data_tp_31c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Bi Cu P2 Se6' _chemical_formula_weight 808.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Bi' 'Bi' -4.1077 10.2566 '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' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 6.5410(9) _cell_length_b 6.5410(9) _cell_length_c 13.263(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 491.43(14) _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 5.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 42.513 _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 1678 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 22.51 _reflns_number_total 220 _reflns_number_gt 193 _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^)+(0.0874P)^2^+5.9745P] 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 220 _refine_ls_number_parameters 17 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1389 _refine_ls_wR_factor_gt 0.1330 _refine_ls_goodness_of_fit_ref 1.232 _refine_ls_restrained_S_all 1.232 _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 Bi Bi 1.3333 0.6667 0.7500 0.0149(8) Uani 1 6 d S . . Se Se 1.3322(3) 0.3031(3) 0.61798(14) 0.0196(9) Uani 1 1 d . . . Cu Cu 1.0000 1.0000 0.7500 0.186(8) Uani 1 6 d S . . P P 1.6667 0.3333 0.6652(6) 0.0102(17) Uani 1 3 d S . . 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 Bi 0.0096(9) 0.0096(9) 0.0256(13) 0.000 0.000 0.0048(4) Se 0.0118(11) 0.0243(13) 0.0266(16) -0.0122(8) -0.0106(7) 0.0119(8) Cu 0.175(11) 0.175(11) 0.209(18) 0.000 0.000 0.087(5) P 0.005(2) 0.005(2) 0.020(4) 0.000 0.000 0.0026(11) _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 Bi Se 2.9502(19) . ? Bi Se 2.9502(19) 3_775 ? Bi Se 2.950(2) 2_755 ? Bi Se 2.9503(19) 6_556 ? Bi Se 2.950(2) 5_756 ? Bi Se 2.9503(19) 4_776 ? Se P 2.187(3) . ? Se Cu 2.7223(19) 1_545 ? Cu Se 2.7222(19) 3_775 ? Cu Se 2.7222(19) 2_655 ? Cu Se 2.7222(19) 1_565 ? Cu Se 2.7223(19) 6_556 ? Cu Se 2.7223(19) 5_766 ? Cu Se 2.7223(19) 4_676 ? P Se 2.187(3) 2_745 ? P Se 2.187(3) 3_875 ? P P 2.251(16) 4_776 ? 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 Se Bi Se 88.38(6) . 3_775 ? Se Bi Se 88.38(6) . 2_755 ? Se Bi Se 88.38(6) 3_775 2_755 ? Se Bi Se 179.76(6) . 6_556 ? Se Bi Se 91.46(7) 3_775 6_556 ? Se Bi Se 91.79(7) 2_755 6_556 ? Se Bi Se 91.46(7) . 5_756 ? Se Bi Se 91.79(7) 3_775 5_756 ? Se Bi Se 179.76(6) 2_755 5_756 ? Se Bi Se 88.37(6) 6_556 5_756 ? Se Bi Se 91.79(7) . 4_776 ? Se Bi Se 179.76(6) 3_775 4_776 ? Se Bi Se 91.46(7) 2_755 4_776 ? Se Bi Se 88.37(6) 6_556 4_776 ? Se Bi Se 88.37(6) 5_756 4_776 ? P Se Cu 106.26(18) . 1_545 ? P Se Bi 99.10(15) . . ? Cu Se Bi 83.38(5) 1_545 . ? Se Cu Se 83.08(5) 3_775 2_655 ? Se Cu Se 83.08(5) 3_775 1_565 ? Se Cu Se 83.08(5) 2_655 1_565 ? Se Cu Se 101.79(8) 3_775 6_556 ? Se Cu Se 173.05(8) 2_655 6_556 ? Se Cu Se 92.53(7) 1_565 6_556 ? Se Cu Se 173.05(8) 3_775 5_766 ? Se Cu Se 92.53(7) 2_655 5_766 ? Se Cu Se 101.79(8) 1_565 5_766 ? Se Cu Se 83.07(5) 6_556 5_766 ? Se Cu Se 92.53(7) 3_775 4_676 ? Se Cu Se 101.79(8) 2_655 4_676 ? Se Cu Se 173.05(8) 1_565 4_676 ? Se Cu Se 83.07(5) 6_556 4_676 ? Se Cu Se 83.07(5) 5_766 4_676 ? Se P Se 112.16(19) 2_745 3_875 ? Se P Se 112.16(19) 2_745 . ? Se P Se 112.16(19) 3_875 . ? Se P P 106.6(2) 2_745 4_776 ? Se P P 106.6(2) 3_875 4_776 ? Se P P 106.6(2) . 4_776 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.989 _refine_diff_density_min -1.819 _refine_diff_density_rms 0.409