#------------------------------------------------------------------------------ #$Date: 2020-10-06 10:38:37 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257400 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/80/1558018.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_1558018 loop_ _publ_author_name 'M\"uller, Matthias' 'Karttunen, Antti J.' 'Buchner, Magnus R.' _publ_section_title ; Speciation of Be2+ in acidic liquid ammonia and formation of tetra- and octanuclear beryllium amido clusters ; _journal_issue 21 _journal_name_full 'Chemical Science' _journal_page_first 5415 _journal_page_last 5422 _journal_paper_doi 10.1039/D0SC01112F _journal_volume 11 _journal_year 2020 _chemical_formula_moiety 'C2 H33 Be4 N15 S2' _chemical_formula_sum 'C2 H33 Be4 N15 S2' _chemical_formula_weight 367.59 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-02-06 deposited with the CCDC. 2020-05-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 97.4540(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.9563(2) _cell_length_b 8.58430(10) _cell_length_c 24.7099(4) _cell_measurement_reflns_used 24774 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 159.36 _cell_measurement_theta_min 7.21 _cell_volume 2094.06(6) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 5.81 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measurement_device_type 'STOE STADIVARI' _diffrn_measurement_method 'rotation method, \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_unetI/netI 0.0252 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.983 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 24637 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.983 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 78.973 _diffrn_reflns_theta_min 3.608 _diffrn_source 'GeniX 3D HF Cu' _exptl_absorpt_coefficient_mu 2.446 _exptl_absorpt_correction_T_max 0.8966 _exptl_absorpt_correction_T_min 0.2652 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; STOE LANA, absorption correction by scaling of reflection intensities. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different absorption corrections on the model structure of tetrakis(\m~2~-acetato)- diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140. Afterwards a spherical absorption correction was performed within STOE LANA. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.166 _exptl_crystal_description block _exptl_crystal_F_000 792 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.224 _refine_diff_density_min -0.138 _refine_diff_density_rms 0.035 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.905 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 340 _refine_ls_number_reflns 4449 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.905 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_gt 0.0239 _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^)+(0.0397P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.0597 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3534 _reflns_number_total 4449 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc01112f2.cif _cod_data_source_block 5_CCDC3 _cod_depositor_comments ;Adding full bibliography for 1558013--1558021.cif. Adding full bibliography for 1558013--1558021.cif. ; _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1558018 _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. ; _shelx_res_file ; TITL 1_a.res in P2(1)/c 5.res created by SHELXL-2018/3 at 11:05:34 on 16-Nov-2018 REM Old TITL 1 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.092, Rweak 0.003, Alpha 0.014 REM 0.302 for 295 systematic absences, Orientation as input REM Formula found by SHELXT: C2 Be4 N15 S2 CELL 1.54178 9.9563 8.5843 24.7099 90.000 97.454 90.000 ZERR 4.000 0.0002 0.0001 0.0004 0.000 0.001 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H BE N S UNIT 8 132 16 60 8 L.S. 10 BOND LIST 4 OMIT 6 1 24 OMIT -1 0 4 OMIT 3 8 19 TEMP -173.15 FMAP 2 HTAB EQIV $1 x, y-1, z HTAB N7 N14_$1 HTAB N7 N11 HTAB N7 N13 EQIV $2 -x+1, y+1/2, -z+1/2 HTAB N2 N11_$2 HTAB N8 N14 EQIV $3 -x+2, -y+2, -z+1 HTAB N8 N12_$3 EQIV $4 x+1, y, z HTAB N9 N11_$4 HTAB N9 S2 EQIV $5 -x+2, -y+1, -z+1 HTAB N9 N15_$5 HTAB N4 N12_$5 EQIV $6 x-1, y, z HTAB N10 S2_$6 HTAB N10 S2_$5 HTAB N5 S1_$2 HTAB N6 S2_$6 HTAB N3 S1_$2 EQIV $7 -x+1, -y+1, -z+1 HTAB N15 S1_$7 HTAB N15 S2_$3 HTAB N15 N12 HTAB N10 N15 HTAB N8 N11_$2 HTAB N14 N13_$2 EQIV $8 -x+1, y-1/2, -z+1/2 HTAB N13 N11_$8 EQIV $9 -x+2, y-1/2, -z+1/2 HTAB N13 S2_$9 PLAN 20 ACTA REM EXTI 0.000188 WGHT 0.039700 FVAR 0.37084 S1 5 0.048156 0.197199 0.274293 11.00000 0.02613 0.03108 = 0.02020 -0.00250 0.00528 -0.00038 S2 5 1.339321 0.798846 0.463558 11.00000 0.01914 0.02337 = 0.02823 0.00117 0.00434 0.00113 N1 4 0.606278 0.532928 0.402333 11.00000 0.01401 0.01540 = 0.01634 0.00167 0.00156 -0.00157 N2 4 0.645119 0.744436 0.320087 11.00000 0.01401 0.01900 = 0.01369 0.00325 0.00134 0.00069 N3 4 0.912660 0.796156 0.369362 11.00000 0.01486 0.01521 = 0.01529 0.00000 0.00225 -0.00232 N4 4 0.870428 0.588371 0.452470 11.00000 0.01566 0.01446 = 0.01367 0.00102 -0.00087 -0.00001 N5 4 0.823780 0.495021 0.342667 11.00000 0.01663 0.01401 = 0.01690 -0.00140 0.00219 -0.00038 N6 4 0.694504 0.838459 0.428771 11.00000 0.01625 0.01490 = 0.01745 -0.00046 0.00352 0.00065 N7 4 0.555585 0.434227 0.290710 11.00000 0.01744 0.02126 = 0.01702 -0.00280 0.00033 -0.00320 N8 4 0.740620 1.056214 0.345074 11.00000 0.02113 0.01601 = 0.02601 0.00500 0.00557 0.00123 N9 4 1.094376 0.539473 0.392479 11.00000 0.01472 0.01820 = 0.01946 -0.00193 0.00157 0.00075 N10 4 0.648937 0.631806 0.514226 11.00000 0.01530 0.02025 = 0.01493 0.00149 0.00171 -0.00031 N11 4 0.231557 0.448470 0.284180 11.00000 0.02615 0.03435 = 0.02886 -0.00751 0.00914 0.00135 N12 4 1.143688 0.800223 0.536203 11.00000 0.03555 0.02482 = 0.04200 -0.00829 0.01536 -0.00529 N13 4 0.722158 0.328474 0.191320 11.00000 0.02827 0.03578 = 0.02832 -0.00064 0.00546 0.00714 N14 4 0.438313 1.147802 0.355008 11.00000 0.02644 0.02528 = 0.04192 0.00147 0.01204 0.00123 N15 4 0.860595 0.842204 0.580956 11.00000 0.02393 0.02377 = 0.02054 -0.00143 0.00272 -0.00179 C1 1 0.155255 0.344595 0.280231 11.00000 0.02145 0.02962 = 0.01608 -0.00304 0.00472 0.00768 C2 1 1.224115 0.799994 0.506121 11.00000 0.02166 0.01524 = 0.02769 -0.00386 0.00083 -0.00177 BE1 3 0.659094 0.553226 0.339090 11.00000 0.01533 0.01693 = 0.01373 -0.00090 0.00041 -0.00224 BE2 3 0.747402 0.856094 0.365805 11.00000 0.01684 0.01311 = 0.01611 0.00196 0.00271 0.00050 BE3 3 0.923048 0.605972 0.389503 11.00000 0.01244 0.01461 = 0.01578 -0.00002 0.00104 0.00043 BE4 3 0.706176 0.647465 0.448570 11.00000 0.01597 0.01493 = 0.01314 0.00080 0.00171 -0.00097 H1A 2 0.522958 0.557840 0.401398 11.00000 0.02874 H1B 2 0.615419 0.436298 0.412808 11.00000 0.03164 H7A 2 0.543857 0.341990 0.303634 11.00000 0.03631 H7B 2 0.472095 0.471069 0.281913 11.00000 0.02718 H7C 2 0.589208 0.421576 0.261373 11.00000 0.03074 H2A 2 0.561471 0.773033 0.317663 11.00000 0.02627 H2B 2 0.666872 0.757589 0.286924 11.00000 0.02620 H8B 2 0.659108 1.093281 0.342630 11.00000 0.03411 H8C 2 0.789924 1.115309 0.368405 11.00000 0.03463 H9A 2 1.119799 0.537979 0.359178 11.00000 0.03517 H9B 2 1.154415 0.600939 0.412937 11.00000 0.03525 H9C 2 1.105021 0.443962 0.405605 11.00000 0.04117 H4B 2 0.917636 0.643887 0.476669 11.00000 0.02550 H4A 2 0.880556 0.495890 0.462811 11.00000 0.02668 H10B 2 0.568894 0.673370 0.513966 11.00000 0.02325 H10A 2 0.645702 0.533159 0.524920 11.00000 0.03157 H5A 2 0.836307 0.400440 0.349508 11.00000 0.03625 H5B 2 0.854248 0.503346 0.311203 11.00000 0.03292 H6A 2 0.613702 0.873151 0.429427 11.00000 0.03768 H3A 2 0.940797 0.808419 0.337301 11.00000 0.03675 H3B 2 0.962787 0.855767 0.391638 11.00000 0.03827 H15B 2 0.882978 0.847917 0.615892 11.00000 0.03909 H15A 2 0.818276 0.930841 0.570806 11.00000 0.04428 H15C 2 0.937119 0.845857 0.565624 11.00000 0.04351 H10C 2 0.700290 0.683460 0.540075 11.00000 0.03917 H6B 2 0.743122 0.896134 0.453442 11.00000 0.03769 H8A 2 0.771453 1.067931 0.311724 11.00000 0.04339 H14C 2 0.450798 1.129570 0.391485 11.00000 0.06524 H14B 2 0.377004 1.225611 0.349565 11.00000 0.05971 H14A 2 0.400913 1.068915 0.340770 11.00000 0.06698 H13B 2 0.793091 0.383060 0.204082 11.00000 0.06505 H13C 2 0.738980 0.238836 0.203001 11.00000 0.05556 H13A 2 0.724784 0.324856 0.155721 11.00000 0.04607 HKLF 4 REM 1_a.res in P2(1)/c REM wR2 = 0.0597, GooF = S = 0.905, Restrained GooF = 0.905 for all data REM R1 = 0.0239 for 3534 Fo > 4sig(Fo) and 0.0355 for all 4449 data REM 340 parameters refined using 0 restraints END WGHT 0.0352 0.0000 REM Instructions for potential hydrogen bonds HTAB N7 N14_$1 HTAB N7 N11 HTAB N7 N13 HTAB N2 N11_$2 HTAB N8 N14 HTAB N8 N12_$3 HTAB N9 N11_$4 HTAB N9 S2 HTAB N9 N15_$5 HTAB N4 N12_$5 HTAB N10 S2_$6 HTAB N10 S2_$5 HTAB N5 S1_$2 HTAB N6 S2_$6 HTAB N3 S1_$2 HTAB N15 S1_$7 HTAB N15 S2_$3 HTAB N15 N12 HTAB N10 N15 HTAB N8 N11_$2 HTAB N14 N13_$2 HTAB N13 N11_$8 HTAB N13 S2_$9 REM Highest difference peak 0.224, deepest hole -0.138, 1-sigma level 0.035 Q1 1 0.6426 0.5908 0.4216 11.00000 0.05 0.22 Q2 1 0.6271 0.5392 0.3697 11.00000 0.05 0.22 Q3 1 0.6921 0.8019 0.3395 11.00000 0.05 0.19 Q4 1 0.8929 0.5989 0.4208 11.00000 0.05 0.19 Q5 1 0.8641 0.5620 0.3603 11.00000 0.05 0.18 Q6 1 0.7320 0.9590 0.3521 11.00000 0.05 0.18 Q7 1 0.6766 0.6375 0.4799 11.00000 0.05 0.18 Q8 1 0.7931 0.6208 0.4394 11.00000 0.05 0.18 Q9 1 0.6985 0.7346 0.4313 11.00000 0.05 0.17 Q10 1 0.9155 0.7062 0.3800 11.00000 0.05 0.17 Q11 1 0.5953 0.4958 0.3108 11.00000 0.05 0.17 Q12 1 0.8351 0.8057 0.3711 11.00000 0.05 0.16 Q13 1 0.7275 0.8410 0.4024 11.00000 0.05 0.16 Q14 1 1.2991 0.7866 0.5012 11.00000 0.05 0.16 Q15 1 0.6353 0.6560 0.3320 11.00000 0.05 0.16 Q16 1 0.7421 0.5269 0.3418 11.00000 0.05 0.16 Q17 1 1.2104 0.7899 0.5351 11.00000 0.05 0.15 Q18 1 0.1046 0.2825 0.2781 11.00000 0.05 0.15 Q19 1 0.2345 0.3865 0.2978 11.00000 0.05 0.13 Q20 1 0.0671 0.2008 0.2288 11.00000 0.05 0.12 ; _shelx_res_checksum 46473 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 S1 S 0.04816(3) 0.19720(4) 0.27429(2) 0.02560(7) Uani 1 1 d . . . . . S2 S 1.33932(3) 0.79885(3) 0.46356(2) 0.02347(7) Uani 1 1 d . . . . . N1 N 0.60628(9) 0.53293(11) 0.40233(3) 0.01529(17) Uani 1 1 d . . . . . N2 N 0.64512(9) 0.74444(10) 0.32009(3) 0.01561(17) Uani 1 1 d . . . . . N3 N 0.91266(9) 0.79616(10) 0.36936(3) 0.01509(17) Uani 1 1 d . . . . . N4 N 0.87043(9) 0.58837(11) 0.45247(3) 0.01484(17) Uani 1 1 d . . . . . N5 N 0.82378(9) 0.49502(10) 0.34267(4) 0.01585(17) Uani 1 1 d . . . . . N6 N 0.69450(10) 0.83846(10) 0.42877(4) 0.01608(18) Uani 1 1 d . . . . . N7 N 0.55559(10) 0.43423(11) 0.29071(4) 0.01874(19) Uani 1 1 d . . . . . N8 N 0.74062(11) 1.05621(11) 0.34507(4) 0.02083(19) Uani 1 1 d . . . . . N9 N 1.09438(9) 0.53947(11) 0.39248(4) 0.01752(18) Uani 1 1 d . . . . . N10 N 0.64894(10) 0.63181(11) 0.51423(4) 0.01685(18) Uani 1 1 d . . . . . N11 N 0.23156(11) 0.44847(12) 0.28418(4) 0.0293(2) Uani 1 1 d . . . . . N12 N 1.14369(11) 0.80022(12) 0.53620(5) 0.0332(2) Uani 1 1 d . . . . . N13 N 0.72216(12) 0.32847(15) 0.19132(5) 0.0306(2) Uani 1 1 d . . . . . N14 N 0.43831(12) 1.14780(14) 0.35501(5) 0.0305(2) Uani 1 1 d . . . . . N15 N 0.86060(11) 0.84220(12) 0.58096(4) 0.0228(2) Uani 1 1 d . . . . . C1 C 0.15526(11) 0.34459(14) 0.28023(4) 0.0222(2) Uani 1 1 d . . . . . C2 C 1.22411(11) 0.79999(12) 0.50612(4) 0.0217(2) Uani 1 1 d . . . . . Be1 Be 0.65909(14) 0.55323(16) 0.33909(5) 0.0155(2) Uani 1 1 d . . . . . Be2 Be 0.74740(14) 0.85609(15) 0.36580(5) 0.0153(2) Uani 1 1 d . . . . . Be3 Be 0.92305(13) 0.60597(15) 0.38950(5) 0.0143(2) Uani 1 1 d . . . . . Be4 Be 0.70618(14) 0.64746(15) 0.44857(5) 0.0147(2) Uani 1 1 d . . . . . H1A H 0.5230(15) 0.5578(16) 0.4014(5) 0.029(4) Uiso 1 1 d . . . . . H1B H 0.6154(15) 0.4363(17) 0.4128(6) 0.032(4) Uiso 1 1 d . . . . . H7A H 0.5439(15) 0.3420(19) 0.3036(6) 0.036(4) Uiso 1 1 d . . . . . H7B H 0.4721(15) 0.4711(16) 0.2819(5) 0.027(4) Uiso 1 1 d . . . . . H7C H 0.5892(14) 0.4216(16) 0.2614(6) 0.031(4) Uiso 1 1 d . . . . . H2A H 0.5615(15) 0.7730(15) 0.3177(5) 0.026(4) Uiso 1 1 d . . . . . H2B H 0.6669(14) 0.7576(15) 0.2869(6) 0.026(4) Uiso 1 1 d . . . . . H8B H 0.6591(16) 1.0933(17) 0.3426(6) 0.034(4) Uiso 1 1 d . . . . . H8C H 0.7899(15) 1.1153(18) 0.3684(6) 0.035(4) Uiso 1 1 d . . . . . H9A H 1.1198(15) 0.5380(17) 0.3592(6) 0.035(4) Uiso 1 1 d . . . . . H9B H 1.1544(15) 0.6009(18) 0.4129(6) 0.035(4) Uiso 1 1 d . . . . . H9C H 1.1050(16) 0.4440(19) 0.4056(6) 0.041(4) Uiso 1 1 d . . . . . H4B H 0.9176(14) 0.6439(16) 0.4767(5) 0.025(4) Uiso 1 1 d . . . . . H4A H 0.8806(14) 0.4959(18) 0.4628(5) 0.027(4) Uiso 1 1 d . . . . . H10B H 0.5689(14) 0.6734(15) 0.5140(5) 0.023(3) Uiso 1 1 d . . . . . H10A H 0.6457(14) 0.5332(18) 0.5249(5) 0.032(4) Uiso 1 1 d . . . . . H5A H 0.8363(15) 0.4004(18) 0.3495(6) 0.036(4) Uiso 1 1 d . . . . . H5B H 0.8542(15) 0.5033(17) 0.3112(6) 0.033(4) Uiso 1 1 d . . . . . H6A H 0.6137(17) 0.8732(18) 0.4294(6) 0.038(4) Uiso 1 1 d . . . . . H3A H 0.9408(15) 0.8084(17) 0.3373(6) 0.037(4) Uiso 1 1 d . . . . . H3B H 0.9628(15) 0.8558(18) 0.3916(6) 0.038(4) Uiso 1 1 d . . . . . H15B H 0.8830(16) 0.8479(18) 0.6159(6) 0.039(4) Uiso 1 1 d . . . . . H15A H 0.8183(17) 0.9308(19) 0.5708(6) 0.044(5) Uiso 1 1 d . . . . . H15C H 0.9371(17) 0.8459(19) 0.5656(6) 0.044(5) Uiso 1 1 d . . . . . H10C H 0.7003(16) 0.6835(18) 0.5401(6) 0.039(4) Uiso 1 1 d . . . . . H6B H 0.7431(16) 0.8961(18) 0.4534(6) 0.038(4) Uiso 1 1 d . . . . . H8A H 0.7715(16) 1.0679(18) 0.3117(7) 0.043(4) Uiso 1 1 d . . . . . H14C H 0.4508(19) 1.130(2) 0.3915(8) 0.065(6) Uiso 1 1 d . . . . . H14B H 0.3770(19) 1.226(2) 0.3496(7) 0.060(5) Uiso 1 1 d . . . . . H14A H 0.401(2) 1.069(2) 0.3408(8) 0.067(6) Uiso 1 1 d . . . . . H13B H 0.793(2) 0.383(2) 0.2041(8) 0.065(6) Uiso 1 1 d . . . . . H13C H 0.7390(18) 0.239(2) 0.2030(7) 0.056(6) Uiso 1 1 d . . . . . H13A H 0.7248(17) 0.3249(19) 0.1557(7) 0.046(5) Uiso 1 1 d . . . . . 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 S1 0.02613(15) 0.03108(15) 0.02020(13) -0.00250(11) 0.00528(10) -0.00038(11) S2 0.01914(13) 0.02337(14) 0.02823(13) 0.00117(11) 0.00434(10) 0.00113(10) N1 0.0140(4) 0.0154(4) 0.0163(4) 0.0017(3) 0.0016(3) -0.0016(3) N2 0.0140(4) 0.0190(4) 0.0137(4) 0.0033(3) 0.0013(3) 0.0007(3) N3 0.0149(4) 0.0152(4) 0.0153(4) 0.0000(3) 0.0023(3) -0.0023(3) N4 0.0157(4) 0.0145(4) 0.0137(4) 0.0010(3) -0.0009(3) 0.0000(3) N5 0.0166(4) 0.0140(4) 0.0169(4) -0.0014(3) 0.0022(3) -0.0004(3) N6 0.0163(4) 0.0149(4) 0.0174(4) -0.0005(3) 0.0035(3) 0.0006(3) N7 0.0174(5) 0.0213(5) 0.0170(4) -0.0028(3) 0.0003(4) -0.0032(4) N8 0.0211(5) 0.0160(5) 0.0260(5) 0.0050(4) 0.0056(4) 0.0012(4) N9 0.0147(4) 0.0182(5) 0.0195(4) -0.0019(3) 0.0016(3) 0.0007(3) N10 0.0153(4) 0.0202(5) 0.0149(4) 0.0015(3) 0.0017(3) -0.0003(4) N11 0.0261(5) 0.0344(6) 0.0289(5) -0.0075(4) 0.0091(4) 0.0013(4) N12 0.0355(6) 0.0248(5) 0.0420(6) -0.0083(5) 0.0154(5) -0.0053(4) N13 0.0283(6) 0.0358(6) 0.0283(5) -0.0006(5) 0.0055(4) 0.0071(5) N14 0.0264(6) 0.0253(6) 0.0419(6) 0.0015(5) 0.0120(5) 0.0012(4) N15 0.0239(5) 0.0238(5) 0.0205(5) -0.0014(4) 0.0027(4) -0.0018(4) C1 0.0215(6) 0.0296(6) 0.0161(5) -0.0030(4) 0.0047(4) 0.0077(4) C2 0.0217(5) 0.0152(5) 0.0277(5) -0.0039(4) 0.0008(4) -0.0018(4) Be1 0.0153(6) 0.0169(6) 0.0137(5) -0.0009(5) 0.0004(5) -0.0022(5) Be2 0.0168(6) 0.0131(6) 0.0161(5) 0.0020(5) 0.0027(5) 0.0005(5) Be3 0.0124(6) 0.0146(6) 0.0158(6) 0.0000(5) 0.0010(5) 0.0004(5) Be4 0.0160(6) 0.0149(6) 0.0131(5) 0.0008(4) 0.0017(5) -0.0010(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Be Be 0.0038 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 Be1 N1 Be4 109.05(8) . . ? Be1 N2 Be2 109.65(8) . . ? Be3 N3 Be2 108.87(8) . . ? Be4 N4 Be3 109.10(7) . . ? Be1 N5 Be3 109.82(8) . . ? Be4 N6 Be2 109.09(8) . . ? N11 C1 S1 179.54(11) . . ? N12 C2 S2 179.61(12) . . ? N5 Be1 N2 109.83(9) . . ? N5 Be1 N1 109.16(8) . . ? N2 Be1 N1 108.86(8) . . ? N5 Be1 N7 109.46(8) . . ? N2 Be1 N7 110.18(8) . . ? N1 Be1 N7 109.32(8) . . ? N2 Be2 N6 108.85(8) . . ? N2 Be2 N3 110.50(9) . . ? N6 Be2 N3 109.44(8) . . ? N2 Be2 N8 110.54(8) . . ? N6 Be2 N8 109.87(8) . . ? N3 Be2 N8 107.62(8) . . ? N3 Be3 N5 109.12(8) . . ? N3 Be3 N4 109.61(8) . . ? N5 Be3 N4 110.35(8) . . ? N3 Be3 N9 109.78(8) . . ? N5 Be3 N9 108.29(8) . . ? N4 Be3 N9 109.68(8) . . ? N4 Be4 N6 109.32(9) . . ? N4 Be4 N1 109.58(8) . . ? N6 Be4 N1 110.21(8) . . ? N4 Be4 N10 110.00(8) . . ? N6 Be4 N10 108.23(8) . . ? N1 Be4 N10 109.48(8) . . ? 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 S1 C1 1.6489(13) . ? S2 C2 1.6538(12) . ? N1 Be1 1.7211(15) . ? N1 Be4 1.7223(16) . ? N2 Be1 1.7080(16) . ? N2 Be2 1.7127(16) . ? N3 Be3 1.7060(16) . ? N3 Be2 1.7153(16) . ? N4 Be4 1.7030(16) . ? N4 Be3 1.7116(15) . ? N5 Be1 1.7054(16) . ? N5 Be3 1.7107(15) . ? N6 Be4 1.7106(15) . ? N6 Be2 1.7128(16) . ? N7 Be1 1.7931(16) . ? N8 Be2 1.7914(16) . ? N9 Be3 1.7912(16) . ? N10 Be4 1.7930(16) . ? N11 C1 1.1673(16) . ? N12 C2 1.1611(15) . ? 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 _geom_hbond_publ_flag N7 H7A N14 0.867(16) 2.417(16) 3.2271(15) 155.7(13) 1_545 yes N7 H7B N11 0.890(15) 2.411(15) 3.2115(15) 149.9(12) . yes N7 H7C N13 0.844(15) 2.446(15) 3.2654(15) 164.0(13) . yes N2 H2B N11 0.882(14) 2.694(14) 3.4690(13) 147.4(11) 2_655 yes N8 H8B N14 0.866(16) 2.306(16) 3.1511(16) 164.9(13) . yes N8 H8C N12 0.870(15) 2.473(15) 3.2519(15) 149.4(13) 3_776 yes N9 H9A N11 0.892(15) 2.408(15) 3.2535(13) 158.4(13) 1_655 yes N9 H9B S2 0.902(15) 2.691(15) 3.5886(10) 173.6(12) . yes N9 H9C N15 0.883(16) 2.497(17) 3.3601(14) 166.0(13) 3_766 yes N4 H4A N12 0.836(15) 2.554(15) 3.3520(14) 160.1(12) 3_766 yes N10 H10B S2 0.872(14) 2.683(14) 3.4821(10) 152.9(11) 1_455 yes N10 H10A S2 0.889(15) 2.866(16) 3.7370(10) 166.7(12) 3_766 yes N5 H5B S1 0.873(15) 2.951(15) 3.7345(10) 150.2(12) 2_655 yes N6 H6A S2 0.860(16) 3.030(16) 3.7615(10) 144.3(12) 1_455 yes N3 H3A S1 0.880(15) 2.934(15) 3.7194(9) 149.6(12) 2_655 yes N15 H15B S1 0.865(16) 2.739(16) 3.5903(10) 168.6(13) 3_666 yes N15 H15A S2 0.890(17) 2.867(17) 3.7548(11) 175.0(14) 3_776 yes N15 H15C N12 0.894(17) 2.302(17) 3.1790(15) 166.6(14) . yes N10 H10C N15 0.884(16) 2.238(17) 3.0855(13) 160.7(14) . yes N8 H8A N11 0.921(16) 2.579(16) 3.3708(14) 144.4(12) 2_655 yes N14 H14A N13 0.83(2) 2.48(2) 3.3019(17) 173.1(17) 2_655 yes N13 H13C N11 0.831(19) 2.525(19) 3.3388(17) 166.5(16) 2_645 yes N13 H13A S2 0.884(17) 2.942(17) 3.8050(12) 165.7(14) 2_745 yes