# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2019

####################################################################### 
# 
# 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_full
_database_code_depnum_ccdc_archive 'CCDC 1865962'
loop_
_audit_author_name
_audit_author_address

'Shiqun Xiang, Xiaofeng Zhang,Hui Chen, Yinghua Li, Weibin Fan and Deguang Huang'
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2018-09-05 deposited with the CCDC.	2019-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        '[Cu(Pz-COO)(Py)2]2  2H2O'
_chemical_name_common            '[Cu(Pz-COO)(Py)2]2  2H2O'
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H24 Cu2 N8 O4, 2(H2 O)'
_chemical_formula_sum            'C28 H28 Cu2 N8 O6'
_chemical_formula_weight         699.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'

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

_cell_length_a                   17.3539(3)
_cell_length_b                   8.80152(17)
_cell_length_c                   19.8411(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3030.55(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4357
_cell_measurement_theta_min      5.0970
_cell_measurement_theta_max      73.3050

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1432
_exptl_absorpt_coefficient_mu    2.202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7195
_exptl_absorpt_correction_T_max  0.7780
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6994
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         5.10
_diffrn_reflns_theta_max         69.98
_reflns_number_total             2851
_reflns_number_gt                2605
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0676P)²+0.9475P] 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         2851
_refine_ls_number_parameters     205
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.1063
_refine_ls_wR_factor_gt          0.1039
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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 0.053045(16) 0.35013(3) 0.058323(14) 0.02577(14) Uani 1 1 d . . .
O1 O -0.14108(8) 0.60985(17) -0.11870(7) 0.0323(3) Uani 1 1 d . . .
O2 O -0.22027(9) 0.42848(17) -0.15519(8) 0.0416(4) Uani 1 1 d . . .
N1 N -0.06690(9) 0.42745(19) -0.03835(8) 0.0251(3) Uani 1 1 d . . .
N2 N -0.03729(10) 0.31629(19) 0.00104(8) 0.0276(4) Uani 1 1 d . . .
N3 N 0.01618(10) 0.19989(18) 0.13071(8) 0.0283(4) Uani 1 1 d . . .
N4 N 0.12980(9) 0.2448(2) -0.01765(8) 0.0303(4) Uani 1 1 d . . .
C1 C -0.07429(13) 0.1865(2) -0.01389(11) 0.0332(4) Uani 1 1 d . . .
H1A H -0.0643 0.0910 0.0066 0.040 Uiso 1 1 calc R . .
C2 C -0.12879(13) 0.2115(2) -0.06319(10) 0.0324(5) Uani 1 1 d . . .
H2A H -0.1629 0.1400 -0.0831 0.039 Uiso 1 1 calc R . .
C3 C -0.12212(11) 0.3656(2) -0.07694(10) 0.0266(4) Uani 1 1 d . . .
C4 C -0.16459(11) 0.4725(2) -0.12062(10) 0.0286(4) Uani 1 1 d . . .
C5 C -0.05748(12) 0.1974(3) 0.15142(11) 0.0350(5) Uani 1 1 d . . .
H5A H -0.0938 0.2602 0.1289 0.042 Uiso 1 1 calc R . .
C6 C -0.08252(15) 0.1077(3) 0.20382(12) 0.0466(6) Uani 1 1 d . . .
H6A H -0.1349 0.1099 0.2176 0.056 Uiso 1 1 calc R . .
C7 C -0.03037(17) 0.0147(3) 0.23599(13) 0.0523(6) Uani 1 1 d . . .
H7A H -0.0463 -0.0489 0.2721 0.063 Uiso 1 1 calc R . .
C8 C 0.04551(16) 0.0154(3) 0.21485(13) 0.0468(6) Uani 1 1 d . . .
H8A H 0.0825 -0.0485 0.2359 0.056 Uiso 1 1 calc R . .
C9 C 0.06664(13) 0.1100(3) 0.16291(11) 0.0344(5) Uani 1 1 d . . .
H9A H 0.1191 0.1118 0.1493 0.041 Uiso 1 1 calc R . .
C10 C 0.11684(14) 0.2705(3) -0.08332(11) 0.0439(5) Uani 1 1 d . . .
H10A H 0.0720 0.3253 -0.0959 0.053 Uiso 1 1 calc R . .
C11 C 0.16600(15) 0.2206(3) -0.13333(12) 0.0502(6) Uani 1 1 d . . .
H11A H 0.1560 0.2446 -0.1792 0.060 Uiso 1 1 calc R . .
C12 C 0.22945(15) 0.1360(3) -0.11621(13) 0.0507(7) Uani 1 1 d . . .
H12A H 0.2633 0.0982 -0.1499 0.061 Uiso 1 1 calc R . .
C13 C 0.24285(15) 0.1071(3) -0.04880(13) 0.0494(6) Uani 1 1 d . . .
H13A H 0.2859 0.0480 -0.0351 0.059 Uiso 1 1 calc R . .
C14 C 0.19253(13) 0.1657(3) -0.00175(11) 0.0367(5) Uani 1 1 d . . .
H14A H 0.2033 0.1487 0.0446 0.044 Uiso 1 1 calc R . .
O3 O 0.28346(13) 0.3416(2) 0.23225(9) 0.0523(5) Uani 1 1 d . . .
H3A H 0.2593(19) 0.409(4) 0.2154(16) 0.063 Uiso 1 1 d . . .
H3B H 0.2834(19) 0.272(4) 0.2096(16) 0.063 Uiso 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
Cu1 N2 1.9590(16) . ?
Cu1 O1 1.9731(14) 5_565 ?
Cu1 N1 2.0118(17) 5_565 ?
Cu1 N3 2.0543(16) . ?
Cu1 N4 2.2149(17) . ?
O1 C4 1.276(2) . ?
O1 Cu1 1.9731(14) 5_565 ?
O2 C4 1.247(2) . ?
N1 C3 1.342(3) . ?
N1 N2 1.354(2) . ?
N1 Cu1 2.0118(17) 5_565 ?
N2 C1 1.343(3) . ?
N3 C9 1.342(3) . ?
N3 C5 1.343(3) . ?
N4 C14 1.330(3) . ?
N4 C10 1.341(3) . ?
C1 C2 1.378(3) . ?
C1 H1A 0.9500 . ?
C2 C3 1.388(3) . ?
C2 H2A 0.9500 . ?
C3 C4 1.477(3) . ?
C5 C6 1.376(3) . ?
C5 H5A 0.9500 . ?
C6 C7 1.377(4) . ?
C6 H6A 0.9500 . ?
C7 C8 1.382(4) . ?
C7 H7A 0.9500 . ?
C8 C9 1.375(3) . ?
C8 H8A 0.9500 . ?
C9 H9A 0.9500 . ?
C10 C11 1.380(3) . ?
C10 H10A 0.9500 . ?
C11 C12 1.372(4) . ?
C11 H11A 0.9500 . ?
C12 C13 1.381(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.379(3) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
O3 H3A 0.80(3) . ?
O3 H3B 0.76(3) . ?

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
N2 Cu1 O1 177.37(7) . 5_565 ?
N2 Cu1 N1 97.43(7) . 5_565 ?
O1 Cu1 N1 81.57(6) 5_565 5_565 ?
N2 Cu1 N3 93.35(7) . . ?
O1 Cu1 N3 86.08(6) 5_565 . ?
N1 Cu1 N3 143.25(7) 5_565 . ?
N2 Cu1 N4 91.31(7) . . ?
O1 Cu1 N4 91.28(6) 5_565 . ?
N1 Cu1 N4 101.62(7) 5_565 . ?
N3 Cu1 N4 113.18(7) . . ?
C4 O1 Cu1 115.77(12) . 5_565 ?
C3 N1 N2 107.88(16) . . ?
C3 N1 Cu1 111.58(13) . 5_565 ?
N2 N1 Cu1 140.51(13) . 5_565 ?
C1 N2 N1 107.80(16) . . ?
C1 N2 Cu1 129.77(14) . . ?
N1 N2 Cu1 121.93(13) . . ?
C9 N3 C5 117.76(18) . . ?
C9 N3 Cu1 120.61(14) . . ?
C5 N3 Cu1 121.39(14) . . ?
C14 N4 C10 117.11(19) . . ?
C14 N4 Cu1 123.36(14) . . ?
C10 N4 Cu1 119.32(15) . . ?
N2 C1 C2 110.42(18) . . ?
N2 C1 H1A 124.8 . . ?
C2 C1 H1A 124.8 . . ?
C1 C2 C3 103.77(18) . . ?
C1 C2 H2A 128.1 . . ?
C3 C2 H2A 128.1 . . ?
N1 C3 C2 110.11(18) . . ?
N1 C3 C4 115.62(17) . . ?
C2 C3 C4 134.16(19) . . ?
O2 C4 O1 123.97(18) . . ?
O2 C4 C3 120.76(18) . . ?
O1 C4 C3 115.26(17) . . ?
N3 C5 C6 122.8(2) . . ?
N3 C5 H5A 118.6 . . ?
C6 C5 H5A 118.6 . . ?
C5 C6 C7 118.9(2) . . ?
C5 C6 H6A 120.5 . . ?
C7 C6 H6A 120.5 . . ?
C6 C7 C8 118.9(2) . . ?
C6 C7 H7A 120.6 . . ?
C8 C7 H7A 120.6 . . ?
C9 C8 C7 119.0(2) . . ?
C9 C8 H8A 120.5 . . ?
C7 C8 H8A 120.5 . . ?
N3 C9 C8 122.7(2) . . ?
N3 C9 H9A 118.7 . . ?
C8 C9 H9A 118.7 . . ?
N4 C10 C11 122.8(2) . . ?
N4 C10 H10A 118.6 . . ?
C11 C10 H10A 118.6 . . ?
C12 C11 C10 119.4(2) . . ?
C12 C11 H11A 120.3 . . ?
C10 C11 H11A 120.3 . . ?
C11 C12 C13 118.3(2) . . ?
C11 C12 H12A 120.8 . . ?
C13 C12 H12A 120.8 . . ?
C14 C13 C12 118.7(2) . . ?
C14 C13 H13A 120.7 . . ?
C12 C13 H13A 120.7 . . ?
N4 C14 C13 123.6(2) . . ?
N4 C14 H14A 118.2 . . ?
C13 C14 H14A 118.2 . . ?
H3A O3 H3B 110(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N1 N2 C1 0.3(2) . . . . ?
Cu1 N1 N2 C1 -177.89(17) 5_565 . . . ?
C3 N1 N2 Cu1 172.96(13) . . . . ?
Cu1 N1 N2 Cu1 -5.3(3) 5_565 . . . ?
O1 Cu1 N2 C1 -118.4(14) 5_565 . . . ?
N1 Cu1 N2 C1 174.23(19) 5_565 . . . ?
N3 Cu1 N2 C1 -41.0(2) . . . . ?
N4 Cu1 N2 C1 72.3(2) . . . . ?
O1 Cu1 N2 N1 70.8(15) 5_565 . . . ?
N1 Cu1 N2 N1 3.37(18) 5_565 . . . ?
N3 Cu1 N2 N1 148.16(15) . . . . ?
N4 Cu1 N2 N1 -98.53(15) . . . . ?
N2 Cu1 N3 C9 142.19(16) . . . . ?
O1 Cu1 N3 C9 -40.38(16) 5_565 . . . ?
N1 Cu1 N3 C9 -110.66(17) 5_565 . . . ?
N4 Cu1 N3 C9 49.33(18) . . . . ?
N2 Cu1 N3 C5 -43.60(17) . . . . ?
O1 Cu1 N3 C5 133.83(17) 5_565 . . . ?
N1 Cu1 N3 C5 63.6(2) 5_565 . . . ?
N4 Cu1 N3 C5 -136.46(16) . . . . ?
N2 Cu1 N4 C14 -147.03(18) . . . . ?
O1 Cu1 N4 C14 33.46(18) 5_565 . . . ?
N1 Cu1 N4 C14 115.12(18) 5_565 . . . ?
N3 Cu1 N4 C14 -52.82(19) . . . . ?
N2 Cu1 N4 C10 38.40(18) . . . . ?
O1 Cu1 N4 C10 -141.11(17) 5_565 . . . ?
N1 Cu1 N4 C10 -59.45(18) 5_565 . . . ?
N3 Cu1 N4 C10 132.61(17) . . . . ?
N1 N2 C1 C2 -0.2(3) . . . . ?
Cu1 N2 C1 C2 -172.04(15) . . . . ?
N2 C1 C2 C3 0.0(3) . . . . ?
N2 N1 C3 C2 -0.4(2) . . . . ?
Cu1 N1 C3 C2 178.42(14) 5_565 . . . ?
N2 N1 C3 C4 176.37(16) . . . . ?
Cu1 N1 C3 C4 -4.8(2) 5_565 . . . ?
C1 C2 C3 N1 0.2(2) . . . . ?
C1 C2 C3 C4 -175.6(2) . . . . ?
Cu1 O1 C4 O2 178.74(17) 5_565 . . . ?
Cu1 O1 C4 C3 0.3(2) 5_565 . . . ?
N1 C3 C4 O2 -175.34(19) . . . . ?
C2 C3 C4 O2 0.4(4) . . . . ?
N1 C3 C4 O1 3.2(3) . . . . ?
C2 C3 C4 O1 178.9(2) . . . . ?
C9 N3 C5 C6 0.2(3) . . . . ?
Cu1 N3 C5 C6 -174.14(18) . . . . ?
N3 C5 C6 C7 -0.9(4) . . . . ?
C5 C6 C7 C8 0.5(4) . . . . ?
C6 C7 C8 C9 0.7(4) . . . . ?
C5 N3 C9 C8 1.0(3) . . . . ?
Cu1 N3 C9 C8 175.39(19) . . . . ?
C7 C8 C9 N3 -1.4(4) . . . . ?
C14 N4 C10 C11 -1.0(4) . . . . ?
Cu1 N4 C10 C11 173.9(2) . . . . ?
N4 C10 C11 C12 2.6(4) . . . . ?
C10 C11 C12 C13 -1.7(4) . . . . ?
C11 C12 C13 C14 -0.7(4) . . . . ?
C10 N4 C14 C13 -1.6(4) . . . . ?
Cu1 N4 C14 C13 -176.2(2) . . . . ?
C12 C13 C14 N4 2.4(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        69.98
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.075
####################################################################### 
# 
# 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_full_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1865967'
loop_
_audit_author_name
_audit_author_address

'Shiqun Xiang, Xiaofeng Zhang,Hui Chen, Yinghua Li, Weibin Fan and Deguang Huang'
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2018-09-05 deposited with the CCDC.	2019-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        '[Cu3(pdc)2(Py)6(H2O)2](H2O)'
_chemical_name_common            '[Cu3(pdc)2(Py)6(H2O)2](H2O)'
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H36 Cu3 N10 O10, 2(H2 O)'
_chemical_formula_sum            'C40 H40 Cu3 N10 O12'
_chemical_formula_weight         1043.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   9.5552(7)
_cell_length_b                   9.6001(7)
_cell_length_c                   12.4239(9)
_cell_angle_alpha                79.964(6)
_cell_angle_beta                 84.269(6)
_cell_angle_gamma                67.980(7)
_cell_volume                     1039.60(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3045
_cell_measurement_theta_min      4.9840
_cell_measurement_theta_max      73.4520

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             533
_exptl_absorpt_coefficient_mu    2.444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8285
_exptl_absorpt_correction_T_max  0.8672
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  Mirror
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6800
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.62
_diffrn_reflns_theta_max         69.99
_reflns_number_total             3916
_reflns_number_gt                3309
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0737P)²+1.1327P] 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         3916
_refine_ls_number_parameters     375
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.1285
_refine_ls_wR_factor_gt          0.1230
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.025
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.48548(5) 0.43605(5) 0.32193(4) 0.01295(16) Uani 1 1 d . . .
Cu2 Cu 0.5000 0.5000 0.0000 0.01339(18) Uani 1 2 d S . .
C1 C 0.1955(3) 0.7130(3) 0.3652(3) 0.0136(6) Uani 1 1 d . . .
C2 C 0.2283(3) 0.7076(3) 0.2455(3) 0.0127(6) Uani 1 1 d . . .
C3 C 0.1579(3) 0.8016(4) 0.1523(3) 0.0132(6) Uani 1 1 d . . .
C4 C 0.2474(3) 0.7342(3) 0.0654(2) 0.0123(6) Uani 1 1 d . . .
C5 C 0.7521(3) 0.2330(3) 0.0569(2) 0.0134(6) Uani 1 1 d . . .
C6 C 0.4198(4) 0.1825(4) 0.2644(3) 0.0212(7) Uani 1 1 d . . .
C7 C 0.3472(4) 0.0812(4) 0.2679(3) 0.0252(8) Uani 1 1 d . . .
C8 C 0.2197(4) 0.0971(4) 0.3348(3) 0.0259(8) Uani 1 1 d . . .
C9 C 0.1683(4) 0.2142(4) 0.3984(3) 0.0246(7) Uani 1 1 d . . .
C10 C 0.2459(4) 0.3118(4) 0.3901(3) 0.0221(7) Uani 1 1 d . . .
C11 C 0.7722(4) 0.4820(4) 0.2711(3) 0.0197(7) Uani 1 1 d . . .
C12 C 0.8793(4) 0.5497(4) 0.2645(3) 0.0215(7) Uani 1 1 d . . .
C13 C 0.8363(4) 0.6912(4) 0.2983(3) 0.0250(7) Uani 1 1 d . . .
C14 C 0.6908(4) 0.7580(4) 0.3367(3) 0.0236(7) Uani 1 1 d . . .
C15 C 0.5907(4) 0.6847(4) 0.3413(3) 0.0200(7) Uani 1 1 d . . .
C16 C 0.7966(4) 0.6171(4) -0.0470(3) 0.0197(7) Uani 1 1 d . . .
C17 C 0.8871(4) 0.7025(4) -0.0500(3) 0.0204(7) Uani 1 1 d . . .
C18 C 0.8327(4) 0.8329(4) -0.0014(3) 0.0198(7) Uani 1 1 d . . .
C19 C 0.6902(4) 0.8722(4) 0.0487(3) 0.0203(7) Uani 1 1 d . . .
C20 C 0.6073(4) 0.7807(4) 0.0485(3) 0.0190(7) Uani 1 1 d . . .
N1 N 0.3508(3) 0.5931(3) 0.2151(2) 0.0117(5) Uani 1 1 d . . .
N2 N 0.3619(3) 0.6091(3) 0.1067(2) 0.0130(5) Uani 1 1 d . . .
N3 N 0.3704(3) 0.2966(3) 0.3245(2) 0.0154(5) Uani 1 1 d . . .
N4 N 0.6307(3) 0.5472(3) 0.3088(2) 0.0147(5) Uani 1 1 d . . .
N5 N 0.6581(3) 0.6542(3) 0.0012(2) 0.0177(6) Uani 1 1 d . . .
O1 O 0.2940(2) 0.6074(2) 0.42634(17) 0.0151(5) Uani 1 1 d . . .
O2 O 0.0836(3) 0.8152(3) 0.39710(18) 0.0166(5) Uani 1 1 d . . .
O3 O 0.6421(2) 0.3289(2) 0.10492(17) 0.0144(4) Uani 1 1 d . . .
O4 O 0.8527(3) 0.1204(2) 0.10335(18) 0.0162(5) Uani 1 1 d . . .
O5 O 0.6214(3) 0.2756(3) 0.4257(2) 0.0159(5) Uani 1 1 d . . .
O6 O 0.8175(3) 0.0560(3) 0.3261(2) 0.0244(5) Uani 1 1 d D . .
H6A H 0.825(4) 0.078(4) 0.2576(10) 0.028(12) Uiso 1 1 d D . .
H6B H 0.903(3) -0.015(4) 0.342(3) 0.026(11) Uiso 1 1 d D . .
H18 H 0.892(4) 0.905(4) -0.002(3) 0.014(9) Uiso 1 1 d . . .
H12 H 0.981(5) 0.497(5) 0.237(3) 0.022(10) Uiso 1 1 d . . .
H3 H 0.083(5) 0.879(5) 0.151(3) 0.020(10) Uiso 1 1 d . . .
H8 H 0.175(5) 0.026(5) 0.334(4) 0.028(11) Uiso 1 1 d . . .
H17 H 0.976(5) 0.668(5) -0.082(3) 0.021(10) Uiso 1 1 d . . .
H10 H 0.213(5) 0.390(5) 0.432(4) 0.023(10) Uiso 1 1 d . . .
H16 H 0.833(5) 0.528(5) -0.076(4) 0.023(10) Uiso 1 1 d . . .
H15 H 0.489(5) 0.728(4) 0.366(3) 0.015(9) Uiso 1 1 d . . .
H13 H 0.905(5) 0.744(5) 0.296(3) 0.024(11) Uiso 1 1 d . . .
H20 H 0.515(5) 0.806(5) 0.083(4) 0.022(10) Uiso 1 1 d . . .
H19 H 0.646(5) 0.952(5) 0.083(4) 0.025(11) Uiso 1 1 d . . .
H14 H 0.650(5) 0.855(6) 0.346(4) 0.029(12) Uiso 1 1 d . . .
H5A H 0.672(5) 0.224(5) 0.398(4) 0.017(12) Uiso 1 1 d . . .
H9 H 0.086(5) 0.223(5) 0.450(4) 0.029(11) Uiso 1 1 d . . .
H6 H 0.499(6) 0.177(6) 0.224(4) 0.036(13) Uiso 1 1 d . . .
H11 H 0.793(5) 0.387(5) 0.252(4) 0.026(11) Uiso 1 1 d . . .
H7 H 0.380(6) 0.007(6) 0.217(4) 0.042(14) Uiso 1 1 d . . .
H5B H 0.662(5) 0.324(5) 0.462(4) 0.026(11) Uiso 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
Cu1 O5 1.965(2) . ?
Cu1 N1 1.969(3) . ?
Cu1 N3 2.021(3) . ?
Cu1 N4 2.024(3) . ?
Cu1 O1 2.398(2) . ?
Cu2 N2 1.922(3) . ?
Cu2 N2 1.922(3) 2_665 ?
Cu2 O3 2.044(2) . ?
Cu2 O3 2.044(2) 2_665 ?
C1 O2 1.236(4) . ?
C1 O1 1.284(4) . ?
C1 C2 1.494(4) . ?
C2 N1 1.346(4) . ?
C2 C3 1.394(4) . ?
C3 C4 1.400(4) . ?
C4 N2 1.347(4) . ?
C4 C5 1.496(4) 2_665 ?
C5 O4 1.241(4) . ?
C5 O3 1.284(4) . ?
C5 C4 1.496(4) 2_665 ?
C6 N3 1.345(5) . ?
C6 C7 1.384(5) . ?
C7 C8 1.378(6) . ?
C8 C9 1.395(5) . ?
C9 C10 1.382(5) . ?
C10 N3 1.348(5) . ?
C11 N4 1.334(4) . ?
C11 C12 1.392(5) . ?
C12 C13 1.392(5) . ?
C13 C14 1.370(6) . ?
C14 C15 1.375(5) . ?
C15 N4 1.352(4) . ?
C16 N5 1.341(4) . ?
C16 C17 1.392(5) . ?
C17 C18 1.384(5) . ?
C18 C19 1.382(5) . ?
C19 C20 1.387(5) . ?
C20 N5 1.343(4) . ?
N1 N2 1.328(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
O5 Cu1 N1 178.49(11) . . ?
O5 Cu1 N3 86.96(10) . . ?
N1 Cu1 N3 92.32(10) . . ?
O5 Cu1 N4 88.44(10) . . ?
N1 Cu1 N4 92.08(11) . . ?
N3 Cu1 N4 170.17(11) . . ?
O5 Cu1 O1 107.62(9) . . ?
N1 Cu1 O1 73.75(9) . . ?
N3 Cu1 O1 94.13(10) . . ?
N4 Cu1 O1 95.54(9) . . ?
N2 Cu2 N2 180.0 . 2_665 ?
N2 Cu2 O3 98.39(10) . . ?
N2 Cu2 O3 81.61(10) 2_665 . ?
N2 Cu2 O3 81.61(10) . 2_665 ?
N2 Cu2 O3 98.39(10) 2_665 2_665 ?
O3 Cu2 O3 180.0 . 2_665 ?
O2 C1 O1 125.9(3) . . ?
O2 C1 C2 120.1(3) . . ?
O1 C1 C2 114.0(3) . . ?
N1 C2 C3 109.2(3) . . ?
N1 C2 C1 117.7(3) . . ?
C3 C2 C1 133.1(3) . . ?
C2 C3 C4 104.2(3) . . ?
N2 C4 C3 108.6(3) . . ?
N2 C4 C5 114.8(3) . 2_665 ?
C3 C4 C5 136.6(3) . 2_665 ?
O4 C5 O3 125.5(3) . . ?
O4 C5 C4 120.0(3) . 2_665 ?
O3 C5 C4 114.5(3) . 2_665 ?
N3 C6 C7 122.1(3) . . ?
C8 C7 C6 119.3(3) . . ?
C7 C8 C9 119.0(3) . . ?
C10 C9 C8 118.5(3) . . ?
N3 C10 C9 122.6(3) . . ?
N4 C11 C12 122.7(3) . . ?
C13 C12 C11 118.4(3) . . ?
C14 C13 C12 118.8(3) . . ?
C13 C14 C15 119.8(4) . . ?
N4 C15 C14 122.1(3) . . ?
N5 C16 C17 123.4(3) . . ?
C18 C17 C16 118.9(3) . . ?
C19 C18 C17 118.3(3) . . ?
C18 C19 C20 119.3(3) . . ?
N5 C20 C19 123.2(3) . . ?
N2 N1 C2 108.7(2) . . ?
N2 N1 Cu1 128.8(2) . . ?
C2 N1 Cu1 122.5(2) . . ?
N1 N2 C4 109.3(2) . . ?
N1 N2 Cu2 135.4(2) . . ?
C4 N2 Cu2 115.2(2) . . ?
C6 N3 C10 118.4(3) . . ?
C6 N3 Cu1 120.7(2) . . ?
C10 N3 Cu1 120.7(2) . . ?
C11 N4 C15 118.2(3) . . ?
C11 N4 Cu1 119.9(2) . . ?
C15 N4 Cu1 121.9(2) . . ?
C16 N5 C20 117.0(3) . . ?
C1 O1 Cu1 112.04(18) . . ?
C5 O3 Cu2 113.89(19) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        69.99
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.498
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.118
####################################################################### 
# 
# 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_full_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1865964'
loop_
_audit_author_name
_audit_author_address

'Shiqun Xiang, Xiaofeng Zhang,Hui Chen, Yinghua Li, Weibin Fan and Deguang Huang'
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2018-09-05 deposited with the CCDC.	2019-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Cu(ligand)(Cl)2(H2O)].H2O'
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H9 Cl2 Cu N3 O3, H2 O'
_chemical_formula_sum            'C9 H11 Cl2 Cu N3 O4'
_chemical_formula_weight         359.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_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                   8.2386(3)
_cell_length_b                   11.5739(4)
_cell_length_c                   13.9034(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.524(3)
_cell_angle_gamma                90.00
_cell_volume                     1325.66(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2584
_cell_measurement_theta_min      4.9610
_cell_measurement_theta_max      71.8490

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             724
_exptl_absorpt_coefficient_mu    6.186
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4572
_exptl_absorpt_correction_T_max  0.5767
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  Mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5148
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         4.97
_diffrn_reflns_theta_max         70.99
_reflns_number_total             2520
_reflns_number_gt                2249
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0399P)²+0.8860P] 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         2520
_refine_ls_number_parameters     177
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0280
_refine_ls_wR_factor_ref         0.0745
_refine_ls_wR_factor_gt          0.0720
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.88197(4) 0.77007(3) 0.31483(2) 0.01674(11) Uani 1 1 d . . .
Cl1 Cl 0.98348(7) 0.78210(5) 0.16363(4) 0.02213(14) Uani 1 1 d . . .
Cl2 Cl 0.66475(6) 0.62380(4) 0.32792(4) 0.01777(13) Uani 1 1 d . . .
O1 O 0.6725(2) 1.00363(15) 0.44131(12) 0.0274(4) Uani 1 1 d . . .
O2 O 0.7271(2) 1.04455(15) 0.59500(12) 0.0256(4) Uani 1 1 d . . .
H2A H 0.6696 1.1028 0.5829 0.038 Uiso 1 1 calc R . .
O3 O 0.73571(19) 0.89764(13) 0.28241(11) 0.0206(3) Uani 1 1 d . . .
H3C H 0.7843 0.9493 0.2468 0.031 Uiso 1 1 d R . .
H3B H 0.7018 0.9324 0.3344 0.031 Uiso 1 1 d R . .
O4 O 0.4344(3) 0.77810(18) 0.44371(14) 0.0402(5) Uani 1 1 d G . .
H4C H 0.4609 0.7726 0.5028 0.060 Uiso 1 1 d G . .
H4B H 0.4985 0.7375 0.4101 0.060 Uiso 1 1 d G . .
N1 N 0.9062(2) 0.81453(16) 0.46132(13) 0.0170(4) Uani 1 1 d . . .
N2 N 1.0140(2) 0.74225(16) 0.50496(14) 0.0176(4) Uani 1 1 d . . .
N3 N 1.0430(2) 0.65371(17) 0.35750(13) 0.0182(4) Uani 1 1 d . . .
C1 C 0.7435(3) 0.9830(2) 0.51671(16) 0.0193(5) Uani 1 1 d . . .
C2 C 0.8605(3) 0.88676(19) 0.53209(16) 0.0183(5) Uani 1 1 d . . .
C3 C 0.9402(3) 0.8607(2) 0.61906(17) 0.0234(5) Uani 1 1 d . . .
H3A H 0.9289 0.8992 0.6790 0.028 Uiso 1 1 calc R . .
C4 C 1.0370(3) 0.7686(2) 0.59951(17) 0.0231(5) Uani 1 1 d . . .
H4A H 1.1073 0.7299 0.6435 0.028 Uiso 1 1 calc R . .
C5 C 1.0851(3) 0.65273(19) 0.45053(16) 0.0178(5) Uani 1 1 d . . .
C6 C 1.1864(3) 0.5711(2) 0.49176(17) 0.0223(5) Uani 1 1 d . . .
H6A H 1.2128 0.5731 0.5584 0.027 Uiso 1 1 calc R . .
C7 C 1.2477(3) 0.4864(2) 0.43243(17) 0.0250(5) Uani 1 1 d . . .
H7A H 1.3188 0.4291 0.4577 0.030 Uiso 1 1 calc R . .
C8 C 1.2050(3) 0.4851(2) 0.33564(17) 0.0250(5) Uani 1 1 d . . .
H8A H 1.2456 0.4269 0.2941 0.030 Uiso 1 1 calc R . .
C9 C 1.1026(3) 0.5699(2) 0.30071(17) 0.0226(5) Uani 1 1 d . . .
H9A H 1.0732 0.5691 0.2345 0.027 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 O3 1.9558(15) . ?
Cu1 N3 1.9778(19) . ?
Cu1 N1 2.1085(19) . ?
Cu1 Cl1 2.2738(6) . ?
Cu1 Cl2 2.4714(6) . ?
O1 C1 1.219(3) . ?
O2 C1 1.309(3) . ?
O2 H2A 0.8400 . ?
O3 H3C 0.8753 . ?
O3 H3B 0.8748 . ?
O4 H4C 0.8500 . ?
O4 H4B 0.8500 . ?
N1 C2 1.347(3) . ?
N1 N2 1.359(3) . ?
N2 C4 1.361(3) . ?
N2 C5 1.413(3) . ?
N3 C5 1.336(3) . ?
N3 C9 1.346(3) . ?
C1 C2 1.487(3) . ?
C2 C3 1.404(3) . ?
C3 C4 1.360(3) . ?
C3 H3A 0.9500 . ?
C4 H4A 0.9500 . ?
C5 C6 1.382(3) . ?
C6 C7 1.380(3) . ?
C6 H6A 0.9500 . ?
C7 C8 1.388(3) . ?
C7 H7A 0.9500 . ?
C8 C9 1.379(3) . ?
C8 H8A 0.9500 . ?
C9 H9A 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Cu1 N3 173.40(7) . . ?
O3 Cu1 N1 95.23(7) . . ?
N3 Cu1 N1 79.58(7) . . ?
O3 Cu1 Cl1 88.38(5) . . ?
N3 Cu1 Cl1 93.88(6) . . ?
N1 Cu1 Cl1 147.75(5) . . ?
O3 Cu1 Cl2 95.11(5) . . ?
N3 Cu1 Cl2 89.75(6) . . ?
N1 Cu1 Cl2 99.11(5) . . ?
Cl1 Cu1 Cl2 112.50(2) . . ?
C1 O2 H2A 109.5 . . ?
Cu1 O3 H3C 111.2 . . ?
Cu1 O3 H3B 110.9 . . ?
H3C O3 H3B 107.7 . . ?
H4C O4 H4B 109.5 . . ?
C2 N1 N2 103.99(17) . . ?
C2 N1 Cu1 146.32(15) . . ?
N2 N1 Cu1 109.68(14) . . ?
N1 N2 C4 112.23(19) . . ?
N1 N2 C5 118.98(18) . . ?
C4 N2 C5 128.79(19) . . ?
C5 N3 C9 117.97(19) . . ?
C5 N3 Cu1 117.61(15) . . ?
C9 N3 Cu1 124.18(15) . . ?
O1 C1 O2 123.8(2) . . ?
O1 C1 C2 125.1(2) . . ?
O2 C1 C2 111.09(19) . . ?
N1 C2 C3 111.4(2) . . ?
N1 C2 C1 123.01(19) . . ?
C3 C2 C1 125.6(2) . . ?
C4 C3 C2 105.5(2) . . ?
C4 C3 H3A 127.3 . . ?
C2 C3 H3A 127.3 . . ?
C3 C4 N2 107.0(2) . . ?
C3 C4 H4A 126.5 . . ?
N2 C4 H4A 126.5 . . ?
N3 C5 C6 123.9(2) . . ?
N3 C5 N2 114.02(19) . . ?
C6 C5 N2 122.1(2) . . ?
C7 C6 C5 117.4(2) . . ?
C7 C6 H6A 121.3 . . ?
C5 C6 H6A 121.3 . . ?
C6 C7 C8 119.7(2) . . ?
C6 C7 H7A 120.1 . . ?
C8 C7 H7A 120.1 . . ?
C9 C8 C7 118.9(2) . . ?
C9 C8 H8A 120.6 . . ?
C7 C8 H8A 120.6 . . ?
N3 C9 C8 122.1(2) . . ?
N3 C9 H9A 119.0 . . ?
C8 C9 H9A 119.0 . . ?

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
O3 Cu1 N1 C2 2.7(3) . . . . ?
N3 Cu1 N1 C2 178.6(3) . . . . ?
Cl1 Cu1 N1 C2 97.9(3) . . . . ?
Cl2 Cu1 N1 C2 -93.4(3) . . . . ?
O3 Cu1 N1 N2 -176.25(14) . . . . ?
N3 Cu1 N1 N2 -0.35(14) . . . . ?
Cl1 Cu1 N1 N2 -80.98(17) . . . . ?
Cl2 Cu1 N1 N2 87.71(14) . . . . ?
C2 N1 N2 C4 -0.7(2) . . . . ?
Cu1 N1 N2 C4 178.72(16) . . . . ?
C2 N1 N2 C5 178.97(19) . . . . ?
Cu1 N1 N2 C5 -1.6(2) . . . . ?
O3 Cu1 N3 C5 40.7(7) . . . . ?
N1 Cu1 N3 C5 2.41(16) . . . . ?
Cl1 Cu1 N3 C5 150.56(16) . . . . ?
Cl2 Cu1 N3 C5 -96.90(16) . . . . ?
O3 Cu1 N3 C9 -145.0(6) . . . . ?
N1 Cu1 N3 C9 176.8(2) . . . . ?
Cl1 Cu1 N3 C9 -35.09(19) . . . . ?
Cl2 Cu1 N3 C9 77.45(18) . . . . ?
N2 N1 C2 C3 0.6(2) . . . . ?
Cu1 N1 C2 C3 -178.4(2) . . . . ?
N2 N1 C2 C1 179.1(2) . . . . ?
Cu1 N1 C2 C1 0.1(4) . . . . ?
O1 C1 C2 N1 3.2(4) . . . . ?
O2 C1 C2 N1 -176.1(2) . . . . ?
O1 C1 C2 C3 -178.6(2) . . . . ?
O2 C1 C2 C3 2.2(3) . . . . ?
N1 C2 C3 C4 -0.3(3) . . . . ?
C1 C2 C3 C4 -178.7(2) . . . . ?
C2 C3 C4 N2 -0.1(3) . . . . ?
N1 N2 C4 C3 0.5(3) . . . . ?
C5 N2 C4 C3 -179.1(2) . . . . ?
C9 N3 C5 C6 0.2(3) . . . . ?
Cu1 N3 C5 C6 174.91(18) . . . . ?
C9 N3 C5 N2 -178.6(2) . . . . ?
Cu1 N3 C5 N2 -3.9(3) . . . . ?
N1 N2 C5 N3 3.7(3) . . . . ?
C4 N2 C5 N3 -176.8(2) . . . . ?
N1 N2 C5 C6 -175.2(2) . . . . ?
C4 N2 C5 C6 4.4(4) . . . . ?
N3 C5 C6 C7 0.4(4) . . . . ?
N2 C5 C6 C7 179.1(2) . . . . ?
C5 C6 C7 C8 -0.8(4) . . . . ?
C6 C7 C8 C9 0.6(4) . . . . ?
C5 N3 C9 C8 -0.4(3) . . . . ?
Cu1 N3 C9 C8 -174.76(18) . . . . ?
C7 C8 C9 N3 0.1(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        70.99
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.068
####################################################################### 
# 
# 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_Ligand1-Hppca
_database_code_depnum_ccdc_archive 'CCDC 1865965'
_audit_update_record             
;
2019-02-15 deposited with the CCDC.	2019-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            Ligand1-Hppca
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H7 N3 O2'
_chemical_formula_sum            'C9 H7 N3 O2'
_chemical_formula_weight         189.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   8.8416(2)
_cell_length_b                   12.3762(3)
_cell_length_c                   15.4438(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.371(2)
_cell_angle_gamma                90.00
_cell_volume                     1688.50(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3061
_cell_measurement_theta_min      4.9980
_cell_measurement_theta_max      71.9830

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             784
_exptl_absorpt_coefficient_mu    0.919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8744
_exptl_absorpt_correction_T_max  0.9641
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  Mirror
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6208
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         4.58
_diffrn_reflns_theta_max         71.00
_reflns_number_total             3203
_reflns_number_gt                2674
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
;

# start Validation Reply Form
_vrf_PLAT906_Ligand1-Hppca       
;
PROBLEM:  Large K Value in the Analysis of Variance ......      3.348 Check 
RESPONSE: The data was collected from a poorly diffracting crystal and 23 
          reflections of "the most disagreeable reflections" were omitted 
          in the refinement of structure, in order to solve the problem of 
          "Number of (Iobs-Icalc)/SigmaW > 10 Outliers". Thus,this problem 
          could be derived from the poor dirraction data of this sample.
;

# end Validation Reply Form

_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)+(0.0530P)²+0.1593P] 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         3203
_refine_ls_number_parameters     261
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0918
_refine_ls_wR_factor_gt          0.0868
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O -0.09355(11) 1.26542(8) -0.04673(6) 0.0212(2) Uani 1 1 d . . .
O2 O 0.04884(10) 1.30981(7) 0.07130(6) 0.0209(2) Uani 1 1 d . . .
O3 O 0.89712(11) 0.48472(8) 0.11450(6) 0.0245(2) Uani 1 1 d . . .
O4 O 0.76971(10) 0.44791(7) -0.01043(6) 0.0214(2) Uani 1 1 d . . .
N1 N 0.07670(12) 1.08596(9) -0.07128(6) 0.0174(2) Uani 1 1 d . . .
N2 N 0.18132(12) 1.00686(9) -0.06225(7) 0.0168(2) Uani 1 1 d . . .
N3 N 0.29402(12) 0.85002(9) -0.11084(7) 0.0203(2) Uani 1 1 d . . .
N4 N 0.72145(11) 0.66622(8) 0.13529(6) 0.0166(2) Uani 1 1 d . . .
N5 N 0.61227(12) 0.74195(8) 0.12441(6) 0.0161(2) Uani 1 1 d . . .
N6 N 0.48606(12) 0.89454(9) 0.16856(7) 0.0198(2) Uani 1 1 d . . .
C1 C 0.01839(14) 1.24912(10) 0.01017(8) 0.0166(3) Uani 1 1 d . . .
C2 C 0.10828(14) 1.15160(10) -0.00414(8) 0.0171(3) Uani 1 1 d . . .
C3 C 0.23251(15) 1.11452(11) 0.04759(8) 0.0204(3) Uani 1 1 d . . .
H3A H 0.2763 1.1473 0.0983 0.024 Uiso 1 1 calc R . .
C4 C 0.27621(14) 1.02109(11) 0.00881(8) 0.0195(3) Uani 1 1 d . . .
H4A H 0.3569 0.9750 0.0276 0.023 Uiso 1 1 calc R . .
C5 C 0.18279(14) 0.92109(10) -0.12368(8) 0.0174(3) Uani 1 1 d . . .
C6 C 0.07394(14) 0.91733(11) -0.19129(8) 0.0193(3) Uani 1 1 d . . .
H6A H -0.0036 0.9703 -0.1971 0.023 Uiso 1 1 calc R . .
C7 C 0.08338(15) 0.83309(11) -0.24978(8) 0.0212(3) Uani 1 1 d . . .
H7A H 0.0115 0.8269 -0.2970 0.025 Uiso 1 1 calc R . .
C8 C 0.19891(16) 0.75777(11) -0.23885(8) 0.0235(3) Uani 1 1 d . . .
H8A H 0.2082 0.6996 -0.2784 0.028 Uiso 1 1 calc R . .
C9 C 0.29992(16) 0.76970(11) -0.16903(9) 0.0233(3) Uani 1 1 d . . .
H9A H 0.3786 0.7178 -0.1617 0.028 Uiso 1 1 calc R . .
C10 C 0.79237(14) 0.50425(10) 0.05415(8) 0.0170(3) Uani 1 1 d . . .
C11 C 0.69829(14) 0.60060(10) 0.06730(8) 0.0165(3) Uani 1 1 d . . .
C12 C 0.57507(14) 0.63389(10) 0.01350(8) 0.0188(3) Uani 1 1 d . . .
H12A H 0.5370 0.6003 -0.0383 0.023 Uiso 1 1 calc R . .
C13 C 0.52193(14) 0.72482(10) 0.05166(8) 0.0182(3) Uani 1 1 d . . .
H13A H 0.4386 0.7678 0.0317 0.022 Uiso 1 1 calc R . .
C14 C 0.60274(14) 0.82887(10) 0.18391(8) 0.0161(3) Uani 1 1 d . . .
C15 C 0.71040(14) 0.84034(11) 0.25144(8) 0.0191(3) Uani 1 1 d . . .
H15A H 0.7913 0.7904 0.2598 0.023 Uiso 1 1 calc R . .
C16 C 0.69416(15) 0.92800(11) 0.30596(8) 0.0211(3) Uani 1 1 d . . .
H16A H 0.7655 0.9400 0.3526 0.025 Uiso 1 1 calc R . .
C17 C 0.57324(15) 0.99822(11) 0.29215(8) 0.0205(3) Uani 1 1 d . . .
H17A H 0.5601 1.0586 0.3291 0.025 Uiso 1 1 calc R . .
C18 C 0.47260(15) 0.97801(11) 0.22340(8) 0.0210(3) Uani 1 1 d . . .
H18A H 0.3892 1.0257 0.2143 0.025 Uiso 1 1 calc R . .
H3B H 0.949(2) 0.4239(19) 0.1002(13) 0.052(6) Uiso 1 1 d . . .
H1A H -0.139(2) 1.3267(19) -0.0310(14) 0.051(6) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.3117(16) . ?
O1 H1A 0.90(2) . ?
O2 C1 1.2276(15) . ?
O3 C10 1.3090(16) . ?
O3 H3B 0.91(2) . ?
O4 C10 1.2266(15) . ?
N1 C2 1.3375(16) . ?
N1 N2 1.3501(15) . ?
N2 C4 1.3649(17) . ?
N2 C5 1.4241(16) . ?
N3 C5 1.3282(17) . ?
N3 C9 1.3425(17) . ?
N4 C11 1.3365(16) . ?
N4 N5 1.3510(15) . ?
N5 C13 1.3678(16) . ?
N5 C14 1.4196(16) . ?
N6 C14 1.3270(17) . ?
N6 C18 1.3442(17) . ?
C1 C2 1.4669(18) . ?
C2 C3 1.4081(18) . ?
C3 C4 1.3653(19) . ?
C3 H3A 0.9500 . ?
C4 H4A 0.9500 . ?
C5 C6 1.3913(18) . ?
C6 C7 1.3842(18) . ?
C6 H6A 0.9500 . ?
C7 C8 1.388(2) . ?
C7 H7A 0.9500 . ?
C8 C9 1.379(2) . ?
C8 H8A 0.9500 . ?
C9 H9A 0.9500 . ?
C10 C11 1.4728(17) . ?
C11 C12 1.4043(18) . ?
C12 C13 1.3630(18) . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9500 . ?
C14 C15 1.3900(18) . ?
C15 C16 1.3845(18) . ?
C15 H15A 0.9500 . ?
C16 C17 1.3874(19) . ?
C16 H16A 0.9500 . ?
C17 C18 1.3797(19) . ?
C17 H17A 0.9500 . ?
C18 H18A 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 H1A 106.4(14) . . ?
C10 O3 H3B 109.2(13) . . ?
C2 N1 N2 103.89(10) . . ?
N1 N2 C4 112.66(10) . . ?
N1 N2 C5 119.78(10) . . ?
C4 N2 C5 127.56(11) . . ?
C5 N3 C9 116.07(11) . . ?
C11 N4 N5 103.79(9) . . ?
N4 N5 C13 112.62(10) . . ?
N4 N5 C14 120.43(10) . . ?
C13 N5 C14 126.93(11) . . ?
C14 N6 C18 116.52(11) . . ?
O2 C1 O1 123.82(12) . . ?
O2 C1 C2 121.09(11) . . ?
O1 C1 C2 115.09(11) . . ?
N1 C2 C3 112.02(11) . . ?
N1 C2 C1 121.30(11) . . ?
C3 C2 C1 126.68(11) . . ?
C4 C3 C2 104.80(11) . . ?
C4 C3 H3A 127.6 . . ?
C2 C3 H3A 127.6 . . ?
N2 C4 C3 106.63(11) . . ?
N2 C4 H4A 126.7 . . ?
C3 C4 H4A 126.7 . . ?
N3 C5 C6 125.09(12) . . ?
N3 C5 N2 114.92(11) . . ?
C6 C5 N2 119.99(11) . . ?
C7 C6 C5 117.16(12) . . ?
C7 C6 H6A 121.4 . . ?
C5 C6 H6A 121.4 . . ?
C6 C7 C8 119.37(12) . . ?
C6 C7 H7A 120.3 . . ?
C8 C7 H7A 120.3 . . ?
C9 C8 C7 118.20(12) . . ?
C9 C8 H8A 120.9 . . ?
C7 C8 H8A 120.9 . . ?
N3 C9 C8 124.11(12) . . ?
N3 C9 H9A 117.9 . . ?
C8 C9 H9A 117.9 . . ?
O4 C10 O3 124.12(12) . . ?
O4 C10 C11 119.88(11) . . ?
O3 C10 C11 116.00(11) . . ?
N4 C11 C12 112.12(11) . . ?
N4 C11 C10 122.09(11) . . ?
C12 C11 C10 125.78(11) . . ?
C13 C12 C11 105.03(11) . . ?
C13 C12 H12A 127.5 . . ?
C11 C12 H12A 127.5 . . ?
C12 C13 N5 106.44(11) . . ?
C12 C13 H13A 126.8 . . ?
N5 C13 H13A 126.8 . . ?
N6 C14 C15 125.08(12) . . ?
N6 C14 N5 114.52(10) . . ?
C15 C14 N5 120.39(11) . . ?
C16 C15 C14 116.83(12) . . ?
C16 C15 H15A 121.6 . . ?
C14 C15 H15A 121.6 . . ?
C15 C16 C17 119.74(12) . . ?
C15 C16 H16A 120.1 . . ?
C17 C16 H16A 120.1 . . ?
C18 C17 C16 118.24(12) . . ?
C18 C17 H17A 120.9 . . ?
C16 C17 H17A 120.9 . . ?
N6 C18 C17 123.58(12) . . ?
N6 C18 H18A 118.2 . . ?
C17 C18 H18A 118.2 . . ?

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
C2 N1 N2 C4 0.42(13) . . . . ?
C2 N1 N2 C5 -179.73(10) . . . . ?
C11 N4 N5 C13 0.16(13) . . . . ?
C11 N4 N5 C14 -178.34(10) . . . . ?
N2 N1 C2 C3 -0.04(14) . . . . ?
N2 N1 C2 C1 -179.66(10) . . . . ?
O2 C1 C2 N1 -179.15(11) . . . . ?
O1 C1 C2 N1 0.53(17) . . . . ?
O2 C1 C2 C3 1.3(2) . . . . ?
O1 C1 C2 C3 -179.03(12) . . . . ?
N1 C2 C3 C4 -0.32(15) . . . . ?
C1 C2 C3 C4 179.27(12) . . . . ?
N1 N2 C4 C3 -0.63(15) . . . . ?
C5 N2 C4 C3 179.53(11) . . . . ?
C2 C3 C4 N2 0.55(14) . . . . ?
C9 N3 C5 C6 0.60(19) . . . . ?
C9 N3 C5 N2 -178.55(11) . . . . ?
N1 N2 C5 N3 177.34(10) . . . . ?
C4 N2 C5 N3 -2.83(18) . . . . ?
N1 N2 C5 C6 -1.86(17) . . . . ?
C4 N2 C5 C6 177.98(12) . . . . ?
N3 C5 C6 C7 -0.36(19) . . . . ?
N2 C5 C6 C7 178.75(11) . . . . ?
C5 C6 C7 C8 -0.20(19) . . . . ?
C6 C7 C8 C9 0.47(19) . . . . ?
C5 N3 C9 C8 -0.3(2) . . . . ?
C7 C8 C9 N3 -0.2(2) . . . . ?
N5 N4 C11 C12 -0.16(13) . . . . ?
N5 N4 C11 C10 -179.02(11) . . . . ?
O4 C10 C11 N4 -178.01(11) . . . . ?
O3 C10 C11 N4 2.09(17) . . . . ?
O4 C10 C11 C12 3.29(19) . . . . ?
O3 C10 C11 C12 -176.61(12) . . . . ?
N4 C11 C12 C13 0.11(15) . . . . ?
C10 C11 C12 C13 178.91(11) . . . . ?
C11 C12 C13 N5 -0.01(14) . . . . ?
N4 N5 C13 C12 -0.10(14) . . . . ?
C14 N5 C13 C12 178.29(11) . . . . ?
C18 N6 C14 C15 -0.19(19) . . . . ?
C18 N6 C14 N5 179.97(11) . . . . ?
N4 N5 C14 N6 -176.70(10) . . . . ?
C13 N5 C14 N6 5.03(18) . . . . ?
N4 N5 C14 C15 3.44(17) . . . . ?
C13 N5 C14 C15 -174.83(12) . . . . ?
N6 C14 C15 C16 -0.65(19) . . . . ?
N5 C14 C15 C16 179.19(11) . . . . ?
C14 C15 C16 C17 0.85(19) . . . . ?
C15 C16 C17 C18 -0.26(19) . . . . ?
C14 N6 C18 C17 0.85(19) . . . . ?
C16 C17 C18 N6 -0.6(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        71.00
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.046
####################################################################### 
# 
# 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_Complex5
_database_code_depnum_ccdc_archive 'CCDC 1876648'
_audit_update_record             
;
2019-02-15 deposited with the CCDC.	2019-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Cu(L)2(Py)2](Et4N)2 3H2O'
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H12 Cu2 N6 O8, C16 H40 N2, H6 O3'
_chemical_formula_sum            'C36 H58 Cu2 N8 O11'
_chemical_formula_weight         905.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P21212
_symmetry_space_group_name_Hall  'P 2 2ab'

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

_cell_length_a                   22.8690(4)
_cell_length_b                   10.96066(16)
_cell_length_c                   8.34393(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2091.48(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5814
_cell_measurement_theta_min      3.8390
_cell_measurement_theta_max      72.9060

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             952
_exptl_absorpt_coefficient_mu    1.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7728
_exptl_absorpt_correction_T_max  0.8396
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  Mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11330
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.87
_diffrn_reflns_theta_max         70.97
_reflns_number_total             3927
_reflns_number_gt                3698
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
;

# start Validation Reply Form
_vrf_PLAT090_Complex5            
;
PROBLEM:  Poor Data / Parameter Ratio (Zmax > 18) ........       5.95 Note   
RESPONSE: The data was collected from a poorly diffracting crystal and the
          crystal structure of pyridine ring, Et4N cation and one water 
          molecule were treated as two-component disordered models with 
         occupancies of 60% and 40%,0.55% and 0.45%, 70% and 30% respectively.
         All the bond lengths and bond angles of disordered models were 
         constrained by using command of DFIX, followed by the average of 
         temperature factors by using commands of DELU/SIMU. The hydrogen 
         atoms were added geometrically except for the hydrogens on water 
        molecules, which was added from the given Fourier maps and their 
        bond lengths, bond angles and thereby temperature factors were 
        constrained by DFIX, DELU/SIMU. Therefore, the parameters increases 
        a lot due to the above operations, which leads to the low 
         Data/Parameter Ratio as shown.
;

# end Validation Reply Form


_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)+(0.1285P)²+2.5528P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.23(7)
_refine_ls_number_reflns         3927
_refine_ls_number_parameters     391
_refine_ls_number_restraints     487
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0635
_refine_ls_wR_factor_ref         0.1806
_refine_ls_wR_factor_gt          0.1764
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.162
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.91700(3) -0.05724(7) 0.63913(9) 0.0322(2) Uani 1 1 d . . .
O1 O 0.84616(17) 0.0409(4) 0.6969(5) 0.0400(9) Uani 1 1 d . A .
O2 O 0.8188(2) 0.2283(4) 0.7739(9) 0.0665(16) Uani 1 1 d . A .
O3 O 1.11105(17) 0.2246(4) 0.7071(5) 0.0381(9) Uani 1 1 d . . .
O4 O 1.0791(2) 0.4045(4) 0.7974(6) 0.0479(10) Uani 1 1 d . A .
N1 N 0.95304(19) 0.1022(4) 0.6560(6) 0.0343(9) Uani 1 1 d . A .
N2 N 1.00835(19) 0.1405(4) 0.6595(5) 0.0328(9) Uani 1 1 d . . .
C1 C 0.8563(3) 0.1547(6) 0.7306(9) 0.0451(14) Uani 1 1 d . . .
C2 C 0.9187(3) 0.1915(5) 0.7132(7) 0.0372(11) Uani 1 1 d . A .
C3 C 0.9536(2) 0.2918(5) 0.7547(8) 0.0402(13) Uani 1 1 d . . .
H3A H 0.9413 0.3680 0.7974 0.048 Uiso 1 1 calc R A .
C4 C 1.0106(3) 0.2537(5) 0.7188(7) 0.0360(11) Uani 1 1 d . A .
C5 C 1.0712(2) 0.3009(5) 0.7433(7) 0.0373(12) Uani 1 1 d . . .
N3 N 0.8967(6) -0.0682(13) 0.3791(11) 0.0345(19) Uani 0.612(19) 1 d PGU A 1
C6 C 0.9397(5) -0.0981(13) 0.2680(14) 0.045(2) Uani 0.612(19) 1 d PGU A 1
H6A H 0.9786 -0.1129 0.3026 0.053 Uiso 0.612(19) 1 calc PR A 1
C7 C 0.9257(4) -0.1065(13) 0.1062(13) 0.045(2) Uani 0.612(19) 1 d PGU A 1
H7A H 0.9551 -0.1269 0.0303 0.054 Uiso 0.612(19) 1 calc PR A 1
C8 C 0.8687(4) -0.0849(12) 0.0556(11) 0.045(2) Uani 0.612(19) 1 d PGU A 1
H8A H 0.8591 -0.0906 -0.0549 0.055 Uiso 0.612(19) 1 calc PR A 1
C9 C 0.8258(4) -0.0550(12) 0.1667(11) 0.0441(19) Uani 0.612(19) 1 d PGU A 1
H9A H 0.7868 -0.0402 0.1321 0.053 Uiso 0.612(19) 1 calc PR A 1
C10 C 0.8398(5) -0.0466(12) 0.3284(11) 0.041(2) Uani 0.612(19) 1 d PGU A 1
H10A H 0.8104 -0.0262 0.4043 0.049 Uiso 0.612(19) 1 calc PR A 1
N3' N 0.8942(10) -0.091(2) 0.3926(19) 0.037(2) Uani 0.388(19) 1 d PGU A 2
C6' C 0.9375(8) -0.124(2) 0.284(2) 0.043(2) Uani 0.388(19) 1 d PGU A 2
H6'A H 0.9769 -0.1311 0.3190 0.052 Uiso 0.388(19) 1 calc PR A 2
C7' C 0.9230(7) -0.1487(17) 0.126(2) 0.044(2) Uani 0.388(19) 1 d PGU A 2
H7'A H 0.9526 -0.1718 0.0519 0.053 Uiso 0.388(19) 1 calc PR A 2
C8' C 0.8653(7) -0.1390(19) 0.0753(18) 0.044(2) Uani 0.388(19) 1 d PGU A 2
H8'A H 0.8554 -0.1555 -0.0332 0.052 Uiso 0.388(19) 1 calc PR A 2
C9' C 0.8220(7) -0.1051(18) 0.1834(19) 0.044(2) Uani 0.388(19) 1 d PGU A 2
H9'A H 0.7826 -0.0984 0.1489 0.053 Uiso 0.388(19) 1 calc PR A 2
C10' C 0.8365(9) -0.0809(16) 0.3421(18) 0.042(2) Uani 0.388(19) 1 d PGU A 2
H10B H 0.8069 -0.0577 0.4160 0.050 Uiso 0.388(19) 1 calc PR A 2
O5 O 0.8117(4) 0.4817(9) 0.796(2) 0.083(4) Uani 0.72(2) 1 d PDU B 1
H5A H 0.8137 0.4054 0.7889 0.099 Uiso 0.72(2) 1 d PRD B 1
H5B H 0.8466(12) 0.505(4) 0.81(2) 0.099 Uiso 0.72(2) 1 d PD B 1
O5' O 0.8095(12) 0.464(3) 0.693(6) 0.087(5) Uani 0.28(2) 1 d PDU B 2
H5C H 0.8122 0.3932 0.7155 0.104 Uiso 0.28(2) 1 d PRD B 2
H5D H 0.776(7) 0.477(9) 0.66(5) 0.104 Uiso 0.28(2) 1 d PD B 2
O6 O 1.0000 0.5000 0.0274(9) 0.072(2) Uani 1 2 d SD . .
H6B H 0.9765 0.5284 -0.0403 0.086 Uiso 0.50 1 d PRD . .
H6C H 1.022(6) 0.462(17) -0.023(5) 0.086 Uiso 0.50 1 d PD . .
N4 N 0.8537(5) 0.4237(11) 0.3024(17) 0.082(2) Uani 0.565(7) 1 d PDU C 1
C11 C 0.8309(8) 0.5438(15) 0.241(3) 0.097(3) Uani 0.565(7) 1 d PDU C 1
H11A H 0.8042 0.5274 0.1499 0.116 Uiso 0.565(7) 1 calc PR C 1
H11B H 0.8643 0.5917 0.1989 0.116 Uiso 0.565(7) 1 calc PR C 1
C12 C 0.7987(9) 0.6211(19) 0.362(3) 0.109(3) Uani 0.565(7) 1 d PDU C 1
H12A H 0.7853 0.6967 0.3114 0.163 Uiso 0.565(7) 1 calc PR C 1
H12B H 0.8249 0.6409 0.4515 0.163 Uiso 0.565(7) 1 calc PR C 1
H12C H 0.7648 0.5758 0.4032 0.163 Uiso 0.565(7) 1 calc PR C 1
C13 C 0.8815(7) 0.3582(13) 0.158(2) 0.078(2) Uani 0.565(7) 1 d PDU C 1
H13A H 0.8547 0.3657 0.0649 0.093 Uiso 0.565(7) 1 calc PR C 1
H13B H 0.9184 0.4002 0.1295 0.093 Uiso 0.565(7) 1 calc PR C 1
C14 C 0.8942(8) 0.2265(14) 0.185(3) 0.085(3) Uani 0.565(7) 1 d PDU C 1
H14A H 0.9120 0.1916 0.0886 0.127 Uiso 0.565(7) 1 calc PR C 1
H14B H 0.8577 0.1833 0.2091 0.127 Uiso 0.565(7) 1 calc PR C 1
H14C H 0.9212 0.2180 0.2755 0.127 Uiso 0.565(7) 1 calc PR C 1
C15 C 0.8102(7) 0.3395(17) 0.378(2) 0.089(3) Uani 0.565(7) 1 d PDU C 1
H15A H 0.7904 0.3790 0.4701 0.107 Uiso 0.565(7) 1 calc PR C 1
H15B H 0.8291 0.2633 0.4150 0.107 Uiso 0.565(7) 1 calc PR C 1
C16 C 0.7620(8) 0.311(2) 0.226(3) 0.099(4) Uani 0.565(7) 1 d PDU C 1
H16A H 0.7309 0.2573 0.2645 0.148 Uiso 0.565(7) 1 calc PR C 1
H16B H 0.7826 0.2722 0.1367 0.148 Uiso 0.565(7) 1 calc PR C 1
H16C H 0.7448 0.3885 0.1894 0.148 Uiso 0.565(7) 1 calc PR C 1
C17 C 0.8979(6) 0.4422(17) 0.4346(19) 0.076(3) Uani 0.565(7) 1 d PDU C 1
H17A H 0.9119 0.3611 0.4700 0.092 Uiso 0.565(7) 1 calc PR C 1
H17B H 0.8777 0.4805 0.5268 0.092 Uiso 0.565(7) 1 calc PR C 1
C18 C 0.9517(7) 0.5208(17) 0.392(2) 0.083(4) Uani 0.565(7) 1 d PDU C 1
H18A H 0.9775 0.5263 0.4858 0.125 Uiso 0.565(7) 1 calc PR C 1
H18B H 0.9388 0.6028 0.3615 0.125 Uiso 0.565(7) 1 calc PR C 1
H18C H 0.9728 0.4832 0.3029 0.125 Uiso 0.565(7) 1 calc PR C 1
N4' N 0.8223(7) 0.4122(14) 0.242(2) 0.085(2) Uani 0.435(7) 1 d PDU C 2
C11' C 0.8345(10) 0.473(2) 0.079(3) 0.096(3) Uani 0.435(7) 1 d PDU C 2
H11C H 0.8743 0.5086 0.0812 0.115 Uiso 0.435(7) 1 calc PR C 2
H11D H 0.8337 0.4100 -0.0057 0.115 Uiso 0.435(7) 1 calc PR C 2
C12' C 0.7913(10) 0.573(2) 0.036(4) 0.099(5) Uani 0.435(7) 1 d PDU C 2
H12D H 0.8013 0.6062 -0.0699 0.149 Uiso 0.435(7) 1 calc PR C 2
H12E H 0.7930 0.6377 0.1161 0.149 Uiso 0.435(7) 1 calc PR C 2
H12F H 0.7517 0.5385 0.0324 0.149 Uiso 0.435(7) 1 calc PR C 2
C13' C 0.8754(8) 0.3398(19) 0.297(3) 0.082(2) Uani 0.435(7) 1 d PDU C 2
H13C H 0.9010 0.3991 0.3525 0.099 Uiso 0.435(7) 1 calc PR C 2
H13D H 0.8609 0.2831 0.3799 0.099 Uiso 0.435(7) 1 calc PR C 2
C14' C 0.9150(10) 0.266(2) 0.193(3) 0.083(3) Uani 0.435(7) 1 d PDU C 2
H14D H 0.9462 0.2309 0.2584 0.124 Uiso 0.435(7) 1 calc PR C 2
H14E H 0.9321 0.3187 0.1103 0.124 Uiso 0.435(7) 1 calc PR C 2
H14F H 0.8926 0.2006 0.1418 0.124 Uiso 0.435(7) 1 calc PR C 2
C15' C 0.7677(11) 0.337(3) 0.273(4) 0.091(3) Uani 0.435(7) 1 d PDU C 2
H15C H 0.7334 0.3914 0.2865 0.109 Uiso 0.435(7) 1 calc PR C 2
H15D H 0.7725 0.2879 0.3711 0.109 Uiso 0.435(7) 1 calc PR C 2
C16' C 0.7577(11) 0.243(3) 0.109(4) 0.110(5) Uani 0.435(7) 1 d PDU C 2
H16D H 0.7222 0.1945 0.1235 0.165 Uiso 0.435(7) 1 calc PR C 2
H16E H 0.7915 0.1887 0.0975 0.165 Uiso 0.435(7) 1 calc PR C 2
H16F H 0.7538 0.2930 0.0116 0.165 Uiso 0.435(7) 1 calc PR C 2
C17' C 0.8174(11) 0.502(2) 0.384(3) 0.099(3) Uani 0.435(7) 1 d PDU C 2
H17C H 0.7804 0.5480 0.3748 0.118 Uiso 0.435(7) 1 calc PR C 2
H17D H 0.8158 0.4544 0.4852 0.118 Uiso 0.435(7) 1 calc PR C 2
C18' C 0.8688(11) 0.592(2) 0.392(4) 0.107(3) Uani 0.435(7) 1 d PDU C 2
H18D H 0.8643 0.6445 0.4867 0.160 Uiso 0.435(7) 1 calc PR C 2
H18E H 0.8692 0.6425 0.2954 0.160 Uiso 0.435(7) 1 calc PR C 2
H18F H 0.9056 0.5467 0.4003 0.160 Uiso 0.435(7) 1 calc PR 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
Cu1 N1 1.937(4) . ?
Cu1 N2 1.943(5) 2_755 ?
Cu1 O1 2.004(4) . ?
Cu1 O3 2.024(4) 2_755 ?
Cu1 N3' 2.154(15) . ?
Cu1 N3 2.222(9) . ?
O1 C1 1.299(7) . ?
O2 C1 1.231(8) . ?
O3 C5 1.273(7) . ?
O3 Cu1 2.024(4) 2_755 ?
O4 C5 1.235(7) . ?
N1 N2 1.333(6) . ?
N1 C2 1.342(7) . ?
N2 C4 1.337(7) . ?
N2 Cu1 1.943(5) 2_755 ?
C1 C2 1.492(8) . ?
C2 C3 1.401(8) . ?
C3 C4 1.402(8) . ?
C3 H3A 0.9500 . ?
C4 C5 1.494(7) . ?
N3 C6 1.3900 . ?
N3 C10 1.3900 . ?
C6 C7 1.3900 . ?
C6 H6A 0.9500 . ?
C7 C8 1.3900 . ?
C7 H7A 0.9500 . ?
C8 C9 1.3900 . ?
C8 H8A 0.9500 . ?
C9 C10 1.3900 . ?
C9 H9A 0.9500 . ?
C10 H10A 0.9500 . ?
N3' C6' 1.3900 . ?
N3' C10' 1.3900 . ?
C6' C7' 1.3900 . ?
C6' H6'A 0.9500 . ?
C7' C8' 1.3900 . ?
C7' H7'A 0.9500 . ?
C8' C9' 1.3900 . ?
C8' H8'A 0.9500 . ?
C9' C10' 1.3900 . ?
C9' H9'A 0.9500 . ?
C10' H10B 0.9500 . ?
O5 H5A 0.8400 . ?
O5 H5B 0.843(12) . ?
O5 H5C 1.1789 . ?
O5 H5D 1.4(2) . ?
O5' H5A 1.0283 . ?
O5' H5B 1.35(11) . ?
O5' H5C 0.7986 . ?
O5' H5D 0.841(12) . ?
O6 H6B 0.8401 . ?
O6 H6C 0.781(12) . ?
N4 C15 1.498(16) . ?
N4 C11 1.507(17) . ?
N4 C17 1.509(16) . ?
N4 C13 1.541(16) . ?
C11 C12 1.513(19) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.490(17) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.709(16) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.542(15) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
N4' C15' 1.52(2) . ?
N4' C13' 1.523(17) . ?
N4' C11' 1.538(19) . ?
N4' C17' 1.546(19) . ?
C11' C12' 1.515(19) . ?
C11' H11C 0.9900 . ?
C11' H11D 0.9900 . ?
C12' H12D 0.9800 . ?
C12' H12E 0.9800 . ?
C12' H12F 0.9800 . ?
C13' C14' 1.488(19) . ?
C13' H13C 0.9900 . ?
C13' H13D 0.9900 . ?
C14' H14D 0.9800 . ?
C14' H14E 0.9800 . ?
C14' H14F 0.9800 . ?
C15' C16' 1.728(18) . ?
C15' H15C 0.9900 . ?
C15' H15D 0.9900 . ?
C16' H16D 0.9800 . ?
C16' H16E 0.9800 . ?
C16' H16F 0.9800 . ?
C17' C18' 1.539(19) . ?
C17' H17C 0.9900 . ?
C17' H17D 0.9900 . ?
C18' H18D 0.9800 . ?
C18' H18E 0.9800 . ?
C18' H18F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N2 92.49(18) . 2_755 ?
N1 Cu1 O1 80.92(17) . . ?
N2 Cu1 O1 160.29(18) 2_755 . ?
N1 Cu1 O3 158.73(19) . 2_755 ?
N2 Cu1 O3 80.12(17) 2_755 2_755 ?
O1 Cu1 O3 99.37(16) . 2_755 ?
N1 Cu1 N3' 109.0(6) . . ?
N2 Cu1 N3' 102.5(7) 2_755 . ?
O1 Cu1 N3' 97.2(7) . . ?
O3 Cu1 N3' 92.1(6) 2_755 . ?
N1 Cu1 N3 102.0(4) . . ?
N2 Cu1 N3 104.1(4) 2_755 . ?
O1 Cu1 N3 95.5(4) . . ?
O3 Cu1 N3 99.1(4) 2_755 . ?
N3' Cu1 N3 7.0(9) . . ?
C1 O1 Cu1 115.1(4) . . ?
C5 O3 Cu1 115.8(3) . 2_755 ?
N2 N1 C2 108.5(4) . . ?
N2 N1 Cu1 133.6(4) . . ?
C2 N1 Cu1 115.8(4) . . ?
N1 N2 C4 109.7(5) . . ?
N1 N2 Cu1 133.1(3) . 2_755 ?
C4 N2 Cu1 115.8(4) . 2_755 ?
O2 C1 O1 124.7(6) . . ?
O2 C1 C2 121.2(5) . . ?
O1 C1 C2 114.1(5) . . ?
N1 C2 C3 109.1(5) . . ?
N1 C2 C1 113.4(5) . . ?
C3 C2 C1 137.1(5) . . ?
C2 C3 C4 104.0(5) . . ?
C2 C3 H3A 128.0 . . ?
C4 C3 H3A 128.0 . . ?
N2 C4 C3 108.7(5) . . ?
N2 C4 C5 114.0(5) . . ?
C3 C4 C5 137.0(5) . . ?
O4 C5 O3 125.9(5) . . ?
O4 C5 C4 120.2(5) . . ?
O3 C5 C4 113.9(5) . . ?
C6 N3 C10 120.0 . . ?
C6 N3 Cu1 121.1(6) . . ?
C10 N3 Cu1 118.9(6) . . ?
N3 C6 C7 120.0 . . ?
N3 C6 H6A 120.0 . . ?
C7 C6 H6A 120.0 . . ?
C8 C7 C6 120.0 . . ?
C8 C7 H7A 120.0 . . ?
C6 C7 H7A 120.0 . . ?
C7 C8 C9 120.0 . . ?
C7 C8 H8A 120.0 . . ?
C9 C8 H8A 120.0 . . ?
C8 C9 C10 120.0 . . ?
C8 C9 H9A 120.0 . . ?
C10 C9 H9A 120.0 . . ?
C9 C10 N3 120.0 . . ?
C9 C10 H10A 120.0 . . ?
N3 C10 H10A 120.0 . . ?
C6' N3' C10' 120.0 . . ?
C6' N3' Cu1 119.5(10) . . ?
C10' N3' Cu1 120.5(10) . . ?
C7' C6' N3' 120.0 . . ?
C7' C6' H6'A 120.0 . . ?
N3' C6' H6'A 120.0 . . ?
C8' C7' C6' 120.0 . . ?
C8' C7' H7'A 120.0 . . ?
C6' C7' H7'A 120.0 . . ?
C7' C8' C9' 120.0 . . ?
C7' C8' H8'A 120.0 . . ?
C9' C8' H8'A 120.0 . . ?
C10' C9' C8' 120.0 . . ?
C10' C9' H9'A 120.0 . . ?
C8' C9' H9'A 120.0 . . ?
C9' C10' N3' 120.0 . . ?
C9' C10' H10B 120.0 . . ?
N3' C10' H10B 120.0 . . ?
H5A O5 H5B 104.6 . . ?
H5A O5 H5C 30.8 . . ?
H5B O5 H5C 107.4 . . ?
H5A O5 H5D 86.3 . . ?
H5B O5 H5D 130(10) . . ?
H5C O5 H5D 60.5 . . ?
H5A O5' H5B 66.5 . . ?
H5A O5' H5C 37.6 . . ?
H5B O5' H5C 96.2 . . ?
H5A O5' H5D 118.6 . . ?
H5B O5' H5D 141(10) . . ?
H5C O5' H5D 108.6 . . ?
H6B O6 H6C 104.5 . . ?
C15 N4 C11 116.8(13) . . ?
C15 N4 C17 102.7(12) . . ?
C11 N4 C17 111.3(13) . . ?
C15 N4 C13 108.5(12) . . ?
C11 N4 C13 106.4(13) . . ?
C17 N4 C13 111.1(12) . . ?
N4 C11 C12 115.4(17) . . ?
N4 C11 H11A 108.4 . . ?
C12 C11 H11A 108.4 . . ?
N4 C11 H11B 108.4 . . ?
C12 C11 H11B 108.4 . . ?
H11A C11 H11B 107.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 N4 114.3(15) . . ?
C14 C13 H13A 108.7 . . ?
N4 C13 H13A 108.7 . . ?
C14 C13 H13B 108.7 . . ?
N4 C13 H13B 108.7 . . ?
H13A C13 H13B 107.6 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N4 C15 C16 103.1(14) . . ?
N4 C15 H15A 111.1 . . ?
C16 C15 H15A 111.1 . . ?
N4 C15 H15B 111.1 . . ?
C16 C15 H15B 111.1 . . ?
H15A C15 H15B 109.1 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 C18 116.2(13) . . ?
N4 C17 H17A 108.2 . . ?
C18 C17 H17A 108.2 . . ?
N4 C17 H17B 108.2 . . ?
C18 C17 H17B 108.2 . . ?
H17A C17 H17B 107.4 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C15' N4' C13' 108.9(19) . . ?
C15' N4' C11' 122(2) . . ?
C13' N4' C11' 110.3(14) . . ?
C15' N4' C17' 98.8(15) . . ?
C13' N4' C17' 99.0(16) . . ?
C11' N4' C17' 114.6(18) . . ?
C12' C11' N4' 113.9(18) . . ?
C12' C11' H11C 108.8 . . ?
N4' C11' H11C 108.8 . . ?
C12' C11' H11D 108.8 . . ?
N4' C11' H11D 108.8 . . ?
H11C C11' H11D 107.7 . . ?
C11' C12' H12D 109.5 . . ?
C11' C12' H12E 109.5 . . ?
H12D C12' H12E 109.5 . . ?
C11' C12' H12F 109.5 . . ?
H12D C12' H12F 109.5 . . ?
H12E C12' H12F 109.5 . . ?
C14' C13' N4' 126.3(18) . . ?
C14' C13' H13C 105.7 . . ?
N4' C13' H13C 105.7 . . ?
C14' C13' H13D 105.7 . . ?
N4' C13' H13D 105.7 . . ?
H13C C13' H13D 106.2 . . ?
C13' C14' H14D 109.5 . . ?
C13' C14' H14E 109.5 . . ?
H14D C14' H14E 109.5 . . ?
C13' C14' H14F 109.5 . . ?
H14D C14' H14F 109.5 . . ?
H14E C14' H14F 109.5 . . ?
N4' C15' C16' 107.3(16) . . ?
N4' C15' H15C 110.3 . . ?
C16' C15' H15C 110.3 . . ?
N4' C15' H15D 110.3 . . ?
C16' C15' H15D 110.3 . . ?
H15C C15' H15D 108.5 . . ?
C15' C16' H16D 109.5 . . ?
C15' C16' H16E 109.5 . . ?
H16D C16' H16E 109.5 . . ?
C15' C16' H16F 109.5 . . ?
H16D C16' H16F 109.5 . . ?
H16E C16' H16F 109.5 . . ?
C18' C17' N4' 112.8(18) . . ?
C18' C17' H17C 109.0 . . ?
N4' C17' H17C 109.0 . . ?
C18' C17' H17D 109.0 . . ?
N4' C17' H17D 109.0 . . ?
H17C C17' H17D 107.8 . . ?
C17' C18' H18D 109.5 . . ?
C17' C18' H18E 109.5 . . ?
H18D C18' H18E 109.5 . . ?
C17' C18' H18F 109.5 . . ?
H18D C18' H18F 109.5 . . ?
H18E C18' H18F 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
N1 Cu1 O1 C1 -5.4(5) . . . . ?
N2 Cu1 O1 C1 66.2(7) 2_755 . . . ?
O3 Cu1 O1 C1 153.1(5) 2_755 . . . ?
N3' Cu1 O1 C1 -113.6(7) . . . . ?
N3 Cu1 O1 C1 -106.7(6) . . . . ?
N2 Cu1 N1 N2 7.5(5) 2_755 . . . ?
O1 Cu1 N1 N2 168.8(6) . . . . ?
O3 Cu1 N1 N2 76.2(7) 2_755 . . . ?
N3' Cu1 N1 N2 -96.7(9) . . . . ?
N3 Cu1 N1 N2 -97.5(6) . . . . ?
N2 Cu1 N1 C2 -153.7(4) 2_755 . . . ?
O1 Cu1 N1 C2 7.7(4) . . . . ?
O3 Cu1 N1 C2 -84.9(6) 2_755 . . . ?
N3' Cu1 N1 C2 102.2(8) . . . . ?
N3 Cu1 N1 C2 101.4(6) . . . . ?
C2 N1 N2 C4 0.2(6) . . . . ?
Cu1 N1 N2 C4 -161.9(4) . . . . ?
C2 N1 N2 Cu1 165.6(4) . . . 2_755 ?
Cu1 N1 N2 Cu1 3.5(8) . . . 2_755 ?
Cu1 O1 C1 O2 -177.4(7) . . . . ?
Cu1 O1 C1 C2 2.3(7) . . . . ?
N2 N1 C2 C3 0.2(7) . . . . ?
Cu1 N1 C2 C3 165.9(4) . . . . ?
N2 N1 C2 C1 -174.2(5) . . . . ?
Cu1 N1 C2 C1 -8.5(7) . . . . ?
O2 C1 C2 N1 -176.3(7) . . . . ?
O1 C1 C2 N1 3.9(8) . . . . ?
O2 C1 C2 C3 11.5(13) . . . . ?
O1 C1 C2 C3 -168.3(7) . . . . ?
N1 C2 C3 C4 -0.5(7) . . . . ?
C1 C2 C3 C4 171.9(7) . . . . ?
N1 N2 C4 C3 -0.5(6) . . . . ?
Cu1 N2 C4 C3 -168.7(4) 2_755 . . . ?
N1 N2 C4 C5 174.2(5) . . . . ?
Cu1 N2 C4 C5 6.0(6) 2_755 . . . ?
C2 C3 C4 N2 0.6(7) . . . . ?
C2 C3 C4 C5 -172.3(6) . . . . ?
Cu1 O3 C5 O4 174.9(5) 2_755 . . . ?
Cu1 O3 C5 C4 -3.5(6) 2_755 . . . ?
N2 C4 C5 O4 180.0(5) . . . . ?
C3 C4 C5 O4 -7.4(11) . . . . ?
N2 C4 C5 O3 -1.5(7) . . . . ?
C3 C4 C5 O3 171.2(7) . . . . ?
N1 Cu1 N3 C6 79.9(5) . . . . ?
N2 Cu1 N3 C6 -15.8(5) 2_755 . . . ?
O1 Cu1 N3 C6 161.7(4) . . . . ?
O3 Cu1 N3 C6 -97.8(4) 2_755 . . . ?
N3' Cu1 N3 C6 -94(8) . . . . ?
N1 Cu1 N3 C10 -101.2(5) . . . . ?
N2 Cu1 N3 C10 163.1(4) 2_755 . . . ?
O1 Cu1 N3 C10 -19.4(5) . . . . ?
O3 Cu1 N3 C10 81.1(5) 2_755 . . . ?
N3' Cu1 N3 C10 85(8) . . . . ?
C10 N3 C6 C7 0.0 . . . . ?
Cu1 N3 C6 C7 178.9(7) . . . . ?
N3 C6 C7 C8 0.0 . . . . ?
C6 C7 C8 C9 0.0 . . . . ?
C7 C8 C9 C10 0.0 . . . . ?
C8 C9 C10 N3 0.0 . . . . ?
C6 N3 C10 C9 0.0 . . . . ?
Cu1 N3 C10 C9 -178.9(7) . . . . ?
N1 Cu1 N3' C6' 77.7(8) . . . . ?
N2 Cu1 N3' C6' -19.4(8) 2_755 . . . ?
O1 Cu1 N3' C6' 160.5(6) . . . . ?
O3 Cu1 N3' C6' -99.7(7) 2_755 . . . ?
N3 Cu1 N3' C6' 84(8) . . . . ?
N1 Cu1 N3' C10' -103.6(9) . . . . ?
N2 Cu1 N3' C10' 159.3(8) 2_755 . . . ?
O1 Cu1 N3' C10' -20.8(10) . . . . ?
O3 Cu1 N3' C10' 78.9(9) 2_755 . . . ?
N3 Cu1 N3' C10' -97(8) . . . . ?
C10' N3' C6' C7' 0.0 . . . . ?
Cu1 N3' C6' C7' 178.7(13) . . . . ?
N3' C6' C7' C8' 0.0 . . . . ?
C6' C7' C8' C9' 0.0 . . . . ?
C7' C8' C9' C10' 0.0 . . . . ?
C8' C9' C10' N3' 0.0 . . . . ?
C6' N3' C10' C9' 0.0 . . . . ?
Cu1 N3' C10' C9' -178.7(13) . . . . ?
C15 N4 C11 C12 56(2) . . . . ?
C17 N4 C11 C12 -62(2) . . . . ?
C13 N4 C11 C12 176.9(16) . . . . ?
C15 N4 C13 C14 -40.0(17) . . . . ?
C11 N4 C13 C14 -166.5(14) . . . . ?
C17 N4 C13 C14 72.2(17) . . . . ?
C11 N4 C15 C16 61.0(19) . . . . ?
C17 N4 C15 C16 -176.9(14) . . . . ?
C13 N4 C15 C16 -59.2(16) . . . . ?
C15 N4 C17 C18 176.8(14) . . . . ?
C11 N4 C17 C18 -57(2) . . . . ?
C13 N4 C17 C18 61.0(19) . . . . ?
C15' N4' C11' C12' 65(3) . . . . ?
C13' N4' C11' C12' -165(2) . . . . ?
C17' N4' C11' C12' -54(3) . . . . ?
C15' N4' C13' C14' 99(2) . . . . ?
C11' N4' C13' C14' -38(3) . . . . ?
C17' N4' C13' C14' -159(2) . . . . ?
C13' N4' C15' C16' -86(2) . . . . ?
C11' N4' C15' C16' 45(3) . . . . ?
C17' N4' C15' C16' 171(2) . . . . ?
C15' N4' C17' C18' 178(3) . . . . ?
C13' N4' C17' C18' 67(3) . . . . ?
C11' N4' C17' C18' -50(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        70.97
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.028
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.104
####################################################################### 
# 
# 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_full_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1865966'
loop_
_audit_author_name
_audit_author_address

'Shiqun Xiang, Xiaofeng Zhang,Hui Chen, Yinghua Li, Weibin Fan and Deguang Huang'
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2018-09-05 deposited with the CCDC.	2019-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        (Et4N)4[Cu(pdc)2](H2O)10
_chemical_name_common            (Et4N)4[Cu(pdc)2](H2O)10
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H2 Cu N4 O8, 4(C8 H20 N), 10(H2 O)'
_chemical_formula_sum            'C42 H102 Cu N8 O18'
_chemical_formula_weight         1070.86

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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                   21.6716(4)
_cell_length_b                   7.91640(15)
_cell_length_c                   32.9340(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.2825(15)
_cell_angle_gamma                90.00
_cell_volume                     5640.92(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6183
_cell_measurement_theta_min      4.0750
_cell_measurement_theta_max      73.8550

_exptl_crystal_description       purple
_exptl_crystal_colour            needle
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2332
_exptl_absorpt_coefficient_mu    1.147
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8378
_exptl_absorpt_correction_T_max  0.9556
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10445
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         4.09
_diffrn_reflns_theta_max         70.00
_reflns_number_total             5324
_reflns_number_gt                4763
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0480P)²+2.6365P] 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         5324
_refine_ls_number_parameters     353
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0304
_refine_ls_wR_factor_ref         0.0849
_refine_ls_wR_factor_gt          0.0818
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.0000 0.0000 0.0000 0.01550(9) Uani 1 2 d S . .
C1 C -0.11488(6) 0.14431(16) -0.01473(4) 0.0178(2) Uani 1 1 d . . .
C2 C 0.08656(6) -0.13740(16) 0.05444(4) 0.0163(2) Uani 1 1 d . . .
C3 C 0.10399(6) -0.18150(16) 0.09414(4) 0.0172(2) Uani 1 1 d . . .
H3 H 0.1416 -0.2317 0.1042 0.021 Uiso 1 1 calc R . .
C4 C 0.05301(6) -0.13462(16) 0.11592(3) 0.0157(2) Uani 1 1 d . . .
C5 C 0.04606(6) -0.15237(16) 0.16093(3) 0.0171(2) Uani 1 1 d . . .
N1 N 0.02929(5) -0.06968(14) 0.05339(3) 0.0178(2) Uani 1 1 d . . .
N2 N 0.00783(5) -0.06685(14) 0.09087(3) 0.0185(2) Uani 1 1 d . . .
O1 O -0.08072(4) 0.08511(12) 0.01540(3) 0.01977(19) Uani 1 1 d . . .
O2 O -0.16751(4) 0.20219(14) -0.01119(3) 0.0265(2) Uani 1 1 d . . .
O3 O -0.00228(5) -0.09895(15) 0.17581(3) 0.0294(2) Uani 1 1 d . . .
O4 O 0.09082(4) -0.21877(12) 0.18100(3) 0.0214(2) Uani 1 1 d . . .
N3 N -0.13423(5) -0.42468(14) 0.07639(3) 0.0203(2) Uani 1 1 d . . .
C6 C -0.12381(6) -0.35375(18) 0.11924(4) 0.0235(3) Uani 1 1 d . . .
H6A H -0.0815 -0.3064 0.1222 0.028 Uiso 1 1 calc R . .
H6B H -0.1532 -0.2597 0.1226 0.028 Uiso 1 1 calc R . .
C7 C -0.13147(7) -0.48072(19) 0.15297(4) 0.0284(3) Uani 1 1 d . . .
H7A H -0.1240 -0.4251 0.1794 0.043 Uiso 1 1 calc R . .
H7B H -0.1018 -0.5730 0.1505 0.043 Uiso 1 1 calc R . .
H7C H -0.1736 -0.5262 0.1509 0.043 Uiso 1 1 calc R . .
C8 C -0.08944(7) -0.56687(18) 0.06915(4) 0.0277(3) Uani 1 1 d . . .
H8A H -0.0992 -0.6134 0.0416 0.033 Uiso 1 1 calc R . .
H8B H -0.0963 -0.6580 0.0890 0.033 Uiso 1 1 calc R . .
C9 C -0.02162(8) -0.5189(2) 0.07256(6) 0.0424(4) Uani 1 1 d . . .
H9A H 0.0036 -0.6187 0.0675 0.064 Uiso 1 1 calc R . .
H9B H -0.0109 -0.4756 0.0999 0.064 Uiso 1 1 calc R . .
H9C H -0.0137 -0.4315 0.0524 0.064 Uiso 1 1 calc R . .
C10 C -0.12600(7) -0.27831(18) 0.04741(4) 0.0262(3) Uani 1 1 d . . .
H10A H -0.1579 -0.1922 0.0521 0.031 Uiso 1 1 calc R . .
H10B H -0.0852 -0.2259 0.0540 0.031 Uiso 1 1 calc R . .
C11 C -0.13025(9) -0.3259(2) 0.00270(5) 0.0405(4) Uani 1 1 d . . .
H11A H -0.1244 -0.2248 -0.0138 0.061 Uiso 1 1 calc R . .
H11B H -0.1710 -0.3747 -0.0044 0.061 Uiso 1 1 calc R . .
H11C H -0.0981 -0.4088 -0.0026 0.061 Uiso 1 1 calc R . .
C12 C -0.19839(7) -0.50163(18) 0.07013(4) 0.0261(3) Uani 1 1 d . . .
H12A H -0.2036 -0.5438 0.0418 0.031 Uiso 1 1 calc R . .
H12B H -0.2010 -0.6001 0.0885 0.031 Uiso 1 1 calc R . .
C13 C -0.25112(7) -0.3832(2) 0.07768(6) 0.0383(4) Uani 1 1 d . . .
H13A H -0.2905 -0.4431 0.0730 0.057 Uiso 1 1 calc R . .
H13B H -0.2499 -0.2867 0.0591 0.057 Uiso 1 1 calc R . .
H13C H -0.2472 -0.3428 0.1058 0.057 Uiso 1 1 calc R . .
N4 N -0.35967(5) -0.22094(14) 0.20546(3) 0.0212(2) Uani 1 1 d . . .
C14 C -0.36892(6) -0.37853(17) 0.23074(4) 0.0227(3) Uani 1 1 d . . .
H14A H -0.4107 -0.4241 0.2236 0.027 Uiso 1 1 calc R . .
H14B H -0.3386 -0.4647 0.2231 0.027 Uiso 1 1 calc R . .
C15 C -0.36243(8) -0.3540(2) 0.27633(4) 0.0326(3) Uani 1 1 d . . .
H15A H -0.3692 -0.4620 0.2899 0.049 Uiso 1 1 calc R . .
H15B H -0.3931 -0.2716 0.2845 0.049 Uiso 1 1 calc R . .
H15C H -0.3208 -0.3124 0.2841 0.049 Uiso 1 1 calc R . .
C16 C -0.29703(7) -0.1417(2) 0.21633(5) 0.0315(3) Uani 1 1 d . . .
H16A H -0.2936 -0.0360 0.2006 0.038 Uiso 1 1 calc R . .
H16B H -0.2951 -0.1109 0.2455 0.038 Uiso 1 1 calc R . .
C17 C -0.24234(7) -0.2522(2) 0.20854(6) 0.0396(4) Uani 1 1 d . . .
H17A H -0.2041 -0.1916 0.2164 0.059 Uiso 1 1 calc R . .
H17B H -0.2430 -0.2809 0.1796 0.059 Uiso 1 1 calc R . .
H17C H -0.2444 -0.3560 0.2246 0.059 Uiso 1 1 calc R . .
C18 C -0.36528(7) -0.27607(18) 0.16135(4) 0.0247(3) Uani 1 1 d . . .
H18A H -0.4061 -0.3300 0.1559 0.030 Uiso 1 1 calc R . .
H18B H -0.3333 -0.3625 0.1570 0.030 Uiso 1 1 calc R . .
C19 C -0.35845(8) -0.1344(2) 0.13097(5) 0.0370(4) Uani 1 1 d . . .
H19A H -0.3626 -0.1801 0.1033 0.055 Uiso 1 1 calc R . .
H19B H -0.3177 -0.0819 0.1355 0.055 Uiso 1 1 calc R . .
H19C H -0.3907 -0.0495 0.1344 0.055 Uiso 1 1 calc R . .
C20 C -0.40767(7) -0.08820(19) 0.21384(5) 0.0311(3) Uani 1 1 d . . .
H20A H -0.4059 -0.0656 0.2435 0.037 Uiso 1 1 calc R . .
H20B H -0.3965 0.0178 0.2001 0.037 Uiso 1 1 calc R . .
C21 C -0.47330(8) -0.1331(3) 0.20034(6) 0.0425(4) Uani 1 1 d . . .
H21A H -0.5008 -0.0401 0.2070 0.064 Uiso 1 1 calc R . .
H21B H -0.4856 -0.2359 0.2144 0.064 Uiso 1 1 calc R . .
H21C H -0.4762 -0.1523 0.1709 0.064 Uiso 1 1 calc R . .
O5 O 0.21978(6) 0.82031(17) 0.17802(4) 0.0398(3) Uani 1 1 d . . .
O6 O 0.25385(5) 0.56977(14) 0.04547(3) 0.0284(2) Uani 1 1 d . . .
O7 O -0.08864(5) 0.09065(14) 0.13069(3) 0.0283(2) Uani 1 1 d . . .
O8 O 0.07751(6) -0.25739(16) 0.26700(3) 0.0354(3) Uani 1 1 d . . .
O9 O -0.21723(6) 0.08575(18) 0.12899(4) 0.0368(3) Uani 1 1 d . . .
H7D H -0.0712(11) 0.059(3) 0.1119(7) 0.048(6) Uiso 1 1 d . . .
H5A H 0.2375(10) 0.752(3) 0.1625(6) 0.042(6) Uiso 1 1 d . . .
H6C H 0.2782(11) 0.600(3) 0.0313(7) 0.052(7) Uiso 1 1 d . . .
H6D H 0.2240(11) 0.634(3) 0.0401(6) 0.044(6) Uiso 1 1 d . . .
H7E H -0.0648(10) 0.043(3) 0.1477(7) 0.041(6) Uiso 1 1 d . . .
H9D H -0.1813(11) 0.088(3) 0.1321(6) 0.039(6) Uiso 1 1 d . . .
H8C H 0.0486(11) -0.209(3) 0.2782(7) 0.049(6) Uiso 1 1 d . . .
H5B H 0.1850(11) 0.801(3) 0.1765(6) 0.037(5) Uiso 1 1 d . . .
H9E H -0.2260(11) 0.078(3) 0.1058(8) 0.050(7) Uiso 1 1 d . . .
H8D H 0.0733(10) -0.235(3) 0.2449(8) 0.050(6) Uiso 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
Cu1 N1 1.9160(10) 5 ?
Cu1 N1 1.9160(10) . ?
Cu1 O1 1.9681(9) 5 ?
Cu1 O1 1.9681(9) . ?
C1 O2 1.2408(16) . ?
C1 O1 1.2918(15) . ?
C1 C2 1.4770(16) 5 ?
C2 N1 1.3507(16) . ?
C2 C3 1.3848(17) . ?
C2 C1 1.4770(16) 5 ?
C3 C4 1.4012(17) . ?
C4 N2 1.3543(16) . ?
C4 C5 1.5051(16) . ?
C5 O3 1.2551(16) . ?
C5 O4 1.2575(16) . ?
N1 N2 1.3440(15) . ?
N3 C8 1.5142(18) . ?
N3 C10 1.5181(17) . ?
N3 C12 1.5211(17) . ?
N3 C6 1.5237(16) . ?
C6 C7 1.514(2) . ?
C8 C9 1.516(2) . ?
C10 C11 1.518(2) . ?
C12 C13 1.510(2) . ?
N4 C20 1.5151(18) . ?
N4 C18 1.5149(17) . ?
N4 C16 1.5194(18) . ?
N4 C14 1.5196(17) . ?
C14 C15 1.5125(18) . ?
C16 C17 1.507(2) . ?
C18 C19 1.516(2) . ?
C20 C21 1.508(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
N1 Cu1 N1 180.00(9) 5 . ?
N1 Cu1 O1 96.58(4) 5 5 ?
N1 Cu1 O1 83.42(4) . 5 ?
N1 Cu1 O1 83.42(4) 5 . ?
N1 Cu1 O1 96.58(4) . . ?
O1 Cu1 O1 180.00(5) 5 . ?
O2 C1 O1 123.44(11) . . ?
O2 C1 C2 121.85(11) . 5 ?
O1 C1 C2 114.70(11) . 5 ?
N1 C2 C3 108.94(10) . . ?
N1 C2 C1 114.83(10) . 5 ?
C3 C2 C1 136.22(11) . 5 ?
C2 C3 C4 103.67(10) . . ?
N2 C4 C3 110.90(10) . . ?
N2 C4 C5 121.81(11) . . ?
C3 C4 C5 127.28(11) . . ?
O3 C5 O4 124.86(11) . . ?
O3 C5 C4 119.08(11) . . ?
O4 C5 C4 116.05(11) . . ?
N2 N1 C2 110.42(10) . . ?
N2 N1 Cu1 136.41(8) . . ?
C2 N1 Cu1 113.16(8) . . ?
N1 N2 C4 106.07(10) . . ?
C1 O1 Cu1 113.89(8) . . ?
C8 N3 C10 111.65(11) . . ?
C8 N3 C12 105.67(10) . . ?
C10 N3 C12 111.09(10) . . ?
C8 N3 C6 110.94(10) . . ?
C10 N3 C6 106.53(10) . . ?
C12 N3 C6 111.04(10) . . ?
C7 C6 N3 114.72(11) . . ?
N3 C8 C9 115.46(12) . . ?
C11 C10 N3 114.70(12) . . ?
C13 C12 N3 115.06(12) . . ?
C20 N4 C18 110.87(11) . . ?
C20 N4 C16 106.52(11) . . ?
C18 N4 C16 111.50(11) . . ?
C20 N4 C14 110.86(11) . . ?
C18 N4 C14 106.44(10) . . ?
C16 N4 C14 110.72(11) . . ?
C15 C14 N4 115.51(12) . . ?
C17 C16 N4 114.91(13) . . ?
N4 C18 C19 114.46(13) . . ?
C21 C20 N4 115.39(13) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        70.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.047
####################################################################### 
# 
# 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_Compound8
_database_code_depnum_ccdc_archive 'CCDC 1940796'
loop_
_audit_author_name
_audit_author_address
'Deguang Huang'
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2019-07-16 deposited with the CCDC.	2019-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 

;
_chemical_name_common            '[Cu3(L)2(2-Me-Py)3(H2O)4].2-Me-Py.THF.2H2O'
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H31 Cu3 N7 O12,C6H7N,C4H8O,H4O2'
_chemical_formula_sum            'C38 H50 Cu3 N8 O15'
_chemical_formula_weight         1049.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/n
_symmetry_space_group_name_Hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_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                   15.3643(2)
_cell_length_b                   16.8900(2)
_cell_length_c                   17.5664(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.5437(14)
_cell_angle_gamma                90.00
_cell_volume                     4412.46(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    12516
_cell_measurement_theta_min      3.9330
_cell_measurement_theta_max      73.3320

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2164
_exptl_absorpt_coefficient_mu    2.339
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7666
_exptl_absorpt_correction_T_max  0.8724
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  Mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33381
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.42
_diffrn_reflns_theta_max         69.99
_reflns_number_total             8355
_reflns_number_gt                7173
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 
;

# start Validation Reply Form
_vrf_PLAT220_Compound8           
;
PROBLEM:  Non-Solvent  Resd 1  C   Ueq(max)/Ueq(min) Range   3.9 Ratio
RESPONSE: The molecules of coordinated 2-Me-Py and solvated THF were treated as
diordered models. The occupancies of the coordinated 2-Me-Py molecule was refined
as 0.68 and 0.32;The occupancies of the THF molecule was refined as 0.5 and 0.5. 
The temperature factors of these atoms have been constrained by using commands
of DELU/SIMU.  
;

# end Validation Reply Form

# start Validation Reply Form
_vrf_PLAT977_Compound8           
;
PROBLEM:  Check Negative Difference Density on H28B  -0.49 eA-3  
RESPONSE: All the hydrogen atoms of water were added from Fourier Maps. The 
bond lengths (H-O) and bond angles (H-O-H) of water were refined freely, with
the refinement of the temperature factors of coordinated water molecules and 
solvated water molecules as -1.5000 and -1.2000, respectively.  
;

# end Validation Reply Form




_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)+(0.0498P)²+3.6215P] 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         8355
_refine_ls_number_parameters     676
_refine_ls_number_restraints     357
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.0920
_refine_ls_wR_factor_gt          0.0880
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.32342(2) 0.650903(18) 0.922153(16) 0.01508(9) Uani 1 1 d . A .
Cu2 Cu 0.491294(18) 0.670583(18) 0.756712(15) 0.01194(8) Uani 1 1 d . . .
Cu3 Cu 0.664211(19) 0.651766(18) 0.596280(16) 0.01371(8) Uani 1 1 d . A .
O1 O 0.35785(10) 0.69980(10) 1.02790(8) 0.0214(3) Uani 1 1 d . A .
O2 O 0.46863(10) 0.76644(11) 1.10982(9) 0.0266(4) Uani 1 1 d . A .
O3 O 0.62179(9) 0.69599(9) 0.79285(8) 0.0149(3) Uani 1 1 d . A .
O4 O 0.72515(10) 0.74488(10) 0.89487(8) 0.0199(3) Uani 1 1 d . A .
O5 O 0.36050(9) 0.69415(9) 0.71961(8) 0.0176(3) Uani 1 1 d . A .
O6 O 0.25661(10) 0.74039(11) 0.61641(9) 0.0272(4) Uani 1 1 d . A .
O7 O 0.62742(10) 0.69175(10) 0.48690(8) 0.0202(3) Uani 1 1 d . A .
O8 O 0.51054(11) 0.74202(12) 0.39798(9) 0.0326(4) Uani 1 1 d . A .
N1 N 0.44141(11) 0.69443(10) 0.91627(9) 0.0131(3) Uani 1 1 d . . .
N2 N 0.49680(11) 0.69208(10) 0.86828(9) 0.0127(3) Uani 1 1 d . A .
N3 N 0.48686(11) 0.69214(10) 0.64607(9) 0.0126(3) Uani 1 1 d . A .
N4 N 0.54294(11) 0.69233(10) 0.59849(9) 0.0125(3) Uani 1 1 d . . .
N5 N 0.25366(12) 0.56425(12) 0.96143(10) 0.0205(4) Uani 1 1 d . . .
N7 N 0.74278(12) 0.56701(11) 0.56713(10) 0.0190(4) Uani 1 1 d . . .
N8 N 0.83734(13) 0.51350(12) 0.75933(11) 0.0249(4) Uani 1 1 d . . .
C1 C 0.43681(14) 0.73203(14) 1.04689(12) 0.0187(4) Uani 1 1 d . . .
C2 C 0.48748(14) 0.72565(12) 0.98566(11) 0.0143(4) Uani 1 1 d . A .
C3 C 0.57471(14) 0.74434(12) 0.98313(11) 0.0147(4) Uani 1 1 d . . .
H3A H 0.6214 0.7669 1.0233 0.018 Uiso 1 1 calc R A .
C4 C 0.57712(13) 0.72204(12) 0.90747(11) 0.0125(4) Uani 1 1 d . A .
C5 C 0.64838(14) 0.72218(12) 0.86418(11) 0.0143(4) Uani 1 1 d . . .
C6 C 0.33360(14) 0.71847(13) 0.64764(12) 0.0169(4) Uani 1 1 d . . .
C7 C 0.40540(13) 0.71788(12) 0.60451(11) 0.0130(4) Uani 1 1 d . A .
C8 C 0.40788(13) 0.73535(12) 0.52776(11) 0.0141(4) Uani 1 1 d . . .
H8B H 0.3607 0.7545 0.4859 0.017 Uiso 1 1 calc R A .
C9 C 0.49612(14) 0.71796(12) 0.52704(11) 0.0140(4) Uani 1 1 d . A .
C10 C 0.54581(14) 0.71831(14) 0.46440(12) 0.0197(4) Uani 1 1 d . . .
C11 C 0.17952(16) 0.58383(15) 0.98440(14) 0.0267(5) Uani 1 1 d . A .
H11A H 0.1607 0.6376 0.9803 0.032 Uiso 1 1 calc R . .
C12 C 0.12941(19) 0.52911(17) 1.01377(16) 0.0362(6) Uani 1 1 d . . .
H12A H 0.0781 0.5452 1.0307 0.043 Uiso 1 1 calc R A .
C13 C 0.15537(19) 0.45081(17) 1.01804(16) 0.0369(6) Uani 1 1 d . A .
H13A H 0.1216 0.4118 1.0372 0.044 Uiso 1 1 calc R . .
C14 C 0.23122(19) 0.42988(17) 0.99408(16) 0.0366(6) Uani 1 1 d . . .
H14A H 0.2496 0.3761 0.9960 0.044 Uiso 1 1 calc R A .
C15 C 0.28081(17) 0.48781(16) 0.96704(15) 0.0300(5) Uani 1 1 d . A .
C16 C 0.3671(2) 0.46800(18) 0.9459(2) 0.0483(8) Uani 1 1 d . . .
H16A H 0.3652 0.4888 0.8935 0.072 Uiso 1 1 calc R A .
H16B H 0.3747 0.4104 0.9460 0.072 Uiso 1 1 calc R . .
H16C H 0.4176 0.4918 0.9845 0.072 Uiso 1 1 calc R . .
N6 N 0.49949(17) 0.54075(9) 0.76133(14) 0.0167(7) Uani 0.683(3) 1 d PGU A 1
C17 C 0.56915(16) 0.51469(12) 0.82305(13) 0.0241(7) Uani 0.683(3) 1 d PGU A 1
H17A H 0.6050 0.5519 0.8578 0.029 Uiso 0.683(3) 1 calc PR A 1
C18 C 0.58633(15) 0.43414(13) 0.83397(13) 0.0301(8) Uani 0.683(3) 1 d PGU A 1
H18A H 0.6339 0.4163 0.8762 0.036 Uiso 0.683(3) 1 calc PR A 1
C19 C 0.5339(2) 0.37965(9) 0.78317(17) 0.0300(8) Uani 0.683(3) 1 d PGU A 1
H19A H 0.5456 0.3246 0.7906 0.036 Uiso 0.683(3) 1 calc PR A 1
C20 C 0.46420(18) 0.40571(11) 0.72144(15) 0.0293(8) Uani 0.683(3) 1 d PGU A 1
H20A H 0.4283 0.3685 0.6867 0.035 Uiso 0.683(3) 1 calc PR A 1
C21 C 0.44701(14) 0.48626(13) 0.71052(12) 0.0207(7) Uani 0.683(3) 1 d PGU A 1
C22 C 0.3748(3) 0.5156(2) 0.6450(2) 0.0306(8) Uani 0.683(3) 1 d PU A 1
H22A H 0.3439 0.4707 0.6146 0.046 Uiso 0.683(3) 1 calc PR A 1
H22B H 0.4006 0.5494 0.6109 0.046 Uiso 0.683(3) 1 calc PR A 1
H22C H 0.3318 0.5464 0.6658 0.046 Uiso 0.683(3) 1 calc PR A 1
N6' N 0.4827(4) 0.5399(2) 0.7421(3) 0.0155(14) Uani 0.317(3) 1 d PGU A 2
C17' C 0.4164(3) 0.5158(3) 0.6768(3) 0.0213(14) Uani 0.317(3) 1 d PGU A 2
H17B H 0.3802 0.5541 0.6437 0.026 Uiso 0.317(3) 1 calc PR A 2
C18' C 0.4033(3) 0.4356(3) 0.6597(3) 0.0276(13) Uani 0.317(3) 1 d PGU A 2
H18B H 0.3580 0.4192 0.6151 0.033 Uiso 0.317(3) 1 calc PR A 2
C19' C 0.4563(5) 0.3796(2) 0.7080(4) 0.0316(16) Uani 0.317(3) 1 d PGU A 2
H19B H 0.4473 0.3249 0.6964 0.038 Uiso 0.317(3) 1 calc PR A 2
C20' C 0.5226(4) 0.4038(3) 0.7734(3) 0.0303(15) Uani 0.317(3) 1 d PGU A 2
H20B H 0.5588 0.3655 0.8064 0.036 Uiso 0.317(3) 1 calc PR A 2
C21' C 0.5357(3) 0.4839(3) 0.7904(3) 0.0214(12) Uani 0.317(3) 1 d PGU A 2
C22' C 0.6080(6) 0.5104(5) 0.8596(5) 0.0335(17) Uani 0.317(3) 1 d PU A 2
H22D H 0.6344 0.4641 0.8906 0.050 Uiso 0.317(3) 1 calc PR A 2
H22E H 0.5822 0.5458 0.8923 0.050 Uiso 0.317(3) 1 calc PR A 2
H22F H 0.6547 0.5385 0.8412 0.050 Uiso 0.317(3) 1 calc PR A 2
C23 C 0.82776(16) 0.58424(15) 0.56574(15) 0.0280(5) Uani 1 1 d . A .
H23A H 0.8473 0.6377 0.5730 0.034 Uiso 1 1 calc R . .
C24 C 0.88743(18) 0.52769(17) 0.55422(17) 0.0375(6) Uani 1 1 d . . .
H24A H 0.9471 0.5417 0.5536 0.045 Uiso 1 1 calc R A .
C25 C 0.8589(2) 0.45013(17) 0.54366(18) 0.0406(7) Uani 1 1 d . A .
H25A H 0.8989 0.4099 0.5357 0.049 Uiso 1 1 calc R . .
C26 C 0.77222(19) 0.43153(15) 0.54473(17) 0.0349(6) Uani 1 1 d . . .
H26A H 0.7515 0.3785 0.5365 0.042 Uiso 1 1 calc R A .
C27 C 0.71493(16) 0.49096(14) 0.55791(14) 0.0251(5) Uani 1 1 d . A .
C28 C 0.62111(19) 0.47363(17) 0.5638(2) 0.0440(7) Uani 1 1 d . . .
H28A H 0.5919 0.5230 0.5729 0.066 Uiso 1 1 calc R A .
H28B H 0.6232 0.4371 0.6076 0.066 Uiso 1 1 calc R . .
H28C H 0.5869 0.4494 0.5146 0.066 Uiso 1 1 calc R . .
C29 C 0.81186(17) 0.43727(15) 0.76510(14) 0.0274(5) Uani 1 1 d . . .
H29A H 0.7497 0.4246 0.7482 0.033 Uiso 1 1 calc R . .
C30 C 0.87142(18) 0.37760(15) 0.79409(15) 0.0318(6) Uani 1 1 d . . .
H30A H 0.8514 0.3247 0.7968 0.038 Uiso 1 1 calc R . .
C31 C 0.96162(18) 0.39693(16) 0.81930(16) 0.0337(6) Uani 1 1 d . . .
H31A H 1.0047 0.3571 0.8403 0.040 Uiso 1 1 calc R . .
C32 C 0.98859(17) 0.47325(16) 0.81398(15) 0.0310(5) Uani 1 1 d . . .
H32A H 1.0504 0.4869 0.8314 0.037 Uiso 1 1 calc R . .
C33 C 0.92499(17) 0.53105(15) 0.78293(14) 0.0277(5) Uani 1 1 d . . .
C34 C 0.9512(2) 0.61464(17) 0.77414(19) 0.0449(7) Uani 1 1 d . . .
H34A H 0.8974 0.6460 0.7512 0.067 Uiso 1 1 calc R . .
H34B H 0.9923 0.6168 0.7396 0.067 Uiso 1 1 calc R . .
H34C H 0.9813 0.6362 0.8259 0.067 Uiso 1 1 calc R . .
O13 O 0.1826(9) 0.4946(8) 0.7477(7) 0.0369(16) Uani 0.515(8) 1 d PU B 1
C35 C 0.1340(7) 0.5033(6) 0.6716(6) 0.0441(16) Uani 0.515(8) 1 d PU B 1
H35A H 0.1736 0.5149 0.6364 0.053 Uiso 0.515(8) 1 calc PR B 1
H35B H 0.0889 0.5461 0.6668 0.053 Uiso 0.515(8) 1 calc PR B 1
C36 C 0.0873(5) 0.4201(4) 0.6524(4) 0.0464(14) Uani 0.515(8) 1 d PU B 1
H36A H 0.0403 0.4107 0.6810 0.056 Uiso 0.515(8) 1 calc PR B 1
H36B H 0.0625 0.4115 0.5954 0.056 Uiso 0.515(8) 1 calc PR B 1
C37 C 0.1708(6) 0.3733(4) 0.6851(4) 0.0497(14) Uani 0.515(8) 1 d PU B 1
H37A H 0.1563 0.3176 0.6945 0.060 Uiso 0.515(8) 1 calc PR B 1
H37B H 0.2110 0.3743 0.6490 0.060 Uiso 0.515(8) 1 calc PR B 1
C38 C 0.2118(10) 0.4129(9) 0.7581(7) 0.0438(18) Uani 0.515(8) 1 d PU B 1
H38A H 0.2781 0.4095 0.7694 0.053 Uiso 0.515(8) 1 calc PR B 1
H38B H 0.1921 0.3884 0.8021 0.053 Uiso 0.515(8) 1 calc PR B 1
O13' O 0.1792(11) 0.4934(10) 0.7574(8) 0.0350(16) Uiso 0.485(8) 1 d PU B 2
C35' C 0.1147(7) 0.5054(7) 0.6784(7) 0.0407(17) Uiso 0.485(8) 1 d PU B 2
H35C H 0.1304 0.5530 0.6517 0.049 Uiso 0.485(8) 1 calc PR B 2
H35D H 0.0520 0.5102 0.6830 0.049 Uiso 0.485(8) 1 calc PR B 2
C36' C 0.1296(6) 0.4240(4) 0.6324(4) 0.0473(15) Uiso 0.485(8) 1 d PU B 2
H36C H 0.0780 0.4125 0.5872 0.057 Uiso 0.485(8) 1 calc PR B 2
H36D H 0.1859 0.4252 0.6148 0.057 Uiso 0.485(8) 1 calc PR B 2
C37' C 0.1348(6) 0.3671(4) 0.6996(4) 0.0429(14) Uiso 0.485(8) 1 d PU B 2
H37C H 0.1578 0.3147 0.6884 0.051 Uiso 0.485(8) 1 calc PR B 2
H37D H 0.0755 0.3602 0.7113 0.051 Uiso 0.485(8) 1 calc PR B 2
C38' C 0.2035(11) 0.4105(11) 0.7688(8) 0.0417(18) Uiso 0.485(8) 1 d PU B 2
H38C H 0.1972 0.3917 0.8206 0.050 Uiso 0.485(8) 1 calc PR B 2
H38D H 0.2661 0.4017 0.7656 0.050 Uiso 0.485(8) 1 calc PR B 2
O9 O 0.30052(11) 0.60396(10) 0.81735(9) 0.0196(3) Uani 1 1 d . . .
H9A H 0.258(2) 0.5754(18) 0.8008(17) 0.029 Uiso 1 1 d . . .
H9B H 0.307(2) 0.6355(18) 0.7827(18) 0.029 Uiso 1 1 d . . .
O10 O 0.21784(12) 0.73713(12) 0.88025(10) 0.0279(4) Uani 1 1 d . . .
H10A H 0.188(2) 0.733(2) 0.838(2) 0.042 Uiso 1 1 d . . .
H10B H 0.193(2) 0.759(2) 0.907(2) 0.042 Uiso 1 1 d . . .
O11 O 0.69262(11) 0.60653(10) 0.70179(9) 0.0183(3) Uani 1 1 d . . .
H11B H 0.682(2) 0.6324(17) 0.7365(18) 0.027 Uiso 1 1 d . . .
H11C H 0.739(2) 0.5829(17) 0.7184(17) 0.027 Uiso 1 1 d . . .
O12 O 0.75893(10) 0.74955(10) 0.63358(9) 0.0186(3) Uani 1 1 d . . .
H12B H 0.785(2) 0.7548(17) 0.6773(18) 0.028 Uiso 1 1 d . . .
H12C H 0.785(2) 0.7671(17) 0.6032(17) 0.028 Uiso 1 1 d . . .
O14 O 0.83235(12) 0.78345(12) 0.79310(10) 0.0276(4) Uani 1 1 d . . .
H14B H 0.886(2) 0.7733(18) 0.8201(18) 0.033 Uiso 1 1 d . . .
H14C H 0.802(2) 0.7671(18) 0.8195(18) 0.033 Uiso 1 1 d . . .
O15 O 0.14140(13) 0.72408(15) 0.71987(10) 0.0402(5) Uani 1 1 d . . .
H15A H 0.091(2) 0.725(2) 0.690(2) 0.048 Uiso 1 1 d . . .
H15B H 0.176(2) 0.736(2) 0.697(2) 0.048 Uiso 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
Cu1 O9 1.9536(15) . ?
Cu1 O1 1.9796(15) . ?
Cu1 N1 1.9828(17) . ?
Cu1 N5 2.0342(19) . ?
Cu1 O10 2.1667(17) . ?
Cu2 N3 1.9617(16) . ?
Cu2 N2 1.9740(16) . ?
Cu2 O5 1.9910(14) . ?
Cu2 O3 1.9920(14) . ?
Cu2 N6 2.1968(15) . ?
Cu2 N6' 2.222(3) . ?
Cu3 O11 1.9501(15) . ?
Cu3 O7 1.9804(14) . ?
Cu3 N4 1.9947(17) . ?
Cu3 N7 2.0197(18) . ?
Cu3 O12 2.1900(16) . ?
O1 C1 1.295(3) . ?
O2 C1 1.236(3) . ?
O3 C5 1.294(2) . ?
O4 C5 1.229(3) . ?
O5 C6 1.294(2) . ?
O6 C6 1.229(3) . ?
O7 C10 1.296(3) . ?
O8 C10 1.224(3) . ?
N1 N2 1.341(2) . ?
N1 C2 1.353(3) . ?
N2 C4 1.351(3) . ?
N3 N4 1.343(2) . ?
N3 C7 1.353(3) . ?
N4 C9 1.351(2) . ?
N5 C11 1.342(3) . ?
N5 C15 1.353(3) . ?
N7 C23 1.344(3) . ?
N7 C27 1.351(3) . ?
N8 C33 1.339(3) . ?
N8 C29 1.357(3) . ?
C1 C2 1.482(3) . ?
C2 C3 1.388(3) . ?
C3 C4 1.391(3) . ?
C3 H3A 0.9500 . ?
C4 C5 1.482(3) . ?
C6 C7 1.487(3) . ?
C7 C8 1.390(3) . ?
C8 C9 1.390(3) . ?
C8 H8B 0.9500 . ?
C9 C10 1.489(3) . ?
C11 C12 1.383(3) . ?
C11 H11A 0.9500 . ?
C12 C13 1.378(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.381(4) . ?
C13 H13A 0.9500 . ?
C14 C15 1.395(4) . ?
C14 H14A 0.9500 . ?
C15 C16 1.501(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
N6 C17 1.3900 . ?
N6 C21 1.3900 . ?
C17 C18 1.3900 . ?
C17 H17A 0.9500 . ?
C18 C19 1.3900 . ?
C18 H18A 0.9500 . ?
C19 C20 1.3900 . ?
C19 H19A 0.9500 . ?
C20 C21 1.3900 . ?
C20 H20A 0.9500 . ?
C21 C22 1.470(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
N6' C17' 1.3900 . ?
N6' C21' 1.3900 . ?
C17' C18' 1.3900 . ?
C17' H17B 0.9500 . ?
C18' C19' 1.3900 . ?
C18' H18B 0.9500 . ?
C19' C20' 1.3900 . ?
C19' H19B 0.9500 . ?
C20' C21' 1.3900 . ?
C20' H20B 0.9500 . ?
C21' C22' 1.493(9) . ?
C22' H22D 0.9800 . ?
C22' H22E 0.9800 . ?
C22' H22F 0.9800 . ?
C23 C24 1.374(4) . ?
C23 H23A 0.9500 . ?
C24 C25 1.379(4) . ?
C24 H24A 0.9500 . ?
C25 C26 1.373(4) . ?
C25 H25A 0.9500 . ?
C26 C27 1.392(3) . ?
C26 H26A 0.9500 . ?
C27 C28 1.500(4) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.371(4) . ?
C29 H29A 0.9500 . ?
C30 C31 1.384(4) . ?
C30 H30A 0.9500 . ?
C31 C32 1.364(4) . ?
C31 H31A 0.9500 . ?
C32 C33 1.392(3) . ?
C32 H32A 0.9500 . ?
C33 C34 1.487(4) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
O13 C35 1.366(15) . ?
O13 C38 1.45(2) . ?
C35 C36 1.575(12) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.494(10) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.442(15) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
O13' C38' 1.45(2) . ?
O13' C35' 1.502(17) . ?
C35' C36' 1.640(14) . ?
C35' H35C 0.9900 . ?
C35' H35D 0.9900 . ?
C36' C37' 1.508(11) . ?
C36' H36C 0.9900 . ?
C36' H36D 0.9900 . ?
C37' C38' 1.577(17) . ?
C37' H37C 0.9900 . ?
C37' H37D 0.9900 . ?
C38' H38C 0.9900 . ?
C38' H38D 0.9900 . ?
O9 H9A 0.80(3) . ?
O9 H9B 0.83(3) . ?
O10 H10A 0.77(3) . ?
O10 H10B 0.77(4) . ?
O11 H11B 0.80(3) . ?
O11 H11C 0.80(3) . ?
O12 H12B 0.78(3) . ?
O12 H12C 0.81(3) . ?
O14 H14B 0.86(3) . ?
O14 H14C 0.78(3) . ?
O15 H15A 0.82(4) . ?
O15 H15B 0.77(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
O9 Cu1 O1 174.90(7) . . ?
O9 Cu1 N1 92.98(7) . . ?
O1 Cu1 N1 82.06(6) . . ?
O9 Cu1 N5 92.41(7) . . ?
O1 Cu1 N5 91.22(7) . . ?
N1 Cu1 N5 148.31(7) . . ?
O9 Cu1 O10 90.59(7) . . ?
O1 Cu1 O10 92.25(7) . . ?
N1 Cu1 O10 110.45(7) . . ?
N5 Cu1 O10 100.69(8) . . ?
N3 Cu2 N2 158.70(7) . . ?
N3 Cu2 O5 81.81(6) . . ?
N2 Cu2 O5 94.38(6) . . ?
N3 Cu2 O3 93.30(6) . . ?
N2 Cu2 O3 81.67(6) . . ?
O5 Cu2 O3 156.02(7) . . ?
N3 Cu2 N6 102.08(8) . . ?
N2 Cu2 N6 99.16(8) . . ?
O5 Cu2 N6 104.80(8) . . ?
O3 Cu2 N6 99.18(8) . . ?
N3 Cu2 N6' 94.79(15) . . ?
N2 Cu2 N6' 106.50(15) . . ?
O5 Cu2 N6' 97.75(15) . . ?
O3 Cu2 N6' 106.07(15) . . ?
N6 Cu2 N6' 9.60(14) . . ?
O11 Cu3 O7 175.50(7) . . ?
O11 Cu3 N4 95.93(7) . . ?
O7 Cu3 N4 82.03(6) . . ?
O11 Cu3 N7 87.59(7) . . ?
O7 Cu3 N7 92.23(7) . . ?
N4 Cu3 N7 150.35(7) . . ?
O11 Cu3 O12 92.17(7) . . ?
O7 Cu3 O12 92.26(6) . . ?
N4 Cu3 O12 106.79(6) . . ?
N7 Cu3 O12 102.46(7) . . ?
C1 O1 Cu1 115.44(13) . . ?
C5 O3 Cu2 115.46(12) . . ?
C6 O5 Cu2 115.58(13) . . ?
C10 O7 Cu3 115.62(13) . . ?
N2 N1 C2 107.87(16) . . ?
N2 N1 Cu1 139.02(13) . . ?
C2 N1 Cu1 112.08(13) . . ?
N1 N2 C4 108.13(16) . . ?
N1 N2 Cu2 138.95(13) . . ?
C4 N2 Cu2 112.38(13) . . ?
N4 N3 C7 108.35(16) . . ?
N4 N3 Cu2 138.52(13) . . ?
C7 N3 Cu2 113.05(13) . . ?
N3 N4 C9 107.68(16) . . ?
N3 N4 Cu3 139.45(13) . . ?
C9 N4 Cu3 111.96(13) . . ?
C11 N5 C15 118.9(2) . . ?
C11 N5 Cu1 118.95(16) . . ?
C15 N5 Cu1 122.16(16) . . ?
C23 N7 C27 118.9(2) . . ?
C23 N7 Cu3 119.76(16) . . ?
C27 N7 Cu3 120.86(15) . . ?
C33 N8 C29 118.3(2) . . ?
O2 C1 O1 124.26(19) . . ?
O2 C1 C2 121.44(19) . . ?
O1 C1 C2 114.30(18) . . ?
N1 C2 C3 110.53(17) . . ?
N1 C2 C1 115.52(18) . . ?
C3 C2 C1 133.95(19) . . ?
C2 C3 C4 103.09(17) . . ?
C2 C3 H3A 128.5 . . ?
C4 C3 H3A 128.5 . . ?
N2 C4 C3 110.38(17) . . ?
N2 C4 C5 115.92(17) . . ?
C3 C4 C5 133.66(18) . . ?
O4 C5 O3 124.49(19) . . ?
O4 C5 C4 121.81(18) . . ?
O3 C5 C4 113.70(17) . . ?
O6 C6 O5 124.53(19) . . ?
O6 C6 C7 121.91(18) . . ?
O5 C6 C7 113.56(17) . . ?
N3 C7 C8 110.16(17) . . ?
N3 C7 C6 115.57(17) . . ?
C8 C7 C6 134.22(18) . . ?
C7 C8 C9 103.19(17) . . ?
C7 C8 H8B 128.4 . . ?
C9 C8 H8B 128.4 . . ?
N4 C9 C8 110.62(17) . . ?
N4 C9 C10 115.82(18) . . ?
C8 C9 C10 133.48(18) . . ?
O8 C10 O7 124.5(2) . . ?
O8 C10 C9 121.3(2) . . ?
O7 C10 C9 114.18(18) . . ?
N5 C11 C12 122.8(2) . . ?
N5 C11 H11A 118.6 . . ?
C12 C11 H11A 118.6 . . ?
C13 C12 C11 118.8(2) . . ?
C13 C12 H12A 120.6 . . ?
C11 C12 H12A 120.6 . . ?
C12 C13 C14 118.9(2) . . ?
C12 C13 H13A 120.5 . . ?
C14 C13 H13A 120.5 . . ?
C13 C14 C15 120.0(3) . . ?
C13 C14 H14A 120.0 . . ?
C15 C14 H14A 120.0 . . ?
N5 C15 C14 120.6(2) . . ?
N5 C15 C16 118.0(2) . . ?
C14 C15 C16 121.3(2) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C17 N6 C21 120.0 . . ?
C17 N6 Cu2 111.76(11) . . ?
C21 N6 Cu2 128.21(11) . . ?
N6 C17 C18 120.0 . . ?
N6 C17 H17A 120.0 . . ?
C18 C17 H17A 120.0 . . ?
C17 C18 C19 120.0 . . ?
C17 C18 H18A 120.0 . . ?
C19 C18 H18A 120.0 . . ?
C20 C19 C18 120.0 . . ?
C20 C19 H19A 120.0 . . ?
C18 C19 H19A 120.0 . . ?
C19 C20 C21 120.0 . . ?
C19 C20 H20A 120.0 . . ?
C21 C20 H20A 120.0 . . ?
C20 C21 N6 120.0 . . ?
C20 C21 C22 121.2(2) . . ?
N6 C21 C22 118.8(2) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C17' N6' C21' 120.0 . . ?
C17' N6' Cu2 113.4(3) . . ?
C21' N6' Cu2 126.6(3) . . ?
N6' C17' C18' 120.0 . . ?
N6' C17' H17B 120.0 . . ?
C18' C17' H17B 120.0 . . ?
C19' C18' C17' 120.0 . . ?
C19' C18' H18B 120.0 . . ?
C17' C18' H18B 120.0 . . ?
C18' C19' C20' 120.0 . . ?
C18' C19' H19B 120.0 . . ?
C20' C19' H19B 120.0 . . ?
C21' C20' C19' 120.0 . . ?
C21' C20' H20B 120.0 . . ?
C19' C20' H20B 120.0 . . ?
C20' C21' N6' 120.0 . . ?
C20' C21' C22' 120.3(4) . . ?
N6' C21' C22' 119.7(4) . . ?
C21' C22' H22D 109.5 . . ?
C21' C22' H22E 109.5 . . ?
H22D C22' H22E 109.5 . . ?
C21' C22' H22F 109.5 . . ?
H22D C22' H22F 109.5 . . ?
H22E C22' H22F 109.5 . . ?
N7 C23 C24 122.7(2) . . ?
N7 C23 H23A 118.7 . . ?
C24 C23 H23A 118.7 . . ?
C23 C24 C25 118.6(3) . . ?
C23 C24 H24A 120.7 . . ?
C25 C24 H24A 120.7 . . ?
C26 C25 C24 119.5(2) . . ?
C26 C25 H25A 120.3 . . ?
C24 C25 H25A 120.3 . . ?
C25 C26 C27 119.6(2) . . ?
C25 C26 H26A 120.2 . . ?
C27 C26 H26A 120.2 . . ?
N7 C27 C26 120.7(2) . . ?
N7 C27 C28 117.3(2) . . ?
C26 C27 C28 122.0(2) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N8 C29 C30 123.2(2) . . ?
N8 C29 H29A 118.4 . . ?
C30 C29 H29A 118.4 . . ?
C29 C30 C31 117.8(2) . . ?
C29 C30 H30A 121.1 . . ?
C31 C30 H30A 121.1 . . ?
C32 C31 C30 119.9(2) . . ?
C32 C31 H31A 120.1 . . ?
C30 C31 H31A 120.1 . . ?
C31 C32 C33 119.6(2) . . ?
C31 C32 H32A 120.2 . . ?
C33 C32 H32A 120.2 . . ?
N8 C33 C32 121.2(2) . . ?
N8 C33 C34 117.1(2) . . ?
C32 C33 C34 121.6(2) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C35 O13 C38 107.5(10) . . ?
O13 C35 C36 102.8(9) . . ?
O13 C35 H35A 111.2 . . ?
C36 C35 H35A 111.2 . . ?
O13 C35 H35B 111.2 . . ?
C36 C35 H35B 111.2 . . ?
H35A C35 H35B 109.1 . . ?
C37 C36 C35 95.0(6) . . ?
C37 C36 H36A 112.7 . . ?
C35 C36 H36A 112.7 . . ?
C37 C36 H36B 112.7 . . ?
C35 C36 H36B 112.7 . . ?
H36A C36 H36B 110.2 . . ?
C38 C37 C36 103.7(8) . . ?
C38 C37 H37A 111.0 . . ?
C36 C37 H37A 111.0 . . ?
C38 C37 H37B 111.0 . . ?
C36 C37 H37B 111.0 . . ?
H37A C37 H37B 109.0 . . ?
C37 C38 O13 106.2(10) . . ?
C37 C38 H38A 110.5 . . ?
O13 C38 H38A 110.5 . . ?
C37 C38 H38B 110.5 . . ?
O13 C38 H38B 110.5 . . ?
H38A C38 H38B 108.7 . . ?
C38' O13' C35' 110.3(12) . . ?
O13' C35' C36' 101.5(9) . . ?
O13' C35' H35C 111.5 . . ?
C36' C35' H35C 111.5 . . ?
O13' C35' H35D 111.5 . . ?
C36' C35' H35D 111.5 . . ?
H35C C35' H35D 109.3 . . ?
C37' C36' C35' 97.8(7) . . ?
C37' C36' H36C 112.2 . . ?
C35' C36' H36C 112.2 . . ?
C37' C36' H36D 112.2 . . ?
C35' C36' H36D 112.2 . . ?
H36C C36' H36D 109.8 . . ?
C36' C37' C38' 101.6(8) . . ?
C36' C37' H37C 111.5 . . ?
C38' C37' H37C 111.5 . . ?
C36' C37' H37D 111.5 . . ?
C38' C37' H37D 111.5 . . ?
H37C C37' H37D 109.3 . . ?
O13' C38' C37' 104.1(11) . . ?
O13' C38' H38C 110.9 . . ?
C37' C38' H38C 110.9 . . ?
O13' C38' H38D 110.9 . . ?
C37' C38' H38D 110.9 . . ?
H38C C38' H38D 109.0 . . ?
Cu1 O9 H9A 121(2) . . ?
Cu1 O9 H9B 114(2) . . ?
H9A O9 H9B 111(3) . . ?
Cu1 O10 H10A 119(2) . . ?
Cu1 O10 H10B 124(2) . . ?
H10A O10 H10B 111(3) . . ?
Cu3 O11 H11B 118(2) . . ?
Cu3 O11 H11C 120(2) . . ?
H11B O11 H11C 109(3) . . ?
Cu3 O12 H12B 122(2) . . ?
Cu3 O12 H12C 119(2) . . ?
H12B O12 H12C 113(3) . . ?
H14B O14 H14C 104(3) . . ?
H15A O15 H15B 109(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O9 Cu1 O1 C1 10.2(9) . . . . ?
N1 Cu1 O1 C1 -3.26(15) . . . . ?
N5 Cu1 O1 C1 145.65(16) . . . . ?
O10 Cu1 O1 C1 -113.59(16) . . . . ?
N3 Cu2 O3 C5 151.87(14) . . . . ?
N2 Cu2 O3 C5 -7.32(14) . . . . ?
O5 Cu2 O3 C5 74.7(2) . . . . ?
N6 Cu2 O3 C5 -105.33(15) . . . . ?
N6' Cu2 O3 C5 -112.2(2) . . . . ?
N3 Cu2 O5 C6 -5.83(15) . . . . ?
N2 Cu2 O5 C6 153.08(15) . . . . ?
O3 Cu2 O5 C6 73.8(2) . . . . ?
N6 Cu2 O5 C6 -106.23(16) . . . . ?
N6' Cu2 O5 C6 -99.6(2) . . . . ?
O11 Cu3 O7 C10 58.2(9) . . . . ?
N4 Cu3 O7 C10 -5.01(16) . . . . ?
N7 Cu3 O7 C10 145.78(16) . . . . ?
O12 Cu3 O7 C10 -111.65(16) . . . . ?
O9 Cu1 N1 N2 -5.9(2) . . . . ?
O1 Cu1 N1 N2 172.9(2) . . . . ?
N5 Cu1 N1 N2 93.6(2) . . . . ?
O10 Cu1 N1 N2 -97.7(2) . . . . ?
O9 Cu1 N1 C2 -172.27(14) . . . . ?
O1 Cu1 N1 C2 6.54(14) . . . . ?
N5 Cu1 N1 C2 -72.8(2) . . . . ?
O10 Cu1 N1 C2 95.98(14) . . . . ?
C2 N1 N2 C4 -0.2(2) . . . . ?
Cu1 N1 N2 C4 -166.97(16) . . . . ?
C2 N1 N2 Cu2 -170.68(16) . . . . ?
Cu1 N1 N2 Cu2 22.6(3) . . . . ?
N3 Cu2 N2 N1 101.0(3) . . . . ?
O5 Cu2 N2 N1 22.3(2) . . . . ?
O3 Cu2 N2 N1 178.5(2) . . . . ?
N6 Cu2 N2 N1 -83.4(2) . . . . ?
N6' Cu2 N2 N1 -77.1(3) . . . . ?
N3 Cu2 N2 C4 -69.2(2) . . . . ?
O5 Cu2 N2 C4 -147.82(14) . . . . ?
O3 Cu2 N2 C4 8.37(13) . . . . ?
N6 Cu2 N2 C4 106.40(15) . . . . ?
N6' Cu2 N2 C4 112.8(2) . . . . ?
N2 Cu2 N3 N4 100.9(3) . . . . ?
O5 Cu2 N3 N4 -178.2(2) . . . . ?
O3 Cu2 N3 N4 25.4(2) . . . . ?
N6 Cu2 N3 N4 -74.7(2) . . . . ?
N6' Cu2 N3 N4 -81.0(2) . . . . ?
N2 Cu2 N3 C7 -75.3(2) . . . . ?
O5 Cu2 N3 C7 5.69(14) . . . . ?
O3 Cu2 N3 C7 -150.70(14) . . . . ?
N6 Cu2 N3 C7 109.17(15) . . . . ?
N6' Cu2 N3 C7 102.9(2) . . . . ?
C7 N3 N4 C9 -0.2(2) . . . . ?
Cu2 N3 N4 C9 -176.51(16) . . . . ?
C7 N3 N4 Cu3 -167.76(16) . . . . ?
Cu2 N3 N4 Cu3 16.0(3) . . . . ?
O11 Cu3 N4 N3 -3.1(2) . . . . ?
O7 Cu3 N4 N3 172.8(2) . . . . ?
N7 Cu3 N4 N3 92.4(2) . . . . ?
O12 Cu3 N4 N3 -97.2(2) . . . . ?
O11 Cu3 N4 C9 -170.30(14) . . . . ?
O7 Cu3 N4 C9 5.66(14) . . . . ?
N7 Cu3 N4 C9 -74.7(2) . . . . ?
O12 Cu3 N4 C9 95.63(14) . . . . ?
O9 Cu1 N5 C11 -117.04(17) . . . . ?
O1 Cu1 N5 C11 66.54(17) . . . . ?
N1 Cu1 N5 C11 143.32(17) . . . . ?
O10 Cu1 N5 C11 -25.98(18) . . . . ?
O9 Cu1 N5 C15 64.67(19) . . . . ?
O1 Cu1 N5 C15 -111.75(18) . . . . ?
N1 Cu1 N5 C15 -35.0(3) . . . . ?
O10 Cu1 N5 C15 155.73(18) . . . . ?
O11 Cu3 N7 C23 -99.05(18) . . . . ?
O7 Cu3 N7 C23 85.45(18) . . . . ?
N4 Cu3 N7 C23 163.19(16) . . . . ?
O12 Cu3 N7 C23 -7.36(18) . . . . ?
O11 Cu3 N7 C27 73.15(17) . . . . ?
O7 Cu3 N7 C27 -102.35(17) . . . . ?
N4 Cu3 N7 C27 -24.6(3) . . . . ?
O12 Cu3 N7 C27 164.84(16) . . . . ?
Cu1 O1 C1 O2 178.63(18) . . . . ?
Cu1 O1 C1 C2 -0.5(2) . . . . ?
N2 N1 C2 C3 0.2(2) . . . . ?
Cu1 N1 C2 C3 170.80(14) . . . . ?
N2 N1 C2 C1 -179.32(17) . . . . ?
Cu1 N1 C2 C1 -8.7(2) . . . . ?
O2 C1 C2 N1 -172.9(2) . . . . ?
O1 C1 C2 N1 6.3(3) . . . . ?
O2 C1 C2 C3 7.8(4) . . . . ?
O1 C1 C2 C3 -173.1(2) . . . . ?
N1 C2 C3 C4 0.0(2) . . . . ?
C1 C2 C3 C4 179.3(2) . . . . ?
N1 N2 C4 C3 0.3(2) . . . . ?
Cu2 N2 C4 C3 173.47(13) . . . . ?
N1 N2 C4 C5 178.35(16) . . . . ?
Cu2 N2 C4 C5 -8.4(2) . . . . ?
C2 C3 C4 N2 -0.1(2) . . . . ?
C2 C3 C4 C5 -177.8(2) . . . . ?
Cu2 O3 C5 O4 -175.83(16) . . . . ?
Cu2 O3 C5 C4 4.7(2) . . . . ?
N2 C4 C5 O4 -176.93(19) . . . . ?
C3 C4 C5 O4 0.6(4) . . . . ?
N2 C4 C5 O3 2.6(3) . . . . ?
C3 C4 C5 O3 -179.9(2) . . . . ?
Cu2 O5 C6 O6 -175.28(18) . . . . ?
Cu2 O5 C6 C7 4.6(2) . . . . ?
N4 N3 C7 C8 0.1(2) . . . . ?
Cu2 N3 C7 C8 177.37(13) . . . . ?
N4 N3 C7 C6 177.73(16) . . . . ?
Cu2 N3 C7 C6 -5.0(2) . . . . ?
O6 C6 C7 N3 -179.9(2) . . . . ?
O5 C6 C7 N3 0.2(3) . . . . ?
O6 C6 C7 C8 -2.9(4) . . . . ?
O5 C6 C7 C8 177.2(2) . . . . ?
N3 C7 C8 C9 0.1(2) . . . . ?
C6 C7 C8 C9 -176.9(2) . . . . ?
N3 N4 C9 C8 0.3(2) . . . . ?
Cu3 N4 C9 C8 171.63(14) . . . . ?
N3 N4 C9 C10 -176.89(17) . . . . ?
Cu3 N4 C9 C10 -5.6(2) . . . . ?
C7 C8 C9 N4 -0.3(2) . . . . ?
C7 C8 C9 C10 176.3(2) . . . . ?
Cu3 O7 C10 O8 -176.7(2) . . . . ?
Cu3 O7 C10 C9 3.3(2) . . . . ?
N4 C9 C10 O8 -178.4(2) . . . . ?
C8 C9 C10 O8 5.2(4) . . . . ?
N4 C9 C10 O7 1.7(3) . . . . ?
C8 C9 C10 O7 -174.8(2) . . . . ?
C15 N5 C11 C12 0.1(4) . . . . ?
Cu1 N5 C11 C12 -178.3(2) . . . . ?
N5 C11 C12 C13 -1.5(4) . . . . ?
C11 C12 C13 C14 1.0(4) . . . . ?
C12 C13 C14 C15 0.8(4) . . . . ?
C11 N5 C15 C14 1.8(4) . . . . ?
Cu1 N5 C15 C14 -179.87(19) . . . . ?
C11 N5 C15 C16 -176.1(2) . . . . ?
Cu1 N5 C15 C16 2.1(3) . . . . ?
C13 C14 C15 N5 -2.3(4) . . . . ?
C13 C14 C15 C16 175.6(3) . . . . ?
N3 Cu2 N6 C17 129.89(11) . . . . ?
N2 Cu2 N6 C17 -48.48(12) . . . . ?
O5 Cu2 N6 C17 -145.52(11) . . . . ?
O3 Cu2 N6 C17 34.49(12) . . . . ?
N6' Cu2 N6 C17 171.0(13) . . . . ?
N3 Cu2 N6 C21 -48.12(18) . . . . ?
N2 Cu2 N6 C21 133.51(17) . . . . ?
O5 Cu2 N6 C21 36.47(19) . . . . ?
O3 Cu2 N6 C21 -143.52(17) . . . . ?
N6' Cu2 N6 C21 -7.0(11) . . . . ?
C21 N6 C17 C18 0.0 . . . . ?
Cu2 N6 C17 C18 -178.19(19) . . . . ?
N6 C17 C18 C19 0.0 . . . . ?
C17 C18 C19 C20 0.0 . . . . ?
C18 C19 C20 C21 0.0 . . . . ?
C19 C20 C21 N6 0.0 . . . . ?
C19 C20 C21 C22 178.9(3) . . . . ?
C17 N6 C21 C20 0.0 . . . . ?
Cu2 N6 C21 C20 177.9(2) . . . . ?
C17 N6 C21 C22 -179.0(3) . . . . ?
Cu2 N6 C21 C22 -1.1(3) . . . . ?
N3 Cu2 N6' C17' -46.2(2) . . . . ?
N2 Cu2 N6' C17' 133.1(2) . . . . ?
O5 Cu2 N6' C17' 36.1(2) . . . . ?
O3 Cu2 N6' C17' -141.1(2) . . . . ?
N6 Cu2 N6' C17' 174.0(14) . . . . ?
N3 Cu2 N6' C21' 133.5(4) . . . . ?
N2 Cu2 N6' C21' -47.2(4) . . . . ?
O5 Cu2 N6' C21' -144.1(4) . . . . ?
O3 Cu2 N6' C21' 38.7(4) . . . . ?
N6 Cu2 N6' C21' -6.3(10) . . . . ?
C21' N6' C17' C18' 0.0 . . . . ?
Cu2 N6' C17' C18' 179.7(4) . . . . ?
N6' C17' C18' C19' 0.0 . . . . ?
C17' C18' C19' C20' 0.0 . . . . ?
C18' C19' C20' C21' 0.0 . . . . ?
C19' C20' C21' N6' 0.0 . . . . ?
C19' C20' C21' C22' -178.8(6) . . . . ?
C17' N6' C21' C20' 0.0 . . . . ?
Cu2 N6' C21' C20' -179.7(5) . . . . ?
C17' N6' C21' C22' 178.8(6) . . . . ?
Cu2 N6' C21' C22' -0.9(7) . . . . ?
C27 N7 C23 C24 0.9(4) . . . . ?
Cu3 N7 C23 C24 173.3(2) . . . . ?
N7 C23 C24 C25 0.0(4) . . . . ?
C23 C24 C25 C26 0.1(4) . . . . ?
C24 C25 C26 C27 -1.2(4) . . . . ?
C23 N7 C27 C26 -2.0(3) . . . . ?
Cu3 N7 C27 C26 -174.25(19) . . . . ?
C23 N7 C27 C28 177.1(2) . . . . ?
Cu3 N7 C27 C28 4.8(3) . . . . ?
C25 C26 C27 N7 2.1(4) . . . . ?
C25 C26 C27 C28 -176.9(3) . . . . ?
C33 N8 C29 C30 0.2(4) . . . . ?
N8 C29 C30 C31 0.7(4) . . . . ?
C29 C30 C31 C32 -0.7(4) . . . . ?
C30 C31 C32 C33 -0.2(4) . . . . ?
C29 N8 C33 C32 -1.2(3) . . . . ?
C29 N8 C33 C34 178.6(2) . . . . ?
C31 C32 C33 N8 1.2(4) . . . . ?
C31 C32 C33 C34 -178.5(3) . . . . ?
C38 O13 C35 C36 33.0(12) . . . . ?
O13 C35 C36 C37 -47.3(10) . . . . ?
C35 C36 C37 C38 43.8(9) . . . . ?
C36 C37 C38 O13 -27.6(11) . . . . ?
C35 O13 C38 C37 -4.6(13) . . . . ?
C38' O13' C35' C36' -18.1(13) . . . . ?
O13' C35' C36' C37' 41.3(10) . . . . ?
C35' C36' C37' C38' -48.0(10) . . . . ?
C35' O13' C38' C37' -11.5(14) . . . . ?
C36' C37' C38' O13' 39.4(12) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        69.99
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.454
_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_full_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1865963'
loop_
_audit_author_name
_audit_author_address

'Shiqun Xiang, Xiaofeng Zhang,Hui Chen, Yinghua Li, Weibin Fan and Deguang Huang'
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2018-09-05 deposited with the CCDC.	2019-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Cu(ligand)(Py)]2'
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H22 Cu N8 O4'
_chemical_formula_sum            'C28 H22 Cu N8 O4'
_chemical_formula_weight         598.08

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
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                   14.1353(7)
_cell_length_b                   10.5943(5)
_cell_length_c                   17.9376(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.500(5)
_cell_angle_gamma                90.00
_cell_volume                     2575.6(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2352
_cell_measurement_theta_min      3.9660
_cell_measurement_theta_max      28.8280

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1228
_exptl_absorpt_coefficient_mu    0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8546
_exptl_absorpt_correction_T_max  0.9314
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies,Version 1.171.36.28 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  Mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5398
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.69
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2518
_reflns_number_gt                2024
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0306P)²+2.3493P] 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         2518
_refine_ls_number_parameters     187
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.0844
_refine_ls_wR_factor_gt          0.0778
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_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 0.2500 0.2500 0.5000 0.01477(14) Uani 1 2 d S . .
O1 O 0.24825(11) 0.43052(16) 0.47735(9) 0.0177(4) Uani 1 1 d . . .
O2 O 0.21611(12) 0.58734(16) 0.39167(10) 0.0224(4) Uani 1 1 d . . .
N1 N 0.18289(13) 0.25794(19) 0.35734(11) 0.0157(4) Uani 1 1 d . . .
N2 N 0.14182(14) 0.2045(2) 0.28663(11) 0.0174(5) Uani 1 1 d . . .
N3 N 0.09501(14) 0.0351(2) 0.20299(11) 0.0210(5) Uani 1 1 d . . .
N4 N 0.38991(13) 0.23971(19) 0.49122(10) 0.0147(4) Uani 1 1 d . . .
C1 C 0.21682(15) 0.4737(2) 0.40903(14) 0.0173(5) Uani 1 1 d . . .
C2 C 0.17730(16) 0.3820(2) 0.34385(13) 0.0179(5) Uani 1 1 d . . .
C3 C 0.13269(19) 0.4088(3) 0.26492(14) 0.0266(6) Uani 1 1 d . . .
H3A H 0.1202 0.4894 0.2410 0.032 Uiso 1 1 calc R . .
C4 C 0.1113(2) 0.2936(3) 0.23023(15) 0.0284(7) Uani 1 1 d . . .
H4A H 0.0808 0.2783 0.1766 0.034 Uiso 1 1 calc R . .
C5 C 0.13712(16) 0.0711(2) 0.27592(13) 0.0182(5) Uani 1 1 d . . .
C6 C 0.17420(16) -0.0100(2) 0.33819(13) 0.0180(5) Uani 1 1 d . . .
H6A H 0.2017 0.0209 0.3895 0.022 Uiso 1 1 calc R . .
C7 C 0.16927(19) -0.1378(3) 0.32220(15) 0.0255(6) Uani 1 1 d . . .
H7A H 0.1947 -0.1971 0.3627 0.031 Uiso 1 1 calc R . .
C8 C 0.1269(2) -0.1788(3) 0.24658(16) 0.0292(7) Uani 1 1 d . . .
H8A H 0.1230 -0.2662 0.2342 0.035 Uiso 1 1 calc R . .
C9 C 0.09081(19) -0.0894(3) 0.18993(15) 0.0277(6) Uani 1 1 d . . .
H9A H 0.0611 -0.1179 0.1384 0.033 Uiso 1 1 calc R . .
C10 C 0.45924(17) 0.3229(3) 0.52900(14) 0.0209(6) Uani 1 1 d . . .
H10A H 0.4411 0.3884 0.5584 0.025 Uiso 1 1 calc R . .
C11 C 0.55590(17) 0.3158(3) 0.52628(14) 0.0241(6) Uani 1 1 d . . .
H11A H 0.6033 0.3753 0.5538 0.029 Uiso 1 1 calc R . .
C12 C 0.58290(17) 0.2220(3) 0.48363(14) 0.0235(6) Uani 1 1 d . . .
H12A H 0.6492 0.2154 0.4816 0.028 Uiso 1 1 calc R . .
C13 C 0.51190(18) 0.1372(3) 0.44351(15) 0.0251(6) Uani 1 1 d . . .
H13A H 0.5281 0.0725 0.4125 0.030 Uiso 1 1 calc R . .
C14 C 0.41704(17) 0.1488(2) 0.44960(15) 0.0215(6) Uani 1 1 d . . .
H14A H 0.3688 0.0896 0.4230 0.026 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 1.9539(17) 7_556 ?
Cu1 O1 1.9539(17) . ?
Cu1 N4 2.0309(18) . ?
Cu1 N4 2.0309(18) 7_556 ?
Cu1 N1 2.4651(18) . ?
Cu1 N1 2.4651(18) 7_556 ?
O1 C1 1.265(3) . ?
O2 C1 1.243(3) . ?
N1 C2 1.334(3) . ?
N1 N2 1.359(3) . ?
N2 C4 1.361(3) . ?
N2 C5 1.425(3) . ?
N3 C5 1.330(3) . ?
N3 C9 1.339(3) . ?
N4 C14 1.339(3) . ?
N4 C10 1.349(3) . ?
C1 C2 1.501(3) . ?
C2 C3 1.406(3) . ?
C3 C4 1.364(4) . ?
C3 H3A 0.9500 . ?
C4 H4A 0.9500 . ?
C5 C6 1.389(3) . ?
C6 C7 1.381(4) . ?
C6 H6A 0.9500 . ?
C7 C8 1.388(4) . ?
C7 H7A 0.9500 . ?
C8 C9 1.377(4) . ?
C8 H8A 0.9500 . ?
C9 H9A 0.9500 . ?
C10 C11 1.383(3) . ?
C10 H10A 0.9500 . ?
C11 C12 1.372(4) . ?
C11 H11A 0.9500 . ?
C12 C13 1.387(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.381(3) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O1 180.0 7_556 . ?
O1 Cu1 N4 90.48(7) 7_556 . ?
O1 Cu1 N4 89.52(7) . . ?
O1 Cu1 N4 89.52(7) 7_556 7_556 ?
O1 Cu1 N4 90.48(7) . 7_556 ?
N4 Cu1 N4 180.000(1) . 7_556 ?
O1 Cu1 N1 103.16(7) 7_556 . ?
O1 Cu1 N1 76.84(7) . . ?
N4 Cu1 N1 91.00(7) . . ?
N4 Cu1 N1 89.00(7) 7_556 . ?
O1 Cu1 N1 76.84(7) 7_556 7_556 ?
O1 Cu1 N1 103.16(7) . 7_556 ?
N4 Cu1 N1 89.00(7) . 7_556 ?
N4 Cu1 N1 91.00(7) 7_556 7_556 ?
N1 Cu1 N1 180.0 . 7_556 ?
C1 O1 Cu1 122.39(15) . . ?
C2 N1 N2 104.68(19) . . ?
C2 N1 Cu1 101.97(14) . . ?
N2 N1 Cu1 152.96(16) . . ?
N1 N2 C4 111.4(2) . . ?
N1 N2 C5 122.01(19) . . ?
C4 N2 C5 126.5(2) . . ?
C5 N3 C9 116.1(2) . . ?
C14 N4 C10 117.9(2) . . ?
C14 N4 Cu1 121.41(16) . . ?
C10 N4 Cu1 120.70(17) . . ?
O2 C1 O1 124.7(2) . . ?
O2 C1 C2 117.2(2) . . ?
O1 C1 C2 118.1(2) . . ?
N1 C2 C3 111.6(2) . . ?
N1 C2 C1 120.4(2) . . ?
C3 C2 C1 128.0(2) . . ?
C4 C3 C2 104.9(2) . . ?
C4 C3 H3A 127.6 . . ?
C2 C3 H3A 127.6 . . ?
N2 C4 C3 107.4(2) . . ?
N2 C4 H4A 126.3 . . ?
C3 C4 H4A 126.3 . . ?
N3 C5 C6 125.1(2) . . ?
N3 C5 N2 114.0(2) . . ?
C6 C5 N2 120.9(2) . . ?
C7 C6 C5 117.0(2) . . ?
C7 C6 H6A 121.5 . . ?
C5 C6 H6A 121.5 . . ?
C6 C7 C8 119.5(2) . . ?
C6 C7 H7A 120.3 . . ?
C8 C7 H7A 120.3 . . ?
C9 C8 C7 118.2(3) . . ?
C9 C8 H8A 120.9 . . ?
C7 C8 H8A 120.9 . . ?
N3 C9 C8 124.1(2) . . ?
N3 C9 H9A 118.0 . . ?
C8 C9 H9A 118.0 . . ?
N4 C10 C11 122.1(2) . . ?
N4 C10 H10A 119.0 . . ?
C11 C10 H10A 119.0 . . ?
C12 C11 C10 119.6(2) . . ?
C12 C11 H11A 120.2 . . ?
C10 C11 H11A 120.2 . . ?
C11 C12 C13 118.9(2) . . ?
C11 C12 H12A 120.5 . . ?
C13 C12 H12A 120.5 . . ?
C14 C13 C12 118.5(3) . . ?
C14 C13 H13A 120.8 . . ?
C12 C13 H13A 120.8 . . ?
N4 C14 C13 123.1(2) . . ?
N4 C14 H14A 118.4 . . ?
C13 C14 H14A 118.4 . . ?

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
O1 Cu1 O1 C1 -126(19) 7_556 . . . ?
N4 Cu1 O1 C1 92.07(17) . . . . ?
N4 Cu1 O1 C1 -87.93(17) 7_556 . . . ?
N1 Cu1 O1 C1 0.94(16) . . . . ?
N1 Cu1 O1 C1 -179.06(16) 7_556 . . . ?
O1 Cu1 N1 C2 176.69(14) 7_556 . . . ?
O1 Cu1 N1 C2 -3.31(14) . . . . ?
N4 Cu1 N1 C2 -92.58(15) . . . . ?
N4 Cu1 N1 C2 87.42(15) 7_556 . . . ?
N1 Cu1 N1 C2 57(29) 7_556 . . . ?
O1 Cu1 N1 N2 6.5(3) 7_556 . . . ?
O1 Cu1 N1 N2 -173.5(3) . . . . ?
N4 Cu1 N1 N2 97.2(3) . . . . ?
N4 Cu1 N1 N2 -82.8(3) 7_556 . . . ?
N1 Cu1 N1 N2 -113(28) 7_556 . . . ?
C2 N1 N2 C4 0.1(3) . . . . ?
Cu1 N1 N2 C4 170.1(3) . . . . ?
C2 N1 N2 C5 177.6(2) . . . . ?
Cu1 N1 N2 C5 -12.3(4) . . . . ?
O1 Cu1 N4 C14 47.12(18) 7_556 . . . ?
O1 Cu1 N4 C14 -132.88(18) . . . . ?
N4 Cu1 N4 C14 145(100) 7_556 . . . ?
N1 Cu1 N4 C14 -56.05(18) . . . . ?
N1 Cu1 N4 C14 123.95(18) 7_556 . . . ?
O1 Cu1 N4 C10 -131.20(18) 7_556 . . . ?
O1 Cu1 N4 C10 48.80(18) . . . . ?
N4 Cu1 N4 C10 -34(100) 7_556 . . . ?
N1 Cu1 N4 C10 125.63(18) . . . . ?
N1 Cu1 N4 C10 -54.37(18) 7_556 . . . ?
Cu1 O1 C1 O2 -178.49(17) . . . . ?
Cu1 O1 C1 C2 1.6(3) . . . . ?
N2 N1 C2 C3 0.1(3) . . . . ?
Cu1 N1 C2 C3 -175.30(17) . . . . ?
N2 N1 C2 C1 -179.42(18) . . . . ?
Cu1 N1 C2 C1 5.2(2) . . . . ?
O2 C1 C2 N1 174.7(2) . . . . ?
O1 C1 C2 N1 -5.4(3) . . . . ?
O2 C1 C2 C3 -4.7(4) . . . . ?
O1 C1 C2 C3 175.2(2) . . . . ?
N1 C2 C3 C4 -0.2(3) . . . . ?
C1 C2 C3 C4 179.3(2) . . . . ?
N1 N2 C4 C3 -0.2(3) . . . . ?
C5 N2 C4 C3 -177.6(2) . . . . ?
C2 C3 C4 N2 0.3(3) . . . . ?
C9 N3 C5 C6 -1.4(3) . . . . ?
C9 N3 C5 N2 178.7(2) . . . . ?
N1 N2 C5 N3 -179.68(19) . . . . ?
C4 N2 C5 N3 -2.5(3) . . . . ?
N1 N2 C5 C6 0.4(3) . . . . ?
C4 N2 C5 C6 177.6(2) . . . . ?
N3 C5 C6 C7 2.0(4) . . . . ?
N2 C5 C6 C7 -178.1(2) . . . . ?
C5 C6 C7 C8 -1.1(4) . . . . ?
C6 C7 C8 C9 -0.2(4) . . . . ?
C5 N3 C9 C8 -0.1(4) . . . . ?
C7 C8 C9 N3 0.8(4) . . . . ?
C14 N4 C10 C11 -0.6(3) . . . . ?
Cu1 N4 C10 C11 177.78(18) . . . . ?
N4 C10 C11 C12 0.4(4) . . . . ?
C10 C11 C12 C13 0.6(4) . . . . ?
C11 C12 C13 C14 -1.5(4) . . . . ?
C10 N4 C14 C13 -0.3(4) . . . . ?
Cu1 N4 C14 C13 -178.66(18) . . . . ?
C12 C13 C14 N4 1.3(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.070
####################################################################### 
# 
# 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_full_CCDC5
_database_code_depnum_ccdc_archive 'CCDC 1872941'
loop_
_audit_author_name
_audit_author_address

'Shiqun Xiang, Xiaofeng Zhang,Hui Chen, Yinghua Li, Weibin Fan and Deguang Huang'
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2018-10-12 deposited with the CCDC.	2019-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            3-Me-Py-Pz-COOH
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H9 N3 O2'
_chemical_formula_sum            'C10 H9 N3 O2'
_chemical_formula_weight         203.20

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   5.7124(7)
_cell_length_b                   7.3887(5)
_cell_length_c                   11.5280(10)
_cell_angle_alpha                92.199(6)
_cell_angle_beta                 98.583(9)
_cell_angle_gamma                99.681(8)
_cell_volume                     473.26(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1335
_cell_measurement_theta_min      6.1010
_cell_measurement_theta_max      75.3020

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             212
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9345
_exptl_absorpt_correction_T_max  0.9665
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  Mirror
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3384
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.89
_diffrn_reflns_theta_max         69.99
_reflns_number_total             1779
_reflns_number_gt                1465
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0458P)²+0.5088P] 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         1779
_refine_ls_number_parameters     140
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1322
_refine_ls_wR_factor_gt          0.1280
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.063
_refine_ls_shift/su_mean         0.003

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
C1 C 0.4236(4) 0.4037(3) 0.64316(19) 0.0228(5) Uani 1 1 d . . .
C2 C 0.3551(4) 0.3296(3) 0.75147(19) 0.0228(5) Uani 1 1 d . . .
C3 C 0.1196(4) 0.2547(3) 0.7680(2) 0.0249(5) Uani 1 1 d . . .
H3A H -0.0242 0.2432 0.7129 0.030 Uiso 1 1 calc R . .
C4 C 0.1440(4) 0.2024(3) 0.8808(2) 0.0247(5) Uani 1 1 d . . .
H4A H 0.0192 0.1451 0.9202 0.030 Uiso 1 1 calc R . .
C5 C 0.4918(4) 0.2254(3) 1.04287(19) 0.0214(5) Uani 1 1 d . . .
C6 C 0.7335(4) 0.2945(3) 1.0816(2) 0.0244(5) Uani 1 1 d . . .
H6A H 0.8321 0.3581 1.0314 0.029 Uiso 1 1 calc R . .
C7 C 0.8251(4) 0.2669(3) 1.1965(2) 0.0269(5) Uani 1 1 d . . .
H7A H 0.9897 0.3120 1.2263 0.032 Uiso 1 1 calc R . .
C8 C 0.6767(4) 0.1731(3) 1.2686(2) 0.0269(5) Uani 1 1 d . . .
C9 C 0.4388(4) 0.1122(3) 1.2186(2) 0.0280(5) Uani 1 1 d . . .
H9A H 0.3348 0.0492 1.2668 0.034 Uiso 1 1 calc R . .
C10 C 0.7675(5) 0.1383(4) 1.3936(2) 0.0359(6) Uani 1 1 d . . .
H10A H 0.6355 0.0707 1.4286 0.054 Uiso 1 1 calc R . .
H10B H 0.8301 0.2560 1.4387 0.054 Uiso 1 1 calc R . .
H10C H 0.8962 0.0654 1.3949 0.054 Uiso 1 1 calc R . .
O1 O 0.6528(3) 0.4631(2) 0.64410(15) 0.0298(4) Uani 1 1 d . . .
O2 O 0.2672(3) 0.4061(2) 0.55681(14) 0.0307(4) Uani 1 1 d . . .
N1 N 0.5168(3) 0.3272(2) 0.84807(16) 0.0228(4) Uani 1 1 d . . .
N2 N 0.3831(3) 0.2484(2) 0.92610(16) 0.0219(4) Uani 1 1 d . . .
N3 N 0.3437(3) 0.1351(3) 1.10782(17) 0.0268(4) Uani 1 1 d . . .
H1 H 0.675(6) 0.510(5) 0.564(3) 0.072(11) Uiso 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
C1 O2 1.237(3) . ?
C1 O1 1.307(3) . ?
C1 C2 1.462(3) . ?
C2 N1 1.339(3) . ?
C2 C3 1.409(3) . ?
C3 C4 1.364(3) . ?
C4 N2 1.368(3) . ?
C5 N3 1.326(3) . ?
C5 C6 1.389(3) . ?
C5 N2 1.425(3) . ?
C6 C7 1.385(3) . ?
C7 C8 1.396(3) . ?
C8 C9 1.387(3) . ?
C8 C10 1.504(3) . ?
C9 N3 1.340(3) . ?
N1 N2 1.352(3) . ?

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 C1 O1 123.7(2) . . ?
O2 C1 C2 119.7(2) . . ?
O1 C1 C2 116.54(19) . . ?
N1 C2 C3 112.3(2) . . ?
N1 C2 C1 122.06(19) . . ?
C3 C2 C1 125.6(2) . . ?
C4 C3 C2 104.70(19) . . ?
C3 C4 N2 106.6(2) . . ?
N3 C5 C6 124.7(2) . . ?
N3 C5 N2 114.43(19) . . ?
C6 C5 N2 120.9(2) . . ?
C7 C6 C5 117.3(2) . . ?
C6 C7 C8 120.3(2) . . ?
C9 C8 C7 116.3(2) . . ?
C9 C8 C10 121.3(2) . . ?
C7 C8 C10 122.4(2) . . ?
N3 C9 C8 125.2(2) . . ?
C2 N1 N2 103.51(17) . . ?
N1 N2 C4 112.86(18) . . ?
N1 N2 C5 120.59(17) . . ?
C4 N2 C5 126.52(19) . . ?
C5 N3 C9 116.22(19) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        69.99
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.057
