# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1400663'
_audit_update_record             
;
2015-06-29 deposited with the CCDC.
2015-07-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H15 N O9 Zn, H2 O'
_chemical_formula_sum            'C15 H17 N O10 Zn'
_chemical_formula_weight         436.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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                   14.2707(5)
_cell_length_b                   11.9131(4)
_cell_length_c                   18.9905(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3228.54(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1792
_exptl_absorpt_coefficient_mu    1.583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6930
_exptl_absorpt_correction_T_max  0.7122
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6912
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.85
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2837
_reflns_number_gt                2066
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0316P)²+2.1993P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2837
_refine_ls_number_parameters     250
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.0869
_refine_ls_wR_factor_gt          0.0789
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.999
_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
Zn1 Zn 0.41862(3) -0.10837(4) 0.23975(2) 0.03179(15) Uani 1 1 d . . .
O4 O 0.35179(17) 0.1701(2) 0.64773(12) 0.0367(7) Uani 1 1 d . . .
O3 O 0.27596(17) 0.0409(2) 0.58503(12) 0.0346(6) Uani 1 1 d . . .
C8 C 0.3412(2) 0.1098(3) 0.59381(17) 0.0227(8) Uani 1 1 d . . .
C1 C 0.4447(3) 0.0278(3) 0.34347(18) 0.0279(9) Uani 1 1 d . . .
O2 O 0.50100(19) 0.0459(3) 0.29463(13) 0.0473(8) Uani 1 1 d . . .
C5 C 0.4841(2) 0.1991(3) 0.53937(16) 0.0202(8) Uani 1 1 d . . .
H5 H 0.4933 0.2370 0.5816 0.024 Uiso 1 1 calc R . .
C3 C 0.5317(2) 0.1601(3) 0.42087(16) 0.0221(8) Uani 1 1 d . . .
H3 H 0.5729 0.1714 0.3836 0.026 Uiso 1 1 calc R . .
N1 N 0.70733(18) 0.2391(2) 0.52747(14) 0.0214(6) Uani 1 1 d . . .
C2 C 0.4574(2) 0.0870(3) 0.41289(16) 0.0196(8) Uani 1 1 d . . .
C4 C 0.5458(2) 0.2169(3) 0.48389(16) 0.0191(7) Uani 1 1 d . . .
C6 C 0.4090(2) 0.1258(3) 0.53287(16) 0.0189(7) Uani 1 1 d . . .
O1 O 0.3785(2) -0.0412(2) 0.33629(12) 0.0508(8) Uani 1 1 d . . .
C7 C 0.3956(2) 0.0695(3) 0.46922(16) 0.0202(8) Uani 1 1 d . . .
H7 H 0.3456 0.0202 0.4642 0.024 Uiso 1 1 calc R . .
C9 C 0.6267(2) 0.2967(3) 0.49347(18) 0.0244(8) Uani 1 1 d . . .
H9A H 0.6459 0.3257 0.4480 0.029 Uiso 1 1 calc R . .
H9B H 0.6071 0.3595 0.5224 0.029 Uiso 1 1 calc R . .
C14 C 0.7251(2) 0.2551(3) 0.59651(17) 0.0297(9) Uani 1 1 d . . .
H14 H 0.6861 0.3009 0.6232 0.036 Uiso 1 1 calc R . .
C11 C 0.8353(2) 0.1148(3) 0.51858(18) 0.0255(8) Uani 1 1 d . . .
H11 H 0.8711 0.0660 0.4915 0.031 Uiso 1 1 calc R . .
C10 C 0.7604(2) 0.1693(3) 0.48927(17) 0.0245(8) Uani 1 1 d . . .
H10 H 0.7463 0.1578 0.4420 0.029 Uiso 1 1 calc R . .
C13 C 0.8004(3) 0.2039(3) 0.62716(18) 0.0317(9) Uani 1 1 d . . .
H13 H 0.8137 0.2171 0.6744 0.038 Uiso 1 1 calc R . .
C12 C 0.8575(2) 0.1324(3) 0.58837(17) 0.0235(8) Uani 1 1 d . . .
O5 O 0.98111(19) -0.0005(2) 0.59171(14) 0.0456(7) Uani 1 1 d . . .
C15 C 0.9440(2) 0.0801(3) 0.62147(19) 0.0277(9) Uani 1 1 d . . .
O6 O 0.97057(18) 0.1281(2) 0.67691(12) 0.0367(7) Uani 1 1 d . . .
O1W O 0.48130(17) -0.2503(2) 0.29221(12) 0.0377(7) Uani 1 1 d . . .
H1WA H 0.5014 -0.2985 0.2608 0.057 Uiso 1 1 d R . .
H1WB H 0.5424 -0.2334 0.3087 0.057 Uiso 1 1 d R . .
O2W O 0.31094(17) -0.2133(2) 0.21233(14) 0.0416(7) Uani 1 1 d . . .
H2WA H 0.3279 -0.2808 0.2196 0.062 Uiso 1 1 d R . .
H2WB H 0.2984 -0.2046 0.1689 0.062 Uiso 1 1 d R . .
O3W O 0.35977(19) 0.0166(2) 0.17407(13) 0.0415(7) Uani 1 1 d . . .
H3WB H 0.3098 -0.0096 0.1546 0.062 Uiso 1 1 d R . .
H3WA H 0.4147 0.0337 0.1445 0.062 Uiso 1 1 d R . .
O4W O 0.3120(2) 0.5744(3) 0.26719(18) 0.0566(9) Uani 1 1 d G . .
H4WA H 0.2590 0.5445 0.2593 0.085 Uiso 1 1 d G . .
H4WB H 0.3541 0.5393 0.2444 0.085 Uiso 1 1 d G . .


_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
Zn1 O6 1.995(2) 2_654 ?
Zn1 O2W 2.049(3) . ?
Zn1 O1 2.081(3) . ?
Zn1 O3W 2.116(3) . ?
Zn1 O1W 2.157(3) . ?
Zn1 O2 2.418(3) . ?
Zn1 C1 2.578(3) . ?
O4 C8 1.260(4) . ?
O3 C8 1.252(4) . ?
C8 C6 1.521(4) . ?
C1 O2 1.246(4) . ?
C1 O1 1.259(4) . ?
C1 C2 1.506(5) . ?
C5 C6 1.388(4) . ?
C5 C4 1.389(4) . ?
C3 C2 1.381(4) . ?
C3 C4 1.389(4) . ?
N1 C10 1.338(4) . ?
N1 C14 1.349(4) . ?
N1 C9 1.487(4) . ?
C2 C7 1.401(4) . ?
C4 C9 1.507(4) . ?
C6 C7 1.395(4) . ?
C14 C13 1.366(5) . ?
C11 C10 1.369(4) . ?
C11 C12 1.379(4) . ?
C13 C12 1.390(5) . ?
C12 C15 1.519(5) . ?
O5 C15 1.234(4) . ?
C15 O6 1.257(4) . ?
O6 Zn1 1.995(2) 2_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Zn1 O2W 111.75(11) 2_654 . ?
O6 Zn1 O1 142.24(11) 2_654 . ?
O2W Zn1 O1 104.61(11) . . ?
O6 Zn1 O3W 92.58(11) 2_654 . ?
O2W Zn1 O3W 88.97(11) . . ?
O1 Zn1 O3W 98.02(11) . . ?
O6 Zn1 O1W 81.67(10) 2_654 . ?
O2W Zn1 O1W 87.13(11) . . ?
O1 Zn1 O1W 90.49(10) . . ?
O3W Zn1 O1W 171.30(10) . . ?
O6 Zn1 O2 87.83(10) 2_654 . ?
O2W Zn1 O2 159.77(10) . . ?
O1 Zn1 O2 57.43(10) . . ?
O3W Zn1 O2 84.96(10) . . ?
O1W Zn1 O2 101.26(10) . . ?
O6 Zn1 C1 114.64(12) 2_654 . ?
O2W Zn1 C1 133.33(12) . . ?
O1 Zn1 C1 28.91(11) . . ?
O3W Zn1 C1 93.72(10) . . ?
O1W Zn1 C1 94.62(10) . . ?
O2 Zn1 C1 28.66(10) . . ?
O3 C8 O4 124.8(3) . . ?
O3 C8 C6 117.0(3) . . ?
O4 C8 C6 118.1(3) . . ?
O2 C1 O1 121.1(3) . . ?
O2 C1 C2 119.5(3) . . ?
O1 C1 C2 119.4(3) . . ?
O2 C1 Zn1 68.5(2) . . ?
O1 C1 Zn1 53.04(17) . . ?
C2 C1 Zn1 168.7(3) . . ?
C1 O2 Zn1 82.8(2) . . ?
C6 C5 C4 121.2(3) . . ?
C2 C3 C4 120.8(3) . . ?
C10 N1 C14 120.5(3) . . ?
C10 N1 C9 119.3(3) . . ?
C14 N1 C9 120.2(3) . . ?
C3 C2 C7 119.5(3) . . ?
C3 C2 C1 119.0(3) . . ?
C7 C2 C1 121.5(3) . . ?
C5 C4 C3 119.2(3) . . ?
C5 C4 C9 119.4(3) . . ?
C3 C4 C9 121.4(3) . . ?
C5 C6 C7 119.0(3) . . ?
C5 C6 C8 120.2(3) . . ?
C7 C6 C8 120.8(3) . . ?
C1 O1 Zn1 98.0(2) . . ?
C6 C7 C2 120.3(3) . . ?
N1 C9 C4 110.8(3) . . ?
N1 C14 C13 120.0(3) . . ?
C10 C11 C12 119.9(3) . . ?
N1 C10 C11 121.1(3) . . ?
C14 C13 C12 120.6(3) . . ?
C11 C12 C13 117.9(3) . . ?
C11 C12 C15 121.5(3) . . ?
C13 C12 C15 120.6(3) . . ?
O5 C15 O6 127.5(4) . . ?
O5 C15 C12 118.6(3) . . ?
O6 C15 C12 113.9(3) . . ?
C15 O6 Zn1 133.3(2) . 2_655 ?

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
O6 Zn1 C1 O2 22.2(2) 2_654 . . . ?
O2W Zn1 C1 O2 -164.5(2) . . . . ?
O1 Zn1 C1 O2 -172.3(4) . . . . ?
O3W Zn1 C1 O2 -72.4(2) . . . . ?
O1W Zn1 C1 O2 105.1(2) . . . . ?
O6 Zn1 C1 O1 -165.6(2) 2_654 . . . ?
O2W Zn1 C1 O1 7.8(3) . . . . ?
O3W Zn1 C1 O1 99.9(2) . . . . ?
O1W Zn1 C1 O1 -82.6(2) . . . . ?
O2 Zn1 C1 O1 172.3(4) . . . . ?
O6 Zn1 C1 C2 -114.6(13) 2_654 . . . ?
O2W Zn1 C1 C2 58.7(14) . . . . ?
O1 Zn1 C1 C2 50.9(13) . . . . ?
O3W Zn1 C1 C2 150.8(13) . . . . ?
O1W Zn1 C1 C2 -31.7(13) . . . . ?
O2 Zn1 C1 C2 -136.8(14) . . . . ?
O1 C1 O2 Zn1 -7.2(3) . . . . ?
C2 C1 O2 Zn1 171.1(3) . . . . ?
O6 Zn1 O2 C1 -159.9(2) 2_654 . . . ?
O2W Zn1 O2 C1 34.2(4) . . . . ?
O1 Zn1 O2 C1 4.4(2) . . . . ?
O3W Zn1 O2 C1 107.3(2) . . . . ?
O1W Zn1 O2 C1 -78.9(2) . . . . ?
C4 C3 C2 C7 -0.3(5) . . . . ?
C4 C3 C2 C1 179.7(3) . . . . ?
O2 C1 C2 C3 -0.2(5) . . . . ?
O1 C1 C2 C3 178.2(3) . . . . ?
Zn1 C1 C2 C3 132.8(12) . . . . ?
O2 C1 C2 C7 179.8(3) . . . . ?
O1 C1 C2 C7 -1.8(5) . . . . ?
Zn1 C1 C2 C7 -47.2(15) . . . . ?
C6 C5 C4 C3 0.0(5) . . . . ?
C6 C5 C4 C9 -179.6(3) . . . . ?
C2 C3 C4 C5 0.2(5) . . . . ?
C2 C3 C4 C9 179.8(3) . . . . ?
C4 C5 C6 C7 -0.1(5) . . . . ?
C4 C5 C6 C8 -178.6(3) . . . . ?
O3 C8 C6 C5 -178.7(3) . . . . ?
O4 C8 C6 C5 4.6(5) . . . . ?
O3 C8 C6 C7 2.9(5) . . . . ?
O4 C8 C6 C7 -173.8(3) . . . . ?
O2 C1 O1 Zn1 8.4(4) . . . . ?
C2 C1 O1 Zn1 -169.9(3) . . . . ?
O6 Zn1 O1 C1 21.7(3) 2_654 . . . ?
O2W Zn1 O1 C1 -174.1(2) . . . . ?
O3W Zn1 O1 C1 -83.1(2) . . . . ?
O1W Zn1 O1 C1 98.7(2) . . . . ?
O2 Zn1 O1 C1 -4.4(2) . . . . ?
C5 C6 C7 C2 0.0(5) . . . . ?
C8 C6 C7 C2 178.5(3) . . . . ?
C3 C2 C7 C6 0.2(5) . . . . ?
C1 C2 C7 C6 -179.8(3) . . . . ?
C10 N1 C9 C4 76.1(3) . . . . ?
C14 N1 C9 C4 -102.3(3) . . . . ?
C5 C4 C9 N1 84.1(4) . . . . ?
C3 C4 C9 N1 -95.5(4) . . . . ?
C10 N1 C14 C13 3.0(5) . . . . ?
C9 N1 C14 C13 -178.6(3) . . . . ?
C14 N1 C10 C11 -1.7(5) . . . . ?
C9 N1 C10 C11 179.9(3) . . . . ?
C12 C11 C10 N1 -0.7(5) . . . . ?
N1 C14 C13 C12 -2.1(5) . . . . ?
C10 C11 C12 C13 1.6(5) . . . . ?
C10 C11 C12 C15 -175.5(3) . . . . ?
C14 C13 C12 C11 -0.2(5) . . . . ?
C14 C13 C12 C15 176.9(3) . . . . ?
C11 C12 C15 O5 -18.6(5) . . . . ?
C13 C12 C15 O5 164.4(3) . . . . ?
C11 C12 C15 O6 159.9(3) . . . . ?
C13 C12 C15 O6 -17.1(5) . . . . ?
O5 C15 O6 Zn1 3.6(6) . . . 2_655 ?
C12 C15 O6 Zn1 -174.8(2) . . . 2_655 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.072
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1400664'
_audit_update_record             
;
2015-06-29 deposited with the CCDC.
2015-07-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H9 N O6 Zn, H2 O '
_chemical_formula_sum            'C15 H11 N O7 Zn'
_chemical_formula_weight         382.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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                   7.4952(2)
_cell_length_b                   17.4170(5)
_cell_length_c                   21.7353(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2837.41(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    1.772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.86988
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6784
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2498
_reflns_number_gt                2141
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0340P)²+2.4737P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2498
_refine_ls_number_parameters     217
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0314
_refine_ls_wR_factor_ref         0.0746
_refine_ls_wR_factor_gt          0.0715
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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
Zn1 Zn 0.03334(4) 1.188447(16) 0.928264(14) 0.02099(12) Uani 1 1 d . . .
O1 O 0.1292(3) 1.08508(11) 0.93569(10) 0.0361(5) Uani 1 1 d . . .
O4 O 0.3750(2) 0.75052(10) 0.99839(8) 0.0268(4) Uani 1 1 d . . .
O2 O 0.3660(3) 1.14170(12) 0.89641(12) 0.0500(6) Uani 1 1 d . . .
O6 O 0.9581(3) 0.75659(12) 0.64221(9) 0.0364(5) Uani 1 1 d . . .
O3 O 0.2052(3) 0.84000(11) 1.04111(10) 0.0384(5) Uani 1 1 d . . .
O5 O 1.0511(3) 0.66363(13) 0.70421(11) 0.0547(7) Uani 1 1 d . . .
N2 N 0.8940(3) 0.87817(12) 0.84548(10) 0.0226(5) Uani 1 1 d . . .
C1 C 0.2907(4) 1.08438(16) 0.91648(12) 0.0275(6) Uani 1 1 d . . .
C8 C 0.3234(3) 0.81929(14) 1.00396(12) 0.0228(6) Uani 1 1 d . . .
C2 C 0.3899(4) 1.00953(14) 0.92354(12) 0.0229(6) Uani 1 1 d . . .
C3 C 0.5642(4) 1.00264(15) 0.90246(12) 0.0242(6) Uani 1 1 d . . .
H4 H 0.6162 1.0427 0.8806 0.029 Uiso 1 1 calc R . .
C5 C 0.5818(3) 0.87554(14) 0.94520(11) 0.0206(6) Uani 1 1 d . . .
H5 H 0.6458 0.8306 0.9521 0.025 Uiso 1 1 calc R . .
C6 C 0.4076(3) 0.88181(14) 0.96625(12) 0.0194(5) Uani 1 1 d . . .
C7 C 0.3134(3) 0.94948(14) 0.95612(12) 0.0218(6) Uani 1 1 d . . .
H7 H 0.1981 0.9545 0.9713 0.026 Uiso 1 1 calc R . .
C4 C 0.6611(3) 0.93622(14) 0.91381(11) 0.0204(5) Uani 1 1 d . . .
C10 C 0.8576(4) 0.93143(16) 0.89845(12) 0.0274(6) Uani 1 1 d . . .
H10A H 0.9012 0.9823 0.8883 0.033 Uiso 1 1 calc R . .
H10B H 0.9224 0.9136 0.9343 0.033 Uiso 1 1 calc R . .
C11 C 0.9467(4) 0.80560(16) 0.85599(13) 0.0306(7) Uani 1 1 d . . .
H11 H 0.9618 0.7885 0.8962 0.037 Uiso 1 1 calc R . .
C16 C 0.9566(3) 0.78179(15) 0.74792(13) 0.0233(6) Uani 1 1 d . . .
C18 C 0.9784(4) 0.75650(17) 0.80770(13) 0.0328(7) Uani 1 1 d . . .
H18 H 1.0146 0.7063 0.8153 0.039 Uiso 1 1 calc R . .
C19 C 0.9936(4) 0.72844(17) 0.69437(13) 0.0292(6) Uani 1 1 d . . .
C20 C 0.9012(4) 0.85695(16) 0.73829(12) 0.0288(6) Uani 1 1 d . . .
H20 H 0.8851 0.8753 0.6985 0.035 Uiso 1 1 calc R . .
C22 C 0.8706(4) 0.90394(16) 0.78766(12) 0.0295(6) Uani 1 1 d . . .
H22 H 0.8332 0.9542 0.7812 0.035 Uiso 1 1 calc R . .
O1W O 0.2933(5) 0.55010(19) 0.7641(2) 0.1427(18) Uani 1 1 d . . .
H1WA H 0.3982 0.5657 0.7560 0.171 Uiso 1 1 d R . .
H1WB H 0.2221 0.5816 0.7471 0.214 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O6 1.9389(19) 4_656 ?
Zn1 O1 1.9452(18) . ?
Zn1 O3 1.9713(19) 5_577 ?
Zn1 O4 1.9911(19) 7_665 ?
O1 C1 1.281(3) . ?
O4 C8 1.265(3) . ?
O4 Zn1 1.9911(18) 7_655 ?
O2 C1 1.227(3) . ?
O6 C19 1.264(4) . ?
O6 Zn1 1.9389(19) 4_646 ?
O3 C8 1.251(3) . ?
O3 Zn1 1.9713(19) 5_577 ?
O5 C19 1.227(4) . ?
N2 C11 1.344(3) . ?
N2 C22 1.346(3) . ?
N2 C10 1.503(3) . ?
C1 C2 1.508(4) . ?
C8 C6 1.502(3) . ?
C2 C7 1.387(4) . ?
C2 C3 1.390(4) . ?
C3 C4 1.388(4) . ?
C3 H4 0.9300 . ?
C5 C6 1.388(4) . ?
C5 C4 1.391(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.391(3) . ?
C7 H7 0.9300 . ?
C4 C10 1.513(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C18 1.375(4) . ?
C11 H11 0.9300 . ?
C16 C18 1.382(4) . ?
C16 C20 1.389(4) . ?
C16 C19 1.515(4) . ?
C18 H18 0.9300 . ?
C20 C22 1.369(4) . ?
C20 H20 0.9300 . ?
C22 H22 0.9300 . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8499 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Zn1 O1 128.31(9) 4_656 . ?
O6 Zn1 O3 116.79(9) 4_656 5_577 ?
O1 Zn1 O3 94.27(9) . 5_577 ?
O6 Zn1 O4 105.13(8) 4_656 7_665 ?
O1 Zn1 O4 108.15(8) . 7_665 ?
O3 Zn1 O4 101.02(8) 5_577 7_665 ?
C1 O1 Zn1 109.33(17) . . ?
C8 O4 Zn1 133.88(18) . 7_655 ?
C19 O6 Zn1 117.67(19) . 4_646 ?
C8 O3 Zn1 141.92(18) . 5_577 ?
C11 N2 C22 120.7(2) . . ?
C11 N2 C10 120.2(2) . . ?
C22 N2 C10 119.1(2) . . ?
O2 C1 O1 122.9(3) . . ?
O2 C1 C2 120.9(3) . . ?
O1 C1 C2 116.1(2) . . ?
O3 C8 O4 123.4(2) . . ?
O3 C8 C6 116.1(2) . . ?
O4 C8 C6 120.4(2) . . ?
C7 C2 C3 119.4(2) . . ?
C7 C2 C1 120.0(2) . . ?
C3 C2 C1 120.3(2) . . ?
C4 C3 C2 120.3(2) . . ?
C4 C3 H4 119.8 . . ?
C2 C3 H4 119.8 . . ?
C6 C5 C4 120.3(2) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C7 119.5(2) . . ?
C5 C6 C8 121.2(2) . . ?
C7 C6 C8 119.2(2) . . ?
C2 C7 C6 120.7(2) . . ?
C2 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C3 C4 C5 119.8(2) . . ?
C3 C4 C10 121.1(2) . . ?
C5 C4 C10 118.8(2) . . ?
N2 C10 C4 112.3(2) . . ?
N2 C10 H10A 109.1 . . ?
C4 C10 H10A 109.1 . . ?
N2 C10 H10B 109.1 . . ?
C4 C10 H10B 109.1 . . ?
H10A C10 H10B 107.9 . . ?
N2 C11 C18 120.4(3) . . ?
N2 C11 H11 119.8 . . ?
C18 C11 H11 119.8 . . ?
C18 C16 C20 118.5(3) . . ?
C18 C16 C19 120.4(2) . . ?
C20 C16 C19 121.1(2) . . ?
C11 C18 C16 120.0(3) . . ?
C11 C18 H18 120.0 . . ?
C16 C18 H18 120.0 . . ?
O5 C19 O6 126.0(3) . . ?
O5 C19 C16 119.6(3) . . ?
O6 C19 C16 114.4(2) . . ?
C22 C20 C16 119.7(2) . . ?
C22 C20 H20 120.1 . . ?
C16 C20 H20 120.1 . . ?
N2 C22 C20 120.7(2) . . ?
N2 C22 H22 119.6 . . ?
C20 C22 H22 119.6 . . ?
H1WA O1W H1WB 106.5 . . ?

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
O6 Zn1 O1 C1 48.8(2) 4_656 . . . ?
O3 Zn1 O1 C1 178.17(19) 5_577 . . . ?
O4 Zn1 O1 C1 -78.76(19) 7_665 . . . ?
Zn1 O1 C1 O2 -0.7(3) . . . . ?
Zn1 O1 C1 C2 175.55(18) . . . . ?
Zn1 O3 C8 O4 -45.3(5) 5_577 . . . ?
Zn1 O3 C8 C6 136.4(3) 5_577 . . . ?
Zn1 O4 C8 O3 148.5(2) 7_655 . . . ?
Zn1 O4 C8 C6 -33.3(4) 7_655 . . . ?
O2 C1 C2 C7 168.6(3) . . . . ?
O1 C1 C2 C7 -7.7(4) . . . . ?
O2 C1 C2 C3 -5.5(4) . . . . ?
O1 C1 C2 C3 178.2(2) . . . . ?
C7 C2 C3 C4 0.1(4) . . . . ?
C1 C2 C3 C4 174.2(2) . . . . ?
C4 C5 C6 C7 -0.5(4) . . . . ?
C4 C5 C6 C8 -175.8(2) . . . . ?
O3 C8 C6 C5 151.2(2) . . . . ?
O4 C8 C6 C5 -27.2(4) . . . . ?
O3 C8 C6 C7 -24.1(4) . . . . ?
O4 C8 C6 C7 157.5(2) . . . . ?
C3 C2 C7 C6 -1.9(4) . . . . ?
C1 C2 C7 C6 -176.0(2) . . . . ?
C5 C6 C7 C2 2.1(4) . . . . ?
C8 C6 C7 C2 177.5(2) . . . . ?
C2 C3 C4 C5 1.5(4) . . . . ?
C2 C3 C4 C10 -172.2(2) . . . . ?
C6 C5 C4 C3 -1.3(4) . . . . ?
C6 C5 C4 C10 172.5(2) . . . . ?
C11 N2 C10 C4 -97.9(3) . . . . ?
C22 N2 C10 C4 81.2(3) . . . . ?
C3 C4 C10 N2 -110.5(3) . . . . ?
C5 C4 C10 N2 75.8(3) . . . . ?
C22 N2 C11 C18 0.3(4) . . . . ?
C10 N2 C11 C18 179.4(3) . . . . ?
N2 C11 C18 C16 0.2(4) . . . . ?
C20 C16 C18 C11 -0.5(4) . . . . ?
C19 C16 C18 C11 179.2(3) . . . . ?
Zn1 O6 C19 O5 8.0(4) 4_646 . . . ?
Zn1 O6 C19 C16 -171.05(17) 4_646 . . . ?
C18 C16 C19 O5 -3.4(4) . . . . ?
C20 C16 C19 O5 176.3(3) . . . . ?
C18 C16 C19 O6 175.7(3) . . . . ?
C20 C16 C19 O6 -4.6(4) . . . . ?
C18 C16 C20 C22 0.3(4) . . . . ?
C19 C16 C20 C22 -179.4(3) . . . . ?
C11 N2 C22 C20 -0.5(4) . . . . ?
C10 N2 C22 C20 -179.6(2) . . . . ?
C16 C20 C22 N2 0.2(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.064
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1400665'
_audit_update_record             
;
2015-06-29 deposited with the CCDC.
2015-07-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H13 N2 O6 Zn, 2(H2 O)'
_chemical_formula_sum            'C20 H17 N2 O8 Zn'
_chemical_formula_weight         478.73

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_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                   11.7220(4)
_cell_length_b                   15.3650(5)
_cell_length_c                   12.7229(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 119.424(4)
_cell_angle_gamma                90.00
_cell_volume                     1995.92(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             980
_exptl_absorpt_coefficient_mu    1.283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.96253
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8032
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.21
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3507
_reflns_number_gt                2702
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0486P)²+2.7489P] 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         3507
_refine_ls_number_parameters     284
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0463
_refine_ls_wR_factor_ref         0.1185
_refine_ls_wR_factor_gt          0.1070
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.004

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
Zn1 Zn 0.82686(4) 0.88186(3) 0.81275(4) 0.03845(17) Uani 1 1 d . . .
O1 O 0.7009(3) 0.7953(2) 0.7097(3) 0.0629(9) Uani 1 1 d . . .
O2 O 0.6446(4) 0.7751(3) 0.8490(3) 0.0849(13) Uani 1 1 d . . .
O3 O 0.3511(6) 0.5181(4) 0.7917(4) 0.184(3) Uani 1 1 d . . .
O4 O 0.2242(3) 0.4729(2) 0.6126(3) 0.0567(8) Uani 1 1 d . . .
O5 O 0.0356(4) 0.7574(3) -0.1549(3) 0.0910(14) Uani 1 1 d . . .
O6 O -0.0292(3) 0.8296(2) -0.0435(2) 0.0576(8) Uani 1 1 d . . .
N1 N 0.3249(3) 0.6447(2) 0.2561(3) 0.0411(8) Uani 1 1 d . . .
N2 N 0.8884(3) 0.9267(2) 0.6976(3) 0.0411(8) Uani 1 1 d . . .
C1 C 0.6341(4) 0.7589(3) 0.7507(4) 0.0477(10) Uani 1 1 d . . .
C2 C 0.5370(4) 0.6920(3) 0.6696(3) 0.0406(9) Uani 1 1 d . . .
C3 C 0.5185(4) 0.6767(3) 0.5544(4) 0.0431(10) Uani 1 1 d . . .
H3 H 0.5652 0.7092 0.5266 0.052 Uiso 1 1 calc R . .
C4 C 0.4314(4) 0.6135(3) 0.4804(3) 0.0422(9) Uani 1 1 d . . .
C5 C 0.3786(4) 0.5797(3) 0.6365(4) 0.0434(10) Uani 1 1 d . . .
C6 C 0.4674(4) 0.6426(3) 0.7100(4) 0.0448(10) Uani 1 1 d . . .
H6 H 0.4803 0.6515 0.7874 0.054 Uiso 1 1 calc R . .
C7 C 0.3594(4) 0.5661(3) 0.5211(3) 0.0434(10) Uani 1 1 d . . .
H7 H 0.2983 0.5253 0.4708 0.052 Uiso 1 1 calc R . .
C8 C 0.4228(4) 0.5921(3) 0.3614(4) 0.0505(11) Uani 1 1 d . . .
H8A H 0.5085 0.6006 0.3690 0.061 Uiso 1 1 calc R . .
H8B H 0.4007 0.5310 0.3442 0.061 Uiso 1 1 calc R . .
C9 C 0.3237(4) 0.6331(3) 0.1512(4) 0.0481(11) Uani 1 1 d . . .
H9 H 0.3838 0.5956 0.1474 0.058 Uiso 1 1 calc R . .
C10 C 0.2406(4) 0.6992(3) 0.2635(4) 0.0499(11) Uani 1 1 d . . .
H10 H 0.2430 0.7068 0.3370 0.060 Uiso 1 1 calc R . .
C11 C 0.1503(4) 0.7443(3) 0.1638(4) 0.0502(11) Uani 1 1 d . . .
H11 H 0.0929 0.7829 0.1702 0.060 Uiso 1 1 calc R . .
C12 C 0.1455(4) 0.7319(3) 0.0552(4) 0.0426(10) Uani 1 1 d . . .
C13 C 0.2349(4) 0.6760(3) 0.0499(4) 0.0479(11) Uani 1 1 d . . .
H13 H 0.2345 0.6675 -0.0226 0.057 Uiso 1 1 calc R . .
C14 C 0.3127(5) 0.5213(3) 0.6850(4) 0.0623(13) Uani 1 1 d . . .
C15 C 0.0425(4) 0.7767(3) -0.0593(4) 0.0501(11) Uani 1 1 d . . .
C17 C 0.9794(5) 0.9883(3) 0.7309(4) 0.0596(13) Uani 1 1 d . . .
H17 H 1.0137 1.0122 0.8077 0.072 Uiso 1 1 calc R . .
C18 C 0.8410(5) 0.8942(3) 0.5874(4) 0.0568(12) Uani 1 1 d . . .
H18 H 0.7765 0.8516 0.5625 0.068 Uiso 1 1 calc R . .
C19 C 1.0245(5) 1.0179(3) 0.6562(4) 0.0625(14) Uani 1 1 d . . .
H19 H 1.0885 1.0610 0.6832 0.075 Uiso 1 1 calc R . .
C20 C 0.9758(4) 0.9844(3) 0.5414(3) 0.0423(9) Uani 1 1 d . . .
C21 C 0.8819(5) 0.9199(3) 0.5081(4) 0.0550(12) Uani 1 1 d . . .
H21 H 0.8468 0.8942 0.4323 0.066 Uiso 1 1 calc R . .
O1W O 0.4531(6) 0.8867(5) 0.4921(6) 0.178(3) Uani 1 1 d . . .
H2 H 0.4738 0.9333 0.5316 0.267 Uiso 1 1 d R . .
H4 H 0.4589 0.8916 0.4387 0.267 Uiso 1 1 d R . .
O2W O 0.8242(5) 0.8589(3) 0.1193(4) 0.0930(14) Uani 1 1 d . . .
H1 H 0.7696 0.8335 0.0546 0.140 Uiso 1 1 d R . .
H25 H 0.855(10) 0.813(7) 0.164(9) 0.21(5) 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
Zn1 O1 1.940(3) . ?
Zn1 O4 1.944(3) 2_656 ?
Zn1 O6 1.951(3) 1_656 ?
Zn1 N2 2.045(3) . ?
O1 C1 1.266(5) . ?
O2 C1 1.220(5) . ?
O3 C14 1.203(5) . ?
O4 C14 1.240(5) . ?
O4 Zn1 1.944(3) 2_646 ?
O5 C15 1.216(5) . ?
O6 C15 1.254(5) . ?
O6 Zn1 1.951(3) 1_454 ?
N1 C10 1.333(5) . ?
N1 C9 1.339(5) . ?
N1 C8 1.502(5) . ?
N2 C18 1.326(5) . ?
N2 C17 1.330(5) . ?
C1 C2 1.505(6) . ?
C2 C6 1.385(5) . ?
C2 C3 1.393(5) . ?
C3 C4 1.388(6) . ?
C3 H3 0.9300 . ?
C4 C7 1.393(6) . ?
C4 C8 1.503(5) . ?
C5 C6 1.392(6) . ?
C5 C7 1.388(5) . ?
C5 C14 1.500(6) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C13 1.363(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.374(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.368(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.383(6) . ?
C12 C15 1.525(6) . ?
C13 H13 0.9300 . ?
C17 C19 1.373(6) . ?
C17 H17 0.9300 . ?
C18 C21 1.371(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.380(6) . ?
C19 H19 0.9300 . ?
C20 C21 1.384(6) . ?
C20 C20 1.500(7) 3_776 ?
C21 H21 0.9300 . ?
O1W H2 0.8392 . ?
O1W H4 0.7199 . ?
O2W H1 0.8499 . ?
O2W H25 0.87(10) . ?

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 Zn1 O4 120.60(14) . 2_656 ?
O1 Zn1 O6 111.83(15) . 1_656 ?
O4 Zn1 O6 99.81(13) 2_656 1_656 ?
O1 Zn1 N2 99.52(13) . . ?
O4 Zn1 N2 114.19(13) 2_656 . ?
O6 Zn1 N2 111.32(13) 1_656 . ?
C1 O1 Zn1 116.3(3) . . ?
C14 O4 Zn1 114.4(3) . 2_646 ?
C15 O6 Zn1 117.1(3) . 1_454 ?
C10 N1 C9 120.5(3) . . ?
C10 N1 C8 122.9(3) . . ?
C9 N1 C8 116.6(3) . . ?
C18 N2 C17 117.3(3) . . ?
C18 N2 Zn1 121.2(3) . . ?
C17 N2 Zn1 121.4(3) . . ?
O2 C1 O1 124.2(4) . . ?
O2 C1 C2 120.3(4) . . ?
O1 C1 C2 115.6(4) . . ?
C6 C2 C3 118.9(4) . . ?
C6 C2 C1 120.3(4) . . ?
C3 C2 C1 120.8(4) . . ?
C4 C3 C2 120.9(4) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C7 119.5(4) . . ?
C3 C4 C8 119.9(4) . . ?
C7 C4 C8 120.5(4) . . ?
C6 C5 C7 119.6(4) . . ?
C6 C5 C14 120.3(4) . . ?
C7 C5 C14 119.8(4) . . ?
C5 C6 C2 120.9(4) . . ?
C5 C6 H6 119.6 . . ?
C2 C6 H6 119.6 . . ?
C5 C7 C4 120.1(4) . . ?
C5 C7 H7 119.9 . . ?
C4 C7 H7 119.9 . . ?
N1 C8 C4 115.2(3) . . ?
N1 C8 H8A 108.5 . . ?
C4 C8 H8A 108.5 . . ?
N1 C8 H8B 108.5 . . ?
C4 C8 H8B 108.5 . . ?
H8A C8 H8B 107.5 . . ?
N1 C9 C13 120.5(4) . . ?
N1 C9 H9 119.8 . . ?
C13 C9 H9 119.8 . . ?
N1 C10 C11 120.9(4) . . ?
N1 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C10 C11 C12 119.5(4) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C11 C12 C13 118.6(4) . . ?
C11 C12 C15 121.5(4) . . ?
C13 C12 C15 119.8(4) . . ?
C9 C13 C12 119.9(4) . . ?
C9 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
O3 C14 O4 121.8(4) . . ?
O3 C14 C5 120.4(4) . . ?
O4 C14 C5 117.6(4) . . ?
O5 C15 O6 126.8(4) . . ?
O5 C15 C12 118.6(4) . . ?
O6 C15 C12 114.6(4) . . ?
N2 C17 C19 122.4(4) . . ?
N2 C17 H17 118.8 . . ?
C19 C17 H17 118.8 . . ?
N2 C18 C21 123.6(4) . . ?
N2 C18 H18 118.2 . . ?
C21 C18 H18 118.2 . . ?
C20 C19 C17 120.6(4) . . ?
C20 C19 H19 119.7 . . ?
C17 C19 H19 119.7 . . ?
C19 C20 C21 116.4(4) . . ?
C19 C20 C20 121.5(5) . 3_776 ?
C21 C20 C20 122.1(5) . 3_776 ?
C18 C21 C20 119.6(4) . . ?
C18 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
H2 O1W H4 110.0 . . ?
H1 O2W H25 97.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 Zn1 O1 C1 -48.5(4) 2_656 . . . ?
O6 Zn1 O1 C1 68.2(4) 1_656 . . . ?
N2 Zn1 O1 C1 -174.1(3) . . . . ?
O1 Zn1 N2 C18 -0.5(4) . . . . ?
O4 Zn1 N2 C18 -130.4(3) 2_656 . . . ?
O6 Zn1 N2 C18 117.5(3) 1_656 . . . ?
O1 Zn1 N2 C17 -179.2(4) . . . . ?
O4 Zn1 N2 C17 50.9(4) 2_656 . . . ?
O6 Zn1 N2 C17 -61.1(4) 1_656 . . . ?
Zn1 O1 C1 O2 0.1(6) . . . . ?
Zn1 O1 C1 C2 180.0(3) . . . . ?
O2 C1 C2 C6 -6.0(7) . . . . ?
O1 C1 C2 C6 174.1(4) . . . . ?
O2 C1 C2 C3 176.1(4) . . . . ?
O1 C1 C2 C3 -3.8(6) . . . . ?
C6 C2 C3 C4 0.4(6) . . . . ?
C1 C2 C3 C4 178.4(4) . . . . ?
C2 C3 C4 C7 1.4(6) . . . . ?
C2 C3 C4 C8 -174.0(4) . . . . ?
C7 C5 C6 C2 0.1(6) . . . . ?
C14 C5 C6 C2 174.6(4) . . . . ?
C3 C2 C6 C5 -1.2(6) . . . . ?
C1 C2 C6 C5 -179.1(4) . . . . ?
C6 C5 C7 C4 1.8(6) . . . . ?
C14 C5 C7 C4 -172.8(4) . . . . ?
C3 C4 C7 C5 -2.5(6) . . . . ?
C8 C4 C7 C5 172.9(4) . . . . ?
C10 N1 C8 C4 -7.5(6) . . . . ?
C9 N1 C8 C4 173.8(4) . . . . ?
C3 C4 C8 N1 -90.2(5) . . . . ?
C7 C4 C8 N1 94.4(5) . . . . ?
C10 N1 C9 C13 -1.0(6) . . . . ?
C8 N1 C9 C13 177.7(4) . . . . ?
C9 N1 C10 C11 0.4(7) . . . . ?
C8 N1 C10 C11 -178.2(4) . . . . ?
N1 C10 C11 C12 1.1(7) . . . . ?
C10 C11 C12 C13 -1.9(7) . . . . ?
C10 C11 C12 C15 176.8(4) . . . . ?
N1 C9 C13 C12 0.1(7) . . . . ?
C11 C12 C13 C9 1.3(7) . . . . ?
C15 C12 C13 C9 -177.4(4) . . . . ?
Zn1 O4 C14 O3 -8.7(8) 2_646 . . . ?
Zn1 O4 C14 C5 166.5(3) 2_646 . . . ?
C6 C5 C14 O3 -12.4(9) . . . . ?
C7 C5 C14 O3 162.2(6) . . . . ?
C6 C5 C14 O4 172.4(4) . . . . ?
C7 C5 C14 O4 -13.1(7) . . . . ?
Zn1 O6 C15 O5 3.7(7) 1_454 . . . ?
Zn1 O6 C15 C12 -174.8(3) 1_454 . . . ?
C11 C12 C15 O5 -173.6(5) . . . . ?
C13 C12 C15 O5 5.0(7) . . . . ?
C11 C12 C15 O6 5.0(6) . . . . ?
C13 C12 C15 O6 -176.4(4) . . . . ?
C18 N2 C17 C19 -0.3(7) . . . . ?
Zn1 N2 C17 C19 178.4(4) . . . . ?
C17 N2 C18 C21 0.9(7) . . . . ?
Zn1 N2 C18 C21 -177.8(4) . . . . ?
N2 C17 C19 C20 0.2(8) . . . . ?
C17 C19 C20 C21 -0.7(7) . . . . ?
C17 C19 C20 C20 -179.7(5) . . . 3_776 ?
N2 C18 C21 C20 -1.3(8) . . . . ?
C19 C20 C21 C18 1.2(7) . . . . ?
C20 C20 C21 C18 -179.8(5) 3_776 . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.560
_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_4
_database_code_depnum_ccdc_archive 'CCDC 1400666'
_audit_update_record             
;
2015-06-29 deposited with the CCDC.
2015-07-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H9 Cd N O6, H2 O'
_chemical_formula_sum            'C15 H11 Br0 Cd N O7'
_chemical_formula_weight         429.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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           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                   17.0363(4)
_cell_length_b                   7.7794(2)
_cell_length_c                   20.1494(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2670.44(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            clourless
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.137
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1696
_exptl_absorpt_coefficient_mu    1.680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.95884
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6841
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2349
_reflns_number_gt                1873
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0225P)²+5.7856P] 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         2349
_refine_ls_number_parameters     217
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0304
_refine_ls_wR_factor_ref         0.0720
_refine_ls_wR_factor_gt          0.0683
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.005
_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
Cd1 Cd 1.214549(16) 1.00185(3) 0.903798(13) 0.01341(11) Uani 1 1 d . . .
O1 O 1.10659(16) 0.8228(3) 0.90776(13) 0.0185(6) Uani 1 1 d . . .
O2 O 1.15537(17) 0.5567(4) 0.89190(14) 0.0230(7) Uani 1 1 d . . .
O3 O 0.85251(17) 0.8442(3) 1.02110(14) 0.0208(7) Uani 1 1 d . . .
O4 O 0.76003(16) 0.6472(3) 1.00162(13) 0.0201(6) Uani 1 1 d . . .
O5 O 0.8576(2) -0.3553(4) 0.68050(15) 0.0301(8) Uani 1 1 d . . .
O6 O 0.75068(19) -0.1906(4) 0.68037(15) 0.0314(8) Uani 1 1 d . . .
N5 N 0.9045(2) 0.0464(4) 0.86757(16) 0.0152(7) Uani 1 1 d . . .
C1 C 1.0200(2) 0.5845(5) 0.91215(18) 0.0131(8) Uani 1 1 d . . .
C2 C 1.0090(2) 0.4075(5) 0.90415(18) 0.0137(8) Uani 1 1 d . . .
H2 H 1.0494 0.3407 0.8869 0.016 Uiso 1 1 calc R . .
C3 C 0.8271(3) 0.0222(5) 0.8615(2) 0.0242(10) Uani 1 1 d . . .
H3 H 0.7932 0.0647 0.8937 0.029 Uiso 1 1 calc R . .
C4 C 0.9551(3) -0.0164(5) 0.8221(2) 0.0223(9) Uani 1 1 d . . .
H4 H 1.0087 0.0027 0.8270 0.027 Uiso 1 1 calc R . .
C5 C 0.8483(3) -0.1333(5) 0.7607(2) 0.0187(9) Uani 1 1 d . . .
C6 C 0.9385(2) 0.3304(5) 0.92159(18) 0.0137(8) Uani 1 1 d . . .
C7 C 1.1005(2) 0.6617(5) 0.90255(18) 0.0142(8) Uani 1 1 d . . .
C8 C 0.7974(3) -0.0656(6) 0.8076(2) 0.0267(10) Uani 1 1 d . . .
H8 H 0.7435 -0.0793 0.8027 0.032 Uiso 1 1 calc R . .
C9 C 0.9590(2) 0.6805(5) 0.93818(18) 0.0128(8) Uani 1 1 d . . .
H9 H 0.9661 0.7979 0.9445 0.015 Uiso 1 1 calc R . .
C10 C 0.9279(3) -0.1081(5) 0.7689(2) 0.0226(10) Uani 1 1 d . . .
H10 H 0.9631 -0.1533 0.7382 0.027 Uiso 1 1 calc R . .
C11 C 0.8769(2) 0.4297(5) 0.94565(19) 0.0139(8) Uani 1 1 d . . .
H11 H 0.8288 0.3788 0.9553 0.017 Uiso 1 1 calc R . .
C12 C 0.9363(3) 0.1365(5) 0.92734(19) 0.0172(9) Uani 1 1 d . . .
H12A H 0.9891 0.0953 0.9356 0.021 Uiso 1 1 calc R . .
H12B H 0.9044 0.1059 0.9654 0.021 Uiso 1 1 calc R . .
C13 C 0.8163(3) -0.2352(5) 0.7018(2) 0.0215(10) Uani 1 1 d . . .
C14 C 0.8279(2) 0.7071(5) 0.99545(18) 0.0128(8) Uani 1 1 d . . .
C20 C 0.8872(2) 0.6066(5) 0.95526(18) 0.0118(8) Uani 1 1 d . . .
O1W O 0.8887(3) 0.3277(7) 0.7580(2) 0.0931(17) Uani 1 1 d . . .
H1WB H 0.8954 0.4165 0.7341 0.140 Uiso 1 1 d R . .
H1WA H 0.8972 0.3158 0.7993 0.140 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O3 2.242(3) 5_777 ?
Cd1 O2 2.269(3) 7_865 ?
Cd1 O1 2.308(3) . ?
Cd1 O6 2.344(3) 6_667 ?
Cd1 O4 2.362(3) 3_567 ?
Cd1 O5 2.373(3) 4_766 ?
O1 C7 1.263(5) . ?
O2 C7 1.260(5) . ?
O2 Cd1 2.269(3) 7_855 ?
O3 C14 1.257(4) . ?
O3 Cd1 2.242(3) 5_777 ?
O4 C14 1.253(5) . ?
O4 Cd1 2.362(3) 3_467 ?
O5 C13 1.245(5) . ?
O5 Cd1 2.373(3) 4_736 ?
O6 C13 1.248(5) . ?
O6 Cd1 2.344(3) 6_547 ?
N5 C3 1.339(5) . ?
N5 C4 1.349(5) . ?
N5 C12 1.495(5) . ?
C1 C9 1.383(5) . ?
C1 C2 1.399(5) . ?
C1 C7 1.509(5) . ?
C2 C6 1.386(5) . ?
C2 H2 0.9300 . ?
C3 C8 1.380(6) . ?
C3 H3 0.9300 . ?
C4 C10 1.369(6) . ?
C4 H4 0.9300 . ?
C5 C8 1.385(6) . ?
C5 C10 1.381(6) . ?
C5 C13 1.528(6) . ?
C6 C11 1.392(5) . ?
C6 C12 1.513(5) . ?
C8 H8 0.9300 . ?
C9 C20 1.394(5) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C20 1.400(5) . ?
C11 H11 0.9300 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C14 C20 1.512(5) . ?
O1W H1WB 0.8500 . ?
O1W H1WA 0.8501 . ?

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 Cd1 O2 117.93(10) 5_777 7_865 ?
O3 Cd1 O1 83.85(10) 5_777 . ?
O2 Cd1 O1 153.53(10) 7_865 . ?
O3 Cd1 O6 164.34(11) 5_777 6_667 ?
O2 Cd1 O6 77.72(11) 7_865 6_667 ?
O1 Cd1 O6 81.32(10) . 6_667 ?
O3 Cd1 O4 83.38(10) 5_777 3_567 ?
O2 Cd1 O4 81.79(10) 7_865 3_567 ?
O1 Cd1 O4 86.41(10) . 3_567 ?
O6 Cd1 O4 100.61(11) 6_667 3_567 ?
O3 Cd1 O5 88.23(11) 5_777 4_766 ?
O2 Cd1 O5 110.00(11) 7_865 4_766 ?
O1 Cd1 O5 83.95(10) . 4_766 ?
O6 Cd1 O5 85.25(11) 6_667 4_766 ?
O4 Cd1 O5 167.84(11) 3_567 4_766 ?
C7 O1 Cd1 131.5(3) . . ?
C7 O2 Cd1 146.0(3) . 7_855 ?
C14 O3 Cd1 124.1(3) . 5_777 ?
C14 O4 Cd1 124.4(2) . 3_467 ?
C13 O5 Cd1 107.8(3) . 4_736 ?
C13 O6 Cd1 131.6(3) . 6_547 ?
C3 N5 C4 121.1(3) . . ?
C3 N5 C12 119.8(3) . . ?
C4 N5 C12 119.1(3) . . ?
C9 C1 C2 118.3(4) . . ?
C9 C1 C7 121.1(3) . . ?
C2 C1 C7 119.9(4) . . ?
C6 C2 C1 120.8(4) . . ?
C6 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
N5 C3 C8 120.2(4) . . ?
N5 C3 H3 119.9 . . ?
C8 C3 H3 119.9 . . ?
N5 C4 C10 120.3(4) . . ?
N5 C4 H4 119.8 . . ?
C10 C4 H4 119.8 . . ?
C8 C5 C10 118.7(4) . . ?
C8 C5 C13 120.2(4) . . ?
C10 C5 C13 121.1(4) . . ?
C2 C6 C11 120.1(3) . . ?
C2 C6 C12 118.2(4) . . ?
C11 C6 C12 120.5(4) . . ?
O2 C7 O1 126.6(4) . . ?
O2 C7 C1 116.0(3) . . ?
O1 C7 C1 117.3(4) . . ?
C3 C8 C5 119.7(4) . . ?
C3 C8 H8 120.2 . . ?
C5 C8 H8 120.2 . . ?
C1 C9 C20 122.0(3) . . ?
C1 C9 H9 119.0 . . ?
C20 C9 H9 119.0 . . ?
C4 C10 C5 120.0(4) . . ?
C4 C10 H10 120.0 . . ?
C5 C10 H10 120.0 . . ?
C6 C11 C20 119.9(4) . . ?
C6 C11 H11 120.0 . . ?
C20 C11 H11 120.0 . . ?
N5 C12 C6 114.5(3) . . ?
N5 C12 H12A 108.6 . . ?
C6 C12 H12A 108.6 . . ?
N5 C12 H12B 108.6 . . ?
C6 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
O5 C13 O6 126.5(4) . . ?
O5 C13 C5 117.1(4) . . ?
O6 C13 C5 116.3(4) . . ?
O4 C14 O3 125.6(4) . . ?
O4 C14 C20 118.5(3) . . ?
O3 C14 C20 115.9(3) . . ?
C9 C20 C11 118.8(4) . . ?
C9 C20 C14 120.3(3) . . ?
C11 C20 C14 119.8(3) . . ?
H1WB O1W H1WA 128.4 . . ?

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
O3 Cd1 O1 C7 -145.7(3) 5_777 . . . ?
O2 Cd1 O1 C7 1.5(5) 7_865 . . . ?
O6 Cd1 O1 C7 39.4(3) 6_667 . . . ?
O4 Cd1 O1 C7 -61.9(3) 3_567 . . . ?
O5 Cd1 O1 C7 125.5(3) 4_766 . . . ?
C9 C1 C2 C6 0.3(6) . . . . ?
C7 C1 C2 C6 170.9(3) . . . . ?
C4 N5 C3 C8 -1.1(6) . . . . ?
C12 N5 C3 C8 -177.9(4) . . . . ?
C3 N5 C4 C10 -0.6(6) . . . . ?
C12 N5 C4 C10 176.2(4) . . . . ?
C1 C2 C6 C11 1.8(6) . . . . ?
C1 C2 C6 C12 -165.7(3) . . . . ?
Cd1 O2 C7 O1 28.0(7) 7_855 . . . ?
Cd1 O2 C7 C1 -149.9(3) 7_855 . . . ?
Cd1 O1 C7 O2 -1.8(6) . . . . ?
Cd1 O1 C7 C1 176.1(2) . . . . ?
C9 C1 C7 O2 165.7(4) . . . . ?
C2 C1 C7 O2 -4.7(5) . . . . ?
C9 C1 C7 O1 -12.4(5) . . . . ?
C2 C1 C7 O1 177.3(3) . . . . ?
N5 C3 C8 C5 2.0(7) . . . . ?
C10 C5 C8 C3 -1.1(7) . . . . ?
C13 C5 C8 C3 178.3(4) . . . . ?
C2 C1 C9 C20 -1.2(6) . . . . ?
C7 C1 C9 C20 -171.7(3) . . . . ?
N5 C4 C10 C5 1.4(6) . . . . ?
C8 C5 C10 C4 -0.6(6) . . . . ?
C13 C5 C10 C4 -180.0(4) . . . . ?
C2 C6 C11 C20 -3.1(6) . . . . ?
C12 C6 C11 C20 164.2(3) . . . . ?
C3 N5 C12 C6 -86.5(5) . . . . ?
C4 N5 C12 C6 96.6(4) . . . . ?
C2 C6 C12 N5 -98.3(4) . . . . ?
C11 C6 C12 N5 94.2(4) . . . . ?
Cd1 O5 C13 O6 -3.9(5) 4_736 . . . ?
Cd1 O5 C13 C5 175.2(3) 4_736 . . . ?
Cd1 O6 C13 O5 -88.4(5) 6_547 . . . ?
Cd1 O6 C13 C5 92.6(4) 6_547 . . . ?
C8 C5 C13 O5 -146.8(4) . . . . ?
C10 C5 C13 O5 32.6(6) . . . . ?
C8 C5 C13 O6 32.3(6) . . . . ?
C10 C5 C13 O6 -148.3(4) . . . . ?
Cd1 O4 C14 O3 -78.4(4) 3_467 . . . ?
Cd1 O4 C14 C20 100.1(3) 3_467 . . . ?
Cd1 O3 C14 O4 8.9(5) 5_777 . . . ?
Cd1 O3 C14 C20 -169.7(2) 5_777 . . . ?
C1 C9 C20 C11 0.0(6) . . . . ?
C1 C9 C20 C14 168.2(3) . . . . ?
C6 C11 C20 C9 2.2(6) . . . . ?
C6 C11 C20 C14 -166.1(3) . . . . ?
O4 C14 C20 C9 169.7(3) . . . . ?
O3 C14 C20 C9 -11.7(5) . . . . ?
O4 C14 C20 C11 -22.3(5) . . . . ?
O3 C14 C20 C11 156.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.096
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1400667'
_audit_update_record             
;
2015-06-29 deposited with the CCDC.
2015-07-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H25 Cd N5 O7, H2 O'
_chemical_formula_sum            'C25 H27 Cd N5 O8'
_chemical_formula_weight         637.92

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'
Cd Cd -0.8075 1.2024 '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           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                   8.6985(4)
_cell_length_b                   9.4824(6)
_cell_length_c                   17.7549(10)
_cell_angle_alpha                80.703(5)
_cell_angle_beta                 77.485(5)
_cell_angle_gamma                65.302(5)
_cell_volume                     1294.72(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             648
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.97815
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9754
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0587
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4569
_reflns_number_gt                3921
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0298P)²+0.1105P] 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         4569
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.0764
_refine_ls_wR_factor_gt          0.0730
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_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
C15 C 0.7481(4) 0.2718(4) 0.10276(19) 0.0271(8) Uani 1 1 d . . .
Cd2 Cd -0.07282(3) 0.96238(3) 0.158236(14) 0.02497(9) Uani 1 1 d . . .
O1W O -0.1283(3) 0.8677(3) 0.05528(13) 0.0353(6) Uani 1 1 d . . .
H3 H -0.1212 0.9325 0.0067 0.053 Uiso 1 1 d R . .
H2 H -0.2248 0.9267 0.0453 0.053 Uiso 1 1 d R . .
O2 O 0.1945(3) 0.7726(3) 0.13353(14) 0.0368(6) Uani 1 1 d . . .
O1 O 0.2758(3) 0.9612(3) 0.07622(15) 0.0410(7) Uani 1 1 d . . .
O5 O 0.5181(4) 0.8242(4) -0.40851(16) 0.0614(9) Uani 1 1 d . . .
O6 O 0.5405(4) 0.5805(4) -0.37196(16) 0.0609(9) Uani 1 1 d . . .
N1 N 0.7887(3) 0.6820(3) -0.17331(14) 0.0233(6) Uani 1 1 d . . .
N3 N -0.0175(4) 1.0300(3) 0.26394(16) 0.0340(7) Uani 1 1 d . . .
N2 N -0.0653(4) 1.1479(4) 0.36899(16) 0.0376(8) Uani 1 1 d . . .
C5 C 0.6875(4) 0.4374(4) 0.06509(18) 0.0221(7) Uani 1 1 d . . .
C4 C 0.5301(4) 0.5481(4) 0.09377(18) 0.0246(8) Uani 1 1 d . . .
H4 H 0.4598 0.5201 0.1353 0.030 Uiso 1 1 calc R . .
C2 C 0.4754(4) 0.7012(4) 0.06119(18) 0.0226(7) Uani 1 1 d . . .
C3 C 0.5807(4) 0.7419(4) -0.00051(18) 0.0238(8) Uani 1 1 d . . .
H3A H 0.5455 0.8444 -0.0219 0.029 Uiso 1 1 calc R . .
C7 C 0.7390(4) 0.6315(4) -0.03119(17) 0.0214(7) Uani 1 1 d . . .
C6 C 0.7911(4) 0.4786(4) 0.00182(17) 0.0227(7) Uani 1 1 d . . .
H6 H 0.8958 0.4036 -0.0185 0.027 Uiso 1 1 calc R . .
C8 C 0.8523(4) 0.6743(4) -0.10050(17) 0.0250(8) Uani 1 1 d . . .
H8A H 0.8522 0.7744 -0.0949 0.030 Uiso 1 1 calc R . .
H8B H 0.9692 0.5971 -0.1030 0.030 Uiso 1 1 calc R . .
C1 C 0.3021(4) 0.8212(4) 0.09254(19) 0.0266(8) Uani 1 1 d . . .
C9 C 0.8153(4) 0.5488(4) -0.20158(19) 0.0293(8) Uani 1 1 d . . .
H9 H 0.8812 0.4535 -0.1783 0.035 Uiso 1 1 calc R . .
C10 C 0.7455(5) 0.5533(4) -0.26456(19) 0.0316(8) Uani 1 1 d . . .
H10 H 0.7628 0.4610 -0.2835 0.038 Uiso 1 1 calc R . .
C11 C 0.6500(4) 0.6937(4) -0.29979(18) 0.0299(8) Uani 1 1 d . . .
C13 C 0.6972(4) 0.8209(4) -0.20717(19) 0.0302(8) Uani 1 1 d . . .
H13 H 0.6794 0.9120 -0.1868 0.036 Uiso 1 1 calc R . .
C12 C 0.6303(4) 0.8289(4) -0.27133(19) 0.0326(9) Uani 1 1 d . . .
H12 H 0.5713 0.9252 -0.2959 0.039 Uiso 1 1 calc R . .
C14 C 0.5607(5) 0.7003(6) -0.3665(2) 0.0430(10) Uani 1 1 d . . .
C18 C -0.1193(5) 1.1521(4) 0.3030(2) 0.0377(9) Uani 1 1 d . . .
H18 H -0.2164 1.2313 0.2868 0.045 Uiso 1 1 calc R . .
C16 C 0.1081(5) 0.9440(4) 0.3077(2) 0.0403(10) Uani 1 1 d . . .
H16 H 0.1984 0.8500 0.2951 0.048 Uiso 1 1 calc R . .
C17 C 0.0809(5) 1.0162(5) 0.3721(2) 0.0410(10) Uani 1 1 d . . .
H17 H 0.1484 0.9828 0.4107 0.049 Uiso 1 1 calc R . .
C19 C -0.1475(6) 1.2684(5) 0.4243(2) 0.0455(11) Uani 1 1 d . . .
H19A H -0.1298 1.2201 0.4760 0.055 Uiso 1 1 calc R . .
H19B H -0.2701 1.3154 0.4239 0.055 Uiso 1 1 calc R . .
C20 C -0.0785(5) 1.3941(4) 0.4062(2) 0.0410(10) Uani 1 1 d . . .
H20A H -0.0696 1.4241 0.3511 0.049 Uiso 1 1 calc R . .
H20B H 0.0362 1.3522 0.4189 0.049 Uiso 1 1 calc R . .
C21 C -0.1893(5) 1.5388(4) 0.4499(2) 0.0416(10) Uani 1 1 d . . .
H21A H -0.2191 1.5059 0.5037 0.050 Uiso 1 1 calc R . .
H21B H -0.1216 1.5989 0.4483 0.050 Uiso 1 1 calc R . .
C22 C -0.3535(5) 1.6439(5) 0.4192(2) 0.0439(11) Uani 1 1 d . . .
H22A H -0.4254 1.5868 0.4233 0.053 Uiso 1 1 calc R . .
H22B H -0.4158 1.7320 0.4505 0.053 Uiso 1 1 calc R . .
O2W O 0.2651(4) 0.0439(4) 0.51019(19) 0.0762(10) Uani 1 1 d . . .
H2WD H 0.2777 0.0833 0.4639 0.091 Uiso 1 1 d R . .
H2WC H 0.3622 -0.0010 0.5249 0.114 Uiso 1 1 d R . .
C24 C -0.3531(5) 1.6624(5) 0.2740(2) 0.0466(11) Uani 1 1 d . . .
H24 H -0.4106 1.5988 0.2741 0.056 Uiso 1 1 calc R . .
N4 N -0.3175(4) 1.7015(3) 0.33723(16) 0.0352(7) Uani 1 1 d . . .
C23 C -0.2353(5) 1.7969(4) 0.3107(2) 0.0350(9) Uani 1 1 d . . .
H23 H -0.1975 1.8412 0.3421 0.042 Uiso 1 1 calc R . .
N5 N -0.2150(4) 1.8198(3) 0.23422(16) 0.0322(7) Uani 1 1 d . . .
C25 C -0.2885(5) 1.7342(5) 0.2118(2) 0.0429(10) Uani 1 1 d . . .
H25 H -0.2932 1.7269 0.1608 0.051 Uiso 1 1 calc R . .
O3 O 0.8907(3) 0.1746(2) 0.07241(13) 0.0347(6) Uani 1 1 d . . .
O4 O 0.6612(3) 0.2388(3) 0.16191(16) 0.0537(9) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C15 O4 1.233(4) . ?
C15 O3 1.263(4) . ?
C15 C5 1.520(4) . ?
Cd2 O2 2.270(2) . ?
Cd2 O3 2.271(2) 1_465 ?
Cd2 N3 2.281(3) . ?
Cd2 N5 2.294(3) 1_545 ?
Cd2 O1W 2.378(2) . ?
O1W H3 0.9814 . ?
O1W H2 0.8300 . ?
O2 C1 1.255(4) . ?
O1 C1 1.245(4) . ?
O5 C14 1.243(5) . ?
O6 C14 1.242(5) . ?
N1 C13 1.344(4) . ?
N1 C9 1.346(4) . ?
N1 C8 1.493(4) . ?
N3 C18 1.321(4) . ?
N3 C16 1.372(5) . ?
N2 C18 1.343(5) . ?
N2 C17 1.364(5) . ?
N2 C19 1.469(5) . ?
C5 C4 1.380(4) . ?
C5 C6 1.393(4) . ?
C4 C2 1.393(4) . ?
C4 H4 0.9300 . ?
C2 C3 1.382(4) . ?
C2 C1 1.512(4) . ?
C3 C7 1.394(4) . ?
C3 H3A 0.9300 . ?
C7 C6 1.393(4) . ?
C7 C8 1.516(4) . ?
C6 H6 0.9300 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.370(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.373(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.384(5) . ?
C11 C14 1.531(5) . ?
C13 C12 1.366(5) . ?
C13 H13 0.9300 . ?
C12 H12 0.9300 . ?
C18 H18 0.9300 . ?
C16 C17 1.353(5) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C19 C20 1.508(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.526(5) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.518(5) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 N4 1.484(4) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
O2W H2WD 0.8500 . ?
O2W H2WC 0.8500 . ?
C24 C25 1.344(5) . ?
C24 N4 1.369(5) . ?
C24 H24 0.9300 . ?
N4 C23 1.345(5) . ?
C23 N5 1.325(4) . ?
C23 H23 0.9300 . ?
N5 C25 1.370(5) . ?
N5 Cd2 2.294(3) 1_565 ?
C25 H25 0.9300 . ?
O3 Cd2 2.271(2) 1_645 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 C15 O3 122.8(3) . . ?
O4 C15 C5 119.8(3) . . ?
O3 C15 C5 117.3(3) . . ?
O2 Cd2 O3 112.03(8) . 1_465 ?
O2 Cd2 N3 93.19(10) . . ?
O3 Cd2 N3 103.84(10) 1_465 . ?
O2 Cd2 N5 100.15(9) . 1_545 ?
O3 Cd2 N5 142.95(10) 1_465 1_545 ?
N3 Cd2 N5 91.80(10) . 1_545 ?
O2 Cd2 O1W 84.62(9) . . ?
O3 Cd2 O1W 81.94(9) 1_465 . ?
N3 Cd2 O1W 174.21(9) . . ?
N5 Cd2 O1W 83.33(9) 1_545 . ?
Cd2 O1W H3 111.5 . . ?
Cd2 O1W H2 108.8 . . ?
H3 O1W H2 68.2 . . ?
C1 O2 Cd2 113.5(2) . . ?
C13 N1 C9 120.8(3) . . ?
C13 N1 C8 119.8(3) . . ?
C9 N1 C8 119.2(3) . . ?
C18 N3 C16 105.1(3) . . ?
C18 N3 Cd2 125.5(3) . . ?
C16 N3 Cd2 128.6(3) . . ?
C18 N2 C17 107.1(3) . . ?
C18 N2 C19 125.1(3) . . ?
C17 N2 C19 127.8(3) . . ?
C4 C5 C6 119.6(3) . . ?
C4 C5 C15 120.2(3) . . ?
C6 C5 C15 120.2(3) . . ?
C5 C4 C2 120.7(3) . . ?
C5 C4 H4 119.6 . . ?
C2 C4 H4 119.6 . . ?
C3 C2 C4 119.3(3) . . ?
C3 C2 C1 120.4(3) . . ?
C4 C2 C1 120.3(3) . . ?
C2 C3 C7 121.0(3) . . ?
C2 C3 H3A 119.5 . . ?
C7 C3 H3A 119.5 . . ?
C6 C7 C3 119.0(3) . . ?
C6 C7 C8 119.9(3) . . ?
C3 C7 C8 121.2(3) . . ?
C7 C6 C5 120.4(3) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
N1 C8 C7 110.3(3) . . ?
N1 C8 H8A 109.6 . . ?
C7 C8 H8A 109.6 . . ?
N1 C8 H8B 109.6 . . ?
C7 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
O1 C1 O2 124.4(3) . . ?
O1 C1 C2 118.0(3) . . ?
O2 C1 C2 117.6(3) . . ?
N1 C9 C10 120.1(3) . . ?
N1 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C9 C10 C11 120.2(3) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C10 C11 C12 118.4(3) . . ?
C10 C11 C14 120.7(4) . . ?
C12 C11 C14 120.8(3) . . ?
N1 C13 C12 120.3(3) . . ?
N1 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C12 C11 120.1(3) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
O6 C14 O5 128.1(4) . . ?
O6 C14 C11 115.6(4) . . ?
O5 C14 C11 116.3(4) . . ?
N3 C18 N2 111.6(3) . . ?
N3 C18 H18 124.2 . . ?
N2 C18 H18 124.2 . . ?
C17 C16 N3 109.9(3) . . ?
C17 C16 H16 125.1 . . ?
N3 C16 H16 125.1 . . ?
C16 C17 N2 106.3(3) . . ?
C16 C17 H17 126.8 . . ?
N2 C17 H17 126.8 . . ?
N2 C19 C20 112.7(3) . . ?
N2 C19 H19A 109.1 . . ?
C20 C19 H19A 109.1 . . ?
N2 C19 H19B 109.1 . . ?
C20 C19 H19B 109.1 . . ?
H19A C19 H19B 107.8 . . ?
C19 C20 C21 113.5(3) . . ?
C19 C20 H20A 108.9 . . ?
C21 C20 H20A 108.9 . . ?
C19 C20 H20B 108.9 . . ?
C21 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
C22 C21 C20 115.0(3) . . ?
C22 C21 H21A 108.5 . . ?
C20 C21 H21A 108.5 . . ?
C22 C21 H21B 108.5 . . ?
C20 C21 H21B 108.5 . . ?
H21A C21 H21B 107.5 . . ?
N4 C22 C21 111.5(3) . . ?
N4 C22 H22A 109.3 . . ?
C21 C22 H22A 109.3 . . ?
N4 C22 H22B 109.3 . . ?
C21 C22 H22B 109.3 . . ?
H22A C22 H22B 108.0 . . ?
H2WD O2W H2WC 109.5 . . ?
C25 C24 N4 106.4(4) . . ?
C25 C24 H24 126.8 . . ?
N4 C24 H24 126.8 . . ?
C23 N4 C24 106.9(3) . . ?
C23 N4 C22 126.0(3) . . ?
C24 N4 C22 127.1(3) . . ?
N5 C23 N4 111.4(3) . . ?
N5 C23 H23 124.3 . . ?
N4 C23 H23 124.3 . . ?
C23 N5 C25 105.0(3) . . ?
C23 N5 Cd2 126.2(3) . 1_565 ?
C25 N5 Cd2 128.6(2) . 1_565 ?
C24 C25 N5 110.3(3) . . ?
C24 C25 H25 124.8 . . ?
N5 C25 H25 124.8 . . ?
C15 O3 Cd2 101.76(19) . 1_645 ?

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 Cd2 O2 C1 19.7(3) 1_465 . . . ?
N3 Cd2 O2 C1 -86.6(2) . . . . ?
N5 Cd2 O2 C1 -179.0(2) 1_545 . . . ?
O1W Cd2 O2 C1 98.8(2) . . . . ?
O2 Cd2 N3 C18 171.5(3) . . . . ?
O3 Cd2 N3 C18 57.9(3) 1_465 . . . ?
N5 Cd2 N3 C18 -88.2(3) 1_545 . . . ?
O1W Cd2 N3 C18 -120.9(9) . . . . ?
O2 Cd2 N3 C16 -20.3(3) . . . . ?
O3 Cd2 N3 C16 -134.0(3) 1_465 . . . ?
N5 Cd2 N3 C16 79.9(3) 1_545 . . . ?
O1W Cd2 N3 C16 47.2(11) . . . . ?
O4 C15 C5 C4 -4.4(5) . . . . ?
O3 C15 C5 C4 177.8(3) . . . . ?
O4 C15 C5 C6 175.0(3) . . . . ?
O3 C15 C5 C6 -2.8(5) . . . . ?
C6 C5 C4 C2 -1.4(5) . . . . ?
C15 C5 C4 C2 178.1(3) . . . . ?
C5 C4 C2 C3 0.0(5) . . . . ?
C5 C4 C2 C1 179.4(3) . . . . ?
C4 C2 C3 C7 1.1(5) . . . . ?
C1 C2 C3 C7 -178.4(3) . . . . ?
C2 C3 C7 C6 -0.7(5) . . . . ?
C2 C3 C7 C8 178.0(3) . . . . ?
C3 C7 C6 C5 -0.8(5) . . . . ?
C8 C7 C6 C5 -179.4(3) . . . . ?
C4 C5 C6 C7 1.8(5) . . . . ?
C15 C5 C6 C7 -177.7(3) . . . . ?
C13 N1 C8 C7 101.5(3) . . . . ?
C9 N1 C8 C7 -74.6(4) . . . . ?
C6 C7 C8 N1 100.0(3) . . . . ?
C3 C7 C8 N1 -78.6(4) . . . . ?
Cd2 O2 C1 O1 10.6(4) . . . . ?
Cd2 O2 C1 C2 -169.6(2) . . . . ?
C3 C2 C1 O1 -18.5(5) . . . . ?
C4 C2 C1 O1 162.1(3) . . . . ?
C3 C2 C1 O2 161.7(3) . . . . ?
C4 C2 C1 O2 -17.8(5) . . . . ?
C13 N1 C9 C10 -1.5(5) . . . . ?
C8 N1 C9 C10 174.5(3) . . . . ?
N1 C9 C10 C11 0.9(5) . . . . ?
C9 C10 C11 C12 1.6(5) . . . . ?
C9 C10 C11 C14 -175.6(3) . . . . ?
C9 N1 C13 C12 -0.3(5) . . . . ?
C8 N1 C13 C12 -176.3(3) . . . . ?
N1 C13 C12 C11 2.8(5) . . . . ?
C10 C11 C12 C13 -3.4(5) . . . . ?
C14 C11 C12 C13 173.7(3) . . . . ?
C10 C11 C14 O6 18.8(5) . . . . ?
C12 C11 C14 O6 -158.2(4) . . . . ?
C10 C11 C14 O5 -160.9(3) . . . . ?
C12 C11 C14 O5 22.1(5) . . . . ?
C16 N3 C18 N2 -0.1(4) . . . . ?
Cd2 N3 C18 N2 170.3(2) . . . . ?
C17 N2 C18 N3 0.8(4) . . . . ?
C19 N2 C18 N3 178.3(3) . . . . ?
C18 N3 C16 C17 -0.5(4) . . . . ?
Cd2 N3 C16 C17 -170.5(2) . . . . ?
N3 C16 C17 N2 1.0(4) . . . . ?
C18 N2 C17 C16 -1.0(4) . . . . ?
C19 N2 C17 C16 -178.5(3) . . . . ?
C18 N2 C19 C20 -89.2(5) . . . . ?
C17 N2 C19 C20 87.8(5) . . . . ?
N2 C19 C20 C21 166.0(3) . . . . ?
C19 C20 C21 C22 -75.8(4) . . . . ?
C20 C21 C22 N4 -59.4(4) . . . . ?
C25 C24 N4 C23 0.9(4) . . . . ?
C25 C24 N4 C22 -176.1(4) . . . . ?
C21 C22 N4 C23 -65.4(5) . . . . ?
C21 C22 N4 C24 111.0(4) . . . . ?
C24 N4 C23 N5 -0.6(4) . . . . ?
C22 N4 C23 N5 176.5(3) . . . . ?
N4 C23 N5 C25 0.1(4) . . . . ?
N4 C23 N5 Cd2 -176.9(2) . . . 1_565 ?
N4 C24 C25 N5 -0.9(5) . . . . ?
C23 N5 C25 C24 0.5(5) . . . . ?
Cd2 N5 C25 C24 177.4(3) 1_565 . . . ?
O4 C15 O3 Cd2 -3.7(4) . . . 1_645 ?
C5 C15 O3 Cd2 174.0(2) . . . 1_645 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.081
####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1400668'
_audit_update_record             
;
2015-06-29 deposited with the CCDC.
2015-07-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H19 Cu N3 O7, 5(H2 O)'
_chemical_formula_sum            'C25 H29 Cu N3 O12'
_chemical_formula_weight         627.05

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           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                   10.1493(5)
_cell_length_b                   11.1061(7)
_cell_length_c                   12.8644(6)
_cell_angle_alpha                109.643(5)
_cell_angle_beta                 101.237(4)
_cell_angle_gamma                94.591(5)
_cell_volume                     1322.76(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             650
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.98979
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9902
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0787
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.88
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4655
_reflns_number_gt                3505
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0413P)²+0.4365P] 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         4655
_refine_ls_number_parameters     370
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0497
_refine_ls_wR_factor_ref         0.1095
_refine_ls_wR_factor_gt          0.1017
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.006
_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
N2 N 0.0289(3) 0.0023(3) 0.2326(3) 0.0214(7) Uani 1 1 d . . .
C23 C 0.0803(4) 0.0422(4) 0.1595(4) 0.0355(11) Uani 1 1 d . . .
H23 H 0.1217 -0.0147 0.1095 0.043 Uiso 1 1 calc R . .
C22 C -0.0331(4) 0.0862(4) 0.3012(3) 0.0302(10) Uani 1 1 d . . .
H22 H -0.0724 0.0597 0.3511 0.036 Uiso 1 1 calc R . .
Cu1 Cu 0.04002(4) 0.82501(4) 0.23724(4) 0.01852(14) Uani 1 1 d . . .
O1W O 0.1084(3) 0.9119(3) 0.4285(2) 0.0355(7) Uani 1 1 d . . .
H1WA H 0.1693 0.8899 0.3946 0.053 Uiso 1 1 d R . .
H1W H 0.1363 0.9895 0.4483 0.053 Uiso 1 1 d R . .
O1 O 0.1834(2) 0.7973(3) 0.1467(2) 0.0252(6) Uani 1 1 d . . .
O5 O 0.7576(3) 0.3932(3) -0.5488(2) 0.0413(8) Uani 1 1 d . . .
O2 O 0.3509(3) 0.8197(3) 0.2959(2) 0.0385(8) Uani 1 1 d . . .
O6 O 0.7859(3) 0.6051(3) -0.5111(3) 0.0498(9) Uani 1 1 d . . .
N1 N 0.0370(3) 0.6444(3) 0.2399(2) 0.0193(7) Uani 1 1 d . . .
N3 N 0.4800(3) 0.5502(4) -0.2671(3) 0.0309(8) Uani 1 1 d . . .
C1 C 0.3053(3) 0.7934(4) 0.1936(3) 0.0240(9) Uani 1 1 d . . .
C16 C 0.0149(3) 0.2525(4) 0.2282(3) 0.0206(8) Uani 1 1 d . . .
C17 C 0.0165(3) 0.3879(4) 0.2309(3) 0.0191(8) Uani 1 1 d . . .
C2 C 0.3979(3) 0.7474(4) 0.1136(3) 0.0222(9) Uani 1 1 d . . .
C11 C 0.6123(4) 0.4213(4) -0.3788(3) 0.0336(10) Uani 1 1 d . . .
H11 H 0.6423 0.3423 -0.4064 0.040 Uiso 1 1 calc R . .
C5 C 0.6269(3) 0.7321(4) 0.0898(3) 0.0219(9) Uani 1 1 d . . .
C6 C 0.5757(3) 0.6629(4) -0.0257(3) 0.0274(10) Uani 1 1 d . . .
H6 H 0.6352 0.6335 -0.0718 0.033 Uiso 1 1 calc R . .
C4 C 0.5388(3) 0.7740(4) 0.1594(3) 0.0214(8) Uani 1 1 d . . .
H4 H 0.5732 0.8199 0.2367 0.026 Uiso 1 1 calc R . .
C10 C 0.5228(4) 0.4372(4) -0.3088(3) 0.0335(10) Uani 1 1 d . . .
H10 H 0.4918 0.3677 -0.2903 0.040 Uiso 1 1 calc R . .
C18 C -0.0118(3) 0.4861(4) 0.3202(3) 0.0222(8) Uani 1 1 d . . .
H18 H -0.0384 0.4675 0.3791 0.027 Uiso 1 1 calc R . .
C14 C 0.6573(3) 0.5247(4) -0.4076(3) 0.0258(9) Uani 1 1 d . . .
C3 C 0.3487(3) 0.6821(4) -0.0017(3) 0.0282(10) Uani 1 1 d . . .
H3 H 0.2556 0.6677 -0.0328 0.034 Uiso 1 1 calc R . .
C20 C -0.0005(3) 0.6112(4) 0.3216(3) 0.0221(9) Uani 1 1 d . . .
H20 H -0.0198 0.6754 0.3823 0.027 Uiso 1 1 calc R . .
C19 C 0.0504(4) 0.4226(4) 0.1433(3) 0.0289(9) Uani 1 1 d . . .
H19 H 0.0660 0.3600 0.0797 0.035 Uiso 1 1 calc R . .
C30 C -0.0416(4) 0.2092(4) 0.3017(3) 0.0287(9) Uani 1 1 d . . .
H30 H -0.0854 0.2636 0.3514 0.034 Uiso 1 1 calc R . .
C13 C 0.6177(4) 0.6430(4) -0.3576(3) 0.0336(10) Uani 1 1 d . . .
H13 H 0.6519 0.7152 -0.3710 0.040 Uiso 1 1 calc R . .
C21 C 0.0605(4) 0.5493(4) 0.1519(3) 0.0261(9) Uani 1 1 d . . .
H21 H 0.0849 0.5706 0.0935 0.031 Uiso 1 1 calc R . .
C15 C 0.7421(4) 0.5060(5) -0.4968(3) 0.0307(10) Uani 1 1 d . . .
C7 C 0.4365(3) 0.6373(4) -0.0727(3) 0.0277(10) Uani 1 1 d . . .
C38 C 0.0746(4) 0.1634(4) 0.1551(4) 0.0357(11) Uani 1 1 d . . .
H38 H 0.1113 0.1862 0.1023 0.043 Uiso 1 1 calc R . .
C12 C 0.5282(4) 0.6546(5) -0.2885(3) 0.0378(11) Uani 1 1 d . . .
H12 H 0.5007 0.7340 -0.2565 0.045 Uiso 1 1 calc R . .
C9 C 0.3767(4) 0.5647(5) -0.1979(3) 0.0404(12) Uani 1 1 d . . .
H9A H 0.3320 0.4794 -0.2086 0.049 Uiso 1 1 calc R . .
H9B H 0.3082 0.6102 -0.2250 0.049 Uiso 1 1 calc R . .
O6W O 0.6898(3) 0.1388(3) 0.4166(3) 0.0595(10) Uani 1 1 d . . .
H6WB H 0.7534 0.1882 0.4716 0.089 Uiso 1 1 d R . .
H6WC H 0.6179 0.1516 0.4313 0.089 Uiso 1 1 d R . .
O2W O 0.4244(3) 0.0848(3) 0.4181(3) 0.0667(10) Uani 1 1 d . . .
H2WB H 0.3484 0.0398 0.3990 0.100 Uiso 1 1 d R . .
H2WA H 0.4242 0.0957 0.4851 0.100 Uiso 1 1 d R . .
O3W O 0.5930(6) 0.0888(5) 0.1716(4) 0.134(2) Uani 1 1 d . . .
H3WD H 0.6280 0.1235 0.1411 0.161 Uiso 1 1 d R . .
H3WB H 0.6531 0.1335 0.2314 0.201 Uiso 1 1 d R . .
O4W O 0.2378(3) 0.1737(3) 0.5552(3) 0.0494(8) Uani 1 1 d . . .
H4WD H 0.2830 0.2218 0.5309 0.074 Uiso 1 1 d R . .
H4WA H 0.2668 0.1965 0.6267 0.074 Uiso 1 1 d R . .
O5W O 0.3226(7) 0.0181(7) 0.0238(6) 0.201(3) Uani 1 1 d . . .
H5WD H 0.3340 0.0462 -0.0198 0.241 Uiso 1 1 d R . .
H5WB H 0.3728 0.0398 0.0810 0.302 Uiso 1 1 d R . .
C8 C 0.7801(3) 0.7636(4) 0.1343(3) 0.0233(9) Uani 1 1 d . . .
O4 O 0.8517(2) 0.7470(3) 0.0648(2) 0.0425(8) Uani 1 1 d . . .
O3 O 0.8302(2) 0.8042(3) 0.2409(2) 0.0243(6) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N2 C23 1.336(4) . ?
N2 C22 1.343(5) . ?
N2 Cu1 2.001(3) 1_545 ?
C23 C38 1.372(5) . ?
C23 H23 0.9300 . ?
C22 C30 1.373(5) . ?
C22 H22 0.9300 . ?
Cu1 N2 2.001(3) 1_565 ?
Cu1 O1 2.015(2) . ?
Cu1 N1 2.015(3) . ?
Cu1 O3 2.135(2) 1_455 ?
Cu1 O1W 2.258(3) . ?
Cu1 H1WA 2.0425 . ?
O1W H1WA 0.8301 . ?
O1W H1W 0.8201 . ?
O1 C1 1.278(4) . ?
O5 C15 1.245(5) . ?
O2 C1 1.230(4) . ?
O6 C15 1.238(5) . ?
N1 C20 1.333(4) . ?
N1 C21 1.341(5) . ?
N3 C10 1.333(5) . ?
N3 C12 1.355(5) . ?
N3 C9 1.487(4) . ?
C1 C2 1.517(5) . ?
C16 C38 1.387(5) . ?
C16 C30 1.388(5) . ?
C16 C17 1.490(5) . ?
C17 C18 1.389(5) . ?
C17 C19 1.400(5) . ?
C2 C3 1.380(5) . ?
C2 C4 1.403(5) . ?
C11 C10 1.380(5) . ?
C11 C14 1.389(5) . ?
C11 H11 0.9300 . ?
C5 C4 1.384(5) . ?
C5 C6 1.392(5) . ?
C5 C8 1.516(5) . ?
C6 C7 1.389(5) . ?
C6 H6 0.9300 . ?
C4 H4 0.9300 . ?
C10 H10 0.9300 . ?
C18 C20 1.379(5) . ?
C18 H18 0.9300 . ?
C14 C13 1.385(6) . ?
C14 C15 1.535(5) . ?
C3 C7 1.399(5) . ?
C3 H3 0.9300 . ?
C20 H20 0.9300 . ?
C19 C21 1.367(5) . ?
C19 H19 0.9300 . ?
C30 H30 0.9300 . ?
C13 C12 1.374(5) . ?
C13 H13 0.9300 . ?
C21 H21 0.9300 . ?
C7 C9 1.510(5) . ?
C38 H38 0.9300 . ?
C12 H12 0.9300 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
O6W H6WB 0.8499 . ?
O6W H6WC 0.8000 . ?
O2W H2WB 0.8299 . ?
O2W H2WA 0.8299 . ?
O3W H3WD 0.7500 . ?
O3W H3WB 0.8501 . ?
O4W H4WD 0.8501 . ?
O4W H4WA 0.8500 . ?
O5W H5WD 0.7501 . ?
O5W H5WB 0.7583 . ?
C8 O4 1.236(4) . ?
C8 O3 1.271(4) . ?
O3 Cu1 2.135(2) 1_655 ?

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
C23 N2 C22 116.6(3) . . ?
C23 N2 Cu1 121.8(3) . 1_545 ?
C22 N2 Cu1 121.6(2) . 1_545 ?
N2 C23 C38 122.8(4) . . ?
N2 C23 H23 118.6 . . ?
C38 C23 H23 118.6 . . ?
N2 C22 C30 123.4(3) . . ?
N2 C22 H22 118.3 . . ?
C30 C22 H22 118.3 . . ?
N2 Cu1 O1 92.50(11) 1_565 . ?
N2 Cu1 N1 176.01(11) 1_565 . ?
O1 Cu1 N1 90.48(11) . . ?
N2 Cu1 O3 89.24(10) 1_565 1_455 ?
O1 Cu1 O3 149.05(10) . 1_455 ?
N1 Cu1 O3 86.84(10) . 1_455 ?
N2 Cu1 O1W 89.66(11) 1_565 . ?
O1 Cu1 O1W 118.29(10) . . ?
N1 Cu1 O1W 91.27(11) . . ?
O3 Cu1 O1W 92.60(9) 1_455 . ?
N2 Cu1 H1WA 94.5 1_565 . ?
O1 Cu1 H1WA 97.1 . . ?
N1 Cu1 H1WA 87.8 . . ?
O3 Cu1 H1WA 113.6 1_455 . ?
O1W Cu1 H1WA 21.5 . . ?
Cu1 O1W H1WA 64.5 . . ?
Cu1 O1W H1W 109.5 . . ?
H1WA O1W H1W 93.6 . . ?
C1 O1 Cu1 120.4(2) . . ?
C20 N1 C21 117.1(3) . . ?
C20 N1 Cu1 122.6(3) . . ?
C21 N1 Cu1 120.0(2) . . ?
C10 N3 C12 120.6(3) . . ?
C10 N3 C9 121.2(4) . . ?
C12 N3 C9 118.3(4) . . ?
O2 C1 O1 125.6(3) . . ?
O2 C1 C2 118.6(3) . . ?
O1 C1 C2 115.8(3) . . ?
C38 C16 C30 115.7(3) . . ?
C38 C16 C17 122.0(3) . . ?
C30 C16 C17 122.2(3) . . ?
C18 C17 C19 116.6(3) . . ?
C18 C17 C16 122.5(3) . . ?
C19 C17 C16 120.9(3) . . ?
C3 C2 C4 119.2(3) . . ?
C3 C2 C1 122.6(3) . . ?
C4 C2 C1 118.2(3) . . ?
C10 C11 C14 119.3(4) . . ?
C10 C11 H11 120.3 . . ?
C14 C11 H11 120.3 . . ?
C4 C5 C6 120.1(3) . . ?
C4 C5 C8 122.0(3) . . ?
C6 C5 C8 117.9(3) . . ?
C7 C6 C5 120.6(3) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C5 C4 C2 120.1(3) . . ?
C5 C4 H4 119.9 . . ?
C2 C4 H4 119.9 . . ?
N3 C10 C11 121.3(4) . . ?
N3 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C20 C18 C17 120.0(3) . . ?
C20 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C13 C14 C11 118.1(4) . . ?
C13 C14 C15 121.1(4) . . ?
C11 C14 C15 120.7(4) . . ?
C2 C3 C7 121.2(3) . . ?
C2 C3 H3 119.4 . . ?
C7 C3 H3 119.4 . . ?
N1 C20 C18 123.1(4) . . ?
N1 C20 H20 118.5 . . ?
C18 C20 H20 118.5 . . ?
C21 C19 C17 119.6(4) . . ?
C21 C19 H19 120.2 . . ?
C17 C19 H19 120.2 . . ?
C22 C30 C16 120.2(4) . . ?
C22 C30 H30 119.9 . . ?
C16 C30 H30 119.9 . . ?
C12 C13 C14 120.6(4) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
N1 C21 C19 123.6(3) . . ?
N1 C21 H21 118.2 . . ?
C19 C21 H21 118.2 . . ?
O5 C15 O6 126.7(4) . . ?
O5 C15 C14 117.1(4) . . ?
O6 C15 C14 116.2(4) . . ?
C6 C7 C3 118.8(3) . . ?
C6 C7 C9 122.4(3) . . ?
C3 C7 C9 118.9(3) . . ?
C23 C38 C16 121.1(3) . . ?
C23 C38 H38 119.5 . . ?
C16 C38 H38 119.5 . . ?
N3 C12 C13 119.9(4) . . ?
N3 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
N3 C9 C7 113.1(3) . . ?
N3 C9 H9A 108.9 . . ?
C7 C9 H9A 108.9 . . ?
N3 C9 H9B 108.9 . . ?
C7 C9 H9B 108.9 . . ?
H9A C9 H9B 107.8 . . ?
H6WB O6W H6WC 109.5 . . ?
H2WB O2W H2WA 88.1 . . ?
H3WD O3W H3WB 87.1 . . ?
H4WD O4W H4WA 109.5 . . ?
H5WD O5W H5WB 120.2 . . ?
O4 C8 O3 122.5(3) . . ?
O4 C8 C5 118.2(3) . . ?
O3 C8 C5 119.3(3) . . ?
C8 O3 Cu1 97.9(2) . 1_655 ?

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
C22 N2 C23 C38 1.7(6) . . . . ?
Cu1 N2 C23 C38 -179.6(3) 1_545 . . . ?
C23 N2 C22 C30 -2.1(6) . . . . ?
Cu1 N2 C22 C30 179.2(3) 1_545 . . . ?
N2 Cu1 O1 C1 110.5(3) 1_565 . . . ?
N1 Cu1 O1 C1 -72.1(3) . . . . ?
O3 Cu1 O1 C1 -156.8(3) 1_455 . . . ?
O1W Cu1 O1 C1 19.6(3) . . . . ?
N2 Cu1 N1 C20 -67.4(18) 1_565 . . . ?
O1 Cu1 N1 C20 154.2(3) . . . . ?
O3 Cu1 N1 C20 -56.7(3) 1_455 . . . ?
O1W Cu1 N1 C20 35.9(3) . . . . ?
N2 Cu1 N1 C21 105.9(17) 1_565 . . . ?
O1 Cu1 N1 C21 -32.4(3) . . . . ?
O3 Cu1 N1 C21 116.7(3) 1_455 . . . ?
O1W Cu1 N1 C21 -150.7(3) . . . . ?
Cu1 O1 C1 O2 -8.7(5) . . . . ?
Cu1 O1 C1 C2 168.9(2) . . . . ?
C38 C16 C17 C18 -163.8(4) . . . . ?
C30 C16 C17 C18 13.6(5) . . . . ?
C38 C16 C17 C19 14.7(5) . . . . ?
C30 C16 C17 C19 -168.0(3) . . . . ?
O2 C1 C2 C3 161.3(4) . . . . ?
O1 C1 C2 C3 -16.5(5) . . . . ?
O2 C1 C2 C4 -19.4(5) . . . . ?
O1 C1 C2 C4 162.8(3) . . . . ?
C4 C5 C6 C7 1.2(6) . . . . ?
C8 C5 C6 C7 -176.4(4) . . . . ?
C6 C5 C4 C2 -0.3(6) . . . . ?
C8 C5 C4 C2 177.2(3) . . . . ?
C3 C2 C4 C5 -1.7(6) . . . . ?
C1 C2 C4 C5 179.0(3) . . . . ?
C12 N3 C10 C11 -2.9(6) . . . . ?
C9 N3 C10 C11 176.0(3) . . . . ?
C14 C11 C10 N3 -0.9(6) . . . . ?
C19 C17 C18 C20 -2.6(5) . . . . ?
C16 C17 C18 C20 176.0(3) . . . . ?
C10 C11 C14 C13 4.7(5) . . . . ?
C10 C11 C14 C15 -172.2(3) . . . . ?
C4 C2 C3 C7 2.8(6) . . . . ?
C1 C2 C3 C7 -178.0(4) . . . . ?
C21 N1 C20 C18 1.9(5) . . . . ?
Cu1 N1 C20 C18 175.4(3) . . . . ?
C17 C18 C20 N1 0.1(5) . . . . ?
C18 C17 C19 C21 3.1(5) . . . . ?
C16 C17 C19 C21 -175.4(3) . . . . ?
N2 C22 C30 C16 0.4(6) . . . . ?
C38 C16 C30 C22 1.7(6) . . . . ?
C17 C16 C30 C22 -175.8(4) . . . . ?
C11 C14 C13 C12 -4.9(6) . . . . ?
C15 C14 C13 C12 172.0(3) . . . . ?
C20 N1 C21 C19 -1.3(5) . . . . ?
Cu1 N1 C21 C19 -175.0(3) . . . . ?
C17 C19 C21 N1 -1.3(6) . . . . ?
C13 C14 C15 O5 -170.4(4) . . . . ?
C11 C14 C15 O5 6.4(5) . . . . ?
C13 C14 C15 O6 8.2(5) . . . . ?
C11 C14 C15 O6 -175.0(4) . . . . ?
C5 C6 C7 C3 -0.2(6) . . . . ?
C5 C6 C7 C9 178.8(4) . . . . ?
C2 C3 C7 C6 -1.9(6) . . . . ?
C2 C3 C7 C9 179.1(4) . . . . ?
N2 C23 C38 C16 0.4(7) . . . . ?
C30 C16 C38 C23 -2.1(6) . . . . ?
C17 C16 C38 C23 175.4(4) . . . . ?
C10 N3 C12 C13 2.7(6) . . . . ?
C9 N3 C12 C13 -176.2(3) . . . . ?
C14 C13 C12 N3 1.3(6) . . . . ?
C10 N3 C9 C7 105.3(4) . . . . ?
C12 N3 C9 C7 -75.8(5) . . . . ?
C6 C7 C9 N3 -12.7(6) . . . . ?
C3 C7 C9 N3 166.3(4) . . . . ?
C4 C5 C8 O4 -165.2(4) . . . . ?
C6 C5 C8 O4 12.3(5) . . . . ?
C4 C5 C8 O3 15.8(6) . . . . ?
C6 C5 C8 O3 -166.6(4) . . . . ?
O4 C8 O3 Cu1 0.7(4) . . . 1_655 ?
C5 C8 O3 Cu1 179.7(3) . . . 1_655 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.445
_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_7
_database_code_depnum_ccdc_archive 'CCDC 1400669'
_audit_update_record             
;
2015-06-29 deposited with the CCDC.
2015-07-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H19 Cu N3 O6, 6(H2 O)'
_chemical_formula_sum            'C27 H31 Cu N3 O12'
_chemical_formula_weight         653.09

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           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                   10.0801(3)
_cell_length_b                   10.8210(5)
_cell_length_c                   13.4386(6)
_cell_angle_alpha                95.194(4)
_cell_angle_beta                 92.144(3)
_cell_angle_gamma                92.391(3)
_cell_volume                     1457.30(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             678
_exptl_absorpt_coefficient_mu    0.818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8342
_exptl_absorpt_correction_T_max  0.8535
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10878
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5109
_reflns_number_gt                4355
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1683P)²+7.7030P] 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         5109
_refine_ls_number_parameters     364
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0892
_refine_ls_wR_factor_ref         0.2718
_refine_ls_wR_factor_gt          0.2601
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.075
_refine_ls_shift/su_mean         0.002

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 0.12625(6) 0.36371(7) -0.04330(5) 0.0184(3) Uani 1 1 d . . .
O1 O 0.1876(4) 0.5723(4) -0.0325(4) 0.0295(10) Uani 1 1 d . . .
O2 O 0.0563(4) 0.7029(5) 0.0503(3) 0.0318(11) Uani 1 1 d . . .
O3 O 0.7517(4) 0.8536(5) 0.0634(4) 0.0351(11) Uani 1 1 d . . .
O4 O 0.6786(4) 0.6570(4) 0.0497(3) 0.0254(10) Uani 1 1 d . . .
O6 O 0.3397(12) 1.0891(12) 0.6458(7) 0.120(4) Uani 1 1 d . . .
O5 O 0.1592(10) 0.9720(10) 0.5992(7) 0.102(3) Uani 1 1 d . . .
N2 N 0.1381(5) 0.3675(5) 0.1077(4) 0.0223(11) Uani 1 1 d . . .
N1 N 0.3110(6) 1.0900(5) 0.2741(5) 0.0339(13) Uani 1 1 d . . .
C16 C 0.2363(7) 0.4364(7) 0.1607(5) 0.0374(17) Uani 1 1 d . . .
H16 H 0.2996 0.4788 0.1264 0.045 Uiso 1 1 calc R . .
C20 C 0.0502(6) 0.3063(7) 0.1595(5) 0.0296(14) Uani 1 1 d . . .
H20 H -0.0166 0.2565 0.1244 0.035 Uiso 1 1 calc R . .
C19 C 0.0543(7) 0.3138(8) 0.2623(5) 0.0371(17) Uani 1 1 d . . .
H19 H -0.0091 0.2699 0.2954 0.045 Uiso 1 1 calc R . .
C17 C 0.2454(8) 0.4458(8) 0.2626(5) 0.0437(19) Uani 1 1 d . . .
H17 H 0.3154 0.4931 0.2959 0.052 Uiso 1 1 calc R . .
C1 C 0.1670(5) 0.6692(6) 0.0191(4) 0.0209(12) Uani 1 1 d . . .
C3 C 0.2825(6) 0.7614(6) 0.0501(4) 0.0208(12) Uani 1 1 d . . .
C4 C 0.4135(6) 0.7265(6) 0.0405(4) 0.0197(12) Uani 1 1 d . . .
H4 H 0.4305 0.6467 0.0137 0.024 Uiso 1 1 calc R . .
C5 C 0.5181(6) 0.8097(6) 0.0707(5) 0.0217(12) Uani 1 1 d . . .
C6 C 0.4932(6) 0.9302(6) 0.1095(5) 0.0259(13) Uani 1 1 d . . .
H6 H 0.5634 0.9866 0.1292 0.031 Uiso 1 1 calc R . .
C7 C 0.3619(6) 0.9658(6) 0.1187(5) 0.0253(13) Uani 1 1 d . . .
C8 C 0.2579(6) 0.8817(6) 0.0880(5) 0.0241(13) Uani 1 1 d . . .
H8 H 0.1708 0.9060 0.0927 0.029 Uiso 1 1 calc R . .
C18 C 0.1538(7) 0.3872(7) 0.3172(5) 0.0345(16) Uani 1 1 d . . .
C9 C 0.3350(7) 1.0936(6) 0.1666(6) 0.0343(16) Uani 1 1 d . . .
H9A H 0.4106 1.1499 0.1587 0.041 Uiso 1 1 calc R . .
H9B H 0.2580 1.1248 0.1333 0.041 Uiso 1 1 calc R . .
C2 C 0.6603(6) 0.7727(6) 0.0613(4) 0.0224(13) Uani 1 1 d . . .
C10 C 0.4120(8) 1.1159(8) 0.3415(7) 0.048(2) Uani 1 1 d . . .
H10 H 0.4941 1.1436 0.3207 0.058 Uiso 1 1 calc R . .
C11 C 0.3957(9) 1.1020(9) 0.4420(7) 0.056(2) Uani 1 1 d . . .
H11 H 0.4668 1.1189 0.4881 0.067 Uiso 1 1 calc R . .
C13 C 0.1712(10) 1.0402(9) 0.4021(7) 0.059(2) Uani 1 1 d . . .
H13 H 0.0878 1.0144 0.4216 0.070 Uiso 1 1 calc R . .
C14 C 0.1902(8) 1.0548(8) 0.3044(6) 0.0441(19) Uani 1 1 d . . .
H14 H 0.1193 1.0405 0.2579 0.053 Uiso 1 1 calc R . .
C12 C 0.2740(9) 1.0631(8) 0.4729(7) 0.050(2) Uani 1 1 d . . .
C15 C 0.2529(13) 1.0396(12) 0.5839(9) 0.074(3) Uani 1 1 d . . .
O2W O 0.5428(11) 0.4943(10) 0.1739(7) 0.108 Uani 1 1 d D . .
H2WB H 0.5833 0.5418 0.1368 0.130 Uiso 1 1 d RD . .
H2WA H 0.540(16) 0.419(3) 0.148(7) 0.163 Uiso 1 1 d D . .
O3W O 0.7350(11) 0.2746(9) 0.4133(7) 0.104 Uani 1 1 d D . .
H3WB H 0.7600 0.2788 0.3539 0.155 Uiso 1 1 d RD . .
H3WA H 0.762(12) 0.216(8) 0.445(4) 0.124 Uiso 1 1 d D . .
O4W O 0.6644(9) 0.2490(10) 0.2125(7) 0.101 Uani 1 1 d . . .
H4WA H 0.6875 0.1909 0.1708 0.152 Uiso 1 1 d RD . .
H4WB H 0.6668 0.3171 0.1856 0.122 Uiso 1 1 d RD . .
O5W O 0.8661(11) 0.0512(9) 0.1937(6) 0.121(4) Uani 1 1 d . . .
H5WB H 0.8205 0.0348 0.2431 0.182 Uiso 1 1 d R . .
H5WA H 0.8405 0.0027 0.1426 0.182 Uiso 1 1 d R . .
O6W O 0.5019(10) 0.7038(9) 0.3204(7) 0.105 Uani 1 1 d . . .
H6WA H 0.5575 0.7653 0.3302 0.157 Uiso 1 1 d R . .
H6WB H 0.5181 0.6415 0.2771 0.157 Uiso 1 1 d R . .
O1W O 0.4540(11) 0.6025(10) 0.4936(7) 0.118 Uani 1 1 d . . .
H1WA H 0.3951 0.6393 0.5223 0.177 Uiso 1 1 d R . .
H1WB H 0.4660 0.6342 0.4407 0.177 Uiso 1 1 d R . .
C22 C 0.0829(8) 0.3464(8) 0.4862(5) 0.0421(18) Uani 1 1 d . . .
H22 H 0.0123 0.2972 0.4556 0.051 Uiso 1 1 calc R . .
C21 C 0.1636(9) 0.4003(8) 0.4262(6) 0.0443(19) Uani 1 1 d . . .
H21 H 0.2331 0.4512 0.4563 0.053 Uiso 1 1 calc R . .
C25 C 0.0926(8) 0.3558(7) 0.5959(5) 0.0366(16) Uani 1 1 d . . .
C24 C 0.0204(12) 0.2746(13) 0.6483(7) 0.082(4) Uani 1 1 d . . .
H24 H -0.0362 0.2140 0.6137 0.098 Uiso 1 1 calc R . .
C26 C 0.1683(14) 0.4417(11) 0.6537(7) 0.090(5) Uani 1 1 d . . .
H26 H 0.2153 0.5035 0.6241 0.108 Uiso 1 1 calc R . .
C23 C 0.0306(11) 0.2816(11) 0.7493(6) 0.067(3) Uani 1 1 d . . .
H23 H -0.0219 0.2263 0.7817 0.081 Uiso 1 1 calc R . .
C27 C 0.1770(14) 0.4393(11) 0.7561(7) 0.091(5) Uani 1 1 d . . .
H27 H 0.2348 0.4972 0.7926 0.109 Uiso 1 1 calc R . .
N3 N 0.1102(5) 0.3619(5) 0.8044(4) 0.0269(12) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O2 1.944(4) 2_565 ?
Cu1 O4 1.993(4) 2_665 ?
Cu1 N2 2.025(5) . ?
Cu1 N3 2.045(5) 1_554 ?
Cu1 O1 2.306(4) . ?
O1 C1 1.234(8) . ?
O2 C1 1.262(7) . ?
O2 Cu1 1.944(4) 2_565 ?
O3 C2 1.242(7) . ?
O4 C2 1.269(8) . ?
O4 Cu1 1.993(4) 2_665 ?
O6 C15 1.253(16) . ?
O5 C15 1.206(15) . ?
N2 C20 1.337(8) . ?
N2 C16 1.354(9) . ?
N1 C10 1.341(10) . ?
N1 C14 1.349(10) . ?
N1 C9 1.478(10) . ?
C16 C17 1.364(10) . ?
C16 H16 0.9300 . ?
C20 C19 1.377(10) . ?
C20 H20 0.9300 . ?
C19 C18 1.398(10) . ?
C19 H19 0.9300 . ?
C17 C18 1.370(11) . ?
C17 H17 0.9300 . ?
C1 C3 1.522(8) . ?
C3 C8 1.390(9) . ?
C3 C4 1.396(8) . ?
C4 C5 1.382(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.396(9) . ?
C5 C2 1.511(8) . ?
C6 C7 1.400(9) . ?
C6 H6 0.9300 . ?
C7 C8 1.384(9) . ?
C7 C9 1.511(9) . ?
C8 H8 0.9300 . ?
C18 C21 1.458(10) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.387(13) . ?
C10 H10 0.9300 . ?
C11 C12 1.371(13) . ?
C11 H11 0.9300 . ?
C13 C14 1.356(13) . ?
C13 C12 1.379(14) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C12 C15 1.557(14) . ?
O2W H2WB 0.8499 . ?
O2W H2WA 0.856(10) . ?
O3W H3WB 0.8500 . ?
O3W H3WA 0.849(10) . ?
O4W H4WA 0.8499 . ?
O4W H4WB 0.8500 . ?
O5W H5WB 0.8500 . ?
O5W H5WA 0.8500 . ?
O6W H6WA 0.8497 . ?
O6W H6WB 0.8745 . ?
O1W H1WA 0.8174 . ?
O1W H1WB 0.8275 . ?
C22 C21 1.322(12) . ?
C22 C25 1.469(10) . ?
C22 H22 0.9300 . ?
C21 H21 0.9300 . ?
C25 C26 1.347(12) . ?
C25 C24 1.376(12) . ?
C24 C23 1.352(12) . ?
C24 H24 0.9300 . ?
C26 C27 1.379(13) . ?
C26 H26 0.9300 . ?
C23 N3 1.315(10) . ?
C23 H23 0.9300 . ?
C27 N3 1.288(11) . ?
C27 H27 0.9300 . ?
N3 Cu1 2.045(5) 1_556 ?

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 Cu1 O4 151.8(2) 2_565 2_665 ?
O2 Cu1 N2 92.3(2) 2_565 . ?
O4 Cu1 N2 90.86(19) 2_665 . ?
O2 Cu1 N3 86.8(2) 2_565 1_554 ?
O4 Cu1 N3 90.4(2) 2_665 1_554 ?
N2 Cu1 N3 178.7(2) . 1_554 ?
O2 Cu1 O1 124.62(19) 2_565 . ?
O4 Cu1 O1 83.38(17) 2_665 . ?
N2 Cu1 O1 90.17(19) . . ?
N3 Cu1 O1 89.49(19) 1_554 . ?
C1 O1 Cu1 139.5(4) . . ?
C1 O2 Cu1 137.2(4) . 2_565 ?
C2 O4 Cu1 107.5(4) . 2_665 ?
C20 N2 C16 117.2(6) . . ?
C20 N2 Cu1 122.8(4) . . ?
C16 N2 Cu1 120.0(4) . . ?
C10 N1 C14 119.9(7) . . ?
C10 N1 C9 119.5(6) . . ?
C14 N1 C9 120.6(6) . . ?
N2 C16 C17 122.1(6) . . ?
N2 C16 H16 118.9 . . ?
C17 C16 H16 118.9 . . ?
N2 C20 C19 122.8(6) . . ?
N2 C20 H20 118.6 . . ?
C19 C20 H20 118.6 . . ?
C20 C19 C18 120.0(6) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C16 C17 C18 121.6(7) . . ?
C16 C17 H17 119.2 . . ?
C18 C17 H17 119.2 . . ?
O1 C1 O2 126.5(6) . . ?
O1 C1 C3 119.4(5) . . ?
O2 C1 C3 114.1(5) . . ?
C8 C3 C4 119.5(5) . . ?
C8 C3 C1 120.0(5) . . ?
C4 C3 C1 120.6(5) . . ?
C5 C4 C3 120.4(6) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 120.0(5) . . ?
C4 C5 C2 120.9(5) . . ?
C6 C5 C2 119.1(5) . . ?
C5 C6 C7 119.8(6) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 H6 120.1 . . ?
C8 C7 C6 119.7(6) . . ?
C8 C7 C9 120.6(6) . . ?
C6 C7 C9 119.7(6) . . ?
C7 C8 C3 120.7(5) . . ?
C7 C8 H8 119.7 . . ?
C3 C8 H8 119.7 . . ?
C17 C18 C19 116.1(6) . . ?
C17 C18 C21 120.9(7) . . ?
C19 C18 C21 123.0(7) . . ?
N1 C9 C7 110.9(6) . . ?
N1 C9 H9A 109.5 . . ?
C7 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 108.0 . . ?
O3 C2 O4 123.4(5) . . ?
O3 C2 C5 120.2(6) . . ?
O4 C2 C5 116.4(5) . . ?
N1 C10 C11 120.9(8) . . ?
N1 C10 H10 119.6 . . ?
C11 C10 H10 119.6 . . ?
C12 C11 C10 119.5(9) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C14 C13 C12 120.9(8) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
N1 C14 C13 120.6(8) . . ?
N1 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C11 C12 C13 118.2(9) . . ?
C11 C12 C15 121.3(9) . . ?
C13 C12 C15 120.4(9) . . ?
O5 C15 O6 128.0(12) . . ?
O5 C15 C12 116.5(12) . . ?
O6 C15 C12 115.4(11) . . ?
H2WB O2W H2WA 110.6 . . ?
H3WB O3W H3WA 118.1 . . ?
H4WA O4W H4WB 109.5 . . ?
H5WB O5W H5WA 109.5 . . ?
H6WA O6W H6WB 119.7 . . ?
H1WA O1W H1WB 107.8 . . ?
C21 C22 C25 127.0(8) . . ?
C21 C22 H22 116.5 . . ?
C25 C22 H22 116.5 . . ?
C22 C21 C18 126.0(8) . . ?
C22 C21 H21 117.0 . . ?
C18 C21 H21 117.0 . . ?
C26 C25 C24 114.4(7) . . ?
C26 C25 C22 124.9(7) . . ?
C24 C25 C22 120.7(7) . . ?
C23 C24 C25 121.0(8) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 H24 119.5 . . ?
C25 C26 C27 120.8(8) . . ?
C25 C26 H26 119.6 . . ?
C27 C26 H26 119.6 . . ?
N3 C23 C24 123.9(8) . . ?
N3 C23 H23 118.1 . . ?
C24 C23 H23 118.1 . . ?
N3 C27 C26 124.2(8) . . ?
N3 C27 H27 117.9 . . ?
C26 C27 H27 117.9 . . ?
C27 N3 C23 115.6(7) . . ?
C27 N3 Cu1 122.4(5) . 1_556 ?
C23 N3 Cu1 122.0(5) . 1_556 ?

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
O2 Cu1 O1 C1 53.0(7) 2_565 . . . ?
O4 Cu1 O1 C1 -130.8(6) 2_665 . . . ?
N2 Cu1 O1 C1 -40.0(6) . . . . ?
N3 Cu1 O1 C1 138.8(6) 1_554 . . . ?
O2 Cu1 N2 C20 15.2(5) 2_565 . . . ?
O4 Cu1 N2 C20 -136.8(5) 2_665 . . . ?
N3 Cu1 N2 C20 65(9) 1_554 . . . ?
O1 Cu1 N2 C20 139.9(5) . . . . ?
O2 Cu1 N2 C16 -163.2(5) 2_565 . . . ?
O4 Cu1 N2 C16 44.8(5) 2_665 . . . ?
N3 Cu1 N2 C16 -114(9) 1_554 . . . ?
O1 Cu1 N2 C16 -38.6(5) . . . . ?
C20 N2 C16 C17 -1.1(11) . . . . ?
Cu1 N2 C16 C17 177.4(6) . . . . ?
C16 N2 C20 C19 1.8(10) . . . . ?
Cu1 N2 C20 C19 -176.7(5) . . . . ?
N2 C20 C19 C18 -0.3(11) . . . . ?
N2 C16 C17 C18 -1.1(13) . . . . ?
Cu1 O1 C1 O2 -42.6(10) . . . . ?
Cu1 O1 C1 C3 137.9(5) . . . . ?
Cu1 O2 C1 O1 1.8(11) 2_565 . . . ?
Cu1 O2 C1 C3 -178.7(4) 2_565 . . . ?
O1 C1 C3 C8 165.4(6) . . . . ?
O2 C1 C3 C8 -14.2(8) . . . . ?
O1 C1 C3 C4 -14.4(8) . . . . ?
O2 C1 C3 C4 166.0(5) . . . . ?
C8 C3 C4 C5 1.6(9) . . . . ?
C1 C3 C4 C5 -178.6(5) . . . . ?
C3 C4 C5 C6 -1.0(9) . . . . ?
C3 C4 C5 C2 179.6(5) . . . . ?
C4 C5 C6 C7 0.7(9) . . . . ?
C2 C5 C6 C7 -180.0(6) . . . . ?
C5 C6 C7 C8 -0.9(9) . . . . ?
C5 C6 C7 C9 176.2(6) . . . . ?
C6 C7 C8 C3 1.5(9) . . . . ?
C9 C7 C8 C3 -175.6(6) . . . . ?
C4 C3 C8 C7 -1.8(9) . . . . ?
C1 C3 C8 C7 178.4(6) . . . . ?
C16 C17 C18 C19 2.5(13) . . . . ?
C16 C17 C18 C21 -178.8(8) . . . . ?
C20 C19 C18 C17 -1.8(11) . . . . ?
C20 C19 C18 C21 179.5(7) . . . . ?
C10 N1 C9 C7 94.8(8) . . . . ?
C14 N1 C9 C7 -81.8(8) . . . . ?
C8 C7 C9 N1 82.2(8) . . . . ?
C6 C7 C9 N1 -94.9(7) . . . . ?
Cu1 O4 C2 O3 2.7(7) 2_665 . . . ?
Cu1 O4 C2 C5 -178.5(4) 2_665 . . . ?
C4 C5 C2 O3 161.3(6) . . . . ?
C6 C5 C2 O3 -18.1(9) . . . . ?
C4 C5 C2 O4 -17.6(8) . . . . ?
C6 C5 C2 O4 163.1(6) . . . . ?
C14 N1 C10 C11 2.8(12) . . . . ?
C9 N1 C10 C11 -173.9(8) . . . . ?
N1 C10 C11 C12 -1.1(14) . . . . ?
C10 N1 C14 C13 -2.9(12) . . . . ?
C9 N1 C14 C13 173.8(7) . . . . ?
C12 C13 C14 N1 1.2(14) . . . . ?
C10 C11 C12 C13 -0.6(14) . . . . ?
C10 C11 C12 C15 176.8(9) . . . . ?
C14 C13 C12 C11 0.5(14) . . . . ?
C14 C13 C12 C15 -176.9(9) . . . . ?
C11 C12 C15 O5 -158.2(11) . . . . ?
C13 C12 C15 O5 19.1(15) . . . . ?
C11 C12 C15 O6 18.5(16) . . . . ?
C13 C12 C15 O6 -164.1(11) . . . . ?
C25 C22 C21 C18 178.5(7) . . . . ?
C17 C18 C21 C22 -178.6(9) . . . . ?
C19 C18 C21 C22 0.0(14) . . . . ?
C21 C22 C25 C26 15.1(16) . . . . ?
C21 C22 C25 C24 -165.7(11) . . . . ?
C26 C25 C24 C23 -1.8(18) . . . . ?
C22 C25 C24 C23 178.9(11) . . . . ?
C24 C25 C26 C27 4.4(19) . . . . ?
C22 C25 C26 C27 -176.4(12) . . . . ?
C25 C24 C23 N3 -2(2) . . . . ?
C25 C26 C27 N3 -4(2) . . . . ?
C26 C27 N3 C23 0(2) . . . . ?
C26 C27 N3 Cu1 -179.5(12) . . . 1_556 ?
C24 C23 N3 C27 2.4(18) . . . . ?
C24 C23 N3 Cu1 -177.7(10) . . . 1_556 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.423
_refine_diff_density_min         -3.383
_refine_diff_density_rms         0.176
