#------------------------------------------------------------------------------ #$Date: 2019-11-17 07:11:48 +0200 (Sun, 17 Nov 2019) $ #$Revision: 228593 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/15/7121513.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_7121513 loop_ _publ_author_name 'Wang, Kai-Yao' 'Ding, Dong' 'Zhang, Shu' 'Wang, Yanlong' 'Liu, Wei' 'Wang, Shuao' 'Wang, Shuai-Hua' 'Liu, Dan' 'Wang, Cheng' _publ_section_title ; Preparation of thermochromic selenidostannates in deep eutectic solvents. ; _journal_issue 38 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 4806 _journal_page_last 4809 _journal_paper_doi 10.1039/c8cc01614c _journal_volume 54 _journal_year 2018 _chemical_formula_sum 'C10 H30 N2 O3 Se7 Sn3' _chemical_formula_weight 1135.15 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2018-02-04 deposited with the CCDC. 2018-04-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.727(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.8365(3) _cell_length_b 13.5796(4) _cell_length_c 20.7384(7) _cell_measurement_reflns_used 10783 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 29.8730 _cell_measurement_theta_min 5.1370 _cell_volume 2767.01(15) _computing_cell_refinement 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'XtaLAB AFC12 (RINC): Kappa dual home/near' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0680 _diffrn_reflns_av_unetI/netI 0.0407 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 27310 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_min 4.912 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 11.908 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.11427 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour YELLOW _exptl_crystal_density_diffrn 2.725 _exptl_crystal_description PLATE _exptl_crystal_F_000 2064 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.080 _refine_diff_density_max 1.695 _refine_diff_density_min -1.107 _refine_diff_density_rms 0.236 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 210 _refine_ls_number_reflns 5601 _refine_ls_number_restraints 13 _refine_ls_restrained_S_all 1.009 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0424 _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^)+(0.0271P)^2^+62.8353P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0922 _refine_ls_wR_factor_ref 0.0974 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4662 _reflns_number_total 5601 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8cc01614c2.cif _cod_data_source_block WKY _cod_depositor_comments 'Adding full bibliography for 7121499--7121514.cif.' _cod_database_code 7121513 _shelx_shelxl_version_number 2014/7 _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. ; _shelx_res_file ; WKY.res created by SHELXL-2014/7 TITL WKY in P2(1)/n CELL 0.71073 9.8365 13.5796 20.7384 90.000 92.727 90.000 ZERR 4.00 0.0003 0.0004 0.0007 0.000 0.003 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O SE SN UNIT 40 120 8 12 28 12 ISOR 0.001 C9 C6 TEMP -173 L.S. 20 BOND DFIX 1.45 0.01 C10 O2 EQIV $1 -x+5/2, y+1/2, -z+1/2 EQIV $2 -x+2, -y+1, -z+1 EQIV $3 x-1/2, -y+3/2, z+1/2 EQIV $4 -x+3/2, y+1/2, -z+1/2 EQIV $5 x-1, y, z EQIV $6 -x+1/2, y+1/2, -z+1/2 EQIV $7 -x+1, -y+1, -z+1 HTAB O1 SE2_$1 HTAB O2 O1W HTAB C2 SE7 HTAB C2 O1 HTAB C3 SE5_$2 HTAB C3 SE2_$3 HTAB C4 SE6_$4 HTAB C4 SE7 HTAB C6 O2 HTAB C6 SE6 HTAB C6 SE3_$4 HTAB C7 SE6 HTAB C7 SE1_$5 HTAB C8 SE6_$6 HTAB C10 SE5_$5 HTAB O1W SE5_$7 FMAP 2 PLAN 20 ACTA HTAB WGHT 0.027100 62.835297 FVAR 0.06165 SN1 6 0.930452 0.532871 0.078067 11.00000 0.01908 0.01547 = 0.01369 -0.00394 0.00421 0.00103 SN2 6 0.774078 0.452720 0.230275 11.00000 0.01725 0.00847 = 0.01591 0.00004 0.00199 -0.00199 SN3 6 0.811436 0.721014 0.193650 11.00000 0.01773 0.00890 = 0.01730 -0.00139 0.00458 0.00086 SE1 5 1.009204 0.703604 0.118330 11.00000 0.02507 0.01921 = 0.02606 -0.00673 0.01294 -0.00637 SE2 5 1.177559 0.494524 0.033152 11.00000 0.01666 0.03242 = 0.01637 -0.00639 0.00253 0.00305 SE3 5 0.964472 0.393449 0.159938 11.00000 0.02184 0.01777 = 0.02210 -0.00045 0.00303 0.00798 SE4 5 0.682560 0.570367 0.128693 11.00000 0.01654 0.01134 = 0.01520 -0.00141 0.00256 0.00088 SE5 5 0.880033 0.341608 0.328632 11.00000 0.02598 0.01901 = 0.02772 0.01076 -0.00972 -0.00734 SE6 5 0.551949 0.362043 0.236321 11.00000 0.01607 0.00991 = 0.02703 0.00340 0.00035 -0.00098 SE7 5 0.826923 0.610090 0.294033 11.00000 0.02553 0.01289 = 0.01447 -0.00233 0.00193 -0.00371 O1 4 1.137476 0.786065 0.454593 11.00000 0.05409 0.05155 = 0.08862 -0.01093 -0.01162 0.00937 AFIX 83 H1D 2 1.208094 0.818476 0.464602 11.00000 -1.50000 AFIX 0 O2 4 0.304439 0.516106 0.417531 11.00000 0.25049 AFIX 83 H2D 2 0.270959 0.499707 0.452465 11.00000 -1.50000 AFIX 0 N1 3 0.858034 0.719769 0.486324 11.00000 0.06377 0.06128 = 0.03875 -0.00748 -0.00360 0.02514 N2 3 0.311567 0.614123 0.280257 11.00000 0.02054 0.03027 = 0.08352 -0.02843 -0.00048 0.00237 C1 1 0.708956 0.695022 0.469795 11.00000 0.06106 0.07307 = 0.05469 -0.01513 -0.01173 0.00105 AFIX 33 H1A 2 0.677595 0.645843 0.500317 11.00000 -1.50000 H1B 2 0.653730 0.754794 0.472623 11.00000 -1.50000 H1C 2 0.699893 0.668550 0.425839 11.00000 -1.50000 AFIX 0 C2 1 0.938392 0.626395 0.480877 11.00000 0.07352 0.04605 = 0.05602 -0.00249 -0.00576 0.01515 AFIX 33 H2A 2 0.912682 0.580135 0.514460 11.00000 -1.50000 H2B 2 0.919179 0.596902 0.438286 11.00000 -1.50000 H2C 2 1.035772 0.641196 0.486329 11.00000 -1.50000 AFIX 0 C3 1 0.870467 0.759495 0.552914 11.00000 0.05834 0.06004 = 0.02584 0.00538 -0.00557 0.02213 AFIX 33 H3A 2 0.847575 0.707884 0.583596 11.00000 -1.50000 H3B 2 0.964091 0.781723 0.562355 11.00000 -1.50000 H3C 2 0.807956 0.815141 0.556819 11.00000 -1.50000 AFIX 0 C4 1 0.890989 0.793383 0.437290 11.00000 0.06903 0.03197 = 0.04502 -0.00496 0.00514 0.00122 AFIX 23 H4A 2 0.813410 0.839413 0.431125 11.00000 -1.20000 H4B 2 0.902935 0.759392 0.395709 11.00000 -1.20000 AFIX 0 C5 1 1.017812 0.851615 0.454858 11.00000 0.04524 0.04606 = 0.05383 0.00034 -0.01833 0.00403 AFIX 23 H5A 2 1.028037 0.905626 0.423394 11.00000 -1.20000 H5B 2 1.010684 0.881106 0.498224 11.00000 -1.20000 AFIX 0 C6 1 0.438114 0.612563 0.322964 11.00000 0.08885 0.08998 = 0.09164 -0.00197 0.00238 0.00123 AFIX 33 H6A 2 0.413764 0.613103 0.368238 11.00000 -1.50000 H6B 2 0.490272 0.552867 0.314420 11.00000 -1.50000 H6C 2 0.493365 0.670694 0.314263 11.00000 -1.50000 AFIX 0 C7 1 0.352896 0.613250 0.213259 11.00000 0.09334 0.17019 = 0.13309 0.09577 0.07626 0.10005 AFIX 33 H7A 2 0.405149 0.553310 0.205510 11.00000 -1.50000 H7B 2 0.271778 0.614739 0.183949 11.00000 -1.50000 H7C 2 0.409385 0.671119 0.205535 11.00000 -1.50000 AFIX 0 C8 1 0.232748 0.704642 0.291806 11.00000 0.07126 0.07712 = 0.23937 -0.09478 -0.08628 0.05544 AFIX 33 H8A 2 0.205027 0.705359 0.336572 11.00000 -1.50000 H8B 2 0.289297 0.762465 0.284044 11.00000 -1.50000 H8C 2 0.151690 0.706085 0.262457 11.00000 -1.50000 AFIX 0 C9 1 0.221773 0.522426 0.290518 11.00000 0.08492 0.08522 = 0.08539 -0.00003 0.00397 -0.00013 AFIX 23 H9A 2 0.265271 0.463814 0.271976 11.00000 -1.20000 H9B 2 0.131959 0.531770 0.267736 11.00000 -1.20000 AFIX 0 C10 1 0.201581 0.504840 0.364608 11.00000 10.20238 AFIX 23 H10A 2 0.125146 0.548118 0.375707 11.00000 -1.20000 H10B 2 0.167587 0.436499 0.367955 11.00000 -1.20000 AFIX 0 O1W 4 0.346532 0.555968 0.554817 11.00000 0.22065 AFIX 3 H1WA 2 0.278761 0.563851 0.578226 11.00000 -1.20000 H1WB 2 0.426972 0.559689 0.571516 11.00000 -1.20000 AFIX 0 HKLF 4 REM WKY in P2(1)/n REM R1 = 0.0424 for 4662 Fo > 4sig(Fo) and 0.0551 for all 5601 data REM 210 parameters refined using 13 restraints END WGHT 0.0262 45.4326 REM Instructions for potential hydrogen bonds HTAB O1 Se2_$1 HTAB O2 O1W HTAB C1 Se7 HTAB C2 Se7 HTAB C2 O1 HTAB C3 Se5_$2 HTAB C3 Se2_$3 HTAB C4 Se6_$4 HTAB C4 Se7 HTAB C6 O2 HTAB C6 Se6 HTAB C6 Se3_$4 HTAB C7 Se6 HTAB C7 Se1_$5 HTAB C8 Se6_$6 HTAB O1W Se5_$7 REM Highest difference peak 1.695, deepest hole -1.107, 1-sigma level 0.236 Q1 1 0.4162 0.5813 0.3451 11.00000 0.05 1.70 Q2 1 0.7794 0.7642 0.4414 11.00000 0.05 1.59 Q3 1 0.4628 0.6304 0.2962 11.00000 0.05 1.51 Q4 1 0.2295 0.5207 0.2555 11.00000 0.05 1.25 Q5 1 0.3910 0.6184 0.4089 11.00000 0.05 1.25 Q6 1 0.9296 0.7766 0.4804 11.00000 0.05 1.22 Q7 1 0.8794 0.7203 0.2141 11.00000 0.05 1.12 Q8 1 0.7002 0.4405 0.2142 11.00000 0.05 1.09 Q9 1 1.2733 0.4968 0.0345 11.00000 0.05 1.09 Q10 1 0.8009 0.4222 0.1985 11.00000 0.05 1.08 Q11 1 0.7204 0.7211 0.1911 11.00000 0.05 1.08 Q12 1 0.2758 0.5297 0.4235 11.00000 0.05 1.04 Q13 1 0.2036 0.5836 0.2970 11.00000 0.05 1.01 Q14 1 0.3997 0.5017 0.3849 11.00000 0.05 0.99 Q15 1 0.7411 0.4224 0.2620 11.00000 0.05 0.97 Q16 1 0.8443 0.5470 0.0702 11.00000 0.05 0.94 Q17 1 0.6006 0.3584 0.1988 11.00000 0.05 0.94 Q18 1 0.3196 0.4263 0.3484 11.00000 0.05 0.94 Q19 1 0.4204 0.5343 0.5781 11.00000 0.05 0.93 Q20 1 1.0151 0.5310 0.0828 11.00000 0.05 0.92 ; _shelx_res_checksum 41960 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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 Sn1 Sn 0.93045(6) 0.53287(4) 0.07807(3) 0.01597(13) Uani 1 1 d . . Sn2 Sn 0.77408(6) 0.45272(4) 0.23027(3) 0.01384(13) Uani 1 1 d . . Sn3 Sn 0.81144(6) 0.72101(4) 0.19365(3) 0.01452(13) Uani 1 1 d . . Se1 Se 1.00920(9) 0.70360(7) 0.11833(4) 0.0231(2) Uani 1 1 d . . Se2 Se 1.17756(9) 0.49452(7) 0.03315(4) 0.0218(2) Uani 1 1 d . . Se3 Se 0.96447(9) 0.39345(6) 0.15994(4) 0.02051(19) Uani 1 1 d . . Se4 Se 0.68256(8) 0.57037(6) 0.12869(4) 0.01430(17) Uani 1 1 d . . Se5 Se 0.88003(10) 0.34161(7) 0.32863(5) 0.0246(2) Uani 1 1 d . . Se6 Se 0.55195(8) 0.36204(6) 0.23632(4) 0.01769(18) Uani 1 1 d . . Se7 Se 0.82692(9) 0.61009(6) 0.29403(4) 0.01760(18) Uani 1 1 d . . O1 O 1.1375(10) 0.7861(7) 0.4546(5) 0.065(3) Uani 1 1 d . . H1D H 1.2081 0.8185 0.4646 0.098 Uiso 1 1 calc R U O2 O 0.304(3) 0.516(2) 0.4175(16) 0.250(13) Uiso 1 1 d D . H2D H 0.2710 0.4997 0.4525 0.376 Uiso 1 1 calc R U N1 N 0.8580(12) 0.7198(9) 0.4863(5) 0.055(3) Uani 1 1 d . . N2 N 0.3116(9) 0.6141(7) 0.2803(6) 0.045(3) Uani 1 1 d . . C1 C 0.7090(15) 0.6950(12) 0.4698(7) 0.063(4) Uani 1 1 d . . H1A H 0.6776 0.6458 0.5003 0.095 Uiso 1 1 calc R U H1B H 0.6537 0.7548 0.4726 0.095 Uiso 1 1 calc R U H1C H 0.6999 0.6686 0.4258 0.095 Uiso 1 1 calc R U C2 C 0.9384(16) 0.6264(10) 0.4809(7) 0.059(4) Uani 1 1 d . . H2A H 0.9127 0.5801 0.5145 0.088 Uiso 1 1 calc R U H2B H 0.9192 0.5969 0.4383 0.088 Uiso 1 1 calc R U H2C H 1.0358 0.6412 0.4863 0.088 Uiso 1 1 calc R U C3 C 0.8705(14) 0.7595(10) 0.5529(5) 0.048(3) Uani 1 1 d . . H3A H 0.8476 0.7079 0.5836 0.072 Uiso 1 1 calc R U H3B H 0.9641 0.7817 0.5624 0.072 Uiso 1 1 calc R U H3C H 0.8080 0.8151 0.5568 0.072 Uiso 1 1 calc R U C4 C 0.8910(15) 0.7934(9) 0.4373(6) 0.049(3) Uani 1 1 d . . H4A H 0.8134 0.8394 0.4311 0.058 Uiso 1 1 calc R U H4B H 0.9029 0.7594 0.3957 0.058 Uiso 1 1 calc R U C5 C 1.0178(13) 0.8516(10) 0.4549(7) 0.049(3) Uani 1 1 d . . H5A H 1.0280 0.9056 0.4234 0.059 Uiso 1 1 calc R U H5B H 1.0107 0.8811 0.4982 0.059 Uiso 1 1 calc R U C6 C 0.438(2) 0.6126(15) 0.3230(10) 0.090(6) Uani 1 1 d . U H6A H 0.4138 0.6131 0.3682 0.135 Uiso 1 1 calc R U H6B H 0.4903 0.5529 0.3144 0.135 Uiso 1 1 calc R U H6C H 0.4934 0.6707 0.3143 0.135 Uiso 1 1 calc R U C7 C 0.353(2) 0.6133(18) 0.2133(10) 0.130(11) Uani 1 1 d . . H7A H 0.4051 0.5533 0.2055 0.195 Uiso 1 1 calc R U H7B H 0.2718 0.6147 0.1839 0.195 Uiso 1 1 calc R U H7C H 0.4094 0.6711 0.2055 0.195 Uiso 1 1 calc R U C8 C 0.2327(18) 0.7046(13) 0.2918(13) 0.132(11) Uani 1 1 d . . H8A H 0.2050 0.7054 0.3366 0.198 Uiso 1 1 calc R U H8B H 0.2893 0.7625 0.2840 0.198 Uiso 1 1 calc R U H8C H 0.1517 0.7061 0.2625 0.198 Uiso 1 1 calc R U C9 C 0.222(2) 0.5224(15) 0.2905(9) 0.085(5) Uani 1 1 d . U H9A H 0.2653 0.4638 0.2720 0.102 Uiso 1 1 calc R U H9B H 0.1320 0.5318 0.2677 0.102 Uiso 1 1 calc R U C10 C 0.202(4) 0.505(3) 0.3646(17) 0.202 Uiso 1 1 d D U H10A H 0.1251 0.5481 0.3757 0.243 Uiso 1 1 calc R U H10B H 0.1676 0.4365 0.3680 0.243 Uiso 1 1 calc R U O1W O 0.347(3) 0.556(2) 0.5548(12) 0.221(11) Uiso 1 1 d . . H1WA H 0.2788 0.5639 0.5782 0.265 Uiso 1 1 d R U H1WB H 0.4270 0.5597 0.5715 0.265 Uiso 1 1 d R U 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 Sn1 0.0191(3) 0.0155(3) 0.0137(3) -0.0039(2) 0.0042(2) 0.0010(2) Sn2 0.0172(3) 0.0085(2) 0.0159(3) 0.0000(2) 0.0020(2) -0.0020(2) Sn3 0.0177(3) 0.0089(3) 0.0173(3) -0.0014(2) 0.0046(2) 0.0009(2) Se1 0.0251(5) 0.0192(4) 0.0261(5) -0.0067(4) 0.0129(4) -0.0064(4) Se2 0.0167(4) 0.0324(5) 0.0164(4) -0.0064(4) 0.0025(3) 0.0031(4) Se3 0.0218(4) 0.0178(4) 0.0221(4) -0.0004(3) 0.0030(3) 0.0080(3) Se4 0.0165(4) 0.0113(4) 0.0152(4) -0.0014(3) 0.0026(3) 0.0009(3) Se5 0.0260(5) 0.0190(4) 0.0277(5) 0.0108(4) -0.0097(4) -0.0073(4) Se6 0.0161(4) 0.0099(4) 0.0270(5) 0.0034(3) 0.0004(3) -0.0010(3) Se7 0.0255(5) 0.0129(4) 0.0145(4) -0.0023(3) 0.0019(3) -0.0037(3) O1 0.054(6) 0.052(6) 0.089(8) -0.011(5) -0.012(5) 0.009(5) N1 0.064(7) 0.061(7) 0.039(6) -0.007(5) -0.004(5) 0.025(6) N2 0.021(4) 0.030(5) 0.084(8) -0.028(5) 0.000(5) 0.002(4) C1 0.061(9) 0.073(10) 0.055(8) -0.015(8) -0.012(7) 0.001(8) C2 0.074(10) 0.046(8) 0.056(8) -0.002(7) -0.006(7) 0.015(7) C3 0.058(8) 0.060(8) 0.026(6) 0.005(6) -0.006(5) 0.022(7) C4 0.069(9) 0.032(6) 0.045(7) -0.005(5) 0.005(6) 0.001(6) C5 0.045(7) 0.046(7) 0.054(8) 0.000(6) -0.018(6) 0.004(6) C6 0.089(6) 0.090(6) 0.092(6) -0.002(2) 0.002(2) 0.001(2) C7 0.093(14) 0.17(2) 0.133(18) 0.096(17) 0.076(14) 0.100(15) C8 0.071(12) 0.077(12) 0.24(3) -0.095(16) -0.086(15) 0.055(10) C9 0.085(5) 0.085(5) 0.085(5) 0.0000(10) 0.0040(10) -0.0001(10) 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' 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' Sn Sn -0.6537 1.4246 '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 Se2 Sn1 Se3 122.34(4) 3_765 . Se2 Sn1 Se1 122.52(4) 3_765 . Se3 Sn1 Se1 115.12(4) . . Se2 Sn1 Se2 90.17(3) 3_765 . Se3 Sn1 Se2 89.70(3) . . Se1 Sn1 Se2 91.36(3) . . Se2 Sn1 Se4 91.94(3) 3_765 . Se3 Sn1 Se4 88.51(3) . . Se1 Sn1 Se4 88.16(3) . . Se2 Sn1 Se4 177.74(4) . . Se6 Sn2 Se7 122.66(3) . . Se6 Sn2 Se3 122.38(4) . . Se7 Sn2 Se3 114.97(4) . . Se6 Sn2 Se5 89.64(3) . . Se7 Sn2 Se5 90.84(3) . . Se3 Sn2 Se5 89.32(3) . . Se6 Sn2 Se4 93.95(3) . . Se7 Sn2 Se4 87.81(3) . . Se3 Sn2 Se4 88.16(3) . . Se5 Sn2 Se4 176.34(3) . . Se5 Sn3 Se1 122.01(4) 2_655 . Se5 Sn3 Se7 122.98(4) 2_655 . Se1 Sn3 Se7 114.99(4) . . Se5 Sn3 Se6 89.22(3) 2_655 2_655 Se1 Sn3 Se6 91.16(3) . 2_655 Se7 Sn3 Se6 88.36(3) . 2_655 Se5 Sn3 Se4 94.07(3) 2_655 . Se1 Sn3 Se4 88.75(3) . . Se7 Sn3 Se4 88.21(3) . . Se6 Sn3 Se4 176.17(3) 2_655 . Sn3 Se1 Sn1 93.18(3) . . Sn1 Se2 Sn1 89.83(3) 3_765 . Sn1 Se3 Sn2 93.99(3) . . Sn3 Se4 Sn1 85.85(3) . . Sn3 Se4 Sn2 85.99(3) . . Sn1 Se4 Sn2 85.48(3) . . Sn3 Se5 Sn2 88.08(3) 2_645 . Sn2 Se6 Sn3 87.88(3) . 2_645 Sn2 Se7 Sn3 93.92(3) . . C4 N1 C3 112.6(11) . . C4 N1 C2 112.8(11) . . C3 N1 C2 110.9(10) . . C4 N1 C1 103.6(11) . . C3 N1 C1 109.0(11) . . C2 N1 C1 107.5(12) . . C7 N2 C8 109.4(16) . . C7 N2 C6 107.5(13) . . C8 N2 C6 110.1(12) . . C7 N2 C9 108.0(15) . . C8 N2 C9 109.8(13) . . C6 N2 C9 111.9(13) . . N1 C4 C5 113.3(11) . . O1 C5 C4 109.5(11) . . N2 C9 C10 111(2) . . O2 C10 C9 127(3) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Sn1 Se2 2.5207(11) 3_765 Sn1 Se3 2.5545(11) . Sn1 Se1 2.5712(10) . Sn1 Se2 2.6949(10) . Sn1 Se4 2.7479(10) . Sn2 Se6 2.5164(10) . Sn2 Se7 2.5534(10) . Sn2 Se3 2.5579(10) . Sn2 Se5 2.7058(10) . Sn2 Se4 2.7605(10) . Sn3 Se5 2.5218(10) 2_655 Sn3 Se1 2.5631(10) . Sn3 Se7 2.5682(10) . Sn3 Se6 2.7197(10) 2_655 Sn3 Se4 2.7284(10) . Se2 Sn1 2.5206(11) 3_765 Se5 Sn3 2.5218(10) 2_645 Se6 Sn3 2.7197(10) 2_645 O1 C5 1.476(15) . O2 C10 1.465(10) . N1 C4 1.473(17) . N1 C3 1.482(15) . N1 C2 1.501(16) . N1 C1 1.527(18) . N2 C7 1.47(2) . N2 C8 1.479(16) . N2 C6 1.49(2) . N2 C9 1.55(2) . C4 C5 1.507(18) . C9 C10 1.58(4) . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1D Se2 0.84 2.64 3.368(10) 145.6 2_755 O2 H2D O1W 0.84 2.34 2.91(4) 125.0 . C2 H2B Se7 0.98 3.09 3.983(15) 152.1 . C2 H2C O1 0.98 2.32 2.989(19) 125.1 . C3 H3B Se5 0.98 3.15 3.656(12) 113.6 3_766 C3 H3C Se2 0.98 2.92 3.854(13) 160.4 4_576 C4 H4B Se6 0.99 3.12 3.787(13) 125.7 2_655 C4 H4B Se7 0.99 2.99 3.904(12) 153.3 . C6 H6A O2 0.98 2.01 2.75(4) 130.0 . C6 H6B Se6 0.98 3.13 4.03(2) 153.4 . C6 H6C Se3 0.98 3.10 3.94(2) 145.7 2_655 C7 H7A Se6 0.98 3.03 3.951(18) 158.0 . C7 H7B Se1 0.98 3.11 4.022(19) 156.3 1_455 C8 H8C Se6 0.98 2.92 3.549(14) 123.2 2 C10 H10B Se5 0.99 3.18 3.91(4) 131.4 1_455 O1W H1WA Se5 0.85 2.85 3.64(3) 156.2 3_666