#------------------------------------------------------------------------------ #$Date: 2018-04-16 14:28:12 +0300 (Mon, 16 Apr 2018) $ #$Revision: 207350 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/15/7121512.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_7121512 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_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C8CC01614C _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 ; 2018-04-12 deposited with the CCDC. 2018-04-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.368(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.8956(4) _cell_length_b 13.6110(5) _cell_length_c 20.8327(7) _cell_measurement_reflns_used 8772 _cell_measurement_temperature 210(2) _cell_measurement_theta_max 29.6600 _cell_measurement_theta_min 4.9440 _cell_volume 2803.54(18) _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 210(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 0.0638 _diffrn_reflns_av_unetI/netI 0.0418 _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 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 26407 _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 4.932 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 11.752 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.20719 _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 ORANGE _exptl_crystal_density_diffrn 2.689 _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 1.402 _refine_diff_density_min -0.984 _refine_diff_density_rms 0.205 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 210 _refine_ls_number_reflns 5678 _refine_ls_number_restraints 13 _refine_ls_restrained_S_all 1.005 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0417 _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^)+(0.0271P)^2^+58.8353P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0973 _refine_ls_wR_factor_ref 0.1036 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4688 _reflns_number_total 5678 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8cc01614c2.cif _cod_data_source_block 1-210K _cod_database_code 7121512 _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 9.8956 13.6110 20.8327 90.000 92.368 90.000 ZERR 4.00 0.0004 0.0005 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 -63 L.S. 20 BOND DFIX 1.45 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 58.835300 FVAR 0.06082 SN1 6 0.929614 0.532014 0.077876 11.00000 0.02977 0.02005 = 0.01812 -0.00386 0.00710 0.00082 SN2 6 0.774947 0.449658 0.229871 11.00000 0.02574 0.01367 = 0.02159 0.00009 0.00417 -0.00324 SN3 6 0.809662 0.718026 0.194054 11.00000 0.02669 0.01374 = 0.02319 -0.00211 0.00751 0.00153 SE1 5 1.005965 0.702111 0.118323 11.00000 0.03334 0.02546 = 0.03576 -0.00872 0.01743 -0.00770 SE2 5 1.176461 0.494919 0.032772 11.00000 0.02518 0.04253 = 0.02246 -0.00690 0.00428 0.00373 SE3 5 0.964498 0.392698 0.158903 11.00000 0.03206 0.02494 = 0.03012 0.00214 0.00617 0.00965 SE4 5 0.682142 0.567739 0.129108 11.00000 0.02414 0.01743 = 0.02075 -0.00150 0.00360 0.00105 SE5 5 0.881472 0.337744 0.326866 11.00000 0.03480 0.02708 = 0.03498 0.01314 -0.01063 -0.00940 SE6 5 0.554833 0.358433 0.236112 11.00000 0.02401 0.01634 = 0.03867 0.00663 0.00011 -0.00139 SE7 5 0.826084 0.606557 0.293536 11.00000 0.03919 0.02002 = 0.01906 -0.00272 0.00100 -0.00473 O1 4 1.138447 0.786626 0.452063 11.00000 0.09799 0.07746 = 0.18525 -0.01821 -0.02314 -0.00512 AFIX 83 H1D 2 1.207344 0.818926 0.461948 11.00000 -1.50000 AFIX 0 O2 4 0.317444 0.513079 0.412397 11.00000 0.32588 AFIX 83 H2D 2 0.288283 0.497531 0.447777 11.00000 -1.50000 AFIX 0 N1 3 0.862597 0.720374 0.487229 11.00000 0.09831 0.07938 = 0.04701 -0.00438 -0.00324 0.04699 N2 3 0.310093 0.613589 0.277821 11.00000 0.02733 0.05624 = 0.08956 -0.02495 -0.00579 0.00471 C1 1 0.714920 0.697186 0.468285 11.00000 0.08412 0.13209 = 0.10835 -0.03395 -0.02670 0.03522 AFIX 33 H1A 2 0.680181 0.649447 0.497989 11.00000 -1.50000 H1B 2 0.661639 0.756900 0.469782 11.00000 -1.50000 H1C 2 0.709360 0.670518 0.425078 11.00000 -1.50000 AFIX 0 C2 1 0.942119 0.628373 0.480760 11.00000 0.13301 0.07906 = 0.09081 0.00107 0.00965 0.05299 AFIX 33 H2A 2 0.919472 0.582830 0.514477 11.00000 -1.50000 H2B 2 0.920800 0.598834 0.439194 11.00000 -1.50000 H2C 2 1.037925 0.643484 0.484392 11.00000 -1.50000 AFIX 0 C3 1 0.871999 0.759496 0.553000 11.00000 0.09073 0.09228 = 0.04140 -0.00431 -0.01655 0.04021 AFIX 33 H3A 2 0.850441 0.707982 0.583081 11.00000 -1.50000 H3B 2 0.963163 0.782997 0.562552 11.00000 -1.50000 H3C 2 0.808602 0.813336 0.556785 11.00000 -1.50000 AFIX 0 C4 1 0.893326 0.792249 0.437001 11.00000 0.09761 0.05412 = 0.06578 0.00351 0.00470 0.01200 AFIX 23 H4A 2 0.816387 0.836830 0.429906 11.00000 -1.20000 H4B 2 0.908499 0.757872 0.396598 11.00000 -1.20000 AFIX 0 C5 1 1.016946 0.850123 0.456919 11.00000 0.07489 0.06182 = 0.09312 0.00139 -0.03424 0.00035 AFIX 23 H5A 2 1.024815 0.907632 0.429016 11.00000 -1.20000 H5B 2 1.009856 0.873162 0.501221 11.00000 -1.20000 AFIX 0 C6 1 0.438971 0.611034 0.315891 11.00000 0.10445 0.10550 = 0.10651 -0.00130 0.00323 0.00029 AFIX 33 H6A 2 0.421172 0.617008 0.361164 11.00000 -1.50000 H6B 2 0.484731 0.549310 0.308421 11.00000 -1.50000 H6C 2 0.495814 0.665102 0.303139 11.00000 -1.50000 AFIX 0 C7 1 0.346613 0.604227 0.210971 11.00000 0.13345 0.19728 = 0.11842 0.08799 0.07910 0.11894 AFIX 33 H7A 2 0.399190 0.544805 0.205834 11.00000 -1.50000 H7B 2 0.265090 0.600933 0.183557 11.00000 -1.50000 H7C 2 0.399842 0.660717 0.199071 11.00000 -1.50000 AFIX 0 C8 1 0.231550 0.699725 0.290713 11.00000 0.08599 0.08823 = 0.22721 -0.07358 -0.05854 0.04790 AFIX 33 H8A 2 0.211062 0.701133 0.335837 11.00000 -1.50000 H8B 2 0.282680 0.757963 0.280257 11.00000 -1.50000 H8C 2 0.147928 0.698179 0.264743 11.00000 -1.50000 AFIX 0 C9 1 0.221953 0.524221 0.291381 11.00000 0.10202 0.10240 = 0.10240 -0.00008 0.00426 -0.00022 AFIX 23 H9A 2 0.131197 0.536031 0.272333 11.00000 -1.20000 H9B 2 0.259376 0.467198 0.269544 11.00000 -1.20000 AFIX 0 C10 1 0.208821 0.498656 0.361253 11.00000 10.23828 AFIX 23 H10A 2 0.184794 0.428847 0.362398 11.00000 -1.20000 H10B 2 0.129775 0.534765 0.375480 11.00000 -1.20000 AFIX 0 O1W 4 0.350475 0.557219 0.556143 11.00000 0.27146 AFIX 3 H1WA 2 0.282704 0.565101 0.579552 11.00000 -1.20000 H1WB 2 0.430915 0.560940 0.572842 11.00000 -1.20000 AFIX 0 HKLF 4 REM WKY in P2(1)/n REM R1 = 0.0417 for 4688 Fo > 4sig(Fo) and 0.0555 for all 5678 data REM 210 parameters refined using 13 restraints END WGHT 0.0287 31.6377 REM Instructions for potential hydrogen bonds HTAB O1 Se2_$1 HTAB O2 O1W HTAB C1 Se7 HTAB C2 Se7 HTAB C2 O1 HTAB C3 Se2_$3 HTAB C4 Se6_$4 HTAB C4 Se7 HTAB C6 O2 HTAB C6 Se6 HTAB C7 Se6 HTAB C7 Se1_$5 HTAB C8 Se6_$6 HTAB O1W Se5_$7 REM Highest difference peak 1.402, deepest hole -0.984, 1-sigma level 0.205 Q1 1 0.7902 0.7583 0.4412 11.00000 0.05 1.40 Q2 1 0.9241 0.4016 0.1146 11.00000 0.05 1.15 Q3 1 0.4164 0.5828 0.3468 11.00000 0.05 1.14 Q4 1 0.8591 0.7057 0.1560 11.00000 0.05 1.12 Q5 1 0.7553 0.7006 0.2250 11.00000 0.05 1.12 Q6 1 1.0607 0.7021 0.1549 11.00000 0.05 1.09 Q7 1 0.8338 0.4481 0.2685 11.00000 0.05 1.04 Q8 1 0.9427 0.7768 0.4794 11.00000 0.05 1.03 Q9 1 0.3315 0.4258 0.3640 11.00000 0.05 0.98 Q10 1 0.8677 0.7094 0.2293 11.00000 0.05 0.97 Q11 1 0.8709 0.5246 0.0290 11.00000 0.05 0.97 Q12 1 0.7514 0.7136 0.1575 11.00000 0.05 0.94 Q13 1 0.2231 0.5262 0.2581 11.00000 0.05 0.92 Q14 1 0.7440 0.5564 0.0977 11.00000 0.05 0.90 Q15 1 0.9027 0.5765 0.1084 11.00000 0.05 0.89 Q16 1 0.8131 0.4233 0.1976 11.00000 0.05 0.89 Q17 1 0.2861 0.4415 0.3334 11.00000 0.05 0.88 Q18 1 1.1805 0.4386 0.0134 11.00000 0.05 0.87 Q19 1 0.8370 0.7523 0.1628 11.00000 0.05 0.87 Q20 1 0.4000 0.6203 0.4032 11.00000 0.05 0.86 ; _shelx_res_checksum 68145 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 0.92961(6) 0.53201(4) 0.07788(3) 0.02248(14) Uani 1 1 d . . Sn2 Sn 0.77495(6) 0.44966(4) 0.22987(3) 0.02024(14) Uani 1 1 d . . Sn3 Sn 0.80966(6) 0.71803(4) 0.19405(3) 0.02103(14) Uani 1 1 d . . Se1 Se 1.00596(10) 0.70211(7) 0.11832(5) 0.0311(2) Uani 1 1 d . . Se2 Se 1.17646(9) 0.49492(8) 0.03277(4) 0.0300(2) Uani 1 1 d . . Se3 Se 0.96450(10) 0.39270(7) 0.15890(5) 0.0289(2) Uani 1 1 d . . Se4 Se 0.68214(9) 0.56774(6) 0.12911(4) 0.02070(18) Uani 1 1 d . . Se5 Se 0.88147(10) 0.33774(7) 0.32687(5) 0.0326(2) Uani 1 1 d . . Se6 Se 0.55483(9) 0.35843(6) 0.23611(5) 0.0264(2) Uani 1 1 d . . Se7 Se 0.82608(10) 0.60656(7) 0.29354(4) 0.0261(2) Uani 1 1 d . . O1 O 1.1384(15) 0.7866(10) 0.4521(8) 0.121(5) Uani 1 1 d . . H1D H 1.2073 0.8189 0.4619 0.182 Uiso 1 1 calc R U O2 O 0.317(4) 0.513(3) 0.412(2) 0.326(19) Uiso 1 1 d D . H2D H 0.2883 0.4975 0.4478 0.489 Uiso 1 1 calc R U N1 N 0.8626(15) 0.7204(10) 0.4872(6) 0.075(4) Uani 1 1 d . . N2 N 0.3101(10) 0.6136(8) 0.2778(6) 0.058(3) Uani 1 1 d . . C1 C 0.7149(19) 0.6972(17) 0.4683(10) 0.109(7) Uani 1 1 d . . H1A H 0.6802 0.6494 0.4980 0.164 Uiso 1 1 calc R U H1B H 0.6616 0.7569 0.4698 0.164 Uiso 1 1 calc R U H1C H 0.7094 0.6705 0.4251 0.164 Uiso 1 1 calc R U C2 C 0.942(2) 0.6284(14) 0.4808(9) 0.101(7) Uani 1 1 d . . H2A H 0.9195 0.5828 0.5145 0.151 Uiso 1 1 calc R U H2B H 0.9208 0.5988 0.4392 0.151 Uiso 1 1 calc R U H2C H 1.0379 0.6435 0.4844 0.151 Uiso 1 1 calc R U C3 C 0.8720(17) 0.7595(13) 0.5530(6) 0.075(5) Uani 1 1 d . . H3A H 0.8504 0.7080 0.5831 0.113 Uiso 1 1 calc R U H3B H 0.9632 0.7830 0.5626 0.113 Uiso 1 1 calc R U H3C H 0.8086 0.8133 0.5568 0.113 Uiso 1 1 calc R U C4 C 0.8933(18) 0.7922(11) 0.4370(8) 0.072(4) Uani 1 1 d . . H4A H 0.8164 0.8368 0.4299 0.087 Uiso 1 1 calc R U H4B H 0.9085 0.7579 0.3966 0.087 Uiso 1 1 calc R U C5 C 1.0169(17) 0.8501(12) 0.4569(9) 0.078(5) Uani 1 1 d . . H5A H 1.0248 0.9076 0.4290 0.093 Uiso 1 1 calc R U H5B H 1.0099 0.8732 0.5012 0.093 Uiso 1 1 calc R U C6 C 0.439(2) 0.6110(16) 0.3159(10) 0.106(6) Uani 1 1 d . U H6A H 0.4212 0.6170 0.3612 0.158 Uiso 1 1 calc R U H6B H 0.4847 0.5493 0.3084 0.158 Uiso 1 1 calc R U H6C H 0.4958 0.6651 0.3031 0.158 Uiso 1 1 calc R U C7 C 0.347(2) 0.604(2) 0.2110(10) 0.148(12) Uani 1 1 d . . H7A H 0.3992 0.5448 0.2058 0.222 Uiso 1 1 calc R U H7B H 0.2651 0.6009 0.1836 0.222 Uiso 1 1 calc R U H7C H 0.3998 0.6607 0.1991 0.222 Uiso 1 1 calc R U C8 C 0.232(2) 0.6997(15) 0.2907(13) 0.136(11) Uani 1 1 d . . H8A H 0.2111 0.7011 0.3358 0.203 Uiso 1 1 calc R U H8B H 0.2827 0.7580 0.2803 0.203 Uiso 1 1 calc R U H8C H 0.1479 0.6982 0.2647 0.203 Uiso 1 1 calc R U C9 C 0.222(2) 0.5242(16) 0.2914(10) 0.102(6) Uani 1 1 d . U H9A H 0.1312 0.5360 0.2723 0.123 Uiso 1 1 calc R U H9B H 0.2594 0.4672 0.2695 0.123 Uiso 1 1 calc R U C10 C 0.209(4) 0.499(4) 0.361(2) 0.238 Uiso 1 1 d D U H10A H 0.1848 0.4288 0.3624 0.286 Uiso 1 1 calc R U H10B H 0.1298 0.5348 0.3755 0.286 Uiso 1 1 calc R U O1W O 0.350(3) 0.557(2) 0.5561(15) 0.271(14) Uiso 1 1 d . . H1WA H 0.2827 0.5651 0.5796 0.326 Uiso 1 1 d R U H1WB H 0.4309 0.5609 0.5728 0.326 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 0.0298(3) 0.0200(3) 0.0181(3) -0.0039(2) 0.0071(2) 0.0008(2) Sn2 0.0257(3) 0.0137(3) 0.0216(3) 0.0001(2) 0.0042(2) -0.0032(2) Sn3 0.0267(3) 0.0137(3) 0.0232(3) -0.0021(2) 0.0075(2) 0.0015(2) Se1 0.0333(5) 0.0255(5) 0.0358(5) -0.0087(4) 0.0174(4) -0.0077(4) Se2 0.0252(5) 0.0425(6) 0.0225(4) -0.0069(4) 0.0043(4) 0.0037(4) Se3 0.0321(5) 0.0249(5) 0.0301(5) 0.0021(4) 0.0062(4) 0.0097(4) Se4 0.0241(4) 0.0174(4) 0.0207(4) -0.0015(3) 0.0036(3) 0.0010(3) Se5 0.0348(5) 0.0271(5) 0.0350(5) 0.0131(4) -0.0106(4) -0.0094(4) Se6 0.0240(4) 0.0163(4) 0.0387(5) 0.0066(4) 0.0001(4) -0.0014(3) Se7 0.0392(5) 0.0200(4) 0.0191(4) -0.0027(3) 0.0010(4) -0.0047(4) O1 0.098(10) 0.077(9) 0.185(16) -0.018(10) -0.023(10) -0.005(8) N1 0.098(10) 0.079(9) 0.047(6) -0.004(6) -0.003(6) 0.047(8) N2 0.027(5) 0.056(7) 0.090(8) -0.025(6) -0.006(5) 0.005(4) C1 0.084(13) 0.132(19) 0.108(15) -0.034(14) -0.027(11) 0.035(13) C2 0.133(17) 0.079(12) 0.091(13) 0.001(10) 0.010(12) 0.053(12) C3 0.091(11) 0.092(12) 0.041(7) -0.004(7) -0.017(7) 0.040(10) C4 0.098(12) 0.054(9) 0.066(9) 0.004(7) 0.005(8) 0.012(8) C5 0.075(10) 0.062(10) 0.093(12) 0.001(9) -0.034(9) 0.000(8) C6 0.104(7) 0.106(7) 0.107(7) -0.001(2) 0.003(2) 0.000(2) C7 0.133(18) 0.20(3) 0.118(17) 0.088(17) 0.079(15) 0.119(19) C8 0.086(14) 0.088(14) 0.23(3) -0.074(17) -0.059(16) 0.048(11) C9 0.102(6) 0.102(6) 0.102(6) -0.0001(10) 0.0043(10) -0.0002(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 122.46(4) 3_765 . Se2 Sn1 Se1 122.50(4) 3_765 . Se3 Sn1 Se1 115.03(4) . . Se2 Sn1 Se2 90.18(3) 3_765 . Se3 Sn1 Se2 89.52(4) . . Se1 Sn1 Se2 91.41(4) . . Se2 Sn1 Se4 92.10(3) 3_765 . Se3 Sn1 Se4 88.45(3) . . Se1 Sn1 Se4 88.16(3) . . Se2 Sn1 Se4 177.53(4) . . Se6 Sn2 Se7 122.65(4) . . Se6 Sn2 Se3 122.54(4) . . Se7 Sn2 Se3 114.81(4) . . Se6 Sn2 Se5 89.71(3) . . Se7 Sn2 Se5 91.16(4) . . Se3 Sn2 Se5 89.35(4) . . Se6 Sn2 Se4 93.72(3) . . Se7 Sn2 Se4 87.75(3) . . Se3 Sn2 Se4 88.05(3) . . Se5 Sn2 Se4 176.45(4) . . Se5 Sn3 Se1 122.06(4) 2_655 . Se5 Sn3 Se7 122.92(4) 2_655 . Se1 Sn3 Se7 115.01(4) . . Se5 Sn3 Se6 89.32(3) 2_655 2_655 Se1 Sn3 Se6 91.10(3) . 2_655 Se7 Sn3 Se6 88.29(3) . 2_655 Se5 Sn3 Se4 94.04(3) 2_655 . Se1 Sn3 Se4 88.75(3) . . Se7 Sn3 Se4 88.27(3) . . Se6 Sn3 Se4 176.13(4) 2_655 . Sn3 Se1 Sn1 93.33(3) . . Sn1 Se2 Sn1 89.82(3) 3_765 . Sn1 Se3 Sn2 94.29(3) . . Sn3 Se4 Sn1 85.66(3) . . Sn3 Se4 Sn2 85.83(3) . . Sn1 Se4 Sn2 85.35(3) . . Sn3 Se5 Sn2 88.19(3) 2_645 . Sn2 Se6 Sn3 88.03(3) . 2_645 Sn2 Se7 Sn3 94.03(3) . . C4 N1 C3 114.5(14) . . C4 N1 C2 111.7(13) . . C3 N1 C2 112.1(12) . . C4 N1 C1 100.2(13) . . C3 N1 C1 109.8(13) . . C2 N1 C1 107.8(16) . . C7 N2 C8 114.0(17) . . C7 N2 C6 105.6(14) . . C8 N2 C6 112.4(14) . . C7 N2 C9 105.8(17) . . C8 N2 C9 107.3(15) . . C6 N2 C9 111.7(15) . . N1 C4 C5 110.0(14) . . O1 C5 C4 109.2(13) . . C10 C9 N2 116(2) . . C9 C10 O2 125(4) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Sn1 Se2 2.5199(11) 3_765 Sn1 Se3 2.5527(11) . Sn1 Se1 2.5668(11) . Sn1 Se2 2.7008(11) . Sn1 Se4 2.7547(10) . Sn2 Se6 2.5152(10) . Sn2 Se7 2.5535(10) . Sn2 Se3 2.5562(11) . Sn2 Se5 2.7090(11) . Sn2 Se4 2.7702(10) . Sn3 Se5 2.5208(11) 2_655 Sn3 Se1 2.5618(10) . Sn3 Se7 2.5682(11) . Sn3 Se6 2.7213(11) 2_655 Sn3 Se4 2.7324(10) . Se2 Sn1 2.5198(11) 3_765 Se5 Sn3 2.5208(11) 2_645 Se6 Sn3 2.7214(11) 2_645 O1 C5 1.49(2) . O2 C10 1.495(19) . N1 C4 1.473(19) . N1 C3 1.469(17) . N1 C2 1.488(19) . N1 C1 1.53(2) . N2 C7 1.46(2) . N2 C8 1.438(19) . N2 C6 1.47(2) . N2 C9 1.53(2) . C4 C5 1.50(2) . C9 C10 1.51(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 0.83 2.66 3.383(14) 146.9 2_755 O2 H2D O1W 0.83 2.45 3.06(5) 130.5 . C2 H2B Se7 0.97 3.14 4.03(2) 153.4 . C2 H2C O1 0.97 2.30 2.98(3) 126.1 . C3 H3B Se5 0.97 3.17 3.669(13) 113.4 3_766 C3 H3C Se2 0.97 2.95 3.877(15) 159.6 4_576 C4 H4B Se6 0.98 3.12 3.773(15) 125.4 2_655 C4 H4B Se7 0.98 3.06 3.950(16) 151.4 . C6 H6A O2 0.97 2.07 2.73(5) 123.9 . C6 H6B Se6 0.97 3.10 4.01(2) 157.0 . C6 H6C Se3 0.97 3.22 3.98(2) 136.8 2_655 C7 H7A Se6 0.97 3.02 3.953(19) 161.5 . C7 H7B Se1 0.97 3.17 4.04(2) 150.6 1_455 C8 H8C Se6 0.97 2.96 3.589(17) 123.3 2 C10 H10A Se5 0.98 3.30 3.95(4) 125.3 1_455 O1W H1WA Se5 0.85 2.91 3.70(3) 156.3 3_666