# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2021

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 2040493'
loop_
_audit_author_name
_audit_author_address
Jing
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2020-12-01 deposited with the CCDC.	2021-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C62 H48 N10 Ni O12'
_chemical_formula_weight         1183.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.389(5)
_cell_length_b                   25.046(5)
_cell_length_c                   10.134(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 106.839(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     2766.8(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1177
_cell_measurement_theta_min      1.87
_cell_measurement_theta_max      25.02

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1228
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.9388
_exptl_absorpt_correction_T_max  0.9546
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15767
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_sigmaI/netI    0.0918
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4854
_reflns_number_gt                2807
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4854
_refine_ls_number_parameters     385
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_gt           0.0627
_refine_ls_wR_factor_ref         0.1936
_refine_ls_wR_factor_gt          0.1582
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.008
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.0000 0.5000 0.0326(3) Uani 1 2 d S . .
N1] N -0.4922(3) 0.46675(15) 0.8083(4) 0.0353(10) Uani 1 1 d . . .
O1 O -0.4230(3) 0.29156(15) 0.4935(5) 0.0647(12) Uani 1 1 d . . .
C1 C -0.3989(4) 0.47318(19) 0.7542(5) 0.0381(12) Uani 1 1 d . . .
H1A H -0.3320 0.4933 0.8034 0.046 Uiso 1 1 calc R . .
N2 N -0.3764(3) 0.37161(16) 0.4226(4) 0.0404(10) Uani 1 1 d . . .
H2A H -0.3224 0.3907 0.4002 0.048 Uiso 1 1 calc R . .
O2 O 0.1778(4) 0.25439(17) 0.3737(4) 0.0658(12) Uani 1 1 d U . .
C2 C -0.3964(4) 0.45176(19) 0.6304(5) 0.0385(12) Uani 1 1 d . . .
H2B H -0.3296 0.4582 0.5973 0.046 Uiso 1 1 calc R . .
N3 N 0.2249(4) 0.25250(16) 0.6049(4) 0.0418(11) Uani 1 1 d . . .
H3A H 0.1980 0.2555 0.6756 0.050 Uiso 1 1 calc R . .
C3 C -0.4931(4) 0.42043(18) 0.5543(5) 0.0344(11) Uani 1 1 d . . .
O3 O 0.1203(5) 0.0502(2) 0.2266(7) 0.124(2) Uani 1 1 d U . .
N4 N 0.4450(3) 0.07912(15) 0.5419(4) 0.0349(10) Uani 1 1 d . . .
C4 C -0.5896(4) 0.4138(2) 0.6100(5) 0.0422(13) Uani 1 1 d . . .
H4A H -0.6569 0.3932 0.5639 0.051 Uiso 1 1 calc R . .
O4 O -0.0681(6) 0.0429(3) 0.1036(9) 0.182(3) Uani 1 1 d U . .
O5 O 0.3148(3) -0.01888(13) 0.4236(4) 0.0391(8) Uani 1 1 d U . .
C5 C -0.5864(4) 0.4377(2) 0.7339(6) 0.0441(13) Uani 1 1 d . . .
H5A H -0.6536 0.4333 0.7674 0.053 Uiso 1 1 calc R . .
N5 N 0.0294(6) 0.0241(3) 0.1832(9) 0.119(3) Uani 1 1 d U . .
O6 O 0.2971(3) -0.04412(15) 0.2070(4) 0.0564(10) Uani 1 1 d U . .
C6 C -0.4926(4) 0.3953(2) 0.4191(5) 0.0455(13) Uani 1 1 d . . .
H6A H -0.5557 0.3680 0.3951 0.055 Uiso 1 1 calc R . .
H6B H -0.5130 0.4223 0.3475 0.055 Uiso 1 1 calc R . .
C7 C -0.3507(5) 0.3208(2) 0.4599(6) 0.0436(13) Uani 1 1 d . . .
C8 C -0.2237(5) 0.3026(2) 0.4620(5) 0.0424(13) Uani 1 1 d . . .
C9 C -0.2028(5) 0.25047(19) 0.4171(5) 0.0416(12) Uani 1 1 d . . .
C10 C -0.0807(5) 0.23557(19) 0.4207(5) 0.0413(12) Uani 1 1 d . . .
C11 C 0.0166(4) 0.2721(2) 0.4749(5) 0.0412(13) Uani 1 1 d . . .
C12 C -0.0067(5) 0.3206(2) 0.5221(6) 0.0503(15) Uani 1 1 d . . .
H12A H 0.0580 0.3436 0.5620 0.060 Uiso 1 1 calc R . .
C13 C -0.1284(5) 0.3364(2) 0.5111(6) 0.0495(14) Uani 1 1 d . . .
H13A H -0.1431 0.3706 0.5380 0.059 Uiso 1 1 calc R . .
C14 C -0.2969(5) 0.2126(2) 0.3667(6) 0.0519(15) Uani 1 1 d . . .
H14A H -0.3773 0.2221 0.3606 0.062 Uiso 1 1 calc R . .
C15 C -0.0605(6) 0.1839(2) 0.3755(6) 0.0573(16) Uani 1 1 d . . .
H15A H 0.0181 0.1739 0.3751 0.069 Uiso 1 1 calc R . .
C16 C -0.1552(7) 0.1487(2) 0.3323(7) 0.0716(19) Uani 1 1 d . . .
H16A H -0.1400 0.1144 0.3059 0.086 Uiso 1 1 calc R . .
C17 C -0.2746(6) 0.1634(2) 0.3271(7) 0.0673(18) Uani 1 1 d . . .
H17A H -0.3385 0.1392 0.2964 0.081 Uiso 1 1 calc R . .
C18 C 0.1472(5) 0.2585(2) 0.4800(6) 0.0425(13) Uani 1 1 d . . .
C19 C 0.3538(4) 0.24114(19) 0.6258(6) 0.0457(13) Uani 1 1 d . . .
H19A H 0.3978 0.2482 0.7214 0.055 Uiso 1 1 calc R . .
H19B H 0.3850 0.2655 0.5695 0.055 Uiso 1 1 calc R . .
C20 C 0.3814(4) 0.18456(19) 0.5915(5) 0.0361(12) Uani 1 1 d . . .
C21 C 0.4972(4) 0.17190(19) 0.5817(5) 0.0395(12) Uani 1 1 d . . .
H21A H 0.5561 0.1985 0.5912 0.047 Uiso 1 1 calc R . .
C22 C 0.5245(4) 0.1200(2) 0.5579(5) 0.0395(12) Uani 1 1 d . . .
H22A H 0.6030 0.1126 0.5526 0.047 Uiso 1 1 calc R . .
C23 C 0.3334(4) 0.0923(2) 0.5477(5) 0.0387(12) Uani 1 1 d . . .
H23A H 0.2750 0.0653 0.5347 0.046 Uiso 1 1 calc R . .
C24 C 0.2987(4) 0.14310(19) 0.5716(5) 0.0408(13) Uani 1 1 d . . .
H24A H 0.2190 0.1495 0.5743 0.049 Uiso 1 1 calc R . .
C25 C -0.0043(7) -0.1344(3) 0.2875(8) 0.095(3) Uani 1 1 d . . .
H25A H -0.0124 -0.1697 0.3115 0.114 Uiso 1 1 calc R . .
C26 C -0.1039(8) -0.1058(5) 0.2240(9) 0.107(3) Uani 1 1 d . . .
H26A H -0.1806 -0.1220 0.2038 0.128 Uiso 1 1 calc R . .
C27 C -0.0965(6) -0.0543(4) 0.1883(10) 0.099(3) Uani 1 1 d . . .
H27A H -0.1661 -0.0346 0.1443 0.119 Uiso 1 1 calc R . .
C28 C 0.1095(6) -0.1115(3) 0.3172(7) 0.078(2) Uani 1 1 d . . .
H28A H 0.1779 -0.1323 0.3588 0.094 Uiso 1 1 calc R . .
C29 C 0.1270(5) -0.0579(2) 0.2872(6) 0.0485(14) Uani 1 1 d . . .
C30 C 0.0231(6) -0.0313(3) 0.2212(8) 0.076(2) Uani 1 1 d . . .
C31 C 0.2565(4) -0.03735(19) 0.3059(6) 0.0393(12) 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
Ni1 O5 2.080(3) . ?
Ni1 O5 2.080(3) 3_656 ?
Ni1 N1] 2.139(4) 2_546 ?
Ni1 N1] 2.139(4) 4_665 ?
Ni1 N4 2.157(4) . ?
Ni1 N4 2.158(4) 3_656 ?
N1] C5 1.334(6) . ?
N1] C1 1.338(6) . ?
N1] Ni1 2.139(4) 2_556 ?
O1 C7 1.223(6) . ?
C1 C2 1.373(7) . ?
N2 C7 1.335(6) . ?
N2 C6 1.441(6) . ?
O2 C18 1.228(6) . ?
C2 C3 1.389(7) . ?
N3 C18 1.327(6) . ?
N3 C19 1.449(6) . ?
C3 C4 1.383(6) . ?
C3 C6 1.510(7) . ?
O3 N5 1.196(8) . ?
N4 C23 1.330(5) . ?
N4 C22 1.345(6) . ?
C4 C5 1.382(7) . ?
O4 N5 1.259(8) . ?
O5 C31 1.273(6) . ?
N5 C30 1.447(10) . ?
O6 C31 1.230(6) . ?
C7 C8 1.510(7) . ?
C8 C13 1.353(7) . ?
C8 C9 1.425(7) . ?
C9 C14 1.411(7) . ?
C9 C10 1.430(7) . ?
C10 C15 1.413(7) . ?
C10 C11 1.420(7) . ?
C11 C12 1.359(7) . ?
C11 C18 1.512(7) . ?
C12 C13 1.414(7) . ?
C14 C17 1.344(8) . ?
C15 C16 1.364(8) . ?
C16 C17 1.395(8) . ?
C19 C20 1.513(6) . ?
C20 C24 1.377(6) . ?
C20 C21 1.388(6) . ?
C21 C22 1.374(7) . ?
C23 C24 1.376(6) . ?
C25 C26 1.338(11) . ?
C25 C28 1.368(9) . ?
C26 C27 1.350(11) . ?
C27 C30 1.426(9) . ?
C28 C29 1.404(8) . ?
C29 C30 1.354(8) . ?
C29 C31 1.521(7) . ?

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
O5 Ni1 O5 180.00(7) . 3_656 ?
O5 Ni1 N1] 86.85(13) . 2_546 ?
O5 Ni1 N1] 93.15(13) 3_656 2_546 ?
O5 Ni1 N1] 93.15(13) . 4_665 ?
O5 Ni1 N1] 86.84(14) 3_656 4_665 ?
N1] Ni1 N1] 180.0 2_546 4_665 ?
O5 Ni1 N4 87.76(13) . . ?
O5 Ni1 N4 92.24(13) 3_656 . ?
N1] Ni1 N4 95.03(14) 2_546 . ?
N1] Ni1 N4 84.97(14) 4_665 . ?
O5 Ni1 N4 92.24(13) . 3_656 ?
O5 Ni1 N4 87.76(13) 3_656 3_656 ?
N1] Ni1 N4 84.97(14) 2_546 3_656 ?
N1] Ni1 N4 95.03(14) 4_665 3_656 ?
N4 Ni1 N4 180.00(8) . 3_656 ?
C5 N1] C1 116.0(4) . . ?
C5 N1] Ni1 119.1(3) . 2_556 ?
C1 N1] Ni1 124.9(3) . 2_556 ?
N1] C1 C2 123.8(5) . . ?
C7 N2 C6 121.6(4) . . ?
C1 C2 C3 120.3(5) . . ?
C18 N3 C19 121.9(4) . . ?
C4 C3 C2 115.9(5) . . ?
C4 C3 C6 122.2(5) . . ?
C2 C3 C6 121.9(4) . . ?
C23 N4 C22 115.2(4) . . ?
C23 N4 Ni1 124.9(3) . . ?
C22 N4 Ni1 119.9(3) . . ?
C5 C4 C3 120.3(5) . . ?
C31 O5 Ni1 129.0(3) . . ?
N1] C5 C4 123.7(5) . . ?
O3 N5 O4 122.7(8) . . ?
O3 N5 C30 122.1(7) . . ?
O4 N5 C30 115.2(7) . . ?
N2 C6 C3 113.2(4) . . ?
O1 C7 N2 122.6(5) . . ?
O1 C7 C8 122.3(5) . . ?
N2 C7 C8 115.1(5) . . ?
C13 C8 C9 120.0(5) . . ?
C13 C8 C7 118.6(5) . . ?
C9 C8 C7 121.4(5) . . ?
C14 C9 C8 123.5(5) . . ?
C14 C9 C10 117.7(5) . . ?
C8 C9 C10 118.8(5) . . ?
C15 C10 C11 122.2(5) . . ?
C15 C10 C9 118.7(5) . . ?
C11 C10 C9 119.1(4) . . ?
C12 C11 C10 120.1(5) . . ?
C12 C11 C18 118.7(5) . . ?
C10 C11 C18 121.1(4) . . ?
C11 C12 C13 120.6(5) . . ?
C8 C13 C12 121.2(5) . . ?
C17 C14 C9 122.3(6) . . ?
C16 C15 C10 120.5(5) . . ?
C15 C16 C17 120.8(5) . . ?
C14 C17 C16 119.9(6) . . ?
O2 C18 N3 123.1(5) . . ?
O2 C18 C11 121.0(5) . . ?
N3 C18 C11 115.8(4) . . ?
N3 C19 C20 114.8(4) . . ?
C24 C20 C21 116.2(4) . . ?
C24 C20 C19 124.2(4) . . ?
C21 C20 C19 119.7(4) . . ?
C22 C21 C20 119.8(4) . . ?
N4 C22 C21 124.2(4) . . ?
N4 C23 C24 124.3(4) . . ?
C23 C24 C20 120.3(4) . . ?
C26 C25 C28 120.0(8) . . ?
C25 C26 C27 122.0(8) . . ?
C26 C27 C30 116.9(8) . . ?
C25 C28 C29 122.5(7) . . ?
C30 C29 C28 114.8(6) . . ?
C30 C29 C31 124.9(5) . . ?
C28 C29 C31 119.3(5) . . ?
C29 C30 C27 123.8(7) . . ?
C29 C30 N5 120.0(6) . . ?
C27 C30 N5 116.2(7) . . ?
O6 C31 O5 126.6(5) . . ?
O6 C31 C29 115.6(5) . . ?
O5 C31 C29 117.6(5) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.072
####################################################################### 
# 
# 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_01
_database_code_depnum_ccdc_archive 'CCDC 2040497'
loop_
_audit_author_name
_audit_author_address
Jing
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2020-12-01 deposited with the CCDC.	2021-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C62 H60 N8 Ni2 O13'
_chemical_formula_weight         1242.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   27.1381(15)
_cell_length_b                   9.5460(5)
_cell_length_c                   26.1291(14)
_cell_angle_alpha                90
_cell_angle_beta                 119.788(2)
_cell_angle_gamma                90
_cell_volume                     5874.6(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4980
_cell_measurement_theta_min      1.729
_cell_measurement_theta_max      28.071

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_F_000             2592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.713
_shelx_estimated_absorpt_T_min   0.901
_shelx_estimated_absorpt_T_max   0.926
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20719
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.729
_diffrn_reflns_theta_max         28.071
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7120
_reflns_number_gt                5059
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0538P)²+3.2797P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7120
_refine_ls_number_parameters     392
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.1107
_refine_ls_wR_factor_gt          0.0985
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_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
Ni1 Ni 0.88744(2) 0.38727(3) 0.60262(2) 0.03562(9) Uani 1 1 d . . . . .
O1 O 0.90524(7) 0.51949(17) 0.67493(6) 0.0488(4) Uani 1 1 d . . . . .
C1 C 0.85438(10) 0.5636(2) 0.64670(10) 0.0403(5) Uani 1 1 d . . . . .
N1 N 0.90832(8) 0.52755(19) 0.55633(8) 0.0412(4) Uani 1 1 d . . . . .
O1W O 1.0000 0.7076(4) 0.7500 0.166(2) Uani 1 2 d S T P . .
O2 O 0.82116(6) 0.51594(16) 0.59648(6) 0.0427(4) Uani 1 1 d . . . . .
C2 C 0.82693(9) 1.1774(2) 0.56120(10) 0.0395(5) Uani 1 1 d . . . . .
N2 N 0.96267(7) 0.27800(19) 0.64007(7) 0.0381(4) Uani 1 1 d . . . . .
O3 O 0.84415(6) 1.19976(16) 0.61531(7) 0.0425(4) Uani 1 1 d . . . . .
N3 N 0.88951(8) 0.90886(19) 0.41134(8) 0.0426(4) Uani 1 1 d . . . . .
H3C H 0.8601 0.8847 0.3787 0.051 Uiso 1 1 d R U . . .
C3 C 0.93453(10) 0.8061(2) 0.44201(10) 0.0445(5) Uani 1 1 d . . . . .
H3A H 0.9700 0.8541 0.4647 0.053 Uiso 1 1 d R U . . .
H3B H 0.9374 0.7498 0.4131 0.053 Uiso 1 1 d R U . . .
O4 O 0.84372(7) 1.25574(16) 0.53396(6) 0.0452(4) Uani 1 1 d . . . . .
N4 N 0.66048(7) 1.40913(19) 0.28383(8) 0.0418(4) Uani 1 1 d . . . . .
H4A H 0.6673 1.3904 0.3190 0.050 Uiso 1 1 d R U . . .
C4 C 0.85216(9) 1.2497(2) 0.36359(9) 0.0367(5) Uani 1 1 d . . . . .
O5 O 0.93012(7) 1.0794(2) 0.47941(8) 0.0635(5) Uani 1 1 d . . . . .
C5 C 0.74287(9) 1.1819(2) 0.34097(9) 0.0394(5) Uani 1 1 d . . . . .
H5A H 0.7056 1.1586 0.3340 0.047 Uiso 1 1 d R U . . .
O6 O 0.68982(8) 1.3911(2) 0.21682(7) 0.0640(5) Uani 1 1 d . . . . .
C7 C 0.74919(9) 1.2936(2) 0.31260(8) 0.0356(5) Uani 1 1 d . . . . .
C9 C 0.84297(9) 1.1311(2) 0.39071(9) 0.0371(5) Uani 1 1 d . . . . .
C10 C 0.80484(9) 1.3335(2) 0.32410(9) 0.0370(5) Uani 1 1 d . . . . .
C20 C 0.89177(9) 1.0392(2) 0.43146(9) 0.0404(5) Uani 1 1 d . . . . .
C21 C 1.05470(9) 0.2463(2) 0.72408(9) 0.0401(5) Uani 1 1 d . . . . .
H21A H 1.0850 0.2848 0.7599 0.048 Uiso 1 1 d R U . . .
C22 C 0.92452(9) 0.7096(2) 0.48177(9) 0.0390(5) Uani 1 1 d . . . . .
C23 C 0.78952(9) 1.0999(2) 0.38005(9) 0.0413(5) Uani 1 1 d . . . . .
H23A H 0.7836 1.0209 0.3991 0.050 Uiso 1 1 d R U . . .
C24 C 1.05888(9) 0.1125(2) 0.70662(9) 0.0376(5) Uani 1 1 d . . . . .
C25 C 0.60865(9) 1.4830(2) 0.24328(11) 0.0502(6) Uani 1 1 d . . . . .
H25A H 0.5880 1.5029 0.2635 0.075 Uiso 1 1 d R U . . .
H25B H 0.6174 1.5692 0.2305 0.075 Uiso 1 1 d R U . . .
C26 C 0.90715(10) 1.2865(3) 0.37354(11) 0.0496(6) Uani 1 1 d . . . . .
H26A H 0.9394 1.2296 0.3988 0.060 Uiso 1 1 d R U . . .
C27 C 0.69762(9) 1.3697(2) 0.26675(9) 0.0415(5) Uani 1 1 d . . . . .
C28 C 0.96735(10) 0.1503(3) 0.62202(10) 0.0542(7) Uani 1 1 d . . . . .
H28A H 0.9368 0.1161 0.5853 0.065 Uiso 1 1 d R U . . .
C29 C 0.92599(12) 0.7562(3) 0.53238(11) 0.0558(7) Uani 1 1 d . . . . .
H29A H 0.9324 0.8538 0.5425 0.067 Uiso 1 1 d R U . . .
C30 C 0.80861(11) 0.8611(2) 0.59796(11) 0.0492(6) Uani 1 1 d . . . . .
H30A H 0.8173 0.8015 0.5739 0.059 Uiso 1 1 d R U . . .
H30B H 0.8430 0.9081 0.6254 0.059 Uiso 1 1 d R U . . .
C31 C 0.78848(12) 0.7695(3) 0.63128(13) 0.0590(7) Uani 1 1 d . . . . .
H31A H 0.7557 0.7170 0.6038 0.071 Uiso 1 1 d R U . . .
H31B H 0.7771 0.8293 0.6531 0.071 Uiso 1 1 d R U . . .
C32 C 0.91514(18) 0.5707(3) 0.47082(14) 0.0871(12) Uani 1 1 d . . . . .
H32A H 0.9149 0.5323 0.4367 0.104 Uiso 1 1 d R U . . .
C33 C 1.00680(9) 0.3246(2) 0.69006(10) 0.0408(5) Uani 1 1 d . . . . .
H33A H 1.0051 0.4176 0.7031 0.049 Uiso 1 1 d R U . . .
C34 C 0.78644(13) 1.0614(3) 0.52653(12) 0.0576(7) Uani 1 1 d . . . . .
H34A H 0.7574(13) 1.105(3) 0.4962(13) 0.069(9) Uiso 1 1 d . . . . .
H34B H 0.8108(14) 1.001(4) 0.5149(15) 0.101(12) Uiso 1 1 d . . . . .
C35 C 1.01399(10) 0.0654(3) 0.65370(11) 0.0555(7) Uani 1 1 d . . . . .
H35A H 1.0154 -0.0263 0.6394 0.067 Uiso 1 1 d R U . . .
C36 C 0.81470(11) 1.4549(3) 0.29914(10) 0.0503(6) Uani 1 1 d . . . . .
H36A H 0.7837 1.5147 0.2736 0.060 Uiso 1 1 d R U . . .
C37 C 0.91462(12) 1.4019(3) 0.34718(12) 0.0617(7) Uani 1 1 d . . . . .
H37A H 0.9517 1.4241 0.3535 0.074 Uiso 1 1 d R U . . .
C38 C 0.91836(12) 0.6630(3) 0.56834(11) 0.0528(6) Uani 1 1 d . . . . .
H38A H 0.9215 0.6977 0.6043 0.063 Uiso 1 1 d R U . . .
C39 C 0.76542(10) 0.9692(3) 0.55841(12) 0.0564(7) Uani 1 1 d . . . . .
H39A H 0.7558 1.0274 0.5821 0.068 Uiso 1 1 d R U . . .
H39B H 0.7315 0.9224 0.5299 0.068 Uiso 1 1 d R U . . .
C40 C 0.86820(12) 1.4881(3) 0.31076(12) 0.0621(7) Uani 1 1 d . . . . .
H40A H 0.8745 1.5706 0.2938 0.075 Uiso 1 1 d R U . . .
C41 C 0.83352(13) 0.6706(3) 0.67438(11) 0.0562(7) Uani 1 1 d . . . . .
H41A H 0.8654 0.7238 0.7029 0.067 Uiso 1 1 d R U . . .
H41B H 0.8181 0.6208 0.6952 0.067 Uiso 1 1 d R U . . .
C42 C 0.90701(17) 0.4828(3) 0.50795(14) 0.0854(11) Uani 1 1 d . . . . .
H42A H 0.8981 0.3862 0.4970 0.102 Uiso 1 1 d 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 O4 2.0220(15) 1_545 ?
Ni1 N2 2.0563(18) . ?
Ni1 N1 2.0635(18) . ?
Ni1 O2 2.1173(15) . ?
Ni1 O1 2.1188(16) . ?
Ni1 O3 2.2542(15) 1_545 ?
Ni1 C1 2.448(2) . ?
Ni1 C2 2.473(2) 1_545 ?
O1 C1 1.271(3) . ?
C1 O2 1.251(3) . ?
C1 C41 1.514(3) . ?
N1 C42 1.318(3) . ?
N1 C38 1.326(3) . ?
C2 O4 1.263(3) . ?
C2 O3 1.267(3) . ?
C2 C34 1.505(3) . ?
C2 Ni1 2.473(2) 1_565 ?
N2 C28 1.336(3) . ?
N2 C33 1.336(3) . ?
O3 Ni1 2.2543(15) 1_565 ?
N3 C20 1.340(3) . ?
N3 C3 1.457(3) . ?
C3 C22 1.511(3) . ?
O4 Ni1 2.0219(15) 1_565 ?
N4 C27 1.343(3) . ?
N4 C25 1.455(3) . ?
C4 C9 1.422(3) . ?
C4 C10 1.427(3) . ?
C4 C26 1.425(3) . ?
O5 C20 1.227(3) . ?
C5 C7 1.357(3) . ?
C5 C23 1.405(3) . ?
O6 C27 1.230(3) . ?
C7 C10 1.437(3) . ?
C7 C27 1.502(3) . ?
C9 C23 1.367(3) . ?
C9 C20 1.502(3) . ?
C10 C36 1.419(3) . ?
C21 C33 1.375(3) . ?
C21 C24 1.380(3) . ?
C22 C32 1.354(4) . ?
C22 C29 1.377(3) . ?
C24 C35 1.387(3) . ?
C24 C25 1.513(3) 8_566 ?
C25 C24 1.513(3) 8_465 ?
C26 C37 1.367(4) . ?
C28 C35 1.379(3) . ?
C29 C38 1.383(3) . ?
C30 C39 1.517(3) . ?
C30 C31 1.515(3) . ?
C31 C41 1.512(4) . ?
C32 C42 1.381(4) . ?
C34 C39 1.505(4) . ?
C36 C40 1.365(3) . ?
C37 C40 1.406(4) . ?

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
O4 Ni1 N2 96.51(7) 1_545 . ?
O4 Ni1 N1 95.38(7) 1_545 . ?
N2 Ni1 N1 96.40(7) . . ?
O4 Ni1 O2 101.02(6) 1_545 . ?
N2 Ni1 O2 159.31(6) . . ?
N1 Ni1 O2 92.83(7) . . ?
O4 Ni1 O1 159.15(7) 1_545 . ?
N2 Ni1 O1 98.35(7) . . ?
N1 Ni1 O1 97.40(7) . . ?
O2 Ni1 O1 62.01(6) . . ?
O4 Ni1 O3 61.22(6) 1_545 1_545 ?
N2 Ni1 O3 89.65(6) . 1_545 ?
N1 Ni1 O3 156.42(7) . 1_545 ?
O2 Ni1 O3 89.23(6) . 1_545 ?
O1 Ni1 O3 104.27(6) . 1_545 ?
O4 Ni1 C1 130.84(7) 1_545 . ?
N2 Ni1 C1 129.36(7) . . ?
N1 Ni1 C1 95.81(7) . . ?
O2 Ni1 C1 30.75(6) . . ?
O1 Ni1 C1 31.27(7) . . ?
O3 Ni1 C1 97.88(6) 1_545 . ?
O4 Ni1 C2 30.60(7) 1_545 1_545 ?
N2 Ni1 C2 94.80(7) . 1_545 ?
N1 Ni1 C2 125.82(7) . 1_545 ?
O2 Ni1 C2 94.73(6) . 1_545 ?
O1 Ni1 C2 132.88(7) . 1_545 ?
O3 Ni1 C2 30.66(6) 1_545 1_545 ?
C1 Ni1 C2 116.36(8) . 1_545 ?
C1 O1 Ni1 88.81(13) . . ?
O2 C1 O1 119.8(2) . . ?
O2 C1 C41 120.0(2) . . ?
O1 C1 C41 120.2(2) . . ?
O2 C1 Ni1 59.87(11) . . ?
O1 C1 Ni1 59.92(11) . . ?
C41 C1 Ni1 178.96(17) . . ?
C42 N1 C38 116.6(2) . . ?
C42 N1 Ni1 117.86(17) . . ?
C38 N1 Ni1 125.30(15) . . ?
C1 O2 Ni1 89.38(14) . . ?
O4 C2 O3 119.5(2) . . ?
O4 C2 C34 117.1(2) . . ?
O3 C2 C34 123.4(2) . . ?
O4 C2 Ni1 54.54(11) . 1_565 ?
O3 C2 Ni1 65.08(11) . 1_565 ?
C34 C2 Ni1 170.72(17) . 1_565 ?
C28 N2 C33 116.94(19) . . ?
C28 N2 Ni1 122.75(15) . . ?
C33 N2 Ni1 119.48(15) . . ?
C2 O3 Ni1 84.27(13) . 1_565 ?
C20 N3 C3 123.13(19) . . ?
N3 C3 C22 113.60(19) . . ?
C2 O4 Ni1 94.86(13) . 1_565 ?
C27 N4 C25 120.5(2) . . ?
C9 C4 C10 119.27(19) . . ?
C9 C4 C26 122.1(2) . . ?
C10 C4 C26 118.6(2) . . ?
C7 C5 C23 121.4(2) . . ?
C5 C7 C10 119.94(19) . . ?
C5 C7 C27 119.67(19) . . ?
C10 C7 C27 120.29(18) . . ?
C23 C9 C4 120.2(2) . . ?
C23 C9 C20 119.33(19) . . ?
C4 C9 C20 120.49(19) . . ?
C36 C10 C4 118.8(2) . . ?
C36 C10 C7 122.6(2) . . ?
C4 C10 C7 118.51(19) . . ?
O5 C20 N3 122.8(2) . . ?
O5 C20 C9 122.9(2) . . ?
N3 C20 C9 114.33(18) . . ?
C33 C21 C24 119.7(2) . . ?
C32 C22 C29 115.6(2) . . ?
C32 C22 C3 122.1(2) . . ?
C29 C22 C3 122.3(2) . . ?
C9 C23 C5 120.6(2) . . ?
C21 C24 C35 117.0(2) . . ?
C21 C24 C25 122.89(19) . 8_566 ?
C35 C24 C25 120.1(2) . 8_566 ?
N4 C25 C24 113.87(18) . 8_465 ?
C37 C26 C4 120.7(2) . . ?
O6 C27 N4 122.9(2) . . ?
O6 C27 C7 121.8(2) . . ?
N4 C27 C7 115.23(18) . . ?
N2 C28 C35 123.0(2) . . ?
C38 C29 C22 120.1(2) . . ?
C39 C30 C31 114.0(2) . . ?
C41 C31 C30 113.6(2) . . ?
C22 C32 C42 121.7(2) . . ?
N2 C33 C21 123.5(2) . . ?
C39 C34 C2 117.5(2) . . ?
C28 C35 C24 119.8(2) . . ?
C40 C36 C10 120.7(2) . . ?
C26 C37 C40 120.3(2) . . ?
N1 C38 C29 123.3(2) . . ?
C34 C39 C30 113.4(2) . . ?
C36 C40 C37 120.7(2) . . ?
C1 C41 C31 114.9(2) . . ?
N1 C42 C32 122.6(3) . . ?

_refine_diff_density_max         0.373
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.050

####################################################################### 
# 
# 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_Ni-1
_database_code_depnum_ccdc_archive 'CCDC 2040496'
loop_
_audit_author_name
_audit_author_address
Jing
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2020-12-01 deposited with the CCDC.	2021-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H30 N4 Ni O9, H2 O'
_chemical_formula_sum            'C32 H32 N4 Ni O10'
_chemical_formula_weight         691.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   10.8482(4)
_cell_length_b                   11.7284(5)
_cell_length_c                   25.7782(9)
_cell_angle_alpha                90
_cell_angle_beta                 100.649(1)
_cell_angle_gamma                90
_cell_volume                     3223.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    5139
_cell_measurement_theta_min      2.2052
_cell_measurement_theta_max      24.4662

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_F_000             1440
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.665
_shelx_estimated_absorpt_T_min   0.907
_shelx_estimated_absorpt_T_max   0.930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18013
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.608
_diffrn_reflns_theta_max         25.062
_diffrn_reflns_theta_full        25.062
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5692
_reflns_number_gt                4563
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0505P)²+1.5409P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5692
_refine_ls_number_parameters     424
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0351
_refine_ls_wR_factor_ref         0.0986
_refine_ls_wR_factor_gt          0.0912
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.026
_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
Ni1 Ni 0.16729(3) 0.22486(3) 0.69821(2) 0.02798(11) Uani 1 1 d . U . . .
O1W O 0.18656(15) 0.07158(14) 0.74144(7) 0.0403(4) Uani 1 1 d . . . . .
H1A H 0.2609 0.0729 0.7630 0.048 Uiso 1 1 d R U . . .
H1B H 0.1343 0.0298 0.7562 0.048 Uiso 1 1 d R U . . .
O2W O 0.17792(15) 0.37816(13) 0.65861(6) 0.0342(4) Uani 1 1 d . U . . .
H2A H 0.1362 0.4357 0.6702 0.041 Uiso 1 1 d R U . . .
H2B H 0.2591 0.3906 0.6695 0.041 Uiso 1 1 d R U . . .
O3W O 0.14120(16) 0.30380(16) 0.76693(7) 0.0430(4) Uani 1 1 d . . . . .
H3A H 0.1036 0.3708 0.7644 0.052 Uiso 1 1 d R U . . .
H3B H 0.2126 0.3066 0.7896 0.052 Uiso 1 1 d R U . . .
O4W O 0.3570(2) 0.2827(2) 0.84467(9) 0.0785(8) Uani 1 1 d . . . . .
H4A H 0.3604 0.2851 0.8793 0.094 Uiso 1 1 d R U . . .
H4B H 0.3801 0.2133 0.8359 0.094 Uiso 1 1 d R U . . .
O1 O 0.11913(19) -0.23002(19) 0.53859(9) 0.0589(6) Uani 1 1 d . . . . .
O2 O 0.48793(19) -0.75459(19) 0.52335(8) 0.0559(5) Uani 1 1 d . . . . .
O3 O 0.35725(14) 0.22769(13) 0.72518(6) 0.0323(4) Uani 1 1 d . . . . .
O4 O 0.42737(16) 0.39746(15) 0.70513(8) 0.0442(5) Uani 1 1 d . . . . .
O5 O 0.42845(15) 0.06645(14) 0.80948(7) 0.0364(4) Uani 1 1 d . . . . .
O6 O 0.49417(15) -0.00340(14) 0.73890(7) 0.0392(4) Uani 1 1 d . . . . .
N1 N 0.19547(18) 0.13806(16) 0.63063(8) 0.0322(5) Uani 1 1 d . . . . .
N2 N 0.2857(2) -0.1735(2) 0.50559(9) 0.0463(6) Uani 1 1 d . . . . .
H2 H 0.3581 -0.1908 0.4988 0.056 Uiso 1 1 calc R U . . .
N3 N 0.50406(18) -0.72141(19) 0.61006(8) 0.0381(5) Uani 1 1 d . . . . .
H3 H 0.4865 -0.6765 0.6341 0.046 Uiso 1 1 calc R U . . .
N4 N 0.97312(18) -0.79027(17) 0.67375(8) 0.0333(5) Uani 1 1 d . . . . .
C1 C 0.1307(2) 0.1614(2) 0.58259(10) 0.0411(6) Uani 1 1 d . . . . .
H1 H 0.0754 0.2227 0.5789 0.049 Uiso 1 1 calc R U . . .
C2 C 0.1411(2) 0.0996(2) 0.53810(10) 0.0427(6) Uani 1 1 d . . . . .
H2C H 0.0927 0.1184 0.5056 0.051 Uiso 1 1 calc R U . . .
C3 C 0.2244(2) 0.0093(2) 0.54250(10) 0.0352(6) Uani 1 1 d . . . . .
C4 C 0.2942(2) -0.0123(2) 0.59165(10) 0.0391(6) Uani 1 1 d . . . . .
H4 H 0.3533 -0.0707 0.5961 0.047 Uiso 1 1 calc R U . . .
C5 C 0.2769(2) 0.0519(2) 0.63422(10) 0.0363(6) Uani 1 1 d . . . . .
H5 H 0.3242 0.0346 0.6672 0.044 Uiso 1 1 calc R U . . .
C6 C 0.2363(3) -0.0591(2) 0.49392(11) 0.0508(7) Uani 1 1 d . . . . .
H6A H 0.1543 -0.0647 0.4714 0.061 Uiso 1 1 calc R U . . .
H6B H 0.2909 -0.0185 0.4744 0.061 Uiso 1 1 calc R U . . .
C7 C 0.2210(3) -0.2515(2) 0.52654(11) 0.0445(7) Uani 1 1 d . . . . .
C8 C 0.2823(2) -0.3673(2) 0.53486(10) 0.0434(6) Uani 1 1 d . . . . .
C9 C 0.2304(2) -0.4607(2) 0.50327(9) 0.0361(6) Uani 1 1 d . . . . .
C10 C 0.1183(3) -0.4505(3) 0.46502(10) 0.0473(7) Uani 1 1 d . . . . .
H10 H 0.0759 -0.3812 0.4611 0.057 Uiso 1 1 calc R U . . .
C11 C 0.0723(3) -0.5400(3) 0.43421(11) 0.0582(8) Uani 1 1 d . . . . .
H11 H -0.0017 -0.5319 0.4097 0.070 Uiso 1 1 calc R U . . .
C12 C 0.1352(3) -0.6435(3) 0.43910(12) 0.0585(8) Uani 1 1 d . . . . .
H12 H 0.1042 -0.7036 0.4169 0.070 Uiso 1 1 calc R U . . .
C13 C 0.2408(3) -0.6585(3) 0.47563(11) 0.0475(7) Uani 1 1 d . . . . .
H13 H 0.2803 -0.7292 0.4787 0.057 Uiso 1 1 calc R U . . .
C14 C 0.2921(2) -0.5682(2) 0.50934(9) 0.0349(6) Uani 1 1 d . . . . .
C15 C 0.4006(2) -0.5804(2) 0.54985(10) 0.0372(6) Uani 1 1 d . . . . .
C16 C 0.4453(3) -0.4884(3) 0.58003(12) 0.0561(8) Uani 1 1 d . . . . .
H16 H 0.5155 -0.4971 0.6065 0.067 Uiso 1 1 calc R U . . .
C17 C 0.3878(3) -0.3813(3) 0.57198(12) 0.0603(9) Uani 1 1 d . . . . .
H17 H 0.4221 -0.3193 0.5922 0.072 Uiso 1 1 calc R U . . .
C18 C 0.4674(2) -0.6926(2) 0.55929(10) 0.0377(6) Uani 1 1 d . . . . .
C19 C 0.5724(2) -0.8257(2) 0.62593(10) 0.0384(6) Uani 1 1 d . . . . .
H19A H 0.5550 -0.8799 0.5971 0.046 Uiso 1 1 calc R U . . .
H19B H 0.5415 -0.8581 0.6557 0.046 Uiso 1 1 calc R U . . .
C20 C 0.7128(2) -0.8105(2) 0.64114(9) 0.0326(5) Uani 1 1 d . . . . .
C21 C 0.7880(2) -0.9041(3) 0.65577(13) 0.0552(8) Uani 1 1 d . . . . .
H21 H 0.7525 -0.9764 0.6551 0.066 Uiso 1 1 calc R U . . .
C22 C 0.9157(2) -0.8909(2) 0.67143(13) 0.0548(8) Uani 1 1 d . . . . .
H22 H 0.9643 -0.9556 0.6809 0.066 Uiso 1 1 calc R U . . .
C23 C 0.9006(2) -0.7012(2) 0.65831(11) 0.0417(6) Uani 1 1 d . . . . .
H23 H 0.9381 -0.6297 0.6589 0.050 Uiso 1 1 calc R U . . .
C24 C 0.7725(2) -0.7084(2) 0.64132(11) 0.0430(7) Uani 1 1 d . . . . .
H24 H 0.7267 -0.6432 0.6299 0.052 Uiso 1 1 calc R U . . .
C25 C 0.4417(2) 0.3016(2) 0.72755(9) 0.0294(5) Uani 1 1 d . . . . .
C26 C 0.5704(2) 0.2693(2) 0.75684(9) 0.0291(5) Uani 1 1 d . . . . .
C27 C 0.5948(2) 0.1610(2) 0.77803(9) 0.0311(5) Uani 1 1 d . . . . .
C28 C 0.7166(2) 0.1328(2) 0.80222(11) 0.0464(7) Uani 1 1 d . . . . .
H28 H 0.7336 0.0604 0.8165 0.056 Uiso 1 1 calc R U . . .
C29 C 0.8122(2) 0.2113(3) 0.80510(12) 0.0556(8) Uani 1 1 d . . . . .
H29 H 0.8932 0.1914 0.8212 0.067 Uiso 1 1 calc R U . . .
C30 C 0.7889(3) 0.3179(3) 0.78450(12) 0.0512(7) Uani 1 1 d . . . . .
H30 H 0.8537 0.3706 0.7866 0.061 Uiso 1 1 calc R U . . .
C31 C 0.6686(2) 0.3472(2) 0.76043(11) 0.0410(6) Uani 1 1 d . . . . .
H31 H 0.6530 0.4199 0.7464 0.049 Uiso 1 1 calc R U . . .
C32 C 0.4966(2) 0.0684(2) 0.77453(10) 0.0307(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
Ni1 O3 2.0497(15) . ?
Ni1 O3W 2.0640(17) . ?
Ni1 O2W 2.0812(16) . ?
Ni1 N1 2.089(2) . ?
Ni1 N4 2.0917(19) 1_465 ?
Ni1 O1W 2.1050(17) . ?
O1W H1A 0.8908 . ?
O1W H1B 0.8857 . ?
O2W H2A 0.8945 . ?
O2W H2B 0.8852 . ?
O3W H3A 0.8823 . ?
O3W H3B 0.8807 . ?
O4W H4A 0.8876 . ?
O4W H4B 0.8934 . ?
O1 C7 1.228(3) . ?
O2 C18 1.230(3) . ?
O3 C25 1.255(3) . ?
O4 C25 1.260(3) . ?
O5 C32 1.267(3) . ?
O6 C32 1.243(3) . ?
N1 C5 1.334(3) . ?
N1 C1 1.334(3) . ?
N2 C7 1.328(4) . ?
N2 C6 1.455(3) . ?
N2 H2 0.8600 . ?
N3 C18 1.339(3) . ?
N3 C19 1.449(3) . ?
N3 H3 0.8600 . ?
N4 C23 1.324(3) . ?
N4 C22 1.330(3) . ?
N4 Ni1 2.0917(19) 1_645 ?
C1 C2 1.379(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.384(3) . ?
C2 H2C 0.9300 . ?
C3 C4 1.374(3) . ?
C3 C6 1.512(4) . ?
C4 C5 1.373(3) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.510(4) . ?
C8 C17 1.360(4) . ?
C8 C9 1.418(4) . ?
C9 C10 1.422(3) . ?
C9 C14 1.423(4) . ?
C10 C11 1.354(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.387(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.354(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.418(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.429(3) . ?
C15 C16 1.365(4) . ?
C15 C18 1.501(4) . ?
C16 C17 1.401(4) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C19 C20 1.511(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C24 1.360(4) . ?
C20 C21 1.378(4) . ?
C21 C22 1.378(4) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 C24 1.381(3) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C26 1.508(3) . ?
C26 C27 1.389(3) . ?
C26 C31 1.394(3) . ?
C27 C28 1.393(3) . ?
C27 C32 1.511(3) . ?
C28 C29 1.378(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.364(4) . ?
C29 H29 0.9300 . ?
C30 C31 1.381(4) . ?
C30 H30 0.9300 . ?
C31 H31 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
O3 Ni1 O3W 89.45(7) . . ?
O3 Ni1 O2W 90.52(6) . . ?
O3W Ni1 O2W 93.57(7) . . ?
O3 Ni1 N1 89.87(7) . . ?
O3W Ni1 N1 177.38(8) . . ?
O2W Ni1 N1 88.97(7) . . ?
O3 Ni1 N4 175.50(7) . 1_465 ?
O3W Ni1 N4 90.38(7) . 1_465 ?
O2W Ni1 N4 93.98(7) . 1_465 ?
N1 Ni1 N4 90.10(8) . 1_465 ?
O3 Ni1 O1W 80.74(6) . . ?
O3W Ni1 O1W 86.83(7) . . ?
O2W Ni1 O1W 171.25(6) . . ?
N1 Ni1 O1W 90.56(7) . . ?
N4 Ni1 O1W 94.76(7) 1_465 . ?
Ni1 O1W H1A 107.8 . . ?
Ni1 O1W H1B 133.7 . . ?
H1A O1W H1B 108.6 . . ?
Ni1 O2W H2A 114.2 . . ?
Ni1 O2W H2B 97.4 . . ?
H2A O2W H2B 107.8 . . ?
Ni1 O3W H3A 118.1 . . ?
Ni1 O3W H3B 110.0 . . ?
H3A O3W H3B 110.7 . . ?
H4A O4W H4B 108.8 . . ?
C25 O3 Ni1 135.00(15) . . ?
C5 N1 C1 116.6(2) . . ?
C5 N1 Ni1 120.56(16) . . ?
C1 N1 Ni1 122.75(16) . . ?
C7 N2 C6 121.2(2) . . ?
C7 N2 H2 119.4 . . ?
C6 N2 H2 119.4 . . ?
C18 N3 C19 122.2(2) . . ?
C18 N3 H3 118.9 . . ?
C19 N3 H3 118.9 . . ?
C23 N4 C22 116.1(2) . . ?
C23 N4 Ni1 122.19(17) . 1_645 ?
C22 N4 Ni1 121.71(17) . 1_645 ?
N1 C1 C2 123.7(2) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C1 C2 C3 119.1(2) . . ?
C1 C2 H2C 120.4 . . ?
C3 C2 H2C 120.4 . . ?
C4 C3 C2 117.2(2) . . ?
C4 C3 C6 123.3(2) . . ?
C2 C3 C6 119.5(2) . . ?
C5 C4 C3 120.2(2) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
N1 C5 C4 123.2(2) . . ?
N1 C5 H5 118.4 . . ?
C4 C5 H5 118.4 . . ?
N2 C6 C3 113.7(2) . . ?
N2 C6 H6A 108.8 . . ?
C3 C6 H6A 108.8 . . ?
N2 C6 H6B 108.8 . . ?
C3 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
O1 C7 N2 122.0(3) . . ?
O1 C7 C8 122.8(3) . . ?
N2 C7 C8 115.2(2) . . ?
C17 C8 C9 120.3(3) . . ?
C17 C8 C7 120.0(3) . . ?
C9 C8 C7 119.7(2) . . ?
C8 C9 C10 122.1(2) . . ?
C8 C9 C14 119.5(2) . . ?
C10 C9 C14 118.4(2) . . ?
C11 C10 C9 121.1(3) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C10 C11 C12 120.2(3) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C13 C12 C11 121.1(3) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C12 C13 C14 121.0(3) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C13 C14 C9 118.1(2) . . ?
C13 C14 C15 123.4(2) . . ?
C9 C14 C15 118.5(2) . . ?
C16 C15 C14 119.7(2) . . ?
C16 C15 C18 119.4(2) . . ?
C14 C15 C18 120.9(2) . . ?
C15 C16 C17 121.5(2) . . ?
C15 C16 H16 119.2 . . ?
C17 C16 H16 119.2 . . ?
C8 C17 C16 120.4(3) . . ?
C8 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
O2 C18 N3 121.7(2) . . ?
O2 C18 C15 123.1(2) . . ?
N3 C18 C15 115.3(2) . . ?
N3 C19 C20 114.4(2) . . ?
N3 C19 H19A 108.7 . . ?
C20 C19 H19A 108.7 . . ?
N3 C19 H19B 108.7 . . ?
C20 C19 H19B 108.7 . . ?
H19A C19 H19B 107.6 . . ?
C24 C20 C21 116.3(2) . . ?
C24 C20 C19 124.1(2) . . ?
C21 C20 C19 119.6(2) . . ?
C22 C21 C20 120.2(3) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
N4 C22 C21 123.4(3) . . ?
N4 C22 H22 118.3 . . ?
C21 C22 H22 118.3 . . ?
N4 C23 C24 123.6(2) . . ?
N4 C23 H23 118.2 . . ?
C24 C23 H23 118.2 . . ?
C20 C24 C23 120.4(2) . . ?
C20 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
O3 C25 O4 124.5(2) . . ?
O3 C25 C26 116.8(2) . . ?
O4 C25 C26 118.6(2) . . ?
C27 C26 C31 119.0(2) . . ?
C27 C26 C25 121.3(2) . . ?
C31 C26 C25 119.6(2) . . ?
C26 C27 C28 119.3(2) . . ?
C26 C27 C32 123.5(2) . . ?
C28 C27 C32 117.1(2) . . ?
C29 C28 C27 120.5(3) . . ?
C29 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
C30 C29 C28 120.5(3) . . ?
C30 C29 H29 119.7 . . ?
C28 C29 H29 119.7 . . ?
C29 C30 C31 119.7(3) . . ?
C29 C30 H30 120.2 . . ?
C31 C30 H30 120.2 . . ?
C30 C31 C26 121.0(3) . . ?
C30 C31 H31 119.5 . . ?
C26 C31 H31 119.5 . . ?
O6 C32 O5 125.3(2) . . ?
O6 C32 C27 116.7(2) . . ?
O5 C32 C27 117.9(2) . . ?

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
C5 N1 C1 C2 2.1(4) . . . . ?
Ni1 N1 C1 C2 -175.0(2) . . . . ?
N1 C1 C2 C3 -1.1(4) . . . . ?
C1 C2 C3 C4 -1.0(4) . . . . ?
C1 C2 C3 C6 179.9(3) . . . . ?
C2 C3 C4 C5 2.1(4) . . . . ?
C6 C3 C4 C5 -178.8(3) . . . . ?
C1 N1 C5 C4 -0.9(4) . . . . ?
Ni1 N1 C5 C4 176.2(2) . . . . ?
C3 C4 C5 N1 -1.2(4) . . . . ?
C7 N2 C6 C3 66.6(4) . . . . ?
C4 C3 C6 N2 23.7(4) . . . . ?
C2 C3 C6 N2 -157.2(3) . . . . ?
C6 N2 C7 O1 -2.4(4) . . . . ?
C6 N2 C7 C8 178.2(2) . . . . ?
O1 C7 C8 C17 -110.6(4) . . . . ?
N2 C7 C8 C17 68.8(4) . . . . ?
O1 C7 C8 C9 70.4(4) . . . . ?
N2 C7 C8 C9 -110.2(3) . . . . ?
C17 C8 C9 C10 178.3(3) . . . . ?
C7 C8 C9 C10 -2.7(4) . . . . ?
C17 C8 C9 C14 -2.3(4) . . . . ?
C7 C8 C9 C14 176.7(2) . . . . ?
C8 C9 C10 C11 178.1(3) . . . . ?
C14 C9 C10 C11 -1.3(4) . . . . ?
C9 C10 C11 C12 -0.8(5) . . . . ?
C10 C11 C12 C13 2.2(5) . . . . ?
C11 C12 C13 C14 -1.4(5) . . . . ?
C12 C13 C14 C9 -0.8(4) . . . . ?
C12 C13 C14 C15 177.6(3) . . . . ?
C8 C9 C14 C13 -177.4(2) . . . . ?
C10 C9 C14 C13 2.1(4) . . . . ?
C8 C9 C14 C15 4.2(4) . . . . ?
C10 C9 C14 C15 -176.4(2) . . . . ?
C13 C14 C15 C16 178.9(3) . . . . ?
C9 C14 C15 C16 -2.8(4) . . . . ?
C13 C14 C15 C18 -0.3(4) . . . . ?
C9 C14 C15 C18 178.1(2) . . . . ?
C14 C15 C16 C17 -0.6(5) . . . . ?
C18 C15 C16 C17 178.6(3) . . . . ?
C9 C8 C17 C16 -1.0(5) . . . . ?
C7 C8 C17 C16 179.9(3) . . . . ?
C15 C16 C17 C8 2.5(5) . . . . ?
C19 N3 C18 O2 1.4(4) . . . . ?
C19 N3 C18 C15 -178.4(2) . . . . ?
C16 C15 C18 O2 -137.0(3) . . . . ?
C14 C15 C18 O2 42.2(4) . . . . ?
C16 C15 C18 N3 42.9(4) . . . . ?
C14 C15 C18 N3 -137.9(2) . . . . ?
C18 N3 C19 C20 98.0(3) . . . . ?
N3 C19 C20 C24 1.3(4) . . . . ?
N3 C19 C20 C21 -178.5(2) . . . . ?
C24 C20 C21 C22 2.4(4) . . . . ?
C19 C20 C21 C22 -177.8(3) . . . . ?
C23 N4 C22 C21 -2.1(5) . . . . ?
Ni1 N4 C22 C21 179.7(3) 1_645 . . . ?
C20 C21 C22 N4 0.4(5) . . . . ?
C22 N4 C23 C24 1.0(4) . . . . ?
Ni1 N4 C23 C24 179.2(2) 1_645 . . . ?
C21 C20 C24 C23 -3.5(4) . . . . ?
C19 C20 C24 C23 176.7(2) . . . . ?
N4 C23 C24 C20 1.9(4) . . . . ?
Ni1 O3 C25 O4 -10.4(4) . . . . ?
Ni1 O3 C25 C26 173.23(15) . . . . ?
O3 C25 C26 C27 2.8(3) . . . . ?
O4 C25 C26 C27 -173.8(2) . . . . ?
O3 C25 C26 C31 179.3(2) . . . . ?
O4 C25 C26 C31 2.8(3) . . . . ?
C31 C26 C27 C28 -0.1(4) . . . . ?
C25 C26 C27 C28 176.5(2) . . . . ?
C31 C26 C27 C32 -177.6(2) . . . . ?
C25 C26 C27 C32 -1.0(4) . . . . ?
C26 C27 C28 C29 -0.1(4) . . . . ?
C32 C27 C28 C29 177.5(3) . . . . ?
C27 C28 C29 C30 0.3(5) . . . . ?
C28 C29 C30 C31 -0.2(5) . . . . ?
C29 C30 C31 C26 0.0(4) . . . . ?
C27 C26 C31 C30 0.2(4) . . . . ?
C25 C26 C31 C30 -176.5(2) . . . . ?
C26 C27 C32 O6 98.1(3) . . . . ?
C28 C27 C32 O6 -79.4(3) . . . . ?
C26 C27 C32 O5 -85.6(3) . . . . ?
C28 C27 C32 O5 96.9(3) . . . . ?

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
O1W H1A O5 0.89 1.99 2.875(2) 177 .
O1W H1B O4 0.89 2.02 2.868(2) 159 2_546
O2W H2A O5 0.89 1.80 2.690(2) 171 2_556
O2W H2B O4 0.89 1.89 2.759(2) 168 .
O3W H3A O6 0.88 1.81 2.685(2) 171 2_556
O3W H3B O4W 0.88 1.93 2.797(3) 168 .
O4W H4A O1 0.89 2.09 2.976(3) 173 2_556
O4W H4B O5 0.89 1.96 2.850(3) 174 .
N2 H2 O2 0.86 1.97 2.824(3) 172 3_646
N3 H3 O4 0.86 2.23 3.065(3) 165 1_545

_refine_diff_density_max         1.018
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.051

####################################################################### 
# 
# 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_01_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2040494'
loop_
_audit_author_name
_audit_author_address
Jing
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2020-12-01 deposited with the CCDC.	2021-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 N6 Ni O12'
_chemical_formula_weight         819.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   24.0029(19)
_cell_length_b                   8.5417(7)
_cell_length_c                   17.6880(13)
_cell_angle_alpha                90
_cell_angle_beta                 92.236(3)
_cell_angle_gamma                90
_cell_volume                     3623.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1185
_cell_measurement_theta_min      1.698
_cell_measurement_theta_max      26.319

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_F_000             1688
_exptl_transmission_factor_min   0.914
_exptl_transmission_factor_max   0.936
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.611
_shelx_estimated_absorpt_T_min   0.914
_shelx_estimated_absorpt_T_max   0.936
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11125
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.698
_diffrn_reflns_theta_max         26.319
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3684
_reflns_number_gt                1960
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1478P)²+10.5588P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3684
_refine_ls_number_parameters     259
_refine_ls_number_restraints     312
_refine_ls_R_factor_all          0.1581
_refine_ls_R_factor_gt           0.0862
_refine_ls_wR_factor_ref         0.2893
_refine_ls_wR_factor_gt          0.2382
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.018
_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
Ni1 Ni 0.2500 0.2500 0.5000 0.0463(4) Uani 1 2 d S . P . .
O1 O 0.16689(16) 0.2713(6) 0.5102(3) 0.0593(14) Uani 1 1 d . . . . .
N1 N 0.23273(19) 0.0668(7) 0.4228(3) 0.0495(14) Uani 1 1 d . . . . .
C1 C 0.1801(2) -0.0498(8) 0.3206(4) 0.0536(15) Uani 1 1 d . U . . .
H1A H 0.1491 -0.0433 0.2849 0.064 Uiso 1 1 d R U . . .
C2 C 0.0585(3) -0.4583(8) 0.2636(4) 0.0592(15) Uani 1 1 d . U . . .
N2 N 0.1482(2) -0.3466(7) 0.2458(3) 0.0495(14) Uani 1 1 d . . . . .
H2A H 0.1314 -0.2945 0.2071 0.059 Uiso 1 1 d R U . . .
O2 O 0.1479(2) 0.1456(9) 0.6162(3) 0.0839(19) Uani 1 1 d . . . . .
O3 O 0.25574(19) 0.0866(6) 0.5871(3) 0.0627(14) Uani 1 1 d . . . . .
C3 C 0.2068(3) -0.3084(9) 0.2640(4) 0.0538(14) Uani 1 1 d . U . . .
H3A H 0.2257 -0.2829 0.2189 0.065 Uiso 1 1 d R U . . .
H3B H 0.2237 -0.4012 0.2852 0.065 Uiso 1 1 d R U . . .
N3 N -0.0972(3) 0.2609(16) 0.4706(7) 0.126(4) Uani 1 1 d . . . . .
C4 C 0.0297(3) -0.6016(8) 0.2567(5) 0.0696(17) Uani 1 1 d . U . . .
O4 O -0.1307(3) 0.1957(15) 0.5059(6) 0.172(5) Uani 1 1 d . . . . .
C5 C 0.0295(3) -0.3251(9) 0.2551(5) 0.0711(18) Uani 1 1 d . U . . .
H5B H 0.0321 -0.2721 0.3030 0.107 Uiso 1 1 d R U . . .
O5 O -0.1088(3) 0.3317(18) 0.4092(8) 0.189(5) Uani 1 1 d . . . . .
O6 O 0.1414(2) -0.5293(7) 0.3343(3) 0.0785(17) Uani 1 1 d . . . . .
C12 C 0.0732(3) 0.2286(11) 0.5345(4) 0.0736(18) Uani 1 1 d . U . . .
C13 C 0.2143(2) -0.1802(9) 0.3205(4) 0.0480(13) Uani 1 1 d . U . . .
C14 C 0.1198(3) -0.4492(8) 0.2837(4) 0.0545(14) Uani 1 1 d . U . . .
C15 C 0.2585(3) -0.1837(9) 0.3731(4) 0.0565(15) Uani 1 1 d . U . . .
H15A H 0.2834 -0.2717 0.3751 0.068 Uiso 1 1 d R U . . .
C17 C 0.1898(2) 0.0687(9) 0.3716(4) 0.0552(15) Uani 1 1 d . U . . .
H17A H 0.1650 0.1570 0.3711 0.066 Uiso 1 1 d R U . . .
C18 C 0.0566(3) 0.3120(12) 0.4699(5) 0.0812(18) Uani 1 1 d . U . . .
H18A H 0.0841 0.3652 0.4414 0.097 Uiso 1 1 d R U . . .
C19 C 0.2656(3) -0.0591(9) 0.4229(4) 0.0570(15) Uani 1 1 d . U . . .
H19A H 0.2961 -0.0637 0.4595 0.068 Uiso 1 1 d R U . . .
C20 C -0.0379(3) 0.2516(12) 0.4928(5) 0.086(2) Uani 1 1 d . U . . .
C21 C 0.1344(3) 0.2115(11) 0.5560(4) 0.0656(17) Uani 1 1 d . U . . .
C24 C 0.0007(3) 0.3245(13) 0.4483(5) 0.0860(19) Uani 1 1 d . U . . .
H24A H -0.0110 0.3784 0.4028 0.103 Uiso 1 1 d R U . . .
C25 C 0.0337(3) 0.1542(14) 0.5753(5) 0.0896(19) Uani 1 1 d . U . . .
H25A H 0.0450 0.0932 0.6188 0.108 Uiso 1 1 d R U . . .
C26 C -0.0233(3) 0.1656(14) 0.5537(5) 0.096(2) Uani 1 1 d . U . . .
H26A H -0.0520 0.1131 0.5803 0.115 Uiso 1 1 d R U . . .
C28 C 0.0573(4) -0.7438(10) 0.2606(6) 0.090(2) Uani 1 1 d . U . . .
H28A H 0.0905 -0.7405 0.2927 0.108 Uiso 1 1 d R U . . .
C30 C 0.0299(4) -0.8799(11) 0.2549(7) 0.113(3) Uani 1 1 d . U . . .
H30A H 0.0489 -0.9782 0.2513 0.170 Uiso 1 1 d R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.018(4) 7_556 ?
Ni1 O1 2.018(4) . ?
Ni1 O3 2.079(5) . ?
Ni1 O3 2.079(5) 7_556 ?
Ni1 N1 2.107(6) 7_556 ?
Ni1 N1 2.107(6) . ?
O1 C21 1.256(9) . ?
N1 C19 1.333(8) . ?
N1 C17 1.346(7) . ?
C1 C17 1.369(9) . ?
C1 C13 1.384(9) . ?
C2 C5 1.340(10) . ?
C2 C4 1.410(10) . ?
C2 C14 1.503(9) . ?
N2 C14 1.311(9) . ?
N2 C3 1.466(8) . ?
O2 C21 1.235(9) . ?
C3 C13 1.488(10) . ?
N3 O4 1.177(14) . ?
N3 O5 1.264(15) . ?
N3 C20 1.464(11) . ?
C4 C28 1.385(10) . ?
C4 C4 1.434(13) 2 ?
C5 C5 1.420(14) 2 ?
O6 C14 1.224(8) . ?
C12 C25 1.371(11) . ?
C12 C18 1.392(12) . ?
C12 C21 1.510(9) . ?
C13 C15 1.384(8) . ?
C15 C19 1.388(10) . ?
C18 C24 1.383(9) . ?
C20 C26 1.338(13) . ?
C20 C24 1.388(13) . ?
C25 C26 1.408(11) . ?
C28 C30 1.338(12) . ?
C30 C30 1.437(19) 2 ?

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 7_556 . ?
O1 Ni1 O3 88.18(19) 7_556 . ?
O1 Ni1 O3 91.82(19) . . ?
O1 Ni1 O3 91.81(19) 7_556 7_556 ?
O1 Ni1 O3 88.18(19) . 7_556 ?
O3 Ni1 O3 180.0 . 7_556 ?
O1 Ni1 N1 87.39(19) 7_556 7_556 ?
O1 Ni1 N1 92.61(19) . 7_556 ?
O3 Ni1 N1 90.7(2) . 7_556 ?
O3 Ni1 N1 89.3(2) 7_556 7_556 ?
O1 Ni1 N1 92.61(19) 7_556 . ?
O1 Ni1 N1 87.39(19) . . ?
O3 Ni1 N1 89.3(2) . . ?
O3 Ni1 N1 90.7(2) 7_556 . ?
N1 Ni1 N1 180.0 7_556 . ?
C21 O1 Ni1 131.5(5) . . ?
C19 N1 C17 116.6(6) . . ?
C19 N1 Ni1 119.8(4) . . ?
C17 N1 Ni1 123.6(5) . . ?
C17 C1 C13 120.8(6) . . ?
C5 C2 C4 118.4(6) . . ?
C5 C2 C14 118.9(6) . . ?
C4 C2 C14 122.6(6) . . ?
C14 N2 C3 123.4(5) . . ?
N2 C3 C13 113.7(5) . . ?
O4 N3 O5 123.3(10) . . ?
O4 N3 C20 120.6(14) . . ?
O5 N3 C20 115.9(11) . . ?
C28 C4 C2 121.6(6) . . ?
C28 C4 C4 118.6(4) . 2 ?
C2 C4 C4 119.7(4) . 2 ?
C2 C5 C5 121.7(4) . 2 ?
C25 C12 C18 119.1(7) . . ?
C25 C12 C21 120.6(8) . . ?
C18 C12 C21 120.1(7) . . ?
C1 C13 C15 117.1(7) . . ?
C1 C13 C3 122.5(5) . . ?
C15 C13 C3 120.4(6) . . ?
O6 C14 N2 122.3(6) . . ?
O6 C14 C2 121.8(7) . . ?
N2 C14 C2 115.9(6) . . ?
C13 C15 C19 118.8(6) . . ?
N1 C17 C1 122.7(6) . . ?
C24 C18 C12 120.7(9) . . ?
N1 C19 C15 124.1(6) . . ?
C26 C20 C24 122.9(8) . . ?
C26 C20 N3 117.9(10) . . ?
C24 C20 N3 119.1(10) . . ?
O2 C21 O1 126.4(6) . . ?
O2 C21 C12 118.8(7) . . ?
O1 C21 C12 114.9(7) . . ?
C18 C24 C20 118.0(9) . . ?
C12 C25 C26 120.6(9) . . ?
C20 C26 C25 118.5(9) . . ?
C30 C28 C4 121.6(8) . . ?
C28 C30 C30 119.7(6) . 2 ?

_refine_diff_density_max         0.737
_refine_diff_density_min         -1.120
_refine_diff_density_rms         0.102

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

data_1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2040498'
loop_
_audit_author_name
_audit_author_address
Jing
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2020-12-01 deposited with the CCDC.	2021-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C68 H56 N8 Ni2 O13'
_chemical_formula_weight         1310.63

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C2/c  '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   27.980(4)
_cell_length_b                   9.5268(11)
_cell_length_c                   26.150(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 121.298(5)
_cell_angle_gamma                90.00
_cell_volume                     5956.1(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2521
_cell_measurement_theta_min      1.73
_cell_measurement_theta_max      26.74

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2720
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.9013
_exptl_absorpt_correction_T_max  0.9262
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19095
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0587
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.73
_diffrn_reflns_theta_max         26.74
_reflns_number_total             6291
_reflns_number_gt                4188
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0535P)²+0.1263P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6291
_refine_ls_number_parameters     411
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.1129
_refine_ls_wR_factor_gt          0.0978
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.608104(14) -0.62245(4) -0.103176(14) 0.03261(12) Uani 1 1 d . . .
O1 O 0.06873(8) -0.5690(2) -0.48265(9) 0.0563(6) Uani 1 1 d . . .
N1 N 0.10666(9) -0.3979(2) -0.41295(10) 0.0384(6) Uani 1 1 d . . .
H1B H 0.1352 -0.3726 -0.3793 0.046 Uiso 1 1 calc R . .
C1 C 0.25388(11) -0.6682(3) -0.34355(11) 0.0354(6) Uani 1 1 d . . .
H1A H 0.2885 -0.6473 -0.3385 0.043 Uiso 1 1 calc R . .
O1W O 0.5000 -0.3001(6) -0.2500 0.223(4) Uani 1 2 d S . .
02 O 0.31138(9) -0.8711(2) -0.21591(8) 0.0563(6) Uani 1 1 d . . .
N2 N 0.08485(9) -0.0165(2) -0.55914(10) 0.0364(5) Uani 1 1 d . . .
C2 C 0.20746(12) -0.5857(3) -0.38213(12) 0.0379(7) Uani 1 1 d . . .
H2A H 0.2119 -0.5090 -0.4013 0.045 Uiso 1 1 calc R . .
O3 O 0.58791(8) -1.49295(19) -0.17620(8) 0.0432(5) Uani 1 1 d . . .
N3 N 0.33469(8) -0.9000(2) -0.28583(9) 0.0352(5) Uani 1 1 d . . .
H3A H 0.3263 -0.8817 -0.3218 0.042 Uiso 1 1 calc R . .
C3 C 0.15573(11) -0.6168(3) -0.39190(11) 0.0337(6) Uani 1 1 d . . .
O4 O 0.67177(8) -1.48481(19) -0.09683(8) 0.0404(5) Uani 1 1 d . . .
N4 N 0.53437(9) -0.7330(2) -0.14219(9) 0.0353(5) Uani 1 1 d . . .
C4 C 0.24921(11) -0.7785(3) -0.31319(11) 0.0308(6) Uani 1 1 d . . .
O5 O 0.65208(8) -0.79951(19) -0.11555(8) 0.0381(5) Uani 1 1 d . . .
C5 C 0.14812(11) -0.7356(3) -0.36351(11) 0.0328(6) Uani 1 1 d . . .
O6 O 0.65388(8) -0.75373(19) -0.03257(8) 0.0391(5) Uani 1 1 d . . .
C6 C 0.19527(11) -0.8170(3) -0.32354(11) 0.0314(6) Uani 1 1 d . . .
C7 C 0.09489(12) -0.7729(3) -0.37324(13) 0.0437(7) Uani 1 1 d . . .
H7A H 0.0639 -0.7175 -0.3980 0.052 Uiso 1 1 calc R . .
C8 C 0.18712(13) -0.9388(3) -0.29766(12) 0.0422(7) Uani 1 1 d . . .
H8A H 0.2175 -0.9951 -0.2723 0.051 Uiso 1 1 calc R . .
C9 C 0.08856(13) -0.8888(4) -0.34688(14) 0.0521(8) Uani 1 1 d . . .
H9A H 0.0535 -0.9116 -0.3535 0.063 Uiso 1 1 calc R . .
C10 C 0.13476(14) -0.9738(3) -0.30976(14) 0.0523(9) Uani 1 1 d . . .
H10A H 0.1298 -1.0549 -0.2932 0.063 Uiso 1 1 calc R . .
C11 C 0.10613(11) -0.5268(3) -0.43359(12) 0.0374(7) Uani 1 1 d . . .
C12 C 0.06082(12) -0.2983(3) -0.44508(12) 0.0401(7) Uani 1 1 d . . .
H12A H 0.0571 -0.2432 -0.4162 0.048 Uiso 1 1 calc R . .
H12B H 0.0263 -0.3503 -0.4689 0.048 Uiso 1 1 calc R . .
C13 C 0.06836(11) -0.2004(3) -0.48535(11) 0.0332(6) Uani 1 1 d . . .
C14 C 0.06804(12) -0.0565(3) -0.47952(13) 0.0431(7) Uani 1 1 d . . .
H14A H 0.0620 -0.0179 -0.4507 0.052 Uiso 1 1 calc R . .
C15 C 0.07530(15) -0.2484(3) -0.53094(15) 0.0554(9) Uani 1 1 d . . .
H15A H 0.0748 -0.3443 -0.5379 0.066 Uiso 1 1 calc R . .
C16 C 0.08301(15) -0.1544(3) -0.56606(15) 0.0548(9) Uani 1 1 d . . .
H16A H 0.0872 -0.1902 -0.5966 0.066 Uiso 1 1 calc R . .
C17 C 0.07665(12) 0.0306(3) -0.51622(13) 0.0446(7) Uani 1 1 d . . .
H17A H 0.0767 0.1271 -0.5107 0.053 Uiso 1 1 calc R . .
C18 C 0.30090(11) -0.8551(3) -0.26749(12) 0.0350(6) Uani 1 1 d . . .
C19 C 0.38510(11) -0.9788(3) -0.24690(13) 0.0422(7) Uani 1 1 d . . .
H19A H 0.3924 -1.0417 -0.2712 0.051 Uiso 1 1 calc R . .
H19B H 0.3786 -1.0361 -0.2204 0.051 Uiso 1 1 calc R . .
C20 C 0.43622(11) -0.8900(3) -0.20953(11) 0.0336(6) Uani 1 1 d . . .
C21 C 0.48168(12) -0.9417(3) -0.15722(13) 0.0527(9) Uani 1 1 d . . .
H21A H 0.4801 -1.0308 -0.1436 0.063 Uiso 1 1 calc R . .
C22 C 0.52916(12) -0.8612(3) -0.12543(13) 0.0515(9) Uani 1 1 d . . .
H22A H 0.5591 -0.8983 -0.0905 0.062 Uiso 1 1 calc R . .
C23 C 0.48988(12) -0.6817(3) -0.19118(13) 0.0411(7) Uani 1 1 d . . .
H23A H 0.4921 -0.5911 -0.2030 0.049 Uiso 1 1 calc R . .
C24 C 0.44096(11) -0.7546(3) -0.22523(12) 0.0388(7) Uani 1 1 d . . .
H24A H 0.4111 -0.7129 -0.2588 0.047 Uiso 1 1 calc R . .
C25 C 0.78158(13) -1.1053(3) -0.10442(15) 0.0540(9) Uani 1 1 d . . .
H25A H 0.8143 -1.0924 -0.1049 0.065 Uiso 1 1 calc R . .
C26 C 0.74447(13) -1.2073(3) -0.13936(14) 0.0455(8) Uani 1 1 d . . .
H26A H 0.7523 -1.2634 -0.1632 0.055 Uiso 1 1 calc R . .
C27 C 0.77098(12) -1.0210(3) -0.06838(14) 0.0491(8) Uani 1 1 d . . .
H27A H 0.7966 -0.9523 -0.0447 0.059 Uiso 1 1 calc R . .
C28 C 0.69552(12) -1.2281(3) -0.13961(12) 0.0373(7) Uani 1 1 d . . .
C29 C 0.72209(12) -1.0385(3) -0.06732(12) 0.0393(7) Uani 1 1 d . . .
C30 C 0.68526(12) -1.1420(3) -0.10332(12) 0.0384(7) Uani 1 1 d . . .
H30A H 0.6523 -1.1547 -0.1033 0.046 Uiso 1 1 calc R . .
C31 C 0.65328(15) -1.3355(3) -0.17941(13) 0.0505(8) Uani 1 1 d . . .
H31A H 0.6678 -1.3846 -0.2010 0.061 Uiso 1 1 calc R . .
H31B H 0.6196 -1.2868 -0.2088 0.061 Uiso 1 1 calc R . .
C32 C 0.63749(12) -1.4432(3) -0.14823(12) 0.0339(6) Uani 1 1 d . . .
C33 C 0.70957(13) -0.9466(3) -0.02906(12) 0.0485(8) Uani 1 1 d . . .
H33A H 0.7445 -0.9079 0.0029 0.058 Uiso 1 1 calc R . .
H33B H 0.6940 -1.0046 -0.0108 0.058 Uiso 1 1 calc R . .
C34 C 0.66981(11) -0.8273(3) -0.06149(12) 0.0338(6) 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
Ni1 O6 2.0388(18) . ?
Ni1 N4 2.054(2) . ?
Ni1 N2 2.069(2) 8_546 ?
Ni1 O3 2.0898(19) 1_565 ?
Ni1 O4 2.1477(19) 1_565 ?
Ni1 O5 2.2086(18) . ?
Ni1 C32 2.447(3) 1_565 ?
Ni1 C34 2.454(3) . ?
O1 C11 1.228(3) . ?
N1 C11 1.338(3) . ?
N1 C12 1.460(3) . ?
C1 C4 1.364(4) . ?
C1 C2 1.400(4) . ?
02 C18 1.232(3) . ?
N2 C16 1.324(3) . ?
N2 C17 1.334(3) . ?
N2 Ni1 2.069(2) 8_445 ?
C2 C3 1.365(4) . ?
O3 C32 1.277(3) . ?
O3 Ni1 2.0897(19) 1_545 ?
N3 C18 1.334(3) . ?
N3 C19 1.448(3) . ?
C3 C5 1.429(4) . ?
C3 C11 1.509(4) . ?
O4 C32 1.243(3) . ?
O4 Ni1 2.1477(19) 1_545 ?
N4 C22 1.331(3) . ?
N4 C23 1.331(3) . ?
C4 C6 1.436(4) . ?
C4 C18 1.502(3) . ?
O5 C34 1.259(3) . ?
C5 C6 1.415(4) . ?
C5 C7 1.420(4) . ?
O6 C34 1.270(3) . ?
C6 C8 1.420(4) . ?
C7 C9 1.361(4) . ?
C8 C10 1.370(4) . ?
C9 C10 1.402(4) . ?
C12 C13 1.501(4) . ?
C13 C14 1.380(4) . ?
C13 C15 1.382(4) . ?
C14 C17 1.381(4) . ?
C15 C16 1.378(4) . ?
C19 C20 1.505(3) . ?
C20 C24 1.381(4) . ?
C20 C21 1.387(4) . ?
C21 C22 1.377(4) . ?
C23 C24 1.372(4) . ?
C25 C26 1.368(4) . ?
C25 C27 1.382(4) . ?
C26 C28 1.380(4) . ?
C27 C29 1.392(4) . ?
C28 C30 1.392(4) . ?
C28 C31 1.500(4) . ?
C29 C30 1.383(4) . ?
C29 C33 1.501(4) . ?
C31 C32 1.512(4) . ?
C32 Ni1 2.447(3) 1_545 ?
C33 C34 1.506(4) . ?

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
O6 Ni1 N4 97.56(8) . . ?
O6 Ni1 N2 96.87(8) . 8_546 ?
N4 Ni1 N2 94.55(9) . 8_546 ?
O6 Ni1 O3 159.09(8) . 1_565 ?
N4 Ni1 O3 97.11(8) . 1_565 ?
N2 Ni1 O3 96.73(8) 8_546 1_565 ?
O6 Ni1 O4 101.47(7) . 1_565 ?
N4 Ni1 O4 158.45(8) . 1_565 ?
N2 Ni1 O4 93.12(8) 8_546 1_565 ?
O3 Ni1 O4 61.96(7) 1_565 1_565 ?
O6 Ni1 O5 61.87(7) . . ?
N4 Ni1 O5 91.60(8) . . ?
N2 Ni1 O5 158.51(8) 8_546 . ?
O3 Ni1 O5 102.93(7) 1_565 . ?
O4 Ni1 O5 88.56(7) 1_565 . ?
O6 Ni1 C32 130.85(9) . 1_565 ?
N4 Ni1 C32 128.37(9) . 1_565 ?
N2 Ni1 C32 95.91(9) 8_546 1_565 ?
O3 Ni1 C32 31.45(8) 1_565 1_565 ?
O4 Ni1 C32 30.51(8) 1_565 1_565 ?
O5 Ni1 C32 96.34(8) . 1_565 ?
O6 Ni1 C34 31.12(8) . . ?
N4 Ni1 C34 96.10(9) . . ?
N2 Ni1 C34 127.86(9) 8_546 . ?
O3 Ni1 C34 132.01(9) 1_565 . ?
O4 Ni1 C34 95.01(8) 1_565 . ?
O5 Ni1 C34 30.77(7) . . ?
C32 Ni1 C34 115.73(9) 1_565 . ?
C11 N1 C12 122.8(2) . . ?
C4 C1 C2 121.2(3) . . ?
C16 N2 C17 115.9(3) . . ?
C16 N2 Ni1 124.1(2) . 8_445 ?
C17 N2 Ni1 119.63(19) . 8_445 ?
C3 C2 C1 120.6(3) . . ?
C32 O3 Ni1 89.90(16) . 1_545 ?
C18 N3 C19 121.8(2) . . ?
C2 C3 C5 120.3(2) . . ?
C2 C3 C11 120.0(2) . . ?
C5 C3 C11 119.7(2) . . ?
C32 O4 Ni1 88.18(16) . 1_545 ?
C22 N4 C23 116.5(2) . . ?
C22 N4 Ni1 124.09(19) . . ?
C23 N4 Ni1 119.05(19) . . ?
C1 C4 C6 119.8(2) . . ?
C1 C4 C18 119.6(2) . . ?
C6 C4 C18 120.6(2) . . ?
C34 O5 Ni1 85.46(16) . . ?
C6 C5 C7 118.9(3) . . ?
C6 C5 C3 119.0(2) . . ?
C7 C5 C3 122.1(3) . . ?
C34 O6 Ni1 92.81(16) . . ?
C5 C6 C8 118.8(2) . . ?
C5 C6 C4 119.0(2) . . ?
C8 C6 C4 122.2(3) . . ?
C9 C7 C5 120.9(3) . . ?
C10 C8 C6 120.4(3) . . ?
C7 C9 C10 120.3(3) . . ?
C8 C10 C9 120.6(3) . . ?
O1 C11 N1 123.1(3) . . ?
O1 C11 C3 122.2(3) . . ?
N1 C11 C3 114.6(2) . . ?
N1 C12 C13 113.9(2) . . ?
C14 C13 C15 115.9(3) . . ?
C14 C13 C12 121.9(3) . . ?
C15 C13 C12 122.2(3) . . ?
C13 C14 C17 120.4(3) . . ?
C16 C15 C13 120.1(3) . . ?
N2 C16 C15 124.2(3) . . ?
N2 C17 C14 123.4(3) . . ?
02 C18 N3 123.0(3) . . ?
02 C18 C4 121.0(3) . . ?
N3 C18 C4 116.0(2) . . ?
N3 C19 C20 114.5(2) . . ?
C24 C20 C21 116.4(2) . . ?
C24 C20 C19 122.5(2) . . ?
C21 C20 C19 121.1(2) . . ?
C22 C21 C20 120.0(3) . . ?
N4 C22 C21 123.3(3) . . ?
N4 C23 C24 123.9(3) . . ?
C23 C24 C20 119.8(3) . . ?
C26 C25 C27 120.7(3) . . ?
C25 C26 C28 120.8(3) . . ?
C25 C27 C29 120.3(3) . . ?
C26 C28 C30 117.9(3) . . ?
C26 C28 C31 121.6(3) . . ?
C30 C28 C31 120.5(3) . . ?
C30 C29 C27 117.6(3) . . ?
C30 C29 C33 121.3(3) . . ?
C27 C29 C33 121.0(3) . . ?
C29 C30 C28 122.6(3) . . ?
C28 C31 C32 115.8(2) . . ?
O4 C32 O3 120.0(2) . . ?
O4 C32 C31 121.5(3) . . ?
O3 C32 C31 118.5(3) . . ?
O4 C32 Ni1 61.31(14) . 1_545 ?
O3 C32 Ni1 58.65(13) . 1_545 ?
C31 C32 Ni1 176.9(2) . 1_545 ?
C29 C33 C34 115.1(2) . . ?
O5 C34 O6 119.8(2) . . ?
O5 C34 C33 122.4(3) . . ?
O6 C34 C33 117.8(2) . . ?
O5 C34 Ni1 63.78(14) . . ?
O6 C34 Ni1 56.07(13) . . ?
C33 C34 Ni1 173.5(2) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        26.74
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.056
####################################################################### 
# 
# 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_01_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2040501'
loop_
_audit_author_name
_audit_author_address
Jing
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2020-12-01 deposited with the CCDC.	2021-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H22 Cu N4 O10'
_chemical_formula_weight         626.03

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.5279(7)
_cell_length_b                   11.1904(6)
_cell_length_c                   20.7164(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.0530(10)
_cell_angle_gamma                90.00
_cell_volume                     2882.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1774
_cell_measurement_theta_min      1.98
_cell_measurement_theta_max      28.24

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            Blue
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1284
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8869
_exptl_absorpt_correction_T_max  0.9152
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20762
_diffrn_reflns_av_R_equivalents  0.0906
_diffrn_reflns_av_unetI/netI     0.1119
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         28.24
_reflns_number_total             7121
_reflns_number_gt                3353
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0803P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7121
_refine_ls_number_parameters     379
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1448
_refine_ls_R_factor_gt           0.0598
_refine_ls_wR_factor_ref         0.1762
_refine_ls_wR_factor_gt          0.1369
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.61669(5) 0.26594(5) 0.14330(3) 0.0366(2) Uani 1 1 d . . .
O1 O 0.4782(3) 0.3847(3) 0.17016(16) 0.0468(9) Uani 1 1 d . . .
N1 N 0.6672(3) 0.2102(3) 0.23437(18) 0.0361(9) Uani 1 1 d . . .
O1W O 0.6565(3) -0.2214(3) 0.24595(17) 0.0554(10) Uani 1 1 d . . .
H1WA H 0.6943 -0.1672 0.2678 0.066 Uiso 1 1 d RD . .
H1WB H 0.7023 -0.2700 0.2326 0.066 Uiso 1 1 d R . .
O2 O 0.5911(3) 0.3077(3) 0.05237(15) 0.0424(8) Uani 1 1 d . . .
N2 N 0.7315(3) 1.1074(3) 0.65012(17) 0.0354(9) Uani 1 1 d . . .
O2W O 0.5634(3) 0.5595(3) 0.25559(17) 0.0561(10) Uani 1 1 d . . .
H2WA H 0.5461 0.5101 0.2249 0.067 Uiso 1 1 d R . .
H2WB H 0.5113 0.5633 0.2782 0.067 Uiso 1 1 d R . .
N3 N 0.9492(4) 0.7227(3) 0.6422(2) 0.0446(11) Uani 1 1 d . . .
H3A H 0.9730 0.7201 0.6030 0.054 Uiso 1 1 d R . .
O3 O 0.5311(3) 0.1231(3) 0.12964(15) 0.0479(9) Uani 1 1 d . . .
O3W O 0.4183(3) 0.1533(4) -0.13025(19) 0.0720(13) Uani 1 1 d . . .
H3WA H 0.4294 0.0787 -0.1252 0.086 Uiso 1 1 d R . .
H3WB H 0.4751 0.1896 -0.1143 0.086 Uiso 1 1 d R . .
N4 N 0.7659(3) 0.1627(3) 0.47974(18) 0.0394(10) Uani 1 1 d . . .
H4A H 0.7186 0.1764 0.5083 0.047 Uiso 1 1 d R . .
O4 O 0.4934(4) 0.3219(4) -0.04298(17) 0.0663(12) Uani 1 1 d . . .
C5 C 0.8717(4) 0.3218(4) 0.5340(2) 0.0370(11) Uani 1 1 d . . .
O5 O 0.4193(4) 0.0051(4) 0.0690(2) 0.0750(14) Uani 1 1 d . . .
C6 C 0.9837(4) 0.4466(4) 0.6130(2) 0.0379(11) Uani 1 1 d . . .
O7 O 0.8609(3) 0.6236(3) 0.71364(16) 0.0486(9) Uani 1 1 d . . .
O8 O 0.9291(3) 0.1987(3) 0.45000(17) 0.0558(10) Uani 1 1 d . . .
C20 C 0.8998(4) 0.6269(4) 0.6620(2) 0.0368(11) Uani 1 1 d . . .
C23 C 0.6829(5) 0.2409(4) 0.3490(2) 0.0454(13) Uani 1 1 d . . .
H23A H 0.6736 0.2946 0.3840 0.055 Uiso 1 1 d R . .
C24 C 0.7967(4) 0.4985(4) 0.5801(3) 0.0449(13) Uani 1 1 d . . .
H24A H 0.7447 0.4876 0.6099 0.054 Uiso 1 1 d R . .
C25 C 0.9722(4) 0.3433(4) 0.5718(2) 0.0371(11) Uani 1 1 d . . .
C26 C 1.1556(5) 0.2907(5) 0.6089(3) 0.0619(17) Uani 1 1 d . . .
H26A H 1.2136 0.2344 0.6098 0.074 Uiso 1 1 d R . .
C27 C 0.7204(4) 0.1268(4) 0.3615(2) 0.0350(11) Uani 1 1 d . . .
C28 C 0.7864(4) 0.3981(4) 0.5381(2) 0.0406(12) Uani 1 1 d . . .
H28A H 0.7209 0.3832 0.5100 0.049 Uiso 1 1 d R . .
C29 C 0.7070(4) 0.9963(4) 0.6306(2) 0.0401(12) Uani 1 1 d . . .
H29A H 0.6346 0.9792 0.6121 0.048 Uiso 1 1 d R . .
C30 C 0.7059(4) 0.0992(4) 0.2463(2) 0.0374(12) Uani 1 1 d . . .
H30A H 0.7154 0.0500 0.2095 0.045 Uiso 1 1 d R . .
C31 C 0.5066(5) 0.2840(4) 0.0129(2) 0.0447(13) Uani 1 1 d . . .
C32 C 0.7417(4) 0.0746(4) 0.4289(2) 0.0419(13) Uani 1 1 d . . .
H32A H 0.6808 0.0280 0.4376 0.050 Uiso 1 1 d R . .
H32B H 0.8022 0.0215 0.4304 0.050 Uiso 1 1 d R . .
C34 C 0.9681(4) 0.8296(4) 0.6808(3) 0.0446(13) Uani 1 1 d . . .
H34A H 1.0374 0.8611 0.6748 0.054 Uiso 1 1 d R . .
H34B H 0.9701 0.8075 0.7257 0.054 Uiso 1 1 d R . .
C35 C 0.6583(4) 0.2797(4) 0.2859(2) 0.0437(13) Uani 1 1 d . . .
H35A H 0.6335 0.3603 0.2782 0.052 Uiso 1 1 d R . .
C36 C 0.8334(4) 1.1300(4) 0.6743(2) 0.0413(12) Uani 1 1 d . . .
H36A H 0.8519 1.2106 0.6870 0.050 Uiso 1 1 d R . .
C37 C 0.9122(4) 1.0443(4) 0.6823(2) 0.0420(12) Uani 1 1 d . . .
H37A H 0.9844 1.0645 0.6998 0.050 Uiso 1 1 d R . .
C38 C 0.8854(4) 0.9261(4) 0.6658(2) 0.0375(11) Uani 1 1 d . . .
C39 C 0.4588(5) 0.1024(5) 0.0804(3) 0.0508(14) Uani 1 1 d . . .
C40 C 0.4200(4) 0.2104(5) 0.0385(3) 0.0544(15) Uani 1 1 d . . .
H40A H 0.3745 0.1802 0.0015 0.065 Uiso 1 1 d R . .
H40B H 0.3770 0.2612 0.0623 0.065 Uiso 1 1 d R . .
C41 C 1.0626(4) 0.2657(5) 0.5735(3) 0.0515(14) Uani 1 1 d . . .
H41A H 1.0540 0.1929 0.5489 0.062 Uiso 1 1 d R . .
C42 C 1.1687(5) 0.3952(6) 0.6472(3) 0.0665(18) Uani 1 1 d . . .
H42A H 1.2385 0.4163 0.6686 0.080 Uiso 1 1 d R . .
C102 C 0.7368(4) 0.0600(4) 0.3088(2) 0.0381(12) Uani 1 1 d . . .
H10A H 0.7660 -0.0192 0.3148 0.046 Uiso 1 1 d RD . .
C105 C 0.8588(4) 0.2227(4) 0.4851(2) 0.0383(11) Uani 1 1 d . . .
C110 C 1.0841(4) 0.4708(5) 0.6490(3) 0.0499(14) Uani 1 1 d . . .
H11A H 1.0907 0.5398 0.6768 0.060 Uiso 1 1 d R . .
C111 C 0.8930(4) 0.5217(4) 0.6169(2) 0.0361(11) Uani 1 1 d . . .
C112 C 0.7814(4) 0.9043(4) 0.6373(2) 0.0420(12) Uani 1 1 d . . .
H11B H 0.7607 0.8247 0.6238 0.050 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O3 1.926(3) . ?
Cu1 O2 1.929(3) . ?
Cu1 N2 2.012(4) 4_575 ?
Cu1 N1 2.014(4) . ?
Cu1 O1 2.307(3) . ?
N1 C35 1.337(6) . ?
N1 C30 1.345(6) . ?
O2 C31 1.283(6) . ?
N2 C29 1.331(5) . ?
N2 C36 1.337(6) . ?
N2 Cu1 2.012(4) 4_576 ?
N3 C20 1.328(6) . ?
N3 C34 1.442(6) . ?
O3 C39 1.300(6) . ?
N4 C105 1.335(6) . ?
N4 C32 1.447(6) . ?
O4 C31 1.224(6) . ?
C5 C28 1.379(7) . ?
C5 C25 1.420(7) . ?
C5 C105 1.497(7) . ?
O5 C39 1.207(6) . ?
C6 C110 1.407(7) . ?
C6 C111 1.424(6) . ?
C6 C25 1.433(6) . ?
O7 C20 1.229(5) . ?
O8 C105 1.238(6) . ?
C20 C111 1.500(6) . ?
C23 C27 1.375(6) . ?
C23 C35 1.375(6) . ?
C24 C111 1.370(7) . ?
C24 C28 1.416(7) . ?
C25 C41 1.424(7) . ?
C26 C41 1.329(7) . ?
C26 C42 1.411(8) . ?
C27 C102 1.358(6) . ?
C27 C32 1.507(6) . ?
C29 C112 1.384(6) . ?
C30 C102 1.377(6) . ?
C31 C40 1.510(8) . ?
C34 C38 1.502(6) . ?
C36 C37 1.372(7) . ?
C37 C38 1.396(6) . ?
C38 C112 1.385(7) . ?
C39 C40 1.531(7) . ?
C42 C110 1.361(7) . ?

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
O3 Cu1 O2 91.98(14) . . ?
O3 Cu1 N2 167.20(16) . 4_575 ?
O2 Cu1 N2 85.98(14) . 4_575 ?
O3 Cu1 N1 89.17(14) . . ?
O2 Cu1 N1 170.17(16) . . ?
N2 Cu1 N1 90.75(15) 4_575 . ?
O3 Cu1 O1 95.28(15) . . ?
O2 Cu1 O1 93.22(13) . . ?
N2 Cu1 O1 97.45(14) 4_575 . ?
N1 Cu1 O1 96.39(14) . . ?
C35 N1 C30 117.0(4) . . ?
C35 N1 Cu1 121.4(3) . . ?
C30 N1 Cu1 121.6(3) . . ?
C31 O2 Cu1 126.7(3) . . ?
C29 N2 C36 117.6(4) . . ?
C29 N2 Cu1 120.0(3) . 4_576 ?
C36 N2 Cu1 122.3(3) . 4_576 ?
C20 N3 C34 123.4(4) . . ?
C39 O3 Cu1 125.8(3) . . ?
C105 N4 C32 120.3(4) . . ?
C28 C5 C25 120.1(4) . . ?
C28 C5 C105 118.7(4) . . ?
C25 C5 C105 121.0(4) . . ?
C110 C6 C111 121.6(5) . . ?
C110 C6 C25 119.3(4) . . ?
C111 C6 C25 119.1(4) . . ?
O7 C20 N3 122.9(5) . . ?
O7 C20 C111 121.4(4) . . ?
N3 C20 C111 115.7(4) . . ?
C27 C23 C35 120.2(4) . . ?
C111 C24 C28 119.9(5) . . ?
C5 C25 C41 123.9(4) . . ?
C5 C25 C6 118.9(4) . . ?
C41 C25 C6 117.1(5) . . ?
C41 C26 C42 121.2(5) . . ?
C102 C27 C23 116.2(4) . . ?
C102 C27 C32 120.3(4) . . ?
C23 C27 C32 123.5(4) . . ?
C5 C28 C24 121.1(5) . . ?
N2 C29 C112 122.5(4) . . ?
N1 C30 C102 121.4(4) . . ?
O4 C31 O2 122.4(5) . . ?
O4 C31 C40 120.1(5) . . ?
O2 C31 C40 117.4(4) . . ?
N4 C32 C27 114.1(4) . . ?
N3 C34 C38 114.8(4) . . ?
N1 C35 C23 122.9(5) . . ?
N2 C36 C37 123.6(4) . . ?
C36 C37 C38 119.0(5) . . ?
C112 C38 C37 117.1(5) . . ?
C112 C38 C34 123.4(4) . . ?
C37 C38 C34 119.5(4) . . ?
O5 C39 O3 122.9(5) . . ?
O5 C39 C40 120.5(5) . . ?
O3 C39 C40 116.5(5) . . ?
C31 C40 C39 116.0(5) . . ?
C26 C41 C25 121.8(5) . . ?
C110 C42 C26 119.6(5) . . ?
C27 C102 C30 121.8(5) . . ?
O8 C105 N4 121.2(5) . . ?
O8 C105 C5 122.1(5) . . ?
N4 C105 C5 116.7(4) . . ?
C42 C110 C6 120.9(5) . . ?
C24 C111 C6 120.7(4) . . ?
C24 C111 C20 118.3(4) . . ?
C6 C111 C20 121.0(4) . . ?
C29 C112 C38 119.9(4) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.24
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.084
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2040502'
loop_
_audit_author_name
_audit_author_address
Jing
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2020-12-01 deposited with the CCDC.	2021-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H36 Cu N4 O7'
_chemical_formula_weight         664.20

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2388(8)
_cell_length_b                   11.4778(8)
_cell_length_c                   12.7315(10)
_cell_angle_alpha                93.977(2)
_cell_angle_beta                 105.839(2)
_cell_angle_gamma                95.628(2)
_cell_volume                     1564.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1289
_cell_measurement_theta_min      1.67
_cell_measurement_theta_max      25.00

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            Blue
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             694
_exptl_absorpt_coefficient_mu    0.753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8955
_exptl_absorpt_correction_T_max  0.9218
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9008
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0844
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5513
_reflns_number_gt                3659
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0682P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5513
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0547
_refine_ls_wR_factor_ref         0.1379
_refine_ls_wR_factor_gt          0.1230
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_restrained_S_all      0.990
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu -0.33297(5) 0.19003(4) 0.51328(4) 0.02965(18) Uani 1 1 d . . .
O1W O -0.3545(3) 0.0050(2) 0.4378(2) 0.0434(8) Uani 1 1 d . . .
H1WA H -0.2986 -0.0127 0.4081 0.052 Uiso 1 1 d R . .
H1WB H -0.4212 -0.0396 0.4053 0.052 Uiso 1 1 d R . .
O1 O -0.2344(3) 0.2688(2) 0.4280(2) 0.0385(7) Uani 1 1 d . . .
N1 N -0.1714(3) 0.1675(3) 0.6221(3) 0.0313(8) Uani 1 1 d . . .
C1 C 0.5715(4) 0.2523(4) 0.6758(3) 0.0331(10) Uani 1 1 d . . .
N2 N 0.2012(3) 0.0148(3) 0.8757(3) 0.0331(9) Uani 1 1 d . . .
H2C H 0.2185 -0.0365 0.8313 0.040 Uiso 1 1 calc R . .
O2 O -0.2336(3) 0.1170(3) 0.3101(3) 0.0517(9) Uani 1 1 d . . .
C2 C 0.4833(4) 0.2592(4) 0.7458(4) 0.0468(12) Uani 1 1 d . . .
H2A H 0.5293 0.2927 0.8194 0.056 Uiso 1 1 calc R . .
H2B H 0.4460 0.1805 0.7504 0.056 Uiso 1 1 calc R . .
O3 O 0.6429(3) 0.3404(2) 0.6721(3) 0.0425(8) Uani 1 1 d . . .
N3 N 0.2141(3) -0.5349(3) 1.1455(3) 0.0368(9) Uani 1 1 d . . .
H3C H 0.2306 -0.4773 1.1961 0.044 Uiso 1 1 calc R . .
C3 C 0.3766(4) 0.3374(4) 0.6965(4) 0.0499(13) Uani 1 1 d . . .
H3A H 0.3319 0.3533 0.7502 0.060 Uiso 1 1 calc R . .
H3B H 0.4140 0.4122 0.6820 0.060 Uiso 1 1 calc R . .
O4 O 0.5668(2) 0.1547(2) 0.6174(2) 0.0334(7) Uani 1 1 d . . .
N4 N 0.5120(3) -0.7641(3) 1.4084(3) 0.0302(8) Uani 1 1 d . . .
C4 C 0.2851(4) 0.2778(4) 0.5911(4) 0.0525(13) Uani 1 1 d . . .
H4A H 0.2418 0.2068 0.6069 0.063 Uiso 1 1 calc R . .
H4B H 0.3307 0.2552 0.5398 0.063 Uiso 1 1 calc R . .
O5 O 0.1673(3) 0.0519(2) 1.0398(2) 0.0452(8) Uani 1 1 d . . .
C5 C 0.1897(5) 0.3581(4) 0.5380(4) 0.0578(15) Uani 1 1 d . . .
H5A H 0.2311 0.4216 0.5096 0.069 Uiso 1 1 calc R . .
H5B H 0.1553 0.3926 0.5932 0.069 Uiso 1 1 calc R . .
O6 O 0.1878(3) -0.5873(2) 0.9650(2) 0.0457(8) Uani 1 1 d . . .
C6 C 0.0830(5) 0.2911(4) 0.4441(4) 0.0544(14) Uani 1 1 d . . .
H6A H 0.0390 0.2304 0.4735 0.065 Uiso 1 1 calc R . .
H6B H 0.1181 0.2528 0.3911 0.065 Uiso 1 1 calc R . .
C7 C -0.0110(5) 0.3721(4) 0.3847(4) 0.0563(14) Uani 1 1 d . . .
H7A H -0.0405 0.4158 0.4385 0.068 Uiso 1 1 calc R . .
H7B H 0.0313 0.4283 0.3494 0.068 Uiso 1 1 calc R . .
C8 C -0.1228(4) 0.3028(4) 0.2983(4) 0.0468(12) Uani 1 1 d . . .
H8A H -0.1734 0.3578 0.2580 0.056 Uiso 1 1 calc R . .
H8B H -0.0929 0.2561 0.2466 0.056 Uiso 1 1 calc R . .
C9 C -0.2034(4) 0.2220(4) 0.3478(4) 0.0346(11) Uani 1 1 d . . .
C10 C -0.0879(4) 0.2600(4) 0.6682(4) 0.0381(11) Uani 1 1 d . . .
H10A H -0.1077 0.3344 0.6510 0.046 Uiso 1 1 calc R . .
C11 C 0.0257(4) 0.2511(4) 0.7399(3) 0.0334(10) Uani 1 1 d . . .
H11A H 0.0804 0.3186 0.7707 0.040 Uiso 1 1 calc R . .
C12 C 0.0591(4) 0.1415(3) 0.7664(3) 0.0271(9) Uani 1 1 d . . .
C13 C -0.0268(4) 0.0474(4) 0.7187(4) 0.0516(14) Uani 1 1 d . . .
H13A H -0.0091 -0.0280 0.7342 0.062 Uiso 1 1 calc R . .
C14 C -0.1393(4) 0.0627(4) 0.6477(4) 0.0492(13) Uani 1 1 d . . .
H14A H -0.1956 -0.0035 0.6162 0.059 Uiso 1 1 calc R . .
C15 C 0.1847(4) 0.1316(3) 0.8433(4) 0.0360(11) Uani 1 1 d . . .
H15A H 0.2483 0.1562 0.8082 0.043 Uiso 1 1 calc R . .
H15B H 0.1974 0.1854 0.9087 0.043 Uiso 1 1 calc R . .
C16 C 0.1905(4) -0.0163(3) 0.9723(3) 0.0296(10) Uani 1 1 d . . .
C17 C 0.2048(4) -0.1428(3) 0.9921(3) 0.0272(9) Uani 1 1 d . . .
C18 C 0.1158(4) -0.2015(4) 1.0292(3) 0.0349(11) Uani 1 1 d . . .
H18A H 0.0525 -0.1617 1.0428 0.042 Uiso 1 1 calc R . .
C19 C 0.1169(4) -0.3211(3) 1.0476(3) 0.0324(10) Uani 1 1 d . . .
H19A H 0.0563 -0.3588 1.0750 0.039 Uiso 1 1 calc R . .
C20 C 0.2074(4) -0.3816(3) 1.0251(3) 0.0288(10) Uani 1 1 d . . .
C21 C 0.3020(4) -0.3246(3) 0.9848(3) 0.0277(9) Uani 1 1 d . . .
C22 C 0.3037(3) -0.2023(3) 0.9719(3) 0.0280(10) Uani 1 1 d . . .
C23 C 0.4066(4) -0.1450(4) 0.9440(4) 0.0385(11) Uani 1 1 d . . .
H23A H 0.4110 -0.0645 0.9380 0.046 Uiso 1 1 calc R . .
C24 C 0.4986(4) -0.2037(4) 0.9257(4) 0.0510(13) Uani 1 1 d . . .
H24A H 0.5655 -0.1635 0.9084 0.061 Uiso 1 1 calc R . .
C25 C 0.4931(4) -0.3253(4) 0.9330(5) 0.0541(14) Uani 1 1 d . . .
H25A H 0.5554 -0.3658 0.9184 0.065 Uiso 1 1 calc R . .
C26 C 0.3981(4) -0.3842(4) 0.9610(4) 0.0423(12) Uani 1 1 d . . .
H26A H 0.3955 -0.4650 0.9647 0.051 Uiso 1 1 calc R . .
C27 C 0.2031(3) -0.5120(3) 1.0414(4) 0.0291(10) Uani 1 1 d . . .
C28 C 0.1988(4) -0.6547(4) 1.1748(4) 0.0394(11) Uani 1 1 d . . .
H28A H 0.1804 -0.7084 1.1086 0.047 Uiso 1 1 calc R . .
H28B H 0.1273 -0.6638 1.2036 0.047 Uiso 1 1 calc R . .
C29 C 0.3094(4) -0.6903(3) 1.2579(3) 0.0283(9) Uani 1 1 d . . .
C30 C 0.3164(4) -0.8077(4) 1.2722(3) 0.0357(11) Uani 1 1 d . . .
H30A H 0.2529 -0.8644 1.2311 0.043 Uiso 1 1 calc R . .
C31 C 0.4173(4) -0.8405(4) 1.3472(4) 0.0368(11) Uani 1 1 d . . .
H31A H 0.4197 -0.9201 1.3558 0.044 Uiso 1 1 calc R . .
C32 C 0.5043(4) -0.6509(4) 1.3959(4) 0.0424(12) Uani 1 1 d . . .
H32A H 0.5690 -0.5960 1.4381 0.051 Uiso 1 1 calc R . .
C33 C 0.4054(4) -0.6108(4) 1.3235(4) 0.0401(12) Uani 1 1 d . . .
H33A H 0.4033 -0.5305 1.3189 0.048 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.954(3) . ?
Cu1 O4 1.998(3) 1_455 ?
Cu1 N1 2.013(3) . ?
Cu1 N4 2.026(3) 1_464 ?
Cu1 O1W 2.232(3) . ?
O1 C9 1.268(5) . ?
N1 C14 1.326(5) . ?
N1 C10 1.330(5) . ?
C1 O3 1.240(5) . ?
C1 O4 1.289(5) . ?
C1 C2 1.507(6) . ?
N2 C16 1.337(5) . ?
N2 C15 1.444(5) . ?
O2 C9 1.245(5) . ?
C2 C3 1.587(6) . ?
N3 C27 1.344(5) . ?
N3 C28 1.455(5) . ?
C3 C4 1.519(6) . ?
O4 Cu1 1.998(3) 1_655 ?
N4 C32 1.328(5) . ?
N4 C31 1.334(5) . ?
N4 Cu1 2.026(3) 1_646 ?
C4 C5 1.530(6) . ?
O5 C16 1.220(5) . ?
C5 C6 1.538(6) . ?
O6 C27 1.219(5) . ?
C6 C7 1.551(6) . ?
C7 C8 1.533(6) . ?
C8 C9 1.518(6) . ?
C10 C11 1.370(5) . ?
C11 C12 1.385(5) . ?
C12 C13 1.360(6) . ?
C12 C15 1.503(5) . ?
C13 C14 1.374(6) . ?
C16 C17 1.507(5) . ?
C17 C18 1.360(6) . ?
C17 C22 1.431(5) . ?
C18 C19 1.409(5) . ?
C19 C20 1.367(5) . ?
C20 C21 1.425(6) . ?
C20 C27 1.523(5) . ?
C21 C26 1.421(5) . ?
C21 C22 1.423(5) . ?
C22 C23 1.416(6) . ?
C23 C24 1.349(6) . ?
C24 C25 1.402(6) . ?
C25 C26 1.350(6) . ?
C28 C29 1.507(5) . ?
C29 C30 1.380(5) . ?
C29 C33 1.379(6) . ?
C30 C31 1.372(5) . ?
C32 C33 1.377(6) . ?

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 O4 164.27(11) . 1_455 ?
O1 Cu1 N1 87.74(13) . . ?
O4 Cu1 N1 93.26(13) 1_455 . ?
O1 Cu1 N4 88.52(13) . 1_464 ?
O4 Cu1 N4 88.56(13) 1_455 1_464 ?
N1 Cu1 N4 172.39(13) . 1_464 ?
O1 Cu1 O1W 100.22(12) . . ?
O4 Cu1 O1W 95.45(11) 1_455 . ?
N1 Cu1 O1W 91.22(12) . . ?
N4 Cu1 O1W 95.97(12) 1_464 . ?
C9 O1 Cu1 126.4(3) . . ?
C14 N1 C10 116.6(4) . . ?
C14 N1 Cu1 123.3(3) . . ?
C10 N1 Cu1 120.1(3) . . ?
O3 C1 O4 121.5(4) . . ?
O3 C1 C2 120.0(4) . . ?
O4 C1 C2 118.3(4) . . ?
C16 N2 C15 122.2(3) . . ?
C1 C2 C3 111.3(4) . . ?
C27 N3 C28 121.8(4) . . ?
C4 C3 C2 112.2(4) . . ?
C1 O4 Cu1 106.3(3) . 1_655 ?
C32 N4 C31 116.8(3) . . ?
C32 N4 Cu1 118.7(3) . 1_646 ?
C31 N4 Cu1 124.4(3) . 1_646 ?
C3 C4 C5 112.0(4) . . ?
C4 C5 C6 112.0(4) . . ?
C5 C6 C7 112.9(4) . . ?
C8 C7 C6 112.4(4) . . ?
C9 C8 C7 112.9(4) . . ?
O2 C9 O1 124.4(4) . . ?
O2 C9 C8 120.0(4) . . ?
O1 C9 C8 115.6(4) . . ?
N1 C10 C11 123.3(4) . . ?
C10 C11 C12 120.0(4) . . ?
C13 C12 C11 116.3(4) . . ?
C13 C12 C15 123.8(4) . . ?
C11 C12 C15 119.9(4) . . ?
C12 C13 C14 120.7(4) . . ?
N1 C14 C13 123.1(4) . . ?
N2 C15 C12 114.2(3) . . ?
O5 C16 N2 122.6(4) . . ?
O5 C16 C17 121.4(4) . . ?
N2 C16 C17 115.9(4) . . ?
C18 C17 C22 119.8(4) . . ?
C18 C17 C16 116.4(4) . . ?
C22 C17 C16 123.7(4) . . ?
C17 C18 C19 121.7(4) . . ?
C20 C19 C18 119.8(4) . . ?
C19 C20 C21 120.7(4) . . ?
C19 C20 C27 118.6(4) . . ?
C21 C20 C27 120.7(4) . . ?
C26 C21 C22 118.5(4) . . ?
C26 C21 C20 122.4(4) . . ?
C22 C21 C20 119.0(4) . . ?
C23 C22 C21 117.8(4) . . ?
C23 C22 C17 123.4(4) . . ?
C21 C22 C17 118.8(4) . . ?
C24 C23 C22 122.0(4) . . ?
C23 C24 C25 119.9(4) . . ?
C26 C25 C24 120.7(4) . . ?
C25 C26 C21 121.0(4) . . ?
O6 C27 N3 124.1(4) . . ?
O6 C27 C20 121.8(4) . . ?
N3 C27 C20 114.0(4) . . ?
N3 C28 C29 115.3(3) . . ?
C30 C29 C33 116.9(4) . . ?
C30 C29 C28 119.6(4) . . ?
C33 C29 C28 123.5(4) . . ?
C31 C30 C29 119.8(4) . . ?
N4 C31 C30 123.3(4) . . ?
N4 C32 C33 123.3(4) . . ?
C32 C33 C29 119.8(4) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.077
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2040500'
loop_
_audit_author_name
_audit_author_address
Jing
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2020-12-01 deposited with the CCDC.	2021-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H36 Cu N4 O9'
_chemical_formula_sum            'C40 H36 Cu N4 O9'
_chemical_formula_weight         780.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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+1/2, -z'

_cell_length_a                   9.0605(6)
_cell_length_b                   14.3095(9)
_cell_length_c                   15.1659(10)
_cell_angle_alpha                90
_cell_angle_beta                 104.665(1)
_cell_angle_gamma                90
_cell_volume                     1902.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    1462
_cell_measurement_theta_min      2.3235
_cell_measurement_theta_max      18.4076

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_F_000             810
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.634
_shelx_estimated_absorpt_T_min   0.911
_shelx_estimated_absorpt_T_max   0.933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.875
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10949
_diffrn_reflns_av_unetI/netI     0.0877
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.388
_diffrn_reflns_theta_max         25.030
_diffrn_reflns_theta_full        25.030
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_point_group_measured_fraction_full 0.884
_reflns_number_total             5928
_reflns_number_gt                3568
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.697
_reflns_Friedel_fraction_max     0.759
_reflns_Friedel_fraction_full    0.760

_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       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0845P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 1122 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.019(12)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5928
_refine_ls_number_parameters     488
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1146
_refine_ls_R_factor_gt           0.0612
_refine_ls_wR_factor_ref         0.1682
_refine_ls_wR_factor_gt          0.1418
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.18637(11) 0.88819(11) 0.85622(7) 0.0613(4) Uani 1 1 d . . . . .
O1W O 0.0042(9) 0.7583(6) 0.8076(6) 0.101(3) Uani 1 1 d . . . . .
H1A H -0.0230 0.7879 0.7524 0.121 Uiso 1 1 d R U . . .
H1B H 0.0610 0.7079 0.7998 0.121 Uiso 1 1 d R U . . .
O1 O 0.4569(13) 0.7787(8) 0.4696(6) 0.119(4) Uani 1 1 d . . . . .
O2 O 0.8645(7) 1.0849(5) 0.2246(4) 0.0662(19) Uani 1 1 d . . . . .
O3 O 0.1256(9) 0.9741(6) 0.7541(5) 0.081(2) Uani 1 1 d . . . . .
O4 O -0.0213(11) 0.8762(9) 0.6616(6) 0.112(3) Uani 1 1 d . . . . .
O5 O -0.224(2) 1.0417(12) 0.6261(11) 0.217(8) Uani 1 1 d . . . . .
O6 O 0.2710(8) 0.8083(5) 0.9594(4) 0.0578(17) Uani 1 1 d . . . . .
O7 O 0.4190(10) 0.9278(6) 1.0060(6) 0.077(2) Uani 1 1 d . . . . .
O8 O 0.6279(13) 0.7442(9) 0.9973(10) 0.144(4) Uani 1 1 d . . . . .
N1 N 0.3453(9) 0.8432(7) 0.7938(5) 0.064(2) Uani 1 1 d . . . . .
N2 N 0.6726(12) 0.8229(7) 0.5689(7) 0.078(3) Uani 1 1 d . . . . .
H2 H 0.7474 0.8618 0.5806 0.094 Uiso 1 1 calc R U . . .
N3 N 0.6718(9) 1.0220(6) 0.1179(6) 0.057(2) Uani 1 1 d . . . . .
H3 H 0.5986 0.9820 0.1069 0.069 Uiso 1 1 calc R U . . .
N4 N 1.0337(9) 0.9478(6) -0.0826(5) 0.058(2) Uani 1 1 d . . . . .
C1 C 0.3140(15) 0.7726(9) 0.7376(10) 0.091(4) Uani 1 1 d . . . . .
H1 H 0.2229 0.7403 0.7314 0.110 Uiso 1 1 calc R U . . .
C2 C 0.4159(17) 0.7445(8) 0.6862(10) 0.093(4) Uani 1 1 d . . . . .
H2A H 0.3900 0.6941 0.6465 0.112 Uiso 1 1 calc R U . . .
C3 C 0.5490(15) 0.7883(9) 0.6929(8) 0.073(3) Uani 1 1 d . . . . .
C4 C 0.5788(15) 0.8584(14) 0.7516(11) 0.133(8) Uani 1 1 d . . . . .
H4 H 0.6698 0.8911 0.7591 0.159 Uiso 1 1 calc R U . . .
C5 C 0.4778(13) 0.8846(16) 0.8025(9) 0.123(5) Uani 1 1 d . . . . .
H5 H 0.5050 0.9331 0.8443 0.148 Uiso 1 1 calc R U . . .
C6 C 0.6590(18) 0.7557(11) 0.6397(11) 0.107(5) Uani 1 1 d . . . . .
H6A H 0.7587 0.7464 0.6812 0.128 Uiso 1 1 calc R U . . .
H6B H 0.6248 0.6961 0.6114 0.128 Uiso 1 1 calc R U . . .
C7 C 0.5751(16) 0.8261(11) 0.4884(9) 0.086(4) Uani 1 1 d . . . . .
C8 C 0.6131(10) 0.8882(11) 0.4178(6) 0.070(3) Uani 1 1 d . . . . .
C9 C 0.4989(11) 0.9399(8) 0.3537(7) 0.064(3) Uani 1 1 d . . . . .
C10 C 0.3471(13) 0.9423(10) 0.3633(8) 0.083(4) Uani 1 1 d . U . . .
H10 H 0.3201 0.9106 0.4104 0.099 Uiso 1 1 calc R U . . .
C11 C 0.2422(14) 0.9926(11) 0.3010(11) 0.104(5) Uani 1 1 d . U . . .
H11 H 0.1422 0.9944 0.3063 0.125 Uiso 1 1 calc R U . . .
C12 C 0.2780(13) 1.0414(10) 0.2296(10) 0.094(4) Uani 1 1 d . . . . .
H12 H 0.2031 1.0744 0.1881 0.113 Uiso 1 1 calc R U . . .
C13 C 0.4245(11) 1.0401(9) 0.2215(8) 0.072(3) Uani 1 1 d . . . . .
H13 H 0.4497 1.0734 0.1747 0.086 Uiso 1 1 calc R U . . .
C14 C 0.5380(10) 0.9890(7) 0.2830(7) 0.053(2) Uani 1 1 d . . . . .
C15 C 0.6951(10) 0.9859(7) 0.2775(6) 0.054(2) Uani 1 1 d . . . . .
C16 C 0.8026(11) 0.9414(9) 0.3433(7) 0.071(3) Uani 1 1 d . . . . .
H16 H 0.9043 0.9431 0.3411 0.085 Uiso 1 1 calc R U . . .
C17 C 0.7626(10) 0.8937(11) 0.4134(6) 0.074(3) Uani 1 1 d . . . . .
H17 H 0.8382 0.8649 0.4582 0.089 Uiso 1 1 calc R U . . .
C18 C 0.7494(10) 1.0357(7) 0.2039(7) 0.048(2) Uani 1 1 d . . . . .
C19 C 0.7045(11) 1.0709(7) 0.0428(6) 0.055(3) Uani 1 1 d . . . . .
H19A H 0.7394 1.1332 0.0630 0.066 Uiso 1 1 calc R U . . .
H19B H 0.6102 1.0774 -0.0044 0.066 Uiso 1 1 calc R U . . .
C20 C 0.8216(10) 1.0262(7) 0.0013(6) 0.046(2) Uani 1 1 d . . . . .
C21 C 0.8488(15) 1.0643(9) -0.0745(8) 0.097(5) Uani 1 1 d . . . . .
H21 H 0.7961 1.1175 -0.1001 0.117 Uiso 1 1 calc R U . . .
C22 C 0.9549(15) 1.0240(10) -0.1139(8) 0.093(4) Uani 1 1 d . . . . .
H22 H 0.9720 1.0521 -0.1657 0.111 Uiso 1 1 calc R U . . .
C23 C 1.0040(14) 0.9102(9) -0.0105(8) 0.091(5) Uani 1 1 d . . . . .
H23 H 1.0547 0.8557 0.0133 0.109 Uiso 1 1 calc R U . . .
C24 C 0.8972(14) 0.9497(10) 0.0324(8) 0.096(4) Uani 1 1 d . . . . .
H24 H 0.8800 0.9209 0.0838 0.115 Uiso 1 1 calc R U . . .
C25 C 0.0385(15) 0.9542(11) 0.6786(9) 0.080(4) Uani 1 1 d . . . . .
C26 C 0.0200(15) 1.0282(9) 0.6090(8) 0.077(3) Uani 1 1 d . . . . .
C27 C -0.105(3) 1.0779(17) 0.5880(13) 0.180(10) Uani 1 1 d . . . . .
C28 C -0.133(3) 1.1500(17) 0.5195(16) 0.190(11) Uani 1 1 d . . . . .
H28 H -0.2234 1.1837 0.5055 0.228 Uiso 1 1 calc R U . . .
C29 C -0.023(4) 1.1665(19) 0.4770(14) 0.175(12) Uani 1 1 d . . . . .
H29 H -0.0337 1.2151 0.4352 0.209 Uiso 1 1 calc R U . . .
C30 C 0.096(3) 1.1153(18) 0.4939(14) 0.145(8) Uani 1 1 d . . . . .
H30 H 0.1692 1.1278 0.4623 0.174 Uiso 1 1 calc R U . . .
C31 C 0.125(2) 1.0390(13) 0.5590(11) 0.123(5) Uani 1 1 d . . . . .
H31 H 0.2092 1.0001 0.5662 0.147 Uiso 1 1 calc R U . . .
C32 C -0.390(3) 1.0673(18) 0.5898(19) 0.243(15) Uani 1 1 d . . . . .
H32A H -0.3991 1.1313 0.5865 0.291 Uiso 1 1 calc R U . . .
H32B H -0.4450 1.0442 0.6280 0.291 Uiso 1 1 calc R U . . .
H32C H -0.4257 1.0422 0.5325 0.291 Uiso 1 1 calc R U . . .
C33 C 0.3837(13) 0.8459(9) 1.0146(7) 0.053(3) Uani 1 1 d . . . . .
C34 C 0.4688(13) 0.7868(8) 1.0891(7) 0.068(3) Uani 1 1 d . . . . .
C35 C 0.5965(17) 0.7371(12) 1.0814(11) 0.101(5) Uani 1 1 d . . . . .
C36 C 0.669(2) 0.6787(14) 1.1471(14) 0.146(7) Uani 1 1 d . . . . .
H36 H 0.7489 0.6415 1.1396 0.175 Uiso 1 1 calc R U . . .
C37 C 0.620(3) 0.6754(16) 1.2264(14) 0.153(9) Uani 1 1 d . . . . .
H37 H 0.6722 0.6359 1.2726 0.183 Uiso 1 1 calc R U . . .
C38 C 0.505(3) 0.7244(15) 1.2413(13) 0.134(7) Uani 1 1 d . . . . .
H38 H 0.4803 0.7230 1.2970 0.161 Uiso 1 1 calc R U . . .
C39 C 0.424(2) 0.7781(10) 1.1688(9) 0.108(5) Uani 1 1 d . . . . .
H39 H 0.3368 0.8091 1.1745 0.130 Uiso 1 1 calc R U . . .
C40 C 0.7559(19) 0.6912(15) 0.9855(17) 0.190(10) Uani 1 1 d . . . . .
H40A H 0.8294 0.6874 1.0402 0.228 Uiso 1 1 d R U . . .
H40B H 0.7985 0.7202 0.9434 0.228 Uiso 1 1 d R U . . .
H40C H 0.7266 0.6317 0.9656 0.228 Uiso 1 1 d 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 O6 1.932(7) . ?
Cu1 O3 1.944(8) . ?
Cu1 N1 2.019(8) . ?
Cu1 N4 2.038(8) 1_456 ?
Cu1 O1W 2.471(9) . ?
O1W H1A 0.9135 . ?
O1W H1B 0.9107 . ?
O1 C7 1.238(14) . ?
O2 C18 1.231(11) . ?
O3 C25 1.247(14) . ?
O4 C25 1.240(17) . ?
O5 C27 1.45(2) . ?
O5 C32 1.50(2) . ?
O6 C33 1.264(13) . ?
O7 C33 1.230(11) . ?
O8 C35 1.380(18) . ?
O8 C40 1.435(17) . ?
N1 C1 1.306(14) . ?
N1 C5 1.315(15) . ?
N2 C7 1.315(15) . ?
N2 C6 1.470(15) . ?
N2 H2 0.8600 . ?
N3 C18 1.331(12) . ?
N3 C19 1.429(12) . ?
N3 H3 0.8600 . ?
N4 C23 1.306(12) . ?
N4 C22 1.324(14) . ?
N4 Cu1 2.038(8) 1_654 ?
C1 C2 1.410(17) . ?
C1 H1 0.9300 . ?
C2 C3 1.341(16) . ?
C2 H2A 0.9300 . ?
C3 C4 1.323(18) . ?
C3 C6 1.506(15) . ?
C4 C5 1.389(16) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.496(16) . ?
C8 C17 1.376(11) . ?
C8 C9 1.434(15) . ?
C9 C14 1.399(13) . ?
C9 C10 1.420(14) . ?
C10 C11 1.364(18) . ?
C10 H10 0.9300 . ?
C11 C12 1.393(19) . ?
C11 H11 0.9300 . ?
C12 C13 1.364(15) . ?
C12 H12 0.9300 . ?
C13 C14 1.406(15) . ?
C13 H13 0.9300 . ?
C14 C15 1.448(12) . ?
C15 C16 1.363(14) . ?
C15 C18 1.507(13) . ?
C16 C17 1.387(14) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C19 C20 1.506(13) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C24 1.314(14) . ?
C20 C21 1.350(13) . ?
C21 C22 1.380(15) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 C24 1.414(15) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C26 1.474(18) . ?
C26 C27 1.30(2) . ?
C26 C31 1.366(18) . ?
C27 C28 1.44(2) . ?
C28 C29 1.33(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.28(3) . ?
C29 H29 0.9300 . ?
C30 C31 1.45(3) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 H32A 0.9200 . ?
C32 H32B 0.9200 . ?
C32 H32C 0.9200 . ?
C33 C34 1.465(15) . ?
C34 C39 1.374(17) . ?
C34 C35 1.388(18) . ?
C35 C36 1.34(2) . ?
C36 C37 1.38(3) . ?
C36 H36 0.9300 . ?
C37 C38 1.32(3) . ?
C37 H37 0.9300 . ?
C38 C39 1.39(2) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C40 H40A 0.9248 . ?
C40 H40B 0.9229 . ?
C40 H40C 0.9191 . ?

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
O6 Cu1 O3 173.2(3) . . ?
O6 Cu1 N1 90.4(3) . . ?
O3 Cu1 N1 85.4(3) . . ?
O6 Cu1 N4 93.1(3) . 1_456 ?
O3 Cu1 N4 90.6(3) . 1_456 ?
N1 Cu1 N4 173.8(4) . 1_456 ?
O6 Cu1 O1W 84.0(3) . . ?
O3 Cu1 O1W 101.8(3) . . ?
N1 Cu1 O1W 97.0(3) . . ?
N4 Cu1 O1W 88.4(3) 1_456 . ?
Cu1 O1W H1A 85.9 . . ?
Cu1 O1W H1B 106.1 . . ?
H1A O1W H1B 106.2 . . ?
C25 O3 Cu1 124.9(10) . . ?
C27 O5 C32 122.9(17) . . ?
C33 O6 Cu1 111.9(7) . . ?
C35 O8 C40 116.0(16) . . ?
C1 N1 C5 117.2(11) . . ?
C1 N1 Cu1 119.3(8) . . ?
C5 N1 Cu1 123.4(9) . . ?
C7 N2 C6 122.7(12) . . ?
C7 N2 H2 118.6 . . ?
C6 N2 H2 118.6 . . ?
C18 N3 C19 123.1(8) . . ?
C18 N3 H3 118.5 . . ?
C19 N3 H3 118.5 . . ?
C23 N4 C22 115.7(9) . . ?
C23 N4 Cu1 121.1(8) . 1_654 ?
C22 N4 Cu1 123.2(7) . 1_654 ?
N1 C1 C2 121.1(12) . . ?
N1 C1 H1 119.4 . . ?
C2 C1 H1 119.4 . . ?
C3 C2 C1 121.8(12) . . ?
C3 C2 H2A 119.1 . . ?
C1 C2 H2A 119.1 . . ?
C4 C3 C2 115.6(10) . . ?
C4 C3 C6 123.1(13) . . ?
C2 C3 C6 121.3(13) . . ?
C3 C4 C5 121.9(13) . . ?
C3 C4 H4 119.1 . . ?
C5 C4 H4 119.1 . . ?
N1 C5 C4 122.4(14) . . ?
N1 C5 H5 118.8 . . ?
C4 C5 H5 118.8 . . ?
N2 C6 C3 112.2(11) . . ?
N2 C6 H6A 109.2 . . ?
C3 C6 H6A 109.2 . . ?
N2 C6 H6B 109.2 . . ?
C3 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
O1 C7 N2 122.2(12) . . ?
O1 C7 C8 120.2(12) . . ?
N2 C7 C8 117.5(12) . . ?
C17 C8 C9 119.1(10) . . ?
C17 C8 C7 118.5(11) . . ?
C9 C8 C7 122.3(9) . . ?
C14 C9 C10 120.4(11) . . ?
C14 C9 C8 120.0(8) . . ?
C10 C9 C8 119.6(10) . . ?
C11 C10 C9 117.7(11) . . ?
C11 C10 H10 121.2 . . ?
C9 C10 H10 121.2 . . ?
C10 C11 C12 123.0(11) . . ?
C10 C11 H11 118.5 . . ?
C12 C11 H11 118.5 . . ?
C13 C12 C11 119.1(13) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C12 C13 C14 120.8(12) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C9 C14 C13 119.0(9) . . ?
C9 C14 C15 118.2(9) . . ?
C13 C14 C15 122.8(9) . . ?
C16 C15 C14 120.2(9) . . ?
C16 C15 C18 117.1(8) . . ?
C14 C15 C18 122.6(9) . . ?
C15 C16 C17 120.9(9) . . ?
C15 C16 H16 119.5 . . ?
C17 C16 H16 119.5 . . ?
C8 C17 C16 121.2(10) . . ?
C8 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
O2 C18 N3 122.4(8) . . ?
O2 C18 C15 119.7(9) . . ?
N3 C18 C15 117.8(8) . . ?
N3 C19 C20 115.8(8) . . ?
N3 C19 H19A 108.3 . . ?
C20 C19 H19A 108.3 . . ?
N3 C19 H19B 108.3 . . ?
C20 C19 H19B 108.3 . . ?
H19A C19 H19B 107.4 . . ?
C24 C20 C21 116.8(10) . . ?
C24 C20 C19 124.2(9) . . ?
C21 C20 C19 118.9(9) . . ?
C20 C21 C22 119.8(11) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 H21 120.1 . . ?
N4 C22 C21 124.1(10) . . ?
N4 C22 H22 118.0 . . ?
C21 C22 H22 118.0 . . ?
N4 C23 C24 122.0(11) . . ?
N4 C23 H23 119.0 . . ?
C24 C23 H23 119.0 . . ?
C20 C24 C23 121.6(10) . . ?
C20 C24 H24 119.2 . . ?
C23 C24 H24 119.2 . . ?
O4 C25 O3 122.5(13) . . ?
O4 C25 C26 122.2(12) . . ?
O3 C25 C26 115.2(13) . . ?
C27 C26 C31 118.9(14) . . ?
C27 C26 C25 120.1(12) . . ?
C31 C26 C25 120.7(13) . . ?
C26 C27 C28 123.4(18) . . ?
C26 C27 O5 113.4(15) . . ?
C28 C27 O5 122(2) . . ?
C29 C28 C27 117(2) . . ?
C29 C28 H28 121.4 . . ?
C27 C28 H28 121.4 . . ?
C30 C29 C28 120(2) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C29 C30 C31 125(2) . . ?
C29 C30 H30 117.7 . . ?
C31 C30 H30 117.7 . . ?
C26 C31 C30 115.6(17) . . ?
C26 C31 H31 122.2 . . ?
C30 C31 H31 122.2 . . ?
O5 C32 H32A 109.5 . . ?
O5 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
O5 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O7 C33 O6 121.5(11) . . ?
O7 C33 C34 122.1(11) . . ?
O6 C33 C34 116.4(11) . . ?
C39 C34 C35 117.7(13) . . ?
C39 C34 C33 121.1(12) . . ?
C35 C34 C33 121.2(11) . . ?
C36 C35 O8 123.9(18) . . ?
C36 C35 C34 121.2(17) . . ?
O8 C35 C34 114.3(13) . . ?
C35 C36 C37 118(2) . . ?
C35 C36 H36 121.1 . . ?
C37 C36 H36 121.1 . . ?
C38 C37 C36 125(2) . . ?
C38 C37 H37 117.7 . . ?
C36 C37 H37 117.7 . . ?
C37 C38 C39 116(2) . . ?
C37 C38 H38 121.9 . . ?
C39 C38 H38 121.9 . . ?
C34 C39 C38 122.0(18) . . ?
C34 C39 H39 119.0 . . ?
C38 C39 H39 119.0 . . ?
O8 C40 H40A 109.9 . . ?
O8 C40 H40B 109.9 . . ?
H40A C40 H40B 108.4 . . ?
O8 C40 H40C 110.8 . . ?
H40A C40 H40C 108.8 . . ?
H40B C40 H40C 109.0 . . ?

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
C5 N1 C1 C2 -2(2) . . . . ?
Cu1 N1 C1 C2 174.0(10) . . . . ?
N1 C1 C2 C3 0(2) . . . . ?
C1 C2 C3 C4 1(2) . . . . ?
C1 C2 C3 C6 178.1(13) . . . . ?
C2 C3 C4 C5 0(2) . . . . ?
C6 C3 C4 C5 -177.3(16) . . . . ?
C1 N1 C5 C4 3(2) . . . . ?
Cu1 N1 C5 C4 -173.1(14) . . . . ?
C3 C4 C5 N1 -2(3) . . . . ?
C7 N2 C6 C3 -82.8(16) . . . . ?
C4 C3 C6 N2 -71.1(19) . . . . ?
C2 C3 C6 N2 111.9(15) . . . . ?
C6 N2 C7 O1 7(2) . . . . ?
C6 N2 C7 C8 -171.6(11) . . . . ?
O1 C7 C8 C17 -140.4(14) . . . . ?
N2 C7 C8 C17 38.3(18) . . . . ?
O1 C7 C8 C9 38(2) . . . . ?
N2 C7 C8 C9 -143.3(12) . . . . ?
C17 C8 C9 C14 5.3(18) . . . . ?
C7 C8 C9 C14 -173.1(11) . . . . ?
C17 C8 C9 C10 -173.7(12) . . . . ?
C7 C8 C9 C10 7.9(18) . . . . ?
C14 C9 C10 C11 0.8(18) . . . . ?
C8 C9 C10 C11 179.8(12) . . . . ?
C9 C10 C11 C12 0(2) . . . . ?
C10 C11 C12 C13 -1(2) . . . . ?
C11 C12 C13 C14 1.2(19) . . . . ?
C10 C9 C14 C13 -0.3(16) . . . . ?
C8 C9 C14 C13 -179.3(11) . . . . ?
C10 C9 C14 C15 178.7(10) . . . . ?
C8 C9 C14 C15 -0.3(15) . . . . ?
C12 C13 C14 C9 -0.7(17) . . . . ?
C12 C13 C14 C15 -179.6(11) . . . . ?
C9 C14 C15 C16 -4.3(15) . . . . ?
C13 C14 C15 C16 174.7(11) . . . . ?
C9 C14 C15 C18 179.7(9) . . . . ?
C13 C14 C15 C18 -1.4(15) . . . . ?
C14 C15 C16 C17 3.9(18) . . . . ?
C18 C15 C16 C17 -179.8(11) . . . . ?
C9 C8 C17 C16 -6(2) . . . . ?
C7 C8 C17 C16 172.6(13) . . . . ?
C15 C16 C17 C8 1(2) . . . . ?
C19 N3 C18 O2 -7.1(14) . . . . ?
C19 N3 C18 C15 174.9(8) . . . . ?
C16 C15 C18 O2 -44.9(14) . . . . ?
C14 C15 C18 O2 131.3(10) . . . . ?
C16 C15 C18 N3 133.2(10) . . . . ?
C14 C15 C18 N3 -50.6(13) . . . . ?
C18 N3 C19 C20 88.6(11) . . . . ?
N3 C19 C20 C24 -3.1(16) . . . . ?
N3 C19 C20 C21 174.5(10) . . . . ?
C24 C20 C21 C22 -2(2) . . . . ?
C19 C20 C21 C22 -179.5(12) . . . . ?
C23 N4 C22 C21 1(2) . . . . ?
Cu1 N4 C22 C21 178.6(11) 1_654 . . . ?
C20 C21 C22 N4 1(2) . . . . ?
C22 N4 C23 C24 -1.5(19) . . . . ?
Cu1 N4 C23 C24 -179.2(10) 1_654 . . . ?
C21 C20 C24 C23 1(2) . . . . ?
C19 C20 C24 C23 178.9(11) . . . . ?
N4 C23 C24 C20 0(2) . . . . ?
Cu1 O3 C25 O4 1.2(18) . . . . ?
Cu1 O3 C25 C26 -174.7(8) . . . . ?
O4 C25 C26 C27 80(2) . . . . ?
O3 C25 C26 C27 -104.4(19) . . . . ?
O4 C25 C26 C31 -93.4(17) . . . . ?
O3 C25 C26 C31 82.6(17) . . . . ?
C31 C26 C27 C28 -6(3) . . . . ?
C25 C26 C27 C28 -179(2) . . . . ?
C31 C26 C27 O5 162.6(17) . . . . ?
C25 C26 C27 O5 -11(3) . . . . ?
C32 O5 C27 C26 -161(2) . . . . ?
C32 O5 C27 C28 8(4) . . . . ?
C26 C27 C28 C29 -1(4) . . . . ?
O5 C27 C28 C29 -168(3) . . . . ?
C27 C28 C29 C30 4(5) . . . . ?
C28 C29 C30 C31 -1(5) . . . . ?
C27 C26 C31 C30 8(3) . . . . ?
C25 C26 C31 C30 -178.8(14) . . . . ?
C29 C30 C31 C26 -5(3) . . . . ?
Cu1 O6 C33 O7 7.9(14) . . . . ?
Cu1 O6 C33 C34 -172.4(8) . . . . ?
O7 C33 C34 C39 93.7(15) . . . . ?
O6 C33 C34 C39 -86.0(14) . . . . ?
O7 C33 C34 C35 -86.7(16) . . . . ?
O6 C33 C34 C35 93.5(14) . . . . ?
C40 O8 C35 C36 -6(2) . . . . ?
C40 O8 C35 C34 -177.8(14) . . . . ?
C39 C34 C35 C36 4(2) . . . . ?
C33 C34 C35 C36 -175.8(15) . . . . ?
C39 C34 C35 O8 175.7(13) . . . . ?
C33 C34 C35 O8 -3.8(19) . . . . ?
O8 C35 C36 C37 -176.7(18) . . . . ?
C34 C35 C36 C37 -6(3) . . . . ?
C35 C36 C37 C38 2(4) . . . . ?
C36 C37 C38 C39 4(4) . . . . ?
C35 C34 C39 C38 2(2) . . . . ?
C33 C34 C39 C38 -178.3(14) . . . . ?
C37 C38 C39 C34 -6(3) . . . . ?

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
N2 H2 O4 0.86 2.15 2.877(15) 142 1_655
N3 H3 O7 0.86 2.08 2.825(12) 144 1_554
O1W H1A O4 0.91 1.87 2.746(14) 159 .
O1W H1B O2 0.91 1.95 2.848(11) 166 2_646

_refine_diff_density_max         0.587
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.063

####################################################################### 
# 
# 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_01_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2040499'
loop_
_audit_author_name
_audit_author_address
Jing
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2020-12-01 deposited with the CCDC.	2021-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Cu N6 O10'
_chemical_formula_weight         792.20

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   26.608(6)
_cell_length_b                   13.302(2)
_cell_length_c                   21.946(4)
_cell_angle_alpha                90
_cell_angle_beta                 111.863(7)
_cell_angle_gamma                90
_cell_volume                     7209(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1180
_cell_measurement_theta_min      1.649
_cell_measurement_theta_max      25.131

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_F_000             3256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.674
_shelx_estimated_absorpt_T_min   0.906
_shelx_estimated_absorpt_T_max   0.930
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20019
_diffrn_reflns_av_unetI/netI     0.1090
_diffrn_reflns_av_R_equivalents  0.0939
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.649
_diffrn_reflns_theta_max         25.131
_diffrn_reflns_theta_full        25.131
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.979
_reflns_number_total             6312
_reflns_number_gt                2883
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0635P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6312
_refine_ls_number_parameters     496
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1486
_refine_ls_R_factor_gt           0.0532
_refine_ls_wR_factor_ref         0.1499
_refine_ls_wR_factor_gt          0.1125
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_restrained_S_all      0.926
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu -0.05219(3) -0.08084(4) 0.65126(3) 0.0521(2) Uani 1 1 d . . . . .
C1 C 0.1462(2) 0.0545(4) 0.5782(2) 0.0599(14) Uani 1 1 d . . . . .
H1A H 0.1774 0.0188 0.6069 0.072 Uiso 1 1 d R U . . .
H1B H 0.1401 0.0350 0.5339 0.072 Uiso 1 1 d R U . . .
O1 O -0.03691(13) -0.2193(2) 0.64186(15) 0.0574(9) Uani 1 1 d . . . . .
N1 N 0.00924(17) -0.0390(3) 0.62440(19) 0.0520(11) Uani 1 1 d . . . . .
O2 O -0.06399(15) 0.0575(3) 0.66801(18) 0.0678(10) Uani 1 1 d . . . . .
N2 N 0.15788(16) 0.1605(3) 0.58697(19) 0.0566(11) Uani 1 1 d . . . . .
H2A H 0.1420 0.2010 0.5523 0.068 Uiso 1 1 d R U . . .
C3 C 0.1900(2) 0.2008(4) 0.6435(3) 0.0577(14) Uani 1 1 d . . . . .
N3 N 0.20382(16) 0.6900(3) 0.68404(19) 0.0591(12) Uani 1 1 d . . . . .
H3A H 0.2255 0.6623 0.7222 0.071 Uiso 1 1 d R U . . .
O3 O -0.09972(15) -0.2223(3) 0.54162(16) 0.0707(11) Uani 1 1 d . . . . .
O4 O -0.10845(16) 0.0702(3) 0.56103(19) 0.0789(12) Uani 1 1 d . . . . .
N4 N 0.09913(16) 0.8803(3) 0.79806(17) 0.0509(11) Uani 1 1 d . . . . .
O5 O 0.21248(15) 0.1493(3) 0.69289(17) 0.0778(12) Uani 1 1 d . . . . .
N5 N -0.0018(3) -0.6685(4) 0.5679(4) 0.116(2) Uani 1 1 d . . . . .
O6 O 0.1566(2) 0.6713(3) 0.57790(19) 0.1184(18) Uani 1 1 d . . . . .
N6 N -0.1348(4) 0.5139(5) 0.6590(4) 0.133(3) Uani 1 1 d . . . . .
O7 O -0.0232(2) -0.7139(4) 0.5172(3) 0.157(3) Uani 1 1 d . . . . .
O8 O 0.0326(3) -0.7042(4) 0.6168(4) 0.193(3) Uani 1 1 d . . . . .
O9 O -0.1664(4) 0.5610(5) 0.6166(4) 0.209(4) Uani 1 1 d . . . . .
C10 C 0.1908(2) 0.5235(4) 0.6388(2) 0.0544(14) Uani 1 1 d . . . . .
O10 O -0.1078(3) 0.5497(4) 0.7123(3) 0.168(3) Uani 1 1 d . . . . .
C11 C 0.22167(19) 0.3647(4) 0.6091(2) 0.0462(12) Uani 1 1 d . . . . .
C12 C 0.0975(2) 0.0235(4) 0.5932(2) 0.0485(13) Uani 1 1 d . . . . .
C13 C 0.16168(19) 0.8258(4) 0.7246(2) 0.0467(12) Uani 1 1 d . . . . .
C14 C -0.0482(2) -0.3694(4) 0.5820(2) 0.0494(13) Uani 1 1 d . . . . .
C18 C -0.0917(2) 0.1057(4) 0.6160(3) 0.0551(14) Uani 1 1 d . . . . .
C19 C 0.1825(2) 0.6347(4) 0.6311(3) 0.0657(16) Uani 1 1 d . . . . .
C20 C 0.0671(2) -0.0593(4) 0.5645(2) 0.0641(16) Uani 1 1 d . . . . .
H20A H 0.0765 -0.0972 0.5331 0.077 Uiso 1 1 d R U . . .
C21 C 0.1937(2) 0.3126(4) 0.6443(2) 0.0512(13) Uani 1 1 d . . . . .
C22 C 0.1687(2) 0.3658(4) 0.6774(3) 0.0706(16) Uani 1 1 d . . . . .
H22A H 0.1522 0.3311 0.7034 0.085 Uiso 1 1 d R U . . .
C23 C -0.1035(2) 0.2136(4) 0.6274(2) 0.0549(14) Uani 1 1 d . . . . .
C24 C 0.1678(2) 0.9173(4) 0.7552(2) 0.0592(14) Uani 1 1 d . . . . .
H24A H 0.1937 0.9642 0.7510 0.071 Uiso 1 1 d R U . . .
C27 C 0.2189(2) 0.4706(4) 0.6056(2) 0.0508(13) Uani 1 1 d . . . . .
C28 C 0.1945(2) 0.7970(4) 0.6845(2) 0.0632(15) Uani 1 1 d . . . . .
H28A H 0.1753 0.8171 0.6398 0.076 Uiso 1 1 d R U . . .
H28B H 0.2283 0.8327 0.7006 0.076 Uiso 1 1 d R U . . .
C29 C 0.1681(2) 0.4711(5) 0.6753(3) 0.0702(16) Uani 1 1 d . . . . .
H29A H 0.1505 0.5082 0.6992 0.084 Uiso 1 1 d R U . . .
C30 C -0.0638(2) -0.2628(4) 0.5871(3) 0.0505(13) Uani 1 1 d . . . . .
C31 C 0.0818(2) 0.0738(4) 0.6377(3) 0.0701(16) Uani 1 1 d . . . . .
H31A H 0.1012 0.1331 0.6585 0.084 Uiso 1 1 d R U . . .
C32 C -0.0806(2) 0.2564(4) 0.6881(2) 0.0795(19) Uani 1 1 d . . . . .
H32A H -0.0561 0.2173 0.7234 0.095 Uiso 1 1 d R U . . .
C33 C 0.1372(2) 0.9410(4) 0.7908(2) 0.0642(15) Uani 1 1 d . . . . .
H33A H 0.1433 1.0050 0.8125 0.077 Uiso 1 1 d R U . . .
C34 C 0.2529(2) 0.3107(4) 0.5791(3) 0.0656(16) Uani 1 1 d . . . . .
H34B H 0.2798 0.2748 0.6141 0.079 Uiso 1 1 d R U . . .
C35 C 0.0931(2) 0.7927(4) 0.7673(3) 0.0673(15) Uani 1 1 d . . . . .
H35A H 0.0663 0.7475 0.7712 0.081 Uiso 1 1 d R U . . .
C36 C -0.1468(3) 0.3689(5) 0.5864(3) 0.108(2) Uani 1 1 d . . . . .
H36A H -0.1683 0.4112 0.5508 0.129 Uiso 1 1 d R U . . .
C37 C -0.0608(3) -0.5261(5) 0.5229(3) 0.0830(19) Uani 1 1 d . . . . .
H37A H -0.0792 -0.5667 0.4849 0.100 Uiso 1 1 d R U . . .
C38 C -0.1247(3) 0.4083(4) 0.6475(3) 0.0823(19) Uani 1 1 d . . . . .
C39 C -0.1361(3) 0.2706(4) 0.5761(3) 0.0854(19) Uani 1 1 d . . . . .
H39A H -0.1515 0.2416 0.5330 0.102 Uiso 1 1 d R U . . .
C40 C 0.0244(2) -0.0882(4) 0.5806(2) 0.0667(16) Uani 1 1 d . . . . .
H40A H 0.0041 -0.1466 0.5595 0.080 Uiso 1 1 d R U . . .
C41 C 0.2465(2) 0.5209(5) 0.5710(3) 0.0730(17) Uani 1 1 d . . . . .
H41A H 0.2452 0.5930 0.5692 0.088 Uiso 1 1 d R U . . .
C42 C -0.0053(2) -0.4128(4) 0.6311(3) 0.0743(17) Uani 1 1 d . . . . .
H42A H 0.0138 -0.3747 0.6700 0.089 Uiso 1 1 d R U . . .
C43 C 0.1228(2) 0.7642(4) 0.7309(3) 0.0726(17) Uani 1 1 d . . . . .
H43A H 0.1163 0.7003 0.7091 0.087 Uiso 1 1 d R U . . .
C44 C -0.0758(2) -0.4275(4) 0.5281(3) 0.0718(16) Uani 1 1 d . . . . .
H44A H -0.1063 -0.3991 0.4933 0.086 Uiso 1 1 d R U . . .
C46 C -0.0179(3) -0.5629(4) 0.5723(4) 0.0765(18) Uani 1 1 d . . . . .
C47 C 0.0385(2) 0.0409(4) 0.6514(3) 0.0668(16) Uani 1 1 d . . . . .
H47A H 0.0290 0.0772 0.6834 0.080 Uiso 1 1 d R U . . .
C48 C 0.0102(3) -0.5094(5) 0.6257(3) 0.093(2) Uani 1 1 d . . . . .
H48A H 0.0411 -0.5386 0.6594 0.112 Uiso 1 1 d R U . . .
C53 C -0.0910(3) 0.3551(5) 0.6981(3) 0.095(2) Uani 1 1 d . . . . .
H53A H -0.0749 0.3852 0.7407 0.114 Uiso 1 1 d R U . . .
C55 C 0.2758(3) 0.4703(6) 0.5431(3) 0.092(2) Uani 1 1 d . . . . .
H55A H 0.2927 0.5053 0.5175 0.110 Uiso 1 1 d R U . . .
C56 C 0.2803(3) 0.3650(6) 0.5486(3) 0.086(2) Uani 1 1 d . . . . .
H56A H 0.3030 0.3307 0.5301 0.103 Uiso 1 1 d R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.913(3) . ?
Cu1 O2 1.925(3) . ?
Cu1 N1 2.011(4) . ?
Cu1 N4 2.025(4) 2_546 ?
C1 N2 1.441(6) . ?
C1 C12 1.508(6) . ?
O1 C30 1.286(5) . ?
N1 C47 1.320(6) . ?
N1 C40 1.343(6) . ?
O2 C18 1.278(6) . ?
N2 C3 1.330(6) . ?
C3 O5 1.232(5) . ?
C3 C21 1.490(7) . ?
N3 C19 1.312(6) . ?
N3 C28 1.445(6) . ?
O3 C30 1.220(5) . ?
O4 C18 1.214(5) . ?
N4 C35 1.327(6) . ?
N4 C33 1.349(6) . ?
N4 Cu1 2.024(4) 2_566 ?
N5 O7 1.206(7) . ?
N5 O8 1.218(8) . ?
N5 C46 1.483(7) . ?
O6 C19 1.215(6) . ?
N6 O9 1.175(8) . ?
N6 O10 1.219(8) . ?
N6 C38 1.469(8) . ?
C10 C29 1.360(7) . ?
C10 C27 1.411(6) . ?
C10 C19 1.496(7) . ?
C11 C27 1.412(6) . ?
C11 C34 1.431(6) . ?
C11 C21 1.434(6) . ?
C12 C31 1.371(6) . ?
C12 C20 1.373(6) . ?
C13 C43 1.367(6) . ?
C13 C24 1.370(6) . ?
C13 C28 1.503(6) . ?
C14 C42 1.372(6) . ?
C14 C44 1.374(6) . ?
C14 C30 1.493(6) . ?
C18 C23 1.511(6) . ?
C20 C40 1.364(7) . ?
C21 C22 1.353(6) . ?
C22 C29 1.401(7) . ?
C23 C39 1.366(7) . ?
C23 C32 1.367(6) . ?
C24 C33 1.358(6) . ?
C27 C41 1.406(7) . ?
C31 C47 1.368(7) . ?
C32 C53 1.375(7) . ?
C34 C56 1.365(7) . ?
C35 C43 1.368(6) . ?
C36 C38 1.353(8) . ?
C36 C39 1.374(7) . ?
C37 C46 1.339(7) . ?
C37 C44 1.389(7) . ?
C38 C53 1.341(8) . ?
C41 C55 1.340(8) . ?
C42 C48 1.367(7) . ?
C46 C48 1.336(8) . ?
C55 C56 1.406(8) . ?

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 O2 175.44(16) . . ?
O1 Cu1 N1 90.33(15) . . ?
O2 Cu1 N1 90.00(15) . . ?
O1 Cu1 N4 90.75(15) . 2_546 ?
O2 Cu1 N4 87.77(15) . 2_546 ?
N1 Cu1 N4 165.11(16) . 2_546 ?
N2 C1 C12 113.5(4) . . ?
C30 O1 Cu1 117.9(3) . . ?
C47 N1 C40 115.5(5) . . ?
C47 N1 Cu1 119.9(4) . . ?
C40 N1 Cu1 124.6(4) . . ?
C18 O2 Cu1 112.9(3) . . ?
C3 N2 C1 123.4(4) . . ?
O5 C3 N2 122.0(5) . . ?
O5 C3 C21 122.4(5) . . ?
N2 C3 C21 115.5(5) . . ?
C19 N3 C28 122.6(4) . . ?
C35 N4 C33 114.8(4) . . ?
C35 N4 Cu1 121.4(4) . 2_566 ?
C33 N4 Cu1 123.8(3) . 2_566 ?
O7 N5 O8 124.1(7) . . ?
O7 N5 C46 119.0(7) . . ?
O8 N5 C46 116.9(7) . . ?
O9 N6 O10 122.9(8) . . ?
O9 N6 C38 119.8(8) . . ?
O10 N6 C38 117.3(8) . . ?
C29 C10 C27 119.0(5) . . ?
C29 C10 C19 119.7(5) . . ?
C27 C10 C19 121.2(5) . . ?
C27 C11 C34 120.2(5) . . ?
C27 C11 C21 119.0(4) . . ?
C34 C11 C21 120.8(5) . . ?
C31 C12 C20 115.7(5) . . ?
C31 C12 C1 122.4(5) . . ?
C20 C12 C1 121.8(5) . . ?
C43 C13 C24 116.0(5) . . ?
C43 C13 C28 122.3(5) . . ?
C24 C13 C28 121.7(5) . . ?
C42 C14 C44 117.4(5) . . ?
C42 C14 C30 121.0(5) . . ?
C44 C14 C30 121.6(5) . . ?
O4 C18 O2 124.7(5) . . ?
O4 C18 C23 120.8(5) . . ?
O2 C18 C23 114.5(5) . . ?
O6 C19 N3 122.0(5) . . ?
O6 C19 C10 120.8(5) . . ?
N3 C19 C10 117.2(5) . . ?
C40 C20 C12 120.9(5) . . ?
C22 C21 C11 119.5(5) . . ?
C22 C21 C3 119.0(5) . . ?
C11 C21 C3 121.4(5) . . ?
C21 C22 C29 120.5(5) . . ?
C39 C23 C32 119.2(5) . . ?
C39 C23 C18 119.9(5) . . ?
C32 C23 C18 120.8(5) . . ?
C33 C24 C13 120.0(5) . . ?
C41 C27 C10 121.7(5) . . ?
C41 C27 C11 118.5(5) . . ?
C10 C27 C11 119.7(5) . . ?
N3 C28 C13 113.2(4) . . ?
C10 C29 C22 121.9(5) . . ?
O3 C30 O1 124.0(5) . . ?
O3 C30 C14 120.9(5) . . ?
O1 C30 C14 115.1(5) . . ?
C47 C31 C12 120.4(5) . . ?
C23 C32 C53 120.6(6) . . ?
N4 C33 C24 124.5(5) . . ?
C56 C34 C11 117.9(6) . . ?
N4 C35 C43 123.6(5) . . ?
C38 C36 C39 119.4(6) . . ?
C46 C37 C44 117.6(5) . . ?
C53 C38 C36 121.7(6) . . ?
C53 C38 N6 118.1(7) . . ?
C36 C38 N6 120.0(7) . . ?
C23 C39 C36 119.9(5) . . ?
N1 C40 C20 123.2(5) . . ?
C55 C41 C27 121.2(6) . . ?
C48 C42 C14 121.1(5) . . ?
C13 C43 C35 121.1(5) . . ?
C14 C44 C37 121.6(5) . . ?
C48 C46 C37 123.0(6) . . ?
C48 C46 N5 118.7(7) . . ?
C37 C46 N5 118.3(6) . . ?
N1 C47 C31 124.3(5) . . ?
C46 C48 C42 119.2(6) . . ?
C38 C53 C32 119.0(6) . . ?
C41 C55 C56 120.4(6) . . ?
C34 C56 C55 121.7(6) . . ?

_refine_diff_density_max         0.340
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.067

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 2042468'
loop_
_audit_author_name
_audit_author_address
Jing
;The Cambridge Crystallographic Data Centre
China
;
_audit_update_record             
;
2020-12-01 deposited with the CCDC.	2021-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H38 N4 Ni O8'
_chemical_formula_sum            'C40 H38 N4 Ni O8'
_chemical_formula_weight         761.43

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   23.655(4)
_cell_length_b                   8.6269(13)
_cell_length_c                   17.550(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.319(3)
_cell_angle_gamma                90
_cell_volume                     3580.5(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3665
_cell_measurement_theta_min      2.3215
_cell_measurement_theta_max      25.7103

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_F_000             1592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    0.602
_shelx_estimated_absorpt_T_min   0.931
_shelx_estimated_absorpt_T_max   0.948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9986
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.722
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.027
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3155
_reflns_number_gt                2442
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0880P)²+12.3358P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3155
_refine_ls_number_parameters     306
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0662
_refine_ls_wR_factor_ref         0.1865
_refine_ls_wR_factor_gt          0.1740
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.186
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001

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 0.2500 0.2500 0.5000 0.0514(3) Uani 1 2 d S . P . .
O1W O 0.24434(14) 0.4172(5) 0.41519(19) 0.0764(11) Uani 1 1 d . . . . .
H1A H 0.2157 0.4023 0.3852 0.092 Uiso 1 1 d R U . . .
H1B H 0.2749 0.4049 0.3903 0.092 Uiso 1 1 d R U . . .
O1 O 0.35661(17) 1.0307(4) 0.6674(2) 0.0893(13) Uani 1 1 d . . . . .
O2 O 0.16625(12) 0.2694(4) 0.5127(2) 0.0696(10) Uani 1 1 d . . . . .
O3 O 0.14865(14) 0.1377(7) 0.6172(2) 0.1042(17) Uani 1 1 d . . . . .
N1 N 0.26698(14) 0.4334(5) 0.5773(2) 0.0569(10) Uani 1 1 d . . . . .
N2 N 0.35002(16) 0.8446(5) 0.7547(2) 0.0590(10) Uani 1 1 d . . . . .
H2 H 0.3667 0.7963 0.7917 0.071 Uiso 1 1 calc R U . . .
C1 C 0.31087(17) 0.4359(5) 0.6264(3) 0.0558(12) Uani 1 1 d . . . . .
H1 H 0.3362 0.3534 0.6259 0.067 Uiso 1 1 calc R U . . .
C2 C 0.32070(18) 0.5530(5) 0.6774(3) 0.0568(12) Uani 1 1 d . . . . .
H2A H 0.3519 0.5486 0.7105 0.068 Uiso 1 1 calc R U . . .
C3 C 0.28434(17) 0.6778(6) 0.6797(2) 0.0524(11) Uani 1 1 d . . . . .
C4 C 0.2390(2) 0.6761(7) 0.6285(3) 0.0765(16) Uani 1 1 d . . . . .
H4 H 0.2133 0.7577 0.6275 0.092 Uiso 1 1 calc R U . . .
C5 C 0.2322(2) 0.5546(7) 0.5796(3) 0.0773(16) Uani 1 1 d . . . . .
H5 H 0.2013 0.5563 0.5458 0.093 Uiso 1 1 calc R U . . .
C6 C 0.29138(19) 0.8070(6) 0.7364(3) 0.0625(13) Uani 1 1 d . . . . .
H6A H 0.2727 0.8989 0.7163 0.075 Uiso 1 1 calc R U . . .
H6B H 0.2727 0.7782 0.7830 0.075 Uiso 1 1 calc R U . . .
C7 C 0.3788(2) 0.9500(5) 0.7169(3) 0.0548(11) Uani 1 1 d . . . . .
C8 C 0.4411(2) 0.9590(5) 0.7364(2) 0.0549(11) Uani 1 1 d . . . . .
C9 C 0.4709(2) 0.8275(6) 0.7434(4) 0.090(2) Uani 1 1 d . . . . .
H9 H 0.4520 0.7332 0.7392 0.107 Uiso 1 1 calc R U . . .
C10 C 0.4701(3) 1.1002(5) 0.7435(4) 0.085(2) Uani 1 1 d . U . . .
C11 C 0.4298(5) 1.2382(11) 0.7632(8) 0.066(3) Uani 0.5 1 d . U P A 1
H11A H 0.3906 1.2284 0.7628 0.079 Uiso 0.5 1 calc R U P A 1
C12 C 0.4561(5) 1.3706(13) 0.7805(10) 0.097(5) Uani 0.5 1 d . . P A 1
H12A H 0.4350 1.4607 0.7862 0.117 Uiso 0.5 1 d R U P A 1
C11' C 0.4541(4) 1.2477(11) 0.7147(7) 0.059(2) Uani 0.5 1 d . . P A 2
H11B H 0.4167 1.2559 0.6976 0.071 Uiso 0.5 1 calc R U P A 2
C12' C 0.4850(5) 1.3769(12) 0.7086(10) 0.090(4) Uani 0.5 1 d . . P A 2
H12B H 0.4679 1.4695 0.6930 0.108 Uiso 0.5 1 d R U P A 2
C13 C 0.13370(18) 0.2066(7) 0.5583(3) 0.0702(16) Uani 1 1 d . . . . .
C14 C 0.07121(16) 0.2181(7) 0.5400(3) 0.095(2) Uani 1 1 d D . . . .
C15 C 0.05330(18) 0.3041(6) 0.4774(3) 0.091(2) Uani 1 1 d D . . . .
H15 H 0.0817 0.3587 0.4533 0.109 Uiso 1 1 calc R U . B 1
C16 C 0.0010(3) 0.321(3) 0.4458(7) 0.090(6) Uani 0.5 1 d D . P C 1
H16 H -0.0048 0.3523 0.3955 0.108 Uiso 0.5 1 calc R U P C 1
C17 C -0.0442(3) 0.2886(14) 0.4942(6) 0.074(4) Uani 0.5 1 d D U P C 1
C18 C -0.0291(3) 0.2133(15) 0.5613(5) 0.074(3) Uani 0.5 1 d D U P C 1
H18 H -0.0576 0.1697 0.5899 0.089 Uiso 0.5 1 calc R U P C 1
C19 C 0.0261(3) 0.1994(12) 0.5882(4) 0.066(3) Uani 0.5 1 d D U P C 1
H19 H 0.0331 0.1771 0.6394 0.079 Uiso 0.5 1 calc R U P C 1
C20 C -0.1048(3) 0.3010(19) 0.4663(8) 0.095(5) Uani 0.5 1 d D . P C 1
H20A H -0.1087 0.2539 0.4169 0.143 Uiso 0.5 1 calc R U P C 1
H20B H -0.1154 0.4083 0.4630 0.143 Uiso 0.5 1 calc R U P C 1
H20C H -0.1289 0.2487 0.5013 0.143 Uiso 0.5 1 calc R U P C 1
C16' C -0.0084(3) 0.3102(19) 0.4734(9) 0.090(6) Uani 0.5 1 d D . P C 2
H16' H -0.0258 0.3885 0.4450 0.107 Uiso 0.5 1 calc R U P C 2
C17' C -0.0418(3) 0.2038(11) 0.5102(6) 0.060(3) Uani 0.5 1 d D . P C 2
C18' C -0.0204(3) 0.0989(11) 0.5645(5) 0.061(3) Uani 0.5 1 d D . P C 2
H18' H -0.0439 0.0306 0.5899 0.073 Uiso 0.5 1 calc R U P C 2
C19' C 0.0374(3) 0.1016(10) 0.5786(5) 0.056(2) Uani 0.5 1 d D U P C 2
H19' H 0.0544 0.0308 0.6119 0.067 Uiso 0.5 1 calc R U P C 2
C20' C -0.1066(3) 0.2056(17) 0.4968(9) 0.090(5) Uani 0.5 1 d D . P C 2
H20D H -0.1233 0.1228 0.5251 0.135 Uiso 0.5 1 calc R U P C 2
H20E H -0.1152 0.1921 0.4435 0.135 Uiso 0.5 1 calc R U P C 2
H20F H -0.1216 0.3029 0.5135 0.135 Uiso 0.5 1 calc R U P C 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 O2 2.006(3) . ?
Ni1 O2 2.006(3) 7_556 ?
Ni1 O1W 2.075(3) 7_556 ?
Ni1 O1W 2.075(3) . ?
Ni1 N1 2.116(4) 7_556 ?
Ni1 N1 2.116(4) . ?
O1W H1A 0.8575 . ?
O1W H1B 0.8600 . ?
O1 C7 1.222(5) . ?
O2 C13 1.247(6) . ?
O3 C13 1.236(7) . ?
N1 C5 1.332(6) . ?
N1 C1 1.334(5) . ?
N2 C7 1.323(6) . ?
N2 C6 1.453(6) . ?
N2 H2 0.8600 . ?
C1 C2 1.366(7) . ?
C1 H1 0.9300 . ?
C2 C3 1.379(6) . ?
C2 H2A 0.9300 . ?
C3 C4 1.383(7) . ?
C3 C6 1.501(7) . ?
C4 C5 1.362(8) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.507(6) . ?
C8 C9 1.339(6) . ?
C8 C10 1.402(7) . ?
C9 C9 1.393(10) 2_656 ?
C9 H9 0.9300 . ?
C10 C11' 1.417(11) . ?
C10 C10 1.428(11) 2_656 ?
C10 C11 1.569(14) . ?
C11 C12 1.332(14) . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9300 . ?
C11' C12' 1.337(15) . ?
C11' H11B 0.9300 . ?
C12' C12' 1.60(3) 2_656 ?
C12' H12B 0.9338 . ?
C13 C14 1.509(6) . ?
C14 C15 1.383(6) . ?
C14 C19' 1.461(7) . ?
C14 C19 1.386(7) . ?
C15 C16 1.353(7) . ?
C15 C16' 1.461(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.408(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.385(8) . ?
C17 C20 1.508(7) . ?
C18 C19 1.384(7) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C16' C17' 1.381(8) . ?
C16' H16' 0.9300 . ?
C17' C18' 1.401(8) . ?
C17' C20' 1.546(7) . ?
C18' C19' 1.384(7) . ?
C18' H18' 0.9300 . ?
C19' H19' 0.9300 . ?
C20' H20D 0.9600 . ?
C20' H20E 0.9600 . ?
C20' H20F 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni1 O2 180.0 . 7_556 ?
O2 Ni1 O1W 91.48(14) . 7_556 ?
O2 Ni1 O1W 88.52(14) 7_556 7_556 ?
O2 Ni1 O1W 88.52(14) . . ?
O2 Ni1 O1W 91.49(14) 7_556 . ?
O1W Ni1 O1W 180.0(2) 7_556 . ?
O2 Ni1 N1 87.72(14) . 7_556 ?
O2 Ni1 N1 92.28(14) 7_556 7_556 ?
O1W Ni1 N1 87.02(15) 7_556 7_556 ?
O1W Ni1 N1 92.97(15) . 7_556 ?
O2 Ni1 N1 92.28(14) . . ?
O2 Ni1 N1 87.72(14) 7_556 . ?
O1W Ni1 N1 92.97(15) 7_556 . ?
O1W Ni1 N1 87.03(15) . . ?
N1 Ni1 N1 180.00(15) 7_556 . ?
Ni1 O1W H1A 111.9 . . ?
Ni1 O1W H1B 103.7 . . ?
H1A O1W H1B 109.4 . . ?
C13 O2 Ni1 131.4(3) . . ?
C5 N1 C1 116.1(4) . . ?
C5 N1 Ni1 119.9(3) . . ?
C1 N1 Ni1 124.0(3) . . ?
C7 N2 C6 122.9(4) . . ?
C7 N2 H2 118.6 . . ?
C6 N2 H2 118.6 . . ?
N1 C1 C2 123.6(4) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C1 C2 C3 120.0(4) . . ?
C1 C2 H2A 120.0 . . ?
C3 C2 H2A 120.0 . . ?
C2 C3 C4 116.5(5) . . ?
C2 C3 C6 122.7(4) . . ?
C4 C3 C6 120.7(4) . . ?
C5 C4 C3 119.8(4) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
N1 C5 C4 124.0(5) . . ?
N1 C5 H5 118.0 . . ?
C4 C5 H5 118.0 . . ?
N2 C6 C3 113.8(3) . . ?
N2 C6 H6A 108.8 . . ?
C3 C6 H6A 108.8 . . ?
N2 C6 H6B 108.8 . . ?
C3 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
O1 C7 N2 122.0(5) . . ?
O1 C7 C8 122.3(5) . . ?
N2 C7 C8 115.7(4) . . ?
C9 C8 C10 118.2(5) . . ?
C9 C8 C7 119.1(4) . . ?
C10 C8 C7 122.6(4) . . ?
C8 C9 C9 122.1(3) . 2_656 ?
C8 C9 H9 119.0 . . ?
C9 C9 H9 119.0 2_656 . ?
C8 C10 C11' 128.5(5) . . ?
C8 C10 C10 119.7(3) . 2_656 ?
C11' C10 C10 108.2(6) . 2_656 ?
C8 C10 C11 112.4(6) . . ?
C10 C10 C11 124.7(4) 2_656 . ?
C12 C11 C10 114.7(10) . . ?
C12 C11 H11A 122.6 . . ?
C10 C11 H11A 122.6 . . ?
C11 C12 H12A 119.5 . . ?
C12' C11' C10 129.4(8) . . ?
C12' C11' H11B 115.3 . . ?
C10 C11' H11B 115.3 . . ?
C11' C12' C12' 99.2(12) . 2_656 ?
C11' C12' H12B 120.3 . . ?
C12' C12' H12B 116.5 2_656 . ?
O3 C13 O2 125.2(4) . . ?
O3 C13 C14 118.1(5) . . ?
O2 C13 C14 116.8(5) . . ?
C15 C14 C19' 125.2(4) . . ?
C15 C14 C19 108.8(5) . . ?
C15 C14 C13 119.0(4) . . ?
C19' C14 C13 113.5(5) . . ?
C19 C14 C13 128.7(5) . . ?
C16 C15 C14 130.1(6) . . ?
C14 C15 C16' 110.2(5) . . ?
C16 C15 H15 114.9 . . ?
C14 C15 H15 114.9 . . ?
C15 C16 C17 115.5(6) . . ?
C15 C16 H16 122.2 . . ?
C17 C16 H16 122.2 . . ?
C18 C17 C16 114.9(6) . . ?
C18 C17 C20 122.3(7) . . ?
C16 C17 C20 121.3(7) . . ?
C17 C18 C19 123.7(6) . . ?
C17 C18 H18 118.1 . . ?
C19 C18 H18 118.1 . . ?
C18 C19 C14 120.9(6) . . ?
C18 C19 H19 119.5 . . ?
C14 C19 H19 119.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17' C16' C15 122.3(7) . . ?
C17' C16' H16' 118.8 . . ?
C15 C16' H16' 118.8 . . ?
C16' C17' C18' 123.1(5) . . ?
C16' C17' C20' 119.9(7) . . ?
C18' C17' C20' 116.8(6) . . ?
C17' C18' C19' 116.8(6) . . ?
C17' C18' H18' 121.6 . . ?
C19' C18' H18' 121.6 . . ?
C14 C19' C18' 118.5(5) . . ?
C14 C19' H19' 120.8 . . ?
C18' C19' H19' 120.8 . . ?
C17' C20' H20D 109.5 . . ?
C17' C20' H20E 109.5 . . ?
H20D C20' H20E 109.5 . . ?
C17' C20' H20F 109.5 . . ?
H20D C20' H20F 109.5 . . ?
H20E C20' H20F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 0.6(7) . . . . ?
Ni1 N1 C1 C2 -178.3(3) . . . . ?
N1 C1 C2 C3 -0.3(7) . . . . ?
C1 C2 C3 C4 -0.2(7) . . . . ?
C1 C2 C3 C6 177.5(4) . . . . ?
C2 C3 C4 C5 0.4(8) . . . . ?
C6 C3 C4 C5 -177.3(5) . . . . ?
C1 N1 C5 C4 -0.4(8) . . . . ?
Ni1 N1 C5 C4 178.5(5) . . . . ?
C3 C4 C5 N1 -0.1(9) . . . . ?
C7 N2 C6 C3 90.7(5) . . . . ?
C2 C3 C6 N2 35.2(6) . . . . ?
C4 C3 C6 N2 -147.2(5) . . . . ?
C6 N2 C7 O1 5.3(7) . . . . ?
C6 N2 C7 C8 -172.1(4) . . . . ?
O1 C7 C8 C9 -133.0(6) . . . . ?
N2 C7 C8 C9 44.4(7) . . . . ?
O1 C7 C8 C10 43.4(7) . . . . ?
N2 C7 C8 C10 -139.2(5) . . . . ?
C10 C8 C9 C9 -0.6(12) . . . 2_656 ?
C7 C8 C9 C9 176.0(8) . . . 2_656 ?
C9 C8 C10 C11' 156.9(10) . . . . ?
C7 C8 C10 C11' -19.5(12) . . . . ?
C9 C8 C10 C10 1.0(11) . . . 2_656 ?
C7 C8 C10 C10 -175.4(7) . . . 2_656 ?
C9 C8 C10 C11 -159.6(7) . . . . ?
C7 C8 C10 C11 24.0(9) . . . . ?
C8 C10 C11 C12 171.5(11) . . . . ?
C10 C10 C11 C12 12.0(18) 2_656 . . . ?
C8 C10 C11' C12' -166.5(13) . . . . ?
C10 C10 C11' C12' -8.5(19) 2_656 . . . ?
C10 C11' C12' C12' -46(2) . . . 2_656 ?
Ni1 O2 C13 O3 15.0(9) . . . . ?
Ni1 O2 C13 C14 -165.7(3) . . . . ?
O3 C13 C14 C15 175.4(6) . . . . ?
O2 C13 C14 C15 -3.9(8) . . . . ?
O3 C13 C14 C19' -20.7(8) . . . . ?
O2 C13 C14 C19' 160.1(6) . . . . ?
O3 C13 C14 C19 19.0(11) . . . . ?
O2 C13 C14 C19 -160.3(8) . . . . ?
C19 C14 C15 C16 -25.5(16) . . . . ?
C13 C14 C15 C16 173.8(14) . . . . ?
C19' C14 C15 C16' 22.5(12) . . . . ?
C13 C14 C15 C16' -175.6(10) . . . . ?
C14 C15 C16 C17 22(3) . . . . ?
C15 C16 C17 C18 -13(3) . . . . ?
C15 C16 C17 C20 -179.3(13) . . . . ?
C16 C17 C18 C19 14(2) . . . . ?
C20 C17 C18 C19 179.7(13) . . . . ?
C17 C18 C19 C14 -19.6(19) . . . . ?
C15 C14 C19 C18 22.1(13) . . . . ?
C13 C14 C19 C18 -179.6(9) . . . . ?
C14 C15 C16' C17' -20(2) . . . . ?
C15 C16' C17' C18' 11(2) . . . . ?
C15 C16' C17' C20' -173.4(14) . . . . ?
C16' C17' C18' C19' -2.2(18) . . . . ?
C20' C17' C18' C19' -177.6(10) . . . . ?
C15 C14 C19' C18' -15.7(12) . . . . ?
C13 C14 C19' C18' -178.5(7) . . . . ?
C17' C18' C19' C14 3.6(13) . . . . ?

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
N2 H2 O3 0.86 2.14 2.871(6) 142 4_556
O1W H1A O1 0.86 2.01 2.801(5) 153 7_566
O1W H1B O3 0.86 1.85 2.650(5) 153 7_556

_refine_diff_density_max         0.780
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.067

