# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_xb7708_0m
_database_code_depnum_ccdc_archive 'CCDC 1405731'
_audit_update_record             
;
2015-06-18 deposited with the CCDC.
2017-01-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H9 Cu N5 O7'
_chemical_formula_weight         374.76

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

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

_cell_length_a                   7.996(2)
_cell_length_b                   8.629(2)
_cell_length_c                   10.973(3)
_cell_angle_alpha                94.860(5)
_cell_angle_beta                 98.907(5)
_cell_angle_gamma                101.907(5)
_cell_volume                     726.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             378
_exptl_absorpt_coefficient_mu    1.549
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.7471
_exptl_absorpt_correction_T_max  0.8606
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         no
_diffrn_standards_interval_count no
_diffrn_standards_interval_time  'no standards in IP'
_diffrn_standards_decay_%        no
_diffrn_reflns_number            3542
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0836
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2516
_reflns_number_gt                1815
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1225P)²+0.0200P] 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         2516
_refine_ls_number_parameters     208
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0686
_refine_ls_wR_factor_ref         0.1991
_refine_ls_wR_factor_gt          0.1798
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.026
_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
O4 O 0.2037(3) 1.1726(3) 0.1441(2) 0.0396(8) Uani 1 1 d . . .
Cu1 Cu -0.09113(5) 0.86625(5) 0.03107(4) 0.02615(12) Uani 1 1 d . . .
O1 O 0.0982(3) 0.7714(3) -0.0175(2) 0.0324(7) Uani 1 1 d . . .
N2 N 0.2286(4) 0.3548(3) -0.0822(3) 0.0312(7) Uani 1 1 d U . .
O2 O 0.2540(3) 1.0001(3) -0.0627(3) 0.0364(7) Uani 1 1 d . . .
O3 O 0.0486(4) 0.9485(3) 0.1954(3) 0.0415(8) Uani 1 1 d . . .
N4 N 0.3218(4) 0.6018(3) -0.0960(3) 0.0302(6) Uani 1 1 d U . .
C3 C 0.2264(4) 0.8546(4) -0.0513(3) 0.0272(10) Uani 1 1 d . . .
C9 C 0.2160(6) 1.0216(5) 0.4429(4) 0.0427(12) Uani 1 1 d . . .
H9 H 0.1235 0.9333 0.4233 0.051 Uiso 1 1 calc R . .
C10 C 0.1602(5) 1.0758(5) 0.2195(4) 0.0345(11) Uani 1 1 d . . .
C5 C 0.3933(5) 1.2493(5) 0.3817(4) 0.0405(12) Uani 1 1 d . . .
H5 H 0.4206 1.3152 0.3214 0.049 Uiso 1 1 calc R . .
C6 C 0.4887(6) 1.2845(5) 0.5003(4) 0.0430(13) Uani 1 1 d . . .
H6 H 0.5806 1.3733 0.5210 0.052 Uiso 1 1 calc R . .
C8 C 0.3089(6) 1.0555(6) 0.5607(4) 0.0513(14) Uani 1 1 d . . .
H8 H 0.2803 0.9916 0.6218 0.062 Uiso 1 1 calc R . .
N3 N 0.2587(5) 0.4986(4) -0.0237(3) 0.0489(9) Uani 1 1 d U . .
O5 O 0.5330(5) 1.1138(5) 0.7829(3) 0.0711(12) Uani 1 1 d . . .
C2 C 0.3726(5) 0.7754(4) -0.0804(4) 0.0336(10) Uani 1 1 d . . .
H2A H 0.4083 0.8106 -0.1560 0.040 Uiso 1 1 calc R . .
H2B H 0.4716 0.8101 -0.0135 0.040 Uiso 1 1 calc R . .
C4 C 0.2581(5) 1.1175(5) 0.3518(4) 0.0340(11) Uani 1 1 d . . .
C1 C 0.3317(5) 0.5209(5) -0.2008(4) 0.0376(4) Uani 1 1 d U . .
H1 H 0.3719 0.5637 -0.2686 0.045 Uiso 1 1 calc R . .
N5 N 0.5520(5) 1.2166(5) 0.7121(3) 0.0543(12) Uani 1 1 d . . .
O6 O 0.6561(5) 1.3467(5) 0.7389(3) 0.0812(15) Uani 1 1 d . . .
C7 C 0.4444(6) 1.1852(5) 0.5870(4) 0.0432(12) Uani 1 1 d . . .
N1 N 0.2750(6) 0.3701(5) -0.1924(4) 0.0669(12) Uani 1 1 d U . .
O1W O 0.0138(13) 0.5979(11) 0.5503(13) 0.355(7) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O4 0.0420(15) 0.0352(15) 0.0351(15) 0.0033(12) -0.0015(12) 0.0004(12)
Cu1 0.0267(2) 0.0164(2) 0.0340(2) 0.00331(17) 0.00557(17) 0.00142(16)
O1 0.0307(12) 0.0174(12) 0.0500(15) 0.0055(11) 0.0121(11) 0.0028(10)
N2 0.0336(15) 0.0258(7) 0.0379(16) 0.0099(8) 0.0128(13) 0.0079(12)
O2 0.0360(13) 0.0170(12) 0.0575(17) 0.0044(12) 0.0134(12) 0.0052(10)
O3 0.0412(15) 0.0336(15) 0.0416(15) 0.0023(13) 0.0033(12) -0.0059(13)
N4 0.0323(14) 0.0185(10) 0.0397(8) 0.0041(5) 0.0066(9) 0.0056(9)
C3 0.0294(17) 0.0185(18) 0.0288(19) -0.0036(15) 0.0007(15) 0.0001(15)
C9 0.046(2) 0.037(2) 0.040(2) 0.0020(19) 0.0024(19) 0.0016(19)
C10 0.0300(17) 0.035(2) 0.040(2) 0.0001(18) 0.0079(16) 0.0108(16)
C5 0.042(2) 0.040(2) 0.037(2) 0.0096(18) 0.0062(17) 0.0001(19)
C6 0.048(2) 0.036(2) 0.037(2) -0.0061(19) -0.0003(19) 0.003(2)
C8 0.063(3) 0.059(3) 0.032(2) 0.011(2) 0.012(2) 0.006(2)
N3 0.065(2) 0.0267(8) 0.0484(14) 0.0041(7) 0.0151(14) -0.0089(14)
O5 0.074(2) 0.104(3) 0.0398(17) 0.0223(18) 0.0085(16) 0.026(2)
C2 0.0302(18) 0.0187(18) 0.052(2) 0.0067(16) 0.0126(16) 0.0001(15)
C4 0.0343(19) 0.028(2) 0.036(2) -0.0021(17) 0.0042(16) 0.0036(16)
C1 0.0400(7) 0.0358(5) 0.0369(6) 0.0040(5) 0.0100(5) 0.0059(5)
N5 0.0464(19) 0.079(3) 0.037(2) -0.003(2) -0.0018(17) 0.0249(18)
O6 0.080(3) 0.094(3) 0.050(2) -0.010(2) -0.0134(19) -0.001(2)
C7 0.051(2) 0.047(2) 0.031(2) 0.0001(19) 0.0042(18) 0.013(2)
N1 0.117(3) 0.0340(7) 0.051(2) -0.0051(14) 0.050(2) -0.0033(18)
O1W 0.323(9) 0.290(9) 0.567(17) 0.176(10) 0.170(11) 0.208(7)

_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
O4 C10 1.261(5) . ?
O4 Cu1 1.962(3) 2_575 ?
Cu1 O3 1.958(3) . ?
Cu1 O2 1.959(3) 2_575 ?
Cu1 O4 1.962(3) 2_575 ?
Cu1 O1 1.984(3) . ?
Cu1 N2 2.161(3) 2_565 ?
Cu1 Cu1 2.6652(9) 2_575 ?
O1 C3 1.250(4) . ?
N2 N3 1.305(4) . ?
N2 N1 1.328(5) . ?
N2 Cu1 2.161(3) 2_565 ?
O2 C3 1.250(4) . ?
O2 Cu1 1.959(3) 2_575 ?
O3 C10 1.243(4) . ?
N4 C1 1.316(5) . ?
N4 N3 1.317(5) . ?
N4 C2 1.458(4) . ?
C3 C2 1.530(5) . ?
C9 C8 1.362(6) . ?
C9 C4 1.388(6) . ?
C9 H9 0.9300 . ?
C10 C4 1.514(5) . ?
C5 C4 1.375(5) . ?
C5 C6 1.377(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.372(6) . ?
C6 H6 0.9300 . ?
C8 C7 1.363(6) . ?
C8 H8 0.9300 . ?
O5 N5 1.230(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C1 N1 1.303(6) . ?
C1 H1 0.9300 . ?
N5 O6 1.234(5) . ?
N5 C7 1.474(5) . ?

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
C10 O4 Cu1 121.1(2) . 2_575 ?
O3 Cu1 O2 89.71(12) . 2_575 ?
O3 Cu1 O4 167.43(11) . 2_575 ?
O2 Cu1 O4 88.48(12) 2_575 2_575 ?
O3 Cu1 O1 90.84(12) . . ?
O2 Cu1 O1 167.50(10) 2_575 . ?
O4 Cu1 O1 88.27(12) 2_575 . ?
O3 Cu1 N2 96.81(11) . 2_565 ?
O2 Cu1 N2 98.85(11) 2_575 2_565 ?
O4 Cu1 N2 95.76(11) 2_575 2_565 ?
O1 Cu1 N2 93.49(11) . 2_565 ?
O3 Cu1 Cu1 82.38(8) . 2_575 ?
O2 Cu1 Cu1 83.59(8) 2_575 2_575 ?
O4 Cu1 Cu1 85.05(8) 2_575 2_575 ?
O1 Cu1 Cu1 84.11(7) . 2_575 ?
N2 Cu1 Cu1 177.44(9) 2_565 2_575 ?
C3 O1 Cu1 121.3(2) . . ?
N3 N2 N1 106.7(3) . . ?
N3 N2 Cu1 128.6(3) . 2_565 ?
N1 N2 Cu1 123.9(2) . 2_565 ?
C3 O2 Cu1 123.2(2) . 2_575 ?
C10 O3 Cu1 124.9(3) . . ?
C1 N4 N3 107.8(3) . . ?
C1 N4 C2 119.7(3) . . ?
N3 N4 C2 132.5(3) . . ?
O1 C3 O2 127.7(4) . . ?
O1 C3 C2 118.5(3) . . ?
O2 C3 C2 113.8(3) . . ?
C8 C9 C4 120.7(4) . . ?
C8 C9 H9 119.6 . . ?
C4 C9 H9 119.6 . . ?
O3 C10 O4 126.5(4) . . ?
O3 C10 C4 117.2(4) . . ?
O4 C10 C4 116.3(3) . . ?
C4 C5 C6 120.4(4) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C7 C6 C5 118.2(4) . . ?
C7 C6 H6 120.9 . . ?
C5 C6 H6 120.9 . . ?
C9 C8 C7 118.6(4) . . ?
C9 C8 H8 120.7 . . ?
C7 C8 H8 120.7 . . ?
N2 N3 N4 108.9(3) . . ?
N4 C2 C3 112.9(3) . . ?
N4 C2 H2A 109.0 . . ?
C3 C2 H2A 109.0 . . ?
N4 C2 H2B 109.0 . . ?
C3 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C5 C4 C9 119.4(4) . . ?
C5 C4 C10 119.8(4) . . ?
C9 C4 C10 120.7(3) . . ?
N1 C1 N4 107.6(4) . . ?
N1 C1 H1 126.2 . . ?
N4 C1 H1 126.2 . . ?
O5 N5 O6 124.1(4) . . ?
O5 N5 C7 118.9(4) . . ?
O6 N5 C7 117.0(4) . . ?
C8 C7 C6 122.6(4) . . ?
C8 C7 N5 118.8(4) . . ?
C6 C7 N5 118.6(4) . . ?
C1 N1 N2 109.0(4) . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         1.344
_refine_diff_density_min         -1.050
_refine_diff_density_rms         0.131

# start Validation Reply Form
_vrf_PLAT430_z                   
;
PROBLEM: Short Inter D...A Contact  O1W   ..  O1W   ..  1.89 Ang.
RESPONSE: Because of the disorderd water molecules, the hydrogen atoms 
have not been added.
;
# end Validation Reply Form
