data_peter _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H6 Ca0.44 Ce0.56 Cu6 O21 P3' _chemical_formula_weight 912.30 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' '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' 'Ce' 'Ce' -0.2486 2.6331 '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' 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 13.2197(18) _cell_length_b 13.2197(18) _cell_length_c 5.8591(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 886.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 869 _exptl_absorpt_coefficient_mu 8.972 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4503 _diffrn_reflns_av_R_equivalents 0.0745 _diffrn_reflns_av_sigmaI/netI 0.0771 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 32.60 _reflns_number_total 1167 _reflns_number_gt 754 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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 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^)+(0.0332P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1167 _refine_ls_number_parameters 56 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0855 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ce Ce 0.6667 0.3333 0.2500 0.0092(3) Uani 0.564(5) 6 d SP . . Ca Ca 0.6667 0.3333 0.2500 0.0092(3) Uani 0.436(5) 6 d SP . . Cu Cu 0.41203(5) 0.31488(5) 0.50330(10) 0.01122(17) Uani 1 1 d . . . P P 0.49310(14) 0.14867(14) 0.7500 0.0066(3) Uani 1 2 d S . . O1 O 0.3903(4) 0.4041(4) 0.2500 0.0119(10) Uani 1 2 d S . . O2 O 0.4175(4) 0.2104(4) 0.7500 0.0106(9) Uani 1 2 d S . . O3 O 0.5665(3) 0.1782(3) 0.5357(5) 0.0127(7) Uani 1 1 d . . . O4 O 0.3639(4) 0.3745(4) 0.7500 0.0095(9) Uani 1 2 d S . . O5 O 0.4446(5) 0.2468(4) 0.2500 0.0153(11) Uani 1 2 d S . . WAT O 0.131(2) 0.160(3) 0.124(5) 0.273(17) Uiso 0.50 1 d P . . 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 Ce 0.0097(3) 0.0097(3) 0.0082(5) 0.000 0.000 0.00483(16) Ca 0.0097(3) 0.0097(3) 0.0082(5) 0.000 0.000 0.00483(16) Cu 0.0193(3) 0.0147(3) 0.0054(3) 0.0003(2) 0.0006(3) 0.0128(2) P 0.0079(7) 0.0065(7) 0.0051(8) 0.000 0.000 0.0033(6) O1 0.015(2) 0.016(2) 0.008(2) 0.000 0.000 0.010(2) O2 0.017(2) 0.011(2) 0.008(2) 0.000 0.000 0.010(2) O3 0.0151(16) 0.0122(15) 0.0116(18) 0.0012(13) 0.0044(14) 0.0075(14) O4 0.014(2) 0.017(2) 0.003(2) 0.000 0.000 0.012(2) O5 0.030(3) 0.019(3) 0.004(2) 0.000 0.000 0.017(2) _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 Ce O3 2.459(3) 2_655 ? Ce O3 2.459(3) 10_556 ? Ce O3 2.459(3) 11_656 ? Ce O3 2.459(3) . ? Ce O3 2.459(3) 3_665 ? Ce O3 2.459(3) 12_666 ? Ce O5 2.563(5) 2_655 ? Ce O5 2.563(5) 3_665 ? Ce O5 2.563(5) . ? Ce Cu 3.5738(7) 11_656 ? Ce Cu 3.5738(7) 2_655 ? Ce Cu 3.5738(7) 3_665 ? Cu O5 1.893(3) . ? Cu O4 1.902(3) . ? Cu O1 2.004(3) . ? Cu O2 2.025(3) . ? Cu O3 2.307(3) 3_665 ? Cu Cu 2.8908(12) 10_557 ? Cu Cu 2.9683(12) 10_556 ? P O3 1.514(3) 10_557 ? P O3 1.514(3) . ? P O1 1.570(5) 8_556 ? P O2 1.575(5) . ? O1 P 1.570(5) 9_556 ? O1 Cu 2.004(3) 10_556 ? O2 Cu 2.025(3) 10_557 ? O3 Cu 2.307(3) 2_655 ? O4 Cu 1.902(3) 10_557 ? O5 Cu 1.893(3) 10_556 ? WAT WAT 1.48(6) 10_556 ? 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 O3 Ce O3 137.03(6) 2_655 10_556 ? O3 Ce O3 85.79(15) 2_655 11_656 ? O3 Ce O3 78.76(12) 10_556 11_656 ? O3 Ce O3 78.76(12) 2_655 . ? O3 Ce O3 85.79(15) 10_556 . ? O3 Ce O3 137.03(6) 11_656 . ? O3 Ce O3 78.76(12) 2_655 3_665 ? O3 Ce O3 137.03(6) 10_556 3_665 ? O3 Ce O3 137.03(6) 11_656 3_665 ? O3 Ce O3 78.76(12) . 3_665 ? O3 Ce O3 137.03(6) 2_655 12_666 ? O3 Ce O3 78.76(12) 10_556 12_666 ? O3 Ce O3 78.76(12) 11_656 12_666 ? O3 Ce O3 137.03(6) . 12_666 ? O3 Ce O3 85.79(15) 3_665 12_666 ? O3 Ce O5 66.98(11) 2_655 2_655 ? O3 Ce O5 70.06(11) 10_556 2_655 ? O3 Ce O5 66.98(11) 11_656 2_655 ? O3 Ce O5 70.06(11) . 2_655 ? O3 Ce O5 137.05(8) 3_665 2_655 ? O3 Ce O5 137.06(8) 12_666 2_655 ? O3 Ce O5 70.06(11) 2_655 3_665 ? O3 Ce O5 137.05(8) 10_556 3_665 ? O3 Ce O5 70.06(11) 11_656 3_665 ? O3 Ce O5 137.05(8) . 3_665 ? O3 Ce O5 66.98(11) 3_665 3_665 ? O3 Ce O5 66.98(11) 12_666 3_665 ? O5 Ce O5 120.0 2_655 3_665 ? O3 Ce O5 137.05(8) 2_655 . ? O3 Ce O5 66.98(11) 10_556 . ? O3 Ce O5 137.05(8) 11_656 . ? O3 Ce O5 66.98(11) . . ? O3 Ce O5 70.06(11) 3_665 . ? O3 Ce O5 70.06(11) 12_666 . ? O5 Ce O5 120.0 2_655 . ? O5 Ce O5 120.0 3_665 . ? O3 Ce Cu 97.46(8) 2_655 11_656 ? O3 Ce Cu 39.82(8) 10_556 11_656 ? O3 Ce Cu 64.18(8) 11_656 11_656 ? O3 Ce Cu 78.31(8) . 11_656 ? O3 Ce Cu 157.05(8) 3_665 11_656 ? O3 Ce Cu 110.82(8) 12_666 11_656 ? O5 Ce Cu 30.67(6) 2_655 11_656 ? O5 Ce Cu 133.36(9) 3_665 11_656 ? O5 Ce Cu 99.99(9) . 11_656 ? O3 Ce Cu 64.18(8) 2_655 2_655 ? O3 Ce Cu 78.31(8) 10_556 2_655 ? O3 Ce Cu 97.46(8) 11_656 2_655 ? O3 Ce Cu 39.82(8) . 2_655 ? O3 Ce Cu 110.82(8) 3_665 2_655 ? O3 Ce Cu 157.05(8) 12_666 2_655 ? O5 Ce Cu 30.67(6) 2_655 2_655 ? O5 Ce Cu 133.36(9) 3_665 2_655 ? O5 Ce Cu 99.99(9) . 2_655 ? Cu Ce Cu 49.07(2) 11_656 2_655 ? O3 Ce Cu 39.82(8) 2_655 3_665 ? O3 Ce Cu 157.05(8) 10_556 3_665 ? O3 Ce Cu 78.31(8) 11_656 3_665 ? O3 Ce Cu 110.82(8) . 3_665 ? O3 Ce Cu 64.18(8) 3_665 3_665 ? O3 Ce Cu 97.46(8) 12_666 3_665 ? O5 Ce Cu 99.99(9) 2_655 3_665 ? O5 Ce Cu 30.67(6) 3_665 3_665 ? O5 Ce Cu 133.36(9) . 3_665 ? Cu Ce Cu 125.890(5) 11_656 3_665 ? Cu Ce Cu 103.964(12) 2_655 3_665 ? O5 Cu O4 174.5(2) . . ? O5 Cu O1 80.36(15) . . ? O4 Cu O1 98.21(15) . . ? O5 Cu O2 98.12(15) . . ? O4 Cu O2 82.75(14) . . ? O1 Cu O2 174.00(18) . . ? O5 Cu O3 86.14(18) . 3_665 ? O4 Cu O3 99.33(17) . 3_665 ? O1 Cu O3 96.48(16) . 3_665 ? O2 Cu O3 89.19(16) . 3_665 ? O5 Cu Cu 141.62(11) . 10_557 ? O4 Cu Cu 40.55(10) . 10_557 ? O1 Cu Cu 137.79(10) . 10_557 ? O2 Cu Cu 44.46(9) . 10_557 ? O3 Cu Cu 85.29(8) 3_665 10_557 ? O5 Cu Cu 38.38(11) . 10_556 ? O4 Cu Cu 139.45(10) . 10_556 ? O1 Cu Cu 42.21(10) . 10_556 ? O2 Cu Cu 135.54(9) . 10_556 ? O3 Cu Cu 94.71(8) 3_665 10_556 ? Cu Cu Cu 180.00(5) 10_557 10_556 ? O5 Cu Ce 43.67(15) . . ? O4 Cu Ce 141.84(14) . . ? O1 Cu Ce 93.42(12) . . ? O2 Cu Ce 89.38(12) . . ? O3 Cu Ce 43.06(8) 3_665 . ? Cu Cu Ce 114.537(10) 10_557 . ? Cu Cu Ce 65.463(10) 10_556 . ? O3 P O3 112.1(3) 10_557 . ? O3 P O1 108.20(17) 10_557 8_556 ? O3 P O1 108.20(17) . 8_556 ? O3 P O2 110.95(17) 10_557 . ? O3 P O2 110.95(17) . . ? O1 P O2 106.2(2) 8_556 . ? P O1 Cu 131.59(11) 9_556 10_556 ? P O1 Cu 131.59(11) 9_556 . ? Cu O1 Cu 95.6(2) 10_556 . ? P O2 Cu 127.00(16) . 10_557 ? P O2 Cu 127.00(16) . . ? Cu O2 Cu 91.07(17) 10_557 . ? P O3 Cu 116.46(19) . 2_655 ? P O3 Ce 142.0(2) . . ? Cu O3 Ce 97.12(12) 2_655 . ? Cu O4 Cu 98.9(2) . 10_557 ? Cu O5 Cu 103.2(2) . 10_556 ? Cu O5 Ce 105.66(18) . . ? Cu O5 Ce 105.66(18) 10_556 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 32.60 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.351 _refine_diff_density_min -1.004 _refine_diff_density_rms 0.255