(3) . . . . ?
N31 C30 C29 C28 -67.9(3) . . . . ?
N16 Ni2 N3 C4 178.28(16) . . . . ?
N16 Ni2 N3 C7 -7.6(3) . . . . ?
N16 C17 C14 N13 -1.4(3) . . . . ?
N16 C17 C18 C19 -0.8(3) . . . . ?
N16 C20 C19 C18 0.3(3) . . . . ?
N3 Ni2 N16 C17 167.84(16) . . . . ?
N3 Ni2 N16 C20 -5.0(3) . . . . ?
N3 C4 C8 N9 -0.7(3) . . . . ?
N3 C4 C5 C6 0.0(3) . . . . ?
N3 C7 C6 C5 1.0(3) . . . . ?
C17 N16 C20 C19 -0.8(3) . . . . ?
C4 N3 C7 C6 -0.9(3) . . . . ?
C4 C5 C6 C7 -0.6(3) . . . . ?
C8 N9 C10 C11 -149.5(2) . . . . ?
C8 C4 C5 C6 172.7(3) . . . . ?
C14 N13 C12 C11 141.4(2) . . . . ?
C14 C17 C18 C19 176.8(3) . . . . ?
C25 N21 C22 C26 -179.1(2) . . . . ?
C25 N21 C22 C23 0.3(3) . . . . ?
C25 C24 C23 C22 1.4(3) . . . . ?
C22 N21 C25 C24 0.6(3) . . . . ?
C12 N13 C14 C17 177.5(2) . . . . ?
C12 C11 C10 N9 -64.2(3) . . . . ?
C26 N27 C28 C29 146.5(2) . . . . ?
C26 C22 C23 C24 178.2(3) . . . . ?
C32 N31 C30 C29 -140.3(2) . . . . ?
C32 C35 C36 C37 171.6(3) . . . . ?
C35 N34 C38 C37 -0.7(3) . . . . ?
C35 C36 C37 C38 -0.3(3) . . . . ?
C38 N34 C35 C32 -173.3(2) . . . . ?
C38 N34 C35 C36 0.5(3) . . . . ?
C30 N31 C32 C35 179.7(2) . . . . ?
C10 N9 C8 C4 179.1(2) . . . . ?
C28 N27 C26 C22 176.7(2) . . . . ?
C20 N16 C17 C14 -177.2(2) . . . . ?
C20 N16 C17 C18 1.0(3) . . . . ?
C20 C19 C18 C17 0.3(3) . . . . ?
C5 C4 C8 N9 -173.2(3) . . . . ?
C23 C22 C26 N27 -178.0(3) . . . . ?
C7 N3 C4 C8 -173.9(2) . . . . ?
C7 N3 C4 C5 0.5(3) . . . . ?
C18 C17 C14 N13 -178.9(3) . . . . ?

_olex2_exptl_crystal_mounting_method 'Mounted on the loop'
_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 1.373
_oxdiff_exptl_absorpt_empirical_full_min 0.657
####################################################################### 
# 
# 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_cucl2sk02dcmmeoh_rt
_database_code_depnum_ccdc_archive 'CCDC 2226394'
loop_
_audit_author_name
_audit_author_address
'Chandra Sekhar Purohit'
;NISER Bhubaneswar
India
;
_audit_update_record             
;
2022-12-14 deposited with the CCDC.	2023-02-20 downloaded from the CCDC.
;
_audit_creation_date             2021-04-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '3(C13 H14 Cu N4 O), C13 H15 Cu N4 O'
_chemical_formula_sum            'C52 H57 Cu4 N16 O4'
_chemical_formula_weight         1224.29
_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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   16.3850(5)
_cell_length_b                   18.8935(7)
_cell_length_c                   18.0821(7)
_cell_angle_alpha                90
_cell_angle_beta                 92.669(3)
_cell_angle_gamma                90
_cell_volume                     5591.6(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8126
_cell_measurement_temperature    298.0(2)
_cell_measurement_theta_max      31.3440
_cell_measurement_theta_min      2.7080
_shelx_estimated_absorpt_T_max   0.746
_shelx_estimated_absorpt_T_min   0.574
_exptl_absorpt_coefficient_mu    1.559
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic yellowish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2516
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            68110
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.489
_diffrn_ambient_temperature      298.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -69.00 118.20   0.30   30.00    --   29.89  54.00-180.00  624
  2  ω    -69.00 118.20   0.30   30.00    --   29.89  54.00 150.00  624
  3  ω    -69.00  -3.90   0.30   30.00    --   29.89  54.00 -90.00  217
  4  ω    -69.00 118.20   0.30   30.00    --   29.89  54.00   0.00  624
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0157617000
_diffrn_orient_matrix_UB_12      -0.0144547000
_diffrn_orient_matrix_UB_13      0.0339558000
_diffrn_orient_matrix_UB_21      0.0020623000
_diffrn_orient_matrix_UB_22      0.0344389000
_diffrn_orient_matrix_UB_23      0.0156043000
_diffrn_orient_matrix_UB_31      -0.0402899000
_diffrn_orient_matrix_UB_32      -0.0038622000
_diffrn_orient_matrix_UB_33      0.0121157000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7820
_reflns_number_total             12794
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         12794
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0520
_refine_ls_restrained_S_all      1.011
_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)+(0.0692P)²+2.3441P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1573
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H1 of O1, H3 of O3, All C(H,H) groups
 At 1.5 times of:
  H2 of O2, H4 of O4
2.a Rotating group:
 O3(H3)
2.b Ternary CH refined with riding coordinates:
 C28(H28), C7(H7), C15(H15), C51(H51)
2.c Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C29(H29A,H29B), C0AA(H0AA,H0AB), C52(H52A,H52B), C14(H14A,
 H14B), C16(H16A,H16B), C50(H50A,H50B), C19(H19A,H19B), C8(H8A,H8B)
2.d Aromatic/amide H refined with riding coordinates:
 C30(H30), C26(H26), C39(H39), C17(H17), C49(H49), C44(H44), C46(H46),
 C34(H34), C32(H32), C45(H45), C40(H40), C47(H47), C33(H33), C21(H21), C24(H24),
  C43(H43), C23(H23), C22(H22), C35(H35), C1AA(H1AA), C9(H9), C37(H37),
 C42(H42), C36(H36), C1(H1A), C13(H13), C2(H2A), C12(H12), C11(H11), C3(H3A)
2.e Idealised tetrahedral OH refined as rotating group:
 O2(H2), O4(H4)
;
_atom_sites_solution_hydrogens   mixed
_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
Cu4 Cu 0.36666(3) 0.69033(2) 0.35242(2) 0.05687(13) Uani 1 1 d . . . . .
Cu3 Cu 0.79716(3) 0.72266(2) 0.67353(2) 0.06017(14) Uani 1 1 d . . . . .
Cu2 Cu 0.73131(3) 0.71498(3) 0.26922(3) 0.06401(15) Uani 1 1 d . . . . .
Cu1 Cu 0.93647(3) 0.79046(3) 0.25541(3) 0.07007(16) Uani 1 1 d . . . . .
N12 N 0.88379(18) 0.67935(17) 0.61783(16) 0.0607(7) Uani 1 1 d . . . . .
O2 O 0.69512(18) 0.63513(19) 0.44718(17) 0.0876(9) Uani 1 1 d . . . . .
H2 H 0.6686 0.6698 0.4331 0.131 Uiso 1 1 calc GR . . . .
N13 N 0.28442(17) 0.64318(17) 0.41059(16) 0.0612(7) Uani 1 1 d . . . . .
N10 N 0.77826(18) 0.62272(17) 0.70501(17) 0.0628(8) Uani 1 1 d . . . . .
N1AA N 0.77482(19) 0.62191(19) 0.30483(18) 0.0691(8) Uani 1 1 d . . . . .
N14 N 0.3971(2) 0.59096(17) 0.32761(18) 0.0672(8) Uani 1 1 d . . . . .
O3 O 0.59753(18) 0.64372(19) 0.69870(17) 0.0871(9) Uani 1 1 d . . . . .
H3 H 0.6231 0.6659 0.6638 0.105 Uiso 1 1 d GR . . . .
N8 N 0.7141(2) 0.66389(19) 0.17626(18) 0.0709(9) Uani 1 1 d . . . . .
N9 N 0.71222(18) 0.75845(18) 0.73894(17) 0.0653(8) Uani 1 1 d . . . . .
N15 N 0.36249(19) 0.78853(16) 0.38667(18) 0.0653(8) Uani 1 1 d . . . . .
N16 N 0.44830(18) 0.72903(17) 0.28553(18) 0.0636(8) Uani 1 1 d . . . . .
N7 N 0.6830(2) 0.80754(17) 0.24588(19) 0.0702(9) Uani 1 1 d . . . . .
O1 O 0.9706(2) 0.8982(2) 0.0962(2) 0.1026(12) Uani 1 1 d . . . . .
H1 H 0.991(4) 0.883(3) 0.127(3) 0.123 Uiso 1 1 d R . . . .
N4 N 0.89220(19) 0.88763(19) 0.2362(2) 0.0735(9) Uani 1 1 d . . . . .
N11 N 0.7963(2) 0.82141(17) 0.63915(19) 0.0715(9) Uani 1 1 d . . . . .
N0AA N 0.7550(2) 0.75855(19) 0.36733(19) 0.0764(9) Uani 1 1 d . . . . .
C31 C 0.8820(2) 0.6066(2) 0.6236(2) 0.0626(9) Uani 1 1 d . . . . .
C30 C 0.8250(2) 0.5793(2) 0.6724(2) 0.0630(9) Uani 1 1 d . . . . .
H30 H 0.8214 0.5309 0.6808 0.076 Uiso 1 1 calc R . . . .
N3 N 0.9080(2) 0.7615(2) 0.1528(2) 0.0854(11) Uani 1 1 d . . . . .
N2 N 0.9713(2) 0.6908(2) 0.2650(3) 0.0874(11) Uani 1 1 d . . . . .
N1 N 0.9642(2) 0.8301(3) 0.35293(19) 0.0884(12) Uani 1 1 d . . . . .
O4 O 0.5727(2) 0.6300(3) 0.3330(2) 0.1216(14) Uani 1 1 d . . . . .
H4 H 0.5423 0.6341 0.3675 0.182 Uiso 1 1 calc GR . . . .
C25 C 0.6829(3) 0.8491(2) 0.3079(3) 0.0750(11) Uani 1 1 d . . . . .
C48 C 0.2991(2) 0.5714(2) 0.4131(2) 0.0648(9) Uani 1 1 d . . . . .
C18 C 0.7387(3) 0.5950(3) 0.1828(2) 0.0770(11) Uani 1 1 d . . . . .
C26 C 0.7243(3) 0.8198(2) 0.3719(3) 0.0815(12) Uani 1 1 d . . . . .
H26 H 0.7286 0.8451 0.4160 0.098 Uiso 1 1 calc R . . . .
C39 C 0.6932(3) 0.8224(2) 0.7252(3) 0.0751(11) Uani 1 1 d . . . . .
H39 H 0.6512 0.8442 0.7495 0.090 Uiso 1 1 calc R . . . .
C17 C 0.7709(3) 0.5755(3) 0.2538(3) 0.0813(12) Uani 1 1 d . . . . .
H17 H 0.7890 0.5296 0.2631 0.098 Uiso 1 1 calc R . . . .
C49 C 0.3599(3) 0.5463(2) 0.3678(2) 0.0728(11) Uani 1 1 d . . . . .
H49 H 0.3731 0.4985 0.3668 0.087 Uiso 1 1 calc R . . . .
C44 C 0.3298(3) 0.8300(2) 0.4384(2) 0.0732(11) Uani 1 1 d . . . . .
H44 H 0.2901 0.8153 0.4702 0.088 Uiso 1 1 calc R . . . .
C27 C 0.6672(2) 0.7179(2) 0.7932(2) 0.0718(11) Uani 1 1 d . . . . .
H27A H 0.6169 0.7425 0.8030 0.086 Uiso 1 1 calc R . . . .
H27B H 0.6998 0.7149 0.8392 0.086 Uiso 1 1 calc R . . . .
C46 C 0.1980(3) 0.5917(3) 0.4872(2) 0.0778(12) Uani 1 1 d . . . . .
H46 H 0.1562 0.5860 0.5198 0.093 Uiso 1 1 calc R . . . .
C34 C 0.9413(2) 0.6952(2) 0.5697(2) 0.0707(10) Uani 1 1 d . . . . .
H34 H 0.9554 0.7408 0.5559 0.085 Uiso 1 1 calc R . . . .
C32 C 0.9390(3) 0.5777(3) 0.5769(2) 0.0763(11) Uani 1 1 d . . . . .
H32 H 0.9496 0.5299 0.5697 0.092 Uiso 1 1 calc R . . . .
C28 C 0.6468(2) 0.6427(2) 0.7655(2) 0.0708(10) Uani 1 1 d . . . . .
H28 H 0.6138 0.6207 0.8031 0.085 Uiso 1 1 calc R . . . .
C45 C 0.2225(2) 0.6552(2) 0.4560(2) 0.0714(10) Uani 1 1 d . . . . .
H45 H 0.1998 0.6993 0.4651 0.086 Uiso 1 1 calc R . . . .
C40 C 0.4637(3) 0.7941(2) 0.2989(3) 0.0775(12) Uani 1 1 d . . . . .
H40 H 0.5035 0.8179 0.2736 0.093 Uiso 1 1 calc R . . . .
C38 C 0.7369(3) 0.8599(2) 0.6721(3) 0.0776(11) Uani 1 1 d . . . . .
C47 C 0.2463(3) 0.5395(2) 0.4613(2) 0.0792(12) Uani 1 1 d . . . . .
H47 H 0.2445 0.4917 0.4735 0.095 Uiso 1 1 calc R . . . .
C29 C 0.7221(2) 0.5969(2) 0.7596(2) 0.0701(10) Uani 1 1 d . . . . .
H29A H 0.7509 0.5947 0.8076 0.084 Uiso 1 1 calc R . . . .
H29B H 0.7052 0.5492 0.7462 0.084 Uiso 1 1 calc R . . . .
C33 C 0.9764(2) 0.6342(3) 0.5437(2) 0.0784(12) Uani 1 1 d . . . . .
H33 H 1.0175 0.6315 0.5101 0.094 Uiso 1 1 calc R . . . .
C0AA C 0.8531(3) 0.9149(3) 0.1680(3) 0.0894(14) Uani 1 1 d . . . . .
H0AA H 0.8612 0.9657 0.1659 0.107 Uiso 1 1 calc R . . . .
H0AB H 0.7948 0.9061 0.1684 0.107 Uiso 1 1 calc R . . . .
C7 C 0.8862(3) 0.8816(3) 0.1010(3) 0.0853(13) Uani 1 1 d . . . . .
H7 H 0.8581 0.9045 0.0584 0.102 Uiso 1 1 calc R . . . .
C52 C 0.4960(2) 0.6890(2) 0.2330(2) 0.0736(11) Uani 1 1 d . . . . .
H52A H 0.5426 0.7171 0.2193 0.088 Uiso 1 1 calc R . . . .
H52B H 0.4625 0.6796 0.1885 0.088 Uiso 1 1 calc R . . . .
C15 C 0.7787(2) 0.6480(2) 0.4389(2) 0.0720(11) Uani 1 1 d . . . . .
H15 H 0.8071 0.6318 0.4848 0.086 Uiso 1 1 calc R . . . .
C41 C 0.4190(3) 0.8292(2) 0.3528(3) 0.0730(11) Uani 1 1 d . . . . .
C21 C 0.6839(3) 0.6706(3) 0.1054(2) 0.0876(13) Uani 1 1 d . . . . .
H21 H 0.6618 0.7121 0.0854 0.105 Uiso 1 1 calc R . . . .
C24 C 0.6413(3) 0.9118(2) 0.2911(3) 0.0908(14) Uani 1 1 d . . . . .
H24 H 0.6324 0.9492 0.3232 0.109 Uiso 1 1 calc R . . . .
C43 C 0.3633(3) 0.8972(2) 0.4380(3) 0.0921(14) Uani 1 1 d . . . . .
H43 H 0.3503 0.9349 0.4683 0.111 Uiso 1 1 calc R . . . .
C23 C 0.6161(3) 0.9074(3) 0.2174(3) 0.0880(14) Uani 1 1 d . . . . .
H23 H 0.5874 0.9417 0.1900 0.106 Uiso 1 1 calc R . . . .
C22 C 0.6414(3) 0.8433(2) 0.1923(3) 0.0767(12) Uani 1 1 d . . . . .
H22 H 0.6310 0.8266 0.1444 0.092 Uiso 1 1 calc R . . . .
C51 C 0.5256(2) 0.6199(2) 0.2667(2) 0.0757(11) Uani 1 1 d . . . . .
H51 H 0.5623 0.5990 0.2314 0.091 Uiso 1 1 calc R . . . .
C35 C 0.8276(3) 0.8652(3) 0.5884(3) 0.0877(13) Uani 1 1 d . . . . .
H35 H 0.8691 0.8534 0.5573 0.105 Uiso 1 1 calc R . . . .
C1AA C 0.9026(3) 0.9274(3) 0.2934(3) 0.0885(13) Uani 1 1 d . . . . .
H1AA H 0.8847 0.9741 0.2919 0.106 Uiso 1 1 calc R . . . .
C10 C 0.9612(3) 0.6565(2) 0.1989(4) 0.0973(16) Uani 1 1 d . . . . .
C14 C 0.7988(3) 0.7255(2) 0.4313(2) 0.0857(13) Uani 1 1 d . . . . .
H14A H 0.7847 0.7500 0.4761 0.103 Uiso 1 1 calc R . . . .
H14B H 0.8571 0.7307 0.4261 0.103 Uiso 1 1 calc R . . . .
C16 C 0.8093(3) 0.6033(3) 0.3786(2) 0.0895(14) Uani 1 1 d . . . . .
H16A H 0.8683 0.6076 0.3786 0.107 Uiso 1 1 calc R . . . .
H16B H 0.7965 0.5542 0.3886 0.107 Uiso 1 1 calc R . . . .
C50 C 0.4568(3) 0.5663(2) 0.2758(3) 0.0852(13) Uani 1 1 d . . . . .
H50A H 0.4293 0.5577 0.2279 0.102 Uiso 1 1 calc R . . . .
H50B H 0.4800 0.5218 0.2934 0.102 Uiso 1 1 calc R . . . .
C9 C 0.9257(3) 0.6972(3) 0.1408(3) 0.1011(16) Uani 1 1 d . . . . .
H9 H 0.9153 0.6773 0.0943 0.121 Uiso 1 1 calc R . . . .
C37 C 0.7307(4) 0.9275(3) 0.6409(3) 0.1038(16) Uani 1 1 d . . . . .
H37 H 0.6944 0.9630 0.6528 0.125 Uiso 1 1 calc R . . . .
C4 C 0.9405(3) 0.9005(3) 0.3572(3) 0.0937(15) Uani 1 1 d . . . . .
C19 C 0.7254(3) 0.5591(3) 0.1160(3) 0.1003(15) Uani 1 1 d . . . . .
H19A H 0.7765 0.5417 0.0981 0.120 Uiso 1 1 calc R . . . .
H19B H 0.6890 0.5192 0.1222 0.120 Uiso 1 1 calc R . . . .
C8 C 0.8667(4) 0.8046(3) 0.0947(3) 0.1072(18) Uani 1 1 d . . . . .
H8A H 0.8081 0.7983 0.0972 0.129 Uiso 1 1 calc R . . . .
H8B H 0.8824 0.7877 0.0468 0.129 Uiso 1 1 calc R . . . .
C42 C 0.4200(3) 0.8969(2) 0.3834(3) 0.0976(15) Uani 1 1 d . . . . .
H42 H 0.4525 0.9346 0.3698 0.117 Uiso 1 1 calc R . . . .
C20 C 0.6901(4) 0.6080(4) 0.0668(3) 0.1000(16) Uani 1 1 d . . . . .
H20 H 0.671(3) 0.600(3) 0.015(3) 0.120 Uiso 1 1 d R . . . .
C36 C 0.7886(4) 0.9306(3) 0.5897(3) 0.1072(17) Uani 1 1 d . . . . .
H36 H 0.8001 0.9696 0.5606 0.129 Uiso 1 1 calc R . . . .
C1 C 1.0028(3) 0.8130(4) 0.4189(3) 0.115(2) Uani 1 1 d . . . . .
H1A H 1.0254 0.7691 0.4309 0.138 Uiso 1 1 calc R . . . .
C13 C 1.0025(3) 0.6430(4) 0.3144(4) 0.116(2) Uani 1 1 d . . . . .
H13 H 1.0153 0.6518 0.3642 0.139 Uiso 1 1 calc R . . . .
C2 C 1.0028(5) 0.8721(6) 0.4656(4) 0.142(3) Uani 1 1 d . . . . .
H2A H 1.0251 0.8742 0.5138 0.170 Uiso 1 1 calc R . . . .
C12 C 1.0122(4) 0.5792(4) 0.2788(6) 0.140(3) Uani 1 1 d . . . . .
H12 H 1.0329 0.5379 0.3003 0.168 Uiso 1 1 calc R . . . .
C11 C 0.9863(4) 0.5872(3) 0.2067(5) 0.130(2) Uani 1 1 d . . . . .
H11 H 0.9856 0.5527 0.1700 0.156 Uiso 1 1 calc R . . . .
C3 C 0.9638(5) 0.9266(5) 0.4273(4) 0.140(3) Uani 1 1 d . . . . .
H3A H 0.9547 0.9721 0.4448 0.169 Uiso 1 1 calc R . . . .


_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
Cu4 N13 1.962(3) . ?
Cu4 N14 1.999(3) . ?
Cu4 N15 1.958(3) . ?
Cu4 N16 1.984(3) . ?
Cu3 N12 1.957(3) . ?
Cu3 N10 2.000(3) . ?
Cu3 N9 1.987(3) . ?
Cu3 N11 1.966(3) . ?
Cu2 N1AA 1.993(3) . ?
Cu2 N8 1.947(3) . ?
Cu2 N7 1.957(3) . ?
Cu2 N0AA 1.978(4) . ?
Cu1 N4 1.998(4) . ?
Cu1 N3 1.970(4) . ?
Cu1 N2 1.972(4) . ?
Cu1 N1 1.950(4) . ?
N12 C31 1.379(5) . ?
N12 C34 1.346(5) . ?
O2 H2 0.8200 . ?
O2 C15 1.405(5) . ?
N13 C48 1.378(5) . ?
N13 C45 1.354(5) . ?
N10 C30 1.283(5) . ?
N10 C29 1.463(5) . ?
N1AA C17 1.272(5) . ?
N1AA C16 1.466(5) . ?
N14 C49 1.285(5) . ?
N14 C50 1.462(5) . ?
O3 H3 0.8792 . ?
O3 C28 1.422(5) . ?
N8 C18 1.367(5) . ?
N8 C21 1.358(5) . ?
N9 C39 1.270(5) . ?
N9 C27 1.470(5) . ?
N15 C44 1.350(5) . ?
N15 C41 1.369(5) . ?
N16 C40 1.275(5) . ?
N16 C52 1.468(5) . ?
N7 C25 1.369(5) . ?
N7 C22 1.342(5) . ?
O1 H1 0.69(6) . ?
O1 C7 1.425(6) . ?
N4 C0AA 1.457(5) . ?
N4 C1AA 1.283(6) . ?
N11 C38 1.374(5) . ?
N11 C35 1.354(6) . ?
N0AA C26 1.266(5) . ?
N0AA C14 1.471(5) . ?
C31 C30 1.413(5) . ?
C31 C32 1.399(5) . ?
C30 H30 0.9300 . ?
N3 C9 1.270(6) . ?
N3 C8 1.468(6) . ?
N2 C10 1.363(7) . ?
N2 C13 1.353(6) . ?
N1 C4 1.388(7) . ?
N1 C1 1.362(6) . ?
O4 H4 0.8200 . ?
O4 C51 1.408(5) . ?
C25 C26 1.425(6) . ?
C25 C24 1.394(6) . ?
C48 C49 1.402(6) . ?
C48 C47 1.393(5) . ?
C18 C17 1.414(6) . ?
C18 C19 1.394(6) . ?
C26 H26 0.9300 . ?
C39 H39 0.9300 . ?
C39 C38 1.414(6) . ?
C17 H17 0.9300 . ?
C49 H49 0.9300 . ?
C44 H44 0.9300 . ?
C44 C43 1.382(6) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.537(6) . ?
C46 H46 0.9300 . ?
C46 C45 1.393(6) . ?
C46 C47 1.361(6) . ?
C34 H34 0.9300 . ?
C34 C33 1.380(6) . ?
C32 H32 0.9300 . ?
C32 C33 1.382(6) . ?
C28 H28 0.9800 . ?
C28 C29 1.515(6) . ?
C45 H45 0.9300 . ?
C40 H40 0.9300 . ?
C40 C41 1.412(6) . ?
C38 C37 1.397(6) . ?
C47 H47 0.9300 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C33 H33 0.9300 . ?
C0AA H0AA 0.9700 . ?
C0AA H0AB 0.9700 . ?
C0AA C7 1.490(7) . ?
C7 H7 0.9800 . ?
C7 C8 1.494(7) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C52 C51 1.511(6) . ?
C15 H15 0.9800 . ?
C15 C14 1.509(6) . ?
C15 C16 1.485(6) . ?
C41 C42 1.393(6) . ?
C21 H21 0.9300 . ?
C21 C20 1.379(7) . ?
C24 H24 0.9300 . ?
C24 C23 1.379(7) . ?
C43 H43 0.9300 . ?
C43 C42 1.387(7) . ?
C23 H23 0.9300 . ?
C23 C22 1.365(7) . ?
C22 H22 0.9300 . ?
C51 H51 0.9800 . ?
C51 C50 1.531(6) . ?
C35 H35 0.9300 . ?
C35 C36 1.392(7) . ?
C1AA H1AA 0.9300 . ?
C1AA C4 1.382(7) . ?
C10 C9 1.406(7) . ?
C10 C11 1.377(7) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C9 H9 0.9300 . ?
C37 H37 0.9300 . ?
C37 C36 1.356(8) . ?
C4 C3 1.396(8) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.391(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C42 H42 0.9300 . ?
C20 H20 0.98(5) . ?
C36 H36 0.9300 . ?
C1 H1A 0.9300 . ?
C1 C2 1.400(10) . ?
C13 H13 0.9300 . ?
C13 C12 1.379(10) . ?
C2 H2A 0.9300 . ?
C2 C3 1.381(10) . ?
C12 H12 0.9300 . ?
C12 C11 1.360(10) . ?
C11 H11 0.9300 . ?
C3 H3A 0.9300 . ?

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
N13 Cu4 N14 83.02(13) . . ?
N13 Cu4 N16 173.52(13) . . ?
N15 Cu4 N13 103.05(14) . . ?
N15 Cu4 N14 166.82(14) . . ?
N15 Cu4 N16 83.00(14) . . ?
N16 Cu4 N14 91.55(13) . . ?
N12 Cu3 N10 82.96(13) . . ?
N12 Cu3 N9 173.48(13) . . ?
N12 Cu3 N11 103.21(14) . . ?
N9 Cu3 N10 91.71(14) . . ?
N11 Cu3 N10 170.61(13) . . ?
N11 Cu3 N9 82.55(14) . . ?
N8 Cu2 N1AA 82.93(15) . . ?
N8 Cu2 N7 102.47(15) . . ?
N8 Cu2 N0AA 174.28(15) . . ?
N7 Cu2 N1AA 173.15(14) . . ?
N7 Cu2 N0AA 83.22(15) . . ?
N0AA Cu2 N1AA 91.43(15) . . ?
N3 Cu1 N4 91.33(16) . . ?
N3 Cu1 N2 82.67(18) . . ?
N2 Cu1 N4 173.33(17) . . ?
N1 Cu1 N4 82.63(18) . . ?
N1 Cu1 N3 173.51(18) . . ?
N1 Cu1 N2 103.5(2) . . ?
C31 N12 Cu3 111.1(2) . . ?
C34 N12 Cu3 141.8(3) . . ?
C34 N12 C31 106.8(3) . . ?
C15 O2 H2 109.5 . . ?
C48 N13 Cu4 110.0(2) . . ?
C45 N13 Cu4 143.3(3) . . ?
C45 N13 C48 106.2(3) . . ?
C30 N10 Cu3 111.7(3) . . ?
C30 N10 C29 120.2(3) . . ?
C29 N10 Cu3 128.1(2) . . ?
C17 N1AA Cu2 111.6(3) . . ?
C17 N1AA C16 119.9(4) . . ?
C16 N1AA Cu2 128.5(3) . . ?
C49 N14 Cu4 111.1(3) . . ?
C49 N14 C50 120.1(4) . . ?
C50 N14 Cu4 128.7(3) . . ?
C28 O3 H3 110.2 . . ?
C18 N8 Cu2 111.5(3) . . ?
C21 N8 Cu2 143.2(3) . . ?
C21 N8 C18 105.3(4) . . ?
C39 N9 Cu3 112.3(3) . . ?
C39 N9 C27 120.1(3) . . ?
C27 N9 Cu3 127.4(3) . . ?
C44 N15 Cu4 142.2(3) . . ?
C44 N15 C41 106.4(3) . . ?
C41 N15 Cu4 110.9(3) . . ?
C40 N16 Cu4 111.8(3) . . ?
C40 N16 C52 120.8(3) . . ?
C52 N16 Cu4 126.8(3) . . ?
C25 N7 Cu2 110.6(3) . . ?
C22 N7 Cu2 142.4(3) . . ?
C22 N7 C25 106.4(4) . . ?
C7 O1 H1 107(5) . . ?
C0AA N4 Cu1 127.9(3) . . ?
C1AA N4 Cu1 111.4(3) . . ?
C1AA N4 C0AA 120.8(4) . . ?
C38 N11 Cu3 111.1(3) . . ?
C35 N11 Cu3 142.8(3) . . ?
C35 N11 C38 105.6(4) . . ?
C26 N0AA Cu2 112.1(3) . . ?
C26 N0AA C14 121.2(4) . . ?
C14 N0AA Cu2 126.6(3) . . ?
N12 C31 C30 115.3(3) . . ?
N12 C31 C32 109.1(4) . . ?
C32 C31 C30 135.6(4) . . ?
N10 C30 C31 118.7(4) . . ?
N10 C30 H30 120.7 . . ?
C31 C30 H30 120.7 . . ?
C9 N3 Cu1 112.4(3) . . ?
C9 N3 C8 120.6(4) . . ?
C8 N3 Cu1 126.9(3) . . ?
C10 N2 Cu1 110.8(3) . . ?
C13 N2 Cu1 142.5(5) . . ?
C13 N2 C10 106.7(5) . . ?
C4 N1 Cu1 111.4(3) . . ?
C1 N1 Cu1 141.2(5) . . ?
C1 N1 C4 107.3(5) . . ?
C51 O4 H4 109.5 . . ?
N7 C25 C26 115.1(4) . . ?
N7 C25 C24 109.2(4) . . ?
C24 C25 C26 135.7(5) . . ?
N13 C48 C49 116.2(3) . . ?
N13 C48 C47 109.5(4) . . ?
C47 C48 C49 134.3(4) . . ?
N8 C18 C17 115.0(4) . . ?
N8 C18 C19 110.8(4) . . ?
C19 C18 C17 134.2(5) . . ?
N0AA C26 C25 118.5(4) . . ?
N0AA C26 H26 120.7 . . ?
C25 C26 H26 120.7 . . ?
N9 C39 H39 120.6 . . ?
N9 C39 C38 118.8(4) . . ?
C38 C39 H39 120.6 . . ?
N1AA C17 C18 118.9(4) . . ?
N1AA C17 H17 120.5 . . ?
C18 C17 H17 120.5 . . ?
N14 C49 C48 118.5(4) . . ?
N14 C49 H49 120.8 . . ?
C48 C49 H49 120.8 . . ?
N15 C44 H44 124.5 . . ?
N15 C44 C43 111.0(4) . . ?
C43 C44 H44 124.5 . . ?
N9 C27 H27A 109.2 . . ?
N9 C27 H27B 109.2 . . ?
N9 C27 C28 111.9(3) . . ?
H27A C27 H27B 107.9 . . ?
C28 C27 H27A 109.2 . . ?
C28 C27 H27B 109.2 . . ?
C45 C46 H46 126.2 . . ?
C47 C46 H46 126.2 . . ?
C47 C46 C45 107.5(4) . . ?
N12 C34 H34 124.8 . . ?
N12 C34 C33 110.4(4) . . ?
C33 C34 H34 124.8 . . ?
C31 C32 H32 126.8 . . ?
C33 C32 C31 106.4(4) . . ?
C33 C32 H32 126.8 . . ?
O3 C28 C27 111.7(3) . . ?
O3 C28 H28 106.6 . . ?
O3 C28 C29 112.3(4) . . ?
C27 C28 H28 106.6 . . ?
C29 C28 C27 112.7(3) . . ?
C29 C28 H28 106.6 . . ?
N13 C45 C46 109.9(4) . . ?
N13 C45 H45 125.1 . . ?
C46 C45 H45 125.1 . . ?
N16 C40 H40 120.7 . . ?
N16 C40 C41 118.7(4) . . ?
C41 C40 H40 120.7 . . ?
N11 C38 C39 114.9(4) . . ?
N11 C38 C37 110.4(4) . . ?
C37 C38 C39 134.6(5) . . ?
C48 C47 H47 126.6 . . ?
C46 C47 C48 106.9(4) . . ?
C46 C47 H47 126.6 . . ?
N10 C29 C28 113.4(3) . . ?
N10 C29 H29A 108.9 . . ?
N10 C29 H29B 108.9 . . ?
C28 C29 H29A 108.9 . . ?
C28 C29 H29B 108.9 . . ?
H29A C29 H29B 107.7 . . ?
C34 C33 C32 107.3(4) . . ?
C34 C33 H33 126.3 . . ?
C32 C33 H33 126.3 . . ?
N4 C0AA H0AA 109.2 . . ?
N4 C0AA H0AB 109.2 . . ?
N4 C0AA C7 112.1(4) . . ?
H0AA C0AA H0AB 107.9 . . ?
C7 C0AA H0AA 109.2 . . ?
C7 C0AA H0AB 109.2 . . ?
O1 C7 C0AA 110.4(4) . . ?
O1 C7 H7 106.2 . . ?
O1 C7 C8 114.5(5) . . ?
C0AA C7 H7 106.2 . . ?
C0AA C7 C8 112.9(5) . . ?
C8 C7 H7 106.2 . . ?
N16 C52 H52A 109.5 . . ?
N16 C52 H52B 109.5 . . ?
N16 C52 C51 110.8(3) . . ?
H52A C52 H52B 108.1 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
O2 C15 H15 106.4 . . ?
O2 C15 C14 113.2(4) . . ?
O2 C15 C16 110.1(4) . . ?
C14 C15 H15 106.4 . . ?
C16 C15 H15 106.4 . . ?
C16 C15 C14 113.7(4) . . ?
N15 C41 C40 115.3(4) . . ?
N15 C41 C42 109.5(4) . . ?
C42 C41 C40 135.1(4) . . ?
N8 C21 H21 124.3 . . ?
N8 C21 C20 111.4(5) . . ?
C20 C21 H21 124.3 . . ?
C25 C24 H24 126.9 . . ?
C23 C24 C25 106.3(5) . . ?
C23 C24 H24 126.9 . . ?
C44 C43 H43 126.9 . . ?
C44 C43 C42 106.2(4) . . ?
C42 C43 H43 126.9 . . ?
C24 C23 H23 126.5 . . ?
C22 C23 C24 107.1(4) . . ?
C22 C23 H23 126.5 . . ?
N7 C22 C23 111.0(4) . . ?
N7 C22 H22 124.5 . . ?
C23 C22 H22 124.5 . . ?
O4 C51 C52 112.3(4) . . ?
O4 C51 H51 106.3 . . ?
O4 C51 C50 112.0(4) . . ?
C52 C51 H51 106.3 . . ?
C52 C51 C50 113.1(3) . . ?
C50 C51 H51 106.3 . . ?
N11 C35 H35 125.0 . . ?
N11 C35 C36 110.0(5) . . ?
C36 C35 H35 125.0 . . ?
N4 C1AA H1AA 120.2 . . ?
N4 C1AA C4 119.7(5) . . ?
C4 C1AA H1AA 120.2 . . ?
N2 C10 C9 115.1(4) . . ?
N2 C10 C11 109.8(6) . . ?
C11 C10 C9 135.1(7) . . ?
N0AA C14 C15 112.6(3) . . ?
N0AA C14 H14A 109.1 . . ?
N0AA C14 H14B 109.1 . . ?
C15 C14 H14A 109.1 . . ?
C15 C14 H14B 109.1 . . ?
H14A C14 H14B 107.8 . . ?
N1AA C16 C15 113.8(4) . . ?
N1AA C16 H16A 108.8 . . ?
N1AA C16 H16B 108.8 . . ?
C15 C16 H16A 108.8 . . ?
C15 C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
N14 C50 C51 112.0(4) . . ?
N14 C50 H50A 109.2 . . ?
N14 C50 H50B 109.2 . . ?
C51 C50 H50A 109.2 . . ?
C51 C50 H50B 109.2 . . ?
H50A C50 H50B 107.9 . . ?
N3 C9 C10 119.1(5) . . ?
N3 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
C38 C37 H37 127.0 . . ?
C36 C37 C38 106.1(5) . . ?
C36 C37 H37 127.0 . . ?
N1 C4 C3 108.9(6) . . ?
C1AA C4 N1 114.9(5) . . ?
C1AA C4 C3 136.1(7) . . ?
C18 C19 H19A 110.5 . . ?
C18 C19 H19B 110.5 . . ?
H19A C19 H19B 108.7 . . ?
C20 C19 C18 106.0(5) . . ?
C20 C19 H19A 110.5 . . ?
C20 C19 H19B 110.5 . . ?
N3 C8 C7 113.3(4) . . ?
N3 C8 H8A 108.9 . . ?
N3 C8 H8B 108.9 . . ?
C7 C8 H8A 108.9 . . ?
C7 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
C41 C42 H42 126.6 . . ?
C43 C42 C41 106.9(4) . . ?
C43 C42 H42 126.6 . . ?
C21 C20 C19 106.5(5) . . ?
C21 C20 H20 126(3) . . ?
C19 C20 H20 128(3) . . ?
C35 C36 H36 126.0 . . ?
C37 C36 C35 108.0(5) . . ?
C37 C36 H36 126.0 . . ?
N1 C1 H1A 125.5 . . ?
N1 C1 C2 109.0(7) . . ?
C2 C1 H1A 125.5 . . ?
N2 C13 H13 125.6 . . ?
N2 C13 C12 108.9(7) . . ?
C12 C13 H13 125.6 . . ?
C1 C2 H2A 126.1 . . ?
C3 C2 C1 107.8(6) . . ?
C3 C2 H2A 126.1 . . ?
C13 C12 H12 125.9 . . ?
C11 C12 C13 108.2(6) . . ?
C11 C12 H12 125.9 . . ?
C10 C11 H11 126.8 . . ?
C12 C11 C10 106.4(7) . . ?
C12 C11 H11 126.8 . . ?
C4 C3 H3A 126.5 . . ?
C2 C3 C4 106.9(7) . . ?
C2 C3 H3A 126.5 . . ?

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
Cu4 N13 C48 C49 -7.9(4) . . . . ?
Cu4 N13 C48 C47 173.2(3) . . . . ?
Cu4 N13 C45 C46 -170.6(3) . . . . ?
Cu4 N14 C49 C48 8.0(5) . . . . ?
Cu4 N14 C50 C51 27.9(6) . . . . ?
Cu4 N15 C44 C43 170.7(4) . . . . ?
Cu4 N15 C41 C40 3.5(5) . . . . ?
Cu4 N15 C41 C42 -174.3(3) . . . . ?
Cu4 N16 C40 C41 -4.1(5) . . . . ?
Cu4 N16 C52 C51 -41.1(5) . . . . ?
Cu3 N12 C31 C30 -5.6(4) . . . . ?
Cu3 N12 C31 C32 173.9(2) . . . . ?
Cu3 N12 C34 C33 -171.6(3) . . . . ?
Cu3 N10 C30 C31 2.0(4) . . . . ?
Cu3 N10 C29 C28 29.8(5) . . . . ?
Cu3 N9 C39 C38 -4.8(5) . . . . ?
Cu3 N9 C27 C28 -37.3(4) . . . . ?
Cu3 N11 C38 C39 3.1(5) . . . . ?
Cu3 N11 C38 C37 -173.1(3) . . . . ?
Cu3 N11 C35 C36 170.9(4) . . . . ?
Cu2 N1AA C17 C18 0.4(5) . . . . ?
Cu2 N1AA C16 C15 26.2(6) . . . . ?
Cu2 N8 C18 C17 -0.1(5) . . . . ?
Cu2 N8 C18 C19 179.5(3) . . . . ?
Cu2 N8 C21 C20 -178.6(4) . . . . ?
Cu2 N7 C25 C26 6.2(5) . . . . ?
Cu2 N7 C25 C24 -174.4(3) . . . . ?
Cu2 N7 C22 C23 171.5(4) . . . . ?
Cu2 N0AA C26 C25 -3.3(5) . . . . ?
Cu2 N0AA C14 C15 -37.8(6) . . . . ?
Cu1 N4 C0AA C7 -32.0(5) . . . . ?
Cu1 N4 C1AA C4 0.0(5) . . . . ?
Cu1 N3 C9 C10 0.2(7) . . . . ?
Cu1 N3 C8 C7 32.3(7) . . . . ?
Cu1 N2 C10 C9 -2.8(6) . . . . ?
Cu1 N2 C10 C11 179.7(4) . . . . ?
Cu1 N2 C13 C12 -179.4(4) . . . . ?
Cu1 N1 C4 C1AA 0.4(5) . . . . ?
Cu1 N1 C4 C3 -178.4(4) . . . . ?
Cu1 N1 C1 C2 177.0(4) . . . . ?
N12 C31 C30 N10 2.4(5) . . . . ?
N12 C31 C32 C33 1.0(4) . . . . ?
N12 C34 C33 C32 0.2(5) . . . . ?
O2 C15 C14 N0AA -59.1(5) . . . . ?
O2 C15 C16 N1AA 67.0(5) . . . . ?
N13 C48 C49 N14 -0.2(6) . . . . ?
N13 C48 C47 C46 1.3(5) . . . . ?
O3 C28 C29 N10 63.6(4) . . . . ?
N8 C18 C17 N1AA -0.2(6) . . . . ?
N8 C18 C19 C20 -0.7(6) . . . . ?
N8 C21 C20 C19 0.5(6) . . . . ?
N9 C39 C38 N11 1.2(6) . . . . ?
N9 C39 C38 C37 176.2(5) . . . . ?
N9 C27 C28 O3 -60.1(4) . . . . ?
N9 C27 C28 C29 67.4(4) . . . . ?
N15 C44 C43 C42 -0.5(6) . . . . ?
N15 C41 C42 C43 0.7(6) . . . . ?
N16 C40 C41 N15 0.5(6) . . . . ?
N16 C40 C41 C42 177.5(5) . . . . ?
N16 C52 C51 O4 -57.3(4) . . . . ?
N16 C52 C51 C50 70.7(5) . . . . ?
N7 C25 C26 N0AA -2.1(6) . . . . ?
N7 C25 C24 C23 0.1(5) . . . . ?
O1 C7 C8 N3 60.2(6) . . . . ?
N4 C0AA C7 O1 -63.1(5) . . . . ?
N4 C0AA C7 C8 66.4(5) . . . . ?
N4 C1AA C4 N1 -0.3(6) . . . . ?
N4 C1AA C4 C3 178.1(6) . . . . ?
N11 C38 C37 C36 -1.6(6) . . . . ?
N11 C35 C36 C37 -1.2(7) . . . . ?
C31 N12 C34 C33 0.4(4) . . . . ?
C31 C32 C33 C34 -0.7(5) . . . . ?
C30 N10 C29 C28 -152.4(4) . . . . ?
C30 C31 C32 C33 -179.8(4) . . . . ?
N2 C10 C9 N3 1.8(8) . . . . ?
N2 C10 C11 C12 -0.1(7) . . . . ?
N2 C13 C12 C11 -0.4(7) . . . . ?
N1 C4 C3 C2 0.7(7) . . . . ?
N1 C1 C2 C3 -0.3(7) . . . . ?
O4 C51 C50 N14 64.2(5) . . . . ?
C25 N7 C22 C23 1.6(5) . . . . ?
C25 C24 C23 C22 0.9(5) . . . . ?
C48 N13 C45 C46 0.0(4) . . . . ?
C18 N8 C21 C20 -1.0(5) . . . . ?
C18 C19 C20 C21 0.1(6) . . . . ?
C26 N0AA C14 C15 138.7(5) . . . . ?
C26 C25 C24 C23 179.2(5) . . . . ?
C39 N9 C27 C28 136.3(4) . . . . ?
C39 C38 C37 C36 -176.8(5) . . . . ?
C17 N1AA C16 C15 -154.6(4) . . . . ?
C17 C18 C19 C20 178.8(5) . . . . ?
C49 N14 C50 C51 -147.7(4) . . . . ?
C49 C48 C47 C46 -177.3(4) . . . . ?
C44 N15 C41 C40 176.8(4) . . . . ?
C44 N15 C41 C42 -1.0(5) . . . . ?
C44 C43 C42 C41 -0.2(6) . . . . ?
C27 N9 C39 C38 -179.3(4) . . . . ?
C27 C28 C29 N10 -63.6(4) . . . . ?
C34 N12 C31 C30 179.7(3) . . . . ?
C34 N12 C31 C32 -0.9(4) . . . . ?
C32 C31 C30 N10 -176.8(4) . . . . ?
C45 N13 C48 C49 178.1(3) . . . . ?
C45 N13 C48 C47 -0.8(4) . . . . ?
C45 C46 C47 C48 -1.3(5) . . . . ?
C40 N16 C52 C51 130.2(4) . . . . ?
C40 C41 C42 C43 -176.4(5) . . . . ?
C38 N11 C35 C36 0.2(5) . . . . ?
C38 C37 C36 C35 1.7(7) . . . . ?
C47 C48 C49 N14 178.4(4) . . . . ?
C47 C46 C45 N13 0.8(5) . . . . ?
C29 N10 C30 C31 -176.1(3) . . . . ?
C0AA N4 C1AA C4 -179.4(4) . . . . ?
C0AA C7 C8 N3 -67.2(6) . . . . ?
C52 N16 C40 C41 -176.6(4) . . . . ?
C52 C51 C50 N14 -63.9(5) . . . . ?
C41 N15 C44 C43 0.9(5) . . . . ?
C21 N8 C18 C17 -178.6(4) . . . . ?
C21 N8 C18 C19 1.0(5) . . . . ?
C24 C25 C26 N0AA 178.8(5) . . . . ?
C24 C23 C22 N7 -1.5(5) . . . . ?
C22 N7 C25 C26 179.7(4) . . . . ?
C22 N7 C25 C24 -1.0(5) . . . . ?
C35 N11 C38 C39 177.1(4) . . . . ?
C35 N11 C38 C37 0.9(5) . . . . ?
C1AA N4 C0AA C7 147.4(4) . . . . ?
C1AA C4 C3 C2 -177.7(6) . . . . ?
C10 N2 C13 C12 0.4(6) . . . . ?
C14 N0AA C26 C25 179.8(4) . . . . ?
C14 C15 C16 N1AA -61.4(5) . . . . ?
C16 N1AA C17 C18 -179.0(4) . . . . ?
C16 C15 C14 N0AA 67.6(5) . . . . ?
C50 N14 C49 C48 -175.6(4) . . . . ?
C9 N3 C8 C7 -151.5(5) . . . . ?
C9 C10 C11 C12 -177.0(6) . . . . ?
C4 N1 C1 C2 0.7(6) . . . . ?
C19 C18 C17 N1AA -179.7(5) . . . . ?
C8 N3 C9 C10 -176.5(5) . . . . ?
C1 N1 C4 C1AA 177.9(4) . . . . ?
C1 N1 C4 C3 -0.9(5) . . . . ?
C1 C2 C3 C4 -0.3(8) . . . . ?
C13 N2 C10 C9 177.4(4) . . . . ?
C13 N2 C10 C11 -0.2(6) . . . . ?
C13 C12 C11 C10 0.3(7) . . . . ?
C11 C10 C9 N3 178.6(6) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.755 0.000 277.6 51.8 ?
2 0.500 -0.105 0.500 277.6 51.8 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2

_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 1.294
_oxdiff_exptl_absorpt_empirical_full_min 0.807
