# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_h4la3
_database_code_depnum_ccdc_archive 'CCDC 2168791'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2022-04-26 deposited with the CCDC.	2022-05-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H20 O7'
_chemical_formula_weight         432.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0132 0.0074
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   22.347(8)
_cell_length_b                   67.02(2)
_cell_length_c                   5.194(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7779(5)
_cell_formula_units_Z            16
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9974
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      30.59

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_F_000             3616
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.131
_shelx_estimated_absorpt_T_min   0.978
_shelx_estimated_absorpt_T_max   0.997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.666
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   SADABS-2014/5

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27960
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -86
_diffrn_reflns_limit_k_max       86
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         2.095
_diffrn_reflns_theta_max         30.196
_diffrn_reflns_theta_full        33.070
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.790
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.790
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.779
_reflns_number_total             4437
_reflns_number_gt                3839
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.791
_reflns_Friedel_fraction_max     0.988
_reflns_Friedel_fraction_full    0.766

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 All non-hydrogens were refined anisotropically.
 Hydrogens were found in a difference Fourier map, placed
 geometrically on their carrier atom and refined with a riding
 model, except those on the phenol-enol oxygens that were refined
 freely with their thermal parameter 1.5 times that of their carrier
 oxygen.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0464P)²+6.4485P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4437
_refine_ls_number_parameters     302
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0389
_refine_ls_wR_factor_ref         0.0938
_refine_ls_wR_factor_gt          0.0891
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.00037(7) 0.58677(3) 0.6365(4) 0.0229(4) Uani 1 1 d . . . . .
H1 H 0.0250(14) 0.5787(5) 0.555(7) 0.034 Uiso 1 1 d . U . . .
O2 O 0.09953(7) 0.57106(2) 0.4910(4) 0.0195(4) Uani 1 1 d . . . . .
O3 O 0.19569(7) 0.55691(3) 0.3163(4) 0.0223(4) Uani 1 1 d . . . . .
H3 H 0.1538(13) 0.5602(4) 0.332(6) 0.033 Uiso 1 1 d . U . . .
O4 O 0.30926(7) 0.58605(3) 0.8423(4) 0.0224(4) Uani 1 1 d . . . . .
O5 O 0.50598(7) 0.55760(3) 0.6828(3) 0.0209(4) Uani 1 1 d . . . . .
H5 H 0.5451(14) 0.5544(4) 0.659(6) 0.031 Uiso 1 1 d . U . . .
O6 O 0.59941(7) 0.54323(2) 0.4969(4) 0.0184(4) Uani 1 1 d . . . . .
O7 O 0.69619(7) 0.52549(3) 0.3572(4) 0.0204(4) Uani 1 1 d . . . . .
H7 H 0.6737(14) 0.5336(4) 0.444(7) 0.031 Uiso 1 1 d . U . . .
C1 C 0.03332(10) 0.59597(4) 0.8193(5) 0.0188(5) Uani 1 1 d . . . . .
C2 C 0.00264(11) 0.60824(4) 0.9911(5) 0.0232(6) Uani 1 1 d . . . . .
H2A H -0.0393 0.6100 0.9722 0.028 Uiso 1 1 calc R U . . .
C3 C 0.03220(12) 0.61782(4) 1.1872(6) 0.0257(6) Uani 1 1 d . . . . .
H3A H 0.0106 0.6260 1.3038 0.031 Uiso 1 1 calc R U . . .
C4 C 0.09412(12) 0.61546(4) 1.2154(5) 0.0236(6) Uani 1 1 d . . . . .
H4A H 0.1147 0.6220 1.3511 0.028 Uiso 1 1 calc R U . . .
C5 C 0.12499(11) 0.60357(4) 1.0458(5) 0.0196(5) Uani 1 1 d . . . . .
H5A H 0.1670 0.6021 1.0657 0.023 Uiso 1 1 calc R U . . .
C6 C 0.09610(10) 0.59348(3) 0.8432(5) 0.0172(5) Uani 1 1 d . . . . .
C7 C 0.12904(10) 0.58045(3) 0.6624(5) 0.0160(5) Uani 1 1 d . . . . .
C8 C 0.19279(10) 0.57839(4) 0.6753(5) 0.0172(5) Uani 1 1 d . . . . .
H8A H 0.2142 0.5854 0.8048 0.021 Uiso 1 1 calc R U . . .
C9 C 0.22377(10) 0.56658(3) 0.5061(5) 0.0154(5) Uani 1 1 d . . . . .
C10 C 0.28886(10) 0.56266(3) 0.5085(5) 0.0146(5) Uani 1 1 d . . . . .
C11 C 0.31158(10) 0.54864(4) 0.3320(5) 0.0174(5) Uani 1 1 d . . . . .
H11A H 0.2849 0.5423 0.2155 0.021 Uiso 1 1 calc R U . . .
C12 C 0.37195(10) 0.54381(4) 0.3236(5) 0.0176(5) Uani 1 1 d . . . . .
H12A H 0.3861 0.5343 0.2022 0.021 Uiso 1 1 calc R U . . .
C13 C 0.41164(10) 0.55290(3) 0.4934(5) 0.0150(5) Uani 1 1 d . . . . .
C14 C 0.39034(10) 0.56685(3) 0.6699(5) 0.0159(5) Uani 1 1 d . . . . .
H14A H 0.4174 0.5730 0.7870 0.019 Uiso 1 1 calc R U . . .
C15 C 0.33004(10) 0.57199(3) 0.6772(5) 0.0163(5) Uani 1 1 d . . . . .
C16 C 0.35095(11) 0.59522(4) 1.0162(5) 0.0225(6) Uani 1 1 d . . . . .
H16A H 0.3689 0.5850 1.1266 0.034 Uiso 1 1 calc R U . . .
H16B H 0.3300 0.6050 1.1231 0.034 Uiso 1 1 calc R U . . .
H16C H 0.3825 0.6019 0.9175 0.034 Uiso 1 1 calc R U . . .
C17 C 0.47674(10) 0.54856(3) 0.4936(5) 0.0157(5) Uani 1 1 d . . . . .
C18 C 0.50506(10) 0.53675(4) 0.3177(5) 0.0178(5) Uani 1 1 d . . . . .
H18A H 0.4824 0.5302 0.1881 0.021 Uiso 1 1 calc R U . . .
C19 C 0.56897(10) 0.53413(3) 0.3268(5) 0.0157(5) Uani 1 1 d . . . . .
C20 C 0.60001(10) 0.52071(3) 0.1473(5) 0.0154(5) Uani 1 1 d . . . . .
C21 C 0.56980(10) 0.51120(3) -0.0562(5) 0.0176(5) Uani 1 1 d . . . . .
H21A H 0.5289 0.5143 -0.0855 0.021 Uiso 1 1 calc R U . . .
C22 C 0.59742(10) 0.49751(4) -0.2145(5) 0.0197(5) Uani 1 1 d . . . . .
H22A H 0.5758 0.4912 -0.3494 0.024 Uiso 1 1 calc R U . . .
C23 C 0.65769(11) 0.49311(4) -0.1730(5) 0.0192(5) Uani 1 1 d . . . . .
H23A H 0.6771 0.4835 -0.2781 0.023 Uiso 1 1 calc R U . . .
C24 C 0.68944(10) 0.50260(4) 0.0190(5) 0.0189(5) Uani 1 1 d . . . . .
H24A H 0.7306 0.4996 0.0433 0.023 Uiso 1 1 calc R U . . .
C25 C 0.66178(10) 0.51658(3) 0.1776(5) 0.0165(5) Uani 1 1 d . . . . .


_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
O1 C1 1.351(3) . ?
O1 H1 0.88(3) . ?
O2 C7 1.274(3) . ?
O3 C9 1.337(3) . ?
O3 H3 0.97(3) . ?
O4 C15 1.356(3) . ?
O4 C16 1.436(3) . ?
O5 C17 1.327(3) . ?
O5 H5 0.91(3) . ?
O6 C19 1.271(3) . ?
O7 C25 1.349(3) . ?
O7 H7 0.86(3) . ?
C1 C2 1.394(4) . ?
C1 C6 1.418(3) . ?
C2 C3 1.373(4) . ?
C2 H2A 0.9500 . ?
C3 C4 1.400(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.374(4) . ?
C4 H4A 0.9500 . ?
C5 C6 1.407(4) . ?
C5 H5A 0.9500 . ?
C6 C7 1.479(3) . ?
C7 C8 1.433(3) . ?
C8 C9 1.370(4) . ?
C8 H8A 0.9500 . ?
C9 C10 1.478(3) . ?
C10 C11 1.407(3) . ?
C10 C15 1.416(3) . ?
C11 C12 1.388(3) . ?
C11 H11A 0.9500 . ?
C12 C13 1.392(3) . ?
C12 H12A 0.9500 . ?
C13 C14 1.393(3) . ?
C13 C17 1.484(3) . ?
C14 C15 1.391(3) . ?
C14 H14A 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.364(3) . ?
C18 C19 1.440(3) . ?
C18 H18A 0.9500 . ?
C19 C20 1.470(3) . ?
C20 C21 1.407(4) . ?
C20 C25 1.417(3) . ?
C21 C22 1.378(3) . ?
C21 H21A 0.9500 . ?
C22 C23 1.396(3) . ?
C22 H22A 0.9500 . ?
C23 C24 1.379(4) . ?
C23 H23A 0.9500 . ?
C24 C25 1.392(3) . ?
C24 H24A 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
C1 O1 H1 106(2) . . ?
C9 O3 H3 106.5(19) . . ?
C15 O4 C16 118.24(18) . . ?
C17 O5 H5 105(2) . . ?
C25 O7 H7 108(2) . . ?
O1 C1 C2 116.8(2) . . ?
O1 C1 C6 123.2(2) . . ?
C2 C1 C6 120.0(2) . . ?
C3 C2 C1 120.9(2) . . ?
C3 C2 H2A 119.5 . . ?
C1 C2 H2A 119.5 . . ?
C2 C3 C4 120.0(2) . . ?
C2 C3 H3A 120.0 . . ?
C4 C3 H3A 120.0 . . ?
C5 C4 C3 119.6(2) . . ?
C5 C4 H4A 120.2 . . ?
C3 C4 H4A 120.2 . . ?
C4 C5 C6 121.9(2) . . ?
C4 C5 H5A 119.1 . . ?
C6 C5 H5A 119.1 . . ?
C5 C6 C1 117.6(2) . . ?
C5 C6 C7 122.0(2) . . ?
C1 C6 C7 120.4(2) . . ?
O2 C7 C8 120.0(2) . . ?
O2 C7 C6 118.5(2) . . ?
C8 C7 C6 121.5(2) . . ?
C9 C8 C7 121.9(2) . . ?
C9 C8 H8A 119.1 . . ?
C7 C8 H8A 119.1 . . ?
O3 C9 C8 121.1(2) . . ?
O3 C9 C10 112.5(2) . . ?
C8 C9 C10 126.5(2) . . ?
C11 C10 C15 117.6(2) . . ?
C11 C10 C9 117.9(2) . . ?
C15 C10 C9 124.5(2) . . ?
C12 C11 C10 121.8(2) . . ?
C12 C11 H11A 119.1 . . ?
C10 C11 H11A 119.1 . . ?
C11 C12 C13 119.8(2) . . ?
C11 C12 H12A 120.1 . . ?
C13 C12 H12A 120.1 . . ?
C12 C13 C14 119.5(2) . . ?
C12 C13 C17 122.7(2) . . ?
C14 C13 C17 117.8(2) . . ?
C15 C14 C13 121.0(2) . . ?
C15 C14 H14A 119.5 . . ?
C13 C14 H14A 119.5 . . ?
O4 C15 C14 121.4(2) . . ?
O4 C15 C10 118.4(2) . . ?
C14 C15 C10 120.2(2) . . ?
O4 C16 H16A 109.5 . . ?
O4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O5 C17 C18 122.2(2) . . ?
O5 C17 C13 113.2(2) . . ?
C18 C17 C13 124.6(2) . . ?
C17 C18 C19 120.6(2) . . ?
C17 C18 H18A 119.7 . . ?
C19 C18 H18A 119.7 . . ?
O6 C19 C18 119.7(2) . . ?
O6 C19 C20 118.8(2) . . ?
C18 C19 C20 121.5(2) . . ?
C21 C20 C25 117.5(2) . . ?
C21 C20 C19 121.8(2) . . ?
C25 C20 C19 120.6(2) . . ?
C22 C21 C20 122.3(2) . . ?
C22 C21 H21A 118.8 . . ?
C20 C21 H21A 118.8 . . ?
C21 C22 C23 118.8(2) . . ?
C21 C22 H22A 120.6 . . ?
C23 C22 H22A 120.6 . . ?
C24 C23 C22 120.7(2) . . ?
C24 C23 H23A 119.7 . . ?
C22 C23 H23A 119.7 . . ?
C23 C24 C25 120.7(2) . . ?
C23 C24 H24A 119.7 . . ?
C25 C24 H24A 119.7 . . ?
O7 C25 C24 117.0(2) . . ?
O7 C25 C20 123.1(2) . . ?
C24 C25 C20 119.9(2) . . ?

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
O1 H1 O2 0.88(3) 1.77(3) 2.567(2) 149(3) .
O3 H3 O2 0.97(3) 1.64(3) 2.518(2) 149(3) .
O5 H5 O6 0.91(3) 1.66(3) 2.494(2) 152(3) .
O7 H7 O6 0.86(3) 1.80(3) 2.572(2) 147(3) .
O7 H7 O3 0.86(3) 2.54(3) 3.181(3) 132(3) 9
O5 H5 O2 0.91(3) 2.39(3) 2.783(2) 106(2) 9
O1 H1 O5 0.88(3) 2.43(3) 3.065(3) 129(3) 9_454
O3 H3 O6 0.97(3) 2.41(3) 2.867(2) 109(2) 9_454

_refine_diff_density_max         0.244
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.048

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_ibcc978
_database_code_depnum_ccdc_archive 'CCDC 2168792'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2022-04-26 deposited with the CCDC.	2022-05-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C120 H93 Cu3 N9 Ni3 O21, 7(C5 H5 N)'
_chemical_formula_sum            'C155 H128 Cu3 N16 Ni3 O21'
_chemical_formula_weight         2917.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0076 0.0040
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0132 0.0074
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Ni Ni 0.3262 1.3024
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Cu Cu 0.2913 1.4803
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   17.429(5)
_cell_length_b                   22.792(7)
_cell_length_c                   23.211(6)
_cell_angle_alpha                119.151(4)
_cell_angle_beta                 92.989(4)
_cell_angle_gamma                108.934(4)
_cell_volume                     7366(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9692
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27.81

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_F_000             2682
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.220
_shelx_estimated_absorpt_T_min   0.918
_shelx_estimated_absorpt_T_max   0.958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.624
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   SADABS-2014/5

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            95429
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.059
_diffrn_reflns_theta_max         27.939
_diffrn_reflns_theta_full        27.825
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             27132
_reflns_number_gt                17689
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 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.
;

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;All non-hydrogens were refined anistropically. One of pyridine
 molecules coordinated to Ni3 is disordered over two positions
 (N8/N18) with relative occupancies 0.44:0.56. Rigid body and
 displacement parameters restraints were used to refine these. 
 The three methoxy groups O4-C16, O11-C41 and O18-C66 show some 
 strong disorder and were refined with displacement parameters 
 restraints as well as with a distance restraint (O-C). For one 
 of these there remains a residual density peak in the vicinity 
 (3 e close to C14-H14A), and it was attempted to refine the
 corresponding methoxy group (O4-C16) over two positions attached
 to C15 and C14. This refinement however did not converge and
 the model was therefore left as is. The three lattice pyridine
 molecules were refined with rigid body and displacement parameters
 restraints due to disorder. A large number of weak residual
 electron density peaks remained in the lattice that seemed to form
 additional highly disordered/diffuse lattice pyridine molecules.
 Their refinement however did not converge properly, and PLATON/SQUEEZE
 was used to analyze and take into account the corresponding void
 spaces. A total of 677 electrons were thus recovered over three
 voids of 185, 1500 and 283 cubic angstroms. These figures would
 agree with at most 9 additional diffuse lattice pyridine molecules
 per unit cell, 4.5 per formula unit. Thus 4 additional lattice
 pyridine were added to the formula and taken into account for the
 density, mu etc.,SQUEEZE
;

_vrf_CHEMW03_ibcc978             
;
PROBLEM:  ALERT: The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10
RESPONSE: This discrepancy corresponds to the four additional
diffuse lattice pyridine molecules that have been added to the 
formula and taken into account for density, mu etc. These
correspond to void spaces that were analyzed and taken into
account by PLATON/SQUEEZE as modeling the remaining residual 
electron density peaks as lattice pyridine did not converge.
This results in a discrepancy between the formula, density and 
mu calculated from the model atom list and those reported that
do take into account the four additional pyridine molecules
not included in the structural model.
;

_vrf_DIFMX01_ibcc978             
;
PROBLEM:  The maximum difference density is > 0.1*ZMAX*1.00
            _refine_diff_density_max given =      3.459
            Test value =      2.900
RESPONSE: There remains one density peak close to C14A, so close
to C14 and thus to one of the methoxy group. It likely
corresponds to some disorder of the position of this
methoxy group (O4-C16). However, it was attempted to split it
over two positions (on C15 and C14), and the refinement was not
stable. it was therefore left as is.
;

_vrf_PLAT097_ibcc978             
;
PROBLEM:  Large Reported Max.  (Positive) Residual Density       3.46 eA-3
RESPONSE: There remains one density peak close to C14A, so close
to C14 and thus to one of the methoxy group. It likely
corresponds to some disorder of the position of this
methoxy group (O4-C16). However, it was attempted to split it
over two positions (on C15 and C14), and the refinement was not
stable. it was therefore left as is.
;

_vrf_DIFMX02_ibcc978             
;
PROBLEM:  The maximum difference density is > 0.1*ZMAX*0.75
            The relevant atom site should be identified.
RESPONSE: There remains one density peak close to C14A, so close
to C14 and thus to one of the methoxy group. It likely
corresponds to some disorder of the position of this
methoxy group (O4-C16). However, it was attempted to split it
over two positions (on C15 and C14), and the refinement was not
stable. it was therefore left as is.
;

_vrf_PLAT094_ibcc978             
;
PROBLEM:  Ratio of Maximum / Minimum Residual Density ....       2.96 Report
RESPONSE: There remains one density peak close to C14A, so close
to C14 and thus to one of the methoxy group. It likely
corresponds to some disorder of the position of this
methoxy group (O4-C16). However, it was attempted to split it
over two positions (on C15 and C14), and the refinement was not
stable. it was therefore left as is.
;

_vrf_PLAT220_ibcc978             
;
PROBLEM:  Non-Solvent Resd 1   C   Ueq(max)/Ueq(min) Range        9.0 Ratio
RESPONSE: This alert is related to the methoxy groups O4-C16,
O11-C41 and O18-C66 showing some strong disorder, especially
with respect to the phenyl they are attached to. This results in
large Ueq for the corresponding C and O when compared with the 
phenyl carbon they are attached to, C15, C14 and C65 respectively.
While this could be due to some positional disorder of the
methoxy groups, attempt at splitting the one methoxy for 
which a residual density peak remained did not converge.
;

_vrf_PLAT230_ibcc978             
;
PROBLEM:  Hirshfeld Test Diff for    O4     --  C15     ..       12.2 s.u.
RESPONSE: This alert is related to the methoxy groups O4-C16,
O11-C41 and O18-C66 showing some strong disorder, especially
with respect to the phenyl they are attached to. This results in
large Ueq for the corresponding C and O when compared with the 
phenyl carbon they are attached to, C15, C14 and C65 respectively.
While this could be due to some positional disorder of the
methoxy groups, attempt at splitting the one methoxy for 
which a residual density peak remained did not converge.
;

# SQUEEZE RESULTS (Version =  50315)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 185 38 ' '
2 0.000 0.083 0.500 1500 397 ' '
3 0.500 1.000 0.500 283 57 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 0 0 1.393
-1 1 0 1.436
0 1 0 1.218
0 -2 1 2.067
1 -2 1 2.072
-1 -1 1 1.947
0 -1 1 1.137
1 -1 1 1.636
-1 0 1 1.555
0 0 1 1.132
1 0 1 2.006
-1 1 1 2.003
0 -1 2 1.916
-1 0 2 2.338
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
TITL ibcc978_a.res in P-1
CELL   17.4290   22.7920   23.2110    119.15     92.99    108.93
SPGR P-1
# Solvent Accessible Volume =    2010.7
# Electrons Found in S.A.V. =     491.3
# Note: Atoms in Void as Cxxx and Qxxx all others
Q101 0.938 0.146 0.070 !       3.97 eA-3
Q102 0.762 0.484 0.405 !       3.19 eA-3
C103 0.627 0.627 0.242 !       3.15 eA-3
C104 0.049 0.045 0.002 !       3.01 eA-3
C105 0.877 0.899 0.343 !       2.83 eA-3
C106 0.613 0.568 0.308 !       2.82 eA-3
C107 0.520 0.945 0.407 !       2.72 eA-3
C108 0.114 0.180 0.436 !       2.70 eA-3
C109 0.873 0.939 0.337 !       2.70 eA-3
C110 0.482 0.915 0.420 !       2.65 eA-3
C111 0.879 0.882 0.391 !       2.62 eA-3
C112 0.409 0.969 0.385 !       2.60 eA-3
C113 0.724 0.196 0.257 !       2.60 eA-3
C114 0.666 0.689 0.297 !       2.53 eA-3
C115 0.094 0.070 0.049 !       2.47 eA-3
C116 1.007 0.982 0.054 !       2.46 eA-3
C117 0.484 0.984 0.391 !       2.46 eA-3
C118 0.852 0.240 0.315 !       2.42 eA-3
C119 0.069 0.029 0.080 !       2.42 eA-3
C120 0.097 0.220 0.422 !       2.33 eA-3
Q121 0.627 0.888 0.447 !       2.32 eA-3
C122 0.364 0.931 0.406 !       2.17 eA-3
C123 0.068 0.570 0.475 !       2.14 eA-3
Q124 0.827 0.157 0.225 !       2.13 eA-3
C125 0.011 0.532 0.447 !       2.10 eA-3
C126 0.552 0.524 0.257 !       2.08 eA-3
Q127 0.742 0.165 0.454 !       2.07 eA-3
C128 0.692 0.687 0.351 !       2.05 eA-3
C129 0.584 0.569 0.195 !       2.03 eA-3
C130 0.020 1.002 0.031 !       2.02 eA-3
C131 0.670 0.635 0.358 !       2.02 eA-3
C132 0.160 0.289 0.468 !       2.01 eA-3
C133 0.397 0.898 0.431 !       2.00 eA-3
C134 0.588 0.563 0.248 !       1.99 eA-3
C135 0.184 0.200 0.494 !       1.99 eA-3
C136 0.951 0.163 0.329 !       1.98 eA-3
C137 0.974 0.626 0.476 !       1.94 eA-3
C138 0.784 0.194 0.280 !       1.93 eA-3
C139 0.927 0.006 0.409 !       1.92 eA-3
Q140 0.292 0.742 0.459 !       1.90 eA-3
C141 0.721 0.258 0.273 !       1.82 eA-3
C142 0.538 0.524 0.202 !       1.79 eA-3
C143 0.646 0.640 0.303 !       1.79 eA-3
C144 0.898 0.131 0.424 !       1.79 eA-3
C145 0.956 0.328 0.491 !       1.79 eA-3
C146 0.759 0.179 0.226 !       1.77 eA-3
C147 0.854 0.187 0.289 !       1.77 eA-3
Q148 0.905 0.127 0.147 !       1.73 eA-3
Q149 0.236 0.710 0.493 !       1.70 eA-3
C150 0.773 0.696 0.492 !       1.70 eA-3
C151 0.833 0.225 0.336 !       1.69 eA-3
C152 0.888 0.344 0.484 !       1.64 eA-3
C153 0.946 0.963 0.452 !       1.64 eA-3
C154 0.782 0.249 0.319 !       1.61 eA-3
Q155 0.281 0.820 0.460 !       1.59 eA-3
C156 0.860 0.302 0.328 !       1.56 eA-3
C157 0.954 0.559 0.453 !       1.56 eA-3
C158 0.014 0.222 0.413 !       1.55 eA-3
Q159 0.331 0.779 0.461 !       1.53 eA-3
C160 0.017 0.179 0.406 !       1.52 eA-3
C161 0.786 0.765 0.491 !       1.51 eA-3
C162 0.783 0.819 0.350 !       1.50 eA-3
Q163 0.815 0.251 0.499 !       1.49 eA-3
Q164 0.185 0.749 0.501 !       1.49 eA-3
C165 0.945 0.018 0.447 !       1.45 eA-3
Q166 0.355 0.736 0.493 !       1.42 eA-3
C167 0.739 0.831 0.295 !       1.38 eA-3
Q168 0.969 0.140 0.119 !       1.35 eA-3
C169 0.911 0.946 0.391 !       1.33 eA-3
C170 0.787 0.893 0.294 !       1.32 eA-3
C171 0.788 0.313 0.299 !       1.31 eA-3
C172 0.187 0.250 0.483 !       1.29 eA-3
Q173 0.498 0.069 0.203 !       1.26 eA-3
Q174 0.073 0.890 0.195 !       1.26 eA-3
Q175 0.788 0.288 0.219 !       1.24 eA-3
C176 0.926 0.141 0.383 !       1.24 eA-3
Q177 0.463 0.202 0.049 !       1.23 eA-3
Q178 0.502 0.127 0.320 !       1.22 eA-3
Q179 0.114 0.859 0.186 !       1.21 eA-3
C180 0.032 0.606 0.468 !       1.20 eA-3
Q181 0.390 0.682 0.467 !       1.19 eA-3
Q182 0.789 0.511 0.318 !       1.17 eA-3
Q183 0.795 0.186 0.500 !       1.17 eA-3
Q184 0.546 0.727 0.048 !       1.12 eA-3
C185 0.873 0.142 0.251 !       1.11 eA-3
Q186 0.854 0.010 0.453 !       1.08 eA-3
Q187 0.541 0.132 0.307 !       1.06 eA-3
C188 0.403 0.902 0.383 !       1.05 eA-3
Q189 0.151 0.361 0.446 !       1.05 eA-3
C190 0.883 0.024 0.422 !       1.04 eA-3
Q191 0.221 0.164 0.275 !       1.03 eA-3
C192 0.462 0.959 0.476 !       1.03 eA-3
C193 0.351 0.912 0.362 !       1.03 eA-3
Q194 0.421 0.650 0.454 !       1.03 eA-3
Q195 0.452 0.245 0.060 !       1.01 eA-3
Q196 0.904 0.406 0.202 !       1.00 eA-3
Q197 0.456 0.108 0.242 !       0.99 eA-3
C198 0.428 0.953 0.436 !       0.98 eA-3
Q199 0.468 0.775 0.060 !       0.97 eA-3
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1206P)²+22.4417P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         27132
_refine_ls_number_parameters     1562
_refine_ls_number_restraints     494
_refine_ls_R_factor_all          0.1190
_refine_ls_R_factor_gt           0.0795
_refine_ls_wR_factor_ref         0.2459
_refine_ls_wR_factor_gt          0.2140
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.49207(4) 0.24753(4) -0.05778(3) 0.03583(18) Uani 1 1 d . . . . .
Cu2 Cu -0.03897(4) -0.27633(4) 0.14860(3) 0.03639(19) Uani 1 1 d . . . . .
Cu3 Cu 0.69797(4) 0.44679(4) 0.68635(3) 0.03673(19) Uani 1 1 d . . . . .
Ni1 Ni 0.43349(5) 0.21992(4) 0.05083(3) 0.03404(19) Uani 1 1 d . . . . .
Ni2 Ni 0.10808(5) -0.13542(4) 0.18647(3) 0.0377(2) Uani 1 1 d . . . . .
Ni3 Ni 0.60551(5) 0.33182(4) 0.53764(3) 0.0467(2) Uani 1 1 d D . . . .
O1 O 0.4839(3) 0.1763(2) -0.1481(2) 0.0487(11) Uani 1 1 d . . . . .
O2 O 0.4033(2) 0.1713(2) -0.05169(18) 0.0339(9) Uani 1 1 d . . . . .
O3 O 0.3478(2) 0.1341(2) 0.04380(18) 0.0371(9) Uani 1 1 d . . . . .
O4 O 0.1630(5) -0.0655(4) -0.1085(4) 0.115(2) Uani 1 1 d D U . . .
O5 O 0.1561(3) -0.0992(2) 0.12945(19) 0.0453(11) Uani 1 1 d . . . . .
O6 O 0.0301(2) -0.2313(2) 0.10411(18) 0.0385(9) Uani 1 1 d . . . . .
O7 O -0.1282(2) -0.3338(2) 0.06755(19) 0.0405(10) Uani 1 1 d . . . . .
O8 O 0.5982(3) 0.3111(2) -0.0508(2) 0.0460(10) Uani 1 1 d . . . . .
O9 O 0.5150(2) 0.2994(2) 0.04251(18) 0.0402(10) Uani 1 1 d . . . . .
O10 O 0.4783(3) 0.2782(2) 0.15123(19) 0.0439(10) Uani 1 1 d . . . . .
O11 O 0.7099(7) 0.4540(6) 0.2825(5) 0.170(4) Uani 1 1 d D U . . .
O12 O 0.6181(3) 0.3313(3) 0.4533(2) 0.0732(18) Uani 1 1 d . . . . .
O13 O 0.7093(2) 0.4264(2) 0.59303(17) 0.0378(9) Uani 1 1 d . . . . .
O14 O 0.7619(3) 0.5478(2) 0.72467(19) 0.0448(10) Uani 1 1 d . . . . .
O15 O -0.1062(2) -0.2910(2) 0.20652(18) 0.0418(10) Uani 1 1 d . . . . .
O16 O 0.0464(2) -0.1872(2) 0.23042(18) 0.0381(9) Uani 1 1 d . . . . .
O17 O 0.1767(3) -0.0487(2) 0.27638(18) 0.0452(10) Uani 1 1 d . . . . .
O18 O 0.2229(5) -0.0072(5) 0.4722(4) 0.132(3) Uani 1 1 d D U . . .
O19 O 0.5005(3) 0.2425(2) 0.4963(2) 0.0627(15) Uani 1 1 d . . . . .
O20 O 0.6081(2) 0.3476(2) 0.63038(17) 0.0371(9) Uani 1 1 d . . . . .
O21 O 0.6486(3) 0.4639(2) 0.76053(19) 0.0450(10) Uani 1 1 d . . . . .
N1 N 0.4089(3) 0.2975(3) -0.0698(3) 0.0479(13) Uani 1 1 d . . . . .
N2 N 0.3422(3) 0.2626(3) 0.0610(2) 0.0404(12) Uani 1 1 d . . . . .
N3 N 0.5188(3) 0.1685(3) 0.0427(3) 0.0419(12) Uani 1 1 d . . . . .
N4 N 0.0137(3) -0.3593(3) 0.1271(3) 0.0443(12) Uani 1 1 d . . . . .
N5 N 0.2027(3) -0.1765(3) 0.1822(2) 0.0429(12) Uani 1 1 d . . . . .
N6 N 0.0209(3) -0.0868(3) 0.1898(2) 0.0430(12) Uani 1 1 d . . . . .
N7 N 0.7982(3) 0.4104(3) 0.7012(3) 0.0479(13) Uani 1 1 d . . . . .
N9 N 0.5305(3) 0.3945(4) 0.5500(3) 0.0583(16) Uani 1 1 d . . . . .
C1 C 0.4205(4) 0.1149(3) -0.1892(3) 0.0451(15) Uani 1 1 d . . . . .
C2 C 0.4140(5) 0.0829(4) -0.2599(3) 0.068(2) Uani 1 1 d . U . . .
H2A H 0.4565 0.1058 -0.2751 0.082 Uiso 1 1 calc R U . . .
C3 C 0.3478(6) 0.0200(5) -0.3062(4) 0.085(3) Uani 1 1 d . U . . .
H3A H 0.3449 0.0003 -0.3534 0.103 Uiso 1 1 calc R U . . .
C4 C 0.2838(6) -0.0168(5) -0.2874(4) 0.090(3) Uani 1 1 d . U . . .
H4A H 0.2367 -0.0597 -0.3207 0.108 Uiso 1 1 calc R U . . .
C5 C 0.2913(5) 0.0110(4) -0.2195(3) 0.070(2) Uani 1 1 d . U . . .
H5A H 0.2498 -0.0149 -0.2057 0.084 Uiso 1 1 calc R U . . .
C6 C 0.3575(4) 0.0761(3) -0.1691(3) 0.0447(15) Uani 1 1 d . . . . .
C7 C 0.3577(3) 0.1034(3) -0.0961(2) 0.0281(11) Uani 1 1 d . . . . .
C8 C 0.3156(3) 0.0540(3) -0.0772(3) 0.0331(12) Uani 1 1 d . . . . .
H8A H 0.2881 0.0037 -0.1127 0.040 Uiso 1 1 calc R U . . .
C9 C 0.3105(4) 0.0721(3) -0.0106(3) 0.0380(13) Uani 1 1 d . . . . .
C10 C 0.2603(3) 0.0134(3) 0.0009(3) 0.0365(13) Uani 1 1 d . . . . .
C11 C 0.2889(4) 0.0230(4) 0.0635(3) 0.0532(18) Uani 1 1 d . . . . .
H11A H 0.3396 0.0635 0.0940 0.064 Uiso 1 1 calc R U . . .
C12 C 0.2460(4) -0.0241(4) 0.0822(3) 0.0496(17) Uani 1 1 d . . . . .
H12A H 0.2672 -0.0156 0.1253 0.060 Uiso 1 1 calc R U . . .
C13 C 0.1710(4) -0.0847(3) 0.0386(3) 0.0381(13) Uani 1 1 d . . . . .
C14 C 0.1429(4) -0.0969(3) -0.0259(3) 0.0442(15) Uani 1 1 d . . . . .
H14A H 0.0932 -0.1383 -0.0570 0.053 Uiso 1 1 calc R U . . .
C15 C 0.1878(4) -0.0485(3) -0.0441(3) 0.0407(14) Uani 1 1 d . . . . .
C16 C 0.0765(8) -0.1341(7) -0.1489(7) 0.168(5) Uani 1 1 d D U . . .
H16A H 0.0607 -0.1447 -0.1951 0.252 Uiso 1 1 calc R U . . .
H16B H 0.0819 -0.1767 -0.1513 0.252 Uiso 1 1 calc R U . . .
H16C H 0.0332 -0.1236 -0.1253 0.252 Uiso 1 1 calc R U . . .
C17 C 0.1275(4) -0.1296(3) 0.0657(3) 0.0412(14) Uani 1 1 d . . . . .
C18 C 0.0635(4) -0.1997(3) 0.0226(3) 0.0398(14) Uani 1 1 d . . . . .
H18A H 0.0489 -0.2158 -0.0243 0.048 Uiso 1 1 calc R U . . .
C19 C 0.0182(3) -0.2491(3) 0.0411(2) 0.0233(10) Uani 1 1 d . . . . .
C20 C -0.0455(3) -0.3209(3) -0.0101(3) 0.0334(12) Uani 1 1 d . . . . .
C21 C -0.0400(4) -0.3542(3) -0.0787(3) 0.0357(13) Uani 1 1 d . . . . .
H21A H 0.0089 -0.3320 -0.0891 0.043 Uiso 1 1 calc R U . . .
C22 C -0.1037(4) -0.4177(3) -0.1307(3) 0.0413(14) Uani 1 1 d . . . . .
H22A H -0.0982 -0.4396 -0.1762 0.050 Uiso 1 1 calc R U . . .
C23 C -0.1756(4) -0.4491(3) -0.1155(3) 0.0421(15) Uani 1 1 d . . . . .
H23A H -0.2213 -0.4911 -0.1513 0.050 Uiso 1 1 calc R U . . .
C24 C -0.1814(4) -0.4199(3) -0.0493(3) 0.0414(14) Uani 1 1 d . . . . .
H24A H -0.2311 -0.4433 -0.0405 0.050 Uiso 1 1 calc R U . . .
C25 C -0.1170(4) -0.3568(3) 0.0062(3) 0.0374(13) Uani 1 1 d . . . . .
C26 C 0.6460(4) 0.3754(3) 0.0024(3) 0.0436(15) Uani 1 1 d . . . . .
C27 C 0.7117(4) 0.4237(4) -0.0077(3) 0.0470(16) Uani 1 1 d . . . . .
H27A H 0.7193 0.4075 -0.0524 0.056 Uiso 1 1 calc R U . . .
C28 C 0.7632(4) 0.4914(3) 0.0440(3) 0.0480(16) Uani 1 1 d . . . . .
H28A H 0.8059 0.5217 0.0348 0.058 Uiso 1 1 calc R U . . .
C29 C 0.7554(4) 0.5184(3) 0.1109(3) 0.0492(16) Uani 1 1 d . . . . .
H29A H 0.7909 0.5668 0.1469 0.059 Uiso 1 1 calc R U . . .
C30 C 0.6945(4) 0.4723(3) 0.1224(3) 0.0484(17) Uani 1 1 d . . . . .
H30A H 0.6888 0.4897 0.1677 0.058 Uiso 1 1 calc R U . . .
C31 C 0.6403(4) 0.4008(3) 0.0708(3) 0.0442(15) Uani 1 1 d . . . . .
C32 C 0.5812(3) 0.3541(3) 0.0889(2) 0.0290(11) Uani 1 1 d . . . . .
C33 C 0.6001(5) 0.3660(3) 0.1540(3) 0.0553(19) Uani 1 1 d . . . . .
H33A H 0.6538 0.4028 0.1827 0.066 Uiso 1 1 calc R U . . .
C34 C 0.5500(4) 0.3307(3) 0.1826(3) 0.0493(17) Uani 1 1 d . . . . .
C35 C 0.5836(5) 0.3522(4) 0.2538(3) 0.0551(18) Uani 1 1 d . U . . .
C36 C 0.5318(5) 0.3116(4) 0.2764(3) 0.079(3) Uani 1 1 d . U . . .
H36A H 0.4781 0.2747 0.2479 0.094 Uiso 1 1 calc R U . . .
C37 C 0.5583(5) 0.3245(4) 0.3404(3) 0.080(2) Uani 1 1 d . U . . .
H37A H 0.5227 0.2953 0.3546 0.096 Uiso 1 1 calc R U . . .
C38 C 0.6356(5) 0.3793(4) 0.3846(3) 0.069(2) Uani 1 1 d . U . . .
C39 C 0.6848(5) 0.4237(4) 0.3638(3) 0.067(2) Uani 1 1 d . U . . .
H39A H 0.7361 0.4636 0.3939 0.081 Uiso 1 1 calc R U . . .
C40 C 0.6586(5) 0.4094(4) 0.2993(3) 0.067(2) Uani 1 1 d . U . . .
C41 C 0.7902(9) 0.5189(8) 0.3457(8) 0.209(7) Uani 1 1 d D U . . .
H41A H 0.8260 0.5501 0.3316 0.313 Uiso 1 1 calc R U . . .
H41B H 0.7710 0.5485 0.3843 0.313 Uiso 1 1 calc R U . . .
H41C H 0.8223 0.4974 0.3592 0.313 Uiso 1 1 calc R U . . .
C42 C 0.6563(5) 0.3875(4) 0.4523(3) 0.061(2) Uani 1 1 d . . . . .
C43 C 0.7132(4) 0.4556(4) 0.5080(3) 0.0537(18) Uani 1 1 d . . . . .
H43A H 0.7341 0.4945 0.5003 0.064 Uiso 1 1 calc R U . . .
C44 C 0.7428(3) 0.4724(3) 0.5753(2) 0.0315(12) Uani 1 1 d . . . . .
C45 C 0.8061(4) 0.5441(3) 0.6260(3) 0.0475(16) Uani 1 1 d . . . . .
C46 C 0.8654(5) 0.5826(4) 0.6040(3) 0.063(2) Uani 1 1 d . . . . .
H46A H 0.8608 0.5613 0.5565 0.075 Uiso 1 1 calc R U . . .
C47 C 0.9288(6) 0.6489(5) 0.6485(4) 0.091(3) Uani 1 1 d . . . . .
H47A H 0.9680 0.6736 0.6324 0.110 Uiso 1 1 calc R U . . .
C48 C 0.9351(6) 0.6793(4) 0.7166(4) 0.090(3) Uani 1 1 d . . . . .
H48A H 0.9795 0.7255 0.7480 0.108 Uiso 1 1 calc R U . . .
C49 C 0.8788(5) 0.6450(4) 0.7411(4) 0.068(2) Uani 1 1 d . . . . .
H49A H 0.8839 0.6689 0.7888 0.082 Uiso 1 1 calc R U . . .
C50 C 0.8143(4) 0.5756(3) 0.6974(3) 0.0502(16) Uani 1 1 d . . . . .
C51 C -0.0755(4) -0.2733(3) 0.2682(3) 0.0414(14) Uani 1 1 d . . . . .
C52 C -0.1216(4) -0.3122(4) 0.2952(3) 0.0542(18) Uani 1 1 d . . . . .
H52A H -0.1740 -0.3519 0.2672 0.065 Uiso 1 1 calc R U . . .
C53 C -0.0952(5) -0.2961(4) 0.3598(3) 0.062(2) Uani 1 1 d . . . . .
H53A H -0.1285 -0.3249 0.3753 0.074 Uiso 1 1 calc R U . . .
C54 C -0.0201(4) -0.2381(4) 0.4024(3) 0.0556(18) Uani 1 1 d . . . . .
H54A H -0.0015 -0.2272 0.4471 0.067 Uiso 1 1 calc R U . . .
C55 C 0.0273(4) -0.1965(3) 0.3800(3) 0.0450(15) Uani 1 1 d . . . . .
H55A H 0.0790 -0.1569 0.4096 0.054 Uiso 1 1 calc R U . . .
C56 C 0.0017(4) -0.2105(3) 0.3142(3) 0.0392(13) Uani 1 1 d . . . . .
C57 C 0.0537(3) -0.1612(3) 0.2951(2) 0.0254(11) Uani 1 1 d . . . . .
C58 C 0.1094(4) -0.0904(3) 0.3442(3) 0.0400(14) Uani 1 1 d . . . . .
H58A H 0.1076 -0.0738 0.3902 0.048 Uiso 1 1 calc R U . . .
C59 C 0.1688(4) -0.0403(3) 0.3325(3) 0.0412(14) Uani 1 1 d . . . . .
C60 C 0.2335(4) 0.0311(3) 0.3920(3) 0.0413(14) Uani 1 1 d . . . . .
C61 C 0.2709(4) 0.0856(4) 0.3789(3) 0.0570(19) Uani 1 1 d . . . . .
H61A H 0.2489 0.0796 0.3371 0.068 Uiso 1 1 calc R U . . .
C62 C 0.3389(4) 0.1477(3) 0.4251(3) 0.0574(19) Uani 1 1 d . . . . .
H62A H 0.3627 0.1846 0.4152 0.069 Uiso 1 1 calc R U . . .
C63 C 0.3745(4) 0.1584(3) 0.4864(3) 0.0442(15) Uani 1 1 d . . . . .
C64 C 0.3325(4) 0.1062(4) 0.5017(3) 0.0556(19) Uani 1 1 d . . . . .
H64A H 0.3520 0.1140 0.5449 0.067 Uiso 1 1 calc R U . . .
C65 C 0.2635(4) 0.0438(3) 0.4555(3) 0.0508(17) Uani 1 1 d . . . . .
C66 C 0.2625(10) 0.0121(8) 0.5421(6) 0.161(5) Uani 1 1 d D U . . .
H66A H 0.2304 -0.0263 0.5500 0.242 Uiso 1 1 calc R U . . .
H66B H 0.3204 0.0160 0.5446 0.242 Uiso 1 1 calc R U . . .
H66C H 0.2623 0.0591 0.5770 0.242 Uiso 1 1 calc R U . . .
C67 C 0.4563(4) 0.2223(3) 0.5294(3) 0.0456(15) Uani 1 1 d . . . . .
C68 C 0.4752(4) 0.2545(3) 0.6002(3) 0.0414(14) Uani 1 1 d . . . . .
H68A H 0.4329 0.2352 0.6179 0.050 Uiso 1 1 calc R U . . .
C69 C 0.5488(3) 0.3114(3) 0.6473(2) 0.0262(11) Uani 1 1 d . . . . .
C70 C 0.5598(4) 0.3378(3) 0.7197(3) 0.0392(14) Uani 1 1 d . . . . .
C71 C 0.5197(4) 0.2869(3) 0.7380(3) 0.0425(14) Uani 1 1 d . . . . .
H71A H 0.4906 0.2365 0.7032 0.051 Uiso 1 1 calc R U . . .
C72 C 0.5219(4) 0.3089(4) 0.8059(3) 0.0475(16) Uani 1 1 d . . . . .
H72A H 0.4956 0.2743 0.8178 0.057 Uiso 1 1 calc R U . . .
C73 C 0.5636(4) 0.3829(4) 0.8554(3) 0.0580(19) Uani 1 1 d . . . . .
H73A H 0.5638 0.3990 0.9016 0.070 Uiso 1 1 calc R U . . .
C74 C 0.6042(4) 0.4331(4) 0.8396(3) 0.0547(19) Uani 1 1 d . . . . .
H74A H 0.6307 0.4834 0.8750 0.066 Uiso 1 1 calc R U . . .
C75 C 0.6078(4) 0.4122(3) 0.7718(3) 0.0445(15) Uani 1 1 d . . . . .
C76 C 0.4267(5) 0.3678(5) -0.0284(4) 0.064(2) Uani 1 1 d . . . . .
H76A H 0.4760 0.3972 0.0081 0.077 Uiso 1 1 calc R U . . .
C77 C 0.3740(7) 0.4006(6) -0.0370(6) 0.088(3) Uani 1 1 d . . . . .
H77A H 0.3877 0.4515 -0.0070 0.106 Uiso 1 1 calc R U . . .
C78 C 0.3034(7) 0.3574(8) -0.0895(7) 0.095(4) Uani 1 1 d . . . . .
H78A H 0.2666 0.3777 -0.0962 0.114 Uiso 1 1 calc R U . . .
C79 C 0.2862(6) 0.2858(7) -0.1316(6) 0.088(3) Uani 1 1 d . . . . .
H79A H 0.2369 0.2553 -0.1682 0.106 Uiso 1 1 calc R U . . .
C80 C 0.3398(4) 0.2569(5) -0.1218(4) 0.064(2) Uani 1 1 d . . . . .
H80A H 0.3276 0.2065 -0.1528 0.077 Uiso 1 1 calc R U . . .
C81 C 0.3548(5) 0.3287(4) 0.1135(3) 0.0548(18) Uani 1 1 d . . . . .
H81A H 0.4103 0.3614 0.1410 0.066 Uiso 1 1 calc R U . . .
C82 C 0.2892(6) 0.3518(5) 0.1299(4) 0.068(2) Uani 1 1 d . . . . .
H82A H 0.2998 0.3992 0.1679 0.081 Uiso 1 1 calc R U . . .
C83 C 0.2099(6) 0.3045(5) 0.0900(4) 0.071(2) Uani 1 1 d . . . . .
H83A H 0.1643 0.3183 0.1011 0.085 Uiso 1 1 calc R U . . .
C84 C 0.1952(5) 0.2367(5) 0.0335(5) 0.070(2) Uani 1 1 d . . . . .
H84A H 0.1407 0.2042 0.0039 0.084 Uiso 1 1 calc R U . . .
C85 C 0.2634(4) 0.2182(4) 0.0221(4) 0.0558(17) Uani 1 1 d . . . . .
H85A H 0.2539 0.1712 -0.0158 0.067 Uiso 1 1 calc R U . . .
C86 C 0.5256(5) 0.1481(4) 0.0872(4) 0.0587(19) Uani 1 1 d . . . . .
H86A H 0.4961 0.1606 0.1217 0.070 Uiso 1 1 calc R U . . .
C87 C 0.5732(7) 0.1101(6) 0.0853(5) 0.099(3) Uani 1 1 d . . . . .
H87A H 0.5779 0.0978 0.1186 0.118 Uiso 1 1 calc R U . . .
C88 C 0.6139(8) 0.0903(7) 0.0348(7) 0.122(4) Uani 1 1 d . U . . .
H88A H 0.6450 0.0618 0.0307 0.147 Uiso 1 1 calc R U . . .
C89 C 0.6086(8) 0.1127(7) -0.0102(6) 0.114(3) Uani 1 1 d . U . . .
H89A H 0.6386 0.1023 -0.0445 0.137 Uiso 1 1 calc R U . . .
C90 C 0.5595(5) 0.1502(5) -0.0043(4) 0.070(2) Uani 1 1 d . . . . .
H90A H 0.5545 0.1638 -0.0366 0.084 Uiso 1 1 calc R U . . .
C91 C 0.0730(5) -0.3671(4) 0.0937(4) 0.0616(19) Uani 1 1 d . . . . .
H91A H 0.1030 -0.3290 0.0868 0.074 Uiso 1 1 calc R U . . .
C92 C 0.0935(5) -0.4267(5) 0.0686(4) 0.073(2) Uani 1 1 d . . . . .
H92A H 0.1376 -0.4289 0.0463 0.087 Uiso 1 1 calc R U . . .
C93 C 0.0489(6) -0.4827(5) 0.0762(4) 0.073(2) Uani 1 1 d . . . . .
H93A H 0.0598 -0.5258 0.0575 0.087 Uiso 1 1 calc R U . . .
C94 C -0.0110(6) -0.4760(5) 0.1110(4) 0.073(2) Uani 1 1 d . . . . .
H94A H -0.0426 -0.5143 0.1171 0.088 Uiso 1 1 calc R U . . .
C95 C -0.0254(4) -0.4136(4) 0.1370(3) 0.0523(17) Uani 1 1 d . . . . .
H95A H -0.0653 -0.4083 0.1634 0.063 Uiso 1 1 calc R U . . .
C96 C 0.2342(4) -0.2007(4) 0.1270(4) 0.0571(18) Uani 1 1 d . . . . .
H96A H 0.2119 -0.1996 0.0894 0.069 Uiso 1 1 calc R U . . .
C97 C 0.2956(5) -0.2267(5) 0.1214(5) 0.072(2) Uani 1 1 d . . . . .
H97A H 0.3145 -0.2436 0.0809 0.086 Uiso 1 1 calc R U . . .
C98 C 0.3293(5) -0.2277(4) 0.1754(4) 0.0622(19) Uani 1 1 d . . . . .
H98A H 0.3734 -0.2440 0.1736 0.075 Uiso 1 1 calc R U . . .
C99 C 0.2985(6) -0.2052(5) 0.2312(5) 0.077(2) Uani 1 1 d . . . . .
H99A H 0.3201 -0.2068 0.2687 0.093 Uiso 1 1 calc R U . . .
C100 C 0.2359(5) -0.1801(5) 0.2336(4) 0.066(2) Uani 1 1 d . . . . .
H10A H 0.2152 -0.1646 0.2733 0.080 Uiso 1 1 calc R U . . .
C101 C -0.0631(5) -0.1232(4) 0.1637(4) 0.0588(18) Uani 1 1 d . . . . .
H10B H -0.0872 -0.1746 0.1450 0.071 Uiso 1 1 calc R U . . .
C102 C -0.1148(6) -0.0894(5) 0.1630(5) 0.082(3) Uani 1 1 d . . . . .
H10C H -0.1735 -0.1170 0.1442 0.099 Uiso 1 1 calc R U . . .
C103 C -0.0806(7) -0.0136(6) 0.1901(7) 0.105(4) Uani 1 1 d . . . . .
H10D H -0.1147 0.0115 0.1898 0.126 Uiso 1 1 calc R U . . .
C104 C 0.0057(7) 0.0229(5) 0.2175(6) 0.103(4) Uani 1 1 d . . . . .
H10E H 0.0316 0.0746 0.2381 0.123 Uiso 1 1 calc R U . . .
C105 C 0.0535(5) -0.0147(4) 0.2150(4) 0.067(2) Uani 1 1 d . . . . .
H10F H 0.1127 0.0114 0.2319 0.080 Uiso 1 1 calc R U . . .
C106 C 0.8665(5) 0.4263(5) 0.6803(4) 0.067(2) Uani 1 1 d . . . . .
H10G H 0.8740 0.4575 0.6631 0.080 Uiso 1 1 calc R U . . .
C107 C 0.9275(5) 0.4009(5) 0.6817(5) 0.072(2) Uani 1 1 d . . . . .
H10H H 0.9763 0.4151 0.6671 0.087 Uiso 1 1 calc R U . . .
C108 C 0.9161(5) 0.3549(5) 0.7045(4) 0.068(2) Uani 1 1 d . . . . .
H10I H 0.9549 0.3332 0.7029 0.081 Uiso 1 1 calc R U . . .
C109 C 0.8476(5) 0.3400(5) 0.7301(5) 0.080(3) Uani 1 1 d . . . . .
H10J H 0.8403 0.3104 0.7491 0.096 Uiso 1 1 calc R U . . .
C110 C 0.7904(5) 0.3685(5) 0.7278(5) 0.074(2) Uani 1 1 d . . . . .
H11B H 0.7434 0.3584 0.7456 0.088 Uiso 1 1 calc R U . . .
N8 N 0.6851(8) 0.2692(7) 0.5242(7) 0.078(3) Uani 0.440(7) 1 d DG U P A 1
C111 C 0.7538(10) 0.2813(7) 0.4973(7) 0.088(3) Uani 0.440(7) 1 d G U P A 1
H11C H 0.7680 0.3174 0.4857 0.106 Uiso 0.440(7) 1 calc R U P A 1
C112 C 0.8018(8) 0.2405(8) 0.4874(8) 0.099(3) Uani 0.440(7) 1 d G U P A 1
H11D H 0.8488 0.2487 0.4691 0.119 Uiso 0.440(7) 1 calc R U P A 1
C113 C 0.7810(9) 0.1877(8) 0.5045(8) 0.098(3) Uani 0.440(7) 1 d G U P A 1
H11E H 0.8138 0.1598 0.4977 0.117 Uiso 0.440(7) 1 calc R U P A 1
C114 C 0.7123(10) 0.1756(7) 0.5314(8) 0.095(3) Uani 0.440(7) 1 d G U P A 1
H11F H 0.6981 0.1395 0.5430 0.114 Uiso 0.440(7) 1 calc R U P A 1
C115 C 0.6643(8) 0.2164(7) 0.5412(7) 0.086(3) Uani 0.440(7) 1 d G U P A 1
H11G H 0.6173 0.2082 0.5596 0.103 Uiso 0.440(7) 1 calc R U P A 1
N18 N 0.6645(7) 0.2628(5) 0.5092(5) 0.072(2) Uani 0.560(7) 1 d DG U P A 2
C121 C 0.7264(7) 0.2659(5) 0.5522(4) 0.095(3) Uani 0.560(7) 1 d G U P A 2
H12D H 0.7425 0.3017 0.5997 0.113 Uiso 0.560(7) 1 calc R U P A 2
C122 C 0.7645(7) 0.2167(7) 0.5257(6) 0.100(3) Uani 0.560(7) 1 d G U P A 2
H12E H 0.8068 0.2189 0.5551 0.119 Uiso 0.560(7) 1 calc R U P A 2
C123 C 0.7408(8) 0.1644(6) 0.4562(6) 0.097(3) Uani 0.560(7) 1 d G U P A 2
H12F H 0.7669 0.1308 0.4381 0.116 Uiso 0.560(7) 1 calc R U P A 2
C124 C 0.6790(8) 0.1613(5) 0.4132(4) 0.098(4) Uani 0.560(7) 1 d G U P A 2
H12G H 0.6628 0.1256 0.3657 0.118 Uiso 0.560(7) 1 calc R U P A 2
C125 C 0.6408(7) 0.2105(6) 0.4397(5) 0.090(3) Uani 0.560(7) 1 d G U P A 2
H12H H 0.5986 0.2084 0.4103 0.108 Uiso 0.560(7) 1 calc R U P A 2
C116 C 0.5473(5) 0.4621(5) 0.6004(5) 0.068(2) Uani 1 1 d . . . . .
H11H H 0.5932 0.4845 0.6385 0.081 Uiso 1 1 calc R U . . .
C117 C 0.5024(7) 0.5018(7) 0.6010(6) 0.098(3) Uani 1 1 d . . . . .
H11I H 0.5159 0.5498 0.6390 0.117 Uiso 1 1 calc R U . . .
C118 C 0.4376(7) 0.4705(9) 0.5455(7) 0.117(4) Uani 1 1 d . . . . .
H11J H 0.4051 0.4964 0.5439 0.140 Uiso 1 1 calc R U . . .
C119 C 0.4210(7) 0.4012(7) 0.4923(7) 0.106(3) Uani 1 1 d . U . . .
H11K H 0.3775 0.3784 0.4525 0.127 Uiso 1 1 calc R U . . .
C120 C 0.4665(5) 0.3659(6) 0.4972(5) 0.091(3) Uani 1 1 d . U . . .
H12B H 0.4523 0.3170 0.4604 0.110 Uiso 1 1 calc R U . . .
N1S N 0.3009(6) 0.2307(4) 0.2113(4) 0.174(4) Uani 1 1 d G U . . .
C1S C 0.2770(5) 0.2862(4) 0.2548(4) 0.162(4) Uani 1 1 d G U . . .
H1SA H 0.2787 0.3233 0.2461 0.194 Uiso 1 1 calc R U . . .
C2S C 0.2508(6) 0.2876(4) 0.3108(4) 0.169(4) Uani 1 1 d G U . . .
H2SA H 0.2346 0.3256 0.3405 0.202 Uiso 1 1 calc R U . . .
C3S C 0.2485(6) 0.2334(4) 0.3234(4) 0.175(4) Uani 1 1 d G U . . .
H3SA H 0.2306 0.2344 0.3617 0.210 Uiso 1 1 calc R U . . .
C4S C 0.2723(4) 0.1779(4) 0.2800(3) 0.185(4) Uani 1 1 d G U . . .
H4SA H 0.2707 0.1409 0.2886 0.222 Uiso 1 1 calc R U . . .
C5S C 0.2985(5) 0.1765(4) 0.2240(4) 0.188(4) Uani 1 1 d G U . . .
H5SA H 0.3148 0.1386 0.1943 0.225 Uiso 1 1 calc R U . . .
N2S N -0.1238(7) -0.7132(5) 0.1598(8) 0.196(4) Uani 1 1 d G U . . .
C6S C -0.0820(7) -0.6391(5) 0.2097(7) 0.182(5) Uani 1 1 d G U . . .
H6SA H -0.0364 -0.6229 0.2456 0.218 Uiso 1 1 calc R U . . .
C7S C -0.1080(9) -0.5891(6) 0.2062(7) 0.177(5) Uani 1 1 d G U . . .
H7SA H -0.0794 -0.5384 0.2401 0.212 Uiso 1 1 calc R U . . .
C8S C -0.1747(9) -0.6114(7) 0.1544(8) 0.199(5) Uani 1 1 d G U . . .
H8SA H -0.1914 -0.5761 0.1534 0.239 Uiso 1 1 calc R U . . .
C9S C -0.2171(7) -0.6853(8) 0.1042(7) 0.222(6) Uani 1 1 d G U . . .
H9SA H -0.2627 -0.7006 0.0688 0.266 Uiso 1 1 calc R U . . .
C10S C -0.1926(10) -0.7370(6) 0.1058(9) 0.207(6) Uani 1 1 d G U . . .
H10K H -0.2212 -0.7875 0.0715 0.249 Uiso 1 1 calc R U . . .
N3S N 0.3920(6) 0.0764(6) 0.2556(6) 0.180(4) Uani 1 1 d G U . . .
C11S C 0.3781(5) 0.0054(5) 0.2378(6) 0.160(4) Uani 1 1 d G U . . .
H11L H 0.3269 -0.0247 0.2395 0.192 Uiso 1 1 calc R U . . .
C12S C 0.4392(7) -0.0217(4) 0.2172(6) 0.168(4) Uani 1 1 d G U . . .
H12C H 0.4297 -0.0702 0.2050 0.202 Uiso 1 1 calc R U . . .
C13S C 0.5141(6) 0.0223(6) 0.2146(6) 0.176(4) Uani 1 1 d G U . . .
H13A H 0.5558 0.0038 0.2006 0.212 Uiso 1 1 calc R U . . .
C14S C 0.5280(6) 0.0933(6) 0.2325(7) 0.182(4) Uani 1 1 d G U . . .
H14B H 0.5792 0.1233 0.2307 0.218 Uiso 1 1 calc R U . . .
C15S C 0.4669(7) 0.1204(4) 0.2530(6) 0.192(5) Uani 1 1 d G U . . .
H15A H 0.4764 0.1689 0.2652 0.230 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O8 1.884(4) . ?
Cu1 O1 1.885(4) . ?
Cu1 O9 1.973(4) . ?
Cu1 O2 1.988(3) . ?
Cu1 N1 2.195(6) . ?
Cu2 O15 1.908(4) . ?
Cu2 O7 1.910(4) . ?
Cu2 O6 1.982(4) . ?
Cu2 O16 1.983(4) . ?
Cu2 N4 2.219(6) . ?
Cu3 O14 1.889(4) . ?
Cu3 O21 1.891(4) . ?
Cu3 O20 1.970(4) . ?
Cu3 O13 2.018(4) . ?
Cu3 N7 2.240(6) . ?
Ni1 O3 1.962(3) . ?
Ni1 O10 1.981(4) . ?
Ni1 O9 2.009(4) . ?
Ni1 O2 2.022(4) . ?
Ni1 N2 2.086(5) . ?
Ni1 N3 2.136(5) . ?
Ni2 O5 1.966(4) . ?
Ni2 O17 1.970(4) . ?
Ni2 O6 2.003(4) . ?
Ni2 O16 2.013(4) . ?
Ni2 N5 2.130(6) . ?
Ni2 N6 2.136(6) . ?
Ni3 O12 1.976(4) . ?
Ni3 O19 1.977(4) . ?
Ni3 O20 1.998(3) . ?
Ni3 N18 2.019(7) . ?
Ni3 O13 2.025(4) . ?
Ni3 N9 2.166(7) . ?
Ni3 N8 2.225(9) . ?
O1 C1 1.295(7) . ?
O2 C7 1.285(6) . ?
O3 C9 1.262(7) . ?
O4 C15 1.352(8) . ?
O4 C16 1.579(11) . ?
O5 C17 1.272(7) . ?
O6 C19 1.298(6) . ?
O7 C25 1.307(7) . ?
O8 C26 1.305(7) . ?
O9 C32 1.294(6) . ?
O10 C34 1.269(7) . ?
O11 C40 1.348(11) . ?
O11 C41 1.620(13) . ?
O12 C42 1.251(7) . ?
O13 C44 1.287(6) . ?
O14 C50 1.308(7) . ?
O15 C51 1.309(7) . ?
O16 C57 1.298(6) . ?
O17 C59 1.242(7) . ?
O18 C65 1.390(9) . ?
O18 C66 1.514(11) . ?
O19 C67 1.255(7) . ?
O20 C69 1.308(6) . ?
O21 C75 1.317(7) . ?
N1 C76 1.316(9) . ?
N1 C80 1.341(9) . ?
N2 C81 1.331(8) . ?
N2 C85 1.345(8) . ?
N3 C90 1.304(9) . ?
N3 C86 1.337(8) . ?
N4 C91 1.330(9) . ?
N4 C95 1.337(8) . ?
N5 C100 1.350(9) . ?
N5 C96 1.351(8) . ?
N6 C105 1.337(9) . ?
N6 C101 1.352(9) . ?
N7 C106 1.316(9) . ?
N7 C110 1.346(8) . ?
N9 C116 1.320(10) . ?
N9 C120 1.334(9) . ?
C1 C2 1.413(8) . ?
C1 C6 1.425(8) . ?
C2 C3 1.356(10) . ?
C2 H2A 0.9500 . ?
C3 C4 1.393(11) . ?
C3 H3A 0.9500 . ?
C4 C5 1.362(10) . ?
C4 H4A 0.9500 . ?
C5 C6 1.399(9) . ?
C5 H5A 0.9500 . ?
C6 C7 1.492(7) . ?
C7 C8 1.407(7) . ?
C8 C9 1.410(8) . ?
C8 H8A 0.9500 . ?
C9 C10 1.499(7) . ?
C10 C15 1.395(8) . ?
C10 C11 1.396(8) . ?
C11 C12 1.364(8) . ?
C11 H11A 0.9500 . ?
C12 C13 1.403(8) . ?
C12 H12A 0.9500 . ?
C13 C14 1.410(8) . ?
C13 C17 1.479(7) . ?
C14 C15 1.391(8) . ?
C14 H14A 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.403(8) . ?
C18 C19 1.416(7) . ?
C18 H18A 0.9500 . ?
C19 C20 1.454(7) . ?
C20 C21 1.415(7) . ?
C20 C25 1.434(8) . ?
C21 C22 1.378(8) . ?
C21 H21A 0.9500 . ?
C22 C23 1.384(8) . ?
C22 H22A 0.9500 . ?
C23 C24 1.370(8) . ?
C23 H23A 0.9500 . ?
C24 C25 1.409(8) . ?
C24 H24A 0.9500 . ?
C26 C31 1.422(8) . ?
C26 C27 1.429(8) . ?
C27 C28 1.347(9) . ?
C27 H27A 0.9500 . ?
C28 C29 1.396(9) . ?
C28 H28A 0.9500 . ?
C29 C30 1.372(8) . ?
C29 H29A 0.9500 . ?
C30 C31 1.401(8) . ?
C30 H30A 0.9500 . ?
C31 C32 1.462(7) . ?
C32 C33 1.400(7) . ?
C33 C34 1.406(9) . ?
C33 H33A 0.9500 . ?
C34 C35 1.495(8) . ?
C35 C36 1.389(9) . ?
C35 C40 1.390(9) . ?
C36 C37 1.386(9) . ?
C36 H36A 0.9500 . ?
C37 C38 1.394(10) . ?
C37 H37A 0.9500 . ?
C38 C39 1.395(9) . ?
C38 C42 1.498(8) . ?
C39 C40 1.383(9) . ?
C39 H39A 0.9500 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.406(9) . ?
C43 C44 1.434(7) . ?
C43 H43A 0.9500 . ?
C44 C45 1.446(7) . ?
C45 C46 1.415(9) . ?
C45 C50 1.426(8) . ?
C46 C47 1.360(10) . ?
C46 H46A 0.9500 . ?
C47 C48 1.363(11) . ?
C47 H47A 0.9500 . ?
C48 C49 1.375(10) . ?
C48 H48A 0.9500 . ?
C49 C50 1.400(9) . ?
C49 H49A 0.9500 . ?
C51 C52 1.398(8) . ?
C51 C56 1.453(8) . ?
C52 C53 1.371(9) . ?
C52 H52A 0.9500 . ?
C53 C54 1.380(9) . ?
C53 H53A 0.9500 . ?
C54 C55 1.367(8) . ?
C54 H54A 0.9500 . ?
C55 C56 1.413(8) . ?
C55 H55A 0.9500 . ?
C56 C57 1.464(7) . ?
C57 C58 1.386(7) . ?
C58 C59 1.421(8) . ?
C58 H58A 0.9500 . ?
C59 C60 1.511(8) . ?
C60 C61 1.388(8) . ?
C60 C65 1.391(8) . ?
C61 C62 1.363(8) . ?
C61 H61A 0.9500 . ?
C62 C63 1.394(8) . ?
C62 H62A 0.9500 . ?
C63 C64 1.396(8) . ?
C63 C67 1.495(8) . ?
C64 C65 1.375(8) . ?
C64 H64A 0.9500 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 C68 1.400(8) . ?
C68 C69 1.383(7) . ?
C68 H68A 0.9500 . ?
C69 C70 1.459(7) . ?
C70 C71 1.414(8) . ?
C70 C75 1.419(8) . ?
C71 C72 1.396(8) . ?
C71 H71A 0.9500 . ?
C72 C73 1.385(10) . ?
C72 H72A 0.9500 . ?
C73 C74 1.362(9) . ?
C73 H73A 0.9500 . ?
C74 C75 1.418(8) . ?
C74 H74A 0.9500 . ?
C76 C77 1.420(12) . ?
C76 H76A 0.9500 . ?
C77 C78 1.362(15) . ?
C77 H77A 0.9500 . ?
C78 C79 1.343(15) . ?
C78 H78A 0.9500 . ?
C79 C80 1.372(12) . ?
C79 H79A 0.9500 . ?
C80 H80A 0.9500 . ?
C81 C82 1.404(11) . ?
C81 H81A 0.9500 . ?
C82 C83 1.363(12) . ?
C82 H82A 0.9500 . ?
C83 C84 1.380(12) . ?
C83 H83A 0.9500 . ?
C84 C85 1.380(11) . ?
C84 H84A 0.9500 . ?
C85 H85A 0.9500 . ?
C86 C87 1.368(12) . ?
C86 H86A 0.9500 . ?
C87 C88 1.363(15) . ?
C87 H87A 0.9500 . ?
C88 C89 1.377(16) . ?
C88 H88A 0.9500 . ?
C89 C90 1.362(12) . ?
C89 H89A 0.9500 . ?
C90 H90A 0.9500 . ?
C91 C92 1.370(11) . ?
C91 H91A 0.9500 . ?
C92 C93 1.363(12) . ?
C92 H92A 0.9500 . ?
C93 C94 1.355(12) . ?
C93 H93A 0.9500 . ?
C94 C95 1.366(11) . ?
C94 H94A 0.9500 . ?
C95 H95A 0.9500 . ?
C96 C97 1.364(11) . ?
C96 H96A 0.9500 . ?
C97 C98 1.370(11) . ?
C97 H97A 0.9500 . ?
C98 C99 1.355(11) . ?
C98 H98A 0.9500 . ?
C99 C100 1.380(11) . ?
C99 H99A 0.9500 . ?
C100 H10A 0.9500 . ?
C101 C102 1.368(11) . ?
C101 H10B 0.9500 . ?
C102 C103 1.403(13) . ?
C102 H10C 0.9500 . ?
C103 C104 1.390(14) . ?
C103 H10D 0.9500 . ?
C104 C105 1.362(12) . ?
C104 H10E 0.9500 . ?
C105 H10F 0.9500 . ?
C106 C107 1.372(11) . ?
C106 H10G 0.9500 . ?
C107 C108 1.354(11) . ?
C107 H10H 0.9500 . ?
C108 C109 1.380(12) . ?
C108 H10I 0.9500 . ?
C109 C110 1.367(12) . ?
C109 H10J 0.9500 . ?
C110 H11B 0.9500 . ?
N8 C111 1.3900 . ?
N8 C115 1.3900 . ?
C111 C112 1.3900 . ?
C111 H11C 0.9500 . ?
C112 C113 1.3900 . ?
C112 H11D 0.9500 . ?
C113 C114 1.3900 . ?
C113 H11E 0.9500 . ?
C114 C115 1.3900 . ?
C114 H11F 0.9500 . ?
C115 H11G 0.9500 . ?
N18 C121 1.3900 . ?
N18 C125 1.3900 . ?
C121 C122 1.3900 . ?
C121 H12D 0.9500 . ?
C122 C123 1.3900 . ?
C122 H12E 0.9500 . ?
C123 C124 1.3900 . ?
C123 H12F 0.9500 . ?
C124 C125 1.3900 . ?
C124 H12G 0.9500 . ?
C125 H12H 0.9500 . ?
C116 C117 1.372(12) . ?
C116 H11H 0.9500 . ?
C117 C118 1.369(15) . ?
C117 H11I 0.9500 . ?
C118 C119 1.367(16) . ?
C118 H11J 0.9500 . ?
C119 C120 1.335(15) . ?
C119 H11K 0.9500 . ?
C120 H12B 0.9500 . ?
N1S C1S 1.3900 . ?
N1S C5S 1.3900 . ?
C1S C2S 1.3900 . ?
C1S H1SA 0.9500 . ?
C2S C3S 1.3900 . ?
C2S H2SA 0.9500 . ?
C3S C4S 1.3900 . ?
C3S H3SA 0.9500 . ?
C4S C5S 1.3900 . ?
C4S H4SA 0.9500 . ?
C5S H5SA 0.9500 . ?
N2S C6S 1.3900 . ?
N2S C10S 1.438(19) . ?
C6S C7S 1.390(17) . ?
C6S H6SA 0.9500 . ?
C7S C8S 1.3900 . ?
C7S H7SA 0.9500 . ?
C8S C9S 1.3900 . ?
C8S H8SA 0.9500 . ?
C9S C10S 1.3900 . ?
C9S H9SA 0.9500 . ?
C10S H10K 0.9500 . ?
N3S C11S 1.3900 . ?
N3S C15S 1.3900 . ?
C11S C12S 1.3900 . ?
C11S H11L 0.9500 . ?
C12S C13S 1.3900 . ?
C12S H12C 0.9500 . ?
C13S C14S 1.3900 . ?
C13S H13A 0.9500 . ?
C14S C15S 1.3900 . ?
C14S H14B 0.9500 . ?
C15S H15A 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
O8 Cu1 O1 91.66(17) . . ?
O8 Cu1 O9 90.48(16) . . ?
O1 Cu1 O9 159.38(19) . . ?
O8 Cu1 O2 161.41(17) . . ?
O1 Cu1 O2 89.70(16) . . ?
O9 Cu1 O2 81.94(15) . . ?
O8 Cu1 N1 103.07(19) . . ?
O1 Cu1 N1 103.8(2) . . ?
O9 Cu1 N1 95.66(19) . . ?
O2 Cu1 N1 94.58(17) . . ?
O15 Cu2 O7 96.13(16) . . ?
O15 Cu2 O6 162.64(18) . . ?
O7 Cu2 O6 88.93(15) . . ?
O15 Cu2 O16 89.18(15) . . ?
O7 Cu2 O16 158.27(17) . . ?
O6 Cu2 O16 80.35(15) . . ?
O15 Cu2 N4 99.08(18) . . ?
O7 Cu2 N4 97.82(18) . . ?
O6 Cu2 N4 96.65(18) . . ?
O16 Cu2 N4 102.14(18) . . ?
O14 Cu3 O21 93.03(17) . . ?
O14 Cu3 O20 161.76(18) . . ?
O21 Cu3 O20 89.67(16) . . ?
O14 Cu3 O13 90.12(15) . . ?
O21 Cu3 O13 158.49(18) . . ?
O20 Cu3 O13 81.03(14) . . ?
O14 Cu3 N7 100.7(2) . . ?
O21 Cu3 N7 106.45(19) . . ?
O20 Cu3 N7 95.79(18) . . ?
O13 Cu3 N7 93.82(18) . . ?
O3 Ni1 O10 97.27(15) . . ?
O3 Ni1 O9 171.27(15) . . ?
O10 Ni1 O9 91.47(15) . . ?
O3 Ni1 O2 91.06(14) . . ?
O10 Ni1 O2 171.43(15) . . ?
O9 Ni1 O2 80.21(14) . . ?
O3 Ni1 N2 87.16(18) . . ?
O10 Ni1 N2 90.45(19) . . ?
O9 Ni1 N2 92.86(18) . . ?
O2 Ni1 N2 91.98(17) . . ?
O3 Ni1 N3 87.21(18) . . ?
O10 Ni1 N3 88.64(19) . . ?
O9 Ni1 N3 92.96(18) . . ?
O2 Ni1 N3 89.76(17) . . ?
N2 Ni1 N3 174.13(18) . . ?
O5 Ni2 O17 98.32(16) . . ?
O5 Ni2 O6 91.52(15) . . ?
O17 Ni2 O6 170.14(15) . . ?
O5 Ni2 O16 170.64(15) . . ?
O17 Ni2 O16 91.03(15) . . ?
O6 Ni2 O16 79.13(15) . . ?
O5 Ni2 N5 88.53(19) . . ?
O17 Ni2 N5 88.70(19) . . ?
O6 Ni2 N5 90.93(18) . . ?
O16 Ni2 N5 92.02(17) . . ?
O5 Ni2 N6 86.96(19) . . ?
O17 Ni2 N6 89.49(19) . . ?
O6 Ni2 N6 91.67(18) . . ?
O16 Ni2 N6 92.83(17) . . ?
N5 Ni2 N6 174.85(18) . . ?
O12 Ni3 O19 97.07(17) . . ?
O12 Ni3 O20 171.02(16) . . ?
O19 Ni3 O20 91.86(16) . . ?
O12 Ni3 N18 86.2(3) . . ?
O19 Ni3 N18 85.7(4) . . ?
O20 Ni3 N18 95.5(3) . . ?
O12 Ni3 O13 90.85(16) . . ?
O19 Ni3 O13 171.77(16) . . ?
O20 Ni3 O13 80.19(14) . . ?
N18 Ni3 O13 97.1(3) . . ?
O12 Ni3 N9 86.6(2) . . ?
O19 Ni3 N9 88.6(2) . . ?
O20 Ni3 N9 92.69(19) . . ?
N18 Ni3 N9 170.2(3) . . ?
O13 Ni3 N9 89.68(19) . . ?
O12 Ni3 N8 92.3(4) . . ?
O19 Ni3 N8 92.6(4) . . ?
O20 Ni3 N8 88.2(4) . . ?
O13 Ni3 N8 89.3(4) . . ?
N9 Ni3 N8 178.5(4) . . ?
C1 O1 Cu1 127.1(4) . . ?
C7 O2 Cu1 131.8(3) . . ?
C7 O2 Ni1 126.9(3) . . ?
Cu1 O2 Ni1 98.22(15) . . ?
C9 O3 Ni1 125.1(3) . . ?
C15 O4 C16 111.9(8) . . ?
C17 O5 Ni2 126.1(4) . . ?
C19 O6 Cu2 130.8(3) . . ?
C19 O6 Ni2 127.4(3) . . ?
Cu2 O6 Ni2 100.10(16) . . ?
C25 O7 Cu2 123.9(4) . . ?
C26 O8 Cu1 127.0(4) . . ?
C32 O9 Cu1 130.0(3) . . ?
C32 O9 Ni1 126.3(3) . . ?
Cu1 O9 Ni1 99.19(17) . . ?
C34 O10 Ni1 124.1(4) . . ?
C40 O11 C41 111.8(9) . . ?
C42 O12 Ni3 123.9(4) . . ?
C44 O13 Cu3 128.7(3) . . ?
C44 O13 Ni3 126.2(3) . . ?
Cu3 O13 Ni3 97.55(15) . . ?
C50 O14 Cu3 125.4(4) . . ?
C51 O15 Cu2 123.9(4) . . ?
C57 O16 Cu2 131.6(3) . . ?
C57 O16 Ni2 127.7(3) . . ?
Cu2 O16 Ni2 99.69(16) . . ?
C59 O17 Ni2 125.8(4) . . ?
C65 O18 C66 114.5(8) . . ?
C67 O19 Ni3 124.6(4) . . ?
C69 O20 Cu3 130.4(3) . . ?
C69 O20 Ni3 126.3(3) . . ?
Cu3 O20 Ni3 100.04(15) . . ?
C75 O21 Cu3 123.6(4) . . ?
C76 N1 C80 118.5(7) . . ?
C76 N1 Cu1 121.4(5) . . ?
C80 N1 Cu1 120.0(5) . . ?
C81 N2 C85 117.4(6) . . ?
C81 N2 Ni1 121.7(5) . . ?
C85 N2 Ni1 119.6(4) . . ?
C90 N3 C86 117.1(6) . . ?
C90 N3 Ni1 126.4(5) . . ?
C86 N3 Ni1 116.3(5) . . ?
C91 N4 C95 115.8(6) . . ?
C91 N4 Cu2 124.3(5) . . ?
C95 N4 Cu2 118.8(5) . . ?
C100 N5 C96 115.1(6) . . ?
C100 N5 Ni2 123.1(5) . . ?
C96 N5 Ni2 121.7(5) . . ?
C105 N6 C101 117.4(6) . . ?
C105 N6 Ni2 116.5(5) . . ?
C101 N6 Ni2 125.8(5) . . ?
C106 N7 C110 116.8(7) . . ?
C106 N7 Cu3 120.4(4) . . ?
C110 N7 Cu3 122.6(5) . . ?
C116 N9 C120 116.0(8) . . ?
C116 N9 Ni3 126.8(5) . . ?
C120 N9 Ni3 116.6(7) . . ?
O1 C1 C2 117.4(5) . . ?
O1 C1 C6 125.4(5) . . ?
C2 C1 C6 117.2(6) . . ?
C3 C2 C1 120.8(6) . . ?
C3 C2 H2A 119.6 . . ?
C1 C2 H2A 119.6 . . ?
C2 C3 C4 122.5(7) . . ?
C2 C3 H3A 118.7 . . ?
C4 C3 H3A 118.7 . . ?
C5 C4 C3 117.4(7) . . ?
C5 C4 H4A 121.3 . . ?
C3 C4 H4A 121.3 . . ?
C4 C5 C6 122.7(7) . . ?
C4 C5 H5A 118.6 . . ?
C6 C5 H5A 118.6 . . ?
C5 C6 C1 119.1(5) . . ?
C5 C6 C7 118.4(5) . . ?
C1 C6 C7 122.5(5) . . ?
O2 C7 C8 122.0(4) . . ?
O2 C7 C6 117.7(4) . . ?
C8 C7 C6 120.0(5) . . ?
C7 C8 C9 126.0(5) . . ?
C7 C8 H8A 117.0 . . ?
C9 C8 H8A 117.0 . . ?
O3 C9 C8 126.9(5) . . ?
O3 C9 C10 113.4(5) . . ?
C8 C9 C10 119.6(5) . . ?
C15 C10 C11 117.8(5) . . ?
C15 C10 C9 126.3(5) . . ?
C11 C10 C9 115.9(5) . . ?
C12 C11 C10 121.8(6) . . ?
C12 C11 H11A 119.1 . . ?
C10 C11 H11A 119.1 . . ?
C11 C12 C13 121.0(5) . . ?
C11 C12 H12A 119.5 . . ?
C13 C12 H12A 119.5 . . ?
C12 C13 C14 117.9(5) . . ?
C12 C13 C17 116.3(5) . . ?
C14 C13 C17 125.8(5) . . ?
C15 C14 C13 120.2(5) . . ?
C15 C14 H14A 119.9 . . ?
C13 C14 H14A 119.9 . . ?
O4 C15 C14 118.3(5) . . ?
O4 C15 C10 120.3(5) . . ?
C14 C15 C10 121.2(5) . . ?
O4 C16 H16A 109.5 . . ?
O4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O5 C17 C18 125.3(5) . . ?
O5 C17 C13 113.4(5) . . ?
C18 C17 C13 121.2(5) . . ?
C17 C18 C19 127.3(5) . . ?
C17 C18 H18A 116.4 . . ?
C19 C18 H18A 116.4 . . ?
O6 C19 C18 121.6(4) . . ?
O6 C19 C20 117.7(4) . . ?
C18 C19 C20 120.7(4) . . ?
C21 C20 C25 119.0(5) . . ?
C21 C20 C19 119.4(5) . . ?
C25 C20 C19 121.5(5) . . ?
C22 C21 C20 121.9(5) . . ?
C22 C21 H21A 119.1 . . ?
C20 C21 H21A 119.1 . . ?
C21 C22 C23 119.0(5) . . ?
C21 C22 H22A 120.5 . . ?
C23 C22 H22A 120.5 . . ?
C24 C23 C22 120.5(5) . . ?
C24 C23 H23A 119.8 . . ?
C22 C23 H23A 119.8 . . ?
C23 C24 C25 123.0(5) . . ?
C23 C24 H24A 118.5 . . ?
C25 C24 H24A 118.5 . . ?
O7 C25 C24 118.4(5) . . ?
O7 C25 C20 125.3(5) . . ?
C24 C25 C20 116.3(5) . . ?
O8 C26 C31 125.3(5) . . ?
O8 C26 C27 118.0(5) . . ?
C31 C26 C27 116.6(5) . . ?
C28 C27 C26 122.1(6) . . ?
C28 C27 H27A 119.0 . . ?
C26 C27 H27A 119.0 . . ?
C27 C28 C29 121.8(5) . . ?
C27 C28 H28A 119.1 . . ?
C29 C28 H28A 119.1 . . ?
C30 C29 C28 117.3(6) . . ?
C30 C29 H29A 121.3 . . ?
C28 C29 H29A 121.3 . . ?
C29 C30 C31 123.4(6) . . ?
C29 C30 H30A 118.3 . . ?
C31 C30 H30A 118.3 . . ?
C30 C31 C26 118.7(5) . . ?
C30 C31 C32 119.3(5) . . ?
C26 C31 C32 122.0(5) . . ?
O9 C32 C33 121.2(5) . . ?
O9 C32 C31 118.9(4) . . ?
C33 C32 C31 119.7(5) . . ?
C32 C33 C34 128.4(6) . . ?
C32 C33 H33A 115.8 . . ?
C34 C33 H33A 115.8 . . ?
O10 C34 C33 124.8(5) . . ?
O10 C34 C35 115.9(5) . . ?
C33 C34 C35 119.2(6) . . ?
C36 C35 C40 117.8(5) . . ?
C36 C35 C34 115.3(6) . . ?
C40 C35 C34 126.9(5) . . ?
C37 C36 C35 120.2(7) . . ?
C37 C36 H36A 119.9 . . ?
C35 C36 H36A 119.9 . . ?
C36 C37 C38 121.8(6) . . ?
C36 C37 H37A 119.1 . . ?
C38 C37 H37A 119.1 . . ?
C37 C38 C39 117.9(6) . . ?
C37 C38 C42 116.2(6) . . ?
C39 C38 C42 125.8(6) . . ?
C40 C39 C38 119.8(6) . . ?
C40 C39 H39A 120.1 . . ?
C38 C39 H39A 120.1 . . ?
O11 C40 C39 116.4(7) . . ?
O11 C40 C35 121.3(7) . . ?
C39 C40 C35 122.3(6) . . ?
O11 C41 H41A 109.5 . . ?
O11 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
O11 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O12 C42 C43 126.1(5) . . ?
O12 C42 C38 114.6(5) . . ?
C43 C42 C38 119.2(5) . . ?
C42 C43 C44 126.8(5) . . ?
C42 C43 H43A 116.6 . . ?
C44 C43 H43A 116.6 . . ?
O13 C44 C43 120.7(5) . . ?
O13 C44 C45 119.0(4) . . ?
C43 C44 C45 120.1(5) . . ?
C46 C45 C50 118.6(5) . . ?
C46 C45 C44 118.7(5) . . ?
C50 C45 C44 122.7(5) . . ?
C47 C46 C45 122.4(6) . . ?
C47 C46 H46A 118.8 . . ?
C45 C46 H46A 118.8 . . ?
C46 C47 C48 118.6(7) . . ?
C46 C47 H47A 120.7 . . ?
C48 C47 H47A 120.7 . . ?
C47 C48 C49 121.8(7) . . ?
C47 C48 H48A 119.1 . . ?
C49 C48 H48A 119.1 . . ?
C48 C49 C50 121.6(7) . . ?
C48 C49 H49A 119.2 . . ?
C50 C49 H49A 119.2 . . ?
O14 C50 C49 117.7(6) . . ?
O14 C50 C45 125.0(6) . . ?
C49 C50 C45 117.0(6) . . ?
O15 C51 C52 119.6(5) . . ?
O15 C51 C56 124.0(5) . . ?
C52 C51 C56 116.2(5) . . ?
C53 C52 C51 123.4(6) . . ?
C53 C52 H52A 118.3 . . ?
C51 C52 H52A 118.3 . . ?
C52 C53 C54 120.1(6) . . ?
C52 C53 H53A 120.0 . . ?
C54 C53 H53A 120.0 . . ?
C55 C54 C53 119.7(6) . . ?
C55 C54 H54A 120.2 . . ?
C53 C54 H54A 120.2 . . ?
C54 C55 C56 122.1(6) . . ?
C54 C55 H55A 119.0 . . ?
C56 C55 H55A 119.0 . . ?
C55 C56 C51 118.4(5) . . ?
C55 C56 C57 118.9(5) . . ?
C51 C56 C57 122.6(5) . . ?
O16 C57 C58 121.6(4) . . ?
O16 C57 C56 117.1(4) . . ?
C58 C57 C56 121.2(5) . . ?
C57 C58 C59 126.5(5) . . ?
C57 C58 H58A 116.8 . . ?
C59 C58 H58A 116.8 . . ?
O17 C59 C58 127.0(5) . . ?
O17 C59 C60 113.0(5) . . ?
C58 C59 C60 120.0(5) . . ?
C61 C60 C65 118.2(5) . . ?
C61 C60 C59 115.8(5) . . ?
C65 C60 C59 125.8(5) . . ?
C62 C61 C60 120.9(6) . . ?
C62 C61 H61A 119.5 . . ?
C60 C61 H61A 119.5 . . ?
C61 C62 C63 121.6(6) . . ?
C61 C62 H62A 119.2 . . ?
C63 C62 H62A 119.2 . . ?
C62 C63 C64 117.1(5) . . ?
C62 C63 C67 118.3(5) . . ?
C64 C63 C67 124.6(5) . . ?
C65 C64 C63 121.3(6) . . ?
C65 C64 H64A 119.4 . . ?
C63 C64 H64A 119.4 . . ?
C64 C65 O18 120.0(6) . . ?
C64 C65 C60 120.5(5) . . ?
O18 C65 C60 119.5(6) . . ?
O18 C66 H66A 109.5 . . ?
O18 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
O18 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
O19 C67 C68 126.7(5) . . ?
O19 C67 C63 114.0(5) . . ?
C68 C67 C63 119.2(5) . . ?
C69 C68 C67 127.2(5) . . ?
C69 C68 H68A 116.4 . . ?
C67 C68 H68A 116.4 . . ?
O20 C69 C68 122.2(4) . . ?
O20 C69 C70 117.0(4) . . ?
C68 C69 C70 120.6(5) . . ?
C71 C70 C75 119.4(5) . . ?
C71 C70 C69 118.0(5) . . ?
C75 C70 C69 122.6(5) . . ?
C72 C71 C70 121.4(6) . . ?
C72 C71 H71A 119.3 . . ?
C70 C71 H71A 119.3 . . ?
C73 C72 C71 118.1(6) . . ?
C73 C72 H72A 121.0 . . ?
C71 C72 H72A 121.0 . . ?
C74 C73 C72 121.9(6) . . ?
C74 C73 H73A 119.1 . . ?
C72 C73 H73A 119.1 . . ?
C73 C74 C75 121.7(6) . . ?
C73 C74 H74A 119.2 . . ?
C75 C74 H74A 119.2 . . ?
O21 C75 C74 118.2(5) . . ?
O21 C75 C70 124.4(5) . . ?
C74 C75 C70 117.1(5) . . ?
N1 C76 C77 121.5(9) . . ?
N1 C76 H76A 119.2 . . ?
C77 C76 H76A 119.2 . . ?
C78 C77 C76 118.3(10) . . ?
C78 C77 H77A 120.8 . . ?
C76 C77 H77A 120.8 . . ?
C79 C78 C77 119.5(9) . . ?
C79 C78 H78A 120.2 . . ?
C77 C78 H78A 120.2 . . ?
C78 C79 C80 120.0(10) . . ?
C78 C79 H79A 120.0 . . ?
C80 C79 H79A 120.0 . . ?
N1 C80 C79 122.1(9) . . ?
N1 C80 H80A 118.9 . . ?
C79 C80 H80A 118.9 . . ?
N2 C81 C82 122.5(7) . . ?
N2 C81 H81A 118.7 . . ?
C82 C81 H81A 118.7 . . ?
C83 C82 C81 118.2(7) . . ?
C83 C82 H82A 120.9 . . ?
C81 C82 H82A 120.9 . . ?
C82 C83 C84 120.7(8) . . ?
C82 C83 H83A 119.7 . . ?
C84 C83 H83A 119.7 . . ?
C85 C84 C83 117.0(8) . . ?
C85 C84 H84A 121.5 . . ?
C83 C84 H84A 121.5 . . ?
N2 C85 C84 124.2(7) . . ?
N2 C85 H85A 117.9 . . ?
C84 C85 H85A 117.9 . . ?
N3 C86 C87 122.9(8) . . ?
N3 C86 H86A 118.5 . . ?
C87 C86 H86A 118.5 . . ?
C88 C87 C86 118.8(9) . . ?
C88 C87 H87A 120.6 . . ?
C86 C87 H87A 120.6 . . ?
C87 C88 C89 118.4(10) . . ?
C87 C88 H88A 120.8 . . ?
C89 C88 H88A 120.8 . . ?
C90 C89 C88 118.4(11) . . ?
C90 C89 H89A 120.8 . . ?
C88 C89 H89A 120.8 . . ?
N3 C90 C89 124.2(9) . . ?
N3 C90 H90A 117.9 . . ?
C89 C90 H90A 117.9 . . ?
N4 C91 C92 124.1(7) . . ?
N4 C91 H91A 118.0 . . ?
C92 C91 H91A 118.0 . . ?
C93 C92 C91 118.3(8) . . ?
C93 C92 H92A 120.8 . . ?
C91 C92 H92A 120.8 . . ?
C94 C93 C92 119.0(8) . . ?
C94 C93 H93A 120.5 . . ?
C92 C93 H93A 120.5 . . ?
C93 C94 C95 119.1(8) . . ?
C93 C94 H94A 120.5 . . ?
C95 C94 H94A 120.5 . . ?
N4 C95 C94 123.5(7) . . ?
N4 C95 H95A 118.3 . . ?
C94 C95 H95A 118.3 . . ?
N5 C96 C97 124.7(7) . . ?
N5 C96 H96A 117.7 . . ?
C97 C96 H96A 117.7 . . ?
C96 C97 C98 118.6(8) . . ?
C96 C97 H97A 120.7 . . ?
C98 C97 H97A 120.7 . . ?
C99 C98 C97 118.8(8) . . ?
C99 C98 H98A 120.6 . . ?
C97 C98 H98A 120.6 . . ?
C98 C99 C100 119.9(8) . . ?
C98 C99 H99A 120.1 . . ?
C100 C99 H99A 120.1 . . ?
N5 C100 C99 122.9(7) . . ?
N5 C100 H10A 118.5 . . ?
C99 C100 H10A 118.5 . . ?
N6 C101 C102 122.9(7) . . ?
N6 C101 H10B 118.6 . . ?
C102 C101 H10B 118.6 . . ?
C101 C102 C103 119.6(9) . . ?
C101 C102 H10C 120.2 . . ?
C103 C102 H10C 120.2 . . ?
C104 C103 C102 116.5(9) . . ?
C104 C103 H10D 121.7 . . ?
C102 C103 H10D 121.7 . . ?
C105 C104 C103 120.6(9) . . ?
C105 C104 H10E 119.7 . . ?
C103 C104 H10E 119.7 . . ?
N6 C105 C104 122.9(8) . . ?
N6 C105 H10F 118.5 . . ?
C104 C105 H10F 118.5 . . ?
N7 C106 C107 124.4(7) . . ?
N7 C106 H10G 117.8 . . ?
C107 C106 H10G 117.8 . . ?
C108 C107 C106 118.1(8) . . ?
C108 C107 H10H 120.9 . . ?
C106 C107 H10H 120.9 . . ?
C107 C108 C109 119.1(8) . . ?
C107 C108 H10I 120.4 . . ?
C109 C108 H10I 120.4 . . ?
C110 C109 C108 118.9(7) . . ?
C110 C109 H10J 120.6 . . ?
C108 C109 H10J 120.6 . . ?
N7 C110 C109 122.4(8) . . ?
N7 C110 H11B 118.8 . . ?
C109 C110 H11B 118.8 . . ?
C111 N8 C115 120.0 . . ?
C111 N8 Ni3 120.4(7) . . ?
C115 N8 Ni3 119.5(7) . . ?
C112 C111 N8 120.0 . . ?
C112 C111 H11C 120.0 . . ?
N8 C111 H11C 120.0 . . ?
C111 C112 C113 120.0 . . ?
C111 C112 H11D 120.0 . . ?
C113 C112 H11D 120.0 . . ?
C114 C113 C112 120.0 . . ?
C114 C113 H11E 120.0 . . ?
C112 C113 H11E 120.0 . . ?
C113 C114 C115 120.0 . . ?
C113 C114 H11F 120.0 . . ?
C115 C114 H11F 120.0 . . ?
C114 C115 N8 120.0 . . ?
C114 C115 H11G 120.0 . . ?
N8 C115 H11G 120.0 . . ?
C121 N18 C125 120.0 . . ?
C121 N18 Ni3 125.6(6) . . ?
C125 N18 Ni3 114.3(6) . . ?
N18 C121 C122 120.0 . . ?
N18 C121 H12D 120.0 . . ?
C122 C121 H12D 120.0 . . ?
C123 C122 C121 120.0 . . ?
C123 C122 H12E 120.0 . . ?
C121 C122 H12E 120.0 . . ?
C122 C123 C124 120.0 . . ?
C122 C123 H12F 120.0 . . ?
C124 C123 H12F 120.0 . . ?
C125 C124 C123 120.0 . . ?
C125 C124 H12G 120.0 . . ?
C123 C124 H12G 120.0 . . ?
C124 C125 N18 120.0 . . ?
C124 C125 H12H 120.0 . . ?
N18 C125 H12H 120.0 . . ?
N9 C116 C117 123.7(9) . . ?
N9 C116 H11H 118.2 . . ?
C117 C116 H11H 118.2 . . ?
C118 C117 C116 118.5(12) . . ?
C118 C117 H11I 120.8 . . ?
C116 C117 H11I 120.8 . . ?
C119 C118 C117 118.2(11) . . ?
C119 C118 H11J 120.9 . . ?
C117 C118 H11J 120.9 . . ?
C120 C119 C118 119.2(10) . . ?
C120 C119 H11K 120.4 . . ?
C118 C119 H11K 120.4 . . ?
N9 C120 C119 124.5(11) . . ?
N9 C120 H12B 117.8 . . ?
C119 C120 H12B 117.8 . . ?
C1S N1S C5S 120.0 . . ?
N1S C1S C2S 120.0 . . ?
N1S C1S H1SA 120.0 . . ?
C2S C1S H1SA 120.0 . . ?
C3S C2S C1S 120.0 . . ?
C3S C2S H2SA 120.0 . . ?
C1S C2S H2SA 120.0 . . ?
C4S C3S C2S 120.0 . . ?
C4S C3S H3SA 120.0 . . ?
C2S C3S H3SA 120.0 . . ?
C3S C4S C5S 120.0 . . ?
C3S C4S H4SA 120.0 . . ?
C5S C4S H4SA 120.0 . . ?
C4S C5S N1S 120.0 . . ?
C4S C5S H5SA 120.0 . . ?
N1S C5S H5SA 120.0 . . ?
C6S N2S C10S 120.0(13) . . ?
C7S C6S N2S 118.9(7) . . ?
C7S C6S H6SA 120.6 . . ?
N2S C6S H6SA 120.6 . . ?
C6S C7S C8S 121.7(7) . . ?
C6S C7S H7SA 119.2 . . ?
C8S C7S H7SA 119.2 . . ?
C7S C8S C9S 120.0 . . ?
C7S C8S H8SA 120.0 . . ?
C9S C8S H8SA 120.0 . . ?
C8S C9S C10S 120.0 . . ?
C8S C9S H9SA 120.0 . . ?
C10S C9S H9SA 120.0 . . ?
C9S C10S N2S 119.4(15) . . ?
C9S C10S H10K 120.3 . . ?
N2S C10S H10K 120.3 . . ?
C11S N3S C15S 120.0 . . ?
N3S C11S C12S 120.0 . . ?
N3S C11S H11L 120.0 . . ?
C12S C11S H11L 120.0 . . ?
C11S C12S C13S 120.0 . . ?
C11S C12S H12C 120.0 . . ?
C13S C12S H12C 120.0 . . ?
C14S C13S C12S 120.0 . . ?
C14S C13S H13A 120.0 . . ?
C12S C13S H13A 120.0 . . ?
C15S C14S C13S 120.0 . . ?
C15S C14S H14B 120.0 . . ?
C13S C14S H14B 120.0 . . ?
C14S C15S N3S 120.0 . . ?
C14S C15S H15A 120.0 . . ?
N3S C15S H15A 120.0 . . ?

_refine_diff_density_max         3.459
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.113

_shelxl_version_number           2014-3




_exptl_crystal_preparation       'Magnetic properties'
