# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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 1433428'
_audit_update_record             
;
2016-01-30 deposited with the CCDC.
2016-02-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         {[Cu(en)2(H2O)]2[Nb3W3O19][Cu]2}?OH
_chemical_formula_sum            'C8 H37 Cu4 N8 Na0 Nb3 O22 W3'
_chemical_formula_weight         1681.90

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'
Na Na 0.0362 0.0249 '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'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pnnm

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

_cell_length_a                   11.2042(13)
_cell_length_b                   14.7102(17)
_cell_length_c                   9.5638(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1576.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5033
_cell_measurement_theta_min      2.540
_cell_measurement_theta_max      25.556

_exptl_crystal_description       block
_exptl_crystal_colour            Purple
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1556
_exptl_absorpt_coefficient_mu    14.680
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6458
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'mercury CCD'
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            5807
_diffrn_reflns_av_R_equivalents  0.0149
_diffrn_reflns_av_sigmaI/netI    0.0146
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.28
_diffrn_reflns_theta_max         25.06
_reflns_number_total             1477
_reflns_number_gt                1470
_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. 

In the structure, the thermal motions of oxygens O2, O3 and O6 from polyoxoanion deviate from normal range, so instruction ISOR was applied for their vibration and thermal restraints.

isor 0.005 o2 o6 o3
;

_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)+(0.0389P)²+119.2780P] 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         1477
_refine_ls_number_parameters     118
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_ref         0.1525
_refine_ls_wR_factor_gt          0.1317
_refine_ls_goodness_of_fit_ref   1.357
_refine_ls_restrained_S_all      1.349
_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
Nb1 Nb 0.63145(8) 0.05426(6) 0.17223(10) 0.0121(3) Uani 0.60 1 d P . .
W1 W 0.63145(8) 0.05426(6) 0.17223(10) 0.0121(3) Uani 0.40 1 d P . .
Nb2 Nb 0.39937(10) 0.13947(7) 0.0000 0.0151(3) Uani 0.30 2 d SP . .
W2 W 0.39937(10) 0.13947(7) 0.0000 0.0151(3) Uani 0.70 2 d SP . .
Cu1 Cu 0.8141(2) 0.26318(19) 0.0000 0.0138(6) Uani 1 2 d S . .
Cu2 Cu 0.7415(4) 0.1223(3) 0.5000 0.0429(10) Uani 1 2 d S . .
O1 O 0.7312(11) 0.0943(9) 0.3033(13) 0.024(3) Uani 1 1 d . . .
O2 O 0.5000 0.0000 0.0000 0.006(4) Uani 1 4 d SU . .
O3 O 0.3287(18) 0.2422(13) 0.0000 0.030(4) Uani 1 2 d SU . .
O4 O 0.7139(15) 0.0898(10) 0.0000 0.015(3) Uani 1 2 d S . .
O5 O 0.5225(9) 0.1566(7) 0.1421(11) 0.012(2) Uani 1 1 d . . .
O6 O 0.3105(8) 0.0703(7) 0.1405(11) 0.008(2) Uani 1 1 d U . .
O7 O 0.5000 0.0000 0.2819(15) 0.011(3) Uani 1 2 d S . .
O1W O 0.944(2) 0.3859(13) 0.0000 0.038(6) Uani 1 2 d S . .
N1 N 0.9176(12) 0.2032(10) 0.1439(14) 0.018(3) Uani 1 1 d . . .
H1A H 0.9500 0.2456 0.2002 0.021 Uiso 1 1 calc R . .
H1B H 0.8734 0.1655 0.1968 0.021 Uiso 1 1 calc R . .
N2 N 0.6983(13) 0.3150(9) 0.1412(15) 0.017(3) Uani 1 1 d . . .
H2A H 0.6576 0.2693 0.1815 0.020 Uiso 1 1 calc R . .
H2B H 0.7394 0.3441 0.2086 0.020 Uiso 1 1 calc R . .
C1 C 1.017(3) 0.149(2) 0.070(2) 0.071(10) Uani 1 1 d . . .
H1C H 1.0124 0.0873 0.1012 0.086 Uiso 1 1 d R . .
H1D H 1.0926 0.1728 0.1012 0.086 Uiso 1 1 d R . .
C2 C 0.612(3) 0.380(2) 0.075(2) 0.063(9) Uani 1 1 d . . .
H2C H 0.6292 0.4404 0.1069 0.075 Uiso 1 1 d R . .
H2D H 0.5333 0.3645 0.1069 0.075 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
Nb1 O1 1.780(12) . ?
Nb1 O4 1.960(9) . ?
Nb1 O5 1.960(10) . ?
Nb1 O6 1.967(10) 2_655 ?
Nb1 O7 1.976(8) . ?
Nb1 O2 2.3494(9) . ?
Nb1 W1 3.2944(19) 6 ?
Nb1 Nb1 3.2944(19) 6 ?
Nb1 Nb2 3.3096(13) 5_655 ?
Nb1 Nb2 3.3236(14) . ?
Nb1 Nb1 3.3504(18) 2_655 ?
Nb2 O3 1.706(19) . ?
Nb2 O5 1.952(10) . ?
Nb2 O5 1.952(10) 6 ?
Nb2 O6 1.958(10) 6 ?
Nb2 O6 1.958(10) . ?
Nb2 O2 2.3410(11) . ?
Nb2 Nb1 3.3096(13) 5_655 ?
Nb2 Nb1 3.3096(13) 2_655 ?
Nb2 Nb1 3.3236(14) 6 ?
Cu1 N1 2.004(14) 6 ?
Cu1 N1 2.004(14) . ?
Cu1 N2 2.022(14) 6 ?
Cu1 N2 2.022(14) . ?
Cu1 O1W 2.318(18) . ?
Cu2 O1 1.929(12) . ?
Cu2 O1 1.929(12) 6_556 ?
Cu2 O3 2.22(2) 7_666 ?
O2 W2 2.3410(11) 5_655 ?
O2 Nb2 2.3410(11) 5_655 ?
O2 W1 2.3494(9) 5_655 ?
O2 Nb1 2.3494(9) 5_655 ?
O2 Nb1 2.3494(9) 2_655 ?
O2 W1 2.3494(9) 2_655 ?
O2 Nb1 2.3494(9) 6 ?
O2 W1 2.3494(9) 6 ?
O3 Cu2 2.22(2) 7_565 ?
O4 W1 1.960(9) 6 ?
O4 Nb1 1.960(9) 6 ?
O6 W1 1.967(10) 2_655 ?
O6 Nb1 1.967(10) 2_655 ?
O7 W1 1.976(8) 2_655 ?
O7 Nb1 1.976(8) 2_655 ?
N1 C1 1.54(3) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C2 1.50(3) . ?
N2 H2A 0.9000 . ?
N2 H2B 0.9000 . ?
C1 C1 1.34(4) 6 ?
C1 H1C 0.9599 . ?
C1 H1D 0.9599 . ?
C2 C2 1.43(4) 6 ?
C2 H2C 0.9599 . ?
C2 H2D 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Nb1 O4 102.0(5) . . ?
O1 Nb1 O5 103.9(5) . . ?
O4 Nb1 O5 88.0(6) . . ?
O1 Nb1 O6 102.1(5) . 2_655 ?
O4 Nb1 O6 87.9(5) . 2_655 ?
O5 Nb1 O6 154.0(4) . 2_655 ?
O1 Nb1 O7 103.2(5) . . ?
O4 Nb1 O7 154.8(5) . . ?
O5 Nb1 O7 85.7(3) . . ?
O6 Nb1 O7 87.3(3) 2_655 . ?
O1 Nb1 O2 179.5(4) . . ?
O4 Nb1 O2 78.3(4) . . ?
O5 Nb1 O2 76.5(3) . . ?
O6 Nb1 O2 77.5(3) 2_655 . ?
O7 Nb1 O2 76.6(4) . . ?
O1 Nb1 W1 134.8(4) . 6 ?
O4 Nb1 W1 32.8(4) . 6 ?
O5 Nb1 W1 81.5(3) . 6 ?
O6 Nb1 W1 81.1(3) 2_655 6 ?
O7 Nb1 W1 122.0(4) . 6 ?
O2 Nb1 W1 45.48(2) . 6 ?
O1 Nb1 Nb1 134.8(4) . 6 ?
O4 Nb1 Nb1 32.8(4) . 6 ?
O5 Nb1 Nb1 81.5(3) . 6 ?
O6 Nb1 Nb1 81.1(3) 2_655 6 ?
O7 Nb1 Nb1 122.0(4) . 6 ?
O2 Nb1 Nb1 45.48(2) . 6 ?
W1 Nb1 Nb1 0.0 6 6 ?
O1 Nb1 Nb2 134.5(4) . 5_655 ?
O4 Nb1 Nb2 82.0(4) . 5_655 ?
O5 Nb1 Nb2 121.6(3) . 5_655 ?
O6 Nb1 Nb2 32.4(3) 2_655 5_655 ?
O7 Nb1 Nb2 80.7(2) . 5_655 ?
O2 Nb1 Nb2 45.02(2) . 5_655 ?
W1 Nb1 Nb2 60.152(19) 6 5_655 ?
Nb1 Nb1 Nb2 60.152(19) 6 5_655 ?
O1 Nb1 Nb2 135.7(4) . . ?
O4 Nb1 Nb2 81.5(4) . . ?
O5 Nb1 Nb2 31.8(3) . . ?
O6 Nb1 Nb2 122.2(3) 2_655 . ?
O7 Nb1 Nb2 80.3(2) . . ?
O2 Nb1 Nb2 44.78(2) . . ?
W1 Nb1 Nb2 60.290(19) 6 . ?
Nb1 Nb1 Nb2 60.290(19) 6 . ?
Nb2 Nb1 Nb2 89.79(3) 5_655 . ?
O1 Nb1 Nb1 135.2(4) . 2_655 ?
O4 Nb1 Nb1 122.8(4) . 2_655 ?
O5 Nb1 Nb1 79.5(3) . 2_655 ?
O6 Nb1 Nb1 81.2(3) 2_655 2_655 ?
O7 Nb1 Nb1 32.0(4) . 2_655 ?
O2 Nb1 Nb1 44.52(2) . 2_655 ?
W1 Nb1 Nb1 90.0 6 2_655 ?
Nb1 Nb1 Nb1 90.0 6 2_655 ?
Nb2 Nb1 Nb1 59.87(3) 5_655 2_655 ?
Nb2 Nb1 Nb1 59.46(3) . 2_655 ?
O3 Nb2 O5 102.3(6) . . ?
O3 Nb2 O5 102.3(6) . 6 ?
O5 Nb2 O5 88.2(6) . 6 ?
O3 Nb2 O6 103.0(6) . 6 ?
O5 Nb2 O6 154.7(4) . 6 ?
O5 Nb2 O6 87.1(4) 6 6 ?
O3 Nb2 O6 103.0(6) . . ?
O5 Nb2 O6 87.1(4) . . ?
O5 Nb2 O6 154.7(4) 6 . ?
O6 Nb2 O6 86.7(6) 6 . ?
O3 Nb2 O2 178.8(7) . . ?
O5 Nb2 O2 76.9(3) . . ?
O5 Nb2 O2 76.9(3) 6 . ?
O6 Nb2 O2 77.8(3) 6 . ?
O6 Nb2 O2 77.8(3) . . ?
O3 Nb2 Nb1 135.6(5) . 5_655 ?
O5 Nb2 Nb1 122.1(3) . 5_655 ?
O5 Nb2 Nb1 80.7(3) 6 5_655 ?
O6 Nb2 Nb1 32.6(3) 6 5_655 ?
O6 Nb2 Nb1 80.8(3) . 5_655 ?
O2 Nb2 Nb1 45.22(2) . 5_655 ?
O3 Nb2 Nb1 135.6(5) . 2_655 ?
O5 Nb2 Nb1 80.7(3) . 2_655 ?
O5 Nb2 Nb1 122.1(3) 6 2_655 ?
O6 Nb2 Nb1 80.8(3) 6 2_655 ?
O6 Nb2 Nb1 32.6(3) . 2_655 ?
O2 Nb2 Nb1 45.22(2) . 2_655 ?
Nb1 Nb2 Nb1 59.70(4) 5_655 2_655 ?
O3 Nb2 Nb1 134.2(5) . . ?
O5 Nb2 Nb1 31.9(3) . . ?
O5 Nb2 Nb1 80.9(3) 6 . ?
O6 Nb2 Nb1 122.8(3) 6 . ?
O6 Nb2 Nb1 82.1(3) . . ?
O2 Nb2 Nb1 44.98(2) . . ?
Nb1 Nb2 Nb1 90.21(3) 5_655 . ?
Nb1 Nb2 Nb1 60.68(3) 2_655 . ?
O3 Nb2 Nb1 134.2(5) . 6 ?
O5 Nb2 Nb1 80.9(3) . 6 ?
O5 Nb2 Nb1 31.9(3) 6 6 ?
O6 Nb2 Nb1 82.1(3) 6 6 ?
O6 Nb2 Nb1 122.8(3) . 6 ?
O2 Nb2 Nb1 44.98(2) . 6 ?
Nb1 Nb2 Nb1 60.68(3) 5_655 6 ?
Nb1 Nb2 Nb1 90.21(3) 2_655 6 ?
Nb1 Nb2 Nb1 59.42(4) . 6 ?
N1 Cu1 N1 86.7(8) 6 . ?
N1 Cu1 N2 94.5(6) 6 6 ?
N1 Cu1 N2 174.8(6) . 6 ?
N1 Cu1 N2 174.8(6) 6 . ?
N1 Cu1 N2 94.5(6) . . ?
N2 Cu1 N2 83.8(8) 6 . ?
N1 Cu1 O1W 88.9(6) 6 . ?
N1 Cu1 O1W 88.9(6) . . ?
N2 Cu1 O1W 96.2(6) 6 . ?
N2 Cu1 O1W 96.2(6) . . ?
O1 Cu2 O1 154.4(8) . 6_556 ?
O1 Cu2 O3 102.6(4) . 7_666 ?
O1 Cu2 O3 102.6(4) 6_556 7_666 ?
Nb1 O1 Cu2 142.6(7) . . ?
Nb2 O2 W2 180.00(5) . 5_655 ?
Nb2 O2 Nb2 180.00(5) . 5_655 ?
W2 O2 Nb2 0.00(5) 5_655 5_655 ?
Nb2 O2 W1 89.76(3) . 5_655 ?
W2 O2 W1 90.24(3) 5_655 5_655 ?
Nb2 O2 W1 90.24(3) 5_655 5_655 ?
Nb2 O2 Nb1 89.76(3) . 5_655 ?
W2 O2 Nb1 90.24(3) 5_655 5_655 ?
Nb2 O2 Nb1 90.24(3) 5_655 5_655 ?
W1 O2 Nb1 0.00(6) 5_655 5_655 ?
Nb2 O2 Nb1 90.24(3) . . ?
W2 O2 Nb1 89.76(3) 5_655 . ?
Nb2 O2 Nb1 89.76(3) 5_655 . ?
W1 O2 Nb1 180.00(6) 5_655 . ?
Nb1 O2 Nb1 180.00(6) 5_655 . ?
Nb2 O2 Nb1 89.76(3) . 2_655 ?
W2 O2 Nb1 90.24(3) 5_655 2_655 ?
Nb2 O2 Nb1 90.24(3) 5_655 2_655 ?
W1 O2 Nb1 89.03(5) 5_655 2_655 ?
Nb1 O2 Nb1 89.03(5) 5_655 2_655 ?
Nb1 O2 Nb1 90.97(5) . 2_655 ?
Nb2 O2 W1 89.76(3) . 2_655 ?
W2 O2 W1 90.24(3) 5_655 2_655 ?
Nb2 O2 W1 90.24(3) 5_655 2_655 ?
W1 O2 W1 89.03(5) 5_655 2_655 ?
Nb1 O2 W1 89.03(5) 5_655 2_655 ?
Nb1 O2 W1 90.97(5) . 2_655 ?
Nb1 O2 W1 0.00(6) 2_655 2_655 ?
Nb2 O2 Nb1 90.24(3) . 6 ?
W2 O2 Nb1 89.76(3) 5_655 6 ?
Nb2 O2 Nb1 89.76(3) 5_655 6 ?
W1 O2 Nb1 90.97(5) 5_655 6 ?
Nb1 O2 Nb1 90.97(5) 5_655 6 ?
Nb1 O2 Nb1 89.03(5) . 6 ?
Nb1 O2 Nb1 180.00(5) 2_655 6 ?
W1 O2 Nb1 180.00(5) 2_655 6 ?
Nb2 O2 W1 90.24(3) . 6 ?
W2 O2 W1 89.76(3) 5_655 6 ?
Nb2 O2 W1 89.76(3) 5_655 6 ?
W1 O2 W1 90.97(5) 5_655 6 ?
Nb1 O2 W1 90.97(5) 5_655 6 ?
Nb1 O2 W1 89.03(5) . 6 ?
Nb1 O2 W1 180.00(5) 2_655 6 ?
W1 O2 W1 180.00(5) 2_655 6 ?
Nb1 O2 W1 0.00(6) 6 6 ?
Nb2 O3 Cu2 178.5(12) . 7_565 ?
W1 O4 Nb1 0.00(7) 6 6 ?
W1 O4 Nb1 114.4(8) 6 . ?
Nb1 O4 Nb1 114.4(8) 6 . ?
Nb2 O5 Nb1 116.3(5) . . ?
Nb2 O6 W1 114.9(5) . 2_655 ?
Nb2 O6 Nb1 114.9(5) . 2_655 ?
W1 O6 Nb1 0.00(8) 2_655 2_655 ?
W1 O7 Nb1 0.00(7) 2_655 2_655 ?
W1 O7 Nb1 115.9(7) 2_655 . ?
Nb1 O7 Nb1 115.9(7) 2_655 . ?
C1 N1 Cu1 109.4(11) . . ?
C1 N1 H1A 109.8 . . ?
Cu1 N1 H1A 109.8 . . ?
C1 N1 H1B 109.8 . . ?
Cu1 N1 H1B 109.8 . . ?
H1A N1 H1B 108.2 . . ?
C2 N2 Cu1 111.9(12) . . ?
C2 N2 H2A 109.2 . . ?
Cu1 N2 H2A 109.2 . . ?
C2 N2 H2B 109.2 . . ?
Cu1 N2 H2B 109.2 . . ?
H2A N2 H2B 107.9 . . ?
C1 C1 N1 117.2(10) 6 . ?
C1 C1 H1C 108.0 6 . ?
N1 C1 H1C 107.8 . . ?
C1 C1 H1D 108.0 6 . ?
N1 C1 H1D 108.0 . . ?
H1C C1 H1D 107.3 . . ?
C2 C2 N2 115.0(10) 6 . ?
C2 C2 H2C 108.5 6 . ?
N2 C2 H2C 109.1 . . ?
C2 C2 H2D 108.5 6 . ?
N2 C2 H2D 107.9 . . ?
H2C C2 H2D 107.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2A O5 0.90 2.28 3.051(17) 144.2 .
N2 H2B O6 0.90 2.07 2.964(17) 169.4 4
N2 H2B O5 0.90 3.48 4.203(18) 139.4 4
N1 H1B O1 0.90 2.16 3.042(18) 165.9 .

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.06
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.686
_refine_diff_density_min         -2.907
_refine_diff_density_rms         0.460
