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

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

data_ebj-149_abs_2
_database_code_depnum_ccdc_archive 'CCDC 2309435'
loop_
_audit_author_name
_audit_author_address
'Antti Marttinen'
;University of Jyvaskyla
Finland
;
_audit_update_record             
;
2023-11-21 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_audit_creation_date             2023-11-20
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C56 H38 Cu2 N10 O8, 6(H2 O)'
_chemical_formula_sum            'C56 H50 Cu2 N10 O14'
_chemical_formula_weight         1214.14
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20 H14 N6 O4 Cu1'
_chemical_oxdiff_usercomment     'green cut rod'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   10.15270(10)
_cell_length_b                   21.4379(3)
_cell_length_c                   12.6218(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.0470(10)
_cell_angle_gamma                90
_cell_volume                     2731.88(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8704
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      76.0520
_cell_measurement_theta_min      4.0570
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.610
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'bluish green'
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plank
_exptl_crystal_F_000             1252
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 13 3 0.0223
0 -13 -3 0.0155
-7 0 0 0.1031
7 -1 0 0.1022
-1 3 -8 0.0197
1 -3 8 0.0148
2 -6 -7 0.0406
-1 9 -6 0.0161

_exptl_crystal_size_max          0.221
_exptl_crystal_size_mid          0.042
_exptl_crystal_size_min          0.035
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0045 13.0204 2.9935 -0.0655 -0.3105 0.9531
0.0045 -13.0204 -2.9935 0.0655 0.3105 -0.9531
-7.0059 -0.0043 0.0096 0.2213 1.0020 0.2990
7.0068 -0.9976 -0.0094 -0.2431 -0.9781 -0.3632
-1.0241 3.0153 -7.9898 1.0273 0.0714 -0.0797
1.0241 -3.0153 7.9898 -1.0273 -0.0714 0.0797
1.9894 -6.0009 -6.9930 0.6200 -0.1431 -0.7465
-1.0246 9.0240 -5.9935 0.9255 -0.0719 0.3844

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16926
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.418
_diffrn_reflns_theta_min         4.081
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1947
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -87.00  -6.00   1.00    6.00    --  -42.17 125.00   0.00   81
  2  ω    -87.00  -6.00   1.00    6.00    --  -42.17 125.00  90.00   81
  3  ω     18.00 117.00   1.00    6.00    --   42.17  37.00  30.00   99
  4  ω     30.00 165.00   1.00   25.00    --  112.00 -15.00  30.00  135
  5  ω     83.00 178.00   1.00   25.00    --  112.00  61.00  60.00   95
  6  ω     84.00 178.00   1.00   25.00    --  112.00  30.00   0.00   94
  7  ω     36.00 145.00   1.00   25.00    --  112.00 -77.00 -60.00  109
  8  ω    104.00 178.00   1.00   25.00    --  112.00 111.00   0.00   74
  9  ω     86.00 178.00   1.00   25.00    --  112.00  45.00 -60.00   92
 10  ω   -114.00 -14.00   1.00    6.00    --  -42.17 -57.00-120.00  100
 11  ω   -114.00 -14.00   1.00    6.00    --  -42.17 -57.00 150.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0317573000
_diffrn_orient_matrix_UB_12      0.0217035000
_diffrn_orient_matrix_UB_13      -0.1163182000
_diffrn_orient_matrix_UB_21      -0.1430083000
_diffrn_orient_matrix_UB_22      -0.0239778000
_diffrn_orient_matrix_UB_23      0.0003484000
_diffrn_orient_matrix_UB_31      -0.0426650000
_diffrn_orient_matrix_UB_32      0.0640725000
_diffrn_orient_matrix_UB_33      0.0396298000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4959
_reflns_number_total             5631
_reflns_odcompleteness_completeness 99.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         5631
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0396
_refine_ls_restrained_S_all      1.042
_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)+(0.0497P)²+2.5813P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1059
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O40A) = Uanis(O40B)
3. Others
 Fixed Sof: O40B(0.5) H40A(0.5) H40B(0.5) O40A(0.5) H40C(0.5) H40D(0.5)
4.a Free rotating group:
 O38(H38A,H38B), O40B(H40A,H40B), O39(H39A,H39B), O40A(H40C,H40D)
4.b Secondary CH2 refined with riding coordinates:
 N22(H22A,H22B)
4.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C17(H17), C27(H27), C19(H19), C5(H5), C4(H4), C2(H2), C33(H33),
 C11(H11), C29(H29), C8(H8), C30(H30), C36(H36), C10(H10), C34(H34), C9(H9),
 C35(H35)
;
_atom_sites_solution_hydrogens   mixed
_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
Cu1 Cu 0.67676(3) 0.29321(2) 0.37991(2) 0.01501(10) Uani 1 1 d . . . . .
O24 O -0.12867(13) 0.29619(7) 0.36038(11) 0.0180(3) Uani 1 1 d . . . . .
O13 O 0.48779(14) 0.27526(7) 0.33759(12) 0.0211(3) Uani 1 1 d . . . . .
O38 O -0.03083(16) 0.37374(9) 0.52770(14) 0.0334(4) Uani 1 1 d G . . . .
H38A H 0.0462 0.3694 0.5604 0.050 Uiso 1 1 d G U . . .
H38B H -0.0383 0.3508 0.4724 0.050 Uiso 1 1 d G U . . .
O25 O -0.21045(15) 0.25621(9) 0.20479(13) 0.0311(4) Uani 1 1 d . . . . .
O15 O 0.36116(16) 0.34573(9) 0.41014(15) 0.0348(4) Uani 1 1 d . . . . .
N26 N 0.65722(17) 0.37811(8) 0.31848(14) 0.0194(4) Uani 1 1 d . . . . .
N1 N 0.69723(17) 0.20521(8) 0.42675(15) 0.0193(4) Uani 1 1 d . . . . .
N28 N 0.60278(18) 0.44921(9) 0.19706(14) 0.0214(4) Uani 1 1 d . . . . .
N3 N 0.64667(19) 0.10949(8) 0.46628(16) 0.0234(4) Uani 1 1 d . . . . .
N22 N 0.19438(18) 0.16737(8) 0.05029(14) 0.0205(4) Uani 1 1 d . . . . .
H22A H 0.1302 0.1327 0.0517 0.025 Uiso 1 1 calc R U . . .
H22B H 0.2840 0.1492 0.0656 0.025 Uiso 1 1 calc R U . . .
C31 C 0.5500(2) 0.47512(10) 0.09692(16) 0.0186(4) Uani 1 1 d . . . . .
C16 C 0.26031(19) 0.27451(9) 0.28170(16) 0.0172(4) Uani 1 1 d . . . . .
C21 C 0.1330(2) 0.28700(9) 0.30587(16) 0.0173(4) Uani 1 1 d . . . . .
H21 H 0.1194 0.3128 0.3649 0.021 Uiso 1 1 calc R U . . .
C32 C 0.5960(2) 0.45102(9) 0.00453(17) 0.0189(4) Uani 1 1 d . . . . .
C17 C 0.28097(19) 0.23523(10) 0.19694(16) 0.0182(4) Uani 1 1 d . . . . .
H17 H 0.3686 0.2264 0.1814 0.022 Uiso 1 1 calc R U . . .
C27 C 0.5817(2) 0.39056(10) 0.23037(16) 0.0200(4) Uani 1 1 d . . . . .
H27 H 0.5204 0.3621 0.1947 0.024 Uiso 1 1 calc R U . . .
C23 C -0.1151(2) 0.27215(10) 0.26899(17) 0.0204(4) Uani 1 1 d . . . . .
C20 C 0.02433(19) 0.26142(10) 0.24295(16) 0.0186(4) Uani 1 1 d . . . . .
C37 C 0.4561(2) 0.52265(10) 0.09626(17) 0.0188(4) Uani 1 1 d . . . . .
C14 C 0.3786(2) 0.30170(10) 0.34936(17) 0.0191(4) Uani 1 1 d . . . . .
C19 C 0.0454(2) 0.22348(10) 0.15694(16) 0.0201(4) Uani 1 1 d . . . . .
H19 H -0.0283 0.2074 0.1127 0.024 Uiso 1 1 calc R U . . .
C12 C 0.5052(2) 0.02339(10) 0.39445(19) 0.0226(4) Uani 1 1 d . . . . .
C18 C 0.1736(2) 0.20888(10) 0.13499(16) 0.0186(4) Uani 1 1 d . . . . .
C5 C 0.8124(2) 0.17216(10) 0.45378(19) 0.0239(4) Uani 1 1 d . . . . .
H5 H 0.8997 0.1883 0.4548 0.029 Uiso 1 1 calc R U . . .
C4 C 0.7809(2) 0.11291(10) 0.4787(2) 0.0260(5) Uani 1 1 d . . . . .
H4 H 0.8409 0.0802 0.5006 0.031 Uiso 1 1 calc R U . . .
C2 C 0.5993(2) 0.16571(10) 0.43551(19) 0.0233(4) Uani 1 1 d . . . . .
H2 H 0.5080 0.1757 0.4219 0.028 Uiso 1 1 calc R U . . .
C33 C 0.6899(2) 0.40143(11) 0.0051(2) 0.0264(5) Uani 1 1 d . . . . .
H33 H 0.7254 0.3834 0.0708 0.032 Uiso 1 1 calc R U . . .
O40B O 0.4912(11) 0.4430(5) 0.5239(8) 0.0443(15) Uani 0.5 1 d G . P A 2
H40A H 0.4587 0.4094 0.4965 0.066 Uiso 0.5 1 d G U P A 2
H40B H 0.4584 0.4716 0.4826 0.066 Uiso 0.5 1 d G U P A 2
C7 C 0.5663(2) 0.03303(10) 0.58811(19) 0.0228(4) Uani 1 1 d . . . . .
C11 C 0.4913(2) -0.04464(10) 0.71271(19) 0.0266(5) Uani 1 1 d . . . . .
H11 H 0.4443 -0.0817 0.7257 0.032 Uiso 1 1 calc R U . . .
C29 C 0.6978(2) 0.47578(11) 0.26945(19) 0.0269(5) Uani 1 1 d . . . . .
H29 H 0.7327 0.5168 0.2676 0.032 Uiso 1 1 calc R U . . .
C6 C 0.5692(2) 0.05408(10) 0.48338(19) 0.0228(4) Uani 1 1 d . . . . .
C8 C 0.6292(2) 0.06572(11) 0.6786(2) 0.0275(5) Uani 1 1 d . . . . .
H8 H 0.6757 0.1033 0.6683 0.033 Uiso 1 1 calc R U . . .
C30 C 0.7311(2) 0.43129(11) 0.34364(19) 0.0266(5) Uani 1 1 d . . . . .
H30 H 0.7953 0.4359 0.4036 0.032 Uiso 1 1 calc R U . . .
O39 O 0.2289(2) 0.36400(14) 0.6219(3) 0.0845(11) Uani 1 1 d G . . . .
H39A H 0.2882 0.3764 0.5841 0.127 Uiso 1 1 d G U . . .
H39B H 0.2565 0.3288 0.6458 0.127 Uiso 1 1 d G U . . .
C36 C 0.4078(2) 0.54541(11) 0.19118(18) 0.0262(5) Uani 1 1 d . . . . .
H36 H 0.4385 0.5274 0.2580 0.031 Uiso 1 1 calc R U . . .
C10 C 0.5543(3) -0.01246(11) 0.7963(2) 0.0301(5) Uani 1 1 d . . . . .
H10 H 0.5521 -0.0277 0.8668 0.036 Uiso 1 1 calc R U . . .
C34 C 0.7288(2) 0.37991(12) -0.0880(2) 0.0332(5) Uani 1 1 d . . . . .
H34 H 0.7886 0.3458 -0.0868 0.040 Uiso 1 1 calc R U . . .
C9 C 0.6235(3) 0.04379(12) 0.7790(2) 0.0321(5) Uani 1 1 d . . . . .
H9 H 0.6659 0.0661 0.8380 0.039 Uiso 1 1 calc R U . . .
C35 C 0.3183(2) 0.59257(12) 0.1865(2) 0.0324(5) Uani 1 1 d . . . . .
H35 H 0.2868 0.6073 0.2502 0.039 Uiso 1 1 calc R U . . .
O40A O 0.4639(11) 0.4286(5) 0.5480(8) 0.0443(15) Uani 0.5 1 d G . P B 1
H40C H 0.4417 0.4169 0.4843 0.066 Uiso 0.5 1 d G U P B 1
H40D H 0.4323 0.4652 0.5510 0.066 Uiso 0.5 1 d G U P B 1


_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 O24 2.0173(14) 1_655 ?
Cu1 O13 1.9744(14) . ?
Cu1 N26 1.9801(18) . ?
Cu1 N1 1.9815(18) . ?
Cu1 N22 2.2999(18) 4_666 ?
O24 Cu1 2.0174(14) 1_455 ?
O24 C23 1.284(3) . ?
O13 C14 1.268(3) . ?
O38 H38A 0.8503 . ?
O38 H38B 0.8500 . ?
O25 C23 1.243(3) . ?
O15 C14 1.241(3) . ?
N26 C27 1.310(3) . ?
N26 C30 1.383(3) . ?
N1 C5 1.379(3) . ?
N1 C2 1.319(3) . ?
N28 C31 1.432(3) . ?
N28 C27 1.350(3) . ?
N28 C29 1.380(3) . ?
N3 C4 1.357(3) . ?
N3 C2 1.340(3) . ?
N3 C6 1.453(3) . ?
N22 Cu1 2.2998(18) 4_565 ?
N22 H22A 0.9900 . ?
N22 H22B 0.9900 . ?
N22 C18 1.424(3) . ?
C31 C32 1.400(3) . ?
C31 C37 1.395(3) . ?
C16 C21 1.385(3) . ?
C16 C17 1.395(3) . ?
C16 C14 1.515(3) . ?
C21 H21 0.9500 . ?
C21 C20 1.402(3) . ?
C32 C37 1.440(3) 3_665 ?
C32 C33 1.428(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.393(3) . ?
C27 H27 0.9500 . ?
C23 C20 1.504(3) . ?
C20 C19 1.391(3) . ?
C37 C32 1.440(3) 3_665 ?
C37 C36 1.428(3) . ?
C19 H19 0.9500 . ?
C19 C18 1.394(3) . ?
C12 C7 1.439(3) 3_656 ?
C12 C11 1.431(3) 3_656 ?
C12 C6 1.401(3) . ?
C5 H5 0.9500 . ?
C5 C4 1.355(3) . ?
C4 H4 0.9500 . ?
C2 H2 0.9500 . ?
C33 H33 0.9500 . ?
C33 C34 1.359(4) . ?
O40B H40A 0.8504 . ?
O40B H40B 0.8495 . ?
C7 C12 1.439(3) 3_656 ?
C7 C6 1.400(3) . ?
C7 C8 1.432(3) . ?
C11 C12 1.431(3) 3_656 ?
C11 H11 0.9500 . ?
C11 C10 1.363(4) . ?
C29 H29 0.9500 . ?
C29 C30 1.354(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.358(4) . ?
C30 H30 0.9500 . ?
O39 H39A 0.8495 . ?
O39 H39B 0.8503 . ?
C36 H36 0.9500 . ?
C36 C35 1.357(4) . ?
C10 H10 0.9500 . ?
C10 C9 1.424(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.413(4) 3_665 ?
C9 H9 0.9500 . ?
C35 C34 1.413(4) 3_665 ?
C35 H35 0.9500 . ?
O40A H40C 0.8498 . ?
O40A H40D 0.8496 . ?

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
O24 Cu1 N22 97.00(6) 1_655 4_666 ?
O13 Cu1 O24 155.40(6) . 1_655 ?
O13 Cu1 N26 91.08(7) . . ?
O13 Cu1 N1 87.91(7) . . ?
O13 Cu1 N22 107.59(7) . 4_666 ?
N26 Cu1 O24 88.98(7) . 1_655 ?
N26 Cu1 N1 174.30(8) . . ?
N26 Cu1 N22 91.33(7) . 4_666 ?
N1 Cu1 O24 89.62(7) . 1_655 ?
N1 Cu1 N22 94.33(7) . 4_666 ?
C23 O24 Cu1 107.22(12) . 1_455 ?
C14 O13 Cu1 135.89(14) . . ?
H38A O38 H38B 109.5 . . ?
C27 N26 Cu1 123.04(15) . . ?
C27 N26 C30 106.37(17) . . ?
C30 N26 Cu1 129.65(14) . . ?
C5 N1 Cu1 128.50(15) . . ?
C2 N1 Cu1 125.44(14) . . ?
C2 N1 C5 106.04(18) . . ?
C27 N28 C31 125.41(18) . . ?
C27 N28 C29 107.51(17) . . ?
C29 N28 C31 126.50(18) . . ?
C4 N3 C6 125.40(18) . . ?
C2 N3 C4 108.07(18) . . ?
C2 N3 C6 126.53(19) . . ?
Cu1 N22 H22A 107.8 4_565 . ?
Cu1 N22 H22B 107.8 4_565 . ?
H22A N22 H22B 107.1 . . ?
C18 N22 Cu1 118.00(13) . 4_565 ?
C18 N22 H22A 107.8 . . ?
C18 N22 H22B 107.8 . . ?
C32 C31 N28 117.73(19) . . ?
C37 C31 N28 118.74(19) . . ?
C37 C31 C32 123.53(19) . . ?
C21 C16 C17 120.33(18) . . ?
C21 C16 C14 120.28(19) . . ?
C17 C16 C14 119.36(18) . . ?
C16 C21 H21 120.1 . . ?
C16 C21 C20 119.79(19) . . ?
C20 C21 H21 120.1 . . ?
C31 C32 C37 117.88(19) . 3_665 ?
C31 C32 C33 123.5(2) . . ?
C33 C32 C37 118.6(2) . 3_665 ?
C16 C17 H17 119.9 . . ?
C18 C17 C16 120.23(19) . . ?
C18 C17 H17 119.9 . . ?
N26 C27 N28 110.89(18) . . ?
N26 C27 H27 124.6 . . ?
N28 C27 H27 124.6 . . ?
O24 C23 C20 116.75(17) . . ?
O25 C23 O24 123.1(2) . . ?
O25 C23 C20 120.10(19) . . ?
C21 C20 C23 121.28(19) . . ?
C19 C20 C21 119.63(19) . . ?
C19 C20 C23 119.05(18) . . ?
C31 C37 C32 118.59(19) . 3_665 ?
C31 C37 C36 122.7(2) . . ?
C36 C37 C32 118.7(2) . 3_665 ?
O13 C14 C16 114.40(18) . . ?
O15 C14 O13 126.60(19) . . ?
O15 C14 C16 119.00(19) . . ?
C20 C19 H19 119.7 . . ?
C20 C19 C18 120.65(19) . . ?
C18 C19 H19 119.7 . . ?
C11 C12 C7 118.4(2) 3_656 3_656 ?
C6 C12 C7 118.1(2) . 3_656 ?
C6 C12 C11 123.5(2) . 3_656 ?
C17 C18 N22 120.38(19) . . ?
C17 C18 C19 119.29(19) . . ?
C19 C18 N22 120.34(18) . . ?
N1 C5 H5 125.5 . . ?
C4 C5 N1 108.91(19) . . ?
C4 C5 H5 125.5 . . ?
N3 C4 H4 126.8 . . ?
C5 C4 N3 106.42(19) . . ?
C5 C4 H4 126.8 . . ?
N1 C2 N3 110.56(19) . . ?
N1 C2 H2 124.7 . . ?
N3 C2 H2 124.7 . . ?
C32 C33 H33 119.9 . . ?
C34 C33 C32 120.2(2) . . ?
C34 C33 H33 119.9 . . ?
H40A O40B H40B 104.5 . . ?
C6 C7 C12 118.5(2) . 3_656 ?
C6 C7 C8 122.9(2) . . ?
C8 C7 C12 118.6(2) . 3_656 ?
C12 C11 H11 119.5 3_656 . ?
C10 C11 C12 121.0(2) . 3_656 ?
C10 C11 H11 119.5 . . ?
N28 C29 H29 127.1 . . ?
C30 C29 N28 105.85(19) . . ?
C30 C29 H29 127.1 . . ?
C12 C6 N3 118.5(2) . . ?
C7 C6 N3 118.0(2) . . ?
C7 C6 C12 123.4(2) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 C7 121.0(2) . . ?
C9 C8 H8 119.5 . . ?
N26 C30 H30 125.3 . . ?
C29 C30 N26 109.38(19) . . ?
C29 C30 H30 125.3 . . ?
H39A O39 H39B 104.5 . . ?
C37 C36 H36 119.8 . . ?
C35 C36 C37 120.4(2) . . ?
C35 C36 H36 119.8 . . ?
C11 C10 H10 119.7 . . ?
C11 C10 C9 120.5(2) . . ?
C9 C10 H10 119.7 . . ?
C33 C34 H34 119.4 . . ?
C33 C34 C35 121.1(2) . 3_665 ?
C35 C34 H34 119.4 3_665 . ?
C8 C9 C10 120.5(2) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C36 C35 C34 120.8(2) . 3_665 ?
C36 C35 H35 119.6 . . ?
C34 C35 H35 119.6 3_665 . ?
H40C O40A H40D 104.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O38 H38A O39 0.85 1.94 2.784(3) 173.8 .
O38 H38B O24 0.85 1.98 2.787(2) 157.0 .
N22 H22B O38 0.99 2.05 2.968(3) 153.7 4_665
O40B H40A O15 0.85 1.95 2.785(11) 166.5 .
O39 H39A O40A 0.85 2.19 2.992(8) 156.3 .
O39 H39B O25 0.85 1.98 2.825(3) 170.4 4_666
O40A H40C O15 0.85 1.93 2.625(11) 138.6 .

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 O24 C23 O25 5.7(3) 1_455 . . . ?
Cu1 O24 C23 C20 -172.04(15) 1_455 . . . ?
Cu1 O13 C14 O15 -12.5(4) . . . . ?
Cu1 O13 C14 C16 168.38(14) . . . . ?
Cu1 N26 C27 N28 -169.91(14) . . . . ?
Cu1 N26 C30 C29 169.33(17) . . . . ?
Cu1 N1 C5 C4 -178.59(16) . . . . ?
Cu1 N1 C2 N3 178.30(15) . . . . ?
Cu1 N22 C18 C17 -98.9(2) 4_565 . . . ?
Cu1 N22 C18 C19 81.2(2) 4_565 . . . ?
O24 C23 C20 C21 -11.7(3) . . . . ?
O24 C23 C20 C19 165.91(19) . . . . ?
O25 C23 C20 C21 170.4(2) . . . . ?
O25 C23 C20 C19 -11.9(3) . . . . ?
N1 C5 C4 N3 0.4(3) . . . . ?
N28 C31 C32 C37 -179.48(17) . . . 3_665 ?
N28 C31 C32 C33 1.4(3) . . . . ?
N28 C31 C37 C32 179.47(17) . . . 3_665 ?
N28 C31 C37 C36 -1.7(3) . . . . ?
N28 C29 C30 N26 -0.6(3) . . . . ?
C31 N28 C27 N26 171.4(2) . . . . ?
C31 N28 C29 C30 -171.1(2) . . . . ?
C31 C32 C33 C34 179.2(2) . . . . ?
C31 C37 C36 C35 178.7(2) . . . . ?
C16 C21 C20 C23 177.88(19) . . . . ?
C16 C21 C20 C19 0.3(3) . . . . ?
C16 C17 C18 N22 -178.23(18) . . . . ?
C16 C17 C18 C19 1.6(3) . . . . ?
C21 C16 C17 C18 0.9(3) . . . . ?
C21 C16 C14 O13 162.94(19) . . . . ?
C21 C16 C14 O15 -16.3(3) . . . . ?
C21 C20 C19 C18 2.3(3) . . . . ?
C32 C31 C37 C32 -0.6(3) . . . 3_665 ?
C32 C31 C37 C36 178.22(19) . . . . ?
C32 C37 C36 C35 -2.5(3) 3_665 . . . ?
C32 C33 C34 C35 2.6(4) . . . 3_665 ?
C17 C16 C21 C20 -1.8(3) . . . . ?
C17 C16 C14 O13 -15.1(3) . . . . ?
C17 C16 C14 O15 165.7(2) . . . . ?
C27 N26 C30 C29 0.4(3) . . . . ?
C27 N28 C31 C32 -67.5(3) . . . . ?
C27 N28 C31 C37 112.5(2) . . . . ?
C27 N28 C29 C30 0.5(3) . . . . ?
C23 C20 C19 C18 -175.40(19) . . . . ?
C20 C19 C18 N22 176.67(19) . . . . ?
C20 C19 C18 C17 -3.2(3) . . . . ?
C37 C31 C32 C37 0.6(3) . . . 3_665 ?
C37 C31 C32 C33 -178.58(19) . . . . ?
C37 C32 C33 C34 0.0(3) 3_665 . . . ?
C37 C36 C35 C34 0.0(4) . . . 3_665 ?
C14 C16 C21 C20 -179.78(18) . . . . ?
C14 C16 C17 C18 178.84(18) . . . . ?
C12 C7 C6 N3 -177.22(18) 3_656 . . . ?
C12 C7 C6 C12 0.6(4) 3_656 . . . ?
C12 C7 C8 C9 0.8(3) 3_656 . . . ?
C12 C11 C10 C9 1.1(4) 3_656 . . . ?
C5 N1 C2 N3 -0.2(3) . . . . ?
C4 N3 C2 N1 0.5(3) . . . . ?
C4 N3 C6 C12 -107.6(3) . . . . ?
C4 N3 C6 C7 70.3(3) . . . . ?
C2 N1 C5 C4 -0.1(3) . . . . ?
C2 N3 C4 C5 -0.5(3) . . . . ?
C2 N3 C6 C12 72.2(3) . . . . ?
C2 N3 C6 C7 -109.9(3) . . . . ?
C7 C12 C6 N3 177.22(18) 3_656 . . . ?
C7 C12 C6 C7 -0.6(4) 3_656 . . . ?
C7 C8 C9 C10 0.0(4) . . . . ?
C11 C12 C6 N3 -1.8(3) 3_656 . . . ?
C11 C12 C6 C7 -179.6(2) 3_656 . . . ?
C11 C10 C9 C8 -1.0(4) . . . . ?
C29 N28 C31 C32 102.6(3) . . . . ?
C29 N28 C31 C37 -77.4(3) . . . . ?
C29 N28 C27 N26 -0.3(3) . . . . ?
C6 N3 C4 C5 179.3(2) . . . . ?
C6 N3 C2 N1 -179.4(2) . . . . ?
C6 C7 C8 C9 179.7(2) . . . . ?
C8 C7 C6 N3 3.9(3) . . . . ?
C8 C7 C6 C12 -178.3(2) . . . . ?
C30 N26 C27 N28 -0.1(3) . . . . ?

_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 1.904
_oxdiff_exptl_absorpt_empirical_full_min 0.739
####################################################################### 
# 
# 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_ebj-150-blue2_abs_2
_database_code_depnum_ccdc_archive 'CCDC 2309437'
loop_
_audit_author_name
_audit_author_address
'Antti Marttinen'
;University of Jyvaskyla
Finland
;
_audit_update_record             
;
2023-11-21 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_audit_creation_date             2023-11-20
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C56 H36 Cu2 N10 O8, 4(H2 O)'
_chemical_formula_sum            'C56 H44 Cu2 N10 O12'
_chemical_formula_weight         1176.09
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H20 N6 O6 Cu1'
_chemical_oxdiff_usercomment     'blue green block'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   10.8808(3)
_cell_length_b                   11.1603(3)
_cell_length_c                   12.5136(3)
_cell_angle_alpha                111.044(2)
_cell_angle_beta                 107.145(2)
_cell_angle_gamma                95.432(2)
_cell_volume                     1320.49(6)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9590
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      78.3890
_cell_measurement_theta_min      4.3490
_shelx_estimated_absorpt_T_max   0.921
_shelx_estimated_absorpt_T_min   0.865
_exptl_absorpt_coefficient_mu    1.619
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.916
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'bluish green'
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             604
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 1 0 0.0179
6 2 -6 0.0330
-1 -7 6 0.0329
-1 -1 -6 0.0159
2 2 4 0.0382
6 3 -3 0.0353
-6 3 -3 0.0087
-3 -3 -3 0.0119
2 -7 4 0.0376

_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.052
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.0004 1.0018 0.0029 0.0444 0.1718 0.0661
5.6595 2.4641 -6.2737 -0.1504 -0.6304 0.7616
-0.8119 -6.6487 5.6418 -0.0446 -0.1801 -0.9826
-1.4103 -1.4793 -5.5778 0.9365 -0.3316 0.1136
2.3955 2.0555 4.4654 -0.9717 0.2335 0.0345
5.8550 3.3136 -2.6090 -0.6670 -0.3611 0.6517
-5.6160 3.4024 -2.6024 0.7262 0.6205 0.2959
-2.7158 -3.1377 -3.2166 0.9489 -0.2277 -0.2184
1.5407 -6.9987 4.0691 -0.1216 -0.5012 -0.8568

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21942
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.519
_diffrn_reflns_theta_min         4.047
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -4.00  79.00   0.50    5.00    --   52.54 -92.00  97.00  166
  2  ω     46.00 105.00   0.50   19.00    --  101.90 -92.00  97.00  118
  3  ω    102.00 158.00   0.50   19.00    --  101.90  92.00-150.00  112
  4  ω    -37.00  -9.00   0.50    5.00    --    6.00 120.00  93.38   56
  5  ω     -9.00  43.00   0.50    5.00    --   14.00  88.00  11.60  104
  6  ω      4.00  41.00   0.50    5.00    --   30.00  92.00 -68.33   74
  7  ω     16.00  43.00   0.50    5.00    --   34.00  79.00-143.24   54
  8  ω     -3.00  79.00   0.50    5.00    --   52.75 -92.00  97.00  164
  9  ω     54.00 132.00   0.50    5.00    --   70.00  76.00-171.13  156
 10  ω     59.00 137.00   0.50    5.00    --   70.00  60.00 -86.90  156
 11  ω     43.00 106.00   0.50   19.00    --  101.90 -99.00-150.00  126
 12  ω     34.00 112.00   0.50   19.00    --  101.90 -57.00  60.00  156
 13  ω     43.00 106.00   0.50   19.00    --  101.90 -99.00   0.00  126
 14  ω     95.00 166.00   0.50   19.00    --  101.90 125.00 150.00  142
 15  ω     32.00 120.00   0.50   19.00    --  101.90 -19.00-120.00  176
 16  ω     43.00 106.00   0.50   19.00    --  101.90 -99.00 -90.00  126
 17  ω     53.00 132.00   0.50   19.00    --  107.75 -88.00  49.89  158
 18  ω     43.00 163.00   0.50   19.00    --  107.75  -7.00-115.48  240
 19  ω     96.00 178.00   0.50   19.00    --  107.75  25.00  82.93  164
 20  ω     52.00 131.00   0.50   19.00    --  107.75 -87.00 -54.84  158
 21  ω     51.00 130.00   0.50   19.00    --  107.75 -86.00 154.51  158
 22  ω     38.00 125.00   0.50   19.00    --  107.75 -20.00-150.48  174
 23  ω     46.00 123.00   0.50   19.00    --  107.75 -75.00-162.50  154
 24  ω     38.00 115.00   0.50   19.00    --  107.75 -46.00-128.82  154
 25  ω     38.00 116.00   0.50   19.00    --  107.75 -47.00  -3.33  156
 26  ω     37.00 114.00   0.50   19.00    --  107.75 -44.00 -74.60  154
 27  ω     47.00 125.00   0.50   19.00    --  107.75 -78.00 -33.37  156
 28  ω     36.00 112.00   0.50   19.00    --  107.75 -40.00 145.67  152
 29  ω     37.00 121.00   0.50   19.00    --  107.75 -23.00  49.05  168
 30  ω     14.00  43.00   0.50    5.00    --   38.00  89.00 129.67   58
 31  ω     66.00 144.00   0.50    5.00    --   74.00  47.00  17.28  156
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1221169000
_diffrn_orient_matrix_UB_12      -0.0772646000
_diffrn_orient_matrix_UB_13      -0.1165385000
_diffrn_orient_matrix_UB_21      -0.0848680000
_diffrn_orient_matrix_UB_22      0.0866182000
_diffrn_orient_matrix_UB_23      0.0579449000
_diffrn_orient_matrix_UB_31      0.0317471000
_diffrn_orient_matrix_UB_32      0.0978163000
_diffrn_orient_matrix_UB_33      -0.0543300000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4924
_reflns_number_total             5597
_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         5597
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0476
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0504P)²+1.2960P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1198
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N38B-C37
 1.34 with sigma of 0.02
3. Others
 Fixed Sof: N6(0.5) H6A(0.5) H6B(0.5) N38B(0.25) H38A(0.25) H38B(0.25)
 N38A(0.25) H38C(0.25) H38D(0.25)
4.a Free rotating group:
 O40(H40A,H40B), O39(H39A,H39B)
4.b Rotating group:
 N6(H6A,H6B)
4.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C18(H18), C9(H9), C12(H12), C10(H10), C29(H29), C25(H25), C36(H36),
 C22(H22), C28(H28), C15(H15), C31(H31), C24(H24), C23(H23), C17(H17), C16(H16)
4.d X=CH2 refined with riding coordinates:
 N38B(H38A,H38B), N38A(H38C,H38D)
;
_atom_sites_solution_hydrogens   mixed
_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
Cu1 Cu 0.5000 0.0000 0.0000 0.02353(13) Uani 1 2 d S . P . .
Cu2 Cu 1.5000 1.0000 0.5000 0.04150(18) Uani 1 2 d S . P . .
O1 O 0.31157(14) 0.00007(15) -0.05420(15) 0.0260(3) Uani 1 1 d . . . . .
O32 O 1.51130(17) 0.82842(18) 0.5048(2) 0.0449(5) Uani 1 1 d . . . . .
O40 O 1.48264(18) 1.08097(19) 0.71084(19) 0.0396(4) Uani 1 1 d G . . . .
H40A H 1.5130 1.1634 0.7284 0.059 Uiso 1 1 d G U . . .
H40B H 1.5428 1.0616 0.7614 0.059 Uiso 1 1 d G U . . .
O2 O 0.35690(17) 0.0258(2) 0.13762(18) 0.0399(4) Uani 1 1 d . . . . .
O33 O 1.4565(2) 0.6879(2) 0.3088(2) 0.0490(5) Uani 1 1 d . . . . .
N30 N 1.30123(19) 0.94952(19) 0.4372(2) 0.0322(5) Uani 1 1 d . . . . .
N8 N 0.54607(18) 0.19421(19) 0.0510(2) 0.0296(4) Uani 1 1 d . . . . .
N11 N 0.66537(19) 0.3963(2) 0.1326(2) 0.0358(5) Uani 1 1 d . . . . .
O39 O 1.2211(2) 1.0190(3) 0.7135(2) 0.0556(6) Uani 1 1 d G . . . .
H39A H 1.2429 1.0218 0.7873 0.083 Uiso 1 1 d G U . . .
H39B H 1.2959 1.0296 0.7022 0.083 Uiso 1 1 d G U . . .
N27 N 1.09805(19) 0.83252(19) 0.3569(2) 0.0348(5) Uani 1 1 d . . . . .
C13 C 0.7788(2) 0.5050(2) 0.1897(3) 0.0352(6) Uani 1 1 d . . . . .
C4 C 0.1340(2) 0.0076(2) 0.0194(2) 0.0256(5) Uani 1 1 d . . . . .
C3 C 0.2765(2) 0.0123(2) 0.0379(2) 0.0274(5) Uani 1 1 d . . . . .
C26 C 0.8236(2) 0.5499(2) 0.1137(3) 0.0358(6) Uani 1 1 d . . . . .
C19 C 0.9469(2) 0.6716(2) 0.3748(3) 0.0353(6) Uani 1 1 d . . . . .
C5 C 0.0923(2) 0.0457(3) 0.1204(2) 0.0308(5) Uani 1 1 d . . . . .
C7 C -0.0423(2) 0.0365(2) 0.0984(2) 0.0292(5) Uani 1 1 d . . . . .
H7 H -0.0721 0.0609 0.1657 0.035 Uiso 1 1 calc R U . . .
C35 C 1.4926(2) 0.6047(2) 0.4641(3) 0.0350(6) Uani 1 1 d . . . . .
C18 C 1.0066(3) 0.7275(3) 0.5051(3) 0.0419(7) Uani 1 1 d . . . . .
H18 H 1.0810 0.7997 0.5444 0.050 Uiso 1 1 calc R U . . .
C9 C 0.4634(2) 0.2787(2) 0.0425(3) 0.0350(6) Uani 1 1 d . . . . .
H9 H 0.3698 0.2530 0.0068 0.042 Uiso 1 1 calc R U . . .
C20 C 0.9898(2) 0.7192(2) 0.2992(3) 0.0351(6) Uani 1 1 d . . . . .
C12 C 0.6673(2) 0.2692(2) 0.1073(3) 0.0338(6) Uani 1 1 d . . . . .
H12 H 0.7452 0.2373 0.1271 0.041 Uiso 1 1 calc R U . . .
C14 C 0.8358(2) 0.5605(2) 0.3174(3) 0.0373(6) Uani 1 1 d . . . . .
C34 C 1.4862(2) 0.7143(3) 0.4203(3) 0.0386(7) Uani 1 1 d . . . . .
C10 C 0.5354(2) 0.4042(3) 0.0929(3) 0.0392(6) Uani 1 1 d . . . . .
H10 H 0.5028 0.4816 0.0994 0.047 Uiso 1 1 calc R U . . .
C29 C 1.2167(3) 1.0322(2) 0.4487(3) 0.0464(8) Uani 1 1 d . . . . .
H29 H 1.2426 1.1257 0.4864 0.056 Uiso 1 1 calc R U . . .
C37 C 1.4730(3) 0.3705(3) 0.4113(3) 0.0464(7) Uani 1 1 d D . . . .
C21 C 0.9334(2) 0.6628(2) 0.1713(3) 0.0364(6) Uani 1 1 d . . . . .
C25 C 0.7679(3) 0.4909(3) -0.0164(3) 0.0406(6) Uani 1 1 d . . . . .
H25 H 0.6970 0.4153 -0.0559 0.049 Uiso 1 1 calc R U . . .
C36 C 1.4656(3) 0.4763(3) 0.3773(3) 0.0426(7) Uani 1 1 d . . . . .
H36 H 1.4417 0.4604 0.2932 0.051 Uiso 1 1 calc R U . . .
C22 C 0.9782(3) 0.7117(3) 0.0956(3) 0.0421(7) Uani 1 1 d . . . . .
H22 H 1.0493 0.7867 0.1323 0.051 Uiso 1 1 calc R U . . .
C28 C 1.0899(3) 0.9610(2) 0.3983(3) 0.0453(7) Uani 1 1 d . . . . .
H28 H 1.0120 0.9941 0.3931 0.054 Uiso 1 1 calc R U . . .
C15 C 0.7892(3) 0.5139(3) 0.3938(3) 0.0440(7) Uani 1 1 d . . . . .
H15 H 0.7155 0.4413 0.3574 0.053 Uiso 1 1 calc R U . . .
C31 C 1.2267(2) 0.8308(2) 0.3811(3) 0.0467(8) Uani 1 1 d . . . . .
H31 H 1.2592 0.7528 0.3599 0.056 Uiso 1 1 calc R U . . .
C24 C 0.8140(3) 0.5404(3) -0.0849(3) 0.0472(7) Uani 1 1 d . . . . .
H24 H 0.7747 0.4997 -0.1716 0.057 Uiso 1 1 calc R U . . .
C23 C 0.9211(3) 0.6531(3) -0.0279(3) 0.0495(8) Uani 1 1 d . . . . .
H23 H 0.9524 0.6872 -0.0769 0.059 Uiso 1 1 calc R U . . .
C17 C 0.9588(3) 0.6791(3) 0.5734(3) 0.0492(7) Uani 1 1 d . . . . .
H17 H 0.9999 0.7177 0.6600 0.059 Uiso 1 1 calc R U . . .
C16 C 0.8476(3) 0.5707(3) 0.5166(3) 0.0496(7) Uani 1 1 d . . . . .
H16 H 0.8143 0.5384 0.5657 0.060 Uiso 1 1 calc R U . . .
N6 N 0.1786(5) 0.0998(7) 0.2362(5) 0.0585(16) Uani 0.5 1 d . . P . .
H6A H 0.1423 0.0803 0.2845 0.070 Uiso 0.5 1 d R U P . .
H6B H 0.2509 0.0683 0.2408 0.070 Uiso 0.5 1 d R U P . .
N38B N 1.4282(19) 0.2547(11) 0.3269(12) 0.071(5) Uani 0.25 1 d D . P A 2
H38A H 1.4826 0.2094 0.2996 0.085 Uiso 0.25 1 calc R U P A 2
H38B H 1.3429 0.2199 0.2958 0.085 Uiso 0.25 1 calc R U P A 2
N38A N 1.5035(12) 0.2693(12) 0.3431(12) 0.045(3) Uani 0.25 1 d . . P A 1
H38C H 1.4413 0.1993 0.2893 0.054 Uiso 0.25 1 calc R U P A 1
H38D H 1.5865 0.2701 0.3502 0.054 Uiso 0.25 1 calc R U P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.9607(15) . ?
Cu1 O1 1.9607(15) 2_655 ?
Cu1 N8 1.9922(19) . ?
Cu1 N8 1.9923(19) 2_655 ?
Cu2 O32 1.9513(17) 2_876 ?
Cu2 O32 1.9514(17) . ?
Cu2 N30 2.0153(19) 2_876 ?
Cu2 N30 2.0153(19) . ?
O1 C3 1.284(3) . ?
O32 C34 1.270(4) . ?
O40 H40A 0.8702 . ?
O40 H40B 0.8697 . ?
O2 C3 1.242(3) . ?
O33 C34 1.248(4) . ?
N30 C29 1.364(3) . ?
N30 C31 1.303(3) . ?
N8 C9 1.373(3) . ?
N8 C12 1.326(3) . ?
N11 C13 1.442(3) . ?
N11 C12 1.342(3) . ?
N11 C10 1.377(3) . ?
O39 H39A 0.8712 . ?
O39 H39B 0.8708 . ?
N27 C20 1.438(3) . ?
N27 C28 1.360(3) . ?
N27 C31 1.346(3) . ?
C13 C26 1.401(4) . ?
C13 C14 1.398(4) . ?
C4 C3 1.492(3) . ?
C4 C5 1.404(3) . ?
C4 C7 1.389(3) 2 ?
C26 C21 1.445(3) . ?
C26 C25 1.423(4) . ?
C19 C18 1.427(4) . ?
C19 C20 1.403(4) . ?
C19 C14 1.442(3) . ?
C5 C7 1.395(3) . ?
C5 N6 1.345(6) . ?
C7 C4 1.389(3) 2 ?
C7 H7 0.9500 . ?
C35 C34 1.509(3) . ?
C35 C37 1.405(5) 2_866 ?
C35 C36 1.391(4) . ?
C18 H18 0.9500 . ?
C18 C17 1.355(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.357(3) . ?
C20 C21 1.399(4) . ?
C12 H12 0.9500 . ?
C14 C15 1.427(4) . ?
C10 H10 0.9500 . ?
C29 H29 0.9500 . ?
C29 C28 1.362(3) . ?
C37 C35 1.405(5) 2_866 ?
C37 C36 1.392(4) . ?
C37 N38B 1.274(11) . ?
C37 N38A 1.289(14) . ?
C21 C22 1.424(4) . ?
C25 H25 0.9500 . ?
C25 C24 1.353(5) . ?
C36 H36 0.9500 . ?
C22 H22 0.9500 . ?
C22 C23 1.354(5) . ?
C28 H28 0.9500 . ?
C15 H15 0.9500 . ?
C15 C16 1.348(5) . ?
C31 H31 0.9500 . ?
C24 H24 0.9500 . ?
C24 C23 1.428(4) . ?
C23 H23 0.9500 . ?
C17 H17 0.9500 . ?
C17 C16 1.425(4) . ?
C16 H16 0.9500 . ?
N6 H6A 0.8867 . ?
N6 H6B 0.8867 . ?
N38B H38A 0.8800 . ?
N38B H38B 0.8800 . ?
N38A H38C 0.8800 . ?
N38A H38D 0.8800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O1 180.0 . 2_655 ?
O1 Cu1 N8 90.36(7) . . ?
O1 Cu1 N8 89.64(7) 2_655 . ?
O1 Cu1 N8 89.64(7) . 2_655 ?
O1 Cu1 N8 90.36(7) 2_655 2_655 ?
N8 Cu1 N8 180.0 . 2_655 ?
O32 Cu2 O32 180.0 2_876 . ?
O32 Cu2 N30 91.19(8) 2_876 2_876 ?
O32 Cu2 N30 88.81(8) . 2_876 ?
O32 Cu2 N30 91.19(8) . . ?
O32 Cu2 N30 88.81(8) 2_876 . ?
N30 Cu2 N30 180.0 2_876 . ?
C3 O1 Cu1 105.69(14) . . ?
C34 O32 Cu2 131.8(2) . . ?
H40A O40 H40B 104.5 . . ?
C29 N30 Cu2 127.23(16) . . ?
C31 N30 Cu2 127.14(17) . . ?
C31 N30 C29 105.6(2) . . ?
C9 N8 Cu1 128.84(15) . . ?
C12 N8 Cu1 125.19(16) . . ?
C12 N8 C9 105.88(19) . . ?
C12 N11 C13 126.3(2) . . ?
C12 N11 C10 107.67(19) . . ?
C10 N11 C13 126.1(2) . . ?
H39A O39 H39B 104.4 . . ?
C28 N27 C20 126.6(2) . . ?
C31 N27 C20 126.1(2) . . ?
C31 N27 C28 107.3(2) . . ?
C26 C13 N11 117.9(3) . . ?
C14 C13 N11 118.0(2) . . ?
C14 C13 C26 124.0(2) . . ?
C5 C4 C3 120.2(2) . . ?
C7 C4 C3 119.7(2) 2 . ?
C7 C4 C5 120.1(2) 2 . ?
O1 C3 C4 117.0(2) . . ?
O2 C3 O1 121.7(2) . . ?
O2 C3 C4 121.2(2) . . ?
C13 C26 C21 117.8(3) . . ?
C13 C26 C25 123.9(2) . . ?
C25 C26 C21 118.2(3) . . ?
C18 C19 C14 118.3(3) . . ?
C20 C19 C18 123.7(2) . . ?
C20 C19 C14 118.0(3) . . ?
C7 C5 C4 118.2(2) . . ?
N6 C5 C4 122.0(3) . . ?
N6 C5 C7 119.7(3) . . ?
C4 C7 C5 121.7(2) 2 . ?
C4 C7 H7 119.1 2 . ?
C5 C7 H7 119.1 . . ?
C37 C35 C34 122.0(3) 2_866 . ?
C36 C35 C34 118.1(3) . . ?
C36 C35 C37 120.0(2) . 2_866 ?
C19 C18 H18 119.5 . . ?
C17 C18 C19 120.9(3) . . ?
C17 C18 H18 119.5 . . ?
N8 C9 H9 125.1 . . ?
C10 C9 N8 109.8(2) . . ?
C10 C9 H9 125.1 . . ?
C19 C20 N27 117.9(3) . . ?
C21 C20 N27 118.3(2) . . ?
C21 C20 C19 123.8(2) . . ?
N8 C12 N11 110.9(2) . . ?
N8 C12 H12 124.6 . . ?
N11 C12 H12 124.6 . . ?
C13 C14 C19 118.1(3) . . ?
C13 C14 C15 123.5(2) . . ?
C15 C14 C19 118.4(3) . . ?
O32 C34 C35 114.3(3) . . ?
O33 C34 O32 125.9(2) . . ?
O33 C34 C35 119.8(3) . . ?
N11 C10 H10 127.1 . . ?
C9 C10 N11 105.8(2) . . ?
C9 C10 H10 127.1 . . ?
N30 C29 H29 125.0 . . ?
C28 C29 N30 110.0(2) . . ?
C28 C29 H29 125.0 . . ?
C36 C37 C35 118.8(3) . 2_866 ?
N38B C37 C35 122.4(7) . 2_866 ?
N38B C37 C36 117.8(7) . . ?
N38A C37 C35 117.3(7) . 2_866 ?
N38A C37 C36 117.6(7) . . ?
C20 C21 C26 118.2(3) . . ?
C20 C21 C22 123.3(2) . . ?
C22 C21 C26 118.6(3) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 C26 121.2(3) . . ?
C24 C25 H25 119.4 . . ?
C35 C36 C37 121.2(3) . . ?
C35 C36 H36 119.4 . . ?
C37 C36 H36 119.4 . . ?
C21 C22 H22 119.4 . . ?
C23 C22 C21 121.1(3) . . ?
C23 C22 H22 119.4 . . ?
N27 C28 C29 105.5(2) . . ?
N27 C28 H28 127.2 . . ?
C29 C28 H28 127.2 . . ?
C14 C15 H15 119.4 . . ?
C16 C15 C14 121.3(3) . . ?
C16 C15 H15 119.4 . . ?
N30 C31 N27 111.7(2) . . ?
N30 C31 H31 124.2 . . ?
N27 C31 H31 124.2 . . ?
C25 C24 H24 119.7 . . ?
C25 C24 C23 120.6(3) . . ?
C23 C24 H24 119.7 . . ?
C22 C23 C24 120.3(3) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C18 C17 H17 119.7 . . ?
C18 C17 C16 120.6(3) . . ?
C16 C17 H17 119.7 . . ?
C15 C16 C17 120.4(3) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C5 N6 H6A 109.5 . . ?
C5 N6 H6B 110.4 . . ?
H6A N6 H6B 108.5 . . ?
C37 N38B H38A 120.0 . . ?
C37 N38B H38B 120.0 . . ?
H38A N38B H38B 120.0 . . ?
C37 N38A H38C 120.0 . . ?
C37 N38A H38D 120.0 . . ?
H38C N38A H38D 120.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O40 H40A O33 0.87 1.90 2.716(3) 154.8 2_876
O40 H40B O2 0.87 2.00 2.851(3) 164.7 2_766
O39 H39A O1 0.87 2.01 2.873(3) 168.7 1_666
O39 H39B O40 0.87 2.02 2.877(3) 168.5 .
N6 H6B O2 0.89 1.94 2.636(5) 134.3 .

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 O1 C3 O2 2.4(3) . . . . ?
Cu1 O1 C3 C4 -176.59(16) . . . . ?
Cu1 N8 C9 C10 177.3(2) . . . . ?
Cu1 N8 C12 N11 -178.10(19) . . . . ?
Cu2 O32 C34 O33 6.3(4) . . . . ?
Cu2 O32 C34 C35 -172.84(16) . . . . ?
Cu2 N30 C29 C28 -177.8(2) . . . . ?
Cu2 N30 C31 N27 177.0(2) . . . . ?
N30 C29 C28 N27 0.8(4) . . . . ?
N8 C9 C10 N11 0.3(4) . . . . ?
N11 C13 C26 C21 177.1(2) . . . . ?
N11 C13 C26 C25 -3.1(4) . . . . ?
N11 C13 C14 C19 -178.3(2) . . . . ?
N11 C13 C14 C15 1.2(4) . . . . ?
N27 C20 C21 C26 -179.2(2) . . . . ?
N27 C20 C21 C22 0.3(4) . . . . ?
C13 N11 C12 N8 -177.8(3) . . . . ?
C13 N11 C10 C9 178.3(3) . . . . ?
C13 C26 C21 C20 1.0(3) . . . . ?
C13 C26 C21 C22 -178.5(2) . . . . ?
C13 C26 C25 C24 178.8(2) . . . . ?
C13 C14 C15 C16 179.9(3) . . . . ?
C4 C5 C7 C4 -0.7(4) . . . 2 ?
C3 C4 C5 C7 -178.4(2) . . . . ?
C3 C4 C5 N6 6.9(5) . . . . ?
C26 C13 C14 C19 0.5(4) . . . . ?
C26 C13 C14 C15 180.0(2) . . . . ?
C26 C21 C22 C23 -1.0(4) . . . . ?
C26 C25 C24 C23 0.5(4) . . . . ?
C19 C18 C17 C16 0.1(4) . . . . ?
C19 C20 C21 C26 0.7(4) . . . . ?
C19 C20 C21 C22 -179.8(2) . . . . ?
C19 C14 C15 C16 -0.6(4) . . . . ?
C5 C4 C3 O1 -167.5(2) . . . . ?
C5 C4 C3 O2 13.5(4) . . . . ?
C7 C4 C3 O1 13.4(3) 2 . . . ?
C7 C4 C3 O2 -165.6(2) 2 . . . ?
C7 C4 C5 C7 0.7(4) 2 . . . ?
C7 C4 C5 N6 -174.0(4) 2 . . . ?
C35 C37 C36 C35 0.5(5) 2_866 . . . ?
C18 C19 C20 N27 -1.6(4) . . . . ?
C18 C19 C20 C21 178.5(2) . . . . ?
C18 C19 C14 C13 -179.1(2) . . . . ?
C18 C19 C14 C15 1.4(4) . . . . ?
C18 C17 C16 C15 0.8(5) . . . . ?
C9 N8 C12 N11 -1.2(3) . . . . ?
C20 N27 C28 C29 178.1(3) . . . . ?
C20 N27 C31 N30 -178.1(3) . . . . ?
C20 C19 C18 C17 178.5(3) . . . . ?
C20 C19 C14 C13 1.2(3) . . . . ?
C20 C19 C14 C15 -178.3(2) . . . . ?
C20 C21 C22 C23 179.4(3) . . . . ?
C12 N8 C9 C10 0.6(3) . . . . ?
C12 N11 C13 C26 98.2(3) . . . . ?
C12 N11 C13 C14 -83.0(3) . . . . ?
C12 N11 C10 C9 -1.0(3) . . . . ?
C14 C13 C26 C21 -1.6(4) . . . . ?
C14 C13 C26 C25 178.1(2) . . . . ?
C14 C19 C18 C17 -1.2(4) . . . . ?
C14 C19 C20 N27 178.1(2) . . . . ?
C14 C19 C20 C21 -1.8(4) . . . . ?
C14 C15 C16 C17 -0.5(5) . . . . ?
C34 C35 C36 C37 178.3(3) . . . . ?
C10 N11 C13 C26 -80.9(4) . . . . ?
C10 N11 C13 C14 97.9(3) . . . . ?
C10 N11 C12 N8 1.4(3) . . . . ?
C29 N30 C31 N27 -0.7(4) . . . . ?
C37 C35 C34 O32 -1.6(4) 2_866 . . . ?
C37 C35 C34 O33 179.3(3) 2_866 . . . ?
C37 C35 C36 C37 -0.6(5) 2_866 . . . ?
C21 C26 C25 C24 -1.5(4) . . . . ?
C21 C22 C23 C24 0.1(4) . . . . ?
C25 C26 C21 C20 -178.7(2) . . . . ?
C25 C26 C21 C22 1.7(3) . . . . ?
C25 C24 C23 C22 0.2(4) . . . . ?
C36 C35 C34 O32 179.6(2) . . . . ?
C36 C35 C34 O33 0.4(4) . . . . ?
C28 N27 C20 C19 -87.0(4) . . . . ?
C28 N27 C20 C21 92.9(4) . . . . ?
C28 N27 C31 N30 1.2(4) . . . . ?
C31 N30 C29 C28 -0.1(4) . . . . ?
C31 N27 C20 C19 92.2(4) . . . . ?
C31 N27 C20 C21 -87.9(4) . . . . ?
C31 N27 C28 C29 -1.2(4) . . . . ?
N6 C5 C7 C4 174.1(4) . . . 2 ?
N38B C37 C36 C35 169.7(11) . . . . ?
N38A C37 C36 C35 -150.7(7) . . . . ?

_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 1.255
_oxdiff_exptl_absorpt_empirical_full_min 0.789
####################################################################### 
# 
# 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_ebj-187b-meoh_abs_2
_database_code_depnum_ccdc_archive 'CCDC 2309443'
loop_
_audit_author_name
_audit_author_address
'Antti Marttinen'
;University of Jyvaskyla
Finland
;
_audit_update_record             
;
2023-11-21 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_audit_creation_date             2023-11-20
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(N O3), C20 H16 N4'
_chemical_formula_sum            'C20 H16 N6 O6'
_chemical_formula_weight         436.39
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20 H14 N6 O6'
_chemical_oxdiff_usercomment     'pale block'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   7.17230(10)
_cell_length_b                   10.30090(10)
_cell_length_c                   13.34380(10)
_cell_angle_alpha                90
_cell_angle_beta                 99.6960(10)
_cell_angle_gamma                90
_cell_volume                     971.773(18)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6750
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      77.3460
_cell_measurement_theta_min      5.4440
_shelx_estimated_absorpt_T_max   0.912
_shelx_estimated_absorpt_T_min   0.876
_exptl_absorpt_coefficient_mu    0.961
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             452
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 1 -2 0.0502
3 -4 -5 0.0613
-3 4 5 0.0411
2 5 -5 0.0591
-2 -5 5 0.0591
2 3 7 0.0582
3 0 5 0.0482
4 -2 2 0.0416
-3 0 -5 0.0515
-4 -4 1 0.0523
3 -3 -6 0.0539
0 -7 0 0.0594

_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.098
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-2.0004 1.0002 -2.0009 0.4968 -0.1817 -0.1480
2.8452 -4.4428 -4.5566 -0.1489 0.0536 0.9874
-2.8246 4.4426 4.6036 0.1418 -0.0510 -0.9886
2.3458 4.7611 -4.9178 0.4299 0.9008 0.0617
-2.3458 -4.7611 4.9178 -0.4299 -0.9008 -0.0617
1.6558 2.6941 6.6788 -0.7126 0.4365 -0.5493
3.3965 -0.2969 4.7624 -0.9022 0.4306 0.0251
4.0399 -2.0578 2.0655 -0.8143 0.3890 0.4308
-3.3538 0.2166 -4.8642 0.9025 -0.4307 -0.0068
-3.8334 -3.7962 1.0425 0.1819 -0.9826 -0.0386
3.0301 -2.9984 -6.1753 0.0599 0.2475 0.9670
-0.0694 -6.6839 -0.1924 -0.3222 -0.6758 0.6630

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10532
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.071
_diffrn_reflns_theta_min         5.455
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     41.00 118.00   0.50    1.00    --   52.72  65.00 130.00  154
  2  ω    -12.00  65.00   0.50    1.00    --   53.07 -65.00  -5.00  154
  3  ω     36.00 113.00   0.50    6.00    --  101.90 -65.00  -5.00  154
  4  ω     91.00 168.00   0.50    6.00    --  101.90  65.00 130.00  154
  5  ω    -46.00 -15.00   0.50    1.00    --    2.00 129.00 169.02   62
  6  ω    -13.00  31.00   0.50    1.00    --   14.00  95.00 136.96   88
  7  ω     12.00  41.00   0.50    1.00    --   38.00  92.00  13.96   58
  8  ω    -13.00  64.00   0.50    1.00    --   52.72 -65.00  -5.00  154
  9  ω     85.00 163.00   0.50    6.00    --  101.90  77.00  90.00  156
 10  ω     43.00 106.00   0.50    6.00    --  101.90 -99.00-150.00  126
 11  ω     43.00 106.00   0.50    6.00    --  101.90 -99.00   0.00  126
 12  ω     52.00 131.00   0.50    6.00    --  107.75 -87.00-168.46  158
 13  ω     36.00 112.00   0.50    6.00    --  107.75 -40.00  37.17  152
 14  ω     62.00 176.00   0.50    6.00    --  107.75  12.00-117.53  228
 15  ω     39.00 117.00   0.50    6.00    --  107.75 -54.00 170.84  156
 16  ω     37.00 114.00   0.50    6.00    --  107.75 -29.00 -55.49  154
 17  ω     39.00 141.00   0.50    6.00    --  107.75 -13.00 -12.03  204
 18  ω     49.00 126.00   0.50    1.00    --   62.00  71.00-105.58  154
 19  ω     63.00 141.00   0.50    1.00    --   74.00  62.00  22.27  156
 20  ω     69.00 147.00   0.50    1.00    --   78.00  51.00 -29.96  156
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1255097000
_diffrn_orient_matrix_UB_12      0.0522860000
_diffrn_orient_matrix_UB_13      -0.0966687000
_diffrn_orient_matrix_UB_21      0.1538460000
_diffrn_orient_matrix_UB_22      0.0998819000
_diffrn_orient_matrix_UB_23      -0.0130802000
_diffrn_orient_matrix_UB_31      0.0897442000
_diffrn_orient_matrix_UB_32      -0.0982581000
_diffrn_orient_matrix_UB_33      -0.0648555000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1878
_reflns_number_total             2060
_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2060
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0377
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0514P)²+0.3327P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1034
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C8(H8), C11(H11), C10(H10), C9(H9), C5(H5), C4(H4)
;
_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
O13 O 0.10830(13) 0.36470(9) 0.60948(7) 0.0299(2) Uani 1 1 d . . . . .
N3 N 0.27227(14) 0.80941(10) 0.57098(7) 0.0213(2) Uani 1 1 d . . . . .
N1 N 0.15841(15) 0.62403(10) 0.60544(8) 0.0244(2) Uani 1 1 d . . . . .
H1 H 0.1404 0.5397 0.6087 0.029 Uiso 1 1 calc R U . . .
O16 O 0.36281(16) 0.38613(11) 0.54426(10) 0.0473(3) Uani 1 1 d . . . . .
N14 N 0.25065(15) 0.31327(11) 0.57993(8) 0.0283(3) Uani 1 1 d . . . . .
O15 O 0.27263(17) 0.19501(11) 0.58674(10) 0.0508(3) Uani 1 1 d . . . . .
C7 C 0.54281(16) 0.95536(11) 0.60196(8) 0.0203(3) Uani 1 1 d . . . . .
C2 C 0.28682(17) 0.68113(11) 0.55956(9) 0.0208(2) Uani 1 1 d . . . . .
H2 H 0.3741 0.6382 0.5246 0.025 Uiso 1 1 calc R U . . .
C6 C 0.38960(16) 0.90601(11) 0.53428(9) 0.0203(3) Uani 1 1 d . . . . .
C12 C 0.34215(16) 0.94689(11) 0.43324(9) 0.0203(3) Uani 1 1 d . . . . .
C8 C 0.58942(18) 0.91214(12) 0.70507(9) 0.0242(3) Uani 1 1 d . . . . .
H8 H 0.5142 0.8475 0.7297 0.029 Uiso 1 1 calc R U . . .
C11 C 0.81441(17) 1.10489(12) 0.63532(9) 0.0238(3) Uani 1 1 d . . . . .
H11 H 0.8914 1.1703 0.6131 0.029 Uiso 1 1 calc R U . . .
C10 C 0.85326(18) 1.06032(13) 0.73285(9) 0.0276(3) Uani 1 1 d . . . . .
H10 H 0.9578 1.0952 0.7780 0.033 Uiso 1 1 calc R U . . .
C9 C 0.74062(19) 0.96298(13) 0.76807(9) 0.0284(3) Uani 1 1 d . . . . .
H9 H 0.7709 0.9330 0.8362 0.034 Uiso 1 1 calc R U . . .
C5 C 0.05802(19) 0.71764(13) 0.64703(11) 0.0318(3) Uani 1 1 d . . . . .
H5 H -0.0423 0.7032 0.6839 0.038 Uiso 1 1 calc R U . . .
C4 C 0.12890(19) 0.83433(13) 0.62552(11) 0.0320(3) Uani 1 1 d . . . . .
H4 H 0.0879 0.9172 0.6443 0.038 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
O13 N14 1.2705(13) . ?
N3 C2 1.3362(15) . ?
N3 C6 1.4411(14) . ?
N3 C4 1.3802(16) . ?
N1 H1 0.8800 . ?
N1 C2 1.3262(15) . ?
N1 C5 1.3750(17) . ?
O16 N14 1.2514(15) . ?
N14 O15 1.2297(16) . ?
C7 C6 1.3955(17) . ?
C7 C12 1.4304(16) 3_676 ?
C7 C8 1.4311(16) . ?
C2 H2 0.9500 . ?
C6 C12 1.3987(16) . ?
C12 C7 1.4303(16) 3_676 ?
C12 C11 1.4270(16) 3_676 ?
C8 H8 0.9500 . ?
C8 C9 1.3602(18) . ?
C11 C12 1.4270(16) 3_676 ?
C11 H11 0.9500 . ?
C11 C10 1.3638(17) . ?
C10 H10 0.9500 . ?
C10 C9 1.4167(19) . ?
C9 H9 0.9500 . ?
C5 H5 0.9500 . ?
C5 C4 1.3545(19) . ?
C4 H4 0.9500 . ?

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
C2 N3 C6 125.64(10) . . ?
C2 N3 C4 108.87(10) . . ?
C4 N3 C6 125.48(10) . . ?
C2 N1 H1 125.5 . . ?
C2 N1 C5 109.08(10) . . ?
C5 N1 H1 125.5 . . ?
O16 N14 O13 118.00(11) . . ?
O15 N14 O13 119.34(11) . . ?
O15 N14 O16 122.66(11) . . ?
C6 C7 C12 118.61(10) . 3_676 ?
C6 C7 C8 122.68(11) . . ?
C12 C7 C8 118.72(11) 3_676 . ?
N3 C2 H2 125.9 . . ?
N1 C2 N3 108.20(10) . . ?
N1 C2 H2 125.9 . . ?
C7 C6 N3 118.21(10) . . ?
C7 C6 C12 123.46(11) . . ?
C12 C6 N3 118.31(10) . . ?
C6 C12 C7 117.93(11) . 3_676 ?
C6 C12 C11 122.88(11) . 3_676 ?
C11 C12 C7 119.19(10) 3_676 3_676 ?
C7 C8 H8 119.8 . . ?
C9 C8 C7 120.48(12) . . ?
C9 C8 H8 119.8 . . ?
C12 C11 H11 120.1 3_676 . ?
C10 C11 C12 119.88(12) . 3_676 ?
C10 C11 H11 120.1 . . ?
C11 C10 H10 119.4 . . ?
C11 C10 C9 121.24(11) . . ?
C9 C10 H10 119.4 . . ?
C8 C9 C10 120.49(11) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
N1 C5 H5 126.4 . . ?
C4 C5 N1 107.22(11) . . ?
C4 C5 H5 126.4 . . ?
N3 C4 H4 126.7 . . ?
C5 C4 N3 106.63(11) . . ?
C5 C4 H4 126.7 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O13 0.88 1.82 2.6971(14) 177.0 .

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
N3 C6 C12 C7 178.79(10) . . . 3_676 ?
N3 C6 C12 C11 -1.42(17) . . . 3_676 ?
N1 C5 C4 N3 -0.07(16) . . . . ?
C7 C6 C12 C7 -0.11(19) . . . 3_676 ?
C7 C6 C12 C11 179.68(11) . . . 3_676 ?
C7 C8 C9 C10 0.57(19) . . . . ?
C2 N3 C6 C7 -97.26(14) . . . . ?
C2 N3 C6 C12 83.77(14) . . . . ?
C2 N3 C4 C5 0.26(15) . . . . ?
C2 N1 C5 C4 -0.14(15) . . . . ?
C6 N3 C2 N1 178.45(10) . . . . ?
C6 N3 C4 C5 -178.54(11) . . . . ?
C6 C7 C8 C9 179.80(11) . . . . ?
C12 C7 C6 N3 -178.79(10) 3_676 . . . ?
C12 C7 C6 C12 0.11(19) 3_676 . . . ?
C12 C7 C8 C9 -0.19(18) 3_676 . . . ?
C12 C11 C10 C9 -0.08(19) 3_676 . . . ?
C8 C7 C6 N3 1.22(17) . . . . ?
C8 C7 C6 C12 -179.88(11) . . . . ?
C11 C10 C9 C8 -0.4(2) . . . . ?
C5 N1 C2 N3 0.30(14) . . . . ?
C4 N3 C2 N1 -0.35(14) . . . . ?
C4 N3 C6 C7 81.34(15) . . . . ?
C4 N3 C6 C12 -97.62(15) . . . . ?

_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 1.262
_oxdiff_exptl_absorpt_empirical_full_min 0.848
####################################################################### 
# 
# 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_ebj-165-b_1r_abs
_database_code_depnum_ccdc_archive 'CCDC 2309436'
loop_
_audit_author_name
_audit_author_address
'Antti Marttinen'
;University of Jyvaskyla
Finland
;
_audit_update_record             
;
2023-11-21 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_audit_creation_date             2023-11-20
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C56 H38 N10 Ni2 O8, 5(H2 O)'
_chemical_formula_sum            'C56 H48 N10 Ni2 O13'
_chemical_formula_weight         1186.46
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20 H20 N6 Ni1 O4'
_chemical_oxdiff_usercomment     'no. 60'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   10.1841(2)
_cell_length_b                   22.1378(4)
_cell_length_c                   12.2623(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.771(2)
_cell_angle_gamma                90
_cell_volume                     2745.30(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8745
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      75.5680
_cell_measurement_theta_min      4.1240
_shelx_estimated_absorpt_T_max   0.985
_shelx_estimated_absorpt_T_min   0.843
_exptl_absorpt_coefficient_mu    1.477
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plank
_exptl_crystal_F_000             1228
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 14 -2 0.0119
0 -14 2 0.0019
-7 0 1 0.0456
7 -1 -1 0.0640
-2 -6 -7 0.0043
2 6 7 0.0060

_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.021
_exptl_crystal_size_min          0.01
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.0689 13.5565 -2.1348 -0.0614 0.3449 0.9366
0.4355 -13.7106 2.2440 0.0777 -0.4320 -0.8985
-6.6089 -0.3518 0.9062 0.1599 -0.8639 0.4777
6.5809 -1.1034 -1.3802 -0.2380 0.8049 -0.5437
-1.6818 -6.2474 -6.5898 -0.8782 -0.4782 -0.0089
1.6818 6.2474 6.5898 0.8782 0.4782 0.0089

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            30247
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.555
_diffrn_reflns_theta_min         3.994
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -83.00 -51.00   1.00   14.00    --  -48.63 -44.00 174.00   32
  2  ω    -23.00  29.00   1.00   14.00    --  -48.63  44.00 -35.00   52
  3  ω     51.00  96.00   1.00   14.00    --   49.50  44.00 -35.00   45
  4  ω    -28.00  53.00   1.00   14.00    --   49.50 -44.00 174.00   81
  5  ω   -125.00 -99.00   1.00   36.00    --  -88.21 -44.00 174.00   26
  6  ω    -45.00 -17.00   1.00   36.00    --  -88.21  44.00 -35.00   28
  7  ω    125.00 175.00   1.00   36.00    --  104.82  44.00 -35.00   50
  8  ω     27.00  52.00   1.00   36.00    --  104.82 -44.00 174.00   25
  9  ω   -120.00 -74.00   1.00   14.00    --  -48.63-125.00 -30.00   46
 10  ω    -38.00 -11.00   1.00   36.00    --  -88.21  45.00 -90.00   27
 11  ω    -44.00 -11.00   1.00   36.00    --  -88.21  45.00  60.00   33
 12  ω   -127.00 -87.00   1.00   36.00    --  -88.21 -95.00 -60.00   40
 13  ω    -47.00 -22.00   1.00   36.00    --  -88.21  45.00 -60.00   25
 14  ω    -44.00 -15.00   1.00   36.00    --  -88.21  45.00  90.00   29
 15  ω    -41.00 -10.00   1.00   36.00    --  -88.21  45.00  30.00   31
 16  ω    -46.00 -13.00   1.00   36.00    --  -88.21  45.00   0.00   33
 17  ω    -47.00 -11.00   1.00   36.00    --  -88.21  45.00-120.00   36
 18  ω    -62.00 -15.00   1.00   36.00    --  -88.21  61.00 120.00   47
 19  ω    127.00 175.00   1.00   36.00    --  104.82  30.00   0.00   48
 20  ω     44.00  70.00   1.00   36.00    --  104.82 -95.00 150.00   26
 21  ω    138.00 171.00   1.00   36.00    --  104.82  45.00-150.00   33
 22  ω     49.00  74.00   1.00   36.00    --  104.82 -61.00-150.00   25
 23  ω     39.00  95.00   1.00   36.00    --  104.82 -95.00  30.00   56
 24  ω     48.00  77.00   1.00   36.00    --  104.82 -77.00-150.00   29
 25  ω     95.00 121.00   1.00   36.00    --  104.82  45.00-150.00   26
 26  ω     27.00  53.00   1.00   36.00    --  104.82 -45.00 120.00   26
 27  ω     57.00  94.00   1.00   36.00    --  104.82 -95.00  90.00   37
 28  ω     32.00  74.00   1.00   36.00    --  104.82 -61.00  30.00   42
 29  ω    132.00 158.00   1.00   36.00    --  104.82 125.00  30.00   26
 30  ω     38.00  64.00   1.00   36.00    --  104.82 -95.00 -30.00   26
 31  ω     67.00 102.00   1.00   36.00    --  104.82 -95.00 -30.00   35
 32  ω     54.00 131.00   1.00   36.00    --  104.82  15.00 -30.00   77
 33  ω    140.00 166.00   1.00   36.00    --  104.82  30.00  90.00   26
 34  ω     80.00 105.00   1.00   36.00    --  104.82 -95.00 150.00   25
 35  ω    137.00 162.00   1.00   36.00    --  104.82  30.00-120.00   25
 36  ω     95.00 167.00   1.00   36.00    --  104.82  15.00  60.00   72
 37  ω     41.00  67.00   1.00   36.00    --  104.82 -61.00  60.00   26
 38  ω     59.00  85.00   1.00   36.00    --  104.82  15.00 150.00   26
 39  ω    103.00 133.00   1.00   36.00    --  104.82  30.00-120.00   30
 40  ω     41.00  67.00   1.00   36.00    --  104.82  15.00  60.00   26
 41  ω    100.00 178.00   1.00   36.00    --  104.82  15.00 150.00   78
 42  ω     95.00 120.00   1.00   36.00    --  104.82  45.00  90.00   25
 43  ω     28.00  54.00   1.00   36.00    --  104.82 -45.00  90.00   26
 44  ω     88.00 114.00   1.00   36.00    --  104.82 125.00  30.00   26
 45  ω     27.00  52.00   1.00   36.00    --  104.82 -45.00 -30.00   25
 46  ω     27.00  52.00   1.00   36.00    --  104.82 -45.00   0.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0082104000
_diffrn_orient_matrix_UB_12      0.0140450000
_diffrn_orient_matrix_UB_13      0.1220491000
_diffrn_orient_matrix_UB_21      0.1294561000
_diffrn_orient_matrix_UB_22      0.0364372000
_diffrn_orient_matrix_UB_23      0.0049829000
_diffrn_orient_matrix_UB_31      -0.0798503000
_diffrn_orient_matrix_UB_32      0.0576151000
_diffrn_orient_matrix_UB_33      -0.0328849000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4147
_reflns_number_total             5747
_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         5747
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0572
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0494P)²+4.2789P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1377
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N22-H22B = N22-H22A
 0.99 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O40A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O38B(0.3) H38A(0.3) H38B(0.3) O38A(0.7) H38C(0.7) H38D(0.7)
 O40A(0.5) H40A(0.5) H40B(0.5)
5.a Free rotating group:
 O39(H39A,H39B), O38B(H38A,H38B), O38A(H38C,H38D), O40A(H40A,H40B)
5.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C27(H27), C19(H19), C21(H21), C2(H2), C8(H8), C36(H36), C11(H11),
 C4(H4), C33(H33), C5(H5), C30(H30), C9(H9), C10(H10), C29(H29), C35(H35),
 C34(H34)
;
_atom_sites_solution_hydrogens   mixed
_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 0.30694(5) 0.28521(2) 0.62713(4) 0.01859(14) Uani 1 1 d . . . . .
O13 O 0.4981(2) 0.27103(10) 0.68176(19) 0.0242(5) Uani 1 1 d . . . . .
O24 O 1.1020(2) 0.29019(10) 0.61657(17) 0.0227(5) Uani 1 1 d . . . . .
O25 O 1.2027(2) 0.25445(11) 0.77192(19) 0.0285(5) Uani 1 1 d . . . . .
O15 O 0.6126(2) 0.33426(12) 0.5862(2) 0.0365(6) Uani 1 1 d . . . . .
O39 O 1.5292(3) 0.12896(13) 0.9547(2) 0.0395(6) Uani 1 1 d G . . . .
H39A H 1.5370 0.1542 1.0095 0.059 Uiso 1 1 d G U . . .
H39B H 1.4454 0.1295 0.9305 0.059 Uiso 1 1 d G U . . .
N26 N 0.3178(3) 0.37082(12) 0.6918(2) 0.0236(6) Uani 1 1 d . . . . .
N3 N 0.3557(3) 0.10570(12) 0.5366(2) 0.0279(6) Uani 1 1 d . . . . .
N1 N 0.2968(3) 0.19770(12) 0.5747(2) 0.0229(6) Uani 1 1 d . . . . .
N22 N 0.8214(3) 0.17592(13) 0.9717(2) 0.0245(6) Uani 1 1 d D . . . .
N28 N 0.3785(3) 0.44298(13) 0.8097(2) 0.0264(6) Uani 1 1 d . . . . .
C18 C 0.8316(3) 0.21325(14) 0.8771(2) 0.0211(6) Uani 1 1 d . . . . .
C17 C 0.7185(3) 0.23576(14) 0.8161(3) 0.0212(6) Uani 1 1 d . . . . .
H17 H 0.6339 0.2269 0.8376 0.025 Uiso 1 1 calc R U . . .
C14 C 0.6039(3) 0.29513(14) 0.6578(3) 0.0213(6) Uani 1 1 d . . . . .
C16 C 0.7284(3) 0.27130(14) 0.7237(2) 0.0202(6) Uani 1 1 d . . . . .
C20 C 0.9658(3) 0.26016(15) 0.7515(3) 0.0218(6) Uani 1 1 d . . . . .
C27 C 0.3992(3) 0.38539(15) 0.7789(3) 0.0255(7) Uani 1 1 d . . . . .
H27 H 0.4637 0.3591 0.8153 0.031 Uiso 1 1 calc R U . . .
C19 C 0.9555(3) 0.22626(15) 0.8459(3) 0.0231(7) Uani 1 1 d . . . . .
H19 H 1.0331 0.2120 0.8888 0.028 Uiso 1 1 calc R U . . .
C31 C 0.4409(3) 0.47181(14) 0.9067(3) 0.0230(7) Uani 1 1 d . . . . .
C32 C 0.5313(3) 0.51840(15) 0.8946(3) 0.0245(7) Uani 1 1 d . . . . .
C37 C 0.4074(3) 0.45234(14) 1.0084(3) 0.0242(7) Uani 1 1 d . . . . .
C21 C 0.8520(3) 0.28307(14) 0.6907(2) 0.0202(6) Uani 1 1 d . . . . .
H21 H 0.8590 0.3066 0.6269 0.024 Uiso 1 1 calc R U . . .
C2 C 0.3973(3) 0.16107(14) 0.5676(3) 0.0252(7) Uani 1 1 d . . . . .
H2 H 0.4875 0.1725 0.5827 0.030 Uiso 1 1 calc R U . . .
C7 C 0.4991(3) 0.02228(15) 0.6095(3) 0.0272(7) Uani 1 1 d . . . . .
C23 C 1.0974(3) 0.26903(15) 0.7129(3) 0.0230(7) Uani 1 1 d . . . . .
C6 C 0.4337(3) 0.05259(14) 0.5184(3) 0.0267(7) Uani 1 1 d . . . . .
C12 C 0.4326(3) 0.03298(15) 0.4104(3) 0.0281(7) Uani 1 1 d . . . . .
C8 C 0.5019(4) 0.04298(16) 0.7199(3) 0.0325(8) Uani 1 1 d . . . . .
H8 H 0.4592 0.0798 0.7341 0.039 Uiso 1 1 calc R U . . .
C36 C 0.6851(3) 0.59549(15) 0.9798(3) 0.0303(8) Uani 1 1 d . . . . .
H36 H 0.7275 0.6154 1.0431 0.036 Uiso 1 1 calc R U . . .
C11 C 0.6300(4) -0.06537(16) 0.6820(3) 0.0327(8) Uani 1 1 d . . . . .
H11 H 0.6736 -0.1024 0.6705 0.039 Uiso 1 1 calc R U . . .
C4 C 0.2205(3) 0.10699(16) 0.5216(3) 0.0318(8) Uani 1 1 d . . . . .
H4 H 0.1632 0.0743 0.4991 0.038 Uiso 1 1 calc R U . . .
C33 C 0.5656(4) 0.53702(16) 0.7905(3) 0.0308(8) Uani 1 1 d . . . . .
H33 H 0.5268 0.5175 0.7256 0.037 Uiso 1 1 calc R U . . .
C5 C 0.1844(3) 0.16384(15) 0.5451(3) 0.0293(7) Uani 1 1 d . . . . .
H5 H 0.0960 0.1782 0.5418 0.035 Uiso 1 1 calc R U . . .
C30 C 0.2413(4) 0.42102(16) 0.6653(3) 0.0332(8) Uani 1 1 d . . . . .
H30 H 0.1730 0.4237 0.6057 0.040 Uiso 1 1 calc R U . . .
O38B O 1.2704(10) 0.1251(5) 0.8322(10) 0.043(2) Uani 0.3 1 d G . P A 2
H38A H 1.1954 0.1094 0.8447 0.065 Uiso 0.3 1 d G U P A 2
H38B H 1.2520 0.1629 0.8177 0.065 Uiso 0.3 1 d G U P A 2
C9 C 0.5646(4) 0.01101(17) 0.8051(3) 0.0348(8) Uani 1 1 d . . . . .
H9 H 0.5656 0.0257 0.8780 0.042 Uiso 1 1 calc R U . . .
C10 C 0.6289(4) -0.04456(17) 0.7857(3) 0.0371(9) Uani 1 1 d . . . . .
H10 H 0.6712 -0.0671 0.8458 0.044 Uiso 1 1 calc R U . . .
C29 C 0.2779(4) 0.46615(17) 0.7369(3) 0.0348(9) Uani 1 1 d . . . . .
H29 H 0.2416 0.5057 0.7370 0.042 Uiso 1 1 calc R U . . .
C35 C 0.7120(4) 0.61221(17) 0.8785(3) 0.0370(9) Uani 1 1 d . . . . .
H35 H 0.7715 0.6446 0.8714 0.044 Uiso 1 1 calc R U . . .
C34 C 0.6532(4) 0.58248(17) 0.7835(3) 0.0370(9) Uani 1 1 d . . . . .
H34 H 0.6754 0.5945 0.7136 0.044 Uiso 1 1 calc R U . . .
O38A O 1.2579(4) 0.1437(2) 0.8930(4) 0.0441(10) Uani 0.7 1 d G . P B 1
H38C H 1.2439 0.1770 0.8557 0.066 Uiso 0.7 1 d G U P B 1
H38D H 1.2227 0.1501 0.9533 0.066 Uiso 0.7 1 d G U P B 1
H22A H 0.740(3) 0.1528(19) 0.964(4) 0.053(13) Uiso 1 1 d D . . . .
H22B H 0.900(4) 0.151(2) 0.992(4) 0.076(17) Uiso 1 1 d D . . . .
O40A O 1.0438(12) 0.0625(4) 0.9752(7) 0.099(3) Uani 0.5 1 d G U P C 1
H40A H 1.0296 0.0399 1.0307 0.149 Uiso 0.5 1 d G U P C 1
H40B H 1.1295 0.0644 0.9783 0.149 Uiso 0.5 1 d G U P C 1


_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 O13 2.008(2) . ?
Ni1 O24 2.078(2) 1_455 ?
Ni1 O25 2.278(2) 1_455 ?
Ni1 N26 2.052(3) . ?
Ni1 N1 2.040(3) . ?
Ni1 N22 2.113(3) 4_565 ?
O13 C14 1.267(4) . ?
O24 Ni1 2.078(2) 1_655 ?
O24 C23 1.277(4) . ?
O25 Ni1 2.278(2) 1_655 ?
O25 C23 1.262(4) . ?
O15 C14 1.244(4) . ?
O39 H39A 0.8706 . ?
O39 H39B 0.8697 . ?
N26 C27 1.313(4) . ?
N26 C30 1.373(4) . ?
N3 C2 1.338(4) . ?
N3 C6 1.451(4) . ?
N3 C4 1.368(4) . ?
N1 C2 1.316(4) . ?
N1 C5 1.381(4) . ?
N22 Ni1 2.113(3) 4_666 ?
N22 C18 1.437(4) . ?
N22 H22A 0.973(19) . ?
N22 H22B 0.98(2) . ?
N28 C27 1.353(4) . ?
N28 C31 1.431(4) . ?
N28 C29 1.376(4) . ?
C18 C17 1.390(4) . ?
C18 C19 1.392(4) . ?
C17 H17 0.9500 . ?
C17 C16 1.393(4) . ?
C14 C16 1.516(4) . ?
C16 C21 1.392(4) . ?
C20 C19 1.394(4) . ?
C20 C21 1.397(4) . ?
C20 C23 1.486(4) . ?
C27 H27 0.9500 . ?
C19 H19 0.9500 . ?
C31 C32 1.403(5) . ?
C31 C37 1.399(5) . ?
C32 C37 1.431(4) 3_667 ?
C32 C33 1.424(5) . ?
C37 C32 1.431(5) 3_667 ?
C37 C36 1.436(5) 3_667 ?
C21 H21 0.9500 . ?
C2 H2 0.9500 . ?
C7 C6 1.401(5) . ?
C7 C12 1.442(5) 3_656 ?
C7 C8 1.427(5) . ?
C23 Ni1 2.513(3) 1_655 ?
C6 C12 1.393(5) . ?
C12 C7 1.442(5) 3_656 ?
C12 C11 1.426(5) 3_656 ?
C8 H8 0.9500 . ?
C8 C9 1.357(5) . ?
C36 C37 1.436(5) 3_667 ?
C36 H36 0.9500 . ?
C36 C35 1.355(5) . ?
C11 C12 1.426(5) 3_656 ?
C11 H11 0.9500 . ?
C11 C10 1.353(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.352(5) . ?
C33 H33 0.9500 . ?
C33 C34 1.355(5) . ?
C5 H5 0.9500 . ?
C30 H30 0.9500 . ?
C30 C29 1.353(5) . ?
O38B H38A 0.8691 . ?
O38B H38B 0.8717 . ?
C9 H9 0.9500 . ?
C9 C10 1.427(5) . ?
C10 H10 0.9500 . ?
C29 H29 0.9500 . ?
C35 H35 0.9500 . ?
C35 C34 1.408(6) . ?
C34 H34 0.9500 . ?
O38A H38C 0.8714 . ?
O38A H38D 0.8699 . ?
O40A H40A 0.8700 . ?
O40A H40B 0.8702 . ?

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
O13 Ni1 O24 162.97(9) . 1_455 ?
O13 Ni1 O25 102.48(9) . 1_455 ?
O13 Ni1 N26 90.55(10) . . ?
O13 Ni1 N1 88.16(10) . . ?
O13 Ni1 N22 101.34(10) . 4_565 ?
O24 Ni1 O25 60.50(8) 1_455 1_455 ?
O24 Ni1 N22 95.65(10) 1_455 4_565 ?
N26 Ni1 O24 89.02(10) . 1_455 ?
N26 Ni1 O25 89.07(10) . 1_455 ?
N26 Ni1 N22 88.05(11) . 4_565 ?
N1 Ni1 O24 91.01(10) . 1_455 ?
N1 Ni1 O25 87.19(10) . 1_455 ?
N1 Ni1 N26 175.69(11) . . ?
N1 Ni1 N22 96.23(11) . 4_565 ?
N22 Ni1 O25 156.03(10) 4_565 1_455 ?
C14 O13 Ni1 132.4(2) . . ?
C23 O24 Ni1 93.96(18) . 1_655 ?
C23 O25 Ni1 85.37(19) . 1_655 ?
H39A O39 H39B 104.6 . . ?
C27 N26 Ni1 122.8(2) . . ?
C27 N26 C30 106.2(3) . . ?
C30 N26 Ni1 130.8(2) . . ?
C2 N3 C6 128.7(3) . . ?
C2 N3 C4 107.4(3) . . ?
C4 N3 C6 123.9(3) . . ?
C2 N1 Ni1 126.5(2) . . ?
C2 N1 C5 106.0(3) . . ?
C5 N1 Ni1 127.4(2) . . ?
Ni1 N22 H22A 99(3) 4_666 . ?
Ni1 N22 H22B 98(3) 4_666 . ?
C18 N22 Ni1 120.9(2) . 4_666 ?
C18 N22 H22A 111(3) . . ?
C18 N22 H22B 113(3) . . ?
H22A N22 H22B 113(4) . . ?
C27 N28 C31 125.7(3) . . ?
C27 N28 C29 107.4(3) . . ?
C29 N28 C31 126.6(3) . . ?
C17 C18 N22 120.4(3) . . ?
C17 C18 C19 119.9(3) . . ?
C19 C18 N22 119.7(3) . . ?
C18 C17 H17 119.8 . . ?
C18 C17 C16 120.3(3) . . ?
C16 C17 H17 119.8 . . ?
O13 C14 C16 114.2(3) . . ?
O15 C14 O13 126.2(3) . . ?
O15 C14 C16 119.6(3) . . ?
C17 C16 C14 119.6(3) . . ?
C21 C16 C17 119.8(3) . . ?
C21 C16 C14 120.5(3) . . ?
C19 C20 C21 120.0(3) . . ?
C19 C20 C23 119.6(3) . . ?
C21 C20 C23 120.3(3) . . ?
N26 C27 N28 110.8(3) . . ?
N26 C27 H27 124.6 . . ?
N28 C27 H27 124.6 . . ?
C18 C19 C20 120.0(3) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C32 C31 N28 118.2(3) . . ?
C37 C31 N28 118.2(3) . . ?
C37 C31 C32 123.6(3) . . ?
C31 C32 C37 118.2(3) . 3_667 ?
C31 C32 C33 122.8(3) . . ?
C33 C32 C37 119.0(3) . 3_667 ?
C31 C37 C32 118.2(3) . 3_667 ?
C31 C37 C36 123.3(3) . 3_667 ?
C32 C37 C36 118.5(3) 3_667 3_667 ?
C16 C21 C20 119.9(3) . . ?
C16 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
N3 C2 H2 124.4 . . ?
N1 C2 N3 111.2(3) . . ?
N1 C2 H2 124.4 . . ?
C6 C7 C12 117.7(3) . 3_656 ?
C6 C7 C8 123.9(3) . . ?
C8 C7 C12 118.4(3) . 3_656 ?
O24 C23 Ni1 55.58(15) . 1_655 ?
O24 C23 C20 118.4(3) . . ?
O25 C23 Ni1 64.59(17) . 1_655 ?
O25 C23 O24 120.2(3) . . ?
O25 C23 C20 121.4(3) . . ?
C20 C23 Ni1 173.8(2) . 1_655 ?
C7 C6 N3 118.9(3) . . ?
C12 C6 N3 117.1(3) . . ?
C12 C6 C7 123.9(3) . . ?
C6 C12 C7 118.3(3) . 3_656 ?
C6 C12 C11 123.5(3) . 3_656 ?
C11 C12 C7 118.2(3) 3_656 3_656 ?
C7 C8 H8 119.4 . . ?
C9 C8 C7 121.2(3) . . ?
C9 C8 H8 119.4 . . ?
C37 C36 H36 120.0 3_667 . ?
C35 C36 C37 120.0(3) . 3_667 ?
C35 C36 H36 120.0 . . ?
C12 C11 H11 119.3 3_656 . ?
C10 C11 C12 121.5(3) . 3_656 ?
C10 C11 H11 119.3 . . ?
N3 C4 H4 126.7 . . ?
C5 C4 N3 106.6(3) . . ?
C5 C4 H4 126.7 . . ?
C32 C33 H33 119.9 . . ?
C34 C33 C32 120.3(3) . . ?
C34 C33 H33 119.9 . . ?
N1 C5 H5 125.6 . . ?
C4 C5 N1 108.8(3) . . ?
C4 C5 H5 125.6 . . ?
N26 C30 H30 125.1 . . ?
C29 C30 N26 109.9(3) . . ?
C29 C30 H30 125.1 . . ?
H38A O38B H38B 104.3 . . ?
C8 C9 H9 119.9 . . ?
C8 C9 C10 120.3(4) . . ?
C10 C9 H9 119.9 . . ?
C11 C10 C9 120.4(4) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
N28 C29 H29 127.1 . . ?
C30 C29 N28 105.8(3) . . ?
C30 C29 H29 127.1 . . ?
C36 C35 H35 119.4 . . ?
C36 C35 C34 121.3(4) . . ?
C34 C35 H35 119.4 . . ?
C33 C34 C35 120.9(4) . . ?
C33 C34 H34 119.5 . . ?
C35 C34 H34 119.5 . . ?
H38C O38A H38D 104.5 . . ?
H40A O40A H40B 104.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O39 H39A O24 0.87 1.86 2.711(3) 163.9 4_666
O39 H39B O38B 0.87 2.03 2.877(10) 163.3 .
O39 H39B O38A 0.87 1.94 2.796(5) 169.6 .
O38A H38C O25 0.87 2.02 2.887(5) 177.2 .
O38A H38D O15 0.87 2.11 2.977(6) 172.3 4_666
O40A H40A O40A 0.87 2.39 2.99(2) 127.0 3_757

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 O13 C14 O15 -3.4(5) . . . . ?
Ni1 O13 C14 C16 177.94(19) . . . . ?
Ni1 O24 C23 O25 -0.2(3) 1_655 . . . ?
Ni1 O24 C23 C20 -178.1(3) 1_655 . . . ?
Ni1 O25 C23 O24 0.2(3) 1_655 . . . ?
Ni1 O25 C23 C20 178.0(3) 1_655 . . . ?
Ni1 N26 C27 N28 -174.8(2) . . . . ?
Ni1 N26 C30 C29 174.4(3) . . . . ?
Ni1 N1 C2 N3 176.2(2) . . . . ?
Ni1 N1 C5 C4 -176.4(3) . . . . ?
Ni1 N22 C18 C17 -85.2(3) 4_666 . . . ?
Ni1 N22 C18 C19 95.6(3) 4_666 . . . ?
O13 C14 C16 C17 -12.4(4) . . . . ?
O13 C14 C16 C21 165.5(3) . . . . ?
O15 C14 C16 C17 168.8(3) . . . . ?
O15 C14 C16 C21 -13.2(5) . . . . ?
N26 C30 C29 N28 -0.5(5) . . . . ?
N3 C6 C12 C7 -175.3(3) . . . 3_656 ?
N3 C6 C12 C11 6.2(5) . . . 3_656 ?
N3 C4 C5 N1 -0.1(4) . . . . ?
N22 C18 C17 C16 -179.2(3) . . . . ?
N22 C18 C19 C20 177.1(3) . . . . ?
N28 C31 C32 C37 179.4(3) . . . 3_667 ?
N28 C31 C32 C33 -1.5(5) . . . . ?
N28 C31 C37 C32 -179.4(3) . . . 3_667 ?
N28 C31 C37 C36 0.7(5) . . . 3_667 ?
C18 C17 C16 C14 179.6(3) . . . . ?
C18 C17 C16 C21 1.6(5) . . . . ?
C17 C18 C19 C20 -2.1(5) . . . . ?
C17 C16 C21 C20 -1.2(5) . . . . ?
C14 C16 C21 C20 -179.2(3) . . . . ?
C27 N26 C30 C29 0.4(4) . . . . ?
C27 N28 C31 C32 111.5(4) . . . . ?
C27 N28 C31 C37 -69.1(4) . . . . ?
C27 N28 C29 C30 0.4(4) . . . . ?
C19 C18 C17 C16 0.0(5) . . . . ?
C19 C20 C21 C16 -0.9(5) . . . . ?
C19 C20 C23 O24 167.1(3) . . . . ?
C19 C20 C23 O25 -10.8(5) . . . . ?
C31 N28 C27 N26 173.9(3) . . . . ?
C31 N28 C29 C30 -173.6(3) . . . . ?
C31 C32 C33 C34 179.7(3) . . . . ?
C32 C31 C37 C32 0.1(5) . . . 3_667 ?
C32 C31 C37 C36 -179.9(3) . . . 3_667 ?
C32 C33 C34 C35 -0.1(6) . . . . ?
C37 C31 C32 C37 -0.1(5) . . . 3_667 ?
C37 C31 C32 C33 179.1(3) . . . . ?
C37 C32 C33 C34 -1.1(5) 3_667 . . . ?
C37 C36 C35 C34 -1.7(5) 3_667 . . . ?
C21 C20 C19 C18 2.5(5) . . . . ?
C21 C20 C23 O24 -9.7(5) . . . . ?
C21 C20 C23 O25 172.4(3) . . . . ?
C2 N3 C6 C7 73.4(5) . . . . ?
C2 N3 C6 C12 -110.1(4) . . . . ?
C2 N3 C4 C5 -0.3(4) . . . . ?
C2 N1 C5 C4 0.5(4) . . . . ?
C7 C6 C12 C7 0.9(6) . . . 3_656 ?
C7 C6 C12 C11 -177.6(3) . . . 3_656 ?
C7 C8 C9 C10 -0.2(6) . . . . ?
C23 C20 C19 C18 -174.3(3) . . . . ?
C23 C20 C21 C16 176.0(3) . . . . ?
C6 N3 C2 N1 179.5(3) . . . . ?
C6 N3 C4 C5 -179.3(3) . . . . ?
C6 C7 C8 C9 178.6(3) . . . . ?
C12 C7 C6 N3 175.3(3) 3_656 . . . ?
C12 C7 C6 C12 -0.9(6) 3_656 . . . ?
C12 C7 C8 C9 -1.5(5) 3_656 . . . ?
C12 C11 C10 C9 -0.2(6) 3_656 . . . ?
C8 C7 C6 N3 -4.9(5) . . . . ?
C8 C7 C6 C12 178.9(3) . . . . ?
C8 C9 C10 C11 1.2(6) . . . . ?
C36 C35 C34 C33 1.5(6) . . . . ?
C4 N3 C2 N1 0.7(4) . . . . ?
C4 N3 C6 C7 -107.9(4) . . . . ?
C4 N3 C6 C12 68.6(5) . . . . ?
C5 N1 C2 N3 -0.7(4) . . . . ?
C30 N26 C27 N28 -0.1(4) . . . . ?
C29 N28 C27 N26 -0.2(4) . . . . ?
C29 N28 C31 C32 -75.6(4) . . . . ?
C29 N28 C31 C37 103.9(4) . . . . ?

_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 2.054
_oxdiff_exptl_absorpt_empirical_full_min 0.561
####################################################################### 
# 
# 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_ebj-177e_r_abs_2
_database_code_depnum_ccdc_archive 'CCDC 2309438'
loop_
_audit_author_name
_audit_author_address
'Antti Marttinen'
;University of Jyvaskyla
Finland
;
_audit_update_record             
;
2023-11-21 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_audit_creation_date             2023-11-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C48 H32 N9 Ni O4, C28 H22 N5 Ni O6, 0.5(H2 O)'
_chemical_formula_sum            'C76 H55 N14 Ni2 O10.50'
_chemical_formula_weight         1449.76
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H20 N6 O6 Ni1'
_chemical_oxdiff_usercomment     'green rod'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   11.2569(11)
_cell_length_b                   13.4025(17)
_cell_length_c                   13.5086(13)
_cell_angle_alpha                61.328(11)
_cell_angle_beta                 71.172(9)
_cell_angle_gamma                75.382(10)
_cell_volume                     1680.8(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    5691
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      78.4760
_cell_measurement_theta_min      3.7840
_shelx_estimated_absorpt_T_max   0.979
_shelx_estimated_absorpt_T_min   0.879
_exptl_absorpt_coefficient_mu    1.309
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plank
_exptl_crystal_F_000             749
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 0 -8 0.0106
-7 -3 -2 0.0548
7 1 2 0.0425
0 0 8 0.0123
0 0 -8 0.0053
0 -8 -4 0.0085
0 8 4 0.0076

_exptl_crystal_size_max          0.101
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.016
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.6562 0.3718 -7.5064 -0.0411 0.4851 0.8735
-7.1524 -2.6302 -1.5076 0.1163 0.8826 -0.4554
7.2247 0.9688 1.9458 0.0750 -0.9487 0.3070
-0.0623 0.1325 7.5125 -0.0647 -0.2580 -0.9640
-0.2780 -0.0217 -7.5488 0.0427 0.3046 0.9515
0.4165 -8.2774 -3.5986 0.9916 -0.1293 0.0089
-0.4165 8.2774 3.5986 -0.9916 0.1293 -0.0089

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0842
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24885
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.994
_diffrn_reflns_theta_min         3.785
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00  16.00   2.00    2.00    --  -51.06  87.00  46.00   45
  2  ω     19.00  47.00   2.00    2.00    --   51.81 -87.00 -70.00   14
  3  ω   -105.00 -75.00   2.00    9.00    --  -87.69  87.00  46.00   15
  4  ω   -154.00 -82.00   2.00    9.00    --  -87.69 -87.00 -70.00   36
  5  ω    140.00 166.00   2.00    9.00    --  101.97  87.00  46.00   13
  6  ω     83.00 131.00   2.00    9.00    --  101.97 -87.00 -70.00   24
  7  ω    -20.00  14.00   2.00    2.00    --   18.00 102.00  99.85   17
  8  ω     12.00  42.00   2.00    2.00    --   42.00  87.00-168.46   15
  9  ω     -2.00  24.00   2.00    2.00    --  -51.06  19.00 -90.00   13
 10  ω     37.00 125.00   2.00    2.00    --   58.00  75.00 -44.93   44
 11  ω   -136.00 -50.00   2.00    2.00    --  -66.00 -71.00 131.43   43
 12  ω   -153.00 -87.00   2.00    9.00    --  -87.69 -99.00  60.00   33
 13  ω     43.00 105.00   2.00    9.00    --  101.97 -99.00  90.00   31
 14  ω     25.00  51.00   2.00    9.00    --  101.97 -38.00-180.00   13
 15  ω     63.00  89.00   2.00    9.00    --  101.97-125.00  60.00   13
 16  ω     28.00  78.00   2.00    9.00    --  101.97 -57.00 -60.00   25
 17  ω     35.00  61.00   2.00    9.00    --  101.97 -57.00   0.00   13
 18  ω     30.00  76.00   2.00    9.00    --  101.97 -57.00-180.00   23
 19  ω     25.00  51.00   2.00    9.00    --  101.97 -38.00-150.00   13
 20  ω     68.00  94.00   2.00    9.00    --  101.97-125.00 -90.00   13
 21  ω     90.00 176.00   2.00    9.00    --  107.25  57.00 101.10   43
 22  ω    144.00 174.00   2.00    9.00    --  107.25  80.00 -13.95   15
 23  ω    129.00 175.00   2.00    9.00    --  107.25  60.00-167.89   23
 24  ω     86.00 118.00   2.00    9.00    --  107.25  80.00 -13.95   16
 25  ω    110.00 174.00   2.00    9.00    --  107.25  71.00  56.75   32
 26  ω    105.00 131.00   2.00    9.00    --  107.25 -83.00-117.80   13
 27  ω     77.00 105.00   2.00    9.00    --  107.25-100.00-127.38   14
 28  ω    137.00 175.00   2.00    9.00    --  107.25   7.00  59.06   19
 29  ω     42.00  82.00   2.00    9.00    --  107.25   7.00  59.06   20
 30  ω     41.00  77.00   2.00    9.00    --  107.25 -83.00-117.80   18
 31  ω     74.00 120.00   2.00    9.00    --  107.25-136.00-107.64   23
 32  ω     42.00  88.00   2.00    9.00    --  107.25 -72.00 -90.28   23
 33  ω     68.00 108.00   2.00    9.00    --  107.25-113.00  35.90   20
 34  ω     93.00 123.00   2.00    9.00    --  107.25  64.00 151.05   15
 35  ω     40.00 106.00   2.00    9.00    --  107.25 -99.00 -44.94   33
 36  ω     48.00  74.00   2.00    9.00    --  107.25-115.00   7.27   13
 37  ω    147.00 173.00   2.00    9.00    --  107.25  49.00 -96.87   13
 38  ω     67.00  95.00   2.00    9.00    --  107.25 -68.00  42.37   14
 39  ω     46.00 106.00   2.00    9.00    --  107.25-100.00 155.07   30
 40  ω    100.00 128.00   2.00    9.00    --  107.25  49.00 -96.87   14
 41  ω     99.00 173.00   2.00    9.00    --  107.25 106.00 -53.07   37
 42  ω     87.00 173.00   2.00    9.00    --  107.25  71.00 166.11   43
 43  ω     80.00 108.00   2.00    9.00    --  107.25-117.00 -65.39   14
 44  ω    148.00 176.00   2.00    9.00    --  107.25 107.00 175.02   14
 45  ω     54.00 106.00   2.00    9.00    --  107.25-104.00 139.77   26
 46  ω    144.00 170.00   2.00    9.00    --  107.25  64.00 151.05   13
 47  ω     55.00  81.00   2.00    9.00    --  107.25 -75.00 136.45   13
 48  ω     92.00 118.00   2.00    9.00    --  107.25 -84.00  -3.44   13
 49  ω     91.00 145.00   2.00    9.00    --  107.25  28.00 157.65   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0276022000
_diffrn_orient_matrix_UB_12      -0.1156439000
_diffrn_orient_matrix_UB_13      -0.0063452000
_diffrn_orient_matrix_UB_21      -0.1250145000
_diffrn_orient_matrix_UB_22      0.0249040000
_diffrn_orient_matrix_UB_23      -0.0358146000
_diffrn_orient_matrix_UB_31      0.0693442000
_diffrn_orient_matrix_UB_32      0.0583949000
_diffrn_orient_matrix_UB_33      -0.1287714000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4828
_reflns_number_total             6775
_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         0.867
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         6775
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0644
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0531P)²+2.0795P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1493
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: N7(0.5) H7A(0.5) H7B(0.5) N38(0.5) H38A(0.5) H38B(0.5) O52(0.25)
 H52A(0.25) H52B(0.25)
3.a Free rotating group:
 O52(H52A,H52B)
3.b Rotating group:
 O51(H51A,H51B), N7(H7A,H7B), N38(H38A,H38B)
3.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C21(H21), C12(H12), C5(H5), C11(H11), C15(H15), C18(H18), C49(H49),
 C42(H42), C46(H46), C36(H36), C17(H17), C40(H40), C24(H24), C43(H43), C27(H27),
  C16(H16), C47(H47), C23(H23), C30(H30), C48(H48), C28(H28), C29(H29)
;
_atom_sites_solution_hydrogens   mixed
_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 1.0000 0.5000 0.0000 0.01805(18) Uani 1 2 d S . P . .
Ni2 Ni 0.5000 1.0000 0.0000 0.0250(2) Uani 1 2 d S . P . .
O1 O 0.8216(2) 0.5396(2) -0.0288(2) 0.0248(5) Uani 1 1 d . . . . .
O32 O 0.3199(2) 1.0097(2) -0.0070(2) 0.0330(6) Uani 1 1 d . . . . .
O2 O 0.7062(2) 0.7095(2) -0.0623(2) 0.0333(6) Uani 1 1 d . . . . .
O51 O 0.5288(2) 0.8208(2) 0.0617(2) 0.0329(6) Uani 1 1 d . . . . .
H51A H 0.4653 0.7980 0.0577 0.049 Uiso 1 1 d R U . . .
H51B H 0.5936 0.8019 0.0149 0.049 Uiso 1 1 d R U . . .
N8 N 0.9357(2) 0.3535(2) 0.1457(2) 0.0222(6) Uani 1 1 d . . . . .
O33 O 0.3123(2) 0.8348(2) 0.0162(3) 0.0421(7) Uani 1 1 d . . . . .
N10 N 0.9303(3) 0.2027(2) 0.3138(2) 0.0276(6) Uani 1 1 d . . . . .
N20 N 0.9549(3) 0.5735(2) 0.1171(2) 0.0246(6) Uani 1 1 d . . . . .
N39 N 0.5697(3) 1.0161(3) -0.1669(3) 0.0314(7) Uani 1 1 d . . . . .
N22 N 0.9500(3) 0.5752(3) 0.2808(3) 0.0325(7) Uani 1 1 d . . . . .
N41 N 0.5793(3) 1.0125(3) -0.3276(3) 0.0381(8) Uani 1 1 d . . . . .
C3 C 0.7187(3) 0.6053(3) -0.0377(3) 0.0229(7) Uani 1 1 d . . . . .
C9 C 1.0040(3) 0.2653(3) 0.2089(3) 0.0236(7) Uani 1 1 d . . . . .
H9 H 1.0926 0.2474 0.1849 0.028 Uiso 1 1 calc R U . . .
C21 C 1.0088(3) 0.5299(3) 0.2056(3) 0.0256(7) Uani 1 1 d . . . . .
H21 H 1.0802 0.4734 0.2145 0.031 Uiso 1 1 calc R U . . .
C4 C 0.6068(3) 0.5493(3) -0.0180(3) 0.0246(7) Uani 1 1 d . . . . .
C19 C 1.0246(3) 0.1076(3) 0.4815(3) 0.0277(7) Uani 1 1 d . . . . .
C44 C 0.5376(4) 1.0062(4) -0.4160(3) 0.0355(9) Uani 1 1 d . . . . .
C25 C 0.9766(4) 0.5377(3) 0.3921(3) 0.0331(8) Uani 1 1 d . . . . .
C14 C 0.9436(3) -0.0046(3) 0.4222(3) 0.0273(7) Uani 1 1 d . . . . .
C6 C 0.3799(3) 0.5634(3) 0.0049(3) 0.0288(7) Uani 1 1 d . . . . .
C12 C 0.8129(3) 0.3479(3) 0.2114(3) 0.0310(8) Uani 1 1 d . . . . .
H12 H 0.7422 0.4008 0.1873 0.037 Uiso 1 1 calc R U . . .
C13 C 0.9689(3) 0.0997(3) 0.4074(3) 0.0263(7) Uani 1 1 d . . . . .
C31 C 1.0839(4) 0.5677(3) 0.3960(3) 0.0347(8) Uani 1 1 d . . . . .
C5 C 0.4875(3) 0.6104(3) -0.0137(3) 0.0289(7) Uani 1 1 d . . . . .
H5 H 0.4783 0.6868 -0.0236 0.035 Uiso 1 1 calc R U . . .
C11 C 0.8087(3) 0.2547(3) 0.3161(3) 0.0326(8) Uani 1 1 d . . . . .
H11 H 0.7363 0.2307 0.3781 0.039 Uiso 1 1 calc R U . . .
C45 C 0.4910(4) 1.1072(4) -0.4992(3) 0.0353(9) Uani 1 1 d . . . . .
C50 C 0.5477(4) 0.8975(4) -0.4114(3) 0.0360(9) Uani 1 1 d . . . . .
C34 C 0.2628(3) 0.9344(3) 0.0042(3) 0.0304(8) Uani 1 1 d . . . . .
C15 C 0.8876(4) -0.0113(3) 0.3451(3) 0.0353(8) Uani 1 1 d . . . . .
H15 H 0.8675 0.0562 0.2802 0.042 Uiso 1 1 calc R U . . .
C18 C 0.9486(4) -0.2138(3) 0.5348(3) 0.0343(8) Uani 1 1 d . . . . .
H18 H 0.9697 -0.2831 0.5976 0.041 Uiso 1 1 calc R U . . .
C26 C 0.8918(4) 0.4711(3) 0.4917(3) 0.0348(8) Uani 1 1 d . . . . .
C35 C 0.1267(3) 0.9669(3) 0.0016(3) 0.0309(8) Uani 1 1 d . . . . .
C49 C 0.5907(4) 0.7939(4) -0.3241(4) 0.0436(10) Uani 1 1 d . . . . .
H49 H 0.6151 0.7964 -0.2643 0.052 Uiso 1 1 calc R U . . .
C42 C 0.6951(4) 1.0296(4) -0.3361(4) 0.0438(10) Uani 1 1 d . . . . .
H42 H 0.7664 1.0384 -0.3997 0.053 Uiso 1 1 calc R U . . .
C46 C 0.4784(4) 1.2169(4) -0.5013(4) 0.0415(10) Uani 1 1 d . . . . .
H46 H 0.5001 1.2221 -0.4417 0.050 Uiso 1 1 calc R U . . .
C36 C 0.0640(3) 1.0628(3) 0.0188(3) 0.0347(8) Uani 1 1 d . . . . .
H36 H 0.1083 1.1055 0.0318 0.042 Uiso 1 1 calc R U . . .
C17 C 0.8926(4) -0.2157(3) 0.4601(4) 0.0398(9) Uani 1 1 d . . . . .
H17 H 0.8731 -0.2866 0.4729 0.048 Uiso 1 1 calc R U . . .
C40 C 0.5057(4) 1.0058(4) -0.2266(3) 0.0396(10) Uani 1 1 d . . . . .
H40 H 0.4188 0.9950 -0.2009 0.048 Uiso 1 1 calc R U . . .
C24 C 0.8558(4) 0.6516(3) 0.1372(3) 0.0365(9) Uani 1 1 d . . . . .
H24 H 0.7995 0.6972 0.0882 0.044 Uiso 1 1 calc R U . . .
C43 C 0.6898(4) 1.0317(4) -0.2361(3) 0.0399(9) Uani 1 1 d . . . . .
H43 H 0.7581 1.0423 -0.2166 0.048 Uiso 1 1 calc R U . . .
C27 C 0.7839(4) 0.4373(4) 0.4862(4) 0.0446(10) Uani 1 1 d . . . . .
H27 H 0.7666 0.4620 0.4131 0.053 Uiso 1 1 calc R U . . .
C16 C 0.8629(4) -0.1148(4) 0.3644(4) 0.0429(10) Uani 1 1 d . . . . .
H16 H 0.8255 -0.1187 0.3128 0.052 Uiso 1 1 calc R U . . .
C47 C 0.4366(4) 1.3132(4) -0.5858(4) 0.0460(11) Uani 1 1 d . . . . .
H47 H 0.4300 1.3850 -0.5852 0.055 Uiso 1 1 calc R U . . .
C37 C -0.0637(4) 1.0974(4) 0.0174(4) 0.0366(9) Uani 1 1 d . . . . .
C23 C 0.8516(4) 0.6530(4) 0.2386(4) 0.0437(10) Uani 1 1 d . . . . .
H23 H 0.7924 0.6985 0.2732 0.052 Uiso 1 1 calc R U . . .
C30 C 1.1690(4) 0.6371(4) 0.2955(4) 0.0455(10) Uani 1 1 d . . . . .
H30 H 1.1542 0.6642 0.2210 0.055 Uiso 1 1 calc R U . . .
C48 C 0.5978(5) 0.6914(4) -0.3239(4) 0.0488(11) Uani 1 1 d . . . . .
H48 H 0.6256 0.6229 -0.2639 0.059 Uiso 1 1 calc R U . . .
C28 C 0.7064(5) 0.3704(4) 0.5848(4) 0.0528(12) Uani 1 1 d . . . . .
H28 H 0.6363 0.3470 0.5799 0.063 Uiso 1 1 calc R U . . .
C29 C 1.2713(5) 0.6651(5) 0.3051(4) 0.0550(12) Uani 1 1 d . . . . .
H29 H 1.3288 0.7091 0.2368 0.066 Uiso 1 1 calc R U . . .
N7 N 0.2701(6) 0.6346(6) 0.0080(7) 0.0401(16) Uani 0.5 1 d . . P . .
H7A H 0.2052 0.5977 0.0258 0.048 Uiso 0.5 1 d R U P . .
H7B H 0.2591 0.6587 0.0615 0.048 Uiso 0.5 1 d R U P . .
N38 N -0.1239(7) 1.1908(7) 0.0422(8) 0.058(2) Uani 0.5 1 d . . P . .
H38A H -0.1901 1.2227 0.0104 0.070 Uiso 0.5 1 d R U P . .
H38B H -0.0720 1.2439 0.0129 0.070 Uiso 0.5 1 d R U P . .
O52 O 0.5626(19) 0.7075(19) 0.2900(18) 0.096(6) Uani 0.25 1 d G . P . .
H52A H 0.6276 0.6669 0.3182 0.144 Uiso 0.25 1 d G U P . .
H52B H 0.5214 0.6637 0.2851 0.144 Uiso 0.25 1 d G U 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
Ni1 O1 2.058(2) 2_765 ?
Ni1 O1 2.058(2) . ?
Ni1 N8 2.084(3) 2_765 ?
Ni1 N8 2.084(3) . ?
Ni1 N20 2.111(3) 2_765 ?
Ni1 N20 2.111(3) . ?
Ni2 O32 2.029(2) . ?
Ni2 O32 2.029(2) 2_675 ?
Ni2 O51 2.105(3) 2_675 ?
Ni2 O51 2.105(3) . ?
Ni2 N39 2.055(3) . ?
Ni2 N39 2.055(3) 2_675 ?
O1 C3 1.267(4) . ?
O32 C34 1.253(4) . ?
O2 C3 1.251(4) . ?
O51 H51A 0.8710 . ?
O51 H51B 0.8711 . ?
N8 C9 1.310(4) . ?
N8 C12 1.378(4) . ?
O33 C34 1.263(5) . ?
N10 C9 1.361(4) . ?
N10 C13 1.439(5) . ?
N10 C11 1.368(5) . ?
N20 C21 1.324(5) . ?
N20 C24 1.379(5) . ?
N39 C40 1.311(5) . ?
N39 C43 1.373(5) . ?
N22 C21 1.340(4) . ?
N22 C25 1.446(5) . ?
N22 C23 1.376(5) . ?
N41 C44 1.460(5) . ?
N41 C42 1.339(5) . ?
N41 C40 1.321(5) . ?
C3 C4 1.514(5) . ?
C9 H9 0.9500 . ?
C21 H21 0.9500 . ?
C4 C6 1.408(5) 2_665 ?
C4 C5 1.384(5) . ?
C19 C14 1.433(5) 2_756 ?
C19 C13 1.395(5) . ?
C19 C18 1.428(5) 2_756 ?
C44 C45 1.390(6) . ?
C44 C50 1.406(6) . ?
C25 C31 1.388(6) . ?
C25 C26 1.403(6) . ?
C14 C19 1.433(5) 2_756 ?
C14 C13 1.404(5) . ?
C14 C15 1.425(5) . ?
C6 C4 1.408(5) 2_665 ?
C6 C5 1.402(5) . ?
C6 N7 1.360(7) . ?
C12 H12 0.9500 . ?
C12 C11 1.362(5) . ?
C31 C26 1.445(5) 2_766 ?
C31 C30 1.423(6) . ?
C5 H5 0.9500 . ?
C11 H11 0.9500 . ?
C45 C50 1.442(5) 2_674 ?
C45 C46 1.427(6) . ?
C50 C45 1.442(5) 2_674 ?
C50 C49 1.418(6) . ?
C34 C35 1.491(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.368(6) . ?
C18 C19 1.428(5) 2_756 ?
C18 H18 0.9500 . ?
C18 C17 1.363(6) . ?
C26 C31 1.445(5) 2_766 ?
C26 C27 1.432(6) . ?
C35 C36 1.389(5) . ?
C35 C37 1.396(5) 2_575 ?
C49 H49 0.9500 . ?
C49 C48 1.355(6) . ?
C42 H42 0.9500 . ?
C42 C43 1.347(6) . ?
C46 H46 0.9500 . ?
C46 C47 1.349(7) . ?
C36 H36 0.9500 . ?
C36 C37 1.397(5) . ?
C17 H17 0.9500 . ?
C17 C16 1.408(6) . ?
C40 H40 0.9500 . ?
C24 H24 0.9500 . ?
C24 C23 1.364(6) . ?
C43 H43 0.9500 . ?
C27 H27 0.9500 . ?
C27 C28 1.356(6) . ?
C16 H16 0.9500 . ?
C47 H47 0.9500 . ?
C47 C48 1.424(7) 2_674 ?
C37 C35 1.396(5) 2_575 ?
C37 N38 1.403(9) . ?
C23 H23 0.9500 . ?
C30 H30 0.9500 . ?
C30 C29 1.357(7) . ?
C48 C47 1.424(7) 2_674 ?
C48 H48 0.9500 . ?
C28 H28 0.9500 . ?
C28 C29 1.416(7) 2_766 ?
C29 C28 1.416(7) 2_766 ?
C29 H29 0.9500 . ?
N7 H7A 0.8885 . ?
N7 H7B 0.8870 . ?
N38 H38A 0.8906 . ?
N38 H38B 0.8909 . ?
O52 H52A 0.8703 . ?
O52 H52B 0.8702 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 180.0 2_765 . ?
O1 Ni1 N8 86.97(10) . . ?
O1 Ni1 N8 93.03(10) 2_765 . ?
O1 Ni1 N8 93.04(10) . 2_765 ?
O1 Ni1 N8 86.96(10) 2_765 2_765 ?
O1 Ni1 N20 84.93(10) . 2_765 ?
O1 Ni1 N20 95.07(10) 2_765 2_765 ?
O1 Ni1 N20 84.93(10) 2_765 . ?
O1 Ni1 N20 95.07(10) . . ?
N8 Ni1 N8 180.0 2_765 . ?
N8 Ni1 N20 94.81(11) 2_765 . ?
N8 Ni1 N20 94.81(11) . 2_765 ?
N8 Ni1 N20 85.19(11) 2_765 2_765 ?
N8 Ni1 N20 85.19(11) . . ?
N20 Ni1 N20 180.0 2_765 . ?
O32 Ni2 O32 180.0 . 2_675 ?
O32 Ni2 O51 92.71(10) . . ?
O32 Ni2 O51 87.29(10) . 2_675 ?
O32 Ni2 O51 92.71(10) 2_675 2_675 ?
O32 Ni2 O51 87.29(10) 2_675 . ?
O32 Ni2 N39 88.20(11) 2_675 . ?
O32 Ni2 N39 91.80(11) . . ?
O32 Ni2 N39 91.80(11) 2_675 2_675 ?
O32 Ni2 N39 88.20(11) . 2_675 ?
O51 Ni2 O51 180.00(7) . 2_675 ?
N39 Ni2 O51 90.79(11) 2_675 . ?
N39 Ni2 O51 90.79(11) . 2_675 ?
N39 Ni2 O51 89.21(11) . . ?
N39 Ni2 O51 89.21(11) 2_675 2_675 ?
N39 Ni2 N39 180.0 2_675 . ?
C3 O1 Ni1 150.4(2) . . ?
C34 O32 Ni2 129.8(2) . . ?
Ni2 O51 H51A 109.4 . . ?
Ni2 O51 H51B 109.5 . . ?
H51A O51 H51B 104.4 . . ?
C9 N8 Ni1 127.2(2) . . ?
C9 N8 C12 106.5(3) . . ?
C12 N8 Ni1 123.9(2) . . ?
C9 N10 C13 127.8(3) . . ?
C9 N10 C11 107.8(3) . . ?
C11 N10 C13 124.5(3) . . ?
C21 N20 Ni1 121.7(2) . . ?
C21 N20 C24 105.6(3) . . ?
C24 N20 Ni1 131.4(3) . . ?
C40 N39 Ni2 124.9(2) . . ?
C40 N39 C43 105.8(3) . . ?
C43 N39 Ni2 129.2(3) . . ?
C21 N22 C25 125.5(3) . . ?
C21 N22 C23 107.1(3) . . ?
C23 N22 C25 127.0(3) . . ?
C42 N41 C44 126.4(3) . . ?
C40 N41 C44 124.6(3) . . ?
C40 N41 C42 109.0(3) . . ?
O1 C3 C4 115.0(3) . . ?
O2 C3 O1 124.7(3) . . ?
O2 C3 C4 120.3(3) . . ?
N8 C9 N10 110.5(3) . . ?
N8 C9 H9 124.8 . . ?
N10 C9 H9 124.8 . . ?
N20 C21 N22 111.7(3) . . ?
N20 C21 H21 124.1 . . ?
N22 C21 H21 124.1 . . ?
C6 C4 C3 121.9(3) 2_665 . ?
C5 C4 C3 119.5(3) . . ?
C5 C4 C6 118.6(3) . 2_665 ?
C13 C19 C14 118.5(3) . 2_756 ?
C13 C19 C18 122.8(3) . 2_756 ?
C18 C19 C14 118.7(3) 2_756 2_756 ?
C45 C44 N41 118.4(4) . . ?
C45 C44 C50 124.1(4) . . ?
C50 C44 N41 117.4(4) . . ?
C31 C25 N22 119.3(3) . . ?
C31 C25 C26 123.2(4) . . ?
C26 C25 N22 117.5(4) . . ?
C13 C14 C19 118.4(3) . 2_756 ?
C13 C14 C15 122.3(3) . . ?
C15 C14 C19 119.2(3) . 2_756 ?
C5 C6 C4 119.0(3) . 2_665 ?
N7 C6 C4 126.2(4) . 2_665 ?
N7 C6 C5 114.8(4) . . ?
N8 C12 H12 125.3 . . ?
C11 C12 N8 109.4(3) . . ?
C11 C12 H12 125.3 . . ?
C19 C13 N10 119.2(3) . . ?
C19 C13 C14 123.1(3) . . ?
C14 C13 N10 117.6(3) . . ?
C25 C31 C26 118.2(4) . 2_766 ?
C25 C31 C30 123.5(4) . . ?
C30 C31 C26 118.3(4) . 2_766 ?
C4 C5 C6 122.4(3) . . ?
C4 C5 H5 118.8 . . ?
C6 C5 H5 118.8 . . ?
N10 C11 H11 127.1 . . ?
C12 C11 N10 105.9(3) . . ?
C12 C11 H11 127.1 . . ?
C44 C45 C50 119.0(4) . 2_674 ?
C44 C45 C46 123.6(4) . . ?
C46 C45 C50 117.4(4) . 2_674 ?
C44 C50 C45 116.9(4) . 2_674 ?
C44 C50 C49 124.2(4) . . ?
C49 C50 C45 118.9(4) . 2_674 ?
O32 C34 O33 124.9(3) . . ?
O32 C34 C35 116.8(3) . . ?
O33 C34 C35 118.3(3) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 C14 120.1(4) . . ?
C16 C15 H15 120.0 . . ?
C19 C18 H18 120.0 2_756 . ?
C17 C18 C19 120.0(4) . 2_756 ?
C17 C18 H18 120.0 . . ?
C25 C26 C31 118.7(4) . 2_766 ?
C25 C26 C27 122.6(4) . . ?
C27 C26 C31 118.7(4) . 2_766 ?
C36 C35 C34 118.2(3) . . ?
C36 C35 C37 120.8(4) . 2_575 ?
C37 C35 C34 121.0(3) 2_575 . ?
C50 C49 H49 119.2 . . ?
C48 C49 C50 121.5(4) . . ?
C48 C49 H49 119.2 . . ?
N41 C42 H42 127.0 . . ?
N41 C42 C43 106.0(3) . . ?
C43 C42 H42 127.0 . . ?
C45 C46 H46 119.2 . . ?
C47 C46 C45 121.6(4) . . ?
C47 C46 H46 119.2 . . ?
C35 C36 H36 119.6 . . ?
C35 C36 C37 120.7(4) . . ?
C37 C36 H36 119.6 . . ?
C18 C17 H17 119.3 . . ?
C18 C17 C16 121.4(4) . . ?
C16 C17 H17 119.3 . . ?
N39 C40 N41 110.3(3) . . ?
N39 C40 H40 124.8 . . ?
N41 C40 H40 124.8 . . ?
N20 C24 H24 125.4 . . ?
C23 C24 N20 109.3(4) . . ?
C23 C24 H24 125.4 . . ?
N39 C43 H43 125.6 . . ?
C42 C43 N39 108.9(4) . . ?
C42 C43 H43 125.6 . . ?
C26 C27 H27 119.8 . . ?
C28 C27 C26 120.4(4) . . ?
C28 C27 H27 119.8 . . ?
C15 C16 C17 120.6(4) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C46 C47 H47 119.6 . . ?
C46 C47 C48 120.8(4) . 2_674 ?
C48 C47 H47 119.6 2_674 . ?
C35 C37 C36 118.5(4) 2_575 . ?
C35 C37 N38 123.3(5) 2_575 . ?
C36 C37 N38 118.2(5) . . ?
N22 C23 H23 126.8 . . ?
C24 C23 N22 106.3(3) . . ?
C24 C23 H23 126.8 . . ?
C31 C30 H30 119.6 . . ?
C29 C30 C31 120.8(4) . . ?
C29 C30 H30 119.6 . . ?
C49 C48 C47 119.7(5) . 2_674 ?
C49 C48 H48 120.1 . . ?
C47 C48 H48 120.1 2_674 . ?
C27 C28 H28 119.6 . . ?
C27 C28 C29 120.7(4) . 2_766 ?
C29 C28 H28 119.6 2_766 . ?
C30 C29 C28 121.0(4) . 2_766 ?
C30 C29 H29 119.5 . . ?
C28 C29 H29 119.5 2_766 . ?
C6 N7 H7A 110.0 . . ?
C6 N7 H7B 109.8 . . ?
H7A N7 H7B 108.8 . . ?
C37 N38 H38A 109.2 . . ?
C37 N38 H38B 111.2 . . ?
H38A N38 H38B 108.1 . . ?
H52A O52 H52B 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O51 H51A O33 0.87 1.86 2.641(4) 148.7 .
O51 H51B O2 0.87 1.95 2.785(3) 158.7 .
N7 H7A O1 0.89 1.92 2.645(7) 137.7 2_665
N7 H7B O33 0.89 2.32 2.898(7) 122.6 .
N38 H38A O33 0.89 1.93 2.636(9) 134.7 2_575
N38 H38A N7 0.89 1.83 2.429(11) 122.5 2_575

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O1 C3 O2 23.2(6) . . . . ?
Ni1 O1 C3 C4 -157.7(3) . . . . ?
Ni1 N8 C9 N10 162.3(2) . . . . ?
Ni1 N8 C12 C11 -162.9(3) . . . . ?
Ni1 N20 C21 N22 -168.1(2) . . . . ?
Ni1 N20 C24 C23 166.2(3) . . . . ?
Ni2 O32 C34 O33 -4.4(6) . . . . ?
Ni2 O32 C34 C35 176.3(2) . . . . ?
Ni2 N39 C40 N41 -175.5(3) . . . . ?
Ni2 N39 C43 C42 175.7(3) . . . . ?
O1 C3 C4 C6 -7.3(5) . . . 2_665 ?
O1 C3 C4 C5 173.2(3) . . . . ?
O32 C34 C35 C36 -17.2(5) . . . . ?
O32 C34 C35 C37 162.9(4) . . . 2_575 ?
O2 C3 C4 C6 171.8(3) . . . 2_665 ?
O2 C3 C4 C5 -7.7(5) . . . . ?
N8 C12 C11 N10 -0.4(4) . . . . ?
O33 C34 C35 C36 163.5(4) . . . . ?
O33 C34 C35 C37 -16.4(6) . . . 2_575 ?
N20 C24 C23 N22 0.5(5) . . . . ?
N22 C25 C31 C26 -179.9(3) . . . 2_766 ?
N22 C25 C31 C30 1.9(6) . . . . ?
N22 C25 C26 C31 180.0(3) . . . 2_766 ?
N22 C25 C26 C27 1.7(6) . . . . ?
N41 C44 C45 C50 178.5(3) . . . 2_674 ?
N41 C44 C45 C46 -1.7(5) . . . . ?
N41 C44 C50 C45 -178.6(3) . . . 2_674 ?
N41 C44 C50 C49 2.6(5) . . . . ?
N41 C42 C43 N39 -0.2(5) . . . . ?
C3 C4 C5 C6 -179.7(3) . . . . ?
C9 N8 C12 C11 0.5(4) . . . . ?
C9 N10 C13 C19 80.0(4) . . . . ?
C9 N10 C13 C14 -102.4(4) . . . . ?
C9 N10 C11 C12 0.1(4) . . . . ?
C21 N20 C24 C23 -0.3(4) . . . . ?
C21 N22 C25 C31 76.2(5) . . . . ?
C21 N22 C25 C26 -103.2(4) . . . . ?
C21 N22 C23 C24 -0.4(5) . . . . ?
C4 C6 C5 C4 -0.9(6) 2_665 . . . ?
C19 C14 C13 N10 -176.9(3) 2_756 . . . ?
C19 C14 C13 C19 0.6(5) 2_756 . . . ?
C19 C14 C15 C16 1.1(5) 2_756 . . . ?
C19 C18 C17 C16 1.6(6) 2_756 . . . ?
C44 N41 C42 C43 178.6(4) . . . . ?
C44 N41 C40 N39 -179.0(4) . . . . ?
C44 C45 C46 C47 177.8(4) . . . . ?
C44 C50 C49 C48 179.7(4) . . . . ?
C25 N22 C21 N20 173.1(3) . . . . ?
C25 N22 C23 C24 -173.1(4) . . . . ?
C25 C31 C30 C29 178.9(4) . . . . ?
C25 C26 C27 C28 178.3(4) . . . . ?
C14 C19 C13 N10 176.8(3) 2_756 . . . ?
C14 C19 C13 C14 -0.6(5) 2_756 . . . ?
C14 C15 C16 C17 -0.1(6) . . . . ?
C6 C4 C5 C6 0.9(6) 2_665 . . . ?
C12 N8 C9 N10 -0.4(4) . . . . ?
C13 N10 C9 N8 179.8(3) . . . . ?
C13 N10 C11 C12 -179.5(3) . . . . ?
C13 C14 C15 C16 -178.9(4) . . . . ?
C31 C25 C26 C31 0.5(6) . . . 2_766 ?
C31 C25 C26 C27 -177.7(4) . . . . ?
C31 C26 C27 C28 0.1(6) 2_766 . . . ?
C31 C30 C29 C28 -2.3(8) . . . 2_766 ?
C11 N10 C9 N8 0.2(4) . . . . ?
C11 N10 C13 C19 -100.5(4) . . . . ?
C11 N10 C13 C14 77.1(4) . . . . ?
C45 C44 C50 C45 1.3(6) . . . 2_674 ?
C45 C44 C50 C49 -177.5(4) . . . . ?
C45 C50 C49 C48 0.9(6) 2_674 . . . ?
C45 C46 C47 C48 0.6(6) . . . 2_674 ?
C50 C44 C45 C50 -1.4(6) . . . 2_674 ?
C50 C44 C45 C46 178.4(3) . . . . ?
C50 C45 C46 C47 -2.4(6) 2_674 . . . ?
C50 C49 C48 C47 1.0(7) . . . 2_674 ?
C34 C35 C36 C37 -180.0(4) . . . . ?
C15 C14 C13 N10 3.1(5) . . . . ?
C15 C14 C13 C19 -179.4(3) . . . . ?
C18 C19 C13 N10 -3.3(5) 2_756 . . . ?
C18 C19 C13 C14 179.3(3) 2_756 . . . ?
C18 C17 C16 C15 -1.3(6) . . . . ?
C26 C25 C31 C26 -0.5(6) . . . 2_766 ?
C26 C25 C31 C30 -178.7(4) . . . . ?
C26 C31 C30 C29 0.7(7) 2_766 . . . ?
C26 C27 C28 C29 1.5(8) . . . 2_766 ?
C35 C36 C37 C35 0.1(7) . . . 2_575 ?
C35 C36 C37 N38 176.3(5) . . . . ?
C42 N41 C44 C45 -88.1(5) . . . . ?
C42 N41 C44 C50 91.8(5) . . . . ?
C42 N41 C40 N39 -1.0(5) . . . . ?
C40 N39 C43 C42 -0.4(5) . . . . ?
C40 N41 C44 C45 89.6(5) . . . . ?
C40 N41 C44 C50 -90.5(5) . . . . ?
C40 N41 C42 C43 0.7(5) . . . . ?
C24 N20 C21 N22 0.1(4) . . . . ?
C43 N39 C40 N41 0.8(5) . . . . ?
C37 C35 C36 C37 -0.1(7) 2_575 . . . ?
C23 N22 C21 N20 0.2(4) . . . . ?
C23 N22 C25 C31 -112.3(5) . . . . ?
C23 N22 C25 C26 68.2(5) . . . . ?
N7 C6 C5 C4 179.2(5) . . . . ?

_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 1.540
_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_ebj-148l-h2o_r_abs_2
_database_code_depnum_ccdc_archive 'CCDC 2309439'
loop_
_audit_author_name
_audit_author_address
'Antti Marttinen'
;University of Jyvaskyla
Finland
;
_audit_update_record             
;
2023-11-21 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_audit_creation_date             2023-11-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C72 H44 Cu8 N8 O32 S4'
_chemical_formula_sum            'C72 H44 Cu8 N8 O32 S4'
_chemical_formula_weight         2169.71
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20 H14 N6 Cu1 O4 S1'
_chemical_oxdiff_usercomment     'Green small block'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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                   10.1534(2)
_cell_length_b                   10.8388(2)
_cell_length_c                   17.2424(2)
_cell_angle_alpha                88.5480(10)
_cell_angle_beta                 89.922(2)
_cell_angle_gamma                84.669(2)
_cell_volume                     1888.72(6)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    16747
_cell_measurement_temperature    120.15
_cell_measurement_theta_max      77.2570
_cell_measurement_theta_min      4.7650
_shelx_estimated_absorpt_T_max   0.923
_shelx_estimated_absorpt_T_min   0.837
_exptl_absorpt_coefficient_mu    4.302
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.974
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1084
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -1 11 0.0163
6 3 0 0.0195
4 -4 -4 0.0135
-4 4 4 0.0059
-4 -4 7 0.0189
-2 0 -10 0.0115
-6 -4 -1 0.0164
0 -2 11 0.0144
0 2 -11 0.0066

_exptl_crystal_size_max          0.043
_exptl_crystal_size_mid          0.024
_exptl_crystal_size_min          0.019
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.1102 -0.6793 10.9272 0.1852 -0.4384 -0.8795
6.1632 3.0931 0.0611 -0.3130 0.7580 -0.5722
4.0825 -4.4162 -4.4118 -0.9996 0.0251 -0.0093
-4.0825 4.4162 4.4118 0.9996 -0.0251 0.0093
-3.5171 -4.1379 7.1127 0.1812 -0.9687 -0.1699
-2.4017 0.4438 -10.3402 -0.0585 0.2971 0.9531
-5.6870 -4.0952 -0.5641 0.1483 -0.8053 0.5740
0.1628 -2.1489 10.5501 0.1221 -0.6414 -0.7575
-0.2059 2.1196 -10.5620 -0.1210 0.6357 0.7624

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34793
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.527
_diffrn_reflns_theta_min         2.563
_diffrn_ambient_temperature      120.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -16.00  24.00   0.50    2.00    --  -51.89  48.00  23.00   80
  2  ω   -127.00 -46.00   0.50    2.00    --  -51.89 -48.00-124.00  162
  3  ω     58.00  83.00   0.50    2.00    --   51.89  48.00  23.00   50
  4  ω    -23.00  40.00   0.50    2.00    --   51.89 -48.00-124.00  126
  5  ω   -159.00-133.00   0.50    7.00    --  -87.58 -48.00-124.00   52
  6  ω    -40.00 -13.00   0.50    7.00    --  -87.58  48.00  23.00   54
  7  ω     31.00  63.00   0.50    7.00    --  102.12 -48.00-124.00   64
  8  ω     88.00 176.00   0.50    7.00    --  102.12  48.00  23.00  176
  9  ω    -45.00 -13.00   0.50    2.00    --    6.00 125.00 -18.47   64
 10  ω    -28.00  -3.00   0.50    2.00    --   14.00 109.00-128.89   50
 11  ω     -4.00  25.00   0.50    2.00    --  -51.89  19.00-180.00   58
 12  ω    -52.00 -14.00   0.50    7.00    --  -87.58  57.00-180.00   76
 13  ω   -116.00 -89.00   0.50    7.00    --  -87.58 -48.00-124.00   54
 14  ω    -54.00 -15.00   0.50    7.00    --  -87.58  57.00 120.00   78
 15  ω    -51.00 -13.00   0.50    7.00    --  -87.58  57.00 -30.00   76
 16  ω     59.00 109.00   0.50    7.00    --  102.12-125.00-150.00  100
 17  ω     61.00 105.00   0.50    7.00    --  102.12 -99.00 -60.00   88
 18  ω     89.00 170.00   0.50    7.00    --  102.12  38.00 -30.00  162
 19  ω     25.00  50.00   0.50    7.00    --  102.12 -38.00 -30.00   50
 20  ω     84.00 111.00   0.50    7.00    --  102.12-125.00 -60.00   54
 21  ω    129.00 157.00   0.50    7.00    --  102.12 125.00 150.00   56
 22  ω     25.00  52.00   0.50    7.00    --  102.12 -38.00  30.00   54
 23  ω     26.00  52.00   0.50    7.00    --  102.12 -38.00 -60.00   52
 24  ω     25.00  51.00   0.50    7.00    --  102.12 -38.00  90.00   52
 25  ω     79.00 111.00   0.50    7.00    --  102.12-125.00 -30.00   64
 26  ω     78.00 106.00   0.50    7.00    --  102.12 -99.00 150.00   56
 27  ω     26.00  51.00   0.50    7.00    --  102.12 -38.00  60.00   50
 28  ω     75.00 111.00   0.50    7.00    --  102.12-125.00  90.00   72
 29  ω     80.00 106.00   0.50    7.00    --  102.12 -99.00-120.00   52
 30  ω     68.00 106.00   0.50    7.00    --  102.12 -99.00  90.00   76
 31  ω     28.00  56.00   0.50    7.00    --  102.12 -57.00-150.00   56
 32  ω    132.00 176.00   0.50    7.00    --  102.12  38.00  60.00   88
 33  ω     30.00  55.00   0.50    7.00    --  102.12 -57.00-180.00   50
 34  ω     80.00 106.00   0.50    7.00    --  102.12 -99.00  60.00   52
 35  ω     70.00 106.00   0.50    7.00    --  102.12 -99.00   0.00   72
 36  ω     79.00 105.00   0.50    7.00    --  102.12 -99.00-180.00   52
 37  ω    103.00 129.00   0.50    7.00    --  102.12  38.00  60.00   52
 38  ω    122.00 148.00   0.50    7.00    --  107.25 123.00  12.76   52
 39  ω    120.00 160.00   0.50    7.00    --  107.25   2.00-130.87   80
 40  ω    115.00 155.00   0.50    7.00    --  107.25 141.00  96.45   80
 41  ω     69.00 123.00   0.50    7.00    --  107.25 -85.00 179.59  108
 42  ω     69.00  95.00   0.50    7.00    --  107.25 141.00  96.45   52
 43  ω     41.00  89.00   0.50    7.00    --  107.25 -70.00-124.67   96
 44  ω     38.00 102.00   0.50    7.00    --  107.25-122.00 178.47  128
 45  ω     42.00  89.00   0.50    7.00    --  107.25 -81.00  -5.66   94
 46  ω     30.00  55.00   0.50    7.00    --  107.25 -41.00  13.18   50
 47  ω     41.00 111.00   0.50    7.00    --  107.25 -83.00  75.05  140
 48  ω    119.00 176.00   0.50    7.00    --  107.25  23.00 161.46  114
 49  ω     85.00 110.00   0.50    7.00    --  107.25  23.00 161.46   50
 50  ω     49.00  74.00   0.50    7.00    --  107.25 -73.00  41.21   50
 51  ω     87.00 115.00   0.50    7.00    --  107.25 -85.00-138.74   56
 52  ω     55.00  82.00   0.50    7.00    --  107.25 -85.00-138.74   54
 53  ω     83.00 109.00   0.50    7.00    --  107.25 -87.00 115.66   52
 54  ω     44.00  90.00   0.50    7.00    --  107.25 -69.00 114.35   92
 55  ω    134.00 174.00   0.50    7.00    --  107.25  17.00-106.43   80
 56  ω     70.00 102.00   0.50    7.00    --  107.25  17.00-106.43   64
 57  ω     33.00  71.00   0.50    7.00    --  107.25 -54.00 148.35   76
 58  ω     94.00 137.00   0.50    7.00    --  107.25 -88.00 -64.06   86
 59  ω     41.00  91.00   0.50    7.00    --  107.25 -88.00 -64.06  100
 60  ω    109.00 135.00   0.50    7.00    --  107.25  59.00 -55.11   52
 61  ω     43.00  71.00   0.50    7.00    --  107.25 -86.00-145.34   56
 62  ω     71.00 143.00   0.50    7.00    --  107.25  16.00 -26.51  144
 63  ω     65.00 106.00   0.50    7.00    --  107.25  18.00 154.65   82
 64  ω     39.00  78.00   0.50    7.00    --  107.25 -71.00  92.29   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1010778000
_diffrn_orient_matrix_UB_12      0.0995468000
_diffrn_orient_matrix_UB_13      0.0334056000
_diffrn_orient_matrix_UB_21      0.0721633000
_diffrn_orient_matrix_UB_22      0.1020952000
_diffrn_orient_matrix_UB_23      -0.0411091000
_diffrn_orient_matrix_UB_31      -0.0883046000
_diffrn_orient_matrix_UB_32      -0.0076181000
_diffrn_orient_matrix_UB_33      -0.0719872000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6949
_reflns_number_total             8038
_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         1.042
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         8038
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0438
_refine_ls_restrained_S_all      1.034
_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)+(0.0551P)²+5.5688P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1118
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 S52-O53A \\sim S52-O54B
 with sigma of 0.02
 S52-O55A \\sim S52-O53B
 with sigma of 0.02
 S52-O54A \\sim S52-O55B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O54B) \\sim Ueq, Uanis(O53B) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C11)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O54B) = Uanis(O54A) = Uanis(O53B) = Uanis(O55A) = Uanis(O53A) =
Uanis(O55B)
4. Others
 Fixed Sof: O53A(0.9) O55A(0.9) O54A(0.9) O54B(0.1) O55B(0.1) O53B(0.1)
5.a Ternary CH refined with riding coordinates:
 O13(H13), O42(H42)
5.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C47(H47), C51(H51), C49(H49), C20(H20), C22(H22), C34(H34), C5(H5),
 C2(H2), C32(H32), C37(H37), C40(H40), C31(H31), C3(H3), C39(H39), C38(H38),
 C8(H8), C11(H11), C9(H9), C10(H10)
;
_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
Cu4 Cu 0.49848(5) 1.36123(4) 0.99721(3) 0.01306(11) Uani 1 1 d . . . . .
Cu3 Cu 0.68271(5) 0.49576(4) 0.86427(3) 0.01305(11) Uani 1 1 d . . . . .
Cu1 Cu 0.18350(5) -0.02480(4) 0.63556(3) 0.01395(11) Uani 1 1 d . . . . .
Cu2 Cu -0.01873(5) 0.13866(4) 0.51194(3) 0.01463(12) Uani 1 1 d . . . . .
S52 S 0.85744(8) 0.98517(7) 0.65544(4) 0.01567(16) Uani 1 1 d D . . . .
S23 S 0.35700(8) 0.48331(7) 0.84356(4) 0.01640(16) Uani 1 1 d . . . . .
O13 O 0.1190(2) -0.0046(2) 0.52911(12) 0.0117(4) Uani 1 1 d . . . . .
H13 H 0.1956 0.0068 0.4940 0.018 Uiso 1 1 calc R U . . .
O42 O 0.6198(2) 0.4922(2) 0.97223(12) 0.0122(4) Uani 1 1 d . . . . .
H42 H 0.6977 0.4816 1.0080 0.018 Uiso 1 1 calc R U . . .
O45 O 0.5928(2) 0.7673(2) 0.95191(13) 0.0175(5) Uani 1 1 d . . . . .
O58 O 0.6209(2) 1.2257(2) 0.96256(12) 0.0153(5) Uani 1 1 d . . . . .
O29 O 0.1268(2) 0.7191(2) 0.53152(13) 0.0169(5) Uani 1 1 d . . . . .
O15 O 0.0874(2) 0.2619(2) 0.55293(13) 0.0179(5) Uani 1 1 d . . . . .
O28 O 0.2524(3) 0.8016(2) 0.62088(14) 0.0194(5) Uani 1 1 d . . . . .
O14 O 0.1988(3) 0.1516(2) 0.64842(14) 0.0228(5) Uani 1 1 d . . . . .
O43 O 0.7307(3) 0.6637(2) 0.86809(14) 0.0202(5) Uani 1 1 d . . . . .
O26 O 0.4654(2) 0.5623(2) 0.83915(13) 0.0193(5) Uani 1 1 d . . . . .
O24 O 0.3978(3) 0.3588(2) 0.87199(13) 0.0209(5) Uani 1 1 d . . . . .
O57 O 0.7149(3) 1.3176(2) 0.86058(15) 0.0257(6) Uani 1 1 d . . . . .
O25 O 0.2470(3) 0.5420(3) 0.88755(15) 0.0261(6) Uani 1 1 d . . . . .
O53A O 0.9789(3) 0.9012(3) 0.65847(15) 0.0206(3) Uani 0.9 1 d D . P A 1
O55A O 0.7570(3) 0.9386(3) 0.60770(15) 0.0206(3) Uani 0.9 1 d D . P A 1
O54A O 0.8835(3) 1.1116(3) 0.63371(15) 0.0206(3) Uani 0.9 1 d D . P A 1
N30 N 0.7248(3) 0.4981(3) 0.75075(16) 0.0199(6) Uani 1 1 d . . . . .
N1 N 0.2226(3) -0.0441(3) 0.74818(16) 0.0200(6) Uani 1 1 d . . . . .
N33 N 0.6766(3) 0.5003(3) 0.62688(16) 0.0208(6) Uani 1 1 d . . . . .
N4 N 0.1724(3) -0.0384(3) 0.87167(16) 0.0208(6) Uani 1 1 d . . . . .
C27 C 0.2003(3) 0.7146(3) 0.59175(16) 0.0106(6) Uani 1 1 d . . . . .
C56 C 0.6805(3) 1.2257(3) 0.89842(18) 0.0157(6) Uani 1 1 d . . . . .
C16 C 0.1603(3) 0.2507(3) 0.61207(19) 0.0164(6) Uani 1 1 d . . . . .
C50 C 0.7935(3) 0.9890(3) 0.75081(18) 0.0144(6) Uani 1 1 d . . . . .
C44 C 0.6765(3) 0.7600(3) 0.89748(18) 0.0141(6) Uani 1 1 d . . . . .
C18 C 0.2633(3) 0.3648(3) 0.71733(18) 0.0161(6) Uani 1 1 d . . . . .
H18 H 0.2793 0.2886 0.7457 0.019 Uiso 1 1 calc R U . . .
C47 C 0.6817(3) 0.9927(3) 0.89800(18) 0.0146(6) Uani 1 1 d . . . . .
H47 H 0.6405 0.9941 0.9475 0.017 Uiso 1 1 calc R U . . .
C48 C 0.7127(3) 1.1026(3) 0.86178(18) 0.0150(6) Uani 1 1 d . . . . .
C51 C 0.7677(3) 0.8778(3) 0.78760(19) 0.0163(6) Uani 1 1 d . . . . .
H51 H 0.7883 0.8013 0.7627 0.020 Uiso 1 1 calc R U . . .
C17 C 0.2049(3) 0.3683(3) 0.64367(19) 0.0163(6) Uani 1 1 d . . . . .
C19 C 0.2973(3) 0.4746(3) 0.74800(18) 0.0145(6) Uani 1 1 d . . . . .
C49 C 0.7681(3) 1.1010(3) 0.78712(18) 0.0155(6) Uani 1 1 d . . . . .
H49 H 0.7879 1.1760 0.7619 0.019 Uiso 1 1 calc R U . . .
C20 C 0.2783(3) 0.5862(3) 0.70618(18) 0.0160(6) Uani 1 1 d . . . . .
H20 H 0.3032 0.6602 0.7280 0.019 Uiso 1 1 calc R U . . .
C21 C 0.2229(3) 0.5894(3) 0.63235(18) 0.0158(6) Uani 1 1 d . . . . .
C22 C 0.1834(3) 0.4802(3) 0.60181(18) 0.0152(6) Uani 1 1 d . . . . .
H22 H 0.1419 0.4823 0.5524 0.018 Uiso 1 1 calc R U . . .
C46 C 0.7115(3) 0.8801(3) 0.86103(18) 0.0148(6) Uani 1 1 d . . . . .
C6 C 0.0876(4) -0.0188(4) 0.93894(19) 0.0199(7) Uani 1 1 d . . . . .
C34 C 0.6326(4) 0.5269(3) 0.69865(19) 0.0201(7) Uani 1 1 d . . . . .
H34 H 0.5458 0.5622 0.7101 0.024 Uiso 1 1 calc R U . . .
C35 C 0.5895(4) 0.5007(4) 0.56050(19) 0.0209(7) Uani 1 1 d . . . . .
C7 C 0.0330(4) -0.1206(4) 0.9721(2) 0.0249(8) Uani 1 1 d . . . . .
C5 C 0.1303(4) -0.0115(4) 0.7989(2) 0.0251(8) Uani 1 1 d . . . . .
H5 H 0.0447 0.0263 0.7858 0.030 Uiso 1 1 calc R U . . .
C12 C 0.0586(4) 0.1010(4) 0.9640(2) 0.0247(8) Uani 1 1 d . . . . .
C2 C 0.3304(4) -0.0941(4) 0.7906(2) 0.0240(7) Uani 1 1 d . . . . .
H2 H 0.4127 -0.1258 0.7693 0.029 Uiso 1 1 calc R U . . .
C36 C 0.5536(4) 0.6120(4) 0.5197(2) 0.0220(7) Uani 1 1 d . . . . .
C41 C 0.5392(4) 0.3887(4) 0.5436(2) 0.0235(7) Uani 1 1 d . . . . .
C32 C 0.8049(4) 0.4454(4) 0.6343(2) 0.0287(8) Uani 1 1 d . . . . .
H32 H 0.8614 0.4142 0.5939 0.034 Uiso 1 1 calc R U . . .
C37 C 0.6050(4) 0.7263(4) 0.5372(2) 0.0274(8) Uani 1 1 d . . . . .
H37 H 0.6658 0.7291 0.5788 0.033 Uiso 1 1 calc R U . . .
C40 C 0.4265(4) 0.7234(4) 0.4130(2) 0.0297(8) Uani 1 1 d . . . . .
H40 H 0.3670 0.7237 0.3705 0.036 Uiso 1 1 calc R U . . .
C31 C 0.8333(4) 0.4452(4) 0.7113(2) 0.0277(8) Uani 1 1 d . . . . .
H31 H 0.9149 0.4137 0.7344 0.033 Uiso 1 1 calc R U . . .
C3 C 0.3009(4) -0.0908(4) 0.8677(2) 0.0260(8) Uani 1 1 d . . . . .
H3 H 0.3572 -0.1188 0.9097 0.031 Uiso 1 1 calc R U . . .
C39 C 0.4784(5) 0.8300(4) 0.4320(3) 0.0372(10) Uani 1 1 d . . . . .
H39 H 0.4544 0.9042 0.4028 0.045 Uiso 1 1 calc R U . . .
C38 C 0.5674(4) 0.8315(4) 0.4946(3) 0.0333(9) Uani 1 1 d . . . . .
H38 H 0.6019 0.9069 0.5074 0.040 Uiso 1 1 calc R U . . .
C8 C 0.0605(5) -0.2424(4) 0.9441(3) 0.0424(12) Uani 1 1 d . U . . .
H8 H 0.1209 -0.2565 0.9024 0.051 Uiso 1 1 calc R U . . .
C11 C 0.1180(5) 0.2048(4) 0.9319(3) 0.0394(11) Uani 1 1 d . U . . .
H11 H 0.1783 0.1942 0.8899 0.047 Uiso 1 1 calc R U . . .
C9 C 0.0020(6) -0.3381(5) 0.9758(4) 0.0614(17) Uani 1 1 d . U . . .
H9 H 0.0212 -0.4188 0.9561 0.074 Uiso 1 1 calc R U . . .
C10 C 0.0883(6) 0.3194(5) 0.9616(4) 0.0591(16) Uani 1 1 d . U . . .
H10 H 0.1286 0.3881 0.9400 0.071 Uiso 1 1 calc R U . . .
O54B O 0.952(2) 1.076(2) 0.6520(14) 0.0206(3) Uani 0.1 1 d D U P A 2
O55B O 0.746(2) 1.035(2) 0.6056(12) 0.0206(3) Uani 0.1 1 d D . P A 2
O53B O 0.886(2) 0.8619(16) 0.6274(13) 0.0206(3) Uani 0.1 1 d D U P A 2


_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 Cu4 3.0151(9) 2_687 ?
Cu4 O42 1.983(2) 2_677 ?
Cu4 O42 2.003(2) 1_565 ?
Cu4 O45 1.935(2) 2_677 ?
Cu4 O58 1.940(2) . ?
Cu4 O24 2.392(2) 1_565 ?
Cu3 O42 1.968(2) . ?
Cu3 O43 1.931(2) . ?
Cu3 O26 2.295(3) . ?
Cu3 O57 1.931(2) 1_545 ?
Cu3 N30 2.003(3) . ?
Cu1 O13 1.950(2) . ?
Cu1 O28 1.967(2) 1_545 ?
Cu1 O14 1.951(2) . ?
Cu1 O53A 2.325(3) 1_445 ?
Cu1 N1 1.985(3) . ?
Cu2 Cu2 3.0329(9) 2_556 ?
Cu2 O13 2.007(2) . ?
Cu2 O13 1.994(2) 2_556 ?
Cu2 O29 1.942(2) 2_566 ?
Cu2 O15 1.940(2) . ?
Cu2 O54A 2.345(3) 1_445 ?
S52 O53A 1.464(3) . ?
S52 O55A 1.446(3) . ?
S52 O54A 1.459(3) . ?
S52 C50 1.767(3) . ?
S52 O54B 1.441(16) . ?
S52 O55B 1.473(16) . ?
S52 O53B 1.436(16) . ?
S23 O26 1.456(3) . ?
S23 O24 1.448(2) . ?
S23 O25 1.455(3) . ?
S23 C19 1.764(3) . ?
O13 Cu2 1.994(2) 2_556 ?
O13 H13 1.0000 . ?
O42 Cu4 2.003(2) 1_545 ?
O42 Cu4 1.983(2) 2_677 ?
O42 H42 1.0000 . ?
O45 Cu4 1.935(2) 2_677 ?
O45 C44 1.264(4) . ?
O58 C56 1.260(4) . ?
O29 Cu2 1.942(2) 2_566 ?
O29 C27 1.277(4) . ?
O15 C16 1.257(4) . ?
O28 Cu1 1.967(2) 1_565 ?
O28 C27 1.240(4) . ?
O14 C16 1.260(4) . ?
O43 C44 1.252(4) . ?
O24 Cu4 2.392(2) 1_545 ?
O57 Cu3 1.931(2) 1_565 ?
O57 C56 1.254(4) . ?
O53A Cu1 2.325(3) 1_665 ?
O54A Cu2 2.345(3) 1_665 ?
N30 C34 1.309(5) . ?
N30 C31 1.380(5) . ?
N1 C5 1.312(5) . ?
N1 C2 1.377(5) . ?
N33 C34 1.344(4) . ?
N33 C35 1.447(4) . ?
N33 C32 1.385(5) . ?
N4 C6 1.452(4) . ?
N4 C5 1.343(4) . ?
N4 C3 1.376(5) . ?
C27 C21 1.510(4) . ?
C56 C48 1.499(4) . ?
C16 C17 1.507(4) . ?
C50 C51 1.394(4) . ?
C50 C49 1.383(5) . ?
C44 C46 1.504(4) . ?
C18 H18 0.9500 . ?
C18 C17 1.401(4) . ?
C18 C19 1.387(5) . ?
C47 H47 0.9500 . ?
C47 C48 1.393(4) . ?
C47 C46 1.399(4) . ?
C48 C49 1.404(4) . ?
C51 H51 0.9500 . ?
C51 C46 1.388(4) . ?
C17 C22 1.395(4) . ?
C19 C20 1.390(4) . ?
C49 H49 0.9500 . ?
C20 H20 0.9500 . ?
C20 C21 1.391(4) . ?
C21 C22 1.399(4) . ?
C22 H22 0.9500 . ?
C6 C7 1.390(5) . ?
C6 C12 1.384(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.400(5) . ?
C35 C41 1.397(5) . ?
C7 C12 1.448(5) 2_557 ?
C7 C8 1.421(6) . ?
C5 H5 0.9500 . ?
C12 C7 1.448(5) 2_557 ?
C12 C11 1.425(6) . ?
C2 H2 0.9500 . ?
C2 C3 1.362(5) . ?
C36 C41 1.443(5) 2_666 ?
C36 C37 1.427(5) . ?
C41 C36 1.443(5) 2_666 ?
C41 C40 1.427(5) 2_666 ?
C32 H32 0.9500 . ?
C32 C31 1.360(5) . ?
C37 H37 0.9500 . ?
C37 C38 1.365(6) . ?
C40 C41 1.427(5) 2_666 ?
C40 H40 0.9500 . ?
C40 C39 1.361(6) . ?
C31 H31 0.9500 . ?
C3 H3 0.9500 . ?
C39 H39 0.9500 . ?
C39 C38 1.410(6) . ?
C38 H38 0.9500 . ?
C8 H8 0.9500 . ?
C8 C9 1.346(7) . ?
C11 H11 0.9500 . ?
C11 C10 1.363(7) . ?
C9 H9 0.9500 . ?
C9 C10 1.422(7) 2_557 ?
C10 C9 1.422(7) 2_557 ?
C10 H10 0.9500 . ?

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
O42 Cu4 Cu4 40.59(6) 1_565 2_687 ?
O42 Cu4 Cu4 41.09(7) 2_677 2_687 ?
O42 Cu4 O42 81.68(10) 2_677 1_565 ?
O42 Cu4 O24 97.02(9) 1_565 1_565 ?
O42 Cu4 O24 92.24(9) 2_677 1_565 ?
O45 Cu4 Cu4 137.98(7) 2_677 2_687 ?
O45 Cu4 O42 99.07(10) 2_677 2_677 ?
O45 Cu4 O42 164.25(10) 2_677 1_565 ?
O45 Cu4 O58 85.02(10) 2_677 . ?
O45 Cu4 O24 98.66(10) 2_677 1_565 ?
O58 Cu4 Cu4 135.10(8) . 2_687 ?
O58 Cu4 O42 94.53(10) . 1_565 ?
O58 Cu4 O42 175.89(10) . 2_677 ?
O58 Cu4 O24 86.62(9) . 1_565 ?
O24 Cu4 Cu4 96.13(6) 1_565 2_687 ?
O42 Cu3 O26 82.76(9) . . ?
O42 Cu3 N30 173.32(12) . . ?
O43 Cu3 O42 94.26(10) . . ?
O43 Cu3 O26 91.96(10) . . ?
O43 Cu3 O57 155.72(12) . 1_545 ?
O43 Cu3 N30 88.42(11) . . ?
O57 Cu3 O42 93.46(10) 1_545 . ?
O57 Cu3 O26 111.85(11) 1_545 . ?
O57 Cu3 N30 86.52(11) 1_545 . ?
N30 Cu3 O26 91.04(11) . . ?
O13 Cu1 O28 92.87(9) . 1_545 ?
O13 Cu1 O14 94.40(9) . . ?
O13 Cu1 O53A 83.53(9) . 1_445 ?
O13 Cu1 N1 171.95(11) . . ?
O28 Cu1 O53A 86.81(10) 1_545 1_445 ?
O28 Cu1 N1 89.88(11) 1_545 . ?
O14 Cu1 O28 154.68(12) . 1_545 ?
O14 Cu1 O53A 118.09(11) . 1_445 ?
O14 Cu1 N1 86.26(11) . . ?
N1 Cu1 O53A 89.07(11) . 1_445 ?
O13 Cu2 Cu2 40.87(6) 2_556 2_556 ?
O13 Cu2 Cu2 40.56(6) . 2_556 ?
O13 Cu2 O13 81.43(9) 2_556 . ?
O13 Cu2 O54A 89.52(9) 2_556 1_445 ?
O13 Cu2 O54A 93.50(10) . 1_445 ?
O29 Cu2 Cu2 137.46(7) 2_566 2_556 ?
O29 Cu2 O13 164.28(10) 2_566 . ?
O29 Cu2 O13 98.73(9) 2_566 2_556 ?
O29 Cu2 O54A 102.22(11) 2_566 1_445 ?
O15 Cu2 Cu2 135.80(8) . 2_556 ?
O15 Cu2 O13 95.24(10) . . ?
O15 Cu2 O13 176.67(10) . 2_556 ?
O15 Cu2 O29 84.45(10) . 2_566 ?
O15 Cu2 O54A 90.80(10) . 1_445 ?
O54A Cu2 Cu2 92.00(7) 1_445 2_556 ?
O53A S52 C50 106.36(15) . . ?
O55A S52 O53A 112.11(16) . . ?
O55A S52 O54A 112.82(17) . . ?
O55A S52 C50 106.12(15) . . ?
O54A S52 O53A 111.88(17) . . ?
O54A S52 C50 107.02(15) . . ?
O54B S52 C50 105.9(9) . . ?
O54B S52 O55B 105.8(15) . . ?
O55B S52 C50 105.1(9) . . ?
O53B S52 C50 113.5(9) . . ?
O53B S52 O54B 122.5(14) . . ?
O53B S52 O55B 102.5(14) . . ?
O26 S23 C19 106.23(15) . . ?
O24 S23 O26 113.12(15) . . ?
O24 S23 O25 112.41(16) . . ?
O24 S23 C19 108.36(15) . . ?
O25 S23 O26 110.72(16) . . ?
O25 S23 C19 105.50(16) . . ?
Cu1 O13 Cu2 114.23(10) . . ?
Cu1 O13 Cu2 117.28(11) . 2_556 ?
Cu1 O13 H13 108.7 . . ?
Cu2 O13 Cu2 98.57(9) 2_556 . ?
Cu2 O13 H13 108.7 . . ?
Cu2 O13 H13 108.7 2_556 . ?
Cu4 O42 Cu4 98.32(10) 2_677 1_545 ?
Cu4 O42 H42 109.3 1_545 . ?
Cu4 O42 H42 109.3 2_677 . ?
Cu3 O42 Cu4 115.30(10) . 2_677 ?
Cu3 O42 Cu4 114.93(10) . 1_545 ?
Cu3 O42 H42 109.3 . . ?
C44 O45 Cu4 129.9(2) . 2_677 ?
C56 O58 Cu4 124.1(2) . . ?
C27 O29 Cu2 127.8(2) . 2_566 ?
C16 O15 Cu2 127.1(2) . . ?
C27 O28 Cu1 130.7(2) . 1_565 ?
C16 O14 Cu1 136.2(2) . . ?
C44 O43 Cu3 132.9(2) . . ?
S23 O26 Cu3 124.45(15) . . ?
S23 O24 Cu4 111.09(13) . 1_545 ?
C56 O57 Cu3 137.0(2) . 1_565 ?
S52 O53A Cu1 120.72(16) . 1_665 ?
S52 O54A Cu2 116.15(15) . 1_665 ?
C34 N30 Cu3 121.3(2) . . ?
C34 N30 C31 106.4(3) . . ?
C31 N30 Cu3 130.4(3) . . ?
C5 N1 Cu1 119.8(2) . . ?
C5 N1 C2 106.1(3) . . ?
C2 N1 Cu1 134.0(3) . . ?
C34 N33 C35 122.8(3) . . ?
C34 N33 C32 107.2(3) . . ?
C32 N33 C35 128.1(3) . . ?
C5 N4 C6 122.7(3) . . ?
C5 N4 C3 107.8(3) . . ?
C3 N4 C6 129.4(3) . . ?
O29 C27 C21 115.6(3) . . ?
O28 C27 O29 127.3(3) . . ?
O28 C27 C21 117.1(3) . . ?
O58 C56 C48 117.0(3) . . ?
O57 C56 O58 127.4(3) . . ?
O57 C56 C48 115.6(3) . . ?
O15 C16 O14 126.9(3) . . ?
O15 C16 C17 116.7(3) . . ?
O14 C16 C17 116.4(3) . . ?
C51 C50 S52 118.7(2) . . ?
C49 C50 S52 120.0(2) . . ?
C49 C50 C51 121.2(3) . . ?
O45 C44 C46 116.8(3) . . ?
O43 C44 O45 127.5(3) . . ?
O43 C44 C46 115.6(3) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
C19 C18 C17 118.7(3) . . ?
C48 C47 H47 120.2 . . ?
C48 C47 C46 119.6(3) . . ?
C46 C47 H47 120.2 . . ?
C47 C48 C56 121.6(3) . . ?
C47 C48 C49 120.1(3) . . ?
C49 C48 C56 118.1(3) . . ?
C50 C51 H51 120.4 . . ?
C46 C51 C50 119.3(3) . . ?
C46 C51 H51 120.4 . . ?
C18 C17 C16 118.9(3) . . ?
C22 C17 C16 120.7(3) . . ?
C22 C17 C18 120.3(3) . . ?
C18 C19 S23 122.5(2) . . ?
C18 C19 C20 121.3(3) . . ?
C20 C19 S23 116.0(2) . . ?
C50 C49 C48 119.2(3) . . ?
C50 C49 H49 120.4 . . ?
C48 C49 H49 120.4 . . ?
C19 C20 H20 120.0 . . ?
C19 C20 C21 119.9(3) . . ?
C21 C20 H20 120.0 . . ?
C20 C21 C27 116.9(3) . . ?
C20 C21 C22 119.4(3) . . ?
C22 C21 C27 123.5(3) . . ?
C17 C22 C21 120.2(3) . . ?
C17 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C47 C46 C44 121.1(3) . . ?
C51 C46 C44 118.4(3) . . ?
C51 C46 C47 120.5(3) . . ?
C7 C6 N4 118.2(3) . . ?
C12 C6 N4 118.6(3) . . ?
C12 C6 C7 123.2(3) . . ?
N30 C34 N33 111.3(3) . . ?
N30 C34 H34 124.4 . . ?
N33 C34 H34 124.4 . . ?
C36 C35 N33 119.6(3) . . ?
C41 C35 N33 117.0(3) . . ?
C41 C35 C36 123.3(3) . . ?
C6 C7 C12 118.7(3) . 2_557 ?
C6 C7 C8 122.4(4) . . ?
C8 C7 C12 118.9(4) . 2_557 ?
N1 C5 N4 111.2(3) . . ?
N1 C5 H5 124.4 . . ?
N4 C5 H5 124.4 . . ?
C6 C12 C7 118.2(3) . 2_557 ?
C6 C12 C11 123.2(4) . . ?
C11 C12 C7 118.6(4) . 2_557 ?
N1 C2 H2 125.2 . . ?
C3 C2 N1 109.5(3) . . ?
C3 C2 H2 125.2 . . ?
C35 C36 C41 118.5(3) . 2_666 ?
C35 C36 C37 123.2(3) . . ?
C37 C36 C41 118.3(3) . 2_666 ?
C35 C41 C36 118.1(3) . 2_666 ?
C35 C41 C40 122.9(3) . 2_666 ?
C40 C41 C36 119.0(4) 2_666 2_666 ?
N33 C32 H32 127.1 . . ?
C31 C32 N33 105.8(3) . . ?
C31 C32 H32 127.1 . . ?
C36 C37 H37 119.8 . . ?
C38 C37 C36 120.5(4) . . ?
C38 C37 H37 119.8 . . ?
C41 C40 H40 119.8 2_666 . ?
C39 C40 C41 120.5(4) . 2_666 ?
C39 C40 H40 119.8 . . ?
N30 C31 H31 125.4 . . ?
C32 C31 N30 109.2(3) . . ?
C32 C31 H31 125.4 . . ?
N4 C3 H3 127.3 . . ?
C2 C3 N4 105.4(3) . . ?
C2 C3 H3 127.3 . . ?
C40 C39 H39 119.7 . . ?
C40 C39 C38 120.7(4) . . ?
C38 C39 H39 119.7 . . ?
C37 C38 C39 121.1(4) . . ?
C37 C38 H38 119.4 . . ?
C39 C38 H38 119.4 . . ?
C7 C8 H8 119.6 . . ?
C9 C8 C7 120.8(4) . . ?
C9 C8 H8 119.6 . . ?
C12 C11 H11 120.0 . . ?
C10 C11 C12 119.9(4) . . ?
C10 C11 H11 120.0 . . ?
C8 C9 H9 119.7 . . ?
C8 C9 C10 120.6(5) . 2_557 ?
C10 C9 H9 119.7 2_557 . ?
C11 C10 C9 121.2(5) . 2_557 ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 2_557 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O13 H13 O55A 1.00 1.91 2.781(3) 143.7 2_666
O13 H13 O55B 1.00 1.87 2.71(2) 139.2 2_666
O42 H42 O25 1.00 1.89 2.772(3) 145.2 2_667
C34 H34 O26 0.95 2.37 2.969(4) 120.7 .

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 O45 C44 O43 -7.7(5) 2_677 . . . ?
Cu4 O45 C44 C46 169.5(2) 2_677 . . . ?
Cu4 O58 C56 O57 29.5(5) . . . . ?
Cu4 O58 C56 C48 -149.4(2) . . . . ?
Cu3 O43 C44 O45 22.0(5) . . . . ?
Cu3 O43 C44 C46 -155.2(2) . . . . ?
Cu3 O57 C56 O58 -10.6(6) 1_565 . . . ?
Cu3 O57 C56 C48 168.3(3) 1_565 . . . ?
Cu3 N30 C34 N33 -168.3(2) . . . . ?
Cu3 N30 C31 C32 165.4(3) . . . . ?
Cu1 O28 C27 O29 40.0(5) 1_565 . . . ?
Cu1 O28 C27 C21 -138.5(2) 1_565 . . . ?
Cu1 O14 C16 O15 4.4(6) . . . . ?
Cu1 O14 C16 C17 -176.6(3) . . . . ?
Cu1 N1 C5 N4 176.2(2) . . . . ?
Cu1 N1 C2 C3 -175.8(3) . . . . ?
Cu2 O29 C27 O28 -25.1(5) 2_566 . . . ?
Cu2 O29 C27 C21 153.5(2) 2_566 . . . ?
Cu2 O15 C16 O14 14.2(5) . . . . ?
Cu2 O15 C16 C17 -164.8(2) . . . . ?
S52 C50 C51 C46 -176.9(3) . . . . ?
S52 C50 C49 C48 177.6(3) . . . . ?
S23 C19 C20 C21 -175.5(3) . . . . ?
O45 C44 C46 C47 16.6(5) . . . . ?
O45 C44 C46 C51 -159.8(3) . . . . ?
O58 C56 C48 C47 -1.9(5) . . . . ?
O58 C56 C48 C49 174.3(3) . . . . ?
O29 C27 C21 C20 -166.9(3) . . . . ?
O29 C27 C21 C22 8.8(5) . . . . ?
O15 C16 C17 C18 167.4(3) . . . . ?
O15 C16 C17 C22 -10.0(5) . . . . ?
O28 C27 C21 C20 11.8(5) . . . . ?
O28 C27 C21 C22 -172.5(3) . . . . ?
O14 C16 C17 C18 -11.7(5) . . . . ?
O14 C16 C17 C22 170.9(3) . . . . ?
O43 C44 C46 C47 -165.9(3) . . . . ?
O43 C44 C46 C51 17.6(5) . . . . ?
O26 S23 O24 Cu4 57.42(18) . . . 1_545 ?
O26 S23 C19 C18 137.9(3) . . . . ?
O26 S23 C19 C20 -45.9(3) . . . . ?
O24 S23 O26 Cu3 4.9(2) . . . . ?
O24 S23 C19 C18 16.1(3) . . . . ?
O24 S23 C19 C20 -167.7(3) . . . . ?
O57 C56 C48 C47 179.1(3) . . . . ?
O57 C56 C48 C49 -4.8(5) . . . . ?
O25 S23 O26 Cu3 132.08(17) . . . . ?
O25 S23 O24 Cu4 -68.89(18) . . . 1_545 ?
O25 S23 C19 C18 -104.5(3) . . . . ?
O25 S23 C19 C20 71.7(3) . . . . ?
O53A S52 O54A Cu2 60.5(2) . . . 1_665 ?
O53A S52 C50 C51 -56.3(3) . . . . ?
O53A S52 C50 C49 124.6(3) . . . . ?
O55A S52 O53A Cu1 130.48(17) . . . 1_665 ?
O55A S52 O54A Cu2 -67.0(2) . . . 1_665 ?
O55A S52 C50 C51 63.2(3) . . . . ?
O55A S52 C50 C49 -115.8(3) . . . . ?
O54A S52 O53A Cu1 2.6(2) . . . 1_665 ?
O54A S52 C50 C51 -176.1(3) . . . . ?
O54A S52 C50 C49 4.9(3) . . . . ?
N1 C2 C3 N4 0.3(5) . . . . ?
N33 C35 C36 C41 -176.6(3) . . . 2_666 ?
N33 C35 C36 C37 3.9(5) . . . . ?
N33 C35 C41 C36 176.7(3) . . . 2_666 ?
N33 C35 C41 C40 -2.0(5) . . . 2_666 ?
N33 C32 C31 N30 0.4(5) . . . . ?
N4 C6 C7 C12 -176.0(3) . . . 2_557 ?
N4 C6 C7 C8 2.0(6) . . . . ?
N4 C6 C12 C7 176.0(3) . . . 2_557 ?
N4 C6 C12 C11 -6.3(6) . . . . ?
C27 C21 C22 C17 -178.4(3) . . . . ?
C56 C48 C49 C50 -177.3(3) . . . . ?
C16 C17 C22 C21 178.8(3) . . . . ?
C50 S52 O53A Cu1 -113.96(17) . . . 1_665 ?
C50 S52 O54A Cu2 176.64(15) . . . 1_665 ?
C50 C51 C46 C44 176.1(3) . . . . ?
C50 C51 C46 C47 -0.3(5) . . . . ?
C18 C17 C22 C21 1.4(5) . . . . ?
C18 C19 C20 C21 0.7(5) . . . . ?
C47 C48 C49 C50 -1.1(5) . . . . ?
C48 C47 C46 C44 -178.5(3) . . . . ?
C48 C47 C46 C51 -2.2(5) . . . . ?
C51 C50 C49 C48 -1.4(5) . . . . ?
C17 C18 C19 S23 173.9(3) . . . . ?
C17 C18 C19 C20 -2.0(5) . . . . ?
C19 S23 O26 Cu3 -113.87(17) . . . . ?
C19 S23 O24 Cu4 174.92(14) . . . 1_545 ?
C19 C18 C17 C16 -176.4(3) . . . . ?
C19 C18 C17 C22 0.9(5) . . . . ?
C19 C20 C21 C27 177.6(3) . . . . ?
C19 C20 C21 C22 1.7(5) . . . . ?
C49 C50 C51 C46 2.1(5) . . . . ?
C20 C21 C22 C17 -2.8(5) . . . . ?
C46 C47 C48 C56 178.9(3) . . . . ?
C46 C47 C48 C49 2.9(5) . . . . ?
C6 N4 C5 N1 -176.3(3) . . . . ?
C6 N4 C3 C2 176.1(4) . . . . ?
C6 C7 C8 C9 -177.5(5) . . . . ?
C6 C12 C11 C10 -177.5(5) . . . . ?
C34 N30 C31 C32 1.2(5) . . . . ?
C34 N33 C35 C36 85.2(5) . . . . ?
C34 N33 C35 C41 -91.1(4) . . . . ?
C34 N33 C32 C31 -1.8(5) . . . . ?
C35 N33 C34 N30 168.0(3) . . . . ?
C35 N33 C32 C31 -166.1(4) . . . . ?
C35 C36 C37 C38 179.2(4) . . . . ?
C7 C6 C12 C7 0.0(6) . . . 2_557 ?
C7 C6 C12 C11 177.7(4) . . . . ?
C7 C12 C11 C10 0.2(8) 2_557 . . . ?
C7 C8 C9 C10 -0.3(11) . . . 2_557 ?
C5 N1 C2 C3 0.1(5) . . . . ?
C5 N4 C6 C7 100.7(4) . . . . ?
C5 N4 C6 C12 -75.5(5) . . . . ?
C5 N4 C3 C2 -0.5(4) . . . . ?
C12 C6 C7 C12 0.0(6) . . . 2_557 ?
C12 C6 C7 C8 177.9(4) . . . . ?
C12 C7 C8 C9 0.5(8) 2_557 . . . ?
C12 C11 C10 C9 -0.3(10) . . . 2_557 ?
C2 N1 C5 N4 -0.4(4) . . . . ?
C36 C35 C41 C36 0.5(6) . . . 2_666 ?
C36 C35 C41 C40 -178.1(4) . . . 2_666 ?
C36 C37 C38 C39 -0.6(7) . . . . ?
C41 C35 C36 C41 -0.5(6) . . . 2_666 ?
C41 C35 C36 C37 179.9(4) . . . . ?
C41 C36 C37 C38 -0.4(6) 2_666 . . . ?
C41 C40 C39 C38 0.3(7) 2_666 . . . ?
C32 N33 C34 N30 2.7(4) . . . . ?
C32 N33 C35 C36 -112.7(4) . . . . ?
C32 N33 C35 C41 71.0(5) . . . . ?
C40 C39 C38 C37 0.7(7) . . . . ?
C31 N30 C34 N33 -2.4(4) . . . . ?
C3 N4 C6 C7 -75.5(5) . . . . ?
C3 N4 C6 C12 108.4(5) . . . . ?
C3 N4 C5 N1 0.6(5) . . . . ?
O54B S52 O53A Cu1 -9.9(10) . . . 1_665 ?
O54B S52 O54A Cu2 83.5(17) . . . 1_665 ?
O54B S52 C50 C51 -141.6(12) . . . . ?
O54B S52 C50 C49 39.4(12) . . . . ?
O55B S52 O53A Cu1 95.0(17) . . . 1_665 ?
O55B S52 O54A Cu2 -82.2(10) . . . 1_665 ?
O55B S52 C50 C51 106.7(11) . . . . ?
O55B S52 C50 C49 -72.3(11) . . . . ?
O53B S52 O53A Cu1 138.9(13) . . . 1_665 ?
O53B S52 O54A Cu2 8.3(16) . . . 1_665 ?
O53B S52 C50 C51 -4.4(12) . . . . ?
O53B S52 C50 C49 176.6(11) . . . . ?

_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 1.262
_oxdiff_exptl_absorpt_empirical_full_min 0.732
####################################################################### 
# 
# 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_ebj-185n-dry-273k_r_abs
_database_code_depnum_ccdc_archive 'CCDC 2309442'
loop_
_audit_author_name
_audit_author_address
'Antti Marttinen'
;University of Jyvaskyla
Finland
;
_audit_update_record             
;
2023-11-21 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_audit_creation_date             2023-11-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C116 H80 N20 Ni3 O16 S2, 12[H2O], 4[C3H7NO]'
_chemical_formula_sum            'C128 H132 N24 Ni3 O32 S2'
_chemical_formula_weight         2758.82
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20 H14 N4 O6 S1 Ni1'
_chemical_oxdiff_usercomment     'light blue/green block'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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                   13.5935(3)
_cell_length_b                   29.6842(9)
_cell_length_c                   17.6639(5)
_cell_angle_alpha                90
_cell_angle_beta                 104.823(3)
_cell_angle_gamma                90
_cell_volume                     6890.4(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    21924
_cell_measurement_temperature    273.00(10)
_cell_measurement_theta_max      77.4390
_cell_measurement_theta_min      2.9540
_shelx_estimated_absorpt_T_max   0.925
_shelx_estimated_absorpt_T_min   0.837
_exptl_absorpt_coefficient_mu    1.442
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 17 -5 0.0236
0 -17 6 0.0285
9 0 -5 0.0560
-9 1 3 0.0688
0 -10 -9 0.0220
1 10 9 0.0474
0 0 -11 0.0223
-2 -19 1 0.0326
1 -18 -5 0.0251
-2 8 10 0.0520
8 4 0 0.0568
-6 -12 -2 0.0470

_exptl_crystal_size_max          0.128
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.055
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.4705 16.5810 -5.4668 0.0034 0.2597 0.9657
0.0772 -16.5817 5.6261 -0.0023 -0.2164 -0.9763
8.7073 -0.4905 -4.6552 0.0759 -0.9611 0.2655
-8.8109 0.7470 3.3091 0.0252 0.9808 -0.1932
-0.4227 -9.7329 -9.4123 0.9996 -0.0251 0.0093
1.4193 10.1184 8.7926 -0.9958 -0.0796 0.0442
-0.2315 -0.1200 -11.0013 0.8633 0.0674 0.5001
-2.2816 -18.6172 0.5601 0.5243 0.0444 -0.8504
0.8936 -17.6780 -4.5791 0.7892 -0.2802 -0.5465
-2.4816 8.2725 10.3385 -0.9337 0.3299 -0.1392
8.2584 4.3322 0.2531 -0.4159 -0.8760 0.2442
-6.2083 -12.0525 -1.6716 0.6588 0.5658 -0.4959

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            74695
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.445
_diffrn_reflns_theta_min         2.977
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      273.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -83.00 -46.00   1.00    1.50    --  -51.89 -43.00 -99.00   37
  2  ω    -30.00  24.00   1.00    1.50    --  -51.89  43.00  51.00   54
  3  ω    -19.00   7.00   1.00    1.50    --   51.89 -43.00 -99.00   26
  4  ω     44.00 112.00   1.00    1.50    --   51.89  43.00  51.00   68
  5  ω   -143.00 -78.00   1.00    5.50    --  -87.58 -43.00 -99.00   65
  6  ω     28.00  54.00   1.00    5.50    --  102.12 -43.00 -99.00   26
  7  ω     92.00 154.00   1.00    5.50    --  102.12  43.00  51.00   62
  8  ω    -44.00 -11.00   1.00    1.50    --    6.00 122.00 178.16   33
  9  ω     -3.00  24.00   1.00    1.50    --  -51.89  19.00 -30.00   27
 10  ω     -4.00  21.00   1.00    1.50    --  -51.89  19.00-180.00   25
 11  ω   -154.00 -87.00   1.00    5.50    --  -87.58 -99.00  60.00   67
 12  ω     25.00  51.00   1.00    5.50    --  102.12 -38.00 -60.00   26
 13  ω    143.00 172.00   1.00    5.50    --  102.12 125.00 -60.00   29
 14  ω     44.00  77.00   1.00    5.50    --  102.12 -57.00-180.00   33
 15  ω     25.00  51.00   1.00    5.50    --  102.12 -38.00 120.00   26
 16  ω     37.00  66.00   1.00    5.50    --  102.12 -57.00 -60.00   29
 17  ω    104.00 175.00   1.00    5.50    --  102.12  38.00  90.00   71
 18  ω     25.00  51.00   1.00    5.50    --  102.12 -38.00 -30.00   26
 19  ω     87.00 134.00   1.00    5.50    --  102.12 125.00 -60.00   47
 20  ω     26.00  52.00   1.00    5.50    --  102.12 -38.00  90.00   26
 21  ω     42.00  93.00   1.00    5.50    --  107.25 -86.00-109.69   51
 22  ω     51.00  76.00   1.00    5.50    --  107.25 -65.00 -49.27   25
 23  ω     97.00 127.00   1.00    5.50    --  107.25-147.00 146.59   30
 24  ω     38.00  94.00   1.00    5.50    --  107.25-147.00 146.59   56
 25  ω    106.00 163.00   1.00    5.50    --  107.25   3.00 -23.04   57
 26  ω     45.00  86.00   1.00    5.50    --  107.25 -66.00  21.08   41
 27  ω     39.00  86.00   1.00    5.50    --  107.25   3.00 -23.04   47
 28  ω     44.00 130.00   1.00    5.50    --  107.25 -79.00 -66.96   86
 29  ω     68.00 141.00   1.00    5.50    --  107.25  19.00-135.88   73
 30  ω     59.00  90.00   1.00    5.50    --  107.25 -63.00 163.26   31
 31  ω    142.00 175.00   1.00    5.50    --  107.25 112.00 -93.21   33
 32  ω     99.00 126.00   1.00    5.50    --  107.25 -81.00 167.35   27
 33  ω     62.00  88.00   1.00    5.50    --  107.25-116.00-101.18   26
 34  ω     43.00  89.00   1.00    5.50    --  107.25 -81.00 167.35   46
 35  ω     40.00  76.00   1.00    5.50    --  107.25 -73.00  -8.76   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0341867000
_diffrn_orient_matrix_UB_12      -0.0263049000
_diffrn_orient_matrix_UB_13      -0.0774694000
_diffrn_orient_matrix_UB_21      -0.1118348000
_diffrn_orient_matrix_UB_22      0.0112049000
_diffrn_orient_matrix_UB_23      -0.0038977000
_diffrn_orient_matrix_UB_31      0.0082779000
_diffrn_orient_matrix_UB_32      0.0432744000
_diffrn_orient_matrix_UB_33      -0.0461043000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11541
_reflns_number_total             14655
_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         1.359
_refine_diff_density_min         -1.279
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         14655
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0809
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1234P)²+8.7724P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2226
_refine_ls_wR_factor_ref         0.2324
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N37-C38A \\sim N37-C38B
 with sigma of 0.02
 N37-C41A \\sim N37-C41B
 with sigma of 0.02
 N39-C38A \\sim N39-C38B
 with sigma of 0.02
 N39-C40A \\sim N39-C40B
 with sigma of 0.02
 C41A-C40A \\sim C41B-C40B
 with sigma of 0.02
 N37-C40A \\sim N37-C40B
 with sigma of 0.04
 N39-C41A \\sim N39-C41B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C2) = Uanis(C5) = Uanis(C4)
Uanis(C9) = Uanis(C8) = Uanis(C7) = Uanis(C6) = Uanis(C12) = Uanis(C11) =
Uanis(C10)
4. Others
 Fixed Sof: C38A(0.55) H38A(0.55) C41A(0.55) H41A(0.55) C40A(0.55) H40A(0.55)
 C40B(0.45) H40B(0.45) C41B(0.45) H41B(0.45) C38B(0.45) H38B(0.45)
5.a Rotating group:
 O77(H77A,H77B)
5.b Aromatic/amide H refined with riding coordinates:
 C65(H65), C67(H67), C69(H69), C2(H2), C14(H14), C57(H57), C33(H33),
 C38A(H38A), C17(H17), C16(H16), C35(H35), C59(H59), C23(H23), C5(H5), C20(H20),
  C36(H36), C51(H51), C54(H54), C47(H47), C30(H30), C60(H60), C52(H52), C4(H4),
 C27(H27), C44(H44), C21(H21), C22(H22), C53(H53), C29(H29), C28(H28), C45(H45),
  C46(H46), C41A(H41A), C40A(H40A), C40B(H40B), C41B(H41B), C38B(H38B),
 C11(H11), C8(H8), C10(H10), C9(H9)
;
_atom_sites_solution_hydrogens   mixed
_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 0.5000 0.5000 0.0000 0.02768(18) Uani 1 2 d S . P . .
Ni2 Ni 0.30631(3) 0.25917(2) 0.59448(3) 0.02791(15) Uani 1 1 d . . . . .
S70 S 0.51906(8) 0.45154(3) 0.82474(5) 0.0461(2) Uani 1 1 d . . . . .
O61 O 0.38285(18) 0.29661(9) 0.68759(13) 0.0402(5) Uani 1 1 d . . . . .
O77 O 0.2893(2) 0.20779(9) 0.67253(15) 0.0454(6) Uani 1 1 d . . . . .
H77A H 0.2746 0.1830 0.6475 0.068 Uiso 1 1 d R U . . .
H77B H 0.3467 0.2026 0.7051 0.068 Uiso 1 1 d R U . . .
O76 O 0.73029(19) 0.27792(9) 0.99928(14) 0.0434(6) Uani 1 1 d . . . . .
O71 O 0.4868(2) 0.46755(9) 0.89145(15) 0.0460(6) Uani 1 1 d . . . . .
O75 O 0.7349(2) 0.34734(9) 1.05047(16) 0.0552(7) Uani 1 1 d . . . . .
N13 N 0.4587(2) 0.44014(9) 0.04566(16) 0.0330(6) Uani 1 1 d . . . . .
N1 N 0.65572(19) 0.48586(10) 0.04124(16) 0.0356(6) Uani 1 1 d . . . . .
N34 N 0.3259(2) 0.31345(10) 0.52343(16) 0.0353(6) Uani 1 1 d . . . . .
O62 O 0.4632(3) 0.24101(10) 0.76399(18) 0.0665(10) Uani 1 1 d . . . . .
N58 N -0.5555(2) 0.23044(11) 0.58611(19) 0.0409(7) Uani 1 1 d . . . . .
N15 N 0.4071(3) 0.39544(11) 0.12693(18) 0.0454(7) Uani 1 1 d . . . . .
N32 N 0.3459(3) 0.35097(11) 0.42133(19) 0.0465(7) Uani 1 1 d . . . . .
N3 N 0.8194(2) 0.48654(12) 0.04790(19) 0.0459(8) Uani 1 1 d . . . . .
N37 N 0.1657(2) 0.28348(12) 0.6016(3) 0.0565(9) Uani 1 1 d D . . . .
N56 N -0.3914(2) 0.22417(13) 0.5980(2) 0.0560(9) Uani 1 1 d . . . . .
O73 O 0.4446(3) 0.45629(12) 0.75342(19) 0.0821(12) Uani 1 1 d . . . . .
O72 O 0.6162(3) 0.47132(11) 0.8225(2) 0.0744(10) Uani 1 1 d . . . . .
C68 C 0.6293(2) 0.33416(11) 0.92363(18) 0.0332(7) Uani 1 1 d . . . . .
C65 C 0.4874(3) 0.36153(12) 0.78915(18) 0.0368(7) Uani 1 1 d . . . . .
H65 H 0.4393 0.3710 0.7444 0.044 Uiso 1 1 calc R U . . .
C64 C 0.5060(2) 0.31588(12) 0.80295(18) 0.0350(7) Uani 1 1 d . . . . .
C67 C 0.6092(2) 0.37936(12) 0.91031(19) 0.0364(7) Uani 1 1 d . . . . .
H67 H 0.6417 0.4006 0.9470 0.044 Uiso 1 1 calc R U . . .
C66 C 0.5405(3) 0.39306(12) 0.84204(19) 0.0368(7) Uani 1 1 d . . . . .
C69 C 0.5778(3) 0.30273(12) 0.87023(19) 0.0363(7) Uani 1 1 d . . . . .
H69 H 0.5915 0.2723 0.8796 0.044 Uiso 1 1 calc R U . . .
C2 C 0.7241(3) 0.49255(19) 0.0022(3) 0.0624(8) Uani 1 1 d . . . . .
H2 H 0.7090 0.5005 -0.0505 0.075 Uiso 1 1 calc R U . . .
C74 C 0.7048(2) 0.31886(12) 0.99771(19) 0.0375(7) Uani 1 1 d . . . . .
C14 C 0.4579(3) 0.43367(12) 0.1192(2) 0.0367(7) Uani 1 1 d . . . . .
H14 H 0.4881 0.4528 0.1603 0.044 Uiso 1 1 calc R U . . .
C57 C -0.4713(2) 0.25245(13) 0.5902(2) 0.0419(8) Uani 1 1 d . . . . .
H57 H -0.4668 0.2837 0.5880 0.050 Uiso 1 1 calc R U . . .
C25 C 0.3581(3) 0.35992(14) 0.3439(2) 0.0474(9) Uani 1 1 d . . . . .
C18 C 0.3882(3) 0.38106(13) 0.1993(2) 0.0439(8) Uani 1 1 d . . . . .
C63 C 0.4476(3) 0.28106(13) 0.74767(19) 0.0402(8) Uani 1 1 d . . . . .
C33 C 0.3186(3) 0.31176(13) 0.4484(2) 0.0413(8) Uani 1 1 d . . . . .
H33 H 0.2971 0.2865 0.4173 0.050 Uiso 1 1 calc R U . . .
C19 C 0.4645(3) 0.35750(14) 0.2522(2) 0.0490(9) Uani 1 1 d . . . . .
C31 C 0.2978(3) 0.39440(14) 0.2154(2) 0.0477(9) Uani 1 1 d . . . . .
N39 N 0.0044(3) 0.28139(14) 0.6011(4) 0.0852(17) Uani 1 1 d D . . . .
C38A C 0.0858(7) 0.2573(5) 0.5953(12) 0.041(5) Uani 0.55 1 d D . P A 1
H38A H 0.0858 0.2262 0.5878 0.049 Uiso 0.55 1 calc R U P A 1
C48 C -0.2559(3) 0.23152(17) 0.5327(3) 0.0623(12) Uani 1 1 d . . . . .
C49 C -0.2886(3) 0.23686(15) 0.6005(3) 0.0588(12) Uani 1 1 d . . . . .
C24 C 0.4491(3) 0.34704(15) 0.3277(2) 0.0504(9) Uani 1 1 d . . . . .
C26 C 0.2809(3) 0.38285(15) 0.2904(2) 0.0517(10) Uani 1 1 d . . . . .
C17 C 0.4084(4) 0.40411(15) 0.0052(2) 0.0547(10) Uani 1 1 d . . . . .
H17 H 0.3985 0.3992 -0.0482 0.066 Uiso 1 1 calc R U . . .
C55 C -0.1249(3) 0.26697(16) 0.6714(4) 0.0701(15) Uani 1 1 d . . . . .
C16 C 0.3755(4) 0.37684(16) 0.0545(3) 0.0674(14) Uani 1 1 d . . . . .
H16 H 0.3384 0.3504 0.0415 0.081 Uiso 1 1 calc R U . . .
C35 C 0.3594(4) 0.35587(15) 0.5462(2) 0.0600(12) Uani 1 1 d . . . . .
H35 H 0.3714 0.3669 0.5970 0.072 Uiso 1 1 calc R U . . .
C43 C -0.1553(3) 0.24704(18) 0.5329(4) 0.0698(15) Uani 1 1 d . . . . .
C50 C -0.2275(3) 0.25368(16) 0.6702(3) 0.0581(12) Uani 1 1 d . . . . .
C59 C -0.5289(3) 0.18613(16) 0.5920(4) 0.0686(14) Uani 1 1 d . . . . .
H59 H -0.5738 0.1623 0.5907 0.082 Uiso 1 1 calc R U . . .
C23 C 0.5295(4) 0.32661(18) 0.3837(3) 0.0661(13) Uani 1 1 d . . . . .
H23 H 0.5220 0.3206 0.4336 0.079 Uiso 1 1 calc R U . . .
C42 C -0.0941(3) 0.26434(16) 0.6017(4) 0.0691(15) Uani 1 1 d . . . . .
C5 C 0.7092(3) 0.47526(19) 0.1162(3) 0.0624(8) Uani 1 1 d . . . . .
H5 H 0.6805 0.4691 0.1575 0.075 Uiso 1 1 calc R U . . .
C20 C 0.5570(4) 0.34384(17) 0.2352(3) 0.0651(12) Uani 1 1 d . . . . .
H20 H 0.5668 0.3492 0.1858 0.078 Uiso 1 1 calc R U . . .
C36 C 0.3726(5) 0.37936(17) 0.4843(3) 0.0721(15) Uani 1 1 d . . . . .
H36 H 0.3953 0.4089 0.4844 0.087 Uiso 1 1 calc R U . . .
C51 C -0.2596(4) 0.25909(18) 0.7407(4) 0.0720(15) Uani 1 1 d . . . . .
H51 H -0.3261 0.2514 0.7403 0.086 Uiso 1 1 calc R U . . .
C54 C -0.0604(3) 0.2819(2) 0.7441(5) 0.0864(19) Uani 1 1 d . . . . .
H54 H 0.0066 0.2898 0.7467 0.104 Uiso 1 1 calc R U . . .
C47 C -0.3173(4) 0.2117(2) 0.4633(4) 0.0786(16) Uani 1 1 d . . . . .
H47 H -0.3827 0.2021 0.4625 0.094 Uiso 1 1 calc R U . . .
C30 C 0.2216(4) 0.42013(19) 0.1625(3) 0.0655(13) Uani 1 1 d . . . . .
H30 H 0.2308 0.4279 0.1138 0.079 Uiso 1 1 calc R U . . .
C60 C -0.4278(4) 0.18172(17) 0.6001(5) 0.087(2) Uani 1 1 d . . . . .
H60 H -0.3907 0.1550 0.6059 0.105 Uiso 1 1 calc R U . . .
C52 C -0.1974(4) 0.2749(2) 0.8078(4) 0.0785(15) Uani 1 1 d . . . . .
H52 H -0.2210 0.2791 0.8522 0.094 Uiso 1 1 calc R U . . .
C4 C 0.8099(3) 0.47519(19) 0.1206(3) 0.0624(8) Uani 1 1 d . . . . .
H4 H 0.8624 0.4687 0.1644 0.075 Uiso 1 1 calc R U . . .
C27 C 0.1884(4) 0.3964(2) 0.3058(3) 0.0795(17) Uani 1 1 d . . . . .
H27 H 0.1754 0.3883 0.3531 0.095 Uiso 1 1 calc R U . . .
C44 C -0.1247(5) 0.2426(3) 0.4622(5) 0.094(2) Uani 1 1 d . . . . .
H44 H -0.0609 0.2532 0.4605 0.113 Uiso 1 1 calc R U . . .
C21 C 0.6292(4) 0.3236(2) 0.2893(4) 0.0834(18) Uani 1 1 d . . . . .
H21 H 0.6887 0.3145 0.2769 0.100 Uiso 1 1 calc R U . . .
C22 C 0.6175(4) 0.3156(2) 0.3657(4) 0.0869(19) Uani 1 1 d . . . . .
H22 H 0.6704 0.3028 0.4036 0.104 Uiso 1 1 calc R U . . .
C53 C -0.0948(4) 0.2848(2) 0.8086(5) 0.096(2) Uani 1 1 d . . . . .
H53 H -0.0501 0.2936 0.8555 0.115 Uiso 1 1 calc R U . . .
C29 C 0.1370(4) 0.4333(2) 0.1819(4) 0.0882(19) Uani 1 1 d . . . . .
H29 H 0.0896 0.4511 0.1475 0.106 Uiso 1 1 calc R U . . .
C28 C 0.1191(5) 0.4204(3) 0.2548(4) 0.102(2) Uani 1 1 d . . . . .
H28 H 0.0589 0.4287 0.2668 0.122 Uiso 1 1 calc R U . . .
C45 C -0.1848(6) 0.2235(3) 0.3977(5) 0.109(3) Uani 1 1 d . . . . .
H45 H -0.1623 0.2214 0.3523 0.131 Uiso 1 1 calc R U . . .
C46 C -0.2830(5) 0.2065(3) 0.3985(4) 0.099(2) Uani 1 1 d . . . . .
H46 H -0.3230 0.1920 0.3547 0.119 Uiso 1 1 calc R U . . .
C41A C 0.1415(7) 0.3256(3) 0.6251(9) 0.076(4) Uani 0.55 1 d D . P A 1
H41A H 0.1862 0.3498 0.6386 0.092 Uiso 0.55 1 calc R U P A 1
C40A C 0.0409(7) 0.3258(3) 0.6253(10) 0.087(4) Uani 0.55 1 d D . P A 1
H40A H 0.0040 0.3496 0.6383 0.105 Uiso 0.55 1 calc R U P A 1
C40B C 0.0131(8) 0.3212(5) 0.5570(12) 0.091(5) Uani 0.45 1 d D . P A 2
H40B H -0.0374 0.3411 0.5315 0.109 Uiso 0.45 1 calc R U P A 2
C41B C 0.1156(8) 0.3223(4) 0.5623(11) 0.081(4) Uani 0.45 1 d D . P A 2
H41B H 0.1482 0.3454 0.5427 0.097 Uiso 0.45 1 calc R U P A 2
C38B C 0.0923(9) 0.2587(5) 0.6155(14) 0.032(4) Uani 0.45 1 d D . P A 2
H38B H 0.1004 0.2291 0.6331 0.038 Uiso 0.45 1 calc R U P A 2
C6 C 0.9120(4) 0.49316(19) 0.0240(4) 0.0713(6) Uani 1 1 d . . . . .
C7 C 0.9427(3) 0.46021(19) -0.0200(4) 0.0713(6) Uani 1 1 d . . . . .
C12 C 0.9655(3) 0.53294(19) 0.0453(4) 0.0713(6) Uani 1 1 d . . . . .
C11 C 0.9345(3) 0.56776(19) 0.0896(4) 0.0713(6) Uani 1 1 d . . . . .
H11 H 0.8748 0.5644 0.1057 0.086 Uiso 1 1 calc R U . . .
C8 C 0.8889(3) 0.41931(19) -0.0382(4) 0.0713(6) Uani 1 1 d . . . . .
H8 H 0.8321 0.4140 -0.0193 0.086 Uiso 1 1 calc R U . . .
C10 C 0.9898(3) 0.60521(19) 0.1085(4) 0.0713(6) Uani 1 1 d . . . . .
H10 H 0.9690 0.6271 0.1388 0.086 Uiso 1 1 calc R U . . .
C9 C 0.9195(3) 0.38754(19) -0.0830(4) 0.0713(6) Uani 1 1 d . . . . .
H9 H 0.8817 0.3613 -0.0969 0.086 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 O71 2.112(3) 3_666 ?
Ni1 O71 2.112(3) 1_554 ?
Ni1 N13 2.087(3) . ?
Ni1 N13 2.087(3) 3_665 ?
Ni1 N1 2.097(3) . ?
Ni1 N1 2.097(3) 3_665 ?
Ni2 O61 2.037(2) . ?
Ni2 O77 2.108(3) . ?
Ni2 O76 2.054(2) 4_565 ?
Ni2 N34 2.101(3) . ?
Ni2 N58 2.103(3) 1_655 ?
Ni2 N37 2.077(3) . ?
S70 O71 1.439(3) . ?
S70 O73 1.407(3) . ?
S70 O72 1.454(3) . ?
S70 C66 1.774(4) . ?
O61 C63 1.279(4) . ?
O77 H77A 0.8561 . ?
O77 H77B 0.8561 . ?
O76 Ni2 2.054(2) 4_666 ?
O76 C74 1.262(4) . ?
O71 Ni1 2.112(3) 1_556 ?
O75 C74 1.247(4) . ?
N13 C14 1.317(4) . ?
N13 C17 1.368(5) . ?
N1 C2 1.307(5) . ?
N1 C5 1.374(5) . ?
N34 C33 1.305(4) . ?
N34 C35 1.364(5) . ?
O62 C63 1.229(5) . ?
N58 Ni2 2.103(3) 1_455 ?
N58 C57 1.303(4) . ?
N58 C59 1.361(6) . ?
N15 C14 1.353(4) . ?
N15 C18 1.432(4) . ?
N15 C16 1.358(5) . ?
N32 C25 1.444(5) . ?
N32 C33 1.346(5) . ?
N32 C36 1.369(6) . ?
N3 C2 1.352(5) . ?
N3 C4 1.365(5) . ?
N3 C6 1.441(5) . ?
N37 C38A 1.318(11) . ?
N37 C41A 1.384(8) . ?
N37 C41B 1.425(11) . ?
N37 C38B 1.312(12) . ?
N56 C57 1.352(5) . ?
N56 C49 1.436(4) . ?
N56 C60 1.358(6) . ?
C68 C67 1.377(5) . ?
C68 C69 1.383(5) . ?
C68 C74 1.511(4) . ?
C65 H65 0.9300 . ?
C65 C64 1.389(5) . ?
C65 C66 1.387(5) . ?
C64 C69 1.387(4) . ?
C64 C63 1.502(5) . ?
C67 H67 0.9300 . ?
C67 C66 1.384(4) . ?
C69 H69 0.9300 . ?
C2 H2 0.9300 . ?
C14 H14 0.9300 . ?
C57 H57 0.9300 . ?
C25 C24 1.392(6) . ?
C25 C26 1.396(6) . ?
C18 C19 1.393(6) . ?
C18 C31 1.387(6) . ?
C33 H33 0.9300 . ?
C19 C24 1.436(5) . ?
C19 C20 1.424(6) . ?
C31 C26 1.444(5) . ?
C31 C30 1.426(6) . ?
N39 C38A 1.345(11) . ?
N39 C42 1.433(5) . ?
N39 C40A 1.434(10) . ?
N39 C40B 1.438(12) . ?
N39 C38B 1.339(12) . ?
C38A H38A 0.9300 . ?
C48 C49 1.391(7) . ?
C48 C43 1.442(6) . ?
C48 C47 1.422(8) . ?
C49 C50 1.389(7) . ?
C24 C23 1.411(6) . ?
C26 C27 1.412(6) . ?
C17 H17 0.9300 . ?
C17 C16 1.346(6) . ?
C55 C50 1.445(5) . ?
C55 C42 1.401(8) . ?
C55 C54 1.427(9) . ?
C16 H16 0.9300 . ?
C35 H35 0.9300 . ?
C35 C36 1.346(6) . ?
C43 C42 1.384(9) . ?
C43 C44 1.419(9) . ?
C50 C51 1.429(8) . ?
C59 H59 0.9300 . ?
C59 C60 1.352(6) . ?
C23 H23 0.9300 . ?
C23 C22 1.352(7) . ?
C5 H5 0.9300 . ?
C5 C4 1.351(5) . ?
C20 H20 0.9300 . ?
C20 C21 1.326(8) . ?
C36 H36 0.9300 . ?
C51 H51 0.9300 . ?
C51 C52 1.352(9) . ?
C54 H54 0.9300 . ?
C54 C53 1.341(10) . ?
C47 H47 0.9300 . ?
C47 C46 1.349(9) . ?
C30 H30 0.9300 . ?
C30 C29 1.340(8) . ?
C60 H60 0.9300 . ?
C52 H52 0.9300 . ?
C52 C53 1.421(8) . ?
C4 H4 0.9300 . ?
C27 H27 0.9300 . ?
C27 C28 1.330(8) . ?
C44 H44 0.9300 . ?
C44 C45 1.345(11) . ?
C21 H21 0.9300 . ?
C21 C22 1.420(8) . ?
C22 H22 0.9300 . ?
C53 H53 0.9300 . ?
C29 H29 0.9300 . ?
C29 C28 1.423(8) . ?
C28 H28 0.9300 . ?
C45 H45 0.9300 . ?
C45 C46 1.432(10) . ?
C46 H46 0.9300 . ?
C41A H41A 0.9300 . ?
C41A C40A 1.368(10) . ?
C40A H40A 0.9300 . ?
C40B H40B 0.9300 . ?
C40B C41B 1.372(12) . ?
C41B H41B 0.9300 . ?
C38B H38B 0.9300 . ?
C6 C7 1.378(7) . ?
C6 C12 1.387(7) . ?
C7 C12 1.443(6) 3_765 ?
C7 C8 1.411(7) . ?
C12 C7 1.443(6) 3_765 ?
C12 C11 1.424(7) . ?
C11 H11 0.9300 . ?
C11 C10 1.336(7) . ?
C8 H8 0.9300 . ?
C8 C9 1.362(7) . ?
C10 H10 0.9300 . ?
C10 C9 1.433(6) 3_765 ?
C9 C10 1.433(6) 3_765 ?
C9 H9 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
O71 Ni1 O71 180.00(13) 3_666 1_554 ?
N13 Ni1 O71 90.36(11) . 3_666 ?
N13 Ni1 O71 89.64(11) . 1_554 ?
N13 Ni1 O71 90.36(11) 3_665 1_554 ?
N13 Ni1 O71 89.64(11) 3_665 3_666 ?
N13 Ni1 N13 180.00(14) . 3_665 ?
N13 Ni1 N1 92.45(11) . . ?
N13 Ni1 N1 87.55(11) 3_665 . ?
N13 Ni1 N1 92.46(11) 3_665 3_665 ?
N13 Ni1 N1 87.54(11) . 3_665 ?
N1 Ni1 O71 93.89(11) . 1_554 ?
N1 Ni1 O71 93.89(11) 3_665 3_666 ?
N1 Ni1 O71 86.11(11) . 3_666 ?
N1 Ni1 O71 86.11(11) 3_665 1_554 ?
N1 Ni1 N1 180.0 . 3_665 ?
O61 Ni2 O77 89.17(10) . . ?
O61 Ni2 O76 178.96(11) . 4_565 ?
O61 Ni2 N34 86.97(11) . . ?
O61 Ni2 N58 89.83(12) . 1_655 ?
O61 Ni2 N37 92.84(14) . . ?
O76 Ni2 O77 91.79(10) 4_565 . ?
O76 Ni2 N34 92.07(11) 4_565 . ?
O76 Ni2 N58 89.79(12) 4_565 1_655 ?
O76 Ni2 N37 87.58(14) 4_565 . ?
N34 Ni2 O77 175.99(11) . . ?
N34 Ni2 N58 90.97(11) . 1_655 ?
N58 Ni2 O77 90.12(11) 1_655 . ?
N37 Ni2 O77 87.43(13) . . ?
N37 Ni2 N34 91.66(13) . . ?
N37 Ni2 N58 176.35(13) . 1_655 ?
O71 S70 O72 110.9(2) . . ?
O71 S70 C66 104.66(16) . . ?
O73 S70 O71 113.6(2) . . ?
O73 S70 O72 112.7(3) . . ?
O73 S70 C66 107.53(19) . . ?
O72 S70 C66 106.83(19) . . ?
C63 O61 Ni2 125.0(2) . . ?
Ni2 O77 H77A 109.6 . . ?
Ni2 O77 H77B 109.6 . . ?
H77A O77 H77B 104.1 . . ?
C74 O76 Ni2 127.7(2) . 4_666 ?
S70 O71 Ni1 157.08(19) . 1_556 ?
C14 N13 Ni1 125.2(2) . . ?
C14 N13 C17 105.8(3) . . ?
C17 N13 Ni1 127.7(2) . . ?
C2 N1 Ni1 125.2(2) . . ?
C2 N1 C5 105.8(3) . . ?
C5 N1 Ni1 128.2(2) . . ?
C33 N34 Ni2 126.1(3) . . ?
C33 N34 C35 105.5(3) . . ?
C35 N34 Ni2 128.0(2) . . ?
C57 N58 Ni2 125.5(3) . 1_455 ?
C57 N58 C59 105.6(3) . . ?
C59 N58 Ni2 127.7(2) . 1_455 ?
C14 N15 C18 123.5(3) . . ?
C14 N15 C16 107.0(3) . . ?
C16 N15 C18 129.4(3) . . ?
C33 N32 C25 127.2(3) . . ?
C33 N32 C36 106.5(3) . . ?
C36 N32 C25 125.9(4) . . ?
C2 N3 C4 106.7(3) . . ?
C2 N3 C6 125.6(4) . . ?
C4 N3 C6 127.6(4) . . ?
C38A N37 Ni2 122.8(6) . . ?
C38A N37 C41A 107.8(7) . . ?
C41A N37 Ni2 128.7(4) . . ?
C41B N37 Ni2 125.8(5) . . ?
C38B N37 Ni2 124.9(6) . . ?
C38B N37 C41B 104.6(8) . . ?
C57 N56 C49 126.2(4) . . ?
C57 N56 C60 106.8(3) . . ?
C60 N56 C49 127.0(3) . . ?
C67 C68 C69 119.8(3) . . ?
C67 C68 C74 120.1(3) . . ?
C69 C68 C74 120.1(3) . . ?
C64 C65 H65 120.0 . . ?
C66 C65 H65 120.0 . . ?
C66 C65 C64 120.0(3) . . ?
C65 C64 C63 121.0(3) . . ?
C69 C64 C65 118.8(3) . . ?
C69 C64 C63 120.2(3) . . ?
C68 C67 H67 120.2 . . ?
C68 C67 C66 119.7(3) . . ?
C66 C67 H67 120.2 . . ?
C65 C66 S70 120.7(3) . . ?
C67 C66 S70 118.8(3) . . ?
C67 C66 C65 120.5(3) . . ?
C68 C69 C64 121.1(3) . . ?
C68 C69 H69 119.4 . . ?
C64 C69 H69 119.4 . . ?
N1 C2 N3 111.5(3) . . ?
N1 C2 H2 124.2 . . ?
N3 C2 H2 124.2 . . ?
O76 C74 C68 115.5(3) . . ?
O75 C74 O76 126.9(3) . . ?
O75 C74 C68 117.6(3) . . ?
N13 C14 N15 110.8(3) . . ?
N13 C14 H14 124.6 . . ?
N15 C14 H14 124.6 . . ?
N58 C57 N56 111.5(3) . . ?
N58 C57 H57 124.3 . . ?
N56 C57 H57 124.3 . . ?
C24 C25 N32 117.9(4) . . ?
C24 C25 C26 123.2(3) . . ?
C26 C25 N32 118.8(3) . . ?
C19 C18 N15 118.4(3) . . ?
C31 C18 N15 117.9(3) . . ?
C31 C18 C19 123.5(3) . . ?
O61 C63 C64 115.3(3) . . ?
O62 C63 O61 125.8(3) . . ?
O62 C63 C64 118.8(3) . . ?
N34 C33 N32 111.8(3) . . ?
N34 C33 H33 124.1 . . ?
N32 C33 H33 124.1 . . ?
C18 C19 C24 118.1(4) . . ?
C18 C19 C20 123.2(4) . . ?
C20 C19 C24 118.7(4) . . ?
C18 C31 C26 118.5(4) . . ?
C18 C31 C30 123.5(4) . . ?
C30 C31 C26 118.0(4) . . ?
C38A N39 C42 126.9(6) . . ?
C38A N39 C40A 106.4(7) . . ?
C42 N39 C40A 125.1(5) . . ?
C42 N39 C40B 120.1(6) . . ?
C38B N39 C42 127.7(6) . . ?
C38B N39 C40B 108.8(8) . . ?
N37 C38A N39 110.8(10) . . ?
N37 C38A H38A 124.6 . . ?
N39 C38A H38A 124.6 . . ?
C49 C48 C43 118.3(5) . . ?
C49 C48 C47 122.9(4) . . ?
C47 C48 C43 118.8(5) . . ?
C48 C49 N56 117.8(5) . . ?
C50 C49 N56 118.6(4) . . ?
C50 C49 C48 123.6(4) . . ?
C25 C24 C19 118.7(4) . . ?
C25 C24 C23 123.0(4) . . ?
C23 C24 C19 118.2(4) . . ?
C25 C26 C31 117.9(4) . . ?
C25 C26 C27 124.2(4) . . ?
C27 C26 C31 117.9(4) . . ?
N13 C17 H17 125.2 . . ?
C16 C17 N13 109.7(4) . . ?
C16 C17 H17 125.2 . . ?
C42 C55 C50 118.5(5) . . ?
C42 C55 C54 123.7(4) . . ?
C54 C55 C50 117.8(5) . . ?
N15 C16 H16 126.6 . . ?
C17 C16 N15 106.7(4) . . ?
C17 C16 H16 126.6 . . ?
N34 C35 H35 125.0 . . ?
C36 C35 N34 110.0(4) . . ?
C36 C35 H35 125.0 . . ?
C42 C43 C48 118.5(5) . . ?
C42 C43 C44 124.2(5) . . ?
C44 C43 C48 117.3(6) . . ?
C49 C50 C55 117.9(5) . . ?
C49 C50 C51 124.4(4) . . ?
C51 C50 C55 117.7(5) . . ?
N58 C59 H59 124.9 . . ?
C60 C59 N58 110.1(4) . . ?
C60 C59 H59 124.9 . . ?
C24 C23 H23 119.6 . . ?
C22 C23 C24 120.8(4) . . ?
C22 C23 H23 119.6 . . ?
C55 C42 N39 118.4(5) . . ?
C43 C42 N39 118.5(5) . . ?
C43 C42 C55 123.0(4) . . ?
N1 C5 H5 125.2 . . ?
C4 C5 N1 109.5(3) . . ?
C4 C5 H5 125.2 . . ?
C19 C20 H20 119.7 . . ?
C21 C20 C19 120.6(4) . . ?
C21 C20 H20 119.7 . . ?
N32 C36 H36 126.9 . . ?
C35 C36 N32 106.2(4) . . ?
C35 C36 H36 126.9 . . ?
C50 C51 H51 118.6 . . ?
C52 C51 C50 122.7(5) . . ?
C52 C51 H51 118.6 . . ?
C55 C54 H54 119.4 . . ?
C53 C54 C55 121.1(5) . . ?
C53 C54 H54 119.4 . . ?
C48 C47 H47 119.2 . . ?
C46 C47 C48 121.6(5) . . ?
C46 C47 H47 119.2 . . ?
C31 C30 H30 119.4 . . ?
C29 C30 C31 121.1(5) . . ?
C29 C30 H30 119.4 . . ?
N56 C60 H60 127.0 . . ?
C59 C60 N56 106.0(4) . . ?
C59 C60 H60 127.0 . . ?
C51 C52 H52 120.9 . . ?
C51 C52 C53 118.3(6) . . ?
C53 C52 H52 120.9 . . ?
N3 C4 H4 126.7 . . ?
C5 C4 N3 106.5(3) . . ?
C5 C4 H4 126.7 . . ?
C26 C27 H27 118.9 . . ?
C28 C27 C26 122.3(5) . . ?
C28 C27 H27 118.9 . . ?
C43 C44 H44 118.9 . . ?
C45 C44 C43 122.3(6) . . ?
C45 C44 H44 118.9 . . ?
C20 C21 H21 119.4 . . ?
C20 C21 C22 121.2(5) . . ?
C22 C21 H21 119.4 . . ?
C23 C22 C21 120.3(5) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C54 C53 C52 122.2(6) . . ?
C54 C53 H53 118.9 . . ?
C52 C53 H53 118.9 . . ?
C30 C29 H29 119.7 . . ?
C30 C29 C28 120.6(5) . . ?
C28 C29 H29 119.7 . . ?
C27 C28 C29 120.1(5) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C44 C45 H45 119.8 . . ?
C44 C45 C46 120.4(7) . . ?
C46 C45 H45 119.8 . . ?
C47 C46 C45 119.5(7) . . ?
C47 C46 H46 120.2 . . ?
C45 C46 H46 120.2 . . ?
N37 C41A H41A 125.7 . . ?
C40A C41A N37 108.5(7) . . ?
C40A C41A H41A 125.7 . . ?
N39 C40A H40A 127.3 . . ?
C41A C40A N39 105.5(7) . . ?
C41A C40A H40A 127.3 . . ?
N39 C40B H40B 129.1 . . ?
C41B C40B N39 101.8(9) . . ?
C41B C40B H40B 129.1 . . ?
N37 C41B H41B 124.3 . . ?
C40B C41B N37 111.5(9) . . ?
C40B C41B H41B 124.3 . . ?
N37 C38B N39 111.6(10) . . ?
N37 C38B H38B 124.2 . . ?
N39 C38B H38B 124.2 . . ?
C7 C6 N3 118.8(4) . . ?
C7 C6 C12 123.0(4) . . ?
C12 C6 N3 118.2(4) . . ?
C6 C7 C12 119.0(5) . 3_765 ?
C6 C7 C8 121.6(4) . . ?
C8 C7 C12 119.3(5) . 3_765 ?
C6 C12 C7 118.0(5) . 3_765 ?
C6 C12 C11 124.0(4) . . ?
C11 C12 C7 118.0(5) . 3_765 ?
C12 C11 H11 119.5 . . ?
C10 C11 C12 120.9(4) . . ?
C10 C11 H11 119.5 . . ?
C7 C8 H8 119.7 . . ?
C9 C8 C7 120.7(4) . . ?
C9 C8 H8 119.7 . . ?
C11 C10 H10 119.3 . . ?
C11 C10 C9 121.4(5) . 3_765 ?
C9 C10 H10 119.3 3_765 . ?
C8 C9 C10 119.5(5) . 3_765 ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 3_765 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O77 H77A O75 0.86 1.89 2.657(4) 148.5 4_565
O77 H77B O62 0.86 2.01 2.687(4) 135.0 .

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 N13 C14 N15 166.6(2) . . . . ?
Ni1 N13 C17 C16 -166.0(4) . . . . ?
Ni1 N1 C2 N3 170.9(3) . . . . ?
Ni1 N1 C5 C4 -170.9(4) . . . . ?
Ni2 O61 C63 O62 -10.9(6) . . . . ?
Ni2 O61 C63 C64 171.0(2) . . . . ?
Ni2 O76 C74 O75 13.1(6) 4_666 . . . ?
Ni2 O76 C74 C68 -166.6(2) 4_666 . . . ?
Ni2 N34 C33 N32 -173.4(2) . . . . ?
Ni2 N34 C35 C36 173.0(4) . . . . ?
Ni2 N58 C57 N56 168.1(3) 1_455 . . . ?
Ni2 N58 C59 C60 -167.1(4) 1_455 . . . ?
Ni2 N37 C38A N39 -179.3(8) . . . . ?
Ni2 N37 C41A C40A -176.2(9) . . . . ?
Ni2 N37 C41B C40B 159.6(12) . . . . ?
Ni2 N37 C38B N39 -167.3(9) . . . . ?
O71 S70 C66 C65 121.1(3) . . . . ?
O71 S70 C66 C67 -57.2(3) . . . . ?
N13 C17 C16 N15 -1.2(6) . . . . ?
N1 C5 C4 N3 0.9(6) . . . . ?
N34 C35 C36 N32 0.5(6) . . . . ?
N58 C59 C60 N56 -0.9(8) . . . . ?
N15 C18 C19 C24 174.0(4) . . . . ?
N15 C18 C19 C20 -5.3(6) . . . . ?
N15 C18 C31 C26 -175.7(4) . . . . ?
N15 C18 C31 C30 2.4(6) . . . . ?
N32 C25 C24 C19 -177.2(4) . . . . ?
N32 C25 C24 C23 -1.2(7) . . . . ?
N32 C25 C26 C31 175.5(4) . . . . ?
N32 C25 C26 C27 -2.9(7) . . . . ?
N3 C6 C7 C12 178.9(5) . . . 3_765 ?
N3 C6 C7 C8 -3.7(9) . . . . ?
N3 C6 C12 C7 -178.9(5) . . . 3_765 ?
N3 C6 C12 C11 0.1(9) . . . . ?
N37 C41A C40A N39 0.4(16) . . . . ?
N56 C49 C50 C55 -179.0(4) . . . . ?
N56 C49 C50 C51 0.4(7) . . . . ?
O73 S70 O71 Ni1 -140.0(4) . . . 1_556 ?
O73 S70 C66 C65 0.0(4) . . . . ?
O73 S70 C66 C67 -178.3(3) . . . . ?
O72 S70 O71 Ni1 -11.9(5) . . . 1_556 ?
O72 S70 C66 C65 -121.2(3) . . . . ?
O72 S70 C66 C67 60.5(3) . . . . ?
C68 C67 C66 S70 -177.9(3) . . . . ?
C68 C67 C66 C65 3.7(5) . . . . ?
C65 C64 C69 C68 0.9(5) . . . . ?
C65 C64 C63 O61 1.6(5) . . . . ?
C65 C64 C63 O62 -176.7(4) . . . . ?
C64 C65 C66 S70 179.1(3) . . . . ?
C64 C65 C66 C67 -2.6(5) . . . . ?
C67 C68 C69 C64 0.2(5) . . . . ?
C67 C68 C74 O76 -169.3(3) . . . . ?
C67 C68 C74 O75 11.0(5) . . . . ?
C66 S70 O71 Ni1 103.0(5) . . . 1_556 ?
C66 C65 C64 C69 0.3(5) . . . . ?
C66 C65 C64 C63 178.4(3) . . . . ?
C69 C68 C67 C66 -2.5(5) . . . . ?
C69 C68 C74 O76 12.9(5) . . . . ?
C69 C68 C74 O75 -166.9(3) . . . . ?
C69 C64 C63 O61 179.7(3) . . . . ?
C69 C64 C63 O62 1.4(6) . . . . ?
C2 N1 C5 C4 -0.8(6) . . . . ?
C2 N3 C4 C5 -0.7(6) . . . . ?
C2 N3 C6 C7 -78.5(7) . . . . ?
C2 N3 C6 C12 100.4(7) . . . . ?
C74 C68 C67 C66 179.6(3) . . . . ?
C74 C68 C69 C64 178.1(3) . . . . ?
C14 N13 C17 C16 1.6(5) . . . . ?
C14 N15 C18 C19 -83.3(5) . . . . ?
C14 N15 C18 C31 91.9(5) . . . . ?
C14 N15 C16 C17 0.3(6) . . . . ?
C57 N58 C59 C60 0.3(6) . . . . ?
C57 N56 C49 C48 -100.8(6) . . . . ?
C57 N56 C49 C50 79.2(6) . . . . ?
C57 N56 C60 C59 1.1(7) . . . . ?
C25 N32 C33 N34 172.6(3) . . . . ?
C25 N32 C36 C35 -172.9(4) . . . . ?
C25 C24 C23 C22 -178.4(6) . . . . ?
C25 C26 C27 C28 176.2(7) . . . . ?
C18 N15 C14 N13 -176.0(3) . . . . ?
C18 N15 C16 C17 176.7(4) . . . . ?
C18 C19 C24 C25 1.5(6) . . . . ?
C18 C19 C24 C23 -174.7(4) . . . . ?
C18 C19 C20 C21 176.4(5) . . . . ?
C18 C31 C26 C25 1.9(6) . . . . ?
C18 C31 C26 C27 -179.7(5) . . . . ?
C18 C31 C30 C29 -177.9(6) . . . . ?
C63 C64 C69 C68 -177.2(3) . . . . ?
C33 N34 C35 C36 -0.3(6) . . . . ?
C33 N32 C25 C24 -81.3(5) . . . . ?
C33 N32 C25 C26 101.8(5) . . . . ?
C33 N32 C36 C35 -0.4(6) . . . . ?
C19 C18 C31 C26 -0.8(6) . . . . ?
C19 C18 C31 C30 177.3(4) . . . . ?
C19 C24 C23 C22 -2.4(8) . . . . ?
C19 C20 C21 C22 -1.1(10) . . . . ?
C31 C18 C19 C24 -0.9(6) . . . . ?
C31 C18 C19 C20 179.9(4) . . . . ?
C31 C26 C27 C28 -2.2(10) . . . . ?
C31 C30 C29 C28 -2.6(11) . . . . ?
N39 C40B C41B N37 5(2) . . . . ?
C38A N37 C41A C40A -6.2(17) . . . . ?
C38A N37 C41B C40B 17.7(19) . . . . ?
C38A N37 C38B N39 -80(4) . . . . ?
C38A N39 C42 C55 110.6(12) . . . . ?
C38A N39 C42 C43 -70.9(13) . . . . ?
C38A N39 C40A C41A 5.4(16) . . . . ?
C38A N39 C40B C41B -24.9(18) . . . . ?
C38A N39 C38B N37 80(4) . . . . ?
C48 C49 C50 C55 1.0(7) . . . . ?
C48 C49 C50 C51 -179.5(4) . . . . ?
C48 C43 C42 N39 -177.6(4) . . . . ?
C48 C43 C42 C55 0.8(7) . . . . ?
C48 C43 C44 C45 -1.9(9) . . . . ?
C48 C47 C46 C45 -3.6(10) . . . . ?
C49 N56 C57 N58 177.0(4) . . . . ?
C49 N56 C60 C59 -176.8(5) . . . . ?
C49 C48 C43 C42 3.3(7) . . . . ?
C49 C48 C43 C44 -178.0(5) . . . . ?
C49 C48 C47 C46 -179.2(6) . . . . ?
C49 C50 C51 C52 178.8(5) . . . . ?
C24 C25 C26 C31 -1.2(7) . . . . ?
C24 C25 C26 C27 -179.6(5) . . . . ?
C24 C19 C20 C21 -2.9(8) . . . . ?
C24 C23 C22 C21 -1.5(10) . . . . ?
C26 C25 C24 C19 -0.4(7) . . . . ?
C26 C25 C24 C23 175.6(5) . . . . ?
C26 C31 C30 C29 0.2(8) . . . . ?
C26 C27 C28 C29 -0.1(12) . . . . ?
C17 N13 C14 N15 -1.4(4) . . . . ?
C55 C50 C51 C52 -1.7(7) . . . . ?
C55 C54 C53 C52 -2.4(10) . . . . ?
C16 N15 C14 N13 0.7(5) . . . . ?
C16 N15 C18 C19 100.8(6) . . . . ?
C16 N15 C18 C31 -84.0(6) . . . . ?
C35 N34 C33 N32 0.1(4) . . . . ?
C43 C48 C49 N56 175.8(4) . . . . ?
C43 C48 C49 C50 -4.3(7) . . . . ?
C43 C48 C47 C46 1.1(8) . . . . ?
C43 C44 C45 C46 -0.5(11) . . . . ?
C50 C55 C42 N39 174.3(4) . . . . ?
C50 C55 C42 C43 -4.1(7) . . . . ?
C50 C55 C54 C53 -1.9(8) . . . . ?
C50 C51 C52 C53 -2.4(9) . . . . ?
C59 N58 C57 N56 0.4(5) . . . . ?
C42 N39 C38A N37 -176.1(8) . . . . ?
C42 N39 C40A C41A 172.2(9) . . . . ?
C42 N39 C40B C41B -171.7(11) . . . . ?
C42 N39 C38B N37 173.1(9) . . . . ?
C42 C55 C50 C49 3.1(6) . . . . ?
C42 C55 C50 C51 -176.4(4) . . . . ?
C42 C55 C54 C53 178.3(6) . . . . ?
C42 C43 C44 C45 176.7(6) . . . . ?
C5 N1 C2 N3 0.4(6) . . . . ?
C20 C19 C24 C25 -179.2(4) . . . . ?
C20 C19 C24 C23 4.6(7) . . . . ?
C20 C21 C22 C23 3.4(11) . . . . ?
C36 N32 C25 C24 89.8(6) . . . . ?
C36 N32 C25 C26 -87.1(6) . . . . ?
C36 N32 C33 N34 0.2(5) . . . . ?
C51 C52 C53 C54 4.6(10) . . . . ?
C54 C55 C50 C49 -176.6(4) . . . . ?
C54 C55 C50 C51 3.9(7) . . . . ?
C54 C55 C42 N39 -5.9(7) . . . . ?
C54 C55 C42 C43 175.7(5) . . . . ?
C47 C48 C49 N56 -3.9(7) . . . . ?
C47 C48 C49 C50 176.1(5) . . . . ?
C47 C48 C43 C42 -177.0(5) . . . . ?
C47 C48 C43 C44 1.6(7) . . . . ?
C30 C31 C26 C25 -176.4(4) . . . . ?
C30 C31 C26 C27 2.1(7) . . . . ?
C30 C29 C28 C27 2.6(13) . . . . ?
C60 N56 C57 N58 -0.9(6) . . . . ?
C60 N56 C49 C48 76.7(7) . . . . ?
C60 N56 C49 C50 -103.3(7) . . . . ?
C4 N3 C2 N1 0.2(6) . . . . ?
C4 N3 C6 C7 104.7(7) . . . . ?
C4 N3 C6 C12 -76.4(7) . . . . ?
C44 C43 C42 N39 3.9(7) . . . . ?
C44 C43 C42 C55 -177.7(5) . . . . ?
C44 C45 C46 C47 3.3(11) . . . . ?
C41A N37 C38A N39 9.9(17) . . . . ?
C41A N37 C41B C40B -88.6(17) . . . . ?
C41A N37 C38B N39 35.6(19) . . . . ?
C40A N39 C38A N37 -9.6(17) . . . . ?
C40A N39 C42 C55 -53.5(11) . . . . ?
C40A N39 C42 C43 125.0(10) . . . . ?
C40A N39 C40B C41B 76.3(14) . . . . ?
C40A N39 C38B N37 -35.1(19) . . . . ?
C40B N39 C38A N37 40.3(17) . . . . ?
C40B N39 C42 C55 -111.3(11) . . . . ?
C40B N39 C42 C43 67.1(12) . . . . ?
C40B N39 C40A C41A -86.6(13) . . . . ?
C40B N39 C38B N37 14(2) . . . . ?
C41B N37 C38A N39 -35.8(16) . . . . ?
C41B N37 C41A C40A 78.7(13) . . . . ?
C41B N37 C38B N39 -11(2) . . . . ?
C38B N37 C38A N39 78(4) . . . . ?
C38B N37 C41A C40A -20.5(17) . . . . ?
C38B N37 C41B C40B 3(2) . . . . ?
C38B N39 C38A N37 -77(4) . . . . ?
C38B N39 C42 C55 91.9(15) . . . . ?
C38B N39 C42 C43 -89.6(15) . . . . ?
C38B N39 C40A C41A 19.4(17) . . . . ?
C38B N39 C40B C41B -11(2) . . . . ?
C6 N3 C2 N1 -177.2(4) . . . . ?
C6 N3 C4 C5 176.6(5) . . . . ?
C6 C7 C8 C9 178.8(6) . . . . ?
C6 C12 C11 C10 179.7(6) . . . . ?
C7 C6 C12 C7 0.0(11) . . . 3_765 ?
C7 C6 C12 C11 178.9(6) . . . . ?
C7 C12 C11 C10 -1.3(9) 3_765 . . . ?
C7 C8 C9 C10 3.3(9) . . . 3_765 ?
C12 C6 C7 C12 0.0(11) . . . 3_765 ?
C12 C6 C7 C8 177.4(6) . . . . ?
C12 C7 C8 C9 -3.8(9) 3_765 . . . ?
C12 C11 C10 C9 2.0(10) . . . 3_765 ?

_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 -0.306 0.000 0.000 1167.7 279.6 '12 H2O,4 DMF'
2 -0.476 0.500 0.500 1167.7 279.6 '12 H2O,4 DMF'

_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 1.426
_oxdiff_exptl_absorpt_empirical_full_min 0.751
####################################################################### 
# 
# 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_ebj-185h_r_abs_2
_database_code_depnum_ccdc_archive 'CCDC 2309440'
loop_
_audit_author_name
_audit_author_address
'Antti Marttinen'
;University of Jyvaskyla
Finland
;
_audit_update_record             
;
2023-11-21 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_audit_creation_date             2023-11-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'C116 H80 N20 Ni3 O16 S2, 12(H2 O), 6(C3 H7 N O)'
_chemical_formula_sum            'C134 H146 N26 Ni3 O34 S2'
_chemical_formula_weight         2905.01
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H20 N6 O4 S1 Ni1'
_chemical_oxdiff_usercomment     'light green block'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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                   13.63110(10)
_cell_length_b                   30.64140(10)
_cell_length_c                   16.96660(10)
_cell_angle_alpha                90
_cell_angle_beta                 104.0130(10)
_cell_angle_gamma                90
_cell_volume                     6875.65(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    40685
_cell_measurement_temperature    120.15
_cell_measurement_theta_max      78.6090
_cell_measurement_theta_min      3.0300
_shelx_estimated_absorpt_T_max   0.889
_shelx_estimated_absorpt_T_min   0.806
_exptl_absorpt_coefficient_mu    1.489
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3040
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 0 -10 0.0533
3 18 -4 0.0668
0 -19 3 0.0417
-8 -8 -1 0.0588
-5 -7 9 0.0466
0 20 0 0.0461
4 -14 -7 0.0500
6 0 -10 0.0578
-5 17 0 0.0600
8 0 1 0.0810
0 5 10 0.0237
-2 -3 -10 0.0654
-9 1 1 0.0605
3 -7 -10 0.0415

_exptl_crystal_size_max          0.151
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.081
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
4.8494 0.1251 -10.4017 -0.8918 0.0209 0.4519
2.9474 17.5508 -4.4306 -0.0154 0.0050 0.9999
0.2940 -18.9676 3.1015 -0.1999 0.2946 -0.9345
-7.6837 -8.3182 -0.5234 -0.0190 -0.8236 -0.5669
-5.3395 -6.8087 9.3048 0.6759 -0.0903 -0.7314
0.4383 19.8517 0.2232 0.4448 -0.0554 0.8939
3.7714 -13.5763 -7.4850 -0.9522 0.1250 -0.2789
5.5135 -0.1775 -10.0213 -0.8882 0.1145 0.4450
-4.5631 16.8946 0.1774 0.5086 -0.5911 0.6260
8.4720 0.3350 0.5203 -0.1791 0.9563 0.2312
-0.0199 5.1667 10.3273 0.8755 0.4765 -0.0806
-1.6731 -3.4826 -9.8221 -0.7560 -0.6477 0.0944
-8.7701 1.4728 1.4739 0.3739 -0.9013 -0.2186
2.5296 -7.2711 -10.2313 -0.9817 -0.1833 0.0522

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            75492
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.076
_diffrn_reflns_theta_min         2.884
_diffrn_ambient_temperature      120.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -54.00 -13.00   1.00    2.00    --  -87.71  57.00  30.00   41
  2  ω     -3.00  23.00   1.00    1.00    --  -54.15  19.00 -30.00   26
  3  ω    -51.00 -13.00   1.00    2.00    --  -87.71  57.00 -60.00   38
  4  ω    -24.00  20.00   1.00    1.00    --  -54.15  35.00-116.00   44
  5  ω    -30.00  -5.00   1.00    1.00    --   14.00 112.00  -4.51   25
  6  ω    -54.00 -29.00   1.00    1.00    --   18.00 154.00-149.09   25
  7  ω     95.00 127.00   1.00    2.00    --  107.25 139.00  48.60   32
  8  ω    145.00 173.00   1.00    2.00    --  107.25 139.00  48.60   28
  9  ω     37.00 101.00   1.00    1.00    --   52.65  35.00-116.00   64
 10  ω     77.00 104.00   1.00    2.00    --  106.00  20.00-135.90   27
 11  ω     86.00 122.00   1.00    2.00    --  101.96  35.00-116.00   36
 12  ω    134.00 176.00   1.00    2.00    --  101.96  35.00-116.00   42
 13  ω    150.00 175.00   1.00    2.00    --  106.00  20.00-135.90   25
 14  ω    123.00 172.00   1.00    2.00    --  107.25  32.00 -22.88   49
 15  ω     48.00  76.00   1.00    2.00    --  107.25 -78.00-111.66   28
 16  ω     36.00  70.00   1.00    2.00    --  107.25 -66.00-142.47   34
 17  ω     34.00  79.00   1.00    2.00    --  101.96 -57.00 -90.00   45
 18  ω    101.00 132.00   1.00    2.00    --  107.25 -78.00-111.66   31
 19  ω     39.00  72.00   1.00    2.00    --  107.25 -57.00-122.12   33
 20  ω     33.00  61.00   1.00    2.00    --  107.25 -52.00 -71.91   28
 21  ω     37.00  71.00   1.00    2.00    --  107.25 -55.00 -49.88   34
 22  ω     59.00  85.00   1.00    2.00    --  107.25 -67.00 -19.91   26
 23  ω     30.00  55.00   1.00    2.00    --  107.25 -43.00  63.79   25
 24  ω     38.00  68.00   1.00    2.00    --  107.25 -51.00  99.72   30
 25  ω     31.00  56.00   1.00    2.00    --  107.25 -42.00 138.20   25
 26  ω     25.00  50.00   1.00    2.00    --  101.96 -38.00 120.00   25
 27  ω     25.00  50.00   1.00    2.00    --  101.96 -38.00  90.00   25
 28  ω     27.00  52.00   1.00    2.00    --  101.96 -38.00-150.00   25
 29  ω     30.00  55.00   1.00    2.00    --  107.25 -41.00 -31.72   25
 30  ω    -20.00  45.00   1.00    1.00    --   52.65 -35.00  86.00   65
 31  ω     27.00  52.00   1.00    2.00    --  101.96 -38.00 150.00   25
 32  ω     54.00 110.00   1.00    2.00    --  107.25 -73.00 108.74   56
 33  ω     38.00 104.00   1.00    2.00    --  101.96 -99.00 120.00   66
 34  ω     48.00  92.00   1.00    2.00    --  107.25-165.00 151.04   44
 35  ω     96.00 131.00   1.00    2.00    --  107.25-165.00 151.04   35
 36  ω     45.00 119.00   1.00    2.00    --  107.25-158.00  91.56   74
 37  ω     38.00  65.00   1.00    2.00    --  107.25-103.00-138.89   27
 38  ω     69.00  95.00   1.00    2.00    --  107.25-103.00-138.89   26
 39  ω    -63.00 -38.00   1.00    1.00    --  -54.15 -35.00  86.00   25
 40  ω   -131.00 -84.00   1.00    1.00    --  -54.15 -35.00  86.00   47
 41  ω   -143.00-118.00   1.00    2.00    --  -87.71 -35.00  86.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0265367000
_diffrn_orient_matrix_UB_12      0.0221656000
_diffrn_orient_matrix_UB_13      0.0736343000
_diffrn_orient_matrix_UB_21      0.1100802000
_diffrn_orient_matrix_UB_22      -0.0057725000
_diffrn_orient_matrix_UB_23      0.0492374000
_diffrn_orient_matrix_UB_31      0.0273719000
_diffrn_orient_matrix_UB_32      0.0447637000
_diffrn_orient_matrix_UB_33      -0.0301428000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13557
_reflns_number_total             14648
_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         1.153
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     935
_refine_ls_number_reflns         14648
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0506
_refine_ls_restrained_S_all      1.063
_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)+(0.0694P)²+8.9673P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1366
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: O98A(0.8) H98A(0.8) H98B(0.8) O98B(0.2) H98C(0.2) H98D(0.2)
3.a Free rotating group:
 O94(H94A,H94B), O95(H95A,H95B), O96(H96A,H96B), O97(H97A,H97B), O83(H83A,
 H83B), O98A(H98A,H98B), O98B(H98C,H98D)
3.b Rotating group:
 O77(H77A,H77B)
3.c Aromatic/amide H refined with riding coordinates:
 C38(H38), C2(H2), C65(H65), C69(H69), C67(H67), C14(H14), C36(H36), C57(H57),
 C35(H35), C17(H17), C41(H41), C5(H5), C54(H54), C33(H33), C4(H4), C27(H27),
 C30(H30), C16(H16), C53(H53), C23(H23), C8(H8), C28(H28), C11(H11), C40(H40),
 C29(H29), C20(H20), C51(H51), C52(H52), C44(H44), C21(H21), C22(H22), C47(H47),
  C9(H9), C10(H10), C87(H87), C59(H59), C45(H45), C60(H60), C46(H46), C81(H81),
 C92(H92)
3.d Idealised Me refined as rotating group:
 C84(H84A,H84B,H84C), C85(H85A,H85B,H85C), C78(H78A,H78B,H78C), C89(H89A,H89B,
 H89C), C79(H79A,H79B,H79C), C90(H90A,H90B,H90C)
;
_atom_sites_solution_hydrogens   mixed
_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 0.5000 0.5000 1.0000 0.01169(11) Uani 1 2 d S . P . .
Ni2 Ni 0.70331(2) 0.73945(2) 0.38767(2) 0.01122(9) Uani 1 1 d . . . . .
S70 S 0.45585(4) 0.55132(2) 0.17465(3) 0.01411(10) Uani 1 1 d . . . . .
O61 O 0.62415(10) 0.70121(5) 0.29395(8) 0.0153(3) Uani 1 1 d . . . . .
O72 O 0.49734(11) 0.53120(5) 0.11154(9) 0.0187(3) Uani 1 1 d . . . . .
O76 O 0.27194(11) 0.71934(5) -0.01922(9) 0.0194(3) Uani 1 1 d . . . . .
O77 O 0.72127(11) 0.78534(5) 0.30188(8) 0.0168(3) Uani 1 1 d . . . . .
H77A H 0.6669 0.7871 0.2645 0.025 Uiso 1 1 d R U . . .
H77B H 0.7283 0.8106 0.3234 0.025 Uiso 1 1 d R U . . .
O71 O 0.52617(13) 0.54881(5) 0.25389(9) 0.0235(3) Uani 1 1 d . . . . .
O75 O 0.27713(12) 0.65433(5) -0.07993(9) 0.0242(3) Uani 1 1 d . . . . .
O62 O 0.54416(12) 0.75523(5) 0.21418(9) 0.0225(3) Uani 1 1 d . . . . .
O73 O 0.35521(12) 0.53573(5) 0.17396(10) 0.0227(3) Uani 1 1 d . . . . .
N1 N 0.34406(12) 0.50682(6) 0.95354(10) 0.0155(3) Uani 1 1 d . . . . .
N13 N 0.53167(13) 0.55911(5) 0.95139(10) 0.0152(3) Uani 1 1 d . . . . .
N34 N 0.68354(12) 0.68833(5) 0.46290(10) 0.0145(3) Uani 1 1 d . . . . .
N37 N 0.56661(12) 0.76823(6) 0.39564(10) 0.0160(3) Uani 1 1 d . . . . .
N32 N 0.66306(14) 0.65051(6) 0.56816(11) 0.0196(4) Uani 1 1 d . . . . .
N3 N 0.18051(13) 0.50472(6) 0.94618(11) 0.0171(3) Uani 1 1 d . . . . .
N39 N 0.40385(13) 0.77650(6) 0.38553(12) 0.0205(4) Uani 1 1 d . . . . .
N58 N -0.14994(14) 0.71732(6) 0.39185(13) 0.0251(4) Uani 1 1 d . . . . .
N15 N 0.57706(15) 0.60440(6) 0.86605(11) 0.0217(4) Uani 1 1 d . . . . .
O94 O 0.14759(17) 0.61045(7) -0.21470(13) 0.0436(5) Uani 1 1 d G . . . .
H94A H 0.1780 0.5937 -0.2410 0.065 Uiso 1 1 d G U . . .
H94B H 0.1910 0.6155 -0.1705 0.065 Uiso 1 1 d G U . . .
O95 O 0.03591(18) 0.65656(7) -0.34979(12) 0.0429(5) Uani 1 1 d G . . . .
H95A H 0.0691 0.6458 -0.3050 0.064 Uiso 1 1 d G U . . .
H95B H 0.0329 0.6837 -0.3405 0.064 Uiso 1 1 d G U . . .
N56 N 0.01331(14) 0.72451(7) 0.39980(14) 0.0295(5) Uani 1 1 d . . . . .
C63 C 0.55794(15) 0.71600(7) 0.23414(12) 0.0153(4) Uani 1 1 d . . . . .
C38 C 0.48092(15) 0.74783(7) 0.39153(13) 0.0169(4) Uani 1 1 d . . . . .
H38 H 0.4739 0.7170 0.3926 0.020 Uiso 1 1 calc R U . . .
C2 C 0.27506(14) 0.50252(7) 0.99529(12) 0.0157(4) Uani 1 1 d . . . . .
H2 H 0.2895 0.4984 1.0524 0.019 Uiso 1 1 calc R U . . .
C65 C 0.50067(15) 0.63822(6) 0.20216(12) 0.0147(4) Uani 1 1 d . . . . .
H65 H 0.5441 0.6292 0.2521 0.018 Uiso 1 1 calc R U . . .
C69 C 0.42560(15) 0.69527(6) 0.10986(12) 0.0147(4) Uani 1 1 d . . . . .
H69 H 0.4171 0.7254 0.0971 0.018 Uiso 1 1 calc R U . . .
C67 C 0.38205(14) 0.62039(7) 0.07531(12) 0.0149(4) Uani 1 1 d . . . . .
H67 H 0.3473 0.5991 0.0381 0.018 Uiso 1 1 calc R U . . .
C14 C 0.52998(15) 0.56647(7) 0.87451(13) 0.0171(4) Uani 1 1 d . . . . .
H14 H 0.4997 0.5476 0.8309 0.021 Uiso 1 1 calc R U . . .
C66 C 0.44505(15) 0.60759(6) 0.14951(12) 0.0143(4) Uani 1 1 d . . . . .
O88 O 0.16784(18) 0.61149(9) 0.42873(16) 0.0589(6) Uani 1 1 d . . . . .
C74 C 0.30065(15) 0.68021(7) -0.02137(12) 0.0169(4) Uani 1 1 d . . . . .
C68 C 0.37070(14) 0.66442(7) 0.05652(12) 0.0150(4) Uani 1 1 d . . . . .
C64 C 0.49254(15) 0.68229(7) 0.18137(12) 0.0150(4) Uani 1 1 d . . . . .
O96 O 0.0668(2) 0.58818(8) -0.45066(15) 0.0592(7) Uani 1 1 d G . . . .
H96A H 0.0468 0.6090 -0.4254 0.089 Uiso 1 1 d G U . . .
H96B H 0.1035 0.6004 -0.4782 0.089 Uiso 1 1 d G U . . .
C6 C 0.08812(15) 0.50239(7) 0.97260(13) 0.0170(4) Uani 1 1 d . . . . .
N86 N 0.30603(19) 0.61150(8) 0.37605(16) 0.0407(5) Uani 1 1 d . . . . .
C31 C 0.69572(18) 0.60842(7) 0.78033(13) 0.0212(4) Uani 1 1 d . . . . .
C12 C 0.06197(15) 0.53777(7) 1.01523(13) 0.0191(4) Uani 1 1 d . . . . .
C36 C 0.66304(17) 0.62079(7) 0.50745(13) 0.0212(4) Uani 1 1 d . . . . .
H36 H 0.6560 0.5900 0.5100 0.025 Uiso 1 1 calc R U . . .
C57 C -0.08082(15) 0.74011(7) 0.36882(13) 0.0183(4) Uani 1 1 d . . . . .
H57 H -0.0951 0.7649 0.3342 0.022 Uiso 1 1 calc R U . . .
C7 C 0.02883(15) 0.46467(7) 0.95581(13) 0.0194(4) Uani 1 1 d . . . . .
C26 C 0.71921(17) 0.62127(7) 0.70538(13) 0.0211(4) Uani 1 1 d . . . . .
C42 C 0.30199(15) 0.76589(7) 0.38595(14) 0.0218(4) Uani 1 1 d . . . . .
C55 C 0.23836(16) 0.74929(7) 0.31520(14) 0.0222(4) Uani 1 1 d . . . . .
C35 C 0.67527(17) 0.64468(7) 0.44286(13) 0.0200(4) Uani 1 1 d . . . . .
H35 H 0.6777 0.6330 0.3915 0.024 Uiso 1 1 calc R U . . .
C17 C 0.58213(17) 0.59389(7) 0.99439(13) 0.0215(4) Uani 1 1 d . . . . .
H17 H 0.5946 0.5976 1.0515 0.026 Uiso 1 1 calc R U . . .
C18 C 0.60004(18) 0.61855(7) 0.79186(13) 0.0220(4) Uani 1 1 d . . . . .
C24 C 0.54694(18) 0.65052(7) 0.65686(13) 0.0228(4) Uani 1 1 d . . . . .
C41 C 0.54435(17) 0.81195(7) 0.39267(16) 0.0253(5) Uani 1 1 d . . . . .
H41 H 0.5920 0.8348 0.3947 0.030 Uiso 1 1 calc R U . . .
C5 C 0.29197(16) 0.51189(8) 0.87371(13) 0.0247(5) Uani 1 1 d . . . . .
H5 H 0.3223 0.5156 0.8293 0.030 Uiso 1 1 calc R U . . .
O82 O 0.6499(2) 0.51958(9) 0.58466(17) 0.0673(7) Uani 1 1 d . . . . .
C54 C 0.27044(17) 0.74336(8) 0.24153(15) 0.0247(5) Uani 1 1 d . . . . .
H54 H 0.3368 0.7516 0.2392 0.030 Uiso 1 1 calc R U . . .
C43 C 0.27179(17) 0.77240(8) 0.45844(15) 0.0257(5) Uani 1 1 d . . . . .
C19 C 0.52509(19) 0.63960(7) 0.73325(14) 0.0234(5) Uani 1 1 d . . . . .
C25 C 0.64306(18) 0.64114(7) 0.64567(13) 0.0213(4) Uani 1 1 d . . . . .
C33 C 0.67565(18) 0.69047(7) 0.53829(13) 0.0217(4) Uani 1 1 d . . . . .
H33 H 0.6784 0.7168 0.5682 0.026 Uiso 1 1 calc R U . . .
C4 C 0.19087(16) 0.51074(9) 0.86794(14) 0.0262(5) Uani 1 1 d . . . . .
H4 H 0.1382 0.5135 0.8200 0.031 Uiso 1 1 calc R U . . .
C27 C 0.81808(18) 0.61269(8) 0.69473(14) 0.0255(5) Uani 1 1 d . . . . .
H27 H 0.8354 0.6219 0.6463 0.031 Uiso 1 1 calc R U . . .
C30 C 0.77056(19) 0.58508(8) 0.83880(14) 0.0256(5) Uani 1 1 d . . . . .
H30 H 0.7555 0.5754 0.8877 0.031 Uiso 1 1 calc R U . . .
C16 C 0.6113(2) 0.62212(8) 0.94262(14) 0.0276(5) Uani 1 1 d . . . . .
H16 H 0.6478 0.6486 0.9563 0.033 Uiso 1 1 calc R U . . .
C50 C 0.13738(16) 0.73666(7) 0.31785(16) 0.0254(5) Uani 1 1 d . . . . .
C53 C 0.20609(19) 0.72595(8) 0.17495(16) 0.0292(5) Uani 1 1 d . . . . .
H53 H 0.2283 0.7212 0.1267 0.035 Uiso 1 1 calc R U . . .
C49 C 0.10891(17) 0.74120(8) 0.39217(17) 0.0273(5) Uani 1 1 d . . . . .
C23 C 0.4685(2) 0.66978(8) 0.59514(15) 0.0297(5) Uani 1 1 d . . . . .
H23 H 0.4814 0.6770 0.5441 0.036 Uiso 1 1 calc R U . . .
C8 C 0.05399(18) 0.42844(8) 0.91159(16) 0.0274(5) Uani 1 1 d . . . . .
H8 H 0.1138 0.4294 0.8922 0.033 Uiso 1 1 calc R U . . .
C28 C 0.88803(19) 0.59144(8) 0.75325(15) 0.0286(5) Uani 1 1 d . . . . .
H28 H 0.9540 0.5865 0.7459 0.034 Uiso 1 1 calc R U . . .
C48 C 0.17202(17) 0.75920(8) 0.46200(16) 0.0280(5) Uani 1 1 d . . . . .
C11 C -0.12065(17) 0.42317(8) 0.97077(17) 0.0288(5) Uani 1 1 d . . . . .
H11 H -0.1789 0.4206 0.9918 0.035 Uiso 1 1 calc R U . . .
C40 C 0.44406(18) 0.81767(8) 0.38640(17) 0.0296(5) Uani 1 1 d . . . . .
H40 H 0.4089 0.8446 0.3833 0.036 Uiso 1 1 calc R U . . .
C29 C 0.86264(19) 0.57664(8) 0.82527(15) 0.0290(5) Uani 1 1 d . . . . .
H29 H 0.9109 0.5606 0.8644 0.035 Uiso 1 1 calc R U . . .
C20 C 0.4270(2) 0.64937(8) 0.74495(15) 0.0305(5) Uani 1 1 d . . . . .
H20 H 0.4120 0.6429 0.7955 0.037 Uiso 1 1 calc R U . . .
C51 C 0.07214(18) 0.71965(8) 0.24632(18) 0.0321(5) Uani 1 1 d . . . . .
H51 H 0.0049 0.7116 0.2466 0.039 Uiso 1 1 calc R U . . .
O97 O 0.1766(3) 0.54519(10) -0.31437(16) 0.0731(9) Uani 1 1 d G . . . .
H97A H 0.1411 0.5565 -0.3577 0.110 Uiso 1 1 d G U . . .
H97B H 0.2373 0.5502 -0.3163 0.110 Uiso 1 1 d G U . . .
C52 C 0.1051(2) 0.71481(9) 0.17748(18) 0.0349(6) Uani 1 1 d . . . . .
H52 H 0.0600 0.7038 0.1299 0.042 Uiso 1 1 calc R U . . .
C44 C 0.33664(19) 0.79147(10) 0.52845(16) 0.0340(6) Uani 1 1 d . . . . .
H44 H 0.4029 0.8001 0.5264 0.041 Uiso 1 1 calc R U . . .
C21 C 0.3554(2) 0.66777(10) 0.68488(17) 0.0374(6) Uani 1 1 d . . . . .
H21 H 0.2906 0.6740 0.6937 0.045 Uiso 1 1 calc R U . . .
C22 C 0.3759(2) 0.67788(9) 0.60856(17) 0.0359(6) Uani 1 1 d . . . . .
H22 H 0.3245 0.6904 0.5667 0.043 Uiso 1 1 calc R U . . .
C47 C 0.1444(2) 0.76600(10) 0.53802(18) 0.0386(6) Uani 1 1 d . . . . .
H47 H 0.0791 0.7573 0.5427 0.046 Uiso 1 1 calc R U . . .
N91 N -0.1516(2) 0.59060(10) 0.3102(2) 0.0519(7) Uani 1 1 d . . . . .
C9 C -0.0061(2) 0.39263(9) 0.89680(19) 0.0372(6) Uani 1 1 d . . . . .
H9 H 0.0107 0.3693 0.8656 0.045 Uiso 1 1 calc R U . . .
N80 N 0.8053(3) 0.49554(9) 0.6496(2) 0.0603(8) Uani 1 1 d . . . . .
C10 C -0.0942(2) 0.38969(9) 0.9277(2) 0.0390(7) Uani 1 1 d . . . . .
H10 H -0.1348 0.3641 0.9181 0.047 Uiso 1 1 calc R U . . .
C87 C 0.2587(2) 0.60594(11) 0.43491(19) 0.0436(7) Uani 1 1 d . . . . .
H87 H 0.2984 0.5969 0.4863 0.052 Uiso 1 1 calc R U . . .
O83 O 0.4482(3) 0.53849(11) 0.55437(19) 0.0775(8) Uani 1 1 d G . . . .
H83A H 0.5085 0.5289 0.5648 0.116 Uiso 1 1 d G U . . .
H83B H 0.4137 0.5191 0.5239 0.116 Uiso 1 1 d G U . . .
O93 O -0.0746(3) 0.64107(11) 0.2511(2) 0.0829(10) Uani 1 1 d . . . . .
C59 C -0.0961(2) 0.68656(9) 0.44639(18) 0.0351(6) Uani 1 1 d . . . . .
H59 H -0.1255 0.6659 0.4755 0.042 Uiso 1 1 calc R U . . .
C45 C 0.3061(2) 0.79767(12) 0.59827(18) 0.0431(7) Uani 1 1 d . . . . .
H45 H 0.3503 0.8109 0.6440 0.052 Uiso 1 1 calc R U . . .
C60 C 0.0045(2) 0.69061(9) 0.45171(19) 0.0383(6) Uani 1 1 d . . . . .
H60 H 0.0576 0.6738 0.4842 0.046 Uiso 1 1 calc R U . . .
C46 C 0.2085(2) 0.78434(12) 0.60235(18) 0.0464(7) Uani 1 1 d . . . . .
H46 H 0.1877 0.7884 0.6514 0.056 Uiso 1 1 calc R U . . .
C81 C 0.7102(3) 0.50435(10) 0.6450(2) 0.0522(8) Uani 1 1 d . . . . .
H81 H 0.6854 0.4986 0.6917 0.063 Uiso 1 1 calc R U . . .
C84 C 0.4138(3) 0.60503(13) 0.3890(2) 0.0533(8) Uani 1 1 d . . . . .
H84A H 0.4415 0.5943 0.4443 0.080 Uiso 1 1 calc R U . . .
H84B H 0.4461 0.6328 0.3815 0.080 Uiso 1 1 calc R U . . .
H84C H 0.4268 0.5836 0.3498 0.080 Uiso 1 1 calc R U . . .
C85 C 0.2539(3) 0.62533(13) 0.2953(2) 0.0606(9) Uani 1 1 d . . . . .
H85A H 0.1826 0.6308 0.2937 0.091 Uiso 1 1 calc R U . . .
H85B H 0.2589 0.6024 0.2562 0.091 Uiso 1 1 calc R U . . .
H85C H 0.2849 0.6522 0.2814 0.091 Uiso 1 1 calc R U . . .
C92 C -0.0730(3) 0.61475(13) 0.3059(2) 0.0560(9) Uani 1 1 d . . . . .
H92 H -0.0124 0.6116 0.3471 0.067 Uiso 1 1 calc R U . . .
C78 C 0.8693(4) 0.47704(14) 0.7229(3) 0.0820(14) Uani 1 1 d . . . . .
H78A H 0.8293 0.4723 0.7630 0.123 Uiso 1 1 calc R U . . .
H78B H 0.9249 0.4972 0.7452 0.123 Uiso 1 1 calc R U . . .
H78C H 0.8968 0.4491 0.7100 0.123 Uiso 1 1 calc R U . . .
C89 C -0.2464(3) 0.59470(18) 0.2505(3) 0.0809(14) Uani 1 1 d . . . . .
H89A H -0.2405 0.5812 0.1995 0.121 Uiso 1 1 calc R U . . .
H89B H -0.2633 0.6257 0.2412 0.121 Uiso 1 1 calc R U . . .
H89C H -0.2998 0.5801 0.2702 0.121 Uiso 1 1 calc R U . . .
C79 C 0.8497(5) 0.50496(16) 0.5812(4) 0.0934(17) Uani 1 1 d . . . . .
H79A H 0.8979 0.5291 0.5955 0.140 Uiso 1 1 calc R U . . .
H79B H 0.7961 0.5131 0.5337 0.140 Uiso 1 1 calc R U . . .
H79C H 0.8850 0.4790 0.5685 0.140 Uiso 1 1 calc R U . . .
C90 C -0.1444(5) 0.56125(15) 0.3797(4) 0.0939(18) Uani 1 1 d . . . . .
H90A H -0.1933 0.5702 0.4104 0.141 Uiso 1 1 calc R U . . .
H90B H -0.0759 0.5626 0.4149 0.141 Uiso 1 1 calc R U . . .
H90C H -0.1591 0.5313 0.3601 0.141 Uiso 1 1 calc R U . . .
O98A O 0.3773(3) 0.52889(9) -0.30631(17) 0.0482(7) Uani 0.8 1 d G . P A 2
H98A H 0.4068 0.5051 -0.2884 0.072 Uiso 0.8 1 d G U P A 2
H98B H 0.4023 0.5358 -0.3458 0.072 Uiso 0.8 1 d G U P A 2
O98B O 0.4503(13) 0.5342(4) -0.3316(9) 0.067(4) Uani 0.2 1 d G . P B 1
H98C H 0.5075 0.5453 -0.3096 0.100 Uiso 0.2 1 d G U P B 1
H98D H 0.4643 0.5097 -0.3495 0.100 Uiso 0.2 1 d G U P B 1


_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 O72 2.1284(14) 1_556 ?
Ni1 O72 2.1284(14) 3_666 ?
Ni1 N1 2.0909(17) . ?
Ni1 N1 2.0909(17) 3_667 ?
Ni1 N13 2.0784(17) . ?
Ni1 N13 2.0784(17) 3_667 ?
Ni2 O61 2.0578(14) . ?
Ni2 O76 2.0616(15) 4_676 ?
Ni2 O77 2.0806(14) . ?
Ni2 N34 2.0789(17) . ?
Ni2 N37 2.0955(17) . ?
Ni2 N58 2.0968(18) 1_655 ?
S70 O72 1.4627(15) . ?
S70 O71 1.4520(15) . ?
S70 O73 1.4500(15) . ?
S70 C66 1.774(2) . ?
O61 C63 1.267(2) . ?
O72 Ni1 2.1284(14) 1_554 ?
O76 Ni2 2.0616(14) 4_575 ?
O76 C74 1.264(3) . ?
O77 H77A 0.8522 . ?
O77 H77B 0.8522 . ?
O75 C74 1.251(3) . ?
O62 C63 1.251(3) . ?
N1 C2 1.314(3) . ?
N1 C5 1.377(3) . ?
N13 C14 1.318(3) . ?
N13 C17 1.378(3) . ?
N34 C35 1.378(3) . ?
N34 C33 1.311(3) . ?
N37 C38 1.312(3) . ?
N37 C41 1.372(3) . ?
N32 C36 1.375(3) . ?
N32 C25 1.435(3) . ?
N32 C33 1.352(3) . ?
N3 C2 1.356(3) . ?
N3 C6 1.437(2) . ?
N3 C4 1.381(3) . ?
N39 C38 1.354(3) . ?
N39 C42 1.428(3) . ?
N39 C40 1.374(3) . ?
N58 Ni2 2.0969(18) 1_455 ?
N58 C57 1.306(3) . ?
N58 C59 1.398(3) . ?
N15 C14 1.352(3) . ?
N15 C18 1.436(3) . ?
N15 C16 1.381(3) . ?
O94 H94A 0.8510 . ?
O94 H94B 0.8490 . ?
O95 H95A 0.8512 . ?
O95 H95B 0.8495 . ?
N56 C57 1.351(3) . ?
N56 C49 1.435(3) . ?
N56 C60 1.386(3) . ?
C63 C64 1.509(3) . ?
C38 H38 0.9500 . ?
C2 H2 0.9500 . ?
C65 H65 0.9500 . ?
C65 C66 1.388(3) . ?
C65 C64 1.393(3) . ?
C69 H69 0.9500 . ?
C69 C68 1.395(3) . ?
C69 C64 1.388(3) . ?
C67 H67 0.9500 . ?
C67 C66 1.397(3) . ?
C67 C68 1.386(3) . ?
C14 H14 0.9500 . ?
O88 C87 1.230(4) . ?
C74 C68 1.510(3) . ?
O96 H96A 0.8491 . ?
O96 H96B 0.8500 . ?
C6 C12 1.397(3) . ?
C6 C7 1.399(3) . ?
N86 C87 1.324(4) . ?
N86 C84 1.445(4) . ?
N86 C85 1.446(4) . ?
C31 C26 1.439(3) . ?
C31 C18 1.400(3) . ?
C31 C30 1.431(3) . ?
C12 C7 1.440(3) 3_567 ?
C12 C11 1.427(3) 3_567 ?
C36 H36 0.9500 . ?
C36 C35 1.361(3) . ?
C57 H57 0.9500 . ?
C7 C12 1.440(3) 3_567 ?
C7 C8 1.427(3) . ?
C26 C25 1.402(3) . ?
C26 C27 1.427(3) . ?
C42 C55 1.396(3) . ?
C42 C43 1.402(3) . ?
C55 C54 1.432(3) . ?
C55 C50 1.441(3) . ?
C35 H35 0.9500 . ?
C17 H17 0.9500 . ?
C17 C16 1.359(3) . ?
C18 C19 1.399(3) . ?
C24 C19 1.438(3) . ?
C24 C25 1.398(3) . ?
C24 C23 1.430(3) . ?
C41 H41 0.9500 . ?
C41 C40 1.357(3) . ?
C5 H5 0.9500 . ?
C5 C4 1.358(3) . ?
O82 C81 1.238(4) . ?
C54 H54 0.9500 . ?
C54 C53 1.360(4) . ?
C43 C48 1.434(3) . ?
C43 C44 1.423(4) . ?
C19 C20 1.430(3) . ?
C33 H33 0.9500 . ?
C4 H4 0.9500 . ?
C27 H27 0.9500 . ?
C27 C28 1.364(3) . ?
C30 H30 0.9500 . ?
C30 C29 1.354(4) . ?
C16 H16 0.9500 . ?
C50 C49 1.413(4) . ?
C50 C51 1.419(4) . ?
C53 H53 0.9500 . ?
C53 C52 1.430(4) . ?
C49 C48 1.398(4) . ?
C23 H23 0.9500 . ?
C23 C22 1.359(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.356(4) . ?
C28 H28 0.9500 . ?
C28 C29 1.423(3) . ?
C48 C47 1.444(4) . ?
C11 C12 1.427(3) 3_567 ?
C11 H11 0.9500 . ?
C11 C10 1.358(4) . ?
C40 H40 0.9500 . ?
C29 H29 0.9500 . ?
C20 H20 0.9500 . ?
C20 C21 1.352(4) . ?
C51 H51 0.9500 . ?
C51 C52 1.357(4) . ?
O97 H97A 0.8505 . ?
O97 H97B 0.8497 . ?
C52 H52 0.9500 . ?
C44 H44 0.9500 . ?
C44 C45 1.361(4) . ?
C21 H21 0.9500 . ?
C21 C22 1.424(4) . ?
C22 H22 0.9500 . ?
C47 H47 0.9500 . ?
C47 C46 1.345(5) . ?
N91 C92 1.318(4) . ?
N91 C89 1.442(5) . ?
N91 C90 1.466(6) . ?
C9 H9 0.9500 . ?
C9 C10 1.425(4) . ?
N80 C81 1.308(5) . ?
N80 C78 1.449(6) . ?
N80 C79 1.463(6) . ?
C10 H10 0.9500 . ?
C87 H87 0.9500 . ?
O83 H83A 0.8501 . ?
O83 H83B 0.8497 . ?
O93 C92 1.227(5) . ?
C59 H59 0.9500 . ?
C59 C60 1.357(4) . ?
C45 H45 0.9500 . ?
C45 C46 1.409(4) . ?
C60 H60 0.9500 . ?
C46 H46 0.9500 . ?
C81 H81 0.9500 . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C92 H92 0.9500 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C89 H89A 0.9800 . ?
C89 H89B 0.9800 . ?
C89 H89C 0.9800 . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C90 H90A 0.9800 . ?
C90 H90B 0.9800 . ?
C90 H90C 0.9800 . ?
O98A H98A 0.8511 . ?
O98A H98B 0.8496 . ?
O98B H98C 0.8502 . ?
O98B H98D 0.8502 . ?

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
O72 Ni1 O72 180.0 3_666 1_556 ?
N1 Ni1 O72 93.19(6) 3_667 3_666 ?
N1 Ni1 O72 86.81(6) 3_667 1_556 ?
N1 Ni1 O72 93.19(6) . 1_556 ?
N1 Ni1 O72 86.81(6) . 3_666 ?
N1 Ni1 N1 180.0 3_667 . ?
N13 Ni1 O72 89.35(6) . 3_666 ?
N13 Ni1 O72 90.65(6) . 1_556 ?
N13 Ni1 O72 89.35(6) 3_667 1_556 ?
N13 Ni1 O72 90.65(6) 3_667 3_666 ?
N13 Ni1 N1 86.96(7) . 3_667 ?
N13 Ni1 N1 86.95(7) 3_667 . ?
N13 Ni1 N1 93.05(7) . . ?
N13 Ni1 N1 93.04(7) 3_667 3_667 ?
N13 Ni1 N13 180.0 . 3_667 ?
O61 Ni2 O76 175.31(6) . 4_676 ?
O61 Ni2 O77 88.44(6) . . ?
O61 Ni2 N34 85.63(6) . . ?
O61 Ni2 N37 88.93(6) . . ?
O61 Ni2 N58 99.18(7) . 1_655 ?
O76 Ni2 O77 90.78(6) 4_676 . ?
O76 Ni2 N34 95.36(6) 4_676 . ?
O76 Ni2 N37 86.46(7) 4_676 . ?
O76 Ni2 N58 85.41(7) 4_676 1_655 ?
O77 Ni2 N37 91.02(6) . . ?
O77 Ni2 N58 88.24(7) . 1_655 ?
N34 Ni2 O77 173.47(6) . . ?
N34 Ni2 N37 91.60(7) . . ?
N34 Ni2 N58 90.01(7) . 1_655 ?
N37 Ni2 N58 171.82(8) . 1_655 ?
O72 S70 C66 104.94(9) . . ?
O71 S70 O72 111.71(9) . . ?
O71 S70 C66 105.78(9) . . ?
O73 S70 O72 112.83(9) . . ?
O73 S70 O71 113.65(10) . . ?
O73 S70 C66 107.17(9) . . ?
C63 O61 Ni2 123.63(13) . . ?
S70 O72 Ni1 158.91(10) . 1_554 ?
C74 O76 Ni2 130.16(13) . 4_575 ?
Ni2 O77 H77A 109.5 . . ?
Ni2 O77 H77B 109.5 . . ?
H77A O77 H77B 104.4 . . ?
C2 N1 Ni1 125.58(14) . . ?
C2 N1 C5 105.99(17) . . ?
C5 N1 Ni1 128.10(14) . . ?
C14 N13 Ni1 125.88(14) . . ?
C14 N13 C17 106.17(17) . . ?
C17 N13 Ni1 126.09(14) . . ?
C35 N34 Ni2 126.51(13) . . ?
C33 N34 Ni2 127.94(14) . . ?
C33 N34 C35 105.56(17) . . ?
C38 N37 Ni2 126.18(14) . . ?
C38 N37 C41 106.10(17) . . ?
C41 N37 Ni2 126.93(14) . . ?
C36 N32 C25 126.04(18) . . ?
C33 N32 C36 107.22(17) . . ?
C33 N32 C25 126.46(18) . . ?
C2 N3 C6 125.45(18) . . ?
C2 N3 C4 107.10(17) . . ?
C4 N3 C6 127.43(18) . . ?
C38 N39 C42 126.14(19) . . ?
C38 N39 C40 107.13(18) . . ?
C40 N39 C42 126.49(19) . . ?
C57 N58 Ni2 124.64(15) . 1_455 ?
C57 N58 C59 104.89(19) . . ?
C59 N58 Ni2 125.74(16) . 1_455 ?
C14 N15 C18 124.24(18) . . ?
C14 N15 C16 107.42(17) . . ?
C16 N15 C18 127.58(19) . . ?
H94A O94 H94B 104.4 . . ?
H95A O95 H95B 104.6 . . ?
C57 N56 C49 129.6(2) . . ?
C57 N56 C60 106.99(19) . . ?
C60 N56 C49 123.0(2) . . ?
O61 C63 C64 115.75(17) . . ?
O62 C63 O61 126.27(18) . . ?
O62 C63 C64 117.95(17) . . ?
N37 C38 N39 111.07(19) . . ?
N37 C38 H38 124.5 . . ?
N39 C38 H38 124.5 . . ?
N1 C2 N3 111.20(18) . . ?
N1 C2 H2 124.4 . . ?
N3 C2 H2 124.4 . . ?
C66 C65 H65 120.2 . . ?
C66 C65 C64 119.67(18) . . ?
C64 C65 H65 120.2 . . ?
C68 C69 H69 119.7 . . ?
C64 C69 H69 119.7 . . ?
C64 C69 C68 120.60(18) . . ?
C66 C67 H67 120.3 . . ?
C68 C67 H67 120.3 . . ?
C68 C67 C66 119.36(18) . . ?
N13 C14 N15 110.92(18) . . ?
N13 C14 H14 124.5 . . ?
N15 C14 H14 124.5 . . ?
C65 C66 S70 120.14(15) . . ?
C65 C66 C67 120.73(18) . . ?
C67 C66 S70 119.11(15) . . ?
O76 C74 C68 114.40(17) . . ?
O75 C74 O76 127.04(19) . . ?
O75 C74 C68 118.56(18) . . ?
C69 C68 C74 118.48(18) . . ?
C67 C68 C69 119.86(18) . . ?
C67 C68 C74 121.66(18) . . ?
C65 C64 C63 120.92(17) . . ?
C69 C64 C63 119.44(18) . . ?
C69 C64 C65 119.61(18) . . ?
H96A O96 H96B 104.5 . . ?
C12 C6 N3 118.41(18) . . ?
C12 C6 C7 122.63(19) . . ?
C7 C6 N3 118.96(19) . . ?
C87 N86 C84 122.0(3) . . ?
C87 N86 C85 122.3(3) . . ?
C84 N86 C85 115.6(3) . . ?
C18 C31 C26 118.5(2) . . ?
C18 C31 C30 123.1(2) . . ?
C30 C31 C26 118.4(2) . . ?
C6 C12 C7 119.00(19) . 3_567 ?
C6 C12 C11 122.28(19) . 3_567 ?
C11 C12 C7 118.7(2) 3_567 3_567 ?
N32 C36 H36 127.2 . . ?
C35 C36 N32 105.61(18) . . ?
C35 C36 H36 127.2 . . ?
N58 C57 N56 112.36(19) . . ?
N58 C57 H57 123.8 . . ?
N56 C57 H57 123.8 . . ?
C6 C7 C12 118.4(2) . 3_567 ?
C6 C7 C8 123.3(2) . . ?
C8 C7 C12 118.3(2) . 3_567 ?
C25 C26 C31 118.2(2) . . ?
C25 C26 C27 123.0(2) . . ?
C27 C26 C31 118.7(2) . . ?
C55 C42 N39 118.8(2) . . ?
C55 C42 C43 123.6(2) . . ?
C43 C42 N39 117.7(2) . . ?
C42 C55 C54 122.6(2) . . ?
C42 C55 C50 118.1(2) . . ?
C54 C55 C50 119.3(2) . . ?
N34 C35 H35 125.0 . . ?
C36 C35 N34 110.00(18) . . ?
C36 C35 H35 125.0 . . ?
N13 C17 H17 125.2 . . ?
C16 C17 N13 109.69(19) . . ?
C16 C17 H17 125.2 . . ?
C31 C18 N15 117.6(2) . . ?
C19 C18 N15 119.1(2) . . ?
C19 C18 C31 123.21(19) . . ?
C25 C24 C19 118.7(2) . . ?
C25 C24 C23 123.0(2) . . ?
C23 C24 C19 118.3(2) . . ?
N37 C41 H41 125.1 . . ?
C40 C41 N37 109.8(2) . . ?
C40 C41 H41 125.1 . . ?
N1 C5 H5 125.0 . . ?
C4 C5 N1 109.90(19) . . ?
C4 C5 H5 125.0 . . ?
C55 C54 H54 119.9 . . ?
C53 C54 C55 120.2(2) . . ?
C53 C54 H54 119.9 . . ?
C42 C43 C48 118.7(2) . . ?
C42 C43 C44 122.4(2) . . ?
C44 C43 C48 119.0(2) . . ?
C18 C19 C24 118.2(2) . . ?
C18 C19 C20 123.0(2) . . ?
C20 C19 C24 118.8(2) . . ?
C26 C25 N32 118.5(2) . . ?
C24 C25 N32 118.4(2) . . ?
C24 C25 C26 123.05(19) . . ?
N34 C33 N32 111.61(19) . . ?
N34 C33 H33 124.2 . . ?
N32 C33 H33 124.2 . . ?
N3 C4 H4 127.1 . . ?
C5 C4 N3 105.81(19) . . ?
C5 C4 H4 127.1 . . ?
C26 C27 H27 119.6 . . ?
C28 C27 C26 120.7(2) . . ?
C28 C27 H27 119.6 . . ?
C31 C30 H30 119.6 . . ?
C29 C30 C31 120.8(2) . . ?
C29 C30 H30 119.6 . . ?
N15 C16 H16 127.1 . . ?
C17 C16 N15 105.79(19) . . ?
C17 C16 H16 127.1 . . ?
C49 C50 C55 118.2(2) . . ?
C49 C50 C51 123.3(2) . . ?
C51 C50 C55 118.5(2) . . ?
C54 C53 H53 120.0 . . ?
C54 C53 C52 120.1(2) . . ?
C52 C53 H53 120.0 . . ?
C50 C49 N56 119.8(2) . . ?
C48 C49 N56 116.7(2) . . ?
C48 C49 C50 123.3(2) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 C24 120.8(2) . . ?
C22 C23 H23 119.6 . . ?
C7 C8 H8 119.5 . . ?
C9 C8 C7 121.0(2) . . ?
C9 C8 H8 119.5 . . ?
C27 C28 H28 119.8 . . ?
C27 C28 C29 120.3(2) . . ?
C29 C28 H28 119.8 . . ?
C43 C48 C47 116.9(2) . . ?
C49 C48 C43 118.1(2) . . ?
C49 C48 C47 125.0(2) . . ?
C12 C11 H11 119.6 3_567 . ?
C10 C11 C12 120.8(2) . 3_567 ?
C10 C11 H11 119.6 . . ?
N39 C40 H40 127.1 . . ?
C41 C40 N39 105.9(2) . . ?
C41 C40 H40 127.1 . . ?
C30 C29 C28 120.9(2) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C19 C20 H20 119.6 . . ?
C21 C20 C19 120.7(2) . . ?
C21 C20 H20 119.6 . . ?
C50 C51 H51 119.8 . . ?
C52 C51 C50 120.5(2) . . ?
C52 C51 H51 119.8 . . ?
H97A O97 H97B 104.5 . . ?
C53 C52 H52 119.3 . . ?
C51 C52 C53 121.4(2) . . ?
C51 C52 H52 119.3 . . ?
C43 C44 H44 119.2 . . ?
C45 C44 C43 121.6(3) . . ?
C45 C44 H44 119.2 . . ?
C20 C21 H21 119.6 . . ?
C20 C21 C22 120.8(2) . . ?
C22 C21 H21 119.6 . . ?
C23 C22 C21 120.5(2) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C48 C47 H47 119.1 . . ?
C46 C47 C48 121.7(3) . . ?
C46 C47 H47 119.1 . . ?
C92 N91 C89 120.9(4) . . ?
C92 N91 C90 119.5(4) . . ?
C89 N91 C90 119.5(4) . . ?
C8 C9 H9 119.7 . . ?
C8 C9 C10 120.5(2) . . ?
C10 C9 H9 119.7 . . ?
C81 N80 C78 120.9(4) . . ?
C81 N80 C79 120.4(4) . . ?
C78 N80 C79 118.7(4) . . ?
C11 C10 C9 120.5(2) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
O88 C87 N86 125.6(3) . . ?
O88 C87 H87 117.2 . . ?
N86 C87 H87 117.2 . . ?
H83A O83 H83B 104.5 . . ?
N58 C59 H59 125.0 . . ?
C60 C59 N58 110.0(2) . . ?
C60 C59 H59 125.0 . . ?
C44 C45 H45 120.2 . . ?
C44 C45 C46 119.6(3) . . ?
C46 C45 H45 120.2 . . ?
N56 C60 H60 127.2 . . ?
C59 C60 N56 105.6(2) . . ?
C59 C60 H60 127.2 . . ?
C47 C46 C45 121.1(3) . . ?
C47 C46 H46 119.4 . . ?
C45 C46 H46 119.4 . . ?
O82 C81 N80 125.3(4) . . ?
O82 C81 H81 117.4 . . ?
N80 C81 H81 117.4 . . ?
N86 C84 H84A 109.5 . . ?
N86 C84 H84B 109.5 . . ?
N86 C84 H84C 109.5 . . ?
H84A C84 H84B 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
N86 C85 H85A 109.5 . . ?
N86 C85 H85B 109.5 . . ?
N86 C85 H85C 109.5 . . ?
H85A C85 H85B 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
N91 C92 H92 118.4 . . ?
O93 C92 N91 123.1(4) . . ?
O93 C92 H92 118.4 . . ?
N80 C78 H78A 109.5 . . ?
N80 C78 H78B 109.5 . . ?
N80 C78 H78C 109.5 . . ?
H78A C78 H78B 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
N91 C89 H89A 109.5 . . ?
N91 C89 H89B 109.5 . . ?
N91 C89 H89C 109.5 . . ?
H89A C89 H89B 109.5 . . ?
H89A C89 H89C 109.5 . . ?
H89B C89 H89C 109.5 . . ?
N80 C79 H79A 109.5 . . ?
N80 C79 H79B 109.5 . . ?
N80 C79 H79C 109.5 . . ?
H79A C79 H79B 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
N91 C90 H90A 109.5 . . ?
N91 C90 H90B 109.5 . . ?
N91 C90 H90C 109.5 . . ?
H90A C90 H90B 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 109.5 . . ?
H98A O98A H98B 104.4 . . ?
H98C O98B H98D 104.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O77 H77A O62 0.85 1.95 2.675(2) 142.7 .
O77 H77B O75 0.85 1.94 2.698(2) 147.8 4_676
O94 H94A O97 0.85 1.94 2.709(3) 150.5 .
O94 H94B O75 0.85 2.07 2.863(2) 155.5 .
O95 H95A O94 0.85 1.97 2.807(3) 168.3 .
O95 H95B O62 0.85 2.08 2.905(2) 164.3 4_575
O96 H96A O95 0.85 1.97 2.801(3) 165.4 .
O97 H97A O96 0.85 1.92 2.765(4) 173.6 .
O97 H97B O98A 0.85 1.98 2.751(5) 149.6 .
O83 H83A O82 0.85 1.90 2.735(5) 168.4 .
O83 H83B O82 0.85 2.19 2.998(5) 160.0 3_666

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 N1 C2 N3 -174.03(13) . . . . ?
Ni1 N1 C5 C4 173.82(17) . . . . ?
Ni1 N13 C14 N15 -165.16(14) . . . . ?
Ni1 N13 C17 C16 164.74(17) . . . . ?
Ni2 O61 C63 O62 14.7(3) . . . . ?
Ni2 O61 C63 C64 -167.30(12) . . . . ?
Ni2 O76 C74 O75 -14.6(3) 4_575 . . . ?
Ni2 O76 C74 C68 165.49(13) 4_575 . . . ?
Ni2 N34 C35 C36 179.99(15) . . . . ?
Ni2 N34 C33 N32 179.80(14) . . . . ?
Ni2 N37 C38 N39 -170.02(14) . . . . ?
Ni2 N37 C41 C40 170.05(17) . . . . ?
Ni2 N58 C57 N56 161.09(17) 1_455 . . . ?
Ni2 N58 C59 C60 -159.1(2) 1_455 . . . ?
O61 C63 C64 C65 4.9(3) . . . . ?
O61 C63 C64 C69 -173.14(18) . . . . ?
O72 S70 C66 C65 -116.96(17) . . . . ?
O72 S70 C66 C67 61.37(17) . . . . ?
O76 C74 C68 C69 -22.9(3) . . . . ?
O76 C74 C68 C67 157.74(19) . . . . ?
O71 S70 O72 Ni1 155.8(2) . . . 1_554 ?
O71 S70 C66 C65 1.28(19) . . . . ?
O71 S70 C66 C67 179.61(16) . . . . ?
O75 C74 C68 C69 157.1(2) . . . . ?
O75 C74 C68 C67 -22.2(3) . . . . ?
O62 C63 C64 C65 -177.00(19) . . . . ?
O62 C63 C64 C69 5.0(3) . . . . ?
O73 S70 O72 Ni1 26.3(3) . . . 1_554 ?
O73 S70 C66 C65 122.85(17) . . . . ?
O73 S70 C66 C67 -58.81(18) . . . . ?
N1 C5 C4 N3 -0.1(3) . . . . ?
N13 C17 C16 N15 0.6(3) . . . . ?
N37 C41 C40 N39 0.0(3) . . . . ?
N32 C36 C35 N34 0.5(3) . . . . ?
N3 C6 C12 C7 -178.15(18) . . . 3_567 ?
N3 C6 C12 C11 3.6(3) . . . 3_567 ?
N3 C6 C7 C12 178.14(18) . . . 3_567 ?
N3 C6 C7 C8 -1.7(3) . . . . ?
N39 C42 C55 C54 -1.4(3) . . . . ?
N39 C42 C55 C50 176.88(19) . . . . ?
N39 C42 C43 C48 -175.8(2) . . . . ?
N39 C42 C43 C44 4.0(3) . . . . ?
N58 C59 C60 N56 0.1(4) . . . . ?
N15 C18 C19 C24 -175.29(19) . . . . ?
N15 C18 C19 C20 2.6(3) . . . . ?
N56 C49 C48 C43 174.2(2) . . . . ?
N56 C49 C48 C47 -6.3(4) . . . . ?
C38 N37 C41 C40 -0.2(3) . . . . ?
C38 N39 C42 C55 -78.1(3) . . . . ?
C38 N39 C42 C43 101.2(3) . . . . ?
C38 N39 C40 C41 0.2(3) . . . . ?
C2 N1 C5 C4 0.2(3) . . . . ?
C2 N3 C6 C12 71.1(3) . . . . ?
C2 N3 C6 C7 -107.9(2) . . . . ?
C2 N3 C4 C5 0.0(3) . . . . ?
C14 N13 C17 C16 -0.4(3) . . . . ?
C14 N15 C18 C31 -93.6(3) . . . . ?
C14 N15 C18 C19 83.2(3) . . . . ?
C14 N15 C16 C17 -0.6(3) . . . . ?
C66 S70 O72 Ni1 -90.1(3) . . . 1_554 ?
C66 C65 C64 C63 -175.23(18) . . . . ?
C66 C65 C64 C69 2.8(3) . . . . ?
C66 C67 C68 C69 3.0(3) . . . . ?
C66 C67 C68 C74 -177.70(18) . . . . ?
C68 C69 C64 C63 174.42(18) . . . . ?
C68 C69 C64 C65 -3.6(3) . . . . ?
C68 C67 C66 S70 177.86(15) . . . . ?
C68 C67 C66 C65 -3.8(3) . . . . ?
C64 C65 C66 S70 179.23(15) . . . . ?
C64 C65 C66 C67 0.9(3) . . . . ?
C64 C69 C68 C67 0.7(3) . . . . ?
C64 C69 C68 C74 -178.62(18) . . . . ?
C6 N3 C2 N1 -178.25(19) . . . . ?
C6 N3 C4 C5 178.3(2) . . . . ?
C6 C7 C8 C9 -179.9(3) . . . . ?
C31 C26 C25 N32 -174.56(19) . . . . ?
C31 C26 C25 C24 2.5(3) . . . . ?
C31 C26 C27 C28 2.1(3) . . . . ?
C31 C18 C19 C24 1.3(3) . . . . ?
C31 C18 C19 C20 179.2(2) . . . . ?
C31 C30 C29 C28 1.2(4) . . . . ?
C12 C6 C7 C12 -0.8(3) . . . 3_567 ?
C12 C6 C7 C8 179.3(2) . . . . ?
C12 C7 C8 C9 0.2(4) 3_567 . . . ?
C12 C11 C10 C9 1.1(5) 3_567 . . . ?
C36 N32 C25 C26 76.9(3) . . . . ?
C36 N32 C25 C24 -100.4(3) . . . . ?
C36 N32 C33 N34 0.1(3) . . . . ?
C57 N58 C59 C60 -2.7(3) . . . . ?
C57 N56 C49 C50 -73.6(3) . . . . ?
C57 N56 C49 C48 110.0(3) . . . . ?
C57 N56 C60 C59 2.4(3) . . . . ?
C7 C6 C12 C7 0.8(4) . . . 3_567 ?
C7 C6 C12 C11 -177.4(2) . . . 3_567 ?
C7 C8 C9 C10 -2.2(5) . . . . ?
C26 C31 C18 N15 178.31(19) . . . . ?
C26 C31 C18 C19 1.7(3) . . . . ?
C26 C31 C30 C29 2.3(3) . . . . ?
C26 C27 C28 C29 1.4(4) . . . . ?
C42 N39 C38 N37 -175.0(2) . . . . ?
C42 N39 C40 C41 174.8(2) . . . . ?
C42 C55 C54 C53 178.2(2) . . . . ?
C42 C55 C50 C49 -0.9(3) . . . . ?
C42 C55 C50 C51 -179.9(2) . . . . ?
C42 C43 C48 C49 -1.2(3) . . . . ?
C42 C43 C48 C47 179.3(2) . . . . ?
C42 C43 C44 C45 179.8(3) . . . . ?
C55 C42 C43 C48 3.5(4) . . . . ?
C55 C42 C43 C44 -176.7(2) . . . . ?
C55 C54 C53 C52 2.0(4) . . . . ?
C55 C50 C49 N56 -173.1(2) . . . . ?
C55 C50 C49 C48 3.1(3) . . . . ?
C55 C50 C51 C52 1.0(4) . . . . ?
C35 N34 C33 N32 0.2(3) . . . . ?
C17 N13 C14 N15 0.0(2) . . . . ?
C18 N15 C14 N13 171.1(2) . . . . ?
C18 N15 C16 C17 -170.9(2) . . . . ?
C18 C31 C26 C25 -3.5(3) . . . . ?
C18 C31 C26 C27 177.3(2) . . . . ?
C18 C31 C30 C29 -179.0(2) . . . . ?
C18 C19 C20 C21 -176.6(3) . . . . ?
C24 C19 C20 C21 1.3(4) . . . . ?
C24 C23 C22 C21 0.7(4) . . . . ?
C41 N37 C38 N39 0.4(2) . . . . ?
C5 N1 C2 N3 -0.2(2) . . . . ?
C54 C55 C50 C49 177.5(2) . . . . ?
C54 C55 C50 C51 -1.5(3) . . . . ?
C54 C53 C52 C51 -2.5(4) . . . . ?
C43 C42 C55 C54 179.3(2) . . . . ?
C43 C42 C55 C50 -2.4(3) . . . . ?
C43 C48 C47 C46 0.8(4) . . . . ?
C43 C44 C45 C46 1.0(5) . . . . ?
C19 C24 C25 N32 177.53(19) . . . . ?
C19 C24 C25 C26 0.4(3) . . . . ?
C19 C24 C23 C22 0.5(4) . . . . ?
C19 C20 C21 C22 -0.1(4) . . . . ?
C25 N32 C36 C35 173.9(2) . . . . ?
C25 N32 C33 N34 -174.1(2) . . . . ?
C25 C26 C27 C28 -176.9(2) . . . . ?
C25 C24 C19 C18 -2.4(3) . . . . ?
C25 C24 C19 C20 179.7(2) . . . . ?
C25 C24 C23 C22 179.3(3) . . . . ?
C33 N34 C35 C36 -0.4(3) . . . . ?
C33 N32 C36 C35 -0.3(2) . . . . ?
C33 N32 C25 C26 -110.0(3) . . . . ?
C33 N32 C25 C24 72.8(3) . . . . ?
C4 N3 C2 N1 0.1(2) . . . . ?
C4 N3 C6 C12 -106.9(3) . . . . ?
C4 N3 C6 C7 74.0(3) . . . . ?
C27 C26 C25 N32 4.5(3) . . . . ?
C27 C26 C25 C24 -178.4(2) . . . . ?
C27 C28 C29 C30 -3.1(4) . . . . ?
C30 C31 C26 C25 175.2(2) . . . . ?
C30 C31 C26 C27 -3.9(3) . . . . ?
C30 C31 C18 N15 -0.3(3) . . . . ?
C30 C31 C18 C19 -177.0(2) . . . . ?
C16 N15 C14 N13 0.4(3) . . . . ?
C16 N15 C18 C31 75.2(3) . . . . ?
C16 N15 C18 C19 -108.0(3) . . . . ?
C50 C55 C54 C53 0.0(3) . . . . ?
C50 C49 C48 C43 -2.1(4) . . . . ?
C50 C49 C48 C47 177.4(2) . . . . ?
C50 C51 C52 C53 0.9(4) . . . . ?
C49 N56 C57 N58 -176.9(3) . . . . ?
C49 N56 C60 C59 175.5(3) . . . . ?
C49 C50 C51 C52 -177.9(2) . . . . ?
C49 C48 C47 C46 -178.6(3) . . . . ?
C23 C24 C19 C18 176.5(2) . . . . ?
C23 C24 C19 C20 -1.5(3) . . . . ?
C23 C24 C25 N32 -1.3(3) . . . . ?
C23 C24 C25 C26 -178.4(2) . . . . ?
C8 C9 C10 C11 1.6(5) . . . . ?
C48 C43 C44 C45 -0.4(4) . . . . ?
C48 C47 C46 C45 -0.2(5) . . . . ?
C40 N39 C38 N37 -0.4(3) . . . . ?
C40 N39 C42 C55 108.3(3) . . . . ?
C40 N39 C42 C43 -72.4(3) . . . . ?
C20 C21 C22 C23 -1.0(5) . . . . ?
C51 C50 C49 N56 5.9(3) . . . . ?
C51 C50 C49 C48 -177.9(2) . . . . ?
C44 C43 C48 C49 179.0(2) . . . . ?
C44 C43 C48 C47 -0.5(4) . . . . ?
C44 C45 C46 C47 -0.8(5) . . . . ?
C59 N58 C57 N56 4.4(3) . . . . ?
C60 N56 C57 N58 -4.4(3) . . . . ?
C60 N56 C49 C50 115.0(3) . . . . ?
C60 N56 C49 C48 -61.4(3) . . . . ?
C84 N86 C87 O88 178.8(3) . . . . ?
C85 N86 C87 O88 0.2(5) . . . . ?
C78 N80 C81 O82 -179.0(3) . . . . ?
C89 N91 C92 O93 -1.5(6) . . . . ?
C79 N80 C81 O82 2.1(6) . . . . ?
C90 N91 C92 O93 -177.5(4) . . . . ?

_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 1.121
_oxdiff_exptl_absorpt_empirical_full_min 0.899
####################################################################### 
# 
# 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_ebj-185n-dry_r_abs
_database_code_depnum_ccdc_archive 'CCDC 2309441'
loop_
_audit_author_name
_audit_author_address
'Antti Marttinen'
;University of Jyvaskyla
Finland
;
_audit_update_record             
;
2023-11-21 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_audit_creation_date             2023-11-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C116 H80 N20 Ni3 O16 S2, 4[C3H7NO], 14[H2O]'
_chemical_formula_sum            'C128 H136 N24 Ni3 O34 S2'
_chemical_formula_weight         2794.85
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20 H14 N4 O6 S1 Ni1'
_chemical_oxdiff_usercomment     'pale/light green cut block'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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                   13.61780(10)
_cell_length_b                   29.7718(2)
_cell_length_c                   17.1157(2)
_cell_angle_alpha                90
_cell_angle_beta                 104.0980(10)
_cell_angle_gamma                90
_cell_volume                     6730.15(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    31802
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      78.6090
_cell_measurement_theta_min      2.9890
_shelx_estimated_absorpt_T_max   0.855
_shelx_estimated_absorpt_T_min   0.777
_exptl_absorpt_coefficient_mu    1.495
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2920
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 1 0.0768
8 5 -6 0.0853
-1 19 -1 0.0616
4 -12 6 0.0613
0 15 7 0.0597
-1 10 -9 0.0509
-8 7 0 0.0568
-3 18 3 0.0488
-4 -9 -7 0.0439
2 -9 -10 0.0431
-1 -18 -4 0.0459
-6 13 4 0.0422
7 -7 3 0.0697
5 16 -1 0.0678
-4 -9 9 0.0772

_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.108
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.9978 -0.0011 0.9993 0.0150 -0.1280 -0.0166
7.9067 4.7938 -6.4262 -0.0782 0.9859 -0.1476
-1.0427 19.0742 -0.8892 0.6669 0.1266 -0.7343
3.7431 -12.4057 5.7424 -0.9902 -0.0794 0.1148
-0.1340 14.5617 7.1259 -0.0256 -0.2198 -0.9752
-0.5312 9.5113 -9.1955 0.8758 0.4770 0.0742
-8.0221 7.2915 0.4770 0.7925 -0.6064 -0.0652
-2.9198 17.9819 2.6247 0.5636 -0.2013 -0.8012
-4.3317 -8.9685 -6.6211 0.4946 -0.1156 0.8614
2.0265 -9.2787 -9.7459 0.1891 0.5436 0.8178
-0.7076 -17.8820 -3.7836 -0.2091 -0.0360 0.9772
-6.2640 13.1552 3.9299 0.6062 -0.5761 -0.5482
6.8835 -6.7723 3.4948 -0.9363 0.3308 -0.1183
4.9781 15.9680 -1.4136 0.1484 0.6105 -0.7780
-4.0853 -9.4716 9.2158 -0.5198 -0.8507 0.0784

_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            73390
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.073
_diffrn_reflns_theta_min         2.969
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -29.00  -4.00   1.00    0.20    --   14.00 110.00-150.99   25
  2  ω    -44.00 -19.00   1.00    1.00    --  -87.58  57.00 -60.00   25
  3  ω    -37.00 -11.00   1.00    1.00    --  -87.58  46.00  92.00   26
  4  ω    -36.00  19.00   1.00    0.20    --  -51.89  46.00  92.00   55
  5  ω     -2.00  23.00   1.00    0.20    --   34.00  98.00 179.40   25
  6  ω     91.00 174.00   1.00    1.00    --  107.25  94.00  85.31   83
  7  ω     40.00 123.00   1.00    0.20    --   51.89  46.00  92.00   83
  8  ω    115.00 154.00   1.00    1.00    --  102.12  46.00  92.00   39
  9  ω    129.00 155.00   1.00    1.00    --  107.25  46.00  75.75   26
 10  ω     43.00 114.00   1.00    1.00    --  107.25   8.00-102.71   71
 11  ω     25.00  50.00   1.00    1.00    --  102.12 -38.00-180.00   25
 12  ω     41.00  73.00   1.00    1.00    --  107.25 -76.00-146.10   32
 13  ω     47.00  73.00   1.00    1.00    --  107.25 -73.00-120.92   26
 14  ω     76.00 117.00   1.00    1.00    --  107.25 -73.00-120.92   41
 15  ω     42.00  71.00   1.00    1.00    --  102.12 -57.00 -90.00   29
 16  ω     51.00  86.00   1.00    1.00    --  107.25 -61.00  14.26   35
 17  ω     35.00  88.00   1.00    1.00    --  107.25 -62.00  57.53   53
 18  ω     28.00  64.00   1.00    1.00    --  102.12 -57.00  90.00   36
 19  ω     35.00  61.00   1.00    1.00    --  102.12 -57.00 150.00   26
 20  ω     34.00  84.00   1.00    1.00    --  107.25 -60.00 119.62   50
 21  ω     29.00  55.00   1.00    1.00    --  102.12 -46.00 -57.00   26
 22  ω     29.00  70.00   1.00    1.00    --  102.12 -57.00-120.00   41
 23  ω     33.00  63.00   1.00    1.00    --  107.25 -56.00-155.83   30
 24  ω     25.00  50.00   1.00    1.00    --  102.12 -38.00   0.00   25
 25  ω     25.00  50.00   1.00    1.00    --  102.12 -38.00 -30.00   25
 26  ω    -23.00  58.00   1.00    0.20    --   51.89 -46.00 -57.00   81
 27  ω     25.00  50.00   1.00    1.00    --  102.12 -38.00  90.00   25
 28  ω    111.00 136.00   1.00    1.00    --  107.25 -84.00 -24.62   25
 29  ω     80.00 129.00   1.00    1.00    --  107.25 -88.00  11.98   49
 30  ω     41.00  76.00   1.00    1.00    --  107.25 -88.00  11.98   35
 31  ω     55.00  97.00   1.00    1.00    --  107.25 -84.00 -24.62   42
 32  ω     48.00 104.00   1.00    1.00    --  107.25-122.00-128.96   56
 33  ω   -112.00 -76.00   1.00    1.00    --  -87.58 -46.00 -57.00   36
 34  ω   -162.00-119.00   1.00    1.00    --  -87.58 -46.00 -57.00   43
 35  ω   -154.00 -87.00   1.00    1.00    --  -87.58 -99.00  60.00   67
 36  ω    -83.00 -37.00   1.00    0.20    --  -51.89 -46.00 -57.00   46
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0771476000
_diffrn_orient_matrix_UB_12      0.0278587000
_diffrn_orient_matrix_UB_13      -0.0619654000
_diffrn_orient_matrix_UB_21      0.0808148000
_diffrn_orient_matrix_UB_22      0.0088437000
_diffrn_orient_matrix_UB_23      -0.0473955000
_diffrn_orient_matrix_UB_31      -0.0336525000
_diffrn_orient_matrix_UB_32      -0.0426801000
_diffrn_orient_matrix_UB_33      -0.0502710000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12816
_reflns_number_total             14350
_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 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         1.723
_refine_diff_density_min         -1.574
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         14350
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0857
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1010P)²+17.9068P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2222
_refine_ls_wR_factor_ref         0.2267
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N37-C38A \\sim N37-C38B
 with sigma of 0.02
 N37-C41A \\sim N37-C41B
 with sigma of 0.02
 N39-C38A \\sim N39-C38B
 with sigma of 0.02
 N39-C40A \\sim N39-C40B
 with sigma of 0.02
 C41A-C40A \\sim C41B-C40B
 with sigma of 0.02
 N37-C40A \\sim N37-C40B
 with sigma of 0.04
 N39-C41A \\sim N39-C41B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(N39) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C44)
\\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C41B) \\sim Ueq, Uanis(C38B) \\sim Ueq, Uanis(C40B) \\sim Ueq: with sigma
of 0.05 and sigma for terminal atoms of 0.1
Uanis(C38A) \\sim Ueq, Uanis(C38B) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C53) = Uanis(C44) = Uanis(C45) = Uanis(C46) = Uanis(C47) = Uanis(C48) =
Uanis(C43) = Uanis(C55) = Uanis(C54) = Uanis(C52) = Uanis(C51) = Uanis(C50)
Uanis(N39) = Uanis(N37) = Uanis(N56) = Uanis(N58)
Uanis(C10) = Uanis(C11) = Uanis(C12) = Uanis(C7) = Uanis(C8) = Uanis(C9)
4. Others
 Fixed Sof: C38A(0.65) H38A(0.65) C41A(0.65) H41A(0.65) C40A(0.65) H40A(0.65)
 C41B(0.35) H41B(0.35) C40B(0.35) H40B(0.35) C38B(0.35) H38B(0.35)
5.a Rotating group:
 O77(H77A,H77B)
5.b Aromatic/amide H refined with riding coordinates:
 C65(H65), C14(H14), C67(H67), C57(H57), C2(H2), C17(H17), C69(H69), C33(H33),
 C27(H27), C20(H20), C16(H16), C5(H5), C59(H59), C29(H29), C47(H47), C23(H23),
 C28(H28), C4(H4), C30(H30), C21(H21), C35(H35), C36(H36), C22(H22), C60(H60),
 C8(H8), C51(H51), C11(H11), C54(H54), C44(H44), C46(H46), C52(H52), C45(H45),
 C9(H9), C53(H53), C10(H10), C38A(H38A), C41A(H41A), C40A(H40A), C41B(H41B),
 C40B(H40B), C38B(H38B)
;
_atom_sites_solution_hydrogens   mixed
_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 1.0000 0.5000 0.0000 0.02551(19) Uani 1 2 d S . P . .
Ni2 Ni 0.79204(4) 0.25859(2) 0.60675(3) 0.02440(15) Uani 1 1 d . . . . .
S70 S 0.52367(6) 0.04844(3) 0.32055(5) 0.0342(2) Uani 1 1 d . . . . .
O75 O 0.36859(18) 0.20377(9) 0.20039(13) 0.0329(5) Uani 1 1 d . . . . .
O72 O 0.48668(19) 0.02919(8) 0.38622(16) 0.0353(5) Uani 1 1 d . . . . .
O77 O 0.78042(19) 0.20738(10) 0.68855(15) 0.0384(6) Uani 1 1 d . . . . .
H77A H 0.7714 0.1816 0.6633 0.058 Uiso 1 1 d R U . . .
H77B H 0.8382 0.2044 0.7238 0.058 Uiso 1 1 d R U . . .
O61 O 0.7186(2) 0.21998(9) 0.51297(16) 0.0436(7) Uani 1 1 d . . . . .
O76 O 0.4553(2) 0.25895(9) 0.27742(15) 0.0423(6) Uani 1 1 d . . . . .
O62 O 0.7243(2) 0.15062(9) 0.56587(17) 0.0464(7) Uani 1 1 d . . . . .
N13 N 0.95692(19) 0.43969(9) 0.04447(17) 0.0284(6) Uani 1 1 d . . . . .
N58 N -0.0711(2) 0.23060(12) 0.5949(3) 0.0527(5) Uani 1 1 d . . . . .
O71 O 0.4478(2) 0.04581(11) 0.24447(17) 0.0490(7) Uani 1 1 d . . . . .
N15 N 0.9018(2) 0.39506(10) 0.12708(18) 0.0321(6) Uani 1 1 d . . . . .
N32 N 0.8273(2) 0.35142(10) 0.42829(17) 0.0322(6) Uani 1 1 d . . . . .
O73 O 0.6215(2) 0.03070(11) 0.3168(2) 0.0536(8) Uani 1 1 d . . . . .
N34 N 0.8077(2) 0.31331(10) 0.53344(16) 0.0299(6) Uani 1 1 d . . . . .
N1 N 0.84565(19) 0.51398(10) -0.04142(19) 0.0308(6) Uani 1 1 d . . . . .
N56 N 0.0921(2) 0.22384(12) 0.6056(3) 0.0527(5) Uani 1 1 d . . . . .
N3 N 0.6820(2) 0.51195(12) -0.0489(2) 0.0406(8) Uani 1 1 d . . . . .
C65 C 0.6072(2) 0.11858(12) 0.4162(2) 0.0310(7) Uani 1 1 d . . . . .
H65 H 0.6425 0.0964 0.4522 0.037 Uiso 1 1 calc R U . . .
C66 C 0.5408(2) 0.10607(12) 0.3446(2) 0.0298(7) Uani 1 1 d . . . . .
C68 C 0.4979(2) 0.18342(12) 0.31231(19) 0.0296(7) Uani 1 1 d . . . . .
C74 C 0.4365(3) 0.21879(13) 0.25935(19) 0.0335(7) Uani 1 1 d . . . . .
C18 C 0.8801(3) 0.38102(11) 0.2013(2) 0.0305(7) Uani 1 1 d . . . . .
C14 C 0.9567(2) 0.43200(12) 0.1200(2) 0.0298(7) Uani 1 1 d . . . . .
H14 H 0.9908 0.4501 0.1640 0.036 Uiso 1 1 calc R U . . .
C67 C 0.4846(2) 0.13793(12) 0.29278(19) 0.0287(7) Uani 1 1 d . . . . .
H67 H 0.4377 0.1288 0.2447 0.034 Uiso 1 1 calc R U . . .
C31 C 0.9549(3) 0.35841(12) 0.2576(2) 0.0327(7) Uani 1 1 d . . . . .
C57 C 0.0138(2) 0.25232(12) 0.5998(2) 0.0289(7) Uani 1 1 d . . . . .
H57 H 0.0194 0.2841 0.5993 0.035 Uiso 1 1 calc R U . . .
C25 C 0.8435(3) 0.36041(12) 0.3492(2) 0.0318(7) Uani 1 1 d . . . . .
C26 C 0.9368(3) 0.34886(12) 0.3352(2) 0.0323(7) Uani 1 1 d . . . . .
C2 C 0.7767(2) 0.50684(12) -0.0011(2) 0.0331(8) Uani 1 1 d . . . . .
H2 H 0.7911 0.4991 0.0543 0.040 Uiso 1 1 calc R U . . .
C17 C 0.8997(3) 0.40606(12) 0.0004(2) 0.0346(7) Uani 1 1 d . . . . .
H17 H 0.8867 0.4027 -0.0564 0.042 Uiso 1 1 calc R U . . .
C69 C 0.5677(3) 0.19589(12) 0.3825(2) 0.0312(7) Uani 1 1 d . . . . .
H69 H 0.5788 0.2268 0.3952 0.037 Uiso 1 1 calc R U . . .
C19 C 0.7873(2) 0.39372(12) 0.2161(2) 0.0308(7) Uani 1 1 d . . . . .
C24 C 0.7674(3) 0.38170(13) 0.2928(2) 0.0344(7) Uani 1 1 d . . . . .
C33 C 0.8119(3) 0.31086(13) 0.4584(2) 0.0346(7) Uani 1 1 d . . . . .
H33 H 0.8050 0.2837 0.4283 0.041 Uiso 1 1 calc R U . . .
C27 C 1.0175(3) 0.32923(14) 0.3959(2) 0.0388(8) Uani 1 1 d . . . . .
H27 H 1.0079 0.3232 0.4480 0.047 Uiso 1 1 calc R U . . .
C63 C 0.6942(3) 0.17853(14) 0.5118(2) 0.0389(8) Uani 1 1 d . . . . .
N37 N 0.6519(2) 0.28139(12) 0.6178(3) 0.0527(5) Uani 1 1 d D . . . .
C64 C 0.6216(2) 0.16356(12) 0.4347(2) 0.0318(7) Uani 1 1 d . . . . .
C6 C 0.5891(2) 0.50592(13) -0.0242(3) 0.0381(9) Uani 1 1 d . . . . .
C49 C 0.1941(2) 0.23570(13) 0.6074(3) 0.0420(10) Uani 1 1 d . . . . .
C20 C 0.7127(3) 0.41893(13) 0.1602(2) 0.0371(8) Uani 1 1 d . . . . .
H20 H 0.7254 0.4279 0.1103 0.045 Uiso 1 1 calc R U . . .
C16 C 0.8648(3) 0.37841(13) 0.0510(2) 0.0412(9) Uani 1 1 d . . . . .
H16 H 0.8231 0.3527 0.0365 0.049 Uiso 1 1 calc R U . . .
C48 C 0.2274(4) 0.2309(2) 0.5367(4) 0.0670(5) Uani 1 1 d . . . . .
C12 C 0.5598(3) 0.53885(18) 0.0221(4) 0.0658(6) Uani 1 1 d . . . . .
C7 C 0.5329(3) 0.46684(18) -0.0483(4) 0.0658(6) Uani 1 1 d . . . . .
C5 C 0.7937(3) 0.52404(18) -0.1185(3) 0.0499(11) Uani 1 1 d . . . . .
H5 H 0.8239 0.5308 -0.1616 0.060 Uiso 1 1 calc R U . . .
C43 C 0.3277(4) 0.2467(2) 0.5362(4) 0.0670(5) Uani 1 1 d . . . . .
C59 C -0.0468(3) 0.18584(14) 0.5970(3) 0.0524(12) Uani 1 1 d . . . . .
H59 H -0.0934 0.1618 0.5947 0.063 Uiso 1 1 calc R U . . .
C50 C 0.2551(4) 0.2520(2) 0.6788(4) 0.0670(5) Uani 1 1 d . . . . .
C29 C 1.1236(3) 0.32676(17) 0.3021(3) 0.0545(12) Uani 1 1 d . . . . .
H29 H 1.1864 0.3185 0.2913 0.065 Uiso 1 1 calc R U . . .
C47 C 0.1668(4) 0.2122(2) 0.4655(4) 0.0670(5) Uani 1 1 d . . . . .
H47 H 0.1012 0.2012 0.4649 0.080 Uiso 1 1 calc R U . . .
C42 C 0.3877(3) 0.26221(15) 0.6073(4) 0.0628(16) Uani 1 1 d . . . . .
C23 C 0.6709(3) 0.39316(17) 0.3067(3) 0.0486(10) Uani 1 1 d . . . . .
H23 H 0.6551 0.3845 0.3557 0.058 Uiso 1 1 calc R U . . .
C28 C 1.1072(3) 0.31924(16) 0.3790(3) 0.0494(11) Uani 1 1 d . . . . .
H28 H 1.1601 0.3069 0.4201 0.059 Uiso 1 1 calc R U . . .
C4 C 0.6927(3) 0.5230(2) -0.1242(3) 0.0575(13) Uani 1 1 d . . . . .
H4 H 0.6400 0.5287 -0.1708 0.069 Uiso 1 1 calc R U . . .
C30 C 1.0503(3) 0.34577(14) 0.2430(3) 0.0417(9) Uani 1 1 d . . . . .
H30 H 1.0625 0.3507 0.1914 0.050 Uiso 1 1 calc R U . . .
C21 C 0.6238(3) 0.43022(17) 0.1776(3) 0.0491(10) Uani 1 1 d . . . . .
H21 H 0.5757 0.4477 0.1404 0.059 Uiso 1 1 calc R U . . .
C55 C 0.3575(4) 0.2644(2) 0.6805(4) 0.0670(5) Uani 1 1 d . . . . .
N39 N 0.4885(2) 0.27941(12) 0.6115(3) 0.0527(5) Uani 1 1 d D U . . .
C35 C 0.8177(4) 0.35729(15) 0.5530(3) 0.0569(13) Uani 1 1 d . . . . .
H35 H 0.8168 0.3695 0.6040 0.068 Uiso 1 1 calc R U . . .
C36 C 0.8293(4) 0.38129(15) 0.4887(3) 0.0551(12) Uani 1 1 d . . . . .
H36 H 0.8373 0.4129 0.4862 0.066 Uiso 1 1 calc R U . . .
C22 C 0.6019(3) 0.4162(2) 0.2505(3) 0.0609(14) Uani 1 1 d . . . . .
H22 H 0.5378 0.4230 0.2602 0.073 Uiso 1 1 calc R U . . .
C60 C 0.0536(3) 0.18098(15) 0.6030(4) 0.0614(15) Uani 1 1 d . . . . .
H60 H 0.0899 0.1536 0.6049 0.074 Uiso 1 1 calc R U . . .
C8 C 0.5616(4) 0.43312(17) -0.0961(4) 0.0658(6) Uani 1 1 d . . . . .
H8 H 0.6243 0.4357 -0.1108 0.079 Uiso 1 1 calc R U . . .
C51 C 0.2208(4) 0.2575(2) 0.7520(4) 0.0670(5) Uani 1 1 d . . . . .
H51 H 0.1526 0.2502 0.7510 0.080 Uiso 1 1 calc R U . . .
C11 C 0.6181(4) 0.57842(18) 0.0454(4) 0.0658(6) Uani 1 1 d . . . . .
H11 H 0.6767 0.5836 0.0258 0.079 Uiso 1 1 calc R U . . .
C54 C 0.4209(4) 0.2777(2) 0.7607(4) 0.0670(5) Uani 1 1 d . . . . .
H54 H 0.4902 0.2847 0.7655 0.080 Uiso 1 1 calc R U . . .
C44 C 0.3582(4) 0.2451(2) 0.4623(4) 0.0670(5) Uani 1 1 d . U . . .
H44 H 0.4228 0.2565 0.4603 0.080 Uiso 1 1 calc R U . . .
C46 C 0.2020(4) 0.2099(2) 0.3971(4) 0.0670(5) Uani 1 1 d . . . . .
H46 H 0.1624 0.1961 0.3498 0.080 Uiso 1 1 calc R U . . .
C52 C 0.2822(4) 0.2728(2) 0.8222(4) 0.0670(5) Uani 1 1 d . . . . .
H52 H 0.2556 0.2782 0.8677 0.080 Uiso 1 1 calc R U . . .
C45 C 0.2993(4) 0.2285(2) 0.3977(4) 0.0670(5) Uani 1 1 d . U . . .
H45 H 0.3213 0.2286 0.3492 0.080 Uiso 1 1 calc R U . . .
C9 C 0.5006(3) 0.39637(18) -0.1222(4) 0.0658(6) Uani 1 1 d . . . . .
H9 H 0.5189 0.3749 -0.1572 0.079 Uiso 1 1 calc R U . . .
C53 C 0.3842(4) 0.2802(2) 0.8265(4) 0.0670(5) Uani 1 1 d . U . . .
H53 H 0.4287 0.2872 0.8770 0.080 Uiso 1 1 calc R U . . .
C10 C 0.5909(3) 0.60888(18) 0.0954(4) 0.0658(6) Uani 1 1 d . . . . .
H10 H 0.6332 0.6341 0.1129 0.079 Uiso 1 1 calc R U . . .
C38A C 0.5744(6) 0.2564(4) 0.6165(10) 0.047(5) Uani 0.65 1 d D U P A 1
H38A H 0.5778 0.2246 0.6190 0.056 Uiso 0.65 1 calc R U P A 1
C41A C 0.6275(4) 0.3233(2) 0.6501(4) 0.0462(15) Uani 0.65 1 d D . P A 1
H41A H 0.6738 0.3469 0.6702 0.055 Uiso 0.65 1 calc R U P A 1
C40A C 0.5268(4) 0.3234(2) 0.6469(5) 0.0478(16) Uani 0.65 1 d D . P A 1
H40A H 0.4889 0.3467 0.6637 0.057 Uiso 0.65 1 calc R U P A 1
C41B C 0.5976(8) 0.3178(6) 0.5536(10) 0.075(6) Uani 0.35 1 d D U P A 2
H41B H 0.6302 0.3376 0.5243 0.089 Uiso 0.35 1 calc R U P A 2
C40B C 0.4966(8) 0.3157(5) 0.5479(10) 0.069(5) Uani 0.35 1 d D U P A 2
H40B H 0.4438 0.3323 0.5134 0.083 Uiso 0.35 1 calc R U P A 2
C38B C 0.5714(8) 0.2571(5) 0.6078(13) 0.023(6) Uani 0.35 1 d D U P A 2
H38B H 0.5715 0.2257 0.5986 0.028 Uiso 0.35 1 calc R U P A 2


_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 O72 2.100(3) 4_665 ?
Ni1 O72 2.100(3) 2_655 ?
Ni1 N13 2.089(3) . ?
Ni1 N13 2.089(3) 3_765 ?
Ni1 N1 2.090(3) . ?
Ni1 N1 2.090(3) 3_765 ?
Ni2 O75 2.024(2) 4_666 ?
Ni2 O77 2.102(3) . ?
Ni2 O61 2.029(3) . ?
Ni2 N58 2.096(3) 1_655 ?
Ni2 N34 2.099(3) . ?
Ni2 N37 2.077(3) . ?
S70 O72 1.456(3) . ?
S70 O71 1.454(3) . ?
S70 O73 1.449(3) . ?
S70 C66 1.766(4) . ?
O75 Ni2 2.024(2) 4_565 ?
O75 C74 1.273(4) . ?
O72 Ni1 2.100(3) 2_645 ?
O77 H77A 0.8744 . ?
O77 H77B 0.8723 . ?
O61 C63 1.277(5) . ?
O76 C74 1.246(5) . ?
O62 C63 1.237(5) . ?
N13 C14 1.313(4) . ?
N13 C17 1.375(5) . ?
N58 Ni2 2.096(3) 1_455 ?
N58 C57 1.309(5) . ?
N58 C59 1.371(5) . ?
N15 C18 1.434(4) . ?
N15 C14 1.352(4) . ?
N15 C16 1.369(5) . ?
N32 C25 1.449(4) . ?
N32 C33 1.349(5) . ?
N32 C36 1.359(5) . ?
N34 C33 1.302(4) . ?
N34 C35 1.350(5) . ?
N1 C2 1.311(4) . ?
N1 C5 1.370(5) . ?
N56 C57 1.348(4) . ?
N56 C49 1.426(4) . ?
N56 C60 1.377(6) . ?
N3 C2 1.357(4) . ?
N3 C6 1.439(4) . ?
N3 C4 1.371(5) . ?
C65 H65 0.9500 . ?
C65 C66 1.385(4) . ?
C65 C64 1.379(5) . ?
C66 C67 1.393(5) . ?
C68 C74 1.503(5) . ?
C68 C67 1.396(5) . ?
C68 C69 1.388(4) . ?
C18 C31 1.393(5) . ?
C18 C19 1.400(5) . ?
C14 H14 0.9500 . ?
C67 H67 0.9500 . ?
C31 C26 1.437(5) . ?
C31 C30 1.431(5) . ?
C57 H57 0.9500 . ?
C25 C26 1.393(5) . ?
C25 C24 1.385(5) . ?
C26 C27 1.439(5) . ?
C2 H2 0.9500 . ?
C17 H17 0.9500 . ?
C17 C16 1.362(5) . ?
C69 H69 0.9500 . ?
C69 C64 1.394(5) . ?
C19 C24 1.450(5) . ?
C19 C20 1.428(5) . ?
C24 C23 1.432(5) . ?
C33 H33 0.9500 . ?
C27 H27 0.9500 . ?
C27 C28 1.354(5) . ?
C63 C64 1.511(4) . ?
N37 C38A 1.287(9) . ?
N37 C41A 1.436(7) . ?
N37 C41B 1.592(10) . ?
N37 C38B 1.290(12) . ?
C6 C12 1.379(7) . ?
C6 C7 1.399(6) . ?
C49 C48 1.400(7) . ?
C49 C50 1.388(8) . ?
C20 H20 0.9500 . ?
C20 C21 1.358(6) . ?
C16 H16 0.9500 . ?
C48 C43 1.446(7) . ?
C48 C47 1.408(9) . ?
C12 C7 1.449(6) 3_665 ?
C12 C11 1.423(7) . ?
C7 C12 1.449(6) 3_665 ?
C7 C8 1.410(8) . ?
C5 H5 0.9500 . ?
C5 C4 1.355(5) . ?
C43 C42 1.370(9) . ?
C43 C44 1.426(8) . ?
C59 H59 0.9500 . ?
C59 C60 1.353(5) . ?
C50 C55 1.437(7) . ?
C50 C51 1.448(8) . ?
C29 H29 0.9500 . ?
C29 C28 1.407(6) . ?
C29 C30 1.359(6) . ?
C47 H47 0.9500 . ?
C47 C46 1.370(8) . ?
C42 C55 1.412(8) . ?
C42 N39 1.450(5) . ?
C23 H23 0.9500 . ?
C23 C22 1.356(6) . ?
C28 H28 0.9500 . ?
C4 H4 0.9500 . ?
C30 H30 0.9500 . ?
C21 H21 0.9500 . ?
C21 C22 1.415(7) . ?
C55 C54 1.486(9) . ?
N39 C38A 1.340(8) . ?
N39 C40A 1.484(8) . ?
N39 C40B 1.557(10) . ?
N39 C38B 1.324(13) . ?
C35 H35 0.9500 . ?
C35 C36 1.353(6) . ?
C36 H36 0.9500 . ?
C22 H22 0.9500 . ?
C60 H60 0.9500 . ?
C8 H8 0.9500 . ?
C8 C9 1.380(7) . ?
C51 H51 0.9500 . ?
C51 C52 1.364(9) . ?
C11 H11 0.9500 . ?
C11 C10 1.358(8) . ?
C54 H54 0.9500 . ?
C54 C53 1.341(8) . ?
C44 H44 0.9500 . ?
C44 C45 1.295(9) . ?
C46 H46 0.9500 . ?
C46 C45 1.434(7) . ?
C52 H52 0.9500 . ?
C52 C53 1.391(7) . ?
C45 H45 0.9500 . ?
C9 H9 0.9500 . ?
C9 C10 1.438(6) 3_665 ?
C53 H53 0.9500 . ?
C10 C9 1.438(7) 3_665 ?
C10 H10 0.9500 . ?
C38A H38A 0.9500 . ?
C41A H41A 0.9500 . ?
C41A C40A 1.360(7) . ?
C40A H40A 0.9500 . ?
C41B H41B 0.9500 . ?
C41B C40B 1.356(12) . ?
C40B H40B 0.9500 . ?
C38B H38B 0.9500 . ?

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
O72 Ni1 O72 180.00(14) 4_665 2_655 ?
N13 Ni1 O72 90.78(11) . 4_665 ?
N13 Ni1 O72 89.22(11) . 2_655 ?
N13 Ni1 O72 90.79(11) 3_765 2_655 ?
N13 Ni1 O72 89.21(11) 3_765 4_665 ?
N13 Ni1 N13 180.0 . 3_765 ?
N13 Ni1 N1 86.92(10) . . ?
N13 Ni1 N1 93.08(10) 3_765 . ?
N13 Ni1 N1 86.92(10) 3_765 3_765 ?
N13 Ni1 N1 93.08(10) . 3_765 ?
N1 Ni1 O72 94.86(11) . 2_655 ?
N1 Ni1 O72 94.86(11) 3_765 4_665 ?
N1 Ni1 O72 85.14(11) . 4_665 ?
N1 Ni1 O72 85.14(11) 3_765 2_655 ?
N1 Ni1 N1 180.0 . 3_765 ?
O75 Ni2 O77 88.96(10) 4_666 . ?
O75 Ni2 O61 178.54(12) 4_666 . ?
O75 Ni2 N58 89.91(14) 4_666 1_655 ?
O75 Ni2 N34 86.33(11) 4_666 . ?
O75 Ni2 N37 93.12(14) 4_666 . ?
O61 Ni2 O77 90.76(11) . . ?
O61 Ni2 N58 88.65(15) . 1_655 ?
O61 Ni2 N34 93.97(11) . . ?
O61 Ni2 N37 88.30(15) . . ?
N58 Ni2 O77 89.38(13) 1_655 . ?
N58 Ni2 N34 91.62(13) 1_655 . ?
N34 Ni2 O77 175.18(11) . . ?
N37 Ni2 O77 87.51(13) . . ?
N37 Ni2 N58 175.62(15) . 1_655 ?
N37 Ni2 N34 91.73(13) . . ?
O72 S70 C66 104.68(15) . . ?
O71 S70 O72 111.48(17) . . ?
O71 S70 C66 106.59(17) . . ?
O73 S70 O72 112.67(19) . . ?
O73 S70 O71 113.62(19) . . ?
O73 S70 C66 107.09(17) . . ?
C74 O75 Ni2 124.6(2) . 4_565 ?
S70 O72 Ni1 155.60(16) . 2_645 ?
Ni2 O77 H77A 109.4 . . ?
Ni2 O77 H77B 109.5 . . ?
H77A O77 H77B 104.2 . . ?
C63 O61 Ni2 129.5(2) . . ?
C14 N13 Ni1 125.2(2) . . ?
C14 N13 C17 106.1(3) . . ?
C17 N13 Ni1 126.7(2) . . ?
C57 N58 Ni2 126.1(3) . 1_455 ?
C57 N58 C59 105.9(3) . . ?
C59 N58 Ni2 126.8(3) . 1_455 ?
C14 N15 C18 123.7(3) . . ?
C14 N15 C16 107.0(3) . . ?
C16 N15 C18 129.0(3) . . ?
C33 N32 C25 126.5(3) . . ?
C33 N32 C36 105.8(3) . . ?
C36 N32 C25 127.6(3) . . ?
C33 N34 Ni2 125.6(3) . . ?
C33 N34 C35 105.8(3) . . ?
C35 N34 Ni2 128.6(3) . . ?
C2 N1 Ni1 125.4(2) . . ?
C2 N1 C5 105.9(3) . . ?
C5 N1 Ni1 127.7(2) . . ?
C57 N56 C49 126.5(3) . . ?
C57 N56 C60 107.0(3) . . ?
C60 N56 C49 126.3(3) . . ?
C2 N3 C6 125.6(3) . . ?
C2 N3 C4 106.9(3) . . ?
C4 N3 C6 127.5(3) . . ?
C66 C65 H65 120.3 . . ?
C64 C65 H65 120.3 . . ?
C64 C65 C66 119.4(3) . . ?
C65 C66 S70 119.2(3) . . ?
C65 C66 C67 121.3(3) . . ?
C67 C66 S70 119.5(2) . . ?
C67 C68 C74 120.9(3) . . ?
C69 C68 C74 119.8(3) . . ?
C69 C68 C67 119.2(3) . . ?
O75 C74 C68 115.0(3) . . ?
O76 C74 O75 126.9(3) . . ?
O76 C74 C68 118.2(3) . . ?
C31 C18 N15 118.7(3) . . ?
C31 C18 C19 123.0(3) . . ?
C19 C18 N15 118.1(3) . . ?
N13 C14 N15 111.3(3) . . ?
N13 C14 H14 124.3 . . ?
N15 C14 H14 124.3 . . ?
C66 C67 C68 119.3(3) . . ?
C66 C67 H67 120.4 . . ?
C68 C67 H67 120.4 . . ?
C18 C31 C26 118.3(3) . . ?
C18 C31 C30 123.2(3) . . ?
C30 C31 C26 118.4(3) . . ?
N58 C57 N56 111.4(3) . . ?
N58 C57 H57 124.3 . . ?
N56 C57 H57 124.3 . . ?
C26 C25 N32 117.9(3) . . ?
C24 C25 N32 118.5(3) . . ?
C24 C25 C26 123.6(3) . . ?
C31 C26 C27 118.3(3) . . ?
C25 C26 C31 118.6(3) . . ?
C25 C26 C27 123.0(3) . . ?
N1 C2 N3 111.3(3) . . ?
N1 C2 H2 124.4 . . ?
N3 C2 H2 124.4 . . ?
N13 C17 H17 125.4 . . ?
C16 C17 N13 109.2(3) . . ?
C16 C17 H17 125.4 . . ?
C68 C69 H69 119.6 . . ?
C68 C69 C64 120.8(3) . . ?
C64 C69 H69 119.6 . . ?
C18 C19 C24 118.3(3) . . ?
C18 C19 C20 123.2(3) . . ?
C20 C19 C24 118.5(3) . . ?
C25 C24 C19 118.0(3) . . ?
C25 C24 C23 123.7(3) . . ?
C23 C24 C19 118.2(3) . . ?
N32 C33 H33 124.0 . . ?
N34 C33 N32 112.0(3) . . ?
N34 C33 H33 124.0 . . ?
C26 C27 H27 119.8 . . ?
C28 C27 C26 120.4(4) . . ?
C28 C27 H27 119.8 . . ?
O61 C63 C64 114.3(3) . . ?
O62 C63 O61 126.9(3) . . ?
O62 C63 C64 118.8(3) . . ?
C38A N37 Ni2 125.3(5) . . ?
C38A N37 C41A 104.0(5) . . ?
C41A N37 Ni2 128.5(3) . . ?
C41B N37 Ni2 116.3(5) . . ?
C38B N37 Ni2 125.2(7) . . ?
C38B N37 C41B 93.0(10) . . ?
C65 C64 C69 120.0(3) . . ?
C65 C64 C63 120.9(3) . . ?
C69 C64 C63 119.1(3) . . ?
C12 C6 N3 118.6(4) . . ?
C12 C6 C7 123.1(4) . . ?
C7 C6 N3 118.3(4) . . ?
C48 C49 N56 118.4(4) . . ?
C50 C49 N56 118.4(4) . . ?
C50 C49 C48 123.2(4) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 C19 120.7(4) . . ?
C21 C20 H20 119.7 . . ?
N15 C16 H16 126.8 . . ?
C17 C16 N15 106.4(3) . . ?
C17 C16 H16 126.8 . . ?
C49 C48 C43 118.5(6) . . ?
C49 C48 C47 122.9(5) . . ?
C47 C48 C43 118.6(5) . . ?
C6 C12 C7 119.4(4) . 3_665 ?
C6 C12 C11 122.0(4) . . ?
C11 C12 C7 118.6(5) . 3_665 ?
C6 C7 C12 117.5(5) . 3_665 ?
C6 C7 C8 123.7(4) . . ?
C8 C7 C12 118.8(5) . 3_665 ?
N1 C5 H5 125.1 . . ?
C4 C5 N1 109.9(4) . . ?
C4 C5 H5 125.1 . . ?
C42 C43 C48 117.7(5) . . ?
C42 C43 C44 124.0(5) . . ?
C44 C43 C48 118.3(6) . . ?
N58 C59 H59 125.1 . . ?
C60 C59 N58 109.8(4) . . ?
C60 C59 H59 125.1 . . ?
C49 C50 C55 118.5(5) . . ?
C49 C50 C51 123.5(5) . . ?
C55 C50 C51 118.0(6) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C30 C29 C28 120.4(4) . . ?
C48 C47 H47 119.8 . . ?
C46 C47 C48 120.4(5) . . ?
C46 C47 H47 119.8 . . ?
C43 C42 C55 124.3(4) . . ?
C43 C42 N39 121.1(5) . . ?
C55 C42 N39 114.6(5) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 C24 120.6(4) . . ?
C22 C23 H23 119.7 . . ?
C27 C28 C29 121.4(4) . . ?
C27 C28 H28 119.3 . . ?
C29 C28 H28 119.3 . . ?
N3 C4 H4 127.0 . . ?
C5 C4 N3 106.1(3) . . ?
C5 C4 H4 127.0 . . ?
C31 C30 H30 119.5 . . ?
C29 C30 C31 120.9(4) . . ?
C29 C30 H30 119.5 . . ?
C20 C21 H21 119.6 . . ?
C20 C21 C22 120.7(4) . . ?
C22 C21 H21 119.6 . . ?
C50 C55 C54 115.4(5) . . ?
C42 C55 C50 117.5(6) . . ?
C42 C55 C54 127.1(5) . . ?
C42 N39 C40A 124.5(4) . . ?
C42 N39 C40B 116.0(5) . . ?
C38A N39 C42 128.6(5) . . ?
C38A N39 C40A 102.2(6) . . ?
C38B N39 C42 128.9(7) . . ?
C38B N39 C40B 96.2(10) . . ?
N34 C35 H35 125.2 . . ?
N34 C35 C36 109.6(4) . . ?
C36 C35 H35 125.2 . . ?
N32 C36 H36 126.6 . . ?
C35 C36 N32 106.7(4) . . ?
C35 C36 H36 126.6 . . ?
C23 C22 C21 121.1(4) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
N56 C60 H60 127.1 . . ?
C59 C60 N56 105.9(4) . . ?
C59 C60 H60 127.1 . . ?
C7 C8 H8 119.2 . . ?
C9 C8 C7 121.5(5) . . ?
C9 C8 H8 119.2 . . ?
C50 C51 H51 118.6 . . ?
C52 C51 C50 122.8(5) . . ?
C52 C51 H51 118.6 . . ?
C12 C11 H11 119.7 . . ?
C10 C11 C12 120.7(5) . . ?
C10 C11 H11 119.7 . . ?
C55 C54 H54 118.7 . . ?
C53 C54 C55 122.7(5) . . ?
C53 C54 H54 118.7 . . ?
C43 C44 H44 119.5 . . ?
C45 C44 C43 121.0(5) . . ?
C45 C44 H44 119.5 . . ?
C47 C46 H46 120.4 . . ?
C47 C46 C45 119.3(6) . . ?
C45 C46 H46 120.4 . . ?
C51 C52 H52 120.3 . . ?
C51 C52 C53 119.4(6) . . ?
C53 C52 H52 120.3 . . ?
C44 C45 C46 122.3(6) . . ?
C44 C45 H45 118.9 . . ?
C46 C45 H45 118.9 . . ?
C8 C9 H9 120.6 . . ?
C8 C9 C10 118.9(5) . 3_665 ?
C10 C9 H9 120.6 3_665 . ?
C54 C53 C52 121.2(6) . . ?
C54 C53 H53 119.4 . . ?
C52 C53 H53 119.4 . . ?
C11 C10 C9 121.3(5) . 3_665 ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 3_665 . ?
N37 C38A N39 114.0(8) . . ?
N37 C38A H38A 123.0 . . ?
N39 C38A H38A 123.0 . . ?
N37 C41A H41A 125.9 . . ?
C40A C41A N37 108.2(5) . . ?
C40A C41A H41A 125.9 . . ?
N39 C40A H40A 127.3 . . ?
C41A C40A N39 105.3(5) . . ?
C41A C40A H40A 127.3 . . ?
N37 C41B H41B 125.9 . . ?
C40B C41B N37 108.1(8) . . ?
C40B C41B H41B 125.9 . . ?
N39 C40B H40B 128.5 . . ?
C41B C40B N39 103.0(8) . . ?
C41B C40B H40B 128.5 . . ?
N37 C38B N39 114.9(11) . . ?
N37 C38B H38B 122.6 . . ?
N39 C38B H38B 122.6 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O77 H77A O62 0.87 1.88 2.658(4) 147.8 .
O77 H77B O76 0.87 1.97 2.688(4) 139.3 4_666

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 N13 C14 N15 164.3(2) . . . . ?
Ni1 N13 C17 C16 -163.7(3) . . . . ?
Ni1 N1 C2 N3 -169.3(3) . . . . ?
Ni1 N1 C5 C4 169.0(4) . . . . ?
Ni2 O75 C74 O76 13.5(5) 4_565 . . . ?
Ni2 O75 C74 C68 -167.7(2) 4_565 . . . ?
Ni2 O61 C63 O62 -12.3(7) . . . . ?
Ni2 O61 C63 C64 168.1(3) . . . . ?
Ni2 N58 C57 N56 167.6(3) 1_455 . . . ?
Ni2 N58 C59 C60 -168.2(4) 1_455 . . . ?
Ni2 N34 C33 N32 -176.9(2) . . . . ?
Ni2 N34 C35 C36 177.9(3) . . . . ?
Ni2 N37 C38A N39 -169.6(7) . . . . ?
Ni2 N37 C41A C40A -178.7(5) . . . . ?
Ni2 N37 C41B C40B 156.0(13) . . . . ?
Ni2 N37 C38B N39 -174.8(9) . . . . ?
S70 C66 C67 C68 179.6(2) . . . . ?
O72 S70 C66 C65 59.7(3) . . . . ?
O72 S70 C66 C67 -118.0(3) . . . . ?
O61 C63 C64 C65 164.3(4) . . . . ?
O61 C63 C64 C69 -16.6(5) . . . . ?
O62 C63 C64 C65 -15.3(6) . . . . ?
O62 C63 C64 C69 163.8(4) . . . . ?
N13 C17 C16 N15 -0.5(5) . . . . ?
N58 C59 C60 N56 0.8(7) . . . . ?
O71 S70 O72 Ni1 158.2(4) . . . 2_645 ?
O71 S70 C66 C65 177.9(3) . . . . ?
O71 S70 C66 C67 0.3(3) . . . . ?
N15 C18 C31 C26 173.2(3) . . . . ?
N15 C18 C31 C30 -4.3(6) . . . . ?
N15 C18 C19 C24 -176.7(3) . . . . ?
N15 C18 C19 C20 1.5(5) . . . . ?
N32 C25 C26 C31 -178.7(3) . . . . ?
N32 C25 C26 C27 -1.0(6) . . . . ?
N32 C25 C24 C19 175.2(3) . . . . ?
N32 C25 C24 C23 -3.7(6) . . . . ?
O73 S70 O72 Ni1 29.1(4) . . . 2_645 ?
O73 S70 C66 C65 -60.2(3) . . . . ?
O73 S70 C66 C67 122.2(3) . . . . ?
N34 C35 C36 N32 -0.5(6) . . . . ?
N1 C5 C4 N3 0.0(6) . . . . ?
N56 C49 C48 C43 174.4(4) . . . . ?
N56 C49 C48 C47 -4.1(7) . . . . ?
N56 C49 C50 C55 -179.4(4) . . . . ?
N56 C49 C50 C51 0.2(7) . . . . ?
N3 C6 C12 C7 -179.4(5) . . . 3_665 ?
N3 C6 C12 C11 0.4(8) . . . . ?
N3 C6 C7 C12 179.4(4) . . . 3_665 ?
N3 C6 C7 C8 -0.6(8) . . . . ?
C65 C66 C67 C68 2.0(5) . . . . ?
C66 S70 O72 Ni1 -86.9(4) . . . 2_645 ?
C66 C65 C64 C69 1.6(5) . . . . ?
C66 C65 C64 C63 -179.3(3) . . . . ?
C68 C69 C64 C65 1.1(5) . . . . ?
C68 C69 C64 C63 -178.0(3) . . . . ?
C74 C68 C67 C66 -178.1(3) . . . . ?
C74 C68 C69 C64 176.6(3) . . . . ?
C18 N15 C14 N13 -173.8(3) . . . . ?
C18 N15 C16 C17 173.6(4) . . . . ?
C18 C31 C26 C25 3.4(5) . . . . ?
C18 C31 C26 C27 -174.4(3) . . . . ?
C18 C31 C30 C29 175.0(4) . . . . ?
C18 C19 C24 C25 3.4(5) . . . . ?
C18 C19 C24 C23 -177.6(4) . . . . ?
C18 C19 C20 C21 179.8(4) . . . . ?
C14 N13 C17 C16 0.5(4) . . . . ?
C14 N15 C18 C31 -79.1(5) . . . . ?
C14 N15 C18 C19 96.2(4) . . . . ?
C14 N15 C16 C17 0.4(4) . . . . ?
C67 C68 C74 O75 4.8(5) . . . . ?
C67 C68 C74 O76 -176.3(3) . . . . ?
C67 C68 C69 C64 -2.2(5) . . . . ?
C31 C18 C19 C24 -1.6(5) . . . . ?
C31 C18 C19 C20 176.6(3) . . . . ?
C31 C26 C27 C28 -1.4(6) . . . . ?
C57 N58 C59 C60 -0.2(6) . . . . ?
C57 N56 C49 C48 -101.1(6) . . . . ?
C57 N56 C49 C50 78.1(6) . . . . ?
C57 N56 C60 C59 -1.0(6) . . . . ?
C25 N32 C33 N34 175.0(3) . . . . ?
C25 N32 C36 C35 -175.5(4) . . . . ?
C25 C26 C27 C28 -179.1(4) . . . . ?
C25 C24 C23 C22 176.4(5) . . . . ?
C26 C31 C30 C29 -2.5(6) . . . . ?
C26 C25 C24 C19 -1.8(6) . . . . ?
C26 C25 C24 C23 179.2(4) . . . . ?
C26 C27 C28 C29 -1.3(7) . . . . ?
C2 N1 C5 C4 0.1(6) . . . . ?
C2 N3 C6 C12 75.4(6) . . . . ?
C2 N3 C6 C7 -104.6(5) . . . . ?
C2 N3 C4 C5 0.0(6) . . . . ?
C17 N13 C14 N15 -0.2(4) . . . . ?
C69 C68 C74 O75 -174.0(3) . . . . ?
C69 C68 C74 O76 4.9(5) . . . . ?
C69 C68 C67 C66 0.7(5) . . . . ?
C19 C18 C31 C26 -1.8(5) . . . . ?
C19 C18 C31 C30 -179.4(4) . . . . ?
C19 C24 C23 C22 -2.6(7) . . . . ?
C19 C20 C21 C22 -1.8(7) . . . . ?
C24 C25 C26 C31 -1.6(6) . . . . ?
C24 C25 C26 C27 176.1(4) . . . . ?
C24 C19 C20 C21 -2.0(6) . . . . ?
C24 C23 C22 C21 -1.2(9) . . . . ?
C33 N32 C25 C26 -73.6(5) . . . . ?
C33 N32 C25 C24 109.2(4) . . . . ?
C33 N32 C36 C35 1.6(5) . . . . ?
C33 N34 C35 C36 -0.7(6) . . . . ?
N37 C41A C40A N39 0.4(7) . . . . ?
N37 C41B C40B N39 2.5(18) . . . . ?
C64 C65 C66 S70 179.3(3) . . . . ?
C64 C65 C66 C67 -3.1(5) . . . . ?
C6 N3 C2 N1 179.0(4) . . . . ?
C6 N3 C4 C5 -178.9(4) . . . . ?
C6 C12 C11 C10 -175.6(5) . . . . ?
C6 C7 C8 C9 -176.3(6) . . . . ?
C49 N56 C57 N58 176.2(5) . . . . ?
C49 N56 C60 C59 -176.3(5) . . . . ?
C49 C48 C43 C42 5.4(7) . . . . ?
C49 C48 C43 C44 -174.9(5) . . . . ?
C49 C48 C47 C46 177.5(5) . . . . ?
C49 C50 C55 C42 4.4(7) . . . . ?
C49 C50 C55 C54 -174.8(5) . . . . ?
C49 C50 C51 C52 178.6(5) . . . . ?
C20 C19 C24 C25 -174.9(3) . . . . ?
C20 C19 C24 C23 4.1(5) . . . . ?
C20 C21 C22 C23 3.4(9) . . . . ?
C16 N15 C18 C31 108.7(5) . . . . ?
C16 N15 C18 C19 -76.0(5) . . . . ?
C16 N15 C14 N13 -0.1(4) . . . . ?
C48 C49 C50 C55 -0.2(7) . . . . ?
C48 C49 C50 C51 179.4(5) . . . . ?
C48 C43 C42 C55 -1.2(8) . . . . ?
C48 C43 C42 N39 -178.9(4) . . . . ?
C48 C43 C44 C45 -2.4(8) . . . . ?
C48 C47 C46 C45 -2.8(8) . . . . ?
C12 C6 C7 C12 -0.6(9) . . . 3_665 ?
C12 C6 C7 C8 179.4(6) . . . . ?
C12 C7 C8 C9 3.8(9) 3_665 . . . ?
C12 C11 C10 C9 -3.9(9) . . . 3_665 ?
C7 C6 C12 C7 0.7(9) . . . 3_665 ?
C7 C6 C12 C11 -179.6(5) . . . . ?
C7 C12 C11 C10 4.1(9) 3_665 . . . ?
C7 C8 C9 C10 -4.1(9) . . . 3_665 ?
C5 N1 C2 N3 -0.1(5) . . . . ?
C43 C48 C47 C46 -1.0(8) . . . . ?
C43 C42 C55 C50 -3.8(8) . . . . ?
C43 C42 C55 C54 175.3(5) . . . . ?
C43 C42 N39 C38A -80.2(11) . . . . ?
C43 C42 N39 C40A 128.7(6) . . . . ?
C43 C42 N39 C40B 51.0(10) . . . . ?
C43 C42 N39 C38B -72.3(14) . . . . ?
C43 C44 C45 C46 -1.5(8) . . . . ?
C59 N58 C57 N56 -0.5(5) . . . . ?
C50 C49 C48 C43 -4.8(7) . . . . ?
C50 C49 C48 C47 176.8(5) . . . . ?
C50 C55 C54 C53 -3.2(8) . . . . ?
C50 C51 C52 C53 -5.1(8) . . . . ?
C47 C48 C43 C42 -176.1(5) . . . . ?
C47 C48 C43 C44 3.6(8) . . . . ?
C47 C46 C45 C44 4.2(8) . . . . ?
C42 C43 C44 C45 177.3(5) . . . . ?
C42 C55 C54 C53 177.7(5) . . . . ?
C42 N39 C38A N37 178.7(8) . . . . ?
C42 N39 C40A C41A 170.8(5) . . . . ?
C42 N39 C40B C41B -166.6(12) . . . . ?
C42 N39 C38B N37 -176.3(9) . . . . ?
C28 C29 C30 C31 -0.2(8) . . . . ?
C4 N3 C2 N1 0.1(5) . . . . ?
C4 N3 C6 C12 -105.8(6) . . . . ?
C4 N3 C6 C7 74.1(6) . . . . ?
C30 C31 C26 C25 -178.9(4) . . . . ?
C30 C31 C26 C27 3.3(5) . . . . ?
C30 C29 C28 C27 2.2(8) . . . . ?
C55 C50 C51 C52 -1.7(8) . . . . ?
C55 C42 N39 C38A 101.8(11) . . . . ?
C55 C42 N39 C40A -49.2(7) . . . . ?
C55 C42 N39 C40B -127.0(9) . . . . ?
C55 C42 N39 C38B 109.8(13) . . . . ?
C55 C54 C53 C52 -3.5(9) . . . . ?
N39 C42 C55 C50 174.1(4) . . . . ?
N39 C42 C55 C54 -6.8(7) . . . . ?
C35 N34 C33 N32 1.8(4) . . . . ?
C36 N32 C25 C26 102.9(5) . . . . ?
C36 N32 C25 C24 -74.3(5) . . . . ?
C36 N32 C33 N34 -2.1(4) . . . . ?
C60 N56 C57 N58 0.9(6) . . . . ?
C60 N56 C49 C48 73.3(7) . . . . ?
C60 N56 C49 C50 -107.5(6) . . . . ?
C51 C50 C55 C42 -175.2(5) . . . . ?
C51 C50 C55 C54 5.6(7) . . . . ?
C51 C52 C53 C54 7.7(8) . . . . ?
C44 C43 C42 C55 179.2(5) . . . . ?
C44 C43 C42 N39 1.4(7) . . . . ?
C38A N37 C41A C40A -14.9(10) . . . . ?
C38A N37 C41B C40B 19.9(17) . . . . ?
C38A N37 C38B N39 92(8) . . . . ?
C38A N39 C40A C41A 13.6(10) . . . . ?
C38A N39 C40B C41B -23.4(17) . . . . ?
C38A N39 C38B N37 -87(8) . . . . ?
C41A N37 C38A N39 25.9(14) . . . . ?
C41A N37 C41B C40B -81.8(15) . . . . ?
C41A N37 C38B N39 14.5(19) . . . . ?
C40A N39 C38A N37 -25.4(14) . . . . ?
C40A N39 C40B C41B 75.2(14) . . . . ?
C40A N39 C38B N37 -14.1(18) . . . . ?
C41B N37 C38A N39 -39.2(15) . . . . ?
C41B N37 C41A C40A 77.3(7) . . . . ?
C41B N37 C38B N39 -49.4(17) . . . . ?
C40B N39 C38A N37 42.3(15) . . . . ?
C40B N39 C40A C41A -83.1(7) . . . . ?
C40B N39 C38B N37 52.8(18) . . . . ?
C38B N37 C38A N39 -79(8) . . . . ?
C38B N37 C41A C40A -8.4(12) . . . . ?
C38B N37 C41B C40B 24.0(17) . . . . ?
C38B N39 C38A N37 83(9) . . . . ?
C38B N39 C40A C41A 7.5(12) . . . . ?
C38B N39 C40B C41B -27.5(16) . . . . ?

_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 -0.787 0.000 0.000 1082.2 306.0 '4 DMF,14 H2O'
2 -0.423 0.500 0.500 1082.2 306.0 '4 DMF,14 H2O'

_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 1.138
_oxdiff_exptl_absorpt_empirical_full_min 0.898
