 
data_1 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'H Cu2 O5 V' 
_chemical_formula_sum             'H Cu2 O5 V' 
  
_chemical_formula_weight          259.03 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'V'  'V'   0.3005   0.5294 
 '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' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            ¡®orthorhombic¡¯ 
_symmetry_space_group_name_H-M    ¡®P2(1)2(1)2(1)¡¯ 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, -y, z+1/2' 
 '-x, y+1/2, -z+1/2' 
 'x+1/2, -y+1/2, -z' 
 
_cell_length_a                    6.053(2) 
_cell_length_b                    8.560(4) 
_cell_length_c                    14.963(6) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      775.2(6) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used           2318
_cell_measurement_theta_min             2.7226
_cell_measurement_theta_max             27.4585 
 
_exptl_crystal_description              'Prism'
_exptl_crystal_colour                   'dark red'
_exptl_crystal_size_max                 0.1000
_exptl_crystal_size_mid                 0.0500
_exptl_crystal_size_min                 0.0500
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     4.439 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              976 
_exptl_absorpt_coefficient_mu     13.130 
_exptl_absorpt_correction_type          'Multi-scan'
_exptl_absorpt_correction_T_max         1.0000
_exptl_absorpt_correction_T_min         0.7273 
_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   ¡®Mercury70¡¯ 
_diffrn_measurement_method        'CCD_Profile_fitting' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             6067 
_diffrn_reflns_av_R_equivalents   0.0284 
_diffrn_reflns_av_sigmaI/netI     0.0295 
_diffrn_reflns_limit_h_min        -7 
_diffrn_reflns_limit_h_max        7 
_diffrn_reflns_limit_k_min        -11 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        -18 
_diffrn_reflns_limit_l_max        19 
_diffrn_reflns_theta_min          2.72 
_diffrn_reflns_theta_max          27.49 
_reflns_number_total              1773 
_reflns_number_gt                 1697 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection              'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement              'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction               'CrystalClear (Rigaku Inc., 2008)'
_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)+(0.0198P)²+0.2894P] 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_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.53(2) 
_refine_ls_number_reflns          1773 
_refine_ls_number_parameters      146 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0234 
_refine_ls_R_factor_gt            0.0216 
_refine_ls_wR_factor_ref          0.0433 
_refine_ls_wR_factor_gt           0.0426 
_refine_ls_goodness_of_fit_ref    1.053 
_refine_ls_restrained_S_all       1.053 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Cu1 Cu -0.27375(12) 0.33689(5) 0.92639(3) 0.01583(13) Uani 1 1 d . . . 
Cu2 Cu -0.02362(8) 0.61979(7) 0.86004(3) 0.00687(11) Uani 1 1 d . . . 
Cu3 Cu 0.23590(9) 0.89767(4) 0.78517(3) 0.00710(10) Uani 1 1 d . . . 
Cu4 Cu 0.46926(8) 0.62209(7) 0.86397(3) 0.00708(11) Uani 1 1 d . . . 
V1 V -0.77225(12) 0.27778(6) 0.84478(4) 0.00529(13) Uani 1 1 d . . . 
V2 V 0.71599(12) 0.93794(6) 0.91993(4) 0.00508(13) Uani 1 1 d . . . 
O1 O -0.7813(6) 0.2081(3) 0.94754(16) 0.0149(6) Uani 1 1 d . . . 
O2 O -0.7532(5) 0.1222(2) 0.77242(15) 0.0085(5) Uani 1 1 d . . . 
O3 O -1.0205(4) 0.3914(4) 0.8249(2) 0.0088(6) Uani 1 1 d . . . 
O4 O -0.5381(5) 0.3939(4) 0.83191(19) 0.0077(6) Uani 1 1 d . . . 
O5 O -0.2758(5) 0.5638(3) 0.93746(15) 0.0072(5) Uani 1 1 d . . . 
H5 H -0.2418 0.6084 0.9863 0.009 Uiso 1 1 d R . . 
O6 O 0.2289(5) 0.6722(2) 0.78552(15) 0.0054(5) Uani 1 1 d . . . 
H6 H 0.2400 0.6284 0.7347 0.007 Uiso 1 1 d R . . 
O7 O 0.4710(5) 0.8533(4) 0.8788(2) 0.0120(6) Uani 1 1 d . . . 
O8 O 0.7260(5) 1.1284(3) 0.88743(16) 0.0123(5) Uani 1 1 d . . . 
O9 O 0.9448(5) 0.8451(4) 0.8783(2) 0.0132(6) Uani 1 1 d . . . 
O10 O 0.7170(5) 0.9234(3) 1.03062(16) 0.0124(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 
Cu1 O8 1.877(2) 1_445 ? 
Cu1 O1 1.926(3) 4_557 ? 
Cu1 O5 1.949(2) . ? 
Cu1 O4 2.190(3) . ? 
Cu1 O3 2.207(3) 1_655 ? 
Cu1 Cu2 3.0235(11) . ? 
Cu1 Cu4 3.0416(11) 1_455 ? 
Cu2 O6 1.945(3) . ? 
Cu2 O9 1.957(3) 1_455 ? 
Cu2 O5 1.975(3) . ? 
Cu2 O3 2.024(3) 1_655 ? 
Cu2 O10 2.221(3) 4_467 ? 
Cu2 O2 2.399(3) 3_456 ? 
Cu2 Cu4 2.9838(13) . ? 
Cu3 O6 1.930(2) . ? 
Cu3 O2 1.932(2) 1_665 ? 
Cu3 O7 2.032(3) . ? 
Cu3 O3 2.102(3) 3_456 ? 
Cu3 O9 2.291(3) 1_455 ? 
Cu3 Cu4 2.9916(11) . ? 
Cu4 O6 1.918(3) . ? 
Cu4 O5 1.959(3) 1_655 ? 
Cu4 O7 1.991(3) . ? 
Cu4 O4 2.012(3) 1_655 ? 
Cu4 O10 2.229(3) 4_467 ? 
Cu4 Cu1 3.0416(11) 1_655 ? 
V1 O1 1.650(2) . ? 
V1 O2 1.720(2) . ? 
V1 O4 1.742(3) . ? 
V1 O3 1.814(3) . ? 
V2 O10 1.661(3) . ? 
V2 O8 1.702(2) . ? 
V2 O9 1.714(3) . ? 
V2 O7 1.762(3) . ? 
O1 Cu1 1.926(3) 4_457 ? 
O2 Cu3 1.932(2) 1_445 ? 
O2 Cu2 2.399(3) 3_446 ? 
O3 Cu2 2.024(3) 1_455 ? 
O3 Cu3 2.102(3) 3_446 ? 
O3 Cu1 2.207(3) 1_455 ? 
O4 Cu4 2.012(3) 1_455 ? 
O5 Cu4 1.959(3) 1_455 ? 
O8 Cu1 1.877(2) 1_665 ? 
O9 Cu2 1.957(3) 1_655 ? 
O9 Cu3 2.291(3) 1_655 ? 
O10 Cu2 2.221(3) 4_567 ? 
O10 Cu4 2.229(3) 4_567 ? 
 
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 
O8 Cu1 O1 96.56(11) 1_445 4_557 ? 
O8 Cu1 O5 166.78(10) 1_445 . ? 
O1 Cu1 O5 96.64(10) 4_557 . ? 
O8 Cu1 O4 90.62(12) 1_445 . ? 
O1 Cu1 O4 131.26(14) 4_557 . ? 
O5 Cu1 O4 80.10(12) . . ? 
O8 Cu1 O3 89.32(12) 1_445 1_655 ? 
O1 Cu1 O3 137.08(14) 4_557 1_655 ? 
O5 Cu1 O3 81.50(12) . 1_655 ? 
O4 Cu1 O3 90.94(10) . 1_655 ? 
O8 Cu1 Cu2 131.29(9) 1_445 . ? 
O1 Cu1 Cu2 119.57(9) 4_557 . ? 
O5 Cu1 Cu2 39.93(8) . . ? 
O4 Cu1 Cu2 88.59(8) . . ? 
O3 Cu1 Cu2 42.02(8) 1_655 . ? 
O8 Cu1 Cu4 131.85(9) 1_445 1_455 ? 
O1 Cu1 Cu4 116.68(9) 4_557 1_455 ? 
O5 Cu1 Cu4 39.02(8) . 1_455 ? 
O4 Cu1 Cu4 41.35(8) . 1_455 ? 
O3 Cu1 Cu4 88.53(8) 1_655 1_455 ? 
Cu2 Cu1 Cu4 60.82(3) . 1_455 ? 
O6 Cu2 O9 85.95(11) . 1_455 ? 
O6 Cu2 O5 178.73(11) . . ? 
O9 Cu2 O5 94.69(11) 1_455 . ? 
O6 Cu2 O3 93.83(11) . 1_655 ? 
O9 Cu2 O3 171.40(13) 1_455 1_655 ? 
O5 Cu2 O3 85.70(11) . 1_655 ? 
O6 Cu2 O10 86.86(11) . 4_467 ? 
O9 Cu2 O10 97.18(12) 1_455 4_467 ? 
O5 Cu2 O10 91.97(11) . 4_467 ? 
O3 Cu2 O10 91.39(11) 1_655 4_467 ? 
O6 Cu2 O2 88.12(10) . 3_456 ? 
O9 Cu2 O2 92.99(11) 1_455 3_456 ? 
O5 Cu2 O2 92.94(10) . 3_456 ? 
O3 Cu2 O2 78.41(10) 1_655 3_456 ? 
O10 Cu2 O2 168.31(9) 4_467 3_456 ? 
O6 Cu2 Cu4 39.09(7) . . ? 
O9 Cu2 Cu4 95.07(9) 1_455 . ? 
O5 Cu2 Cu4 139.70(8) . . ? 
O3 Cu2 Cu4 90.12(8) 1_655 . ? 
O10 Cu2 Cu4 48.02(8) 4_467 . ? 
O2 Cu2 Cu4 125.41(7) 3_456 . ? 
O6 Cu2 Cu1 140.07(7) . . ? 
O9 Cu2 Cu1 133.98(9) 1_455 . ? 
O5 Cu2 Cu1 39.30(7) . . ? 
O3 Cu2 Cu1 46.88(9) 1_655 . ? 
O10 Cu2 Cu1 87.32(7) 4_467 . ? 
O2 Cu2 Cu1 89.77(6) 3_456 . ? 
Cu4 Cu2 Cu1 119.96(3) . . ? 
O6 Cu3 O2 174.44(10) . 1_665 ? 
O6 Cu3 O7 80.01(12) . . ? 
O2 Cu3 O7 103.30(12) 1_665 . ? 
O6 Cu3 O3 87.89(12) . 3_456 ? 
O2 Cu3 O3 88.23(12) 1_665 3_456 ? 
O7 Cu3 O3 165.87(13) . 3_456 ? 
O6 Cu3 O9 77.60(11) . 1_455 ? 
O2 Cu3 O9 106.37(11) 1_665 1_455 ? 
O7 Cu3 O9 94.74(11) . 1_455 ? 
O3 Cu3 O9 89.70(12) 3_456 1_455 ? 
O6 Cu3 Cu4 38.82(8) . . ? 
O2 Cu3 Cu4 143.80(8) 1_665 . ? 
O7 Cu3 Cu4 41.45(9) . . ? 
O3 Cu3 Cu4 125.57(9) 3_456 . ? 
O9 Cu3 Cu4 88.19(8) 1_455 . ? 
O6 Cu4 O5 176.21(10) . 1_655 ? 
O6 Cu4 O7 81.34(10) . . ? 
O5 Cu4 O7 100.76(11) 1_655 . ? 
O6 Cu4 O4 93.13(10) . 1_655 ? 
O5 Cu4 O4 84.49(10) 1_655 1_655 ? 
O7 Cu4 O4 172.52(13) . 1_655 ? 
O6 Cu4 O10 87.29(11) . 4_467 ? 
O5 Cu4 O10 95.61(11) 1_655 4_467 ? 
O7 Cu4 O10 95.65(11) . 4_467 ? 
O4 Cu4 O10 89.09(11) 1_655 4_467 ? 
O6 Cu4 Cu2 39.75(8) . . ? 
O5 Cu4 Cu2 142.81(8) 1_655 . ? 
O7 Cu4 Cu2 90.80(8) . . ? 
O4 Cu4 Cu2 88.10(8) 1_655 . ? 
O10 Cu4 Cu2 47.79(7) 4_467 . ? 
O6 Cu4 Cu3 39.12(6) . . ? 
O5 Cu4 Cu3 142.55(7) 1_655 . ? 
O7 Cu4 Cu3 42.49(9) . . ? 
O4 Cu4 Cu3 131.39(9) 1_655 . ? 
O10 Cu4 Cu3 95.34(7) 4_467 . ? 
Cu2 Cu4 Cu3 61.67(2) . . ? 
O6 Cu4 Cu1 139.07(7) . 1_655 ? 
O5 Cu4 Cu1 38.79(7) 1_655 1_655 ? 
O7 Cu4 Cu1 139.54(9) . 1_655 ? 
O4 Cu4 Cu1 45.99(8) 1_655 1_655 ? 
O10 Cu4 Cu1 89.59(7) 4_467 1_655 ? 
Cu2 Cu4 Cu1 120.80(3) . 1_655 ? 
Cu3 Cu4 Cu1 174.47(2) . 1_655 ? 
O1 V1 O2 107.97(12) . . ? 
O1 V1 O4 109.66(15) . . ? 
O2 V1 O4 108.52(14) . . ? 
O1 V1 O3 108.60(15) . . ? 
O2 V1 O3 111.58(14) . . ? 
O4 V1 O3 110.47(11) . . ? 
O10 V2 O8 110.89(12) . . ? 
O10 V2 O9 108.93(15) . . ? 
O8 V2 O9 108.16(15) . . ? 
O10 V2 O7 108.73(15) . . ? 
O8 V2 O7 108.90(15) . . ? 
O9 V2 O7 111.25(13) . . ? 
V1 O1 Cu1 169.78(17) . 4_457 ? 
V1 O2 Cu3 134.87(14) . 1_445 ? 
V1 O2 Cu2 119.25(12) . 3_446 ? 
Cu3 O2 Cu2 93.09(9) 1_445 3_446 ? 
V1 O3 Cu2 118.89(15) . 1_455 ? 
V1 O3 Cu3 130.97(17) . 3_446 ? 
Cu2 O3 Cu3 99.96(13) 1_455 3_446 ? 
V1 O3 Cu1 110.44(15) . 1_455 ? 
Cu2 O3 Cu1 91.10(12) 1_455 1_455 ? 
Cu3 O3 Cu1 96.52(11) 3_446 1_455 ? 
V1 O4 Cu4 123.07(16) . 1_455 ? 
V1 O4 Cu1 113.32(15) . . ? 
Cu4 O4 Cu1 92.65(12) 1_455 . ? 
Cu1 O5 Cu4 102.19(12) . 1_455 ? 
Cu1 O5 Cu2 100.77(12) . . ? 
Cu4 O5 Cu2 102.56(11) 1_455 . ? 
Cu4 O6 Cu3 102.06(11) . . ? 
Cu4 O6 Cu2 101.16(11) . . ? 
Cu3 O6 Cu2 104.45(12) . . ? 
V2 O7 Cu4 116.88(16) . . ? 
V2 O7 Cu3 138.89(19) . . ? 
Cu4 O7 Cu3 96.06(13) . . ? 
V2 O8 Cu1 145.26(15) . 1_665 ? 
V2 O9 Cu2 125.91(17) . 1_655 ? 
V2 O9 Cu3 138.71(18) . 1_655 ? 
Cu2 O9 Cu3 91.91(12) 1_655 1_655 ? 
V2 O10 Cu2 138.11(17) . 4_567 ? 
V2 O10 Cu4 136.15(17) . 4_567 ? 
Cu2 O10 Cu4 84.20(9) 4_567 4_567 ? 
 
_diffrn_measured_fraction_theta_max    0.993 
_diffrn_reflns_theta_full              27.49 
_diffrn_measured_fraction_theta_full   0.993 
_refine_diff_density_max    0.469 
_refine_diff_density_min   -0.616 
_refine_diff_density_rms    0.127 
