#------------------------------------------------------------------------------ #$Date: 2022-12-21 14:56:43 +0200 (Wed, 21 Dec 2022) $ #$Revision: 279962 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/81/1568136.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1568136 loop_ _publ_author_name 'Zhou, Xiuquan' 'Kolluru, Venkata Surya Chaitanya' 'Xu, Wenqian' 'Wang, Luqing' 'Chang, Tieyan' 'Chen, Yu-Sheng' 'Yu, Lei' 'Wen, Jianguo' 'Chan, Maria K. Y.' 'Chung, Duck Young' 'Kanatzidis, Mercouri G.' _publ_section_title ; Discovery of chalcogenides structures and compositions using mixed fluxes ; _journal_issue 7938 _journal_name_full Nature _journal_page_first 72 _journal_page_last 77 _journal_paper_doi 10.1038/s41586-022-05307-7 _journal_volume 612 _journal_year 2022 _chemical_formula_moiety '0.5(Cu8 Na8.79 O2 Se8)' _chemical_formula_sum 'Cu4 Na4.39 O Se4' _chemical_formula_weight 687.04 _space_group_crystal_system tetragonal _space_group_IT_number 87 _space_group_name_Hall '-I 4' _space_group_name_H-M_alt 'I 4/m' _atom_sites_solution_hydrogens . _atom_sites_solution_primary dual _audit_contact_author_name ; ; _audit_creation_date 2021-08-31 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 11.2320(16) _cell_length_b 11.2320(16) _cell_length_c 4.0301(8) _cell_measurement_reflns_used 1193 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 58.266 _cell_measurement_theta_min 7.256 _cell_volume 508.43(14) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.967 _diffrn_measured_fraction_theta_max 0.967 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_unetI/netI 0.0488 _diffrn_reflns_Laue_measured_fraction_full 0.967 _diffrn_reflns_Laue_measured_fraction_max 0.967 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 2 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_number 380 _diffrn_reflns_point_group_measured_fraction_full 0.967 _diffrn_reflns_point_group_measured_fraction_max 0.967 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.133 _diffrn_reflns_theta_min 3.628 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 22.698 _exptl_absorpt_correction_type none _exptl_crystal_density_diffrn 4.488 _exptl_crystal_description needle _exptl_crystal_F_000 617 _refine_diff_density_max 1.205 _refine_diff_density_min -1.742 _refine_diff_density_rms 0.314 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.884 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 24 _refine_ls_number_reflns 380 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.884 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0384 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0587P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0856 _refine_ls_wR_factor_ref 0.0879 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 277 _reflns_number_total 380 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL i4m_a.res in I4/m i4m.res created by SHELXL-2018/3 at 01:52:34 on 31-Aug-2021 REM Old TITL I4m in I4/m REM SHELXT solution in I4/m: R1 0.080, Rweak 0.008, Alpha 0.019 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: O Na2 Se4 CELL 0.71073 11.232 11.232 4.0301 90 90 90 ZERR 2 0.0016 0.0016 0.0008 0 0 0 LATT 2 SYMM -X,-Y,+Z SYMM -Y,+X,+Z SYMM +Y,-X,+Z SFAC Cu Na O Se UNIT 8 8.79 2 8 L.S. 4 PLAN 20 list 4 fmap 2 acta REM REM REM WGHT 0.058700 FVAR 0.24657 SE01 4 0.718365 0.932370 0.500000 10.50000 0.01785 0.01390 = 0.00931 0.00000 0.00000 0.00115 CU02 1 0.578516 1.096501 0.500000 10.50000 0.03010 0.01750 = 0.01512 0.00000 0.00000 0.00295 NA03 2 0.615294 0.684015 0.500000 10.50000 0.02266 0.01686 = 0.03285 0.00000 0.00000 0.00005 O004 3 0.500000 0.500000 0.500000 10.12500 0.01747 0.01747 = 0.02712 0.00000 0.00000 0.00000 NA00 2 0.500000 0.500000 0.000000 0.04923 0.01864 0.01864 = -0.00111 0.00000 0.00000 0.00000 HKLF 4 REM i4m_a.res in I4/m REM wR2 = 0.0879, GooF = S = 0.884, Restrained GooF = 0.884 for all data REM R1 = 0.0384 for 277 Fo > 4sig(Fo) and 0.0510 for all 380 data REM 24 parameters refined using 0 restraints END WGHT 0.0587 0.0000 REM Highest difference peak 1.205, deepest hole -1.742, 1-sigma level 0.314 Q1 1 0.6825 1.0369 0.5000 10.50000 0.05 1.20 Q2 1 0.4737 1.0632 0.5000 10.50000 0.05 1.02 Q3 1 0.7457 0.8256 0.5000 10.50000 0.05 1.00 Q4 1 0.6215 0.9890 0.5000 10.50000 0.05 0.99 Q5 1 0.6966 1.1517 0.5000 10.50000 0.05 0.91 Q6 1 0.6675 0.8887 0.6141 11.00000 0.05 0.91 Q7 1 0.6195 0.6714 0.0000 10.50000 0.05 0.90 Q8 1 0.6575 0.9785 0.3857 11.00000 0.05 0.88 Q9 1 0.7184 0.5957 0.3937 11.00000 0.05 0.87 Q10 1 0.6121 0.8927 0.5000 10.50000 0.05 0.84 Q11 1 0.7687 0.9017 0.3594 11.00000 0.05 0.77 Q12 1 0.7738 1.0488 0.5000 10.50000 0.05 0.73 Q13 1 0.5565 0.6779 0.5447 11.00000 0.05 0.70 Q14 1 0.4376 1.1193 0.5000 10.50000 0.05 0.70 Q15 1 0.5000 1.0000 0.2500 10.25000 0.05 0.64 Q16 1 0.6728 0.6292 0.7619 11.00000 0.05 0.59 Q17 1 0.7591 0.9882 0.6166 11.00000 0.05 0.59 Q18 1 0.6839 0.7303 0.6402 11.00000 0.05 0.55 Q19 1 0.8549 0.8650 0.5000 10.50000 0.05 0.54 Q20 1 0.4992 0.7760 0.3921 11.00000 0.05 0.54 REM The information below was added by Olex2. REM REM R1 = 0.0384 for 277 Fo > 4sig(Fo) and 0.0510 for all 380 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.20, deepest hole -1.74 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0510 REM R1_gt = 0.0384 REM wR_ref = 0.0879 REM GOOF = 0.884 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 380 REM Reflections_gt = 277 REM Parameters = n/a REM Hole = -1.74 REM Peak = 1.20 REM Flack = n/a ; _cod_data_source_file I_Cu4Na4.4OSe4.cif _cod_data_source_block I _cod_original_cell_volume 508.43(18) _cod_database_code 1568136 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Se01 Se 0.71836(9) 0.93237(9) 0.500000 0.0137(3) Uani 1 2 d S T P . . Cu02 Cu 0.57852(12) 1.09650(12) 0.500000 0.0209(4) Uani 1 2 d S T P . . Na03 Na 0.6153(4) 0.6840(4) 0.500000 0.0241(9) Uani 1 2 d S T P . . O004 O 0.500000 0.500000 0.500000 0.021(3) Uani 1 8 d S T P . . Na00 Na 0.500000 0.500000 0.000000 0.012(6) Uani 0.39(4) 8 d S T 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 Se01 0.0178(6) 0.0139(5) 0.0093(4) 0.000 0.000 0.0012(4) Cu02 0.0301(8) 0.0175(7) 0.0151(5) 0.000 0.000 0.0030(5) Na03 0.023(2) 0.0169(19) 0.033(2) 0.000 0.000 0.0001(16) O004 0.017(4) 0.017(4) 0.027(7) 0.000 0.000 0.000 Na00 0.019(8) 0.019(8) -0.001(8) 0.000 0.000 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.3201 1.2651 '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' O O 0.0106 0.0060 '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' 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 Cu02 Se01 Cu02 70.99(5) . 15_465 Cu02 Se01 Cu02 70.99(5) . 15_466 Cu02 Se01 Cu02 111.41(7) 15_465 15_466 Cu02 Se01 Na03 140.70(9) 15_465 7_655 Cu02 Se01 Na03 150.47(9) 15_466 13_665 Cu02 Se01 Na03 77.05(7) 15_466 13_666 Cu02 Se01 Na03 72.10(7) 15_465 7_654 Cu02 Se01 Na03 73.92(9) . 7_655 Cu02 Se01 Na03 74.85(6) 15_465 . Cu02 Se01 Na03 77.05(7) 15_465 13_665 Cu02 Se01 Na03 74.85(6) 15_466 . Cu02 Se01 Na03 140.70(9) 15_466 7_654 Cu02 Se01 Na03 136.48(6) . 13_666 Cu02 Se01 Na03 72.10(7) 15_466 7_655 Cu02 Se01 Na03 150.47(9) 15_465 13_666 Cu02 Se01 Na03 117.03(10) . . Cu02 Se01 Na03 136.48(6) . 13_665 Cu02 Se01 Na03 73.92(9) . 7_654 Cu02 Se01 Na00 116.93(5) . 5 Cu02 Se01 Na00 123.88(3) 15_466 5 Cu02 Se01 Na00 123.88(3) 15_465 5 Na03 Se01 Na03 138.82(5) . 7_655 Na03 Se01 Na03 82.93(12) 13_666 13_665 Na03 Se01 Na03 80.71(12) . 13_666 Na03 Se01 Na03 68.58(15) 13_666 7_655 Na03 Se01 Na03 120.09(15) 13_666 7_654 Na03 Se01 Na03 80.71(12) . 13_665 Na03 Se01 Na03 81.74(11) 7_655 7_654 Na03 Se01 Na03 68.58(15) 13_665 7_654 Na03 Se01 Na03 138.82(5) . 7_654 Na03 Se01 Na03 120.09(15) 13_665 7_655 Na03 Se01 Na00 126.04(10) . 5 Na03 Se01 Na00 60.22(9) 13_666 5 Na03 Se01 Na00 59.87(8) 7_655 5 Na03 Se01 Na00 59.87(8) 7_654 5 Na03 Se01 Na00 60.22(9) 13_665 5 Se01 Cu02 Se01 117.37(4) . 7_655 Se01 Cu02 Se01 117.37(4) . 7_654 Se01 Cu02 Se01 111.41(7) 7_655 7_654 Se01 Cu02 Cu02 79.57(6) . 9_676 Se01 Cu02 Cu02 113.41(4) . 7_654 Se01 Cu02 Cu02 54.22(5) 7_655 7_655 Se01 Cu02 Cu02 169.84(5) 7_654 15_466 Se01 Cu02 Cu02 54.79(4) . 15_465 Se01 Cu02 Cu02 126.52(7) 7_654 7_655 Se01 Cu02 Cu02 126.52(7) 7_655 7_654 Se01 Cu02 Cu02 169.84(5) 7_655 15_465 Se01 Cu02 Cu02 113.41(4) . 7_655 Se01 Cu02 Cu02 54.79(4) . 15_466 Se01 Cu02 Cu02 78.73(3) 7_654 15_465 Se01 Cu02 Cu02 113.81(5) 7_654 9_676 Se01 Cu02 Cu02 54.22(5) 7_654 7_654 Se01 Cu02 Cu02 78.73(3) 7_655 15_466 Se01 Cu02 Cu02 113.81(5) 7_655 9_676 Se01 Cu02 Na03 178.99(10) . 9_676 Se01 Cu02 Na03 59.35(4) 7_655 11_576 Se01 Cu02 Na03 60.50(7) 7_654 7_654 Se01 Cu02 Na03 119.46(9) . 11_576 Se01 Cu02 Na03 62.06(9) . 7_654 Se01 Cu02 Na03 120.10(8) 7_655 7_654 Se01 Cu02 Na03 62.06(9) . 7_655 Se01 Cu02 Na03 63.01(5) 7_655 9_676 Se01 Cu02 Na03 60.50(7) 7_655 7_655 Se01 Cu02 Na03 59.35(4) 7_654 11_576 Se01 Cu02 Na03 63.01(5) 7_654 9_676 Se01 Cu02 Na03 120.10(8) 7_654 7_655 Cu02 Cu02 Cu02 120.65(3) 7_655 15_465 Cu02 Cu02 Cu02 60.323(16) 9_676 15_466 Cu02 Cu02 Cu02 91.12(6) 15_465 15_466 Cu02 Cu02 Cu02 60.323(16) 9_676 15_465 Cu02 Cu02 Cu02 60.324(16) 9_676 7_655 Cu02 Cu02 Cu02 59.35(3) 7_655 15_466 Cu02 Cu02 Cu02 59.35(3) 7_654 15_465 Cu02 Cu02 Cu02 91.12(6) 7_654 7_655 Cu02 Cu02 Cu02 120.65(3) 7_654 15_466 Cu02 Cu02 Cu02 60.324(16) 9_676 7_654 Cu02 Cu02 Na03 99.42(11) 9_676 9_676 Cu02 Cu02 Na03 124.71(5) 15_466 9_676 Cu02 Cu02 Na03 160.97(11) 9_676 11_576 Cu02 Cu02 Na03 123.47(9) 9_676 7_654 Cu02 Cu02 Na03 63.73(8) 15_466 7_655 Cu02 Cu02 Na03 97.45(5) 7_654 7_654 Cu02 Cu02 Na03 63.73(8) 15_465 7_654 Cu02 Cu02 Na03 171.37(6) 7_655 7_654 Cu02 Cu02 Na03 129.01(5) 15_466 11_576 Cu02 Cu02 Na03 124.71(5) 15_465 9_676 Cu02 Cu02 Na03 65.96(7) 7_654 9_676 Cu02 Cu02 Na03 97.45(5) 7_655 7_655 Cu02 Cu02 Na03 107.86(7) 7_654 11_576 Cu02 Cu02 Na03 107.86(7) 7_655 11_576 Cu02 Cu02 Na03 171.37(6) 7_654 7_655 Cu02 Cu02 Na03 129.01(5) 15_465 11_576 Cu02 Cu02 Na03 123.47(9) 9_676 7_655 Cu02 Cu02 Na03 114.61(10) 15_465 7_655 Cu02 Cu02 Na03 114.61(10) 15_466 7_654 Cu02 Cu02 Na03 65.96(7) 7_655 9_676 Na03 Cu02 Na03 118.68(5) 9_676 7_655 Na03 Cu02 Na03 70.55(12) 7_654 11_576 Na03 Cu02 Na03 73.97(10) 7_655 7_654 Na03 Cu02 Na03 70.55(12) 7_655 11_576 Na03 Cu02 Na03 118.68(5) 9_676 7_654 Na03 Cu02 Na03 61.55(16) 9_676 11_576 Se01 Na03 Se01 97.43(2) 13_666 15_466 Se01 Na03 Se01 99.29(12) . 13_665 Se01 Na03 Se01 174.78(18) 13_665 15_466 Se01 Na03 Se01 174.78(18) 13_666 15_465 Se01 Na03 Se01 82.93(11) 13_666 13_665 Se01 Na03 Se01 85.81(11) . 15_465 Se01 Na03 Se01 99.29(12) . 13_666 Se01 Na03 Se01 81.74(11) 15_465 15_466 Se01 Na03 Se01 85.81(11) . 15_466 Se01 Na03 Se01 97.43(2) 13_665 15_465 Se01 Na03 Cu02 44.66(6) . 15_465 Se01 Na03 Cu02 43.60(6) 13_665 3_755 Se01 Na03 Cu02 44.01(5) 15_465 15_465 Se01 Na03 Cu02 44.66(6) . 15_466 Se01 Na03 Cu02 136.75(7) 13_666 9_676 Se01 Na03 Cu02 88.99(6) 13_666 15_466 Se01 Na03 Cu02 136.75(7) 13_665 9_676 Se01 Na03 Cu02 141.18(17) 13_665 15_466 Se01 Na03 Cu02 44.89(6) 15_465 9_676 Se01 Na03 Cu02 44.89(6) 15_466 9_676 Se01 Na03 Cu02 138.49(7) 15_465 3_755 Se01 Na03 Cu02 138.49(7) 15_466 3_755 Se01 Na03 Cu02 93.90(12) 15_466 15_465 Se01 Na03 Cu02 87.57(13) . 3_755 Se01 Na03 Cu02 43.60(6) 13_666 3_755 Se01 Na03 Cu02 141.18(17) 13_666 15_465 Se01 Na03 Cu02 93.90(12) 15_465 15_466 Se01 Na03 Cu02 63.98(9) . 9_676 Se01 Na03 Cu02 44.01(5) 15_466 15_466 Se01 Na03 Cu02 88.99(6) 13_665 15_465 Se01 Na03 Na00 112.10(15) 15_466 . Se01 Na03 Na00 113.10(14) 13_665 1_556 Se01 Na03 Na00 62.79(6) 15_465 . Se01 Na03 Na00 62.79(6) 15_466 1_556 Se01 Na03 Na00 139.49(6) . . Se01 Na03 Na00 63.19(6) 13_665 . Se01 Na03 Na00 112.10(15) 15_465 1_556 Se01 Na03 Na00 63.19(6) 13_666 1_556 Se01 Na03 Na00 113.11(14) 13_666 . Se01 Na03 Na00 139.49(6) . 1_556 Cu02 Na03 Cu02 50.31(7) 9_676 15_466 Cu02 Na03 Cu02 50.31(7) 9_676 15_465 Cu02 Na03 Cu02 73.97(10) 15_466 15_465 Cu02 Na03 Cu02 109.45(12) 15_465 3_755 Cu02 Na03 Cu02 109.45(12) 15_466 3_755 Cu02 Na03 Cu02 151.55(16) 9_676 3_755 O004 Na03 Se01 86.99(12) . 15_466 O004 Na03 Se01 87.82(11) . 13_665 O004 Na03 Se01 86.99(12) . 15_465 O004 Na03 Se01 87.82(11) . 13_666 O004 Na03 Se01 170.5(2) . . O004 Na03 Cu02 129.89(12) . 15_466 O004 Na03 Cu02 101.96(14) . 3_755 O004 Na03 Cu02 129.89(12) . 15_465 O004 Na03 Cu02 106.49(16) . 9_676 O004 Na03 Na00 39.56(6) . . O004 Na03 Na00 39.56(6) . 1_556 Na00 Na03 Cu02 102.64(12) . 9_676 Na00 Na03 Cu02 99.20(10) . 3_755 Na00 Na03 Cu02 96.39(5) . 15_465 Na00 Na03 Cu02 151.35(16) . 15_466 Na00 Na03 Cu02 151.35(16) 1_556 15_465 Na00 Na03 Cu02 96.39(5) 1_556 15_466 Na00 Na03 Cu02 99.20(10) 1_556 3_755 Na00 Na03 Cu02 102.64(12) 1_556 9_676 Na00 Na03 Na00 79.12(11) . 1_556 Na03 O004 Na03 90.0 . 3_655 Na03 O004 Na03 90.0 9_666 11_566 Na03 O004 Na03 180.0 3_655 11_566 Na03 O004 Na03 90.0 9_666 3_655 Na03 O004 Na03 90.0 . 11_566 Na03 O004 Na03 180.0 . 9_666 Na00 O004 Na03 90.0 . . Na00 O004 Na03 90.0 . 3_655 Na00 O004 Na03 90.0 1_556 . Na00 O004 Na03 90.0 1_556 3_655 Na00 O004 Na03 90.0 . 11_566 Na00 O004 Na03 90.0 1_556 9_666 Na00 O004 Na03 90.0 1_556 11_566 Na00 O004 Na03 90.0 . 9_666 Na00 O004 Na00 180.0 1_556 . Se01 Na00 Se01 180.0 5_444 13_665 Na03 Na00 Se01 56.60(8) 9_666 5_444 Na03 Na00 Se01 122.66(7) 3_654 13_665 Na03 Na00 Se01 57.34(7) 11_565 13_665 Na03 Na00 Se01 123.40(8) 9_665 13_665 Na03 Na00 Se01 56.60(8) 1_554 13_665 Na03 Na00 Se01 122.66(7) 11_565 5_444 Na03 Na00 Se01 57.34(7) 3_655 5_444 Na03 Na00 Se01 56.60(8) 9_665 5_444 Na03 Na00 Se01 56.60(8) . 13_665 Na03 Na00 Se01 122.66(7) 11_566 5_444 Na03 Na00 Se01 57.34(7) 11_566 13_665 Na03 Na00 Se01 57.34(7) 3_654 5_444 Na03 Na00 Se01 123.40(8) 9_666 13_665 Na03 Na00 Se01 122.66(7) 3_655 13_665 Na03 Na00 Se01 123.40(8) . 5_444 Na03 Na00 Se01 123.40(8) 1_554 5_444 Na03 Na00 Na03 100.88(11) 11_566 3_655 Na03 Na00 Na03 100.88(11) 3_654 11_565 Na03 Na00 Na03 180.0 . 9_665 Na03 Na00 Na03 79.12(11) 11_566 11_565 Na03 Na00 Na03 66.07(6) 3_654 1_554 Na03 Na00 Na03 113.93(6) 9_665 3_655 Na03 Na00 Na03 66.07(6) 9_665 11_565 Na03 Na00 Na03 79.12(11) 3_654 3_655 Na03 Na00 Na03 100.88(11) 9_665 1_554 Na03 Na00 Na03 113.93(6) 11_566 1_554 Na03 Na00 Na03 66.07(6) . 3_655 Na03 Na00 Na03 180.0 11_565 3_655 Na03 Na00 Na03 113.93(6) . 3_654 Na03 Na00 Na03 113.93(6) . 11_565 Na03 Na00 Na03 113.93(6) 3_654 9_666 Na03 Na00 Na03 113.93(6) 1_554 3_655 Na03 Na00 Na03 113.93(6) 11_565 9_666 Na03 Na00 Na03 79.12(11) . 1_554 Na03 Na00 Na03 180.0 1_554 9_666 Na03 Na00 Na03 100.88(11) . 9_666 Na03 Na00 Na03 66.07(6) 3_655 9_666 Na03 Na00 Na03 66.07(6) 11_565 1_554 Na03 Na00 Na03 113.93(6) 9_665 11_566 Na03 Na00 Na03 79.12(11) 9_665 9_666 Na03 Na00 Na03 66.07(6) . 11_566 Na03 Na00 Na03 180.0 11_566 3_654 Na03 Na00 Na03 66.07(6) 11_566 9_666 Na03 Na00 Na03 66.07(6) 9_665 3_654 O004 Na00 Se01 90.0 1_554 5_444 O004 Na00 Se01 90.0 . 5_444 O004 Na00 Se01 90.0 . 13_665 O004 Na00 Se01 90.0 1_554 13_665 O004 Na00 Na03 129.56(6) 1_554 3_655 O004 Na00 Na03 129.56(6) 1_554 . O004 Na00 Na03 50.44(6) . . O004 Na00 Na03 50.44(6) . 11_566 O004 Na00 Na03 129.56(6) 1_554 9_666 O004 Na00 Na03 50.44(6) 1_554 11_565 O004 Na00 Na03 50.44(6) 1_554 1_554 O004 Na00 Na03 50.44(6) . 9_666 O004 Na00 Na03 50.44(6) 1_554 3_654 O004 Na00 Na03 129.56(6) . 3_654 O004 Na00 Na03 50.44(6) 1_554 9_665 O004 Na00 Na03 129.56(6) . 11_565 O004 Na00 Na03 50.44(6) . 3_655 O004 Na00 Na03 129.56(6) . 1_554 O004 Na00 Na03 129.56(6) 1_554 11_566 O004 Na00 Na03 129.56(6) . 9_665 O004 Na00 O004 180.0 1_554 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Se01 Cu02 2.4220(17) . Se01 Cu02 2.4391(10) 15_465 Se01 Cu02 2.4391(10) 15_466 Se01 Na03 3.080(4) 7_655 Se01 Na03 3.043(3) 13_666 Se01 Na03 3.043(3) 13_665 Se01 Na03 3.080(4) 7_654 Se01 Na03 3.020(5) . Se01 Na00 3.2533(11) 5 Cu02 Cu02 2.8223(14) 7_655 Cu02 Cu02 2.8223(14) 7_654 Cu02 Cu02 2.8223(14) 15_466 Cu02 Cu02 2.8223(14) 15_465 Cu02 Cu02 2.795(3) 9_676 Cu02 Na03 3.289(5) 9_676 Cu02 Na03 3.447(5) 11_576 Cu02 Na03 3.349(4) 7_655 Cu02 Na03 3.349(4) 7_654 Na03 O004 2.439(5) . Na03 Na00 3.164(4) . Na03 Na00 3.164(4) 1_556 O004 Na00 2.0151(4) 1_556 O004 Na00 2.0151(4) . loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 2 0 146.59 41 1 3 0 367.86 35.5 3 3 0 564.54 25 0 4 0 268.57 22.2 2 4 0 2875.61 42.7 4 4 0 195.88 20.3 -3 5 0 947.21 29.5 1 5 0 32.7 20.3 3 5 0 208.68 25.6 5 5 0 201.08 17.3 -4 6 0 311.07 21.1 -2 6 0 114.39 21.8 0 6 0 2857.81 31.2 2 6 0 25.8 21.1 4 6 0 107.29 25.1 6 6 0 1093.19 23.8 -5 7 0 -5.2 12.5 -3 7 0 41.2 12.4 -1 7 0 3318.17 29 1 7 0 644.04 20.2 3 7 0 359.46 20.4 5 7 0 191.28 17.7 7 7 0 1328.97 20.1 -6 8 0 30.9 11.4 -4 8 0 701.83 17.4 -2 8 0 -5.9 18.2 0 8 0 518.05 18.4 2 8 0 581.64 18.3 4 8 0 749.13 21.5 6 8 0 721.83 18.8 8 8 0 9.8 12.4 -7 9 0 212.48 14.3 -5 9 0 767.92 16.3 -3 9 0 20 15.1 -1 9 0 781.82 19 1 9 0 5.4 13.7 3 9 0 410.76 16.9 5 9 0 516.45 19.8 7 9 0 8.3 17.1 9 9 0 255.27 16.1 -8 10 0 543.05 15.2 -6 10 0 33.9 14.1 -4 10 0 17.8 10.5 -2 10 0 1045.1 21 0 10 0 304.67 16.5 2 10 0 -5.3 13.8 4 10 0 356.16 17.2 6 10 0 557.04 17.2 8 10 0 87.29 19.7 10 10 0 0.3 16.4 -9 11 0 54.89 16.5 -7 11 0 37.5 14.5 -5 11 0 59.49 13.9 -3 11 0 0.4 10.7 -1 11 0 498.25 16.3 1 11 0 531.85 15 3 11 0 53.09 15 5 11 0 316.27 18.4 7 11 0 6.5 16 9 11 0 239.88 20.2 -8 12 0 52.59 14.4 -6 12 0 -0.5 13.9 -4 12 0 19.7 14.4 -2 12 0 26.3 17.1 0 12 0 56.39 14.6 2 12 0 89.09 13.8 4 12 0 14.5 14.3 6 12 0 41.6 15.9 8 12 0 450.75 21.6 -7 13 0 205.38 16.3 -5 13 0 -14.4 14.4 -3 13 0 243.48 14.2 -1 13 0 282.47 15.6 1 13 0 22.2 13.4 3 13 0 7.3 14.5 7 13 0 139.19 18 -6 14 0 5.9 11.8 -4 14 0 80.39 15.6 -2 14 0 12 14.1 0 14 0 187.48 15 2 14 0 55.39 15.8 4 14 0 20.1 16.2 6 14 0 282.27 16.6 -3 15 0 7.7 16.2 -1 15 0 14.4 15.3 1 15 0 21.7 14.7 3 15 0 172.08 17.1 0 1 1 82.79 13.7 -1 2 1 232.18 13.7 1 2 1 824.92 17.2 -2 3 1 2197.98 22.4 0 3 1 709.63 17 2 3 1 2752.92 22.1 -3 4 1 3218.68 24.2 -1 4 1 1095.09 20.1 1 4 1 434.16 15.7 3 4 1 3112.79 25 -4 5 1 88.39 15.4 -2 5 1 264.47 17.1 0 5 1 1450.05 20.8 2 5 1 79.99 10.6 4 5 1 325.77 14.6 -5 6 1 2627.74 22.9 -3 6 1 47.8 17.6 -1 6 1 76.09 15.2 1 6 1 427.26 19.4 3 6 1 342.27 12.5 5 6 1 5.7 10.3 -6 7 1 149.29 15.5 -4 7 1 1026.4 26 -2 7 1 57.59 17.6 0 7 1 27 17 2 7 1 2255.67 26.2 4 7 1 305.47 10.6 6 7 1 204.98 15 -5 8 1 137.19 25.4 -3 8 1 5.2 18.8 -1 8 1 46.3 19.4 1 8 1 7.7 19.6 3 8 1 255.17 10.7 5 8 1 479.95 12.4 7 8 1 24.1 12.3 -8 9 1 121.29 15.8 -6 9 1 209.78 20.9 -4 9 1 1046.8 24.7 -2 9 1 11.7 21.3 0 9 1 307.07 18.8 2 9 1 309.77 26.3 4 9 1 19 13.9 6 9 1 54.99 12.4 8 9 1 72.59 17.3 -9 10 1 53.39 17.5 -7 10 1 26.4 14.1 -5 10 1 144.69 17.7 -3 10 1 1106.99 21.8 -1 10 1 4 16.5 1 10 1 53.29 20 3 10 1 1281.07 25.5 5 10 1 14.5 13.3 7 10 1 3 17.1 9 10 1 168.68 17.8 -10 11 1 4.7 17.5 -8 11 1 320.27 12.8 -6 11 1 -0.4 11.6 -4 11 1 297.37 17.3 -2 11 1 78.19 16.7 0 11 1 105.69 14.9 2 11 1 99.59 19.3 4 11 1 415.86 15.1 6 11 1 382.46 16.2 8 11 1 85.89 18.4 10 11 1 216.78 19.1 -9 12 1 99.29 13.1 -7 12 1 167.78 11.9 -5 12 1 164.38 14.8 -3 12 1 61.59 16.4 -1 12 1 500.45 18.7 1 12 1 72.99 15 3 12 1 9.9 16.8 5 12 1 192.98 15.2 7 12 1 47.1 18.5 9 12 1 4.3 19.7 -6 13 1 232.68 17.4 -4 13 1 252.37 15.4 -2 13 1 4.8 16.6 0 13 1 0.6 15.1 2 13 1 679.23 17.5 4 13 1 2 15.4 6 13 1 26.8 16.4 -5 14 1 294.37 15.6 -3 14 1 21.6 11.7 -1 14 1 50.19 15.9 1 14 1 320.27 16.1 3 14 1 27.7 15.4 5 14 1 217.58 18.2 -2 15 1 114.09 19.5 0 15 1 8.3 18.9 0 0 2 9999 36.7 1 1 2 881.81 13.4 0 2 2 140.89 11.1 2 2 2 313.27 11.4 -1 3 2 1194.58 15.3 1 3 2 199.78 11 3 3 2 262.57 11.5 -2 4 2 456.75 12.1 0 4 2 119.29 10 2 4 2 1506.85 14.6 4 4 2 80.79 9.9 -3 5 2 654.83 12.3 -1 5 2 1076.69 13.9 1 5 2 7.1 10.6 3 5 2 108.49 11.1 5 5 2 86.59 10.4 -4 6 2 232.38 12.7 -2 6 2 64.99 10.6 0 6 2 1962.5 16.8 2 6 2 23.9 11.3 4 6 2 67.79 11.6 6 6 2 726.43 15 -5 7 2 10 10.1 -3 7 2 37.3 13.4 -1 7 2 2359.96 20.7 1 7 2 471.45 14.7 3 7 2 236.58 12.6 5 7 2 156.98 11.7 7 7 2 1019 16 -6 8 2 17.8 14.3 -4 8 2 645.04 18.5 -2 8 2 7.1 15.4 0 8 2 416.66 14.3 2 8 2 489.55 14.5 4 8 2 494.55 14.3 6 8 2 472.85 14.8 8 8 2 9.4 11.4 -3 9 2 17.3 16.9 -1 9 2 620.14 17.2 1 9 2 2.9 14.9 3 9 2 326.17 13.4 5 9 2 376.96 14.6 7 9 2 6.6 13.3 9 9 2 245.08 14.8 -4 10 2 11.5 16.9 -2 10 2 819.42 20.5 0 10 2 218.28 15.6 2 10 2 0.4 14.5 4 10 2 291.87 13.9 6 10 2 424.76 14.2 8 10 2 79.29 12.9 10 10 2 7.1 15 -9 11 2 57.99 20.6 -7 11 2 22 33.2 -5 11 2 69.19 26.5 -3 11 2 3 20.2 -1 11 2 370.16 18.2 1 11 2 426.66 15.8 3 11 2 35.8 15.4 5 11 2 274.87 14.3 7 11 2 7.1 15.1 9 11 2 200.38 19.5 -6 12 2 -2 33.2 -4 12 2 34.6 22.4 -2 12 2 20.9 20 0 12 2 45.6 17.9 2 12 2 81.49 14.4 4 12 2 16.5 15.2 6 12 2 38.8 15 -3 13 2 181.58 17 -1 13 2 232.38 19.8 1 13 2 22.4 15.6 3 13 2 6.6 15.6 5 13 2 14.1 16.5 -2 14 2 6.9 17.4 0 14 2 178.28 19.1 2 14 2 51.19 17.2 0 1 3 62.69 8.6 -1 2 3 77.99 8.4 1 2 3 347.97 11.2 -2 3 3 819.62 12.7 0 3 3 254.77 11 2 3 3 1000.3 12.6 -3 4 3 1462.55 15.2 -1 4 3 460.25 12 1 4 3 188.78 11 3 4 3 1638.44 14.1 -4 5 3 26.3 11.8 -2 5 3 102.89 10.6 0 5 3 628.24 12.4 2 5 3 9.2 8.8 4 5 3 133.99 11 -5 6 3 1234.78 15 -3 6 3 15.1 11.3 -1 6 3 71.99 12.4 1 6 3 243.78 10.8 3 6 3 177.88 10.4 5 6 3 3.9 12.5 -6 7 3 86.19 14.3 -4 7 3 399.66 14.9 -2 7 3 91.59 12.5 0 7 3 19.5 13.3 2 7 3 1359.76 16.1 4 7 3 160.58 13.2 6 7 3 99.79 14.7 -7 8 3 197.18 18.1 -5 8 3 58.59 16.7 -3 8 3 -0.1 14.2 -1 8 3 30 14.7 1 8 3 5.3 13.2 3 8 3 108.69 13.3 5 8 3 338.27 14.9 7 8 3 10.6 16.1 -8 9 3 68.39 19.1 -6 9 3 137.29 19.3 -4 9 3 498.95 16.8 -2 9 3 6.5 16.7 0 9 3 194.58 14.3 2 9 3 130.89 14.7 4 9 3 10 14.9 6 9 3 24.5 15.2 8 9 3 52.89 18.3 -7 10 3 10.8 28.7 -5 10 3 90.79 18.5 -3 10 3 594.94 18.1 -1 10 3 8.1 16.4 1 10 3 10 14.3 3 10 3 694.03 16.2 5 10 3 7.2 15.7 7 10 3 2.3 16.7 -6 11 3 14.3 21.3 -4 11 3 207.58 17.9 -2 11 3 47.4 18.3 0 11 3 84.79 17.4 2 11 3 68.89 16.8 4 11 3 210.08 16.3 6 11 3 249.28 17.5 -3 12 3 36.3 20.3 -1 12 3 365.36 19 1 12 3 52.49 16.1 3 12 3 3.2 16.3 0 0 4 2674.33 16.9 1 1 4 276.07 10.6 0 2 4 32.7 9 2 2 4 135.79 10 -1 3 4 526.45 12 1 3 4 84.79 11 3 3 4 66.09 11.1 -2 4 4 139.29 12.9 0 4 4 14.5 11.2 2 4 4 489.85 13.4 4 4 4 25.6 12 -3 5 4 300.27 12.9 -1 5 4 305.87 14.7 1 5 4 12.2 12.8 3 5 4 37 12.1 5 5 4 11.8 12.9 -4 6 4 111.79 12.6 -2 6 4 20.7 11.2 0 6 4 767.72 15 2 6 4 7.6 12.9 4 6 4 60.69 12.4 6 6 4 310.97 15.9 -5 7 4 5.4 17.2 -3 7 4 8.1 14.6 -1 7 4 868.61 16 1 7 4 217.88 13.3 3 7 4 91.39 14.7 5 7 4 79.09 15.5 7 7 4 498.75 17.5 -6 8 4 15 21.5 -4 8 4 333.47 17.5 -2 8 4 0.6 15.9 0 8 4 190.48 16.5 2 8 4 257.77 15.2 4 8 4 198.48 15.7 6 8 4 191.28 17.7 -5 9 4 270.07 22.4 -3 9 4 2.3 18.6 -1 9 4 280.37 17.1 1 9 4 4.3 17 3 9 4 184.38 18.1 5 9 4 177.48 16.8 -2 10 4 495.65 18.7 0 10 4 75.69 15.9 2 10 4 1.9 17.5 0 1 5 41.4 13.7 -1 2 5 24.2 12.3 1 2 5 154.68 12.9 -2 3 5 213.08 13.7 0 3 5 60.79 15.6 2 3 5 227.98 15.1 -3 4 5 465.45 18 -1 4 5 139.59 15.7 1 4 5 54.59 15 3 4 5 610.74 15.9 -4 5 5 10.3 20.3 -2 5 5 42.4 17.7 0 5 5 209.58 14.8 2 5 5 -0.6 16.9 4 5 5 42.9 15.6 -1 6 5 45.6 17.5 1 6 5 103.79 15.8