 
data_1 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'Cl4 Cu7 Na2 O14 Se4' 
_chemical_formula_sum 
 'Cl4 Cu7 Na2 O14 Se4' 
_chemical_formula_weight         1172.47 
 
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' 
 'Na'  'Na'   0.0362   0.0249 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.1484   0.1585 
 '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' 
 'Se'  'Se'  -0.0929   2.2259 
 '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                    7.446(2) 
_cell_length_b                    8.349(3) 
_cell_length_c                    9.137(3) 
_cell_angle_alpha                 110.335(7) 
_cell_angle_beta                  106.166(3) 
_cell_angle_gamma                 105.161(7) 
_cell_volume                      469.3(2) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used           1628
_cell_measurement_theta_min             2.6041
_cell_measurement_theta_max             27.4700 
 
_exptl_crystal_description              'Prism'
_exptl_crystal_colour                   'Colorless'
_exptl_crystal_size_max                 0.2000
_exptl_crystal_size_mid                 0.2000
_exptl_crystal_size_min                 0.2000
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     4.149 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              541 
_exptl_absorpt_coefficient_mu     16.215 
_exptl_absorpt_correction_type          'Multi-scan'
_exptl_absorpt_correction_T_max         1.0000
_exptl_absorpt_correction_T_min         0.4580
_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   'CCD' 
_diffrn_measurement_method        'CCD_Profile_fitting' 
_diffrn_detector_area_resol_mean  28.5714  
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             5788 
_diffrn_reflns_av_R_equivalents   0.0354 
_diffrn_reflns_av_sigmaI/netI     0.0414 
_diffrn_reflns_limit_h_min        -8 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -10 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        -11 
_diffrn_reflns_limit_l_max        11 
_diffrn_reflns_theta_min          2.60 
_diffrn_reflns_theta_max          27.47 
_reflns_number_total              2149 
_reflns_number_gt                 1887 
_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)+(0.0161P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    none 
_refine_ls_hydrogen_treatment     none 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          2122 
_refine_ls_number_parameters      142 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0269 
_refine_ls_R_factor_gt            0.0221 
_refine_ls_wR_factor_ref          0.0501 
_refine_ls_wR_factor_gt           0.0486 
_refine_ls_goodness_of_fit_ref    1.032 
_refine_ls_restrained_S_all       1.032 
_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 
Se1 Se 0.19617(6) 0.79530(5) 0.96083(5) 0.01168(10) Uani 1 1 d . . . 
Se2 Se -0.80201(6) 0.08221(5) 0.38936(5) 0.01193(10) Uani 1 1 d . . . 
Cu1 Cu -0.5000 0.5000 0.5000 0.01222(15) Uani 1 2 d S . . 
Cu2 Cu -0.44494(7) 0.33564(6) 0.77772(6) 0.01386(12) Uani 1 1 d . . . 
Cu3 Cu 0.17130(7) 0.44376(6) 0.64734(6) 0.01355(12) Uani 1 1 d . . . 
Cu4 Cu -0.60675(7) 0.25741(6) 0.13585(6) 0.01412(12) Uani 1 1 d . . . 
Cl1 Cl -0.23844(15) 0.61208(12) 1.03522(12) 0.0193(2) Uani 1 1 d . . . 
Na Na -0.2992(3) 0.0909(2) 0.3170(2) 0.0232(4) Uani 1 1 d . . . 
O1 O -0.4555(4) 0.5106(3) 0.3064(3) 0.0102(5) Uani 1 1 d . . . 
O2 O -0.6499(4) 0.2332(3) 0.3428(3) 0.0190(6) Uani 1 1 d . . . 
O3 O -0.6331(4) 0.1085(3) 0.5715(3) 0.0169(6) Uani 1 1 d . . . 
O4 O -0.9407(4) 0.1976(3) 0.4591(3) 0.0200(7) Uani 1 1 d . . . 
O5 O 0.3797(4) 0.8411(3) 1.1441(3) 0.0175(6) Uani 1 1 d . . . 
O6 O 0.2947(4) 0.7100(3) 0.8154(3) 0.0126(6) Uani 1 1 d . . . 
O7 O 0.2419(4) 1.0060(3) 0.9642(3) 0.0195(7) Uani 1 1 d . . . 
Cl2 Cl -0.15313(15) 0.40924(13) 0.62098(13) 0.0204(2) 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 
Se1 O5 1.681(3) . ? 
Se1 O7 1.690(2) . ? 
Se1 O6 1.724(3) . ? 
Se1 Na 3.2117(18) 2_566 ? 
Se2 O4 1.692(3) . ? 
Se2 O3 1.684(3) . ? 
Se2 O2 1.717(3) . ? 
Se2 Na 3.4630(17) 2_456 ? 
Cu1 O1 1.915(2) 2_466 ? 
Cu1 O1 1.915(2) . ? 
Cu1 O2 1.963(2) . ? 
Cu1 O2 1.963(2) 2_466 ? 
Cu1 Cu4 2.9675(9) 2_466 ? 
Cu1 Cu4 2.9675(9) . ? 
Cu2 O1 1.912(2) 2_466 ? 
Cu2 O3 1.941(3) . ? 
Cu2 O5 1.959(3) 2_567 ? 
Cu2 Cl1 2.3625(12) . ? 
Cu2 Na 3.2323(18) 2_456 ? 
Cu3 O4 1.930(3) 1_655 ? 
Cu3 O1 1.942(3) 2_566 ? 
Cu3 O6 1.979(2) . ? 
Cu3 Cl2 2.2890(13) . ? 
Cu3 Na 3.5492(18) . ? 
Cu3 Na 3.622(2) 2_566 ? 
Cu4 O7 1.904(2) 1_444 ? 
Cu4 O1 1.911(2) . ? 
Cu4 O2 2.071(3) . ? 
Cu4 O6 2.163(3) 2_566 ? 
Cu4 Cl1 2.4075(11) 2_466 ? 
Cu4 Na 3.3271(18) . ? 
Cl1 Cu4 2.4075(11) 2_466 ? 
Na O3 2.256(3) 2_456 ? 
Na O6 2.370(3) 2_566 ? 
Na O4 2.372(3) 1_655 ? 
Na O5 2.357(3) 1_444 ? 
Na O7 2.604(3) 2_566 ? 
Na Cl2 2.764(2) . ? 
Na Se1 3.2117(18) 2_566 ? 
Na Cu2 3.2323(18) 2_456 ? 
Na Se2 3.4630(17) 2_456 ? 
Na Cu3 3.622(2) 2_566 ? 
O1 Cu2 1.912(2) 2_466 ? 
O1 Cu3 1.942(3) 2_566 ? 
O3 Na 2.256(3) 2_456 ? 
O4 Cu3 1.930(3) 1_455 ? 
O4 Na 2.372(3) 1_455 ? 
O5 Cu2 1.959(3) 2_567 ? 
O5 Na 2.357(3) 1_666 ? 
O6 Cu4 2.163(3) 2_566 ? 
O6 Na 2.370(3) 2_566 ? 
O7 Cu4 1.904(2) 1_666 ? 
O7 Na 2.604(3) 2_566 ? 
 
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 
O5 Se1 O7 103.66(12) . . ? 
O5 Se1 O6 101.13(13) . . ? 
O7 Se1 O6 97.45(13) . . ? 
O5 Se1 Na 122.01(10) . 2_566 ? 
O7 Se1 Na 53.95(10) . 2_566 ? 
O6 Se1 Na 46.16(9) . 2_566 ? 
O4 Se2 O3 102.87(13) . . ? 
O4 Se2 O2 102.56(13) . . ? 
O3 Se2 O2 101.14(13) . . ? 
O4 Se2 Na 99.64(10) . 2_456 ? 
O3 Se2 Na 33.37(9) . 2_456 ? 
O2 Se2 Na 133.26(10) . 2_456 ? 
O1 Cu1 O1 180.000(1) 2_466 . ? 
O1 Cu1 O2 96.88(10) 2_466 . ? 
O1 Cu1 O2 83.12(10) . . ? 
O1 Cu1 O2 83.12(10) 2_466 2_466 ? 
O1 Cu1 O2 96.88(10) . 2_466 ? 
O2 Cu1 O2 180.00(11) . 2_466 ? 
O1 Cu1 Cu4 39.09(7) 2_466 2_466 ? 
O1 Cu1 Cu4 140.91(7) . 2_466 ? 
O2 Cu1 Cu4 135.92(7) . 2_466 ? 
O2 Cu1 Cu4 44.08(7) 2_466 2_466 ? 
O1 Cu1 Cu4 140.91(7) 2_466 . ? 
O1 Cu1 Cu4 39.09(7) . . ? 
O2 Cu1 Cu4 44.08(7) . . ? 
O2 Cu1 Cu4 135.92(7) 2_466 . ? 
Cu4 Cu1 Cu4 180.0 2_466 . ? 
O1 Cu2 O3 93.08(11) 2_466 . ? 
O1 Cu2 O5 172.60(11) 2_466 2_567 ? 
O3 Cu2 O5 82.30(11) . 2_567 ? 
O1 Cu2 Cl1 85.83(8) 2_466 . ? 
O3 Cu2 Cl1 175.32(9) . . ? 
O5 Cu2 Cl1 98.31(8) 2_567 . ? 
O1 Cu2 Na 126.74(8) 2_466 2_456 ? 
O3 Cu2 Na 43.33(8) . 2_456 ? 
O5 Cu2 Na 46.43(9) 2_567 2_456 ? 
Cl1 Cu2 Na 134.76(4) . 2_456 ? 
O4 Cu3 O1 96.34(11) 1_655 2_566 ? 
O4 Cu3 O6 171.20(11) 1_655 . ? 
O1 Cu3 O6 81.37(10) 2_566 . ? 
O4 Cu3 Cl2 88.66(9) 1_655 . ? 
O1 Cu3 Cl2 174.30(8) 2_566 . ? 
O6 Cu3 Cl2 94.09(8) . . ? 
O4 Cu3 Na 38.68(9) 1_655 . ? 
O1 Cu3 Na 134.27(8) 2_566 . ? 
O6 Cu3 Na 141.34(8) . . ? 
Cl2 Cu3 Na 51.12(4) . . ? 
O4 Cu3 Na 134.42(9) 1_655 2_566 ? 
O1 Cu3 Na 86.16(7) 2_566 2_566 ? 
O6 Cu3 Na 37.20(8) . 2_566 ? 
Cl2 Cu3 Na 92.29(4) . 2_566 ? 
Na Cu3 Na 117.55(3) . 2_566 ? 
O7 Cu4 O1 179.41(10) 1_444 . ? 
O7 Cu4 O2 100.13(11) 1_444 . ? 
O1 Cu4 O2 80.38(10) . . ? 
O7 Cu4 O6 102.68(11) 1_444 2_566 ? 
O1 Cu4 O6 77.44(10) . 2_566 ? 
O2 Cu4 O6 104.77(11) . 2_566 ? 
O7 Cu4 Cl1 94.86(8) 1_444 2_466 ? 
O1 Cu4 Cl1 84.58(8) . 2_466 ? 
O2 Cu4 Cl1 128.94(9) . 2_466 ? 
O6 Cu4 Cl1 119.01(7) 2_566 2_466 ? 
O7 Cu4 Cu1 141.31(8) 1_444 . ? 
O1 Cu4 Cu1 39.19(7) . . ? 
O2 Cu4 Cu1 41.24(7) . . ? 
O6 Cu4 Cu1 92.55(7) 2_566 . ? 
Cl1 Cu4 Cu1 108.54(4) 2_466 . ? 
O7 Cu4 Na 84.94(9) 1_444 . ? 
O1 Cu4 Na 95.53(8) . . ? 
O2 Cu4 Na 67.36(9) . . ? 
O6 Cu4 Na 45.26(7) 2_566 . ? 
Cl1 Cu4 Na 163.17(4) 2_466 . ? 
Cu1 Cu4 Na 81.01(4) . . ? 
Cu2 Cl1 Cu4 80.99(4) . 2_466 ? 
O3 Na O6 169.08(12) 2_456 2_566 ? 
O3 Na O4 93.91(11) 2_456 1_655 ? 
O6 Na O4 96.71(11) 2_566 1_655 ? 
O3 Na O5 67.56(10) 2_456 1_444 ? 
O6 Na O5 103.79(11) 2_566 1_444 ? 
O4 Na O5 149.32(12) 1_655 1_444 ? 
O3 Na O7 121.72(11) 2_456 2_566 ? 
O6 Na O7 61.87(9) 2_566 2_566 ? 
O4 Na O7 85.71(11) 1_655 2_566 ? 
O5 Na O7 84.16(10) 1_444 2_566 ? 
O3 Na Cl2 95.26(9) 2_456 . ? 
O6 Na Cl2 86.03(8) 2_566 . ? 
O4 Na Cl2 69.89(8) 1_655 . ? 
O5 Na Cl2 133.40(11) 1_444 . ? 
O7 Na Cl2 137.26(9) 2_566 . ? 
O3 Na Se1 153.33(10) 2_456 2_566 ? 
O6 Na Se1 31.64(6) 2_566 2_566 ? 
O4 Na Se1 84.56(8) 1_655 2_566 ? 
O5 Na Se1 101.14(8) 1_444 2_566 ? 
O7 Na Se1 31.63(6) 2_566 2_566 ? 
Cl2 Na Se1 109.01(6) . 2_566 ? 
O3 Na Cu2 36.18(7) 2_456 2_456 ? 
O6 Na Cu2 138.15(8) 2_566 2_456 ? 
O4 Na Cu2 115.04(8) 1_655 2_456 ? 
O5 Na Cu2 37.03(6) 1_444 2_456 ? 
O7 Na Cu2 92.71(7) 2_566 2_456 ? 
Cl2 Na Cu2 129.08(6) . 2_456 ? 
Se1 Na Cu2 121.85(5) 2_566 2_456 ? 
O3 Na Cu4 128.71(10) 2_456 . ? 
O6 Na Cu4 40.41(7) 2_566 . ? 
O4 Na Cu4 134.34(8) 1_655 . ? 
O5 Na Cu4 73.21(8) 1_444 . ? 
O7 Na Cu4 84.39(7) 2_566 . ? 
Cl2 Na Cu4 88.36(5) . . ? 
Se1 Na Cu4 64.71(3) 2_566 . ? 
Cu2 Na Cu4 109.87(5) 2_456 . ? 
O3 Na Se2 24.24(7) 2_456 2_456 ? 
O6 Na Se2 163.37(8) 2_566 2_456 ? 
O4 Na Se2 71.58(8) 1_655 2_456 ? 
O5 Na Se2 91.77(8) 1_444 2_456 ? 
O7 Na Se2 126.76(8) 2_566 2_456 ? 
Cl2 Na Se2 78.92(5) . 2_456 ? 
Se1 Na Se2 150.75(6) 2_566 2_456 ? 
Cu2 Na Se2 58.44(3) 2_456 2_456 ? 
Cu4 Na Se2 144.54(6) . 2_456 ? 
O3 Na Cu3 101.14(8) 2_456 . ? 
O6 Na Cu3 86.85(8) 2_566 . ? 
O4 Na Cu3 30.56(6) 1_655 . ? 
O5 Na Cu3 167.83(9) 1_444 . ? 
O7 Na Cu3 106.36(8) 2_566 . ? 
Cl2 Na Cu3 40.15(3) . . ? 
Se1 Na Cu3 91.02(4) 2_566 . ? 
Cu2 Na Cu3 134.07(5) 2_456 . ? 
Cu4 Na Cu3 113.22(5) . . ? 
Se2 Na Cu3 77.10(4) 2_456 . ? 
O3 Na Cu3 150.33(9) 2_456 2_566 ? 
O6 Na Cu3 30.32(6) 2_566 2_566 ? 
O4 Na Cu3 82.96(7) 1_655 2_566 ? 
O5 Na Cu3 125.34(9) 1_444 2_566 ? 
O7 Na Cu3 87.58(7) 2_566 2_566 ? 
Cl2 Na Cu3 55.88(4) . 2_566 ? 
Se1 Na Cu3 56.01(3) 2_566 2_566 ? 
Cu2 Na Cu3 161.98(6) 2_456 2_566 ? 
Cu4 Na Cu3 52.20(3) . 2_566 ? 
Se2 Na Cu3 133.70(5) 2_456 2_566 ? 
Cu3 Na Cu3 62.45(3) . 2_566 ? 
Cu1 O1 Cu4 101.72(11) . . ? 
Cu1 O1 Cu2 116.82(13) . 2_466 ? 
Cu4 O1 Cu2 108.27(12) . 2_466 ? 
Cu1 O1 Cu3 107.67(11) . 2_566 ? 
Cu4 O1 Cu3 105.60(12) . 2_566 ? 
Cu2 O1 Cu3 115.33(12) 2_466 2_566 ? 
Se2 O2 Cu1 122.55(14) . . ? 
Se2 O2 Cu4 140.65(14) . . ? 
Cu1 O2 Cu4 94.67(10) . . ? 
Se2 O3 Cu2 129.10(14) . . ? 
Se2 O3 Na 122.39(14) . 2_456 ? 
Cu2 O3 Na 100.48(12) . 2_456 ? 
Se2 O4 Cu3 125.06(15) . 1_455 ? 
Se2 O4 Na 123.83(13) . 1_455 ? 
Cu3 O4 Na 110.76(13) 1_455 1_455 ? 
Se1 O5 Cu2 128.27(14) . 2_567 ? 
Se1 O5 Na 130.76(14) . 1_666 ? 
Cu2 O5 Na 96.54(12) 2_567 1_666 ? 
Se1 O6 Cu3 121.28(14) . . ? 
Se1 O6 Cu4 128.16(13) . 2_566 ? 
Cu3 O6 Cu4 95.52(10) . 2_566 ? 
Se1 O6 Na 102.20(12) . 2_566 ? 
Cu3 O6 Na 112.48(12) . 2_566 ? 
Cu4 O6 Na 94.33(10) 2_566 2_566 ? 
Se1 O7 Cu4 135.11(15) . 1_666 ? 
Se1 O7 Na 94.42(11) . 2_566 ? 
Cu4 O7 Na 117.73(13) 1_666 2_566 ? 
Cu3 Cl2 Na 88.73(5) . . ? 
 
_diffrn_measured_fraction_theta_max    0.987 
_diffrn_reflns_theta_full              27.47 
_diffrn_measured_fraction_theta_full   0.987 
_refine_diff_density_max    0.601 
_refine_diff_density_min   -0.796 
_refine_diff_density_rms    0.154 
