#------------------------------------------------------------------------------ #$Date: 2020-10-06 10:38:37 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257400 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/80/1558020.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_1558020 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_sum 'C2 H36 Be4 N16' _chemical_formula_weight 320.51 _space_group_crystal_system trigonal _space_group_IT_number 143 _space_group_name_Hall 'P 3' _space_group_name_H-M_alt 'P 3' _atom_sites_solution_hydrogens mixed _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 90 _cell_angle_gamma 120 _cell_formula_units_Z 3 _cell_length_a 14.1334(3) _cell_length_b 14.1334(3) _cell_length_c 8.5563(3) _cell_measurement_reflns_used 29697 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 158.92 _cell_measurement_theta_min 7.22 _cell_volume 1480.16(7) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 5.81 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.992 _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 0.0318 _diffrn_reflns_av_unetI/netI 0.0210 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 31215 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.977 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 79.077 _diffrn_reflns_theta_min 3.611 _diffrn_source 'GeniX 3D HF Cu' _exptl_absorpt_coefficient_mu 0.616 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.079 _exptl_crystal_description Cuboctahedron _exptl_crystal_F_000 528 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.213 _refine_diff_density_min -0.188 _refine_diff_density_rms 0.030 _refine_ls_abs_structure_details ; Twinning involves inversion, so Flack parameter cannot be determined ; _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 255 _refine_ls_number_reflns 4168 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.995 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0340 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0564P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0840 _refine_ls_wR_factor_ref 0.0862 _reflns_Friedel_coverage 0.970 _reflns_Friedel_fraction_full 0.995 _reflns_Friedel_fraction_max 0.962 _reflns_number_gt 3657 _reflns_number_total 4168 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc01112f2.cif _cod_data_source_block 3 _cod_depositor_comments ;Adding full bibliography for 1558013--1558021.cif. Adding full bibliography for 1558013--1558021.cif. ; _cod_original_cell_volume 1480.16(8) _cod_database_code 1558020 _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 P3 3.res created by SHELXL-2018/3 at 19:13:04 on 30-Oct-2018 REM Old TITL 1 in P-3 REM SHELXT solution in P3: R1 0.084, Rweak 0.015, Alpha 0.005 REM 0.000 for 0 systematic absences, Orientation as input REM Flack x = 0.312 ( 0.066 ) from 1599 Parsons' quotients REM Formula found by SHELXT: C Be2 N8 CELL 1.54178 14.1334 14.1334 8.5563 90.000 90.000 120.000 ZERR 3.000 0.0003 0.0003 0.0003 0.000 0.000 0.000 LATT -1 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SFAC C H BE N UNIT 6 108 12 48 L.S. 10 BOND ACTA LIST 4 TEMP -173.15 FMAP 2 PLAN 20 HTAB HTAB N8 N13 EQIV $4 -x+y, -x, z HTAB N9 N14_$4 HTAB N9 N14 EQIV $3 -y, x-y, z HTAB N9 N14_$3 HTAB N10 N16 HTAB N10 N18 EQIV $6 -y+1, x-y, z HTAB N11 N17_$6 EQIV $5 -x+y+1, -x+1, z HTAB N11 N17_$5 HTAB N11 N17 EQIV $7 -y+1, x-y, z+1 HTAB N12 N17_$7 EQIV $8 x+1, y, z+1 HTAB N12 N18_$8 EQIV $9 -y, x-y, z-1 HTAB N13 N17_$9 EQIV $10 -x+y, -x+1, z-1 HTAB N13 N17_$10 EQIV $11 x, y, z-1 HTAB N13 N18_$11 HTAB N14 N15 HTAB N14 N16_$9 HTAB N15 N18_$3 EQIV $12 x, y, z+1 HTAB N16 N13_$12 HTAB N16 N14_$12 TWIN 1 0 0 0 1 0 0 0 -1 REM EXTI 0.000093 REM 1_a.res in P3 REM wR2 = 0.0831, GooF = S = 0.961, Restrained GooF = 0.961 for all data REM R1 = 0.0330 for 3657 Fo > 4sig(Fo) and 0.0395 for all 4168 data REM 273 parameters refined using 1 restraints WGHT 0.056400 BASF 0.00027 FVAR 0.46156 0.65553 N1 4 0.270264 0.736200 0.092749 11.00000 0.02369 0.02370 = 0.02258 -0.00052 0.00050 0.01255 AFIX 23 H1A 2 0.269536 0.736966 0.199082 11.00000 -1.20000 H1B 2 0.236960 0.772997 0.057439 11.00000 -1.20000 AFIX 0 N2 4 0.201597 0.606056 -0.173860 11.00000 0.02462 0.02487 = 0.02340 -0.00275 -0.00255 0.01219 AFIX 23 H2A 2 0.162968 0.536600 -0.211249 11.00000 -1.20000 H2B 2 0.169195 0.643878 -0.208493 11.00000 -1.20000 AFIX 0 N3 4 0.066735 0.131829 0.535791 11.00000 0.02244 0.02071 = 0.02305 0.00180 0.00099 0.01001 AFIX 23 H3A 2 0.033117 0.167950 0.498986 11.00000 -1.20000 H3B 2 0.136824 0.166756 0.500318 11.00000 -1.20000 AFIX 0 N4 4 0.131663 0.066030 0.803822 11.00000 0.02080 0.02199 = 0.02339 -0.00050 -0.00153 0.00974 AFIX 23 H4A 2 0.132137 0.066282 0.910174 11.00000 -1.20000 H4B 2 0.202155 0.101351 0.770017 11.00000 -1.20000 AFIX 0 N5 4 0.798753 0.406122 1.439056 11.00000 0.02335 0.02537 = 0.02469 -0.00341 -0.00197 0.01192 AFIX 23 H5A 2 0.868752 0.444785 1.403734 11.00000 -1.20000 H5B 2 0.800290 0.406926 1.545388 11.00000 -1.20000 AFIX 0 N6 4 0.741719 0.276376 1.172928 11.00000 0.02503 0.02434 = 0.02434 -0.00291 -0.00105 0.01337 AFIX 23 H6A 2 0.712983 0.207105 1.135553 11.00000 -1.20000 H6B 2 0.811837 0.316175 1.138451 11.00000 -1.20000 REM ##### AFIX 0 N7 4 0.333333 0.666667 -0.451883 10.33333 0.02935 0.02935 = 0.02318 0.00000 0.00000 0.01467 AFIX 137 H7A 2 0.394080 0.666752 -0.487335 10.33333 -1.50000 H7B 2 0.333248 0.727328 -0.487335 10.33333 -1.50000 H7C 2 0.272672 0.605920 -0.487335 10.33333 -1.50000 AFIX 0 N8 4 0.063477 0.536488 0.096068 11.00000 0.02289 0.02705 = 0.02745 0.00091 0.00063 0.01181 AFIX 137 H8A 2 0.035168 0.581457 0.084489 11.00000 -1.50000 H8B 2 0.062267 0.519457 0.198889 11.00000 -1.50000 H8C 2 0.022866 0.474211 0.040125 11.00000 -1.50000 AFIX 0 N9 4 0.000000 0.000000 0.259381 10.33333 0.02534 0.02534 = 0.02389 0.00000 0.00000 0.01267 AFIX 137 H9A 2 0.065038 0.055159 0.223929 10.33333 -1.50000 H9B 2 -0.055159 0.009879 0.223929 10.33333 -1.50000 H9C 2 -0.009879 -0.065038 0.223929 10.33333 -1.50000 AFIX 0 N10 4 0.134278 0.270543 0.805201 11.00000 0.02511 0.02200 = 0.02635 -0.00206 0.00020 0.01157 AFIX 137 H10A 2 0.206084 0.293218 0.822005 11.00000 -1.50000 H10B 2 0.103034 0.274516 0.896119 11.00000 -1.50000 H10C 2 0.128400 0.314162 0.732220 11.00000 -1.50000 AFIX 0 N11 4 0.666667 0.333333 0.896061 10.33333 0.02711 0.02711 = 0.02490 0.00000 0.00000 0.01356 AFIX 137 H11A 2 0.675382 0.277458 0.860610 10.33333 -1.50000 H11B 2 0.722542 0.397924 0.860610 10.33333 -1.50000 H11C 2 0.602076 0.324618 0.860610 10.33333 -1.50000 AFIX 0 N12 4 0.813950 0.212189 1.451104 11.00000 0.02894 0.02864 = 0.02854 -0.00237 -0.00485 0.01617 AFIX 137 H12A 2 0.791399 0.189250 1.550600 11.00000 -1.50000 H12B 2 0.886686 0.261888 1.451208 11.00000 -1.50000 H12C 2 0.801340 0.153999 1.390765 11.00000 -1.50000 AFIX 0 N13 4 -0.069140 0.360217 -0.163808 11.00000 0.02786 0.03159 = 0.03670 -0.00327 -0.00310 0.01367 N14 4 -0.222970 0.000862 0.176193 11.00000 0.03206 0.03219 = 0.03504 0.00159 -0.00436 0.01248 N15 4 -0.387654 -0.058267 0.470681 11.00000 0.04498 0.03611 = 0.03500 0.00115 0.00052 0.02013 N16 4 0.007495 0.256219 1.126459 11.00000 0.03265 0.03322 = 0.03265 -0.00329 0.00242 0.01758 N17 4 0.436910 0.302778 0.787296 11.00000 0.06104 0.04681 = 0.05209 0.01121 0.01189 0.03227 N18 4 0.088533 0.395731 0.522810 11.00000 0.06901 0.06002 = 0.05596 0.00661 0.01367 0.04407 C1 1 0.382044 0.317571 0.857126 11.00000 0.03995 0.03379 = 0.05781 -0.00491 0.01416 0.01294 C2 1 0.087233 0.446728 0.431000 11.00000 0.06119 0.04337 = 0.03454 0.00671 0.00948 0.02898 BE1 3 0.333333 0.666667 -0.240857 10.33333 0.02559 0.02559 = 0.02184 0.00000 0.00000 0.01279 BE2 3 0.201202 0.603930 0.026748 11.00000 0.02029 0.02247 = 0.02471 0.00041 0.00052 0.01054 BE3 3 0.000000 0.000000 0.469213 10.33333 0.02284 0.02284 = 0.02120 0.00000 0.00000 0.01142 BE4 3 0.066147 0.132525 0.736962 11.00000 0.02318 0.01955 = 0.02319 -0.00081 0.00060 0.01047 BE5 3 0.666667 0.333333 1.106147 10.33333 0.02498 0.02498 = 0.02000 0.00000 0.00000 0.01249 BE6 3 0.739569 0.274404 1.373385 11.00000 0.02355 0.02463 = 0.02675 -0.00238 -0.00324 0.01355 H13A 2 -0.125893 0.302290 -0.166437 11.00000 0.03606 H13B 2 -0.082571 0.421669 -0.184990 11.00000 0.06137 H13C 2 -0.024833 0.357607 -0.240476 11.00000 0.05984 H14A 2 -0.249032 0.018345 0.091494 11.00000 0.03722 H14B 2 -0.257607 0.000652 0.253254 11.00000 0.06038 H14C 2 -0.230467 -0.069770 0.148259 11.00000 0.05631 H15A 2 -0.456282 -0.079011 0.454034 11.00000 0.02405 H15B 2 -0.395860 -0.130925 0.485179 11.00000 0.06419 H15C 2 -0.371121 -0.031941 0.572035 11.00000 0.09225 H16A 2 -0.021553 0.287824 1.059504 11.00000 0.05274 H16B 2 -0.042555 0.197410 1.159994 11.00000 0.03780 H16C 2 0.022254 0.294343 1.222001 11.00000 0.04585 HKLF 4 REM 1_a.res in P3 REM wR2 = 0.0862, GooF = S = 0.995, Restrained GooF = 0.995 for all data REM R1 = 0.0340 for 3657 Fo > 4sig(Fo) and 0.0407 for all 4168 data REM 255 parameters refined using 1 restraints END WGHT 0.0561 0.0000 REM Instructions for potential hydrogen bonds HTAB N8 N13 HTAB N9 N14_$4 HTAB N9 N14 HTAB N9 N14_$3 HTAB N10 N16 HTAB N10 N18 HTAB N11 N17_$6 HTAB N11 N17_$5 HTAB N11 N17 HTAB N12 N17_$7 HTAB N12 N18_$8 HTAB N13 N17_$9 HTAB N13 N17_$10 HTAB N13 N18_$11 HTAB N14 N15 HTAB N14 N16_$9 HTAB N15 N18_$3 HTAB N16 N13_$12 HTAB N16 N14_$12 REM Highest difference peak 0.213, deepest hole -0.188, 1-sigma level 0.030 Q1 1 0.1446 0.4602 0.4673 11.00000 0.05 0.21 Q2 1 0.2164 0.6086 -0.1077 11.00000 0.05 0.16 Q3 1 0.0390 0.3731 0.4341 11.00000 0.05 0.15 Q4 1 0.6667 0.3333 1.6428 10.33333 0.05 0.11 Q5 1 0.0771 0.1321 0.6460 11.00000 0.05 0.11 Q6 1 0.4650 0.3761 0.8201 11.00000 0.05 0.11 Q7 1 0.1352 0.4724 0.2701 11.00000 0.05 0.10 Q8 1 0.2294 0.7820 -0.1223 11.00000 0.05 0.10 Q9 1 0.1553 0.2374 0.7727 11.00000 0.05 0.10 Q10 1 0.2426 0.8127 -0.0073 11.00000 0.05 0.10 Q11 1 -0.0136 0.1782 0.9979 11.00000 0.05 0.10 Q12 1 0.3333 0.6667 -0.3837 10.33333 0.05 0.09 Q13 1 0.4555 0.2363 0.8863 11.00000 0.05 0.09 Q14 1 0.1425 0.4997 0.5923 11.00000 0.05 0.09 Q15 1 0.0984 0.0984 0.8161 11.00000 0.05 0.08 Q16 1 0.1162 0.6940 0.2228 11.00000 0.05 0.08 Q17 1 0.3333 0.6667 -0.6855 10.33333 0.05 0.08 Q18 1 0.2000 0.7230 -0.2706 11.00000 0.05 0.08 Q19 1 0.4177 0.3225 0.6527 11.00000 0.05 0.08 Q20 1 0.4808 0.2933 0.9398 11.00000 0.05 0.08 ; _shelx_res_checksum 94365 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 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 N1 N 0.27026(13) 0.73620(13) 0.09275(19) 0.0230(4) Uani 1 1 d . . . . . H1A H 0.269536 0.736966 0.199082 0.028 Uiso 1 1 calc R U . . . H1B H 0.236960 0.772997 0.057439 0.028 Uiso 1 1 calc R U . . . N2 N 0.20160(14) 0.60606(14) -0.17386(19) 0.0244(4) Uani 1 1 d . . . . . H2A H 0.162968 0.536600 -0.211249 0.029 Uiso 1 1 calc R U . . . H2B H 0.169195 0.643878 -0.208493 0.029 Uiso 1 1 calc R U . . . N3 N 0.06673(13) 0.13183(13) 0.53579(17) 0.0224(3) Uani 1 1 d . . . . . H3A H 0.033117 0.167950 0.498986 0.027 Uiso 1 1 calc R U . . . H3B H 0.136824 0.166756 0.500318 0.027 Uiso 1 1 calc R U . . . N4 N 0.13166(13) 0.06603(13) 0.80382(18) 0.0225(4) Uani 1 1 d . . . . . H4A H 0.132137 0.066282 0.910174 0.027 Uiso 1 1 calc R U . . . H4B H 0.202155 0.101351 0.770017 0.027 Uiso 1 1 calc R U . . . N5 N 0.79875(13) 0.40612(13) 1.4391(2) 0.0246(3) Uani 1 1 d . . . . . H5A H 0.868752 0.444785 1.403734 0.030 Uiso 1 1 calc R U . . . H5B H 0.800290 0.406926 1.545388 0.030 Uiso 1 1 calc R U . . . N6 N 0.74172(14) 0.27638(13) 1.1729(2) 0.0241(3) Uani 1 1 d . . . . . H6A H 0.712983 0.207105 1.135553 0.029 Uiso 1 1 calc R U . . . H6B H 0.811837 0.316175 1.138451 0.029 Uiso 1 1 calc R U . . . N7 N 0.333333 0.666667 -0.4519(3) 0.0273(6) Uani 1 3 d S T P . . H7A H 0.394080 0.666752 -0.487335 0.041 Uiso 0.3333 1 calc R U P . . H7B H 0.333248 0.727328 -0.487335 0.041 Uiso 0.3333 1 calc R U P . . H7C H 0.272672 0.605920 -0.487335 0.041 Uiso 0.3333 1 calc R U P . . N8 N 0.06348(13) 0.53649(14) 0.0961(2) 0.0261(4) Uani 1 1 d . . . . . H8A H 0.035168 0.581457 0.084489 0.039 Uiso 1 1 calc R U . . . H8B H 0.062267 0.519457 0.198889 0.039 Uiso 1 1 calc R U . . . H8C H 0.022866 0.474211 0.040125 0.039 Uiso 1 1 calc R U . . . N9 N 0.000000 0.000000 0.2594(3) 0.0249(6) Uani 1 3 d S T P . . H9A H 0.065038 0.055159 0.223929 0.037 Uiso 0.3333 1 calc R U P . . H9B H -0.055159 0.009879 0.223929 0.037 Uiso 0.3333 1 calc R U P . . H9C H -0.009879 -0.065038 0.223929 0.037 Uiso 0.3333 1 calc R U P . . N10 N 0.13428(13) 0.27054(12) 0.80520(18) 0.0246(4) Uani 1 1 d . . . . . H10A H 0.206084 0.293218 0.822005 0.037 Uiso 1 1 calc R U . . . H10B H 0.103034 0.274516 0.896119 0.037 Uiso 1 1 calc R U . . . H10C H 0.128400 0.314162 0.732220 0.037 Uiso 1 1 calc R U . . . N11 N 0.666667 0.333333 0.8961(3) 0.0264(6) Uani 1 3 d S T P . . H11A H 0.675382 0.277458 0.860610 0.040 Uiso 0.3333 1 calc R U P . . H11B H 0.722542 0.397924 0.860610 0.040 Uiso 0.3333 1 calc R U P . . H11C H 0.602076 0.324618 0.860610 0.040 Uiso 0.3333 1 calc R U P . . N12 N 0.81395(13) 0.21219(13) 1.4511(2) 0.0279(3) Uani 1 1 d . . . . . H12A H 0.791399 0.189250 1.550600 0.042 Uiso 1 1 calc R U . . . H12B H 0.886686 0.261888 1.451208 0.042 Uiso 1 1 calc R U . . . H12C H 0.801340 0.153999 1.390765 0.042 Uiso 1 1 calc R U . . . N13 N -0.06914(16) 0.36022(17) -0.1638(3) 0.0326(4) Uani 1 1 d . . . . . N14 N -0.22297(16) 0.00086(17) 0.1762(2) 0.0347(4) Uani 1 1 d . . . . . N15 N -0.38765(19) -0.05827(19) 0.4707(3) 0.0388(5) Uani 1 1 d . . . . . N16 N 0.00750(18) 0.25622(18) 1.1265(2) 0.0323(4) Uani 1 1 d . . . . . N17 N 0.4369(2) 0.3028(2) 0.7873(3) 0.0510(6) Uani 1 1 d . . . . . N18 N 0.0885(2) 0.3957(2) 0.5228(3) 0.0564(7) Uani 1 1 d . . . . . C1 C 0.3820(2) 0.3176(2) 0.8571(3) 0.0463(6) Uani 1 1 d . . . . . C2 C 0.0872(2) 0.4467(2) 0.4310(3) 0.0451(6) Uani 1 1 d . . . . . Be1 Be 0.333333 0.666667 -0.2409(5) 0.0243(8) Uani 1 3 d S T P . . Be2 Be 0.20120(19) 0.60393(19) 0.0267(3) 0.0226(5) Uani 1 1 d . . . . . Be3 Be 0.000000 0.000000 0.4692(5) 0.0223(8) Uani 1 3 d S T P . . Be4 Be 0.06615(19) 0.13253(19) 0.7370(3) 0.0221(5) Uani 1 1 d . . . . . Be5 Be 0.666667 0.333333 1.1061(5) 0.0233(7) Uani 1 3 d S T P . . Be6 Be 0.73957(19) 0.2744(2) 1.3734(3) 0.0243(5) Uani 1 1 d . . . . . H13A H -0.126(2) 0.302(2) -0.166(3) 0.036(7) Uiso 1 1 d . . . . . H13B H -0.083(3) 0.422(3) -0.185(4) 0.061(9) Uiso 1 1 d . . . . . H13C H -0.025(3) 0.358(3) -0.240(4) 0.060(9) Uiso 1 1 d . . . . . H14A H -0.249(2) 0.018(2) 0.091(3) 0.037(7) Uiso 1 1 d . . . . . H14B H -0.258(3) 0.001(3) 0.253(4) 0.060(10) Uiso 1 1 d . . . . . H14C H -0.230(2) -0.070(3) 0.148(4) 0.056(9) Uiso 1 1 d . . . . . H15A H -0.456(2) -0.079(2) 0.454(3) 0.024(6) Uiso 1 1 d . . . . . H15B H -0.396(3) -0.131(3) 0.485(4) 0.064(10) Uiso 1 1 d . . . . . H15C H -0.371(3) -0.032(3) 0.572(4) 0.092(14) Uiso 1 1 d . . . . . H16A H -0.022(2) 0.288(2) 1.060(3) 0.053(9) Uiso 1 1 d . . . . . H16B H -0.043(2) 0.197(2) 1.160(3) 0.038(8) Uiso 1 1 d . . . . . H16C H 0.022(2) 0.294(2) 1.222(3) 0.046(8) 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 N1 0.0237(8) 0.0237(8) 0.0226(9) -0.0005(6) 0.0005(6) 0.0125(6) N2 0.0246(8) 0.0249(8) 0.0234(9) -0.0028(6) -0.0026(6) 0.0122(6) N3 0.0224(7) 0.0207(7) 0.0231(8) 0.0018(6) 0.0010(6) 0.0100(6) N4 0.0208(7) 0.0220(7) 0.0234(9) -0.0005(6) -0.0015(6) 0.0097(6) N5 0.0233(7) 0.0254(8) 0.0247(8) -0.0034(6) -0.0020(6) 0.0119(6) N6 0.0250(8) 0.0243(8) 0.0243(7) -0.0029(6) -0.0010(6) 0.0134(6) N7 0.0293(9) 0.0293(9) 0.0232(15) 0.000 0.000 0.0147(5) N8 0.0229(8) 0.0271(8) 0.0275(9) 0.0009(6) 0.0006(6) 0.0118(7) N9 0.0253(8) 0.0253(8) 0.0239(14) 0.000 0.000 0.0127(4) N10 0.0251(8) 0.0220(8) 0.0264(10) -0.0021(6) 0.0002(6) 0.0116(6) N11 0.0271(8) 0.0271(8) 0.0249(15) 0.000 0.000 0.0136(4) N12 0.0289(8) 0.0286(8) 0.0285(8) -0.0024(7) -0.0048(7) 0.0162(7) N13 0.0279(9) 0.0316(10) 0.0367(10) -0.0033(8) -0.0031(8) 0.0137(8) N14 0.0321(9) 0.0322(10) 0.0350(10) 0.0016(8) -0.0044(8) 0.0125(8) N15 0.0450(12) 0.0361(10) 0.0350(10) 0.0012(8) 0.0005(9) 0.0201(10) N16 0.0326(9) 0.0332(10) 0.0327(9) -0.0033(8) 0.0024(7) 0.0176(8) N17 0.0610(15) 0.0468(13) 0.0521(14) 0.0112(11) 0.0119(11) 0.0323(12) N18 0.0690(17) 0.0600(16) 0.0560(15) 0.0066(12) 0.0137(12) 0.0441(14) C1 0.0399(14) 0.0338(12) 0.0578(16) -0.0049(11) 0.0142(12) 0.0129(11) C2 0.0612(17) 0.0434(14) 0.0345(12) 0.0067(11) 0.0095(11) 0.0290(13) Be1 0.0256(12) 0.0256(12) 0.022(2) 0.000 0.000 0.0128(6) Be2 0.0203(10) 0.0225(11) 0.0247(12) 0.0004(8) 0.0005(8) 0.0105(9) Be3 0.0228(11) 0.0228(11) 0.0212(19) 0.000 0.000 0.0114(6) Be4 0.0232(11) 0.0195(10) 0.0232(11) -0.0008(8) 0.0006(8) 0.0105(9) Be5 0.0250(11) 0.0250(11) 0.0200(17) 0.000 0.000 0.0125(6) Be6 0.0236(11) 0.0246(11) 0.0267(11) -0.0024(9) -0.0032(9) 0.0135(9) 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' 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 Be2 N1 Be2 109.44(17) . 3_565 ? Be1 N2 Be2 109.67(18) . . ? Be3 N3 Be4 109.72(17) . . ? Be4 N4 Be4 109.98(17) . 3 ? Be6 N5 Be6 109.64(18) . 2_655 ? Be6 N6 Be5 109.27(18) . . ? N2 Be1 N2 109.39(14) 3_565 2_665 ? N2 Be1 N2 109.39(14) 3_565 . ? N2 Be1 N2 109.39(14) 2_665 . ? N2 Be1 N7 109.55(14) 3_565 . ? N2 Be1 N7 109.55(14) 2_665 . ? N2 Be1 N7 109.55(14) . . ? N1 Be2 N2 108.36(15) . . ? N1 Be2 N1 110.02(17) . 2_665 ? N2 Be2 N1 109.92(15) . 2_665 ? N1 Be2 N8 110.28(15) . . ? N2 Be2 N8 109.53(15) . . ? N1 Be2 N8 108.72(14) 2_665 . ? N3 Be3 N3 109.50(13) 2 3 ? N3 Be3 N3 109.50(13) 2 . ? N3 Be3 N3 109.50(13) 3 . ? N3 Be3 N9 109.44(13) 2 . ? N3 Be3 N9 109.44(13) 3 . ? N3 Be3 N9 109.44(13) . . ? N4 Be4 N4 108.93(16) . 2 ? N4 Be4 N3 108.97(14) . . ? N4 Be4 N3 109.71(15) 2 . ? N4 Be4 N10 110.21(15) . . ? N4 Be4 N10 109.65(14) 2 . ? N3 Be4 N10 109.35(14) . . ? N6 Be5 N6 109.52(14) . 3_665 ? N6 Be5 N6 109.52(14) . 2_655 ? N6 Be5 N6 109.52(14) 3_665 2_655 ? N6 Be5 N11 109.42(14) . . ? N6 Be5 N11 109.42(14) 3_665 . ? N6 Be5 N11 109.42(14) 2_655 . ? N5 Be6 N6 108.41(15) . . ? N5 Be6 N5 109.94(17) . 3_665 ? N6 Be6 N5 110.02(15) . 3_665 ? N5 Be6 N12 108.84(15) . . ? N6 Be6 N12 111.54(15) . . ? N5 Be6 N12 108.08(15) 3_665 . ? 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 N1 Be2 1.715(3) . ? N1 Be2 1.718(3) 3_565 ? N2 Be1 1.713(2) . ? N2 Be2 1.717(3) . ? N3 Be3 1.711(2) . ? N3 Be4 1.721(3) . ? N4 Be4 1.714(3) . ? N4 Be4 1.716(3) 3 ? N5 Be6 1.710(3) . ? N5 Be6 1.716(3) 2_655 ? N6 Be6 1.715(3) . ? N6 Be5 1.719(2) . ? N7 Be1 1.806(5) . ? N8 Be2 1.787(3) . ? N9 Be3 1.795(5) . ? N10 Be4 1.787(3) . ? N11 Be5 1.798(5) . ? N12 Be6 1.801(3) . ? N17 C1 1.079(3) . ? N18 C2 1.072(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 _geom_hbond_publ_flag N8 H8C N13 0.91 2.29 3.161(3) 160.7 . yes N9 H9A N14 0.91 2.35 3.237(2) 165.9 3 yes N9 H9B N14 0.91 2.35 3.237(2) 165.9 . yes N9 H9C N14 0.91 2.35 3.237(2) 165.9 2 yes N10 H10B N16 0.91 2.33 3.232(3) 171.4 . yes N10 H10C N18 0.91 2.35 3.245(3) 169.3 . yes N11 H11A N17 0.91 2.28 3.193(3) 176.5 2_655 yes N11 H11B N17 0.91 2.28 3.193(3) 176.5 3_665 yes N11 H11C N17 0.91 2.28 3.193(3) 176.5 . yes N12 H12A N17 0.91 2.33 3.224(3) 166.1 2_656 yes N12 H12B N18 0.91 2.59 3.478(3) 166.3 1_656 yes N13 H13A N17 0.81(3) 2.47(3) 3.277(3) 172(2) 2_554 yes N13 H13B N17 0.99(3) 2.46(3) 3.446(3) 173(3) 3_564 yes N13 H13C N18 0.92(3) 2.47(3) 3.360(3) 163(3) 1_554 yes N14 H14B N15 0.82(3) 2.45(3) 3.243(3) 163(3) . yes N14 H14C N16 0.98(3) 2.38(3) 3.345(3) 170(3) 2_554 yes N15 H15B N18 0.98(3) 2.51(3) 3.491(4) 174(3) 2 yes N16 H16A N13 0.94(3) 2.42(3) 3.331(3) 165(3) 1_556 yes N16 H16B N14 0.83(3) 2.67(3) 3.473(3) 162(3) 1_556 yes