# Electronic Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011


data_global
_journal_name_full               'New J.Chem.'
_journal_coden_cambridge         0440
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
loop_
_publ_author_address
;Laboratorio de Rayos X y Materiales Moleculares
Dpto. F\'isica Fundamental II. Facultad de F\'isica
Universidad de La Laguna
E-38204. La Laguna. Tenerife
Spain
;
_publ_contact_author_address     
;Laboratorio de Rayos X y Materiales Moleculares
Dpto. F\'isica Fundamental II. Facultad de F\'isica
Universidad de La Laguna
E-38204. La Laguna. Tenerife
Spain
;
_publ_contact_author_email       caruiz@ull.es
_publ_contact_author_fax         +34922318320
_publ_contact_author_phone       +34922318300
_publ_contact_author_name        'Professor Catalina Ruiz-Perez'
_publ_author_name                P.C.Ruiz-Perez

data_compound1
_database_code_depnum_ccdc_archive 'CCDC 812329'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'K2, Cu5, 4(C3 H2 N O4), 3(H2 O)'
_chemical_formula_sum            'C12 H14 Cu5 K2 N4 O19'
_chemical_formula_weight         914.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   20.103(4)
_cell_length_b                   18.970(4)
_cell_length_c                   6.3120(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.13(3)
_cell_angle_gamma                90.00
_cell_volume                     2323.6(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1804
_exptl_absorpt_coefficient_mu    5.777
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_correction_T_min  0.36
_exptl_absorpt_correction_T_max  0.38
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.75130
_diffrn_source                   synchrotron
_diffrn_source_type              'ESRF-CRG BM16'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9.6
_diffrn_radiation_detector       'ADSC Q210r CCD (binned mode)'
_diffrn_measurement_device_type  'Single-axis HUBER diffractometer'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17407
_diffrn_reflns_av_R_equivalents  0.1356
_diffrn_reflns_av_sigmaI/netI    0.0783
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.52
_diffrn_reflns_theta_max         29.19
_reflns_number_total             2640
_reflns_number_gt                2387
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'MxCube (ESRF, 2006)'
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1135P)^2^+146.7373P] where P=(Fo^2^+2Fc^2^)/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     SHELXL
_refine_ls_extinction_coef       0.0050(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         2640
_refine_ls_number_parameters     193
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_gt           0.0990
_refine_ls_wR_factor_ref         0.2654
_refine_ls_wR_factor_gt          0.2600
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_restrained_S_all      1.112
_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
C1 C 0.4663(6) 0.2939(6) 0.476(2) 0.026(2) Uani 1 1 d . . .
C2 C 0.3977(5) 0.2543(6) 0.398(2) 0.025(2) Uani 1 1 d . . .
H2A H 0.3654 0.2767 0.4674 0.029 Uiso 1 1 calc R . .
H2B H 0.3808 0.2630 0.2416 0.029 Uiso 1 1 calc R . .
C3 C 0.3929(5) 0.1771(6) 0.4309(19) 0.022(2) Uani 1 1 d . . .
C4 C 0.3283(5) -0.1095(6) 0.3983(18) 0.021(2) Uani 1 1 d . . .
C5 C 0.2522(5) -0.1045(6) 0.325(2) 0.024(2) Uani 1 1 d . . .
H5A H 0.2342 -0.1362 0.4175 0.029 Uiso 1 1 calc R . .
H5B H 0.2383 -0.1234 0.1776 0.029 Uiso 1 1 calc R . .
C6 C 0.2149(6) -0.0341(7) 0.322(4) 0.053(5) Uani 1 1 d . . .
N1 N 0.4496(4) 0.1404(5) 0.5072(16) 0.0207(18) Uani 1 1 d . . .
N2 N 0.3658(4) -0.0534(5) 0.4635(17) 0.0227(19) Uani 1 1 d . . .
O1 O 0.4618(4) 0.3582(4) 0.4962(15) 0.032(2) Uani 1 1 d . . .
O2 O 0.5256(4) 0.2625(4) 0.5243(15) 0.0267(17) Uani 1 1 d . . .
O3 O 0.4351(3) 0.0680(4) 0.5332(14) 0.0226(16) Uani 1 1 d . . .
O4 O 0.3332(4) 0.1478(4) 0.3849(13) 0.0216(16) Uani 1 1 d . . .
O5 O 0.3562(4) -0.1714(4) 0.3993(13) 0.0203(15) Uani 1 1 d . . .
O6 O 0.4361(4) -0.0691(4) 0.5355(14) 0.0234(16) Uani 1 1 d . . .
O7 O 0.1525(6) -0.0392(6) 0.305(4) 0.113(8) Uani 1 1 d . . .
O8 O 0.2449(4) 0.0262(4) 0.3318(17) 0.033(2) Uani 1 1 d . . .
O9 O 0.1943(4) 0.1928(5) 0.2475(17) 0.034(2) Uani 1 1 d . . .
O10 O 0.0000 0.0261(8) -0.2500 0.054(4) Uani 1 2 d S . .
Cu1 Cu 0.5000 0.0000 0.5000 0.0170(5) Uani 1 2 d S . .
Cu2 Cu 0.54378(6) 0.16490(7) 0.5286(2) 0.0200(5) Uani 1 1 d . . .
Cu3 Cu 0.34016(6) 0.04527(7) 0.4211(2) 0.0181(4) Uani 1 1 d . . .
K1 K 0.09686(14) 0.08794(16) 0.1870(7) 0.0453(9) 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
C1 0.017(5) 0.019(5) 0.039(6) 0.003(4) 0.001(4) 0.000(4)
C2 0.016(5) 0.023(5) 0.032(6) 0.000(4) 0.001(4) 0.008(4)
C3 0.012(4) 0.019(5) 0.033(6) -0.005(4) 0.003(4) 0.003(4)
C4 0.013(4) 0.020(5) 0.031(5) 0.005(4) 0.005(4) 0.001(4)
C5 0.014(5) 0.021(5) 0.034(6) 0.005(4) 0.000(4) -0.002(4)
C6 0.010(5) 0.019(6) 0.121(15) -0.009(7) 0.001(7) -0.003(4)
N1 0.009(4) 0.020(4) 0.031(5) -0.001(4) 0.001(3) 0.003(3)
N2 0.006(4) 0.023(5) 0.037(5) 0.004(4) 0.002(3) 0.000(3)
O1 0.024(4) 0.018(4) 0.045(5) 0.004(3) -0.008(4) -0.005(3)
O2 0.012(3) 0.021(4) 0.046(5) 0.003(3) 0.004(3) -0.002(3)
O3 0.005(3) 0.017(4) 0.044(5) -0.002(3) 0.005(3) -0.003(3)
O4 0.011(3) 0.020(4) 0.033(4) -0.004(3) 0.003(3) 0.000(3)
O5 0.010(3) 0.018(4) 0.031(4) 0.002(3) 0.002(3) -0.001(3)
O6 0.008(3) 0.024(4) 0.035(4) 0.005(3) 0.001(3) 0.003(3)
O7 0.012(5) 0.028(6) 0.28(2) 0.008(10) 0.001(9) 0.000(4)
O8 0.013(4) 0.017(4) 0.064(6) 0.005(4) 0.000(4) 0.002(3)
O9 0.013(4) 0.027(4) 0.062(6) 0.005(4) 0.008(4) 0.003(3)
O10 0.052(9) 0.028(7) 0.098(14) 0.000 0.046(10) 0.000
Cu1 0.0069(8) 0.0166(9) 0.0259(10) 0.0011(6) 0.0015(6) -0.0006(6)
Cu2 0.0077(6) 0.0175(7) 0.0326(8) 0.0018(5) 0.0016(5) -0.0011(4)
Cu3 0.0074(6) 0.0177(7) 0.0274(7) 0.0003(5) 0.0014(5) -0.0010(4)
K1 0.0201(13) 0.0276(14) 0.084(3) -0.0043(14) 0.0067(14) 0.0060(10)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.233(15) . ?
C1 O2 1.295(13) . ?
C1 C2 1.535(15) . ?
C1 K1 3.444(12) 8_556 ?
C2 C3 1.486(15) . ?
C3 O4 1.285(13) . ?
C3 N1 1.315(13) . ?
C4 O5 1.301(13) . ?
C4 N2 1.306(14) . ?
C4 C5 1.480(14) . ?
C5 C6 1.529(17) . ?
C6 O7 1.234(17) . ?
C6 O8 1.288(15) . ?
C6 K1 3.265(13) . ?
N1 O3 1.422(12) . ?
N1 Cu2 1.920(9) . ?
N2 O6 1.399(11) . ?
N2 Cu3 1.942(9) . ?
O1 K1 2.768(11) 7_556 ?
O1 K1 2.857(9) 8_556 ?
O2 Cu2 1.886(8) . ?
O2 K1 3.223(9) 8_556 ?
O3 Cu1 1.886(7) . ?
O3 Cu3 1.903(7) . ?
O4 Cu3 1.959(8) . ?
O5 Cu2 1.946(7) 5_656 ?
O6 Cu1 1.888(8) . ?
O6 Cu2 1.928(8) 5_656 ?
O7 K1 2.681(12) . ?
O7 K1 3.06(2) 6_556 ?
O8 Cu3 1.885(8) . ?
O8 K1 3.106(8) . ?
O9 K1 2.748(9) . ?
O10 K1 3.005(11) 6 ?
O10 K1 3.005(11) 5 ?
O10 K1 3.158(7) . ?
O10 K1 3.158(7) 2_554 ?
Cu1 O3 1.886(7) 5_656 ?
Cu1 O6 1.888(8) 5_656 ?
Cu2 O6 1.928(8) 5_656 ?
Cu2 O5 1.946(7) 5_656 ?
K1 O1 2.768(11) 7_556 ?
K1 O1 2.857(9) 8_455 ?
K1 O10 3.005(11) 5 ?
K1 O7 3.06(2) 6 ?
K1 O2 3.223(9) 8_455 ?
K1 C1 3.444(12) 8_455 ?
K1 K1 4.173(6) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 O2 121.3(10) . . ?
O1 C1 C2 115.6(10) . . ?
O2 C1 C2 123.1(10) . . ?
O1 C1 K1 52.1(6) . 8_556 ?
O2 C1 K1 69.3(6) . 8_556 ?
C2 C1 K1 166.7(8) . 8_556 ?
C3 C2 C1 121.5(9) . . ?
O4 C3 N1 121.5(10) . . ?
O4 C3 C2 119.1(9) . . ?
N1 C3 C2 119.5(10) . . ?
O5 C4 N2 121.3(9) . . ?
O5 C4 C5 117.9(10) . . ?
N2 C4 C5 120.7(10) . . ?
C4 C5 C6 121.6(10) . . ?
O7 C6 O8 121.8(13) . . ?
O7 C6 C5 114.6(12) . . ?
O8 C6 C5 123.5(11) . . ?
O7 C6 K1 51.7(8) . . ?
O8 C6 K1 71.5(7) . . ?
C5 C6 K1 160.7(9) . . ?
C3 N1 O3 111.7(8) . . ?
C3 N1 Cu2 129.9(8) . . ?
O3 N1 Cu2 117.0(6) . . ?
C4 N2 O6 112.4(9) . . ?
C4 N2 Cu3 129.1(7) . . ?
O6 N2 Cu3 117.3(7) . . ?
C1 O1 K1 119.7(8) . 7_556 ?
C1 O1 K1 108.0(7) . 8_556 ?
K1 O1 K1 95.8(3) 7_556 8_556 ?
C1 O2 Cu2 128.1(7) . . ?
C1 O2 K1 88.6(6) . 8_556 ?
Cu2 O2 K1 142.3(4) . 8_556 ?
N1 O3 Cu1 118.6(5) . . ?
N1 O3 Cu3 113.1(6) . . ?
Cu1 O3 Cu3 117.3(4) . . ?
C3 O4 Cu3 111.7(7) . . ?
C4 O5 Cu2 111.2(6) . 5_656 ?
N2 O6 Cu1 118.3(6) . . ?
N2 O6 Cu2 112.4(6) . 5_656 ?
Cu1 O6 Cu2 116.3(4) . 5_656 ?
C6 O7 K1 107.1(10) . . ?
C6 O7 K1 121.8(17) . 6_556 ?
K1 O7 K1 106.2(6) . 6_556 ?
C6 O8 Cu3 127.8(8) . . ?
C6 O8 K1 85.4(7) . . ?
Cu3 O8 K1 146.8(4) . . ?
K1 O10 K1 87.9(4) 6 5 ?
K1 O10 K1 96.31(14) 6 . ?
K1 O10 K1 115.15(16) 5 . ?
K1 O10 K1 115.15(16) 6 2_554 ?
K1 O10 K1 96.31(14) 5 2_554 ?
K1 O10 K1 136.4(5) . 2_554 ?
O3 Cu1 O3 180.0(3) . 5_656 ?
O3 Cu1 O6 92.9(3) . 5_656 ?
O3 Cu1 O6 87.1(3) 5_656 5_656 ?
O3 Cu1 O6 87.1(3) . . ?
O3 Cu1 O6 92.9(3) 5_656 . ?
O6 Cu1 O6 180.0(5) 5_656 . ?
O2 Cu2 N1 93.0(4) . . ?
O2 Cu2 O6 166.7(4) . 5_656 ?
N1 Cu2 O6 90.8(4) . 5_656 ?
O2 Cu2 O5 97.2(3) . 5_656 ?
N1 Cu2 O5 166.3(4) . 5_656 ?
O6 Cu2 O5 81.3(3) 5_656 5_656 ?
O8 Cu3 O3 175.1(4) . . ?
O8 Cu3 N2 93.9(4) . . ?
O3 Cu3 N2 87.9(3) . . ?
O8 Cu3 O4 96.9(3) . . ?
O3 Cu3 O4 81.5(3) . . ?
N2 Cu3 O4 169.0(3) . . ?
O7 K1 O9 112.5(3) . . ?
O7 K1 O1 110.9(6) . 7_556 ?
O9 K1 O1 93.2(3) . 7_556 ?
O7 K1 O1 136.1(3) . 8_455 ?
O9 K1 O1 111.4(3) . 8_455 ?
O1 K1 O1 68.6(3) 7_556 8_455 ?
O7 K1 O10 63.5(3) . 5 ?
O9 K1 O10 164.9(3) . 5 ?
O1 K1 O10 75.9(3) 7_556 5 ?
O1 K1 O10 74.7(3) 8_455 5 ?
O7 K1 O7 74.6(4) . 6 ?
O9 K1 O7 86.2(3) . 6 ?
O1 K1 O7 174.1(4) 7_556 6 ?
O1 K1 O7 106.2(4) 8_455 6 ?
O10 K1 O7 105.7(3) 5 6 ?
O7 K1 O8 44.0(3) . . ?
O9 K1 O8 68.8(2) . . ?
O1 K1 O8 118.9(3) 7_556 . ?
O1 K1 O8 172.5(3) 8_455 . ?
O10 K1 O8 107.1(3) 5 . ?
O7 K1 O8 66.3(3) 6 . ?
O7 K1 O10 91.4(5) . . ?
O9 K1 O10 130.2(3) . . ?
O1 K1 O10 119.1(2) 7_556 . ?
O1 K1 O10 57.5(3) 8_455 . ?
O10 K1 O10 64.85(16) 5 . ?
O7 K1 O10 57.8(2) 6 . ?
O8 K1 O10 116.2(3) . . ?
O7 K1 O2 177.3(5) . 8_455 ?
O9 K1 O2 69.4(2) . 8_455 ?
O1 K1 O2 70.6(2) 7_556 8_455 ?
O1 K1 O2 42.0(2) 8_455 8_455 ?
O10 K1 O2 115.2(2) 5 8_455 ?
O7 K1 O2 103.8(3) 6 8_455 ?
O8 K1 O2 137.5(2) . 8_455 ?
O10 K1 O2 85.8(3) . 8_455 ?
O7 K1 C6 21.2(4) . . ?
O9 K1 C6 91.9(3) . . ?
O1 K1 C6 119.4(4) 7_556 . ?
O1 K1 C6 155.4(3) 8_455 . ?
O10 K1 C6 84.7(3) 5 . ?
O7 K1 C6 66.5(5) 6 . ?
O8 K1 C6 23.1(3) . . ?
O10 K1 C6 101.8(4) . . ?
O2 K1 C6 160.0(3) 8_455 . ?
O7 K1 C1 156.0(3) . 8_455 ?
O9 K1 C1 91.5(3) . 8_455 ?
O1 K1 C1 67.3(3) 7_556 8_455 ?
O1 K1 C1 19.9(3) 8_455 8_455 ?
O10 K1 C1 93.7(3) 5 8_455 ?
O7 K1 C1 106.9(4) 6 8_455 ?
O8 K1 C1 159.1(3) . 8_455 ?
O10 K1 C1 70.8(3) . 8_455 ?
O2 K1 C1 22.1(2) 8_455 8_455 ?
C6 K1 C1 172.3(4) . 8_455 ?
O7 K1 K1 106.8(4) . 2 ?
O9 K1 K1 129.8(2) . 2 ?
O1 K1 K1 42.93(18) 7_556 2 ?
O1 K1 K1 41.3(2) 8_455 2 ?
O10 K1 K1 46.0(2) 5 2 ?
O7 K1 K1 134.6(3) 6 2 ?
O8 K1 K1 144.5(2) . 2 ?
O10 K1 K1 76.89(9) . 2 ?
O2 K1 K1 72.63(15) 8_455 2 ?
C6 K1 K1 126.9(3) . 2 ?
C1 K1 K1 54.5(2) 8_455 2 ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        29.19
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         2.341
_refine_diff_density_min         -1.901
_refine_diff_density_rms         0.341