#------------------------------------------------------------------------------ #$Date: 2023-10-27 03:59:32 +0300 (Fri, 27 Oct 2023) $ #$Revision: 287133 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/75/7247586.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_7247586 loop_ _publ_author_name 'Zhang, Lirong' 'Zhao, Huiling' 'Liu, Xin' 'Teri, Gele' 'Baiyin, Menghe' _publ_section_title ; Syntheses, crystal structure, and photoelectric properties of two Zn-based chalcogenidoantimonates Zn-Sb-Q (Q = S, Se). ; _journal_name_full 'Physical chemistry chemical physics : PCCP' _journal_paper_doi 10.1039/d3cp04074g _journal_year 2023 _chemical_formula_moiety '2(C12 H32 N8 Sb2 Se5 Zn2)' _chemical_formula_sum 'C24 H64 N16 Sb4 Se10 Zn4' _chemical_formula_weight 2114.99 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-04-11 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2023-07-09 deposited with the CCDC. 2023-10-23 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.921(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 30.4965(11) _cell_length_b 7.8250(2) _cell_length_c 23.6797(8) _cell_measurement_reflns_used 8742 _cell_measurement_temperature 301(2) _cell_measurement_theta_max 20.48 _cell_measurement_theta_min 2.50 _cell_volume 5630.0(3) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _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 301.0 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1320 _diffrn_reflns_av_unetI/netI 0.0744 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_number 97277 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.090 _diffrn_reflns_theta_min 2.093 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 10.064 _exptl_absorpt_correction_T_max 0.7463 _exptl_absorpt_correction_T_min 0.5637 _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.495 _exptl_crystal_description block _exptl_crystal_F_000 3936 _refine_diff_density_max 0.974 _refine_diff_density_min -0.999 _refine_diff_density_rms 0.199 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 262 _refine_ls_number_reflns 9799 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.076 _refine_ls_R_factor_all 0.1100 _refine_ls_R_factor_gt 0.0418 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0057P)^2^+22.1091P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.0874 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5380 _reflns_number_total 9799 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL mo_t_20230411_f_300k_0m_a.res in C2/c mo_t_20230411_f_300k_0m.res created by SHELXL-2018/3 at 16:25:03 on 11-Apr-2023 REM Old TITL mo_T_20230411_F_300K_0m in C2/c REM SHELXT solution in C2/c: R1 0.137, Rweak 0.005, Alpha 0.020 REM 0.193 for 441 systematic absences, Orientation as input REM Formula found by SHELXT: C13 N7 Zn7 Sb2 CELL 0.71073 30.4965 7.825 23.6797 90 94.921 90 ZERR 4 0.0011 0.0002 0.0008 0 0.002 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H N Sb Se Zn UNIT 96 256 64 16 40 16 L.S. 20 0 0 PLAN 20 TEMP 27.85 list 4 fmap 2 53 acta REM REM REM WGHT 0.005700 22.109100 FVAR 0.06930 SB1 4 0.665156 0.687598 0.275062 11.00000 0.03638 0.03715 = 0.03285 0.00044 0.00389 -0.00246 SB2 4 0.549537 0.814927 0.195362 11.00000 0.03378 0.03725 = 0.03510 0.00242 -0.00266 0.00256 SE03 5 0.583497 0.580115 0.263230 11.00000 0.03956 0.03253 = 0.03451 0.00395 0.00459 -0.00129 SE1 5 0.703480 0.396764 0.270641 11.00000 0.03716 0.04437 = 0.03175 -0.00215 0.00080 0.00222 ZN1 6 0.686880 0.333261 0.168251 11.00000 0.03637 0.03165 = 0.03305 -0.00188 0.00340 0.00245 SE4 5 0.585759 1.082401 0.236262 11.00000 0.08101 0.03502 = 0.03257 -0.00343 0.01741 -0.00815 ZN2 6 0.571914 1.116279 0.336634 11.00000 0.03765 0.03824 = 0.02824 -0.00132 0.00478 -0.00099 SE2 5 0.671058 0.737091 0.379644 11.00000 0.04207 0.07490 = 0.03747 -0.01575 -0.00430 0.01294 SE3 5 0.590612 0.793859 0.109987 11.00000 0.10278 0.03994 = 0.03052 0.00275 0.01807 0.00547 N2 3 0.680795 0.281235 0.066357 11.00000 0.03754 0.02947 = 0.03364 -0.00261 0.00304 0.00341 N8 3 0.562995 0.878458 0.372108 11.00000 0.03967 0.03437 = 0.03355 -0.00384 0.00287 -0.00096 AFIX 23 H8A 2 0.545347 0.817034 0.348072 11.00000 -1.20000 H8B 2 0.588878 0.825375 0.376355 11.00000 -1.20000 AFIX 0 N4 3 0.621941 0.386849 0.144946 11.00000 0.04125 0.04110 = 0.03777 0.00277 0.01056 0.00810 AFIX 23 H4A 2 0.605771 0.347533 0.171679 11.00000 -1.20000 H4B 2 0.618570 0.499784 0.143485 11.00000 -1.20000 AFIX 0 N1 3 0.696810 0.072424 0.163360 11.00000 0.04256 0.03571 = 0.04232 0.00675 -0.00420 0.00440 AFIX 23 H1A 2 0.716396 0.040674 0.191427 11.00000 -1.20000 H1B 2 0.671640 0.018854 0.168077 11.00000 -1.20000 AFIX 0 N6 3 0.518063 1.286467 0.329422 11.00000 0.04365 0.04326 = 0.04817 0.01009 0.00285 -0.00403 AFIX 23 H6A 2 0.521120 1.357700 0.300723 11.00000 -1.20000 H6B 2 0.493416 1.227144 0.321390 11.00000 -1.20000 AFIX 0 N3 3 0.734072 0.498577 0.137122 11.00000 0.05034 0.04226 = 0.04060 -0.01208 0.00439 -0.00956 AFIX 23 H3A 2 0.734849 0.594996 0.157119 11.00000 -1.20000 H3B 2 0.760463 0.449853 0.142614 11.00000 -1.20000 AFIX 0 N7 3 0.564380 1.186354 0.432185 11.00000 0.05242 0.03742 = 0.03293 -0.00611 0.00810 -0.00333 N5 3 0.634422 1.212766 0.362865 11.00000 0.04847 0.12151 = 0.04075 0.00171 0.00274 -0.03498 C1 1 0.712472 0.019431 0.109252 11.00000 0.04674 0.02744 = 0.05911 -0.00415 0.00290 0.00842 AFIX 23 H1C 2 0.711701 -0.104236 0.106525 11.00000 -1.20000 H1D 2 0.742732 0.056015 0.107675 11.00000 -1.20000 AFIX 0 C5 1 0.637840 0.347633 0.046930 11.00000 0.04636 0.04568 = 0.02742 0.00124 -0.00488 0.00492 AFIX 23 H5A 2 0.627818 0.294377 0.011140 11.00000 -1.20000 H5B 2 0.639949 0.469743 0.040650 11.00000 -1.20000 AFIX 0 C11 1 0.544442 0.882553 0.426546 11.00000 0.05299 0.04825 = 0.03673 0.00748 0.00995 -0.00832 AFIX 23 H11A 2 0.549702 0.773867 0.445635 11.00000 -1.20000 H11B 2 0.512874 0.899556 0.420657 11.00000 -1.20000 AFIX 0 C2 1 0.684268 0.095741 0.059768 11.00000 0.04527 0.03334 = 0.04603 -0.01024 0.00180 -0.00026 AFIX 23 H2A 2 0.697192 0.070073 0.024712 11.00000 -1.20000 H2B 2 0.655128 0.045234 0.057726 11.00000 -1.20000 AFIX 0 C8 1 0.513968 1.386036 0.380922 11.00000 0.06763 0.04385 = 0.06687 -0.00330 0.03041 0.01332 AFIX 23 H8C 2 0.484597 1.434140 0.379919 11.00000 -1.20000 H8D 2 0.534832 1.479830 0.382426 11.00000 -1.20000 AFIX 0 C3 1 0.725547 0.540961 0.076686 11.00000 0.05477 0.04540 = 0.04255 0.00055 0.01152 -0.00990 AFIX 23 H3C 2 0.750837 0.598638 0.063303 11.00000 -1.20000 H3D 2 0.700292 0.616289 0.071017 11.00000 -1.20000 AFIX 0 C12 1 0.716664 0.374987 0.044178 11.00000 0.04769 0.04354 = 0.02948 -0.00452 0.01153 0.00380 AFIX 23 H12A 2 0.709228 0.400280 0.004407 11.00000 -1.20000 H12B 2 0.743025 0.305063 0.047203 11.00000 -1.20000 AFIX 0 C4 1 0.604794 0.313706 0.089775 11.00000 0.03121 0.04723 = 0.05307 -0.00598 0.00178 0.00153 AFIX 23 H4C 2 0.576775 0.365882 0.077288 11.00000 -1.20000 H4D 2 0.600305 0.191654 0.093539 11.00000 -1.20000 AFIX 0 C10 1 0.564397 1.022718 0.462890 11.00000 0.06726 0.05476 = 0.02522 -0.00192 0.00584 -0.00987 AFIX 23 H10A 2 0.548007 1.035647 0.495972 11.00000 -1.20000 H10B 2 0.594421 0.992335 0.475852 11.00000 -1.20000 AFIX 0 C6 1 0.644065 1.235577 0.423983 11.00000 0.04369 0.07560 = 0.05326 -0.00282 -0.00540 -0.01484 C9 1 0.522399 1.277588 0.433206 11.00000 0.07328 0.05613 = 0.05356 -0.00457 0.02665 0.01172 AFIX 23 H9A 2 0.523186 1.349492 0.466646 11.00000 -1.20000 H9B 2 0.498672 1.195794 0.435119 11.00000 -1.20000 AFIX 0 C7 1 0.603010 1.291692 0.450314 11.00000 0.09254 0.05466 = 0.04330 -0.01258 -0.00721 -0.02905 AFIX 23 H7A 2 0.608307 1.285910 0.491249 11.00000 -1.20000 H7B 2 0.596767 1.409802 0.440109 11.00000 -1.20000 AFIX 0 HKLF 4 REM mo_t_20230411_f_300k_0m_a.res in C2/c REM wR2 = 0.0874, GooF = S = 1.076, Restrained GooF = 1.076 for all data REM R1 = 0.0418 for 5380 Fo > 4sig(Fo) and 0.1100 for all 9799 data REM 262 parameters refined using 0 restraints END WGHT 0.0056 22.0928 REM Highest difference peak 0.974, deepest hole -0.999, 1-sigma level 0.199 Q1 1 0.7976 0.4238 0.1605 11.00000 0.05 0.97 Q2 1 0.6597 1.2523 0.3598 11.00000 0.05 0.85 Q3 1 0.5405 1.3963 0.2433 11.00000 0.05 0.76 Q4 1 0.5624 1.1964 0.3815 11.00000 0.05 0.75 Q5 1 0.5995 1.0052 0.3021 11.00000 0.05 0.74 Q6 1 0.7018 -0.0357 0.2642 11.00000 0.05 0.71 Q7 1 0.6628 0.7820 0.2776 11.00000 0.05 0.70 Q8 1 0.5976 0.6150 0.3212 11.00000 0.05 0.69 Q9 1 0.6394 1.3405 0.3780 11.00000 0.05 0.69 Q10 1 0.8009 0.4013 0.2018 11.00000 0.05 0.68 Q11 1 0.5795 0.8113 0.3199 11.00000 0.05 0.68 Q12 1 0.7607 0.6750 0.1625 11.00000 0.05 0.68 Q13 1 0.6568 1.3788 0.4377 11.00000 0.05 0.67 Q14 1 0.6211 0.7126 0.1400 11.00000 0.05 0.66 Q15 1 0.6385 1.1989 0.5211 11.00000 0.05 0.66 Q16 1 0.6775 0.7623 0.3605 11.00000 0.05 0.63 Q17 1 0.5404 0.6917 0.0781 11.00000 0.05 0.63 Q18 1 0.7029 0.6430 0.2568 11.00000 0.05 0.61 Q19 1 0.6781 0.6960 0.2755 11.00000 0.05 0.61 Q20 1 0.5785 0.1867 0.0206 11.00000 0.05 0.61 REM The information below was added by Olex2. REM REM R1 = 0.0418 for 5380 Fo > 4sig(Fo) and 0.1100 for all 101403 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.97, deepest hole -1.00 REM Mean Shift 0, Max Shift 0.002. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1100 REM R1_gt = 0.0418 REM wR_ref = 0.0874 REM GOOF = 1.076 REM Shift_max = 0.002 REM Shift_mean = 0 REM Reflections_all = 101403 REM Reflections_gt = 5380 REM Parameters = n/a REM Hole = -1.00 REM Peak = 0.97 REM Flack = n/a ; _cod_data_source_file d3cp04074g2.cif _cod_data_source_block mo_t_20230411_f_300k_0m _cod_database_code 7247586 _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 ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups, All N(H,H) groups 2.a Secondary CH2 refined with riding coordinates: N8(H8A,H8B), N4(H4A,H4B), N1(H1A,H1B), N6(H6A,H6B), N3(H3A,H3B), C1(H1C,H1D), C5(H5A,H5B), C11(H11A,H11B), C2(H2A,H2B), C8(H8C,H8D), C3(H3C,H3D), C12(H12A, H12B), C4(H4C,H4D), C10(H10A,H10B), C9(H9A,H9B), C7(H7A,H7B) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+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 Sb1 Sb 0.66516(2) 0.68760(4) 0.27506(2) 0.03541(9) Uani 1 1 d . . . . . Sb2 Sb 0.54954(2) 0.81493(4) 0.19536(2) 0.03570(9) Uani 1 1 d . . . . . Se03 Se 0.58350(2) 0.58011(6) 0.26323(2) 0.03545(13) Uani 1 1 d . . . . . Se1 Se 0.70348(2) 0.39676(7) 0.27064(2) 0.03788(13) Uani 1 1 d . . . . . Zn1 Zn 0.68688(2) 0.33326(7) 0.16825(3) 0.03366(14) Uani 1 1 d . . . . . Se4 Se 0.58576(2) 1.08240(7) 0.23626(2) 0.04881(16) Uani 1 1 d . . . . . Zn2 Zn 0.57191(2) 1.11628(7) 0.33663(2) 0.03460(14) Uani 1 1 d . . . . . Se2 Se 0.67106(2) 0.73709(9) 0.37964(3) 0.05193(17) Uani 1 1 d . . . . . Se3 Se 0.59061(3) 0.79386(7) 0.10999(2) 0.05704(19) Uani 1 1 d . . . . . N2 N 0.68079(14) 0.2812(5) 0.06636(17) 0.0335(10) Uani 1 1 d . . . . . N8 N 0.56299(14) 0.8785(5) 0.37211(17) 0.0359(10) Uani 1 1 d . . . . . H8A H 0.545347 0.817034 0.348072 0.043 Uiso 1 1 calc R . . . . H8B H 0.588878 0.825375 0.376355 0.043 Uiso 1 1 calc R . . . . N4 N 0.62194(14) 0.3868(5) 0.14495(18) 0.0396(11) Uani 1 1 d . . . . . H4A H 0.605771 0.347533 0.171679 0.048 Uiso 1 1 calc R . . . . H4B H 0.618570 0.499784 0.143485 0.048 Uiso 1 1 calc R . . . . N1 N 0.69681(15) 0.0724(5) 0.16336(18) 0.0406(11) Uani 1 1 d . . . . . H1A H 0.716396 0.040674 0.191427 0.049 Uiso 1 1 calc R . . . . H1B H 0.671640 0.018854 0.168077 0.049 Uiso 1 1 calc R . . . . N6 N 0.51806(16) 1.2865(6) 0.3294(2) 0.0451(11) Uani 1 1 d . . . . . H6A H 0.521120 1.357700 0.300723 0.054 Uiso 1 1 calc R . . . . H6B H 0.493416 1.227144 0.321390 0.054 Uiso 1 1 calc R . . . . N3 N 0.73407(16) 0.4986(6) 0.13712(18) 0.0444(11) Uani 1 1 d . . . . . H3A H 0.734849 0.594996 0.157119 0.053 Uiso 1 1 calc R . . . . H3B H 0.760463 0.449853 0.142614 0.053 Uiso 1 1 calc R . . . . N7 N 0.56438(16) 1.1864(5) 0.43218(18) 0.0407(11) Uani 1 1 d . . . . . N5 N 0.63442(18) 1.2128(8) 0.3629(2) 0.0703(17) Uani 1 1 d . . . . . C1 C 0.71247(19) 0.0194(6) 0.1093(2) 0.0445(14) Uani 1 1 d . . . . . H1C H 0.711701 -0.104236 0.106525 0.053 Uiso 1 1 calc R . . . . H1D H 0.742732 0.056015 0.107675 0.053 Uiso 1 1 calc R . . . . C5 C 0.63784(18) 0.3476(7) 0.0469(2) 0.0403(13) Uani 1 1 d . . . . . H5A H 0.627818 0.294377 0.011140 0.048 Uiso 1 1 calc R . . . . H5B H 0.639949 0.469743 0.040650 0.048 Uiso 1 1 calc R . . . . C11 C 0.5444(2) 0.8826(7) 0.4265(2) 0.0456(14) Uani 1 1 d . . . . . H11A H 0.549702 0.773867 0.445635 0.055 Uiso 1 1 calc R . . . . H11B H 0.512874 0.899556 0.420657 0.055 Uiso 1 1 calc R . . . . C2 C 0.68427(19) 0.0957(6) 0.0598(2) 0.0417(13) Uani 1 1 d . . . . . H2A H 0.697192 0.070073 0.024712 0.050 Uiso 1 1 calc R . . . . H2B H 0.655128 0.045234 0.057726 0.050 Uiso 1 1 calc R . . . . C8 C 0.5140(2) 1.3860(7) 0.3809(3) 0.0580(18) Uani 1 1 d . . . . . H8C H 0.484597 1.434140 0.379919 0.070 Uiso 1 1 calc R . . . . H8D H 0.534832 1.479830 0.382426 0.070 Uiso 1 1 calc R . . . . C3 C 0.7255(2) 0.5410(7) 0.0767(2) 0.0472(14) Uani 1 1 d . . . . . H3C H 0.750837 0.598638 0.063303 0.057 Uiso 1 1 calc R . . . . H3D H 0.700292 0.616289 0.071017 0.057 Uiso 1 1 calc R . . . . C12 C 0.71666(19) 0.3750(6) 0.0442(2) 0.0398(13) Uani 1 1 d . . . . . H12A H 0.709228 0.400280 0.004407 0.048 Uiso 1 1 calc R . . . . H12B H 0.743025 0.305063 0.047203 0.048 Uiso 1 1 calc R . . . . C4 C 0.60479(18) 0.3137(7) 0.0898(2) 0.0439(13) Uani 1 1 d . . . . . H4C H 0.576775 0.365882 0.077288 0.053 Uiso 1 1 calc R . . . . H4D H 0.600305 0.191654 0.093539 0.053 Uiso 1 1 calc R . . . . C10 C 0.5644(2) 1.0227(7) 0.4629(2) 0.0490(15) Uani 1 1 d . . . . . H10A H 0.548007 1.035647 0.495972 0.059 Uiso 1 1 calc R . . . . H10B H 0.594421 0.992335 0.475852 0.059 Uiso 1 1 calc R . . . . C6 C 0.6441(2) 1.2356(9) 0.4240(3) 0.0581(17) Uani 1 1 d . . . . . C9 C 0.5224(2) 1.2776(8) 0.4332(3) 0.0598(18) Uani 1 1 d . . . . . H9A H 0.523186 1.349492 0.466646 0.072 Uiso 1 1 calc R . . . . H9B H 0.498672 1.195794 0.435119 0.072 Uiso 1 1 calc R . . . . C7 C 0.6030(2) 1.2917(8) 0.4503(3) 0.064(2) Uani 1 1 d . . . . . H7A H 0.608307 1.285910 0.491249 0.077 Uiso 1 1 calc R . . . . H7B H 0.596767 1.409802 0.440109 0.077 Uiso 1 1 calc R . . . . 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 Sb1 0.0364(2) 0.03715(18) 0.03285(19) 0.00044(14) 0.00389(15) -0.00246(15) Sb2 0.0338(2) 0.03725(18) 0.0351(2) 0.00242(15) -0.00266(15) 0.00256(15) Se03 0.0396(3) 0.0325(3) 0.0345(3) 0.0040(2) 0.0046(2) -0.0013(2) Se1 0.0372(3) 0.0444(3) 0.0317(3) -0.0021(2) 0.0008(2) 0.0022(2) Zn1 0.0364(3) 0.0317(3) 0.0330(3) -0.0019(2) 0.0034(3) 0.0025(2) Se4 0.0810(5) 0.0350(3) 0.0326(3) -0.0034(2) 0.0174(3) -0.0081(3) Zn2 0.0377(4) 0.0382(3) 0.0282(3) -0.0013(2) 0.0048(3) -0.0010(3) Se2 0.0421(4) 0.0749(4) 0.0375(3) -0.0158(3) -0.0043(3) 0.0129(3) Se3 0.1028(6) 0.0399(3) 0.0305(3) 0.0027(2) 0.0181(3) 0.0055(3) N2 0.038(3) 0.029(2) 0.034(2) -0.0026(17) 0.0030(19) 0.0034(18) N8 0.040(3) 0.034(2) 0.034(2) -0.0038(18) 0.003(2) -0.0010(19) N4 0.041(3) 0.041(2) 0.038(3) 0.0028(19) 0.011(2) 0.008(2) N1 0.043(3) 0.036(2) 0.042(3) 0.007(2) -0.004(2) 0.004(2) N6 0.044(3) 0.043(3) 0.048(3) 0.010(2) 0.003(2) -0.004(2) N3 0.050(3) 0.042(2) 0.041(3) -0.012(2) 0.004(2) -0.010(2) N7 0.052(3) 0.037(2) 0.033(2) -0.0061(19) 0.008(2) -0.003(2) N5 0.048(3) 0.122(5) 0.041(3) 0.002(3) 0.003(3) -0.035(3) C1 0.047(4) 0.027(3) 0.059(4) -0.004(2) 0.003(3) 0.008(2) C5 0.046(3) 0.046(3) 0.027(3) 0.001(2) -0.005(2) 0.005(2) C11 0.053(4) 0.048(3) 0.037(3) 0.007(2) 0.010(3) -0.008(3) C2 0.045(3) 0.033(3) 0.046(3) -0.010(2) 0.002(3) 0.000(2) C8 0.068(5) 0.044(3) 0.067(4) -0.003(3) 0.030(4) 0.013(3) C3 0.055(4) 0.045(3) 0.043(3) 0.001(3) 0.012(3) -0.010(3) C12 0.048(3) 0.044(3) 0.029(3) -0.005(2) 0.012(2) 0.004(2) C4 0.031(3) 0.047(3) 0.053(4) -0.006(3) 0.002(3) 0.002(2) C10 0.067(4) 0.055(3) 0.025(3) -0.002(2) 0.006(3) -0.010(3) C6 0.044(4) 0.076(4) 0.053(4) -0.003(3) -0.005(3) -0.015(3) C9 0.073(5) 0.056(4) 0.054(4) -0.005(3) 0.027(4) 0.012(3) C7 0.093(6) 0.055(4) 0.043(4) -0.013(3) -0.007(4) -0.029(4) 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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' Zn Zn 0.2839 1.4301 '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 _geom_angle_publ_flag Se1 Sb1 Se03 98.22(2) . . ? Se2 Sb1 Se03 98.21(2) . . ? Se2 Sb1 Se1 100.59(2) . . ? Se4 Sb2 Se03 102.20(2) . . ? Se3 Sb2 Se03 104.81(2) . . ? Se3 Sb2 Se4 97.67(2) . . ? Sb2 Se03 Sb1 99.43(2) . . ? Zn1 Se1 Sb1 99.32(2) . . ? N2 Zn1 Se1 172.33(11) . . ? N4 Zn1 Se1 109.43(12) . . ? N4 Zn1 N2 77.19(16) . . ? N4 Zn1 N1 109.21(18) . . ? N4 Zn1 N3 116.81(18) . . ? N1 Zn1 Se1 103.50(12) . . ? N1 Zn1 N2 77.23(15) . . ? N1 Zn1 N3 118.49(18) . . ? N3 Zn1 Se1 97.47(12) . . ? N3 Zn1 N2 75.73(15) . . ? Zn2 Se4 Sb2 110.75(3) . . ? N8 Zn2 Se4 109.53(11) . . ? N8 Zn2 N6 118.16(17) . . ? N8 Zn2 N7 78.03(15) . . ? N8 Zn2 N5 110.6(2) . . ? N6 Zn2 Se4 100.75(13) . . ? N6 Zn2 N7 77.98(17) . . ? N7 Zn2 Se4 171.66(11) . . ? N5 Zn2 Se4 95.62(15) . . ? N5 Zn2 N6 118.6(2) . . ? N5 Zn2 N7 78.04(19) . . ? C5 N2 Zn1 104.2(3) . . ? C5 N2 C2 113.2(4) . . ? C5 N2 C12 113.1(4) . . ? C2 N2 Zn1 105.7(3) . . ? C12 N2 Zn1 106.1(3) . . ? C12 N2 C2 113.5(4) . . ? C11 N8 Zn2 114.5(3) . . ? C4 N4 Zn1 114.7(3) . . ? C1 N1 Zn1 112.9(3) . . ? C8 N6 Zn2 113.0(4) . . ? C3 N3 Zn1 114.1(3) . . ? C10 N7 Zn2 106.0(3) . . ? C9 N7 Zn2 106.6(3) . . ? C9 N7 C10 112.2(5) . . ? C9 N7 C7 113.6(5) . . ? C7 N7 Zn2 105.6(3) . . ? C7 N7 C10 112.1(5) . . ? C6 N5 Zn2 116.0(4) . . ? N1 C1 C2 111.0(4) . . ? N2 C5 C4 111.1(4) . . ? N8 C11 C10 111.0(4) . . ? N2 C2 C1 110.5(4) . . ? N6 C8 C9 111.4(5) . . ? N3 C3 C12 108.0(4) . . ? N2 C12 C3 110.8(4) . . ? N4 C4 C5 108.6(4) . . ? N7 C10 C11 111.8(4) . . ? N5 C6 C7 109.9(5) . . ? N7 C9 C8 110.4(5) . . ? N7 C7 C6 112.8(5) . . ? 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 Sb1 Se03 2.6207(6) . ? Sb1 Se1 2.5646(6) . ? Sb1 Se2 2.4978(7) . ? Sb2 Se03 2.5973(6) . ? Sb2 Se4 2.5210(7) . ? Sb2 Se3 2.4734(7) . ? Se1 Zn1 2.4842(8) . ? Zn1 N2 2.438(4) . ? Zn1 N4 2.053(4) . ? Zn1 N1 2.068(4) . ? Zn1 N3 2.114(4) . ? Se4 Zn2 2.4637(8) . ? Zn2 N8 2.069(4) . ? Zn2 N6 2.110(5) . ? Zn2 N7 2.358(4) . ? Zn2 N5 2.094(5) . ? N2 C5 1.447(6) . ? N2 C2 1.465(6) . ? N2 C12 1.452(6) . ? N8 C11 1.452(6) . ? N4 C4 1.480(7) . ? N1 C1 1.465(7) . ? N6 C8 1.461(7) . ? N3 C3 1.470(7) . ? N7 C10 1.472(7) . ? N7 C9 1.468(7) . ? N7 C7 1.471(7) . ? N5 C6 1.463(8) . ? C1 C2 1.515(7) . ? C5 C4 1.514(8) . ? C11 C10 1.491(7) . ? C8 C9 1.505(8) . ? C3 C12 1.522(7) . ? C6 C7 1.511(10) . ?