# Copyright The Royal Society of Chemistry, 1998 data_zlm2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12 H28 Cu15 Na2 O45 P12' _chemical_formula_weight 2263.28 _chemical_melting_point ? _chemical_compound_source ? 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' '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' 'P' 'P' 0.1023 0.0942 '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' _symmetry_cell_setting 'Trigonal' _symmetry_space_group_name_H-M 'P-3 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 11.720(20) _cell_length_b 11.720(2) _cell_length_c 9.5309(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1133.7(19) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11 _cell_measurement_theta_min 4.74 _cell_measurement_theta_max 8.83 _exptl_crystal_description 'hexagon' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.315 _exptl_crystal_density_method ? _exptl_crystal_F_000 1097 _exptl_absorpt_coefficient_mu 7.451 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.3416 _exptl_absorpt_correction_T_max 0.8801 _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 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 5.18 _diffrn_reflns_number 1938 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.1160 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1320 _reflns_number_observed 840 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 12 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R-factor obs. 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 w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0550P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1308 _refine_ls_number_parameters 132 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0939 _refine_ls_R_factor_obs 0.0565 _refine_ls_wR_factor_all 0.1659 _refine_ls_wR_factor_obs 0.1384 _refine_ls_goodness_of_fit_all 1.069 _refine_ls_goodness_of_fit_obs 1.288 _refine_ls_restrained_S_all 1.230 _refine_ls_restrained_S_obs 1.288 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.59828(15) 0.44821(15) 0.9535(2) 0.0255(4) Uani 1 d . . Cu2 Cu 0.5000 0.5000 0.5000 0.0205(5) Uani 1 d S . Cu3 Cu 1.05101(14) 0.69960(15) 0.7308(2) 0.0300(5) Uani 1 d . . P1 P 0.5795(3) 0.6760(3) 0.7795(3) 0.0134(6) Uani 1 d . . P2 P 0.7618(3) 0.5814(3) 0.6841(3) 0.0118(6) Uani 1 d . . Na1 Na 0.6667 0.3333 0.4444(9) 0.014(2) Uani 1 d S . O4 O 0.5415(7) 0.5806(7) 0.9013(9) 0.021(2) Uani 1 d . . O6 O 0.8998(7) 0.6277(7) 0.6272(9) 0.017(2) Uani 1 d . . O5 O 0.7408(7) 0.5058(7) 0.8209(9) 0.019(2) Uani 1 d . . O8 O 0.6667 0.3333 1.0299(15) 0.021(3) Uani 1 d S . H8A H 0.6058 0.2690 1.0748(15) 0.031 Uiso 0.33 d PR . O3 O 0.6602(6) 0.5077(7) 0.5701(9) 0.019(2) Uani 1 d . . O7 O 0.7904(8) 0.8199(8) 0.6176(10) 0.034(2) Uani 1 d . . H7A H 0.7425(8) 0.7842(8) 0.5498(10) 0.051 Uiso 1 calc R . C2 C 0.8394(10) 0.7942(10) 0.8534(14) 0.022(3) Uani 1 d . . H2A H 0.8153(10) 0.7344(10) 0.9312(14) 0.032 Uiso 1 calc R . H2B H 0.8314(10) 0.8689(10) 0.8802(14) 0.032 Uiso 1 calc R . H2C H 0.9288(10) 0.8233(10) 0.8268(14) 0.032 Uiso 1 calc R . C1 C 0.7509(10) 0.7263(9) 0.7333(13) 0.014(2) Uani 1 d . . O2 O 0.4966(7) 0.6118(8) 0.6520(9) 0.024(2) Uani 1 d . . O1 O 0.5728(7) 0.7956(8) 0.8301(10) 0.026(2) Uani 1 d . . O1W O 1.0000 1.0000 0.5000 0.057(9) Uani 1 d S . H1WA H 0.9420 0.9203 0.5157 0.085 Uiso 0.33 d PR . 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 Cu1 0.0327(9) 0.0289(8) 0.0203(9) 0.0101(7) 0.0107(8) 0.0194(7) Cu2 0.0142(9) 0.0340(12) 0.0142(12) -0.0056(10) -0.0037(9) 0.0128(9) Cu3 0.0235(8) 0.0313(9) 0.0305(10) -0.0042(8) -0.0050(8) 0.0102(7) P1 0.0130(13) 0.0195(14) 0.0085(15) 0.0055(13) 0.0039(13) 0.0087(12) P2 0.0126(13) 0.0125(14) 0.009(2) -0.0018(13) 0.0018(13) 0.0055(11) Na1 0.013(2) 0.013(2) 0.016(4) 0.000 0.000 0.0067(10) O4 0.017(4) 0.031(5) 0.018(5) 0.011(4) 0.007(4) 0.014(4) O6 0.012(4) 0.022(4) 0.015(5) -0.005(4) 0.001(4) 0.008(3) O5 0.026(4) 0.018(4) 0.017(5) 0.012(4) 0.015(4) 0.014(4) O8 0.028(4) 0.028(4) 0.006(7) 0.000 0.000 0.014(2) O3 0.009(4) 0.024(4) 0.020(5) -0.016(4) -0.007(4) 0.005(3) O7 0.042(5) 0.031(5) 0.030(6) 0.010(5) 0.015(5) 0.018(4) C2 0.016(5) 0.020(6) 0.028(8) -0.009(6) 0.000(6) 0.008(5) C1 0.016(5) 0.009(5) 0.016(6) 0.008(5) 0.012(5) 0.006(4) O2 0.015(4) 0.040(5) 0.018(5) 0.001(4) 0.001(4) 0.016(4) O1 0.026(4) 0.033(5) 0.025(5) -0.002(4) 0.005(4) 0.019(4) O1W 0.036(8) 0.036(8) 0.098(27) 0.000 0.000 0.018(4) _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 O5 1.927(7) . ? Cu1 O8 2.016(5) . ? Cu1 O4 2.032(7) . ? Cu1 O4 2.040(8) 4_667 ? Cu2 O3 1.952(8) 4_666 ? Cu2 O3 1.952(8) . ? Cu2 O2 1.967(8) . ? Cu2 O2 1.967(8) 4_666 ? Cu2 Cu3 3.045(3) 5_566 ? Cu2 Cu3 3.045(3) 2_655 ? Cu2 Na1 3.424(3) 4_666 ? Cu2 Na1 3.424(3) . ? Cu3 O1 1.822(9) 2_765 ? Cu3 O6 1.825(8) . ? Cu3 Cu2 3.045(2) 3_665 ? P1 O2 1.501(9) . ? P1 O4 1.516(8) . ? P1 O1 1.521(8) . ? P1 C1 1.842(11) . ? P2 O3 1.522(8) . ? P2 O6 1.525(8) . ? P2 O5 1.525(8) . ? P2 C1 1.827(10) . ? P2 Na1 3.416(6) . ? Na1 O3 2.402(9) 3_665 ? Na1 O3 2.402(8) 2_655 ? Na1 O3 2.402(8) . ? Na1 O2 2.481(8) 5_556 ? Na1 O2 2.481(8) 6_656 ? Na1 O2 2.481(8) 4_666 ? Na1 P2 3.416(6) 3_665 ? Na1 P2 3.416(7) 2_655 ? Na1 Cu2 3.4244(14) 2_655 ? Na1 Cu2 3.424(6) 3_665 ? O4 Cu1 2.040(8) 4_667 ? O8 Cu1 2.016(6) 3_665 ? O8 Cu1 2.016(5) 2_655 ? O7 C1 1.458(13) . ? C2 C1 1.48(2) . ? O2 Na1 2.481(8) 4_666 ? O1 Cu3 1.822(8) 3_675 ? 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 Cu1 O8 84.6(4) . . ? O5 Cu1 O4 97.5(3) . . ? O8 Cu1 O4 171.7(4) . . ? O5 Cu1 O4 170.6(3) . 4_667 ? O8 Cu1 O4 101.5(4) . 4_667 ? O4 Cu1 O4 75.5(4) . 4_667 ? O3 Cu2 O3 180.0(1) 4_666 . ? O3 Cu2 O2 86.8(3) 4_666 . ? O3 Cu2 O2 93.2(3) . . ? O3 Cu2 O2 93.2(3) 4_666 4_666 ? O3 Cu2 O2 86.8(3) . 4_666 ? O2 Cu2 O2 180.0 . 4_666 ? O3 Cu2 Cu3 103.0(3) 4_666 5_566 ? O3 Cu2 Cu3 77.0(3) . 5_566 ? O2 Cu2 Cu3 114.6(2) . 5_566 ? O2 Cu2 Cu3 65.4(2) 4_666 5_566 ? O3 Cu2 Cu3 77.0(3) 4_666 2_655 ? O3 Cu2 Cu3 103.0(3) . 2_655 ? O2 Cu2 Cu3 65.4(2) . 2_655 ? O2 Cu2 Cu3 114.6(2) 4_666 2_655 ? Cu3 Cu2 Cu3 180.0 5_566 2_655 ? O3 Cu2 Na1 43.1(2) 4_666 4_666 ? O3 Cu2 Na1 136.9(2) . 4_666 ? O2 Cu2 Na1 45.5(2) . 4_666 ? O2 Cu2 Na1 134.5(2) 4_666 4_666 ? Cu3 Cu2 Na1 106.24(12) 5_566 4_666 ? Cu3 Cu2 Na1 73.76(12) 2_655 4_666 ? O3 Cu2 Na1 136.9(2) 4_666 . ? O3 Cu2 Na1 43.1(2) . . ? O2 Cu2 Na1 134.5(2) . . ? O2 Cu2 Na1 45.5(2) 4_666 . ? Cu3 Cu2 Na1 73.76(12) 5_566 . ? Cu3 Cu2 Na1 106.24(12) 2_655 . ? Na1 Cu2 Na1 180.0 4_666 . ? O1 Cu3 O6 177.8(4) 2_765 . ? O1 Cu3 Cu2 121.6(3) 2_765 3_665 ? O6 Cu3 Cu2 58.8(2) . 3_665 ? O2 P1 O4 111.8(5) . . ? O2 P1 O1 113.6(5) . . ? O4 P1 O1 107.8(5) . . ? O2 P1 C1 107.2(5) . . ? O4 P1 C1 106.9(5) . . ? O1 P1 C1 109.3(4) . . ? O3 P2 O6 109.7(5) . . ? O3 P2 O5 115.3(4) . . ? O6 P2 O5 110.2(4) . . ? O3 P2 C1 108.2(5) . . ? O6 P2 C1 108.3(4) . . ? O5 P2 C1 104.8(5) . . ? O3 P2 Na1 37.8(3) . . ? O6 P2 Na1 84.4(3) . . ? O5 P2 Na1 100.8(3) . . ? C1 P2 Na1 144.9(4) . . ? O3 Na1 O3 97.3(4) 3_665 2_655 ? O3 Na1 O3 97.3(3) 3_665 . ? O3 Na1 O3 97.3(3) 2_655 . ? O3 Na1 O2 89.3(2) 3_665 5_556 ? O3 Na1 O2 66.9(3) 2_655 5_556 ? O3 Na1 O2 163.6(3) . 5_556 ? O3 Na1 O2 66.9(3) 3_665 6_656 ? O3 Na1 O2 163.6(3) 2_655 6_656 ? O3 Na1 O2 89.3(2) . 6_656 ? O2 Na1 O2 107.1(3) 5_556 6_656 ? O3 Na1 O2 163.6(3) 3_665 4_666 ? O3 Na1 O2 89.3(3) 2_655 4_666 ? O3 Na1 O2 66.9(3) . 4_666 ? O2 Na1 O2 107.1(3) 5_556 4_666 ? O2 Na1 O2 107.1(3) 6_656 4_666 ? O3 Na1 P2 22.9(2) 3_665 3_665 ? O3 Na1 P2 74.5(3) 2_655 3_665 ? O3 Na1 P2 100.9(3) . 3_665 ? O2 Na1 P2 79.6(2) 5_556 3_665 ? O2 Na1 P2 89.6(2) 6_656 3_665 ? O2 Na1 P2 158.6(3) 4_666 3_665 ? O3 Na1 P2 100.9(3) 3_665 2_655 ? O3 Na1 P2 22.9(2) 2_655 2_655 ? O3 Na1 P2 74.5(2) . 2_655 ? O2 Na1 P2 89.6(2) 5_556 2_655 ? O2 Na1 P2 158.6(3) 6_656 2_655 ? O2 Na1 P2 79.6(2) 4_666 2_655 ? P2 Na1 P2 80.2(2) 3_665 2_655 ? O3 Na1 P2 74.5(2) 3_665 . ? O3 Na1 P2 100.9(3) 2_655 . ? O3 Na1 P2 22.9(2) . . ? O2 Na1 P2 158.6(3) 5_556 . ? O2 Na1 P2 79.6(2) 6_656 . ? O2 Na1 P2 89.6(2) 4_666 . ? P2 Na1 P2 80.2(2) 3_665 . ? P2 Na1 P2 80.2(2) 2_655 . ? O3 Na1 Cu2 87.1(2) 3_665 2_655 ? O3 Na1 Cu2 33.7(2) 2_655 2_655 ? O3 Na1 Cu2 130.6(3) . 2_655 ? O2 Na1 Cu2 34.4(2) 5_556 2_655 ? O2 Na1 Cu2 135.8(2) 6_656 2_655 ? O2 Na1 Cu2 106.2(2) 4_666 2_655 ? P2 Na1 Cu2 67.51(10) 3_665 2_655 ? P2 Na1 Cu2 56.48(8) 2_655 2_655 ? P2 Na1 Cu2 128.7(2) . 2_655 ? O3 Na1 Cu2 33.7(2) 3_665 3_665 ? O3 Na1 Cu2 130.6(3) 2_655 3_665 ? O3 Na1 Cu2 87.1(2) . 3_665 ? O2 Na1 Cu2 106.2(2) 5_556 3_665 ? O2 Na1 Cu2 34.4(2) 6_656 3_665 ? O2 Na1 Cu2 135.8(2) 4_666 3_665 ? P2 Na1 Cu2 56.48(9) 3_665 3_665 ? P2 Na1 Cu2 128.7(2) 2_655 3_665 ? P2 Na1 Cu2 67.51(9) . 3_665 ? Cu2 Na1 Cu2 117.65(7) 2_655 3_665 ? O3 Na1 Cu2 130.6(3) 3_665 . ? O3 Na1 Cu2 87.1(2) 2_655 . ? O3 Na1 Cu2 33.7(2) . . ? O2 Na1 Cu2 135.8(2) 5_556 . ? O2 Na1 Cu2 106.2(2) 6_656 . ? O2 Na1 Cu2 34.4(2) 4_666 . ? P2 Na1 Cu2 128.7(2) 3_665 . ? P2 Na1 Cu2 67.51(11) 2_655 . ? P2 Na1 Cu2 56.48(9) . . ? Cu2 Na1 Cu2 117.65(10) 2_655 . ? Cu2 Na1 Cu2 117.65(10) 3_665 . ? P1 O4 Cu1 131.5(5) . . ? P1 O4 Cu1 123.9(4) . 4_667 ? Cu1 O4 Cu1 104.5(4) . 4_667 ? P2 O6 Cu3 125.7(5) . . ? P2 O5 Cu1 128.5(4) . . ? Cu1 O8 Cu1 107.7(4) 3_665 2_655 ? Cu1 O8 Cu1 107.7(4) 3_665 . ? Cu1 O8 Cu1 107.7(4) 2_655 . ? P2 O3 Cu2 137.1(5) . . ? P2 O3 Na1 119.3(4) . . ? Cu2 O3 Na1 103.2(3) . . ? O7 C1 C2 107.9(8) . . ? O7 C1 P2 111.2(8) . . ? C2 C1 P2 110.0(8) . . ? O7 C1 P1 107.9(7) . . ? C2 C1 P1 110.2(8) . . ? P2 C1 P1 109.6(5) . . ? P1 O2 Cu2 135.0(5) . . ? P1 O2 Na1 124.0(5) . 4_666 ? Cu2 O2 Na1 100.1(4) . 4_666 ? P1 O1 Cu3 121.3(5) . 3_675 ? _refine_diff_density_max 1.906 _refine_diff_density_min -1.287 _refine_diff_density_rms 0.234