#------------------------------------------------------------------------------ #$Date: 2020-10-06 10:38:37 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257400 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/80/1558015.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_1558015 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 '[Be4(NH2)6(NH3)4]+4NH3' _chemical_formula_sum 'Be4 Br2 H36 N14' _chemical_formula_weight 428.29 _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 geom _audit_creation_method SHELXL-2014/7 _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 14.2177(13) _cell_length_b 14.2177(13) _cell_length_c 8.5600(12) _cell_measurement_reflns_used 16758 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 150.00 _cell_measurement_theta_min 7.12 _cell_volume 1498.5(3) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 5.81 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 0.0638 _diffrn_reflns_av_unetI/netI 0.0427 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 12189 _diffrn_reflns_point_group_measured_fraction_full 0.937 _diffrn_reflns_point_group_measured_fraction_max 0.929 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 75.476 _diffrn_reflns_theta_min 3.590 _diffrn_source 'GeniX 3D HF Cu' _exptl_absorpt_coefficient_mu 5.228 _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. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.424 _exptl_crystal_description block _exptl_crystal_F_000 660 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_transmission_factor_max 1.0000 _exptl_transmission_factor_min 0.0728 _refine_diff_density_max 1.946 _refine_diff_density_min -1.089 _refine_diff_density_rms 0.275 _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 1.019 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 188 _refine_ls_number_reflns 3765 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.019 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0697 _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^)+(0.1581P)^2^+1.0011P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1757 _refine_ls_wR_factor_ref 0.1768 _reflns_Friedel_coverage 0.860 _reflns_Friedel_fraction_full 0.876 _reflns_Friedel_fraction_max 0.859 _reflns_number_gt 3698 _reflns_number_total 3765 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc01112f2.cif _cod_data_source_block 5_CCDC2 _cod_depositor_comments ;Adding full bibliography for 1558013--1558021.cif. Adding full bibliography for 1558013--1558021.cif. ; _cod_original_formula_sum 'Be4 H36 Br2 N14' _cod_database_code 1558015 _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 ; 5.res created by SHELXL-2014/7 TITL 1_b.res in P3 REM Old TITL 1 in P-3 REM SHELXT solution in P3 REM R1 0.142, Rweak 0.025, Alpha 0.049, Orientation as input REM Flack x = 0.449 ( 0.038 ) from Parsons' quotients REM Formula found by SHELXT: Be10 N19 Br3 CELL 1.54178 14.2177 14.2177 8.5600 90.000 90.000 120.000 ZERR 3.000 0.0013 0.0013 0.0012 0.000 0.000 0.000 LATT -1 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SFAC BE H N BR UNIT 12 108 42 6 L.S. 10 BOND $H TWIN 0 1 0 1 0 0 0 0 1 ACTA TEMP -173.15 LIST 4 FMAP 2 HTAB HTAB N2 Br1 EQIV $1 -y+1, x-y, z HTAB N4 Br2_$1 HTAB N5 Br1 EQIV $2 -x+y, -x, z-1 HTAB N7 N15_$2 EQIV $3 x, y, z-1 HTAB N7 N15_$3 EQIV $4 -y, x-y, z-1 HTAB N7 N15_$4 HTAB N8 Br1 EQIV $5 -y+1, x-y, z-1 HTAB N8 Br2_$5 EQIV $6 -x+y, -x, z HTAB N8 N14_$6 HTAB N9 Br2_$3 HTAB N9 Br2_$5 EQIV $7 -x+y+1, -x+1, z-1 HTAB N9 Br2_$7 HTAB N10 Br1 EQIV $8 -y+1, x-y+1, z HTAB N10 N13_$8 HTAB N10 Br2 HTAB N11 Br1 HTAB N11 Br1_$8 EQIV $9 -x+y, -x+1, z HTAB N11 Br1_$9 EQIV $10 x, y, z+1 HTAB N12 Br1_$10 HTAB N12 Br2_$9 PLAN 20 SHEL 999999 0.795 REM EXTI 0.000000 WGHT 0.158100 1.001100 BASF 0.00265 FVAR 0.24429 BR1 4 0.310568 0.407649 0.579763 11.00000 0.01855 0.01521 = 0.02140 -0.00025 -0.00003 0.00853 BR2 4 0.679861 0.586551 1.228124 11.00000 0.02200 0.01878 = 0.01975 0.00064 0.00062 0.01132 N1 3 0.130726 0.068317 0.278485 11.00000 0.01677 0.01371 = 0.01869 0.00218 0.00143 0.00573 AFIX 23 H1A 2 0.164363 0.137922 0.242798 11.00000 -1.20000 H1B 2 0.167747 0.036039 0.241748 11.00000 -1.20000 AFIX 0 N2 3 0.063444 0.130942 0.546393 11.00000 0.01365 0.01604 = 0.01528 -0.00197 0.00089 0.00514 AFIX 23 H2A 2 0.097417 0.201213 0.513519 11.00000 -1.20000 H2B 2 0.063413 0.130799 0.652701 11.00000 -1.20000 AFIX 0 N3 3 0.597307 0.395616 0.589254 11.00000 0.01544 0.01504 = 0.02090 0.00428 0.00391 0.00740 AFIX 23 H3A 2 0.629089 0.464776 0.552060 11.00000 -1.20000 H3B 2 0.527555 0.359000 0.554234 11.00000 -1.20000 AFIX 0 N4 3 0.534039 0.264643 0.855776 11.00000 0.01541 0.01610 = 0.01939 0.00588 0.00443 0.00696 AFIX 23 H4A 2 0.532582 0.263832 0.962064 11.00000 -1.20000 H4B 2 0.464339 0.228662 0.820470 11.00000 -1.20000 AFIX 0 N5 3 0.257448 0.535563 0.933803 11.00000 0.01515 0.01401 = 0.02297 -0.00165 0.00211 0.00794 AFIX 23 H5A 2 0.284685 0.494495 0.894860 11.00000 -1.20000 H5B 2 0.187639 0.506666 0.900353 11.00000 -1.20000 AFIX 0 N6 3 0.201686 0.607058 1.200376 11.00000 0.01566 0.01956 = 0.01774 0.00290 0.00237 0.00881 AFIX 23 H6A 2 0.200329 0.606393 1.306667 11.00000 -1.20000 H6B 2 0.131999 0.575614 1.165422 11.00000 -1.20000 AFIX 0 N7 3 0.000000 0.000000 0.002283 10.33333 0.02258 0.02258 = 0.00960 0.00000 0.00000 0.01129 AFIX 137 H7A 2 -0.008721 -0.064230 -0.033153 10.33333 -1.50000 H7B 2 0.064230 0.055509 -0.033153 10.33333 -1.50000 H7C 2 -0.055509 0.008721 -0.033153 10.33333 -1.50000 AFIX 0 N8 3 0.269103 0.138405 0.548401 11.00000 0.01572 0.01445 = 0.02406 -0.00408 -0.00321 0.00773 AFIX 137 H8A 2 0.297122 0.211249 0.537098 11.00000 -1.50000 H8B 2 0.309680 0.117099 0.492527 11.00000 -1.50000 H8C 2 0.270150 0.122499 0.651137 11.00000 -1.50000 AFIX 0 N9 3 0.666667 0.333333 0.315095 10.33333 0.01913 0.01913 = 0.01459 0.00000 0.00000 0.00957 AFIX 137 H9A 2 0.658669 0.389280 0.279659 10.33333 -1.50000 H9B 2 0.610720 0.269389 0.279659 10.33333 -1.50000 H9C 2 0.730611 0.341331 0.279659 10.33333 -1.50000 AFIX 0 N10 3 0.530858 0.466969 0.859443 11.00000 0.02283 0.02755 = 0.01882 -0.00018 0.00475 0.01705 AFIX 137 H10A 2 0.458427 0.426036 0.839814 11.00000 -1.50000 H10B 2 0.558012 0.532061 0.809899 11.00000 -1.50000 H10C 2 0.541787 0.478111 0.964159 11.00000 -1.50000 AFIX 0 N11 3 0.333333 0.666667 0.658378 10.33333 0.01438 0.01438 = 0.01480 0.00000 0.00000 0.00719 AFIX 137 H11A 2 0.298414 0.596987 0.622942 10.33333 -1.50000 H11B 2 0.403013 0.701427 0.622942 10.33333 -1.50000 H11C 2 0.298573 0.701586 0.622942 10.33333 -1.50000 AFIX 0 N12 3 0.186618 0.397996 1.206107 11.00000 0.01577 0.01874 = 0.02381 0.00245 0.00119 0.00918 AFIX 137 H12A 2 0.203141 0.396712 1.308505 11.00000 -1.50000 H12B 2 0.204953 0.355233 1.149840 11.00000 -1.50000 H12C 2 0.114116 0.372680 1.196336 11.00000 -1.50000 AFIX 0 N13 3 0.062614 0.420589 0.592492 11.00000 0.02211 0.02750 = 0.02108 0.00094 -0.00061 0.01449 N14 3 -0.011273 0.238364 0.871052 11.00000 0.02852 0.02610 = 0.02308 -0.00369 0.00156 0.01540 N15 3 0.227171 0.230995 0.925760 11.00000 0.02489 0.03198 = 0.02476 0.00888 0.00664 0.01704 N16 3 0.405502 0.346669 1.212244 11.00000 0.05098 0.02711 = 0.02664 0.00019 0.00281 0.02731 BE1 1 0.000000 0.000000 0.210582 10.33333 0.01872 0.01872 = 0.00994 0.00000 0.00000 0.00936 BE2 1 0.132615 0.068572 0.478715 11.00000 0.01881 0.01716 = 0.01109 -0.00122 -0.00349 0.01037 BE3 1 0.666667 0.333333 0.523143 10.33333 0.02089 0.02089 = 0.01121 0.00000 0.00000 0.01044 BE4 1 0.598679 0.397269 0.789268 11.00000 0.01716 0.01929 = 0.02436 0.00012 0.00057 0.00977 BE5 1 0.333333 0.666667 0.867997 10.33333 0.01741 0.01741 = 0.01502 0.00000 0.00000 0.00871 BE6 1 0.260701 0.534504 1.134555 11.00000 0.01366 0.01860 = 0.02086 0.00289 0.00601 0.00887 HKLF 4 REM 1_b.res in P3 REM R1 = 0.0697 for 3698 Fo > 4sig(Fo) and 0.0705 for all 3765 data REM 188 parameters refined using 1 restraints END WGHT 0.1450 0.5585 REM Instructions for potential hydrogen bonds HTAB N2 Br1 HTAB N4 Br2_$1 HTAB N5 Br1 HTAB N7 N15_$2 HTAB N7 N15_$3 HTAB N7 N15_$4 HTAB N8 Br1 HTAB N8 Br2_$5 HTAB N8 N14_$6 HTAB N9 Br2_$3 HTAB N9 Br2_$5 HTAB N9 Br2_$7 HTAB N10 Br1 HTAB N10 N13_$8 HTAB N10 Br2 HTAB N11 Br1 HTAB N11 Br1_$8 HTAB N11 Br1_$9 HTAB N12 Br1_$10 HTAB N12 Br2_$9 REM Highest difference peak 1.946, deepest hole -1.089, 1-sigma level 0.275 Q1 1 0.0676 0.4120 0.5304 11.00000 0.05 1.73 Q2 1 0.2521 0.3657 0.6754 11.00000 0.05 0.84 Q3 1 0.7171 0.5567 1.3422 11.00000 0.05 0.82 Q4 1 0.6130 0.4120 0.6623 11.00000 0.05 0.82 Q5 1 0.6604 0.5337 1.1222 11.00000 0.05 0.81 Q6 1 0.6832 0.5878 1.1490 11.00000 0.05 0.80 Q7 1 0.7384 0.6309 1.1417 11.00000 0.05 0.73 Q8 1 0.2405 0.5233 1.0174 11.00000 0.05 0.72 Q9 1 0.3948 0.4354 0.5603 11.00000 0.05 0.67 Q10 1 0.5083 0.4902 0.8019 11.00000 0.05 0.65 Q11 1 0.3532 0.3805 0.6480 11.00000 0.05 0.64 Q12 1 0.0699 0.2036 1.0218 11.00000 0.05 0.64 Q13 1 0.4972 0.2286 0.4046 11.00000 0.05 0.63 Q14 1 0.2867 0.4441 0.4625 11.00000 0.05 0.62 Q15 1 0.2384 0.4238 1.2004 11.00000 0.05 0.61 Q16 1 0.7590 0.6716 1.2173 11.00000 0.05 0.60 Q17 1 0.1418 0.4143 1.1024 11.00000 0.05 0.59 Q18 1 0.2691 0.4974 1.3998 11.00000 0.05 0.59 Q19 1 0.3333 0.6667 0.7462 10.33333 0.05 0.59 Q20 1 0.2350 0.3188 0.5818 11.00000 0.05 0.58 ; _shelx_res_checksum 71720 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 Br1 Br 0.31057(8) 0.40765(7) 0.57976(9) 0.0183(3) Uani 1 1 d . . . . . Br2 Br 0.67986(8) 0.58655(8) 1.22812(7) 0.0197(3) Uani 1 1 d . . . . . N1 N 0.1307(6) 0.0683(6) 0.2785(9) 0.0172(15) Uani 1 1 d . . . . . H1A H 0.1644 0.1379 0.2428 0.021 Uiso 1 1 calc R U . . . H1B H 0.1677 0.0360 0.2417 0.021 Uiso 1 1 calc R U . . . N2 N 0.0634(6) 0.1309(6) 0.5464(9) 0.0160(14) Uani 1 1 d . . . . . H2A H 0.0974 0.2012 0.5135 0.019 Uiso 1 1 calc R U . . . H2B H 0.0634 0.1308 0.6527 0.019 Uiso 1 1 calc R U . . . N3 N 0.5973(7) 0.3956(7) 0.5893(9) 0.0172(14) Uani 1 1 d . . . . . H3A H 0.6291 0.4648 0.5521 0.021 Uiso 1 1 calc R U . . . H3B H 0.5276 0.3590 0.5542 0.021 Uiso 1 1 calc R U . . . N4 N 0.5340(6) 0.2646(6) 0.8558(10) 0.0174(14) Uani 1 1 d . . . . . H4A H 0.5326 0.2638 0.9621 0.021 Uiso 1 1 calc R U . . . H4B H 0.4643 0.2287 0.8205 0.021 Uiso 1 1 calc R U . . . N5 N 0.2574(7) 0.5356(6) 0.9338(9) 0.0171(15) Uani 1 1 d . . . . . H5A H 0.2847 0.4945 0.8949 0.021 Uiso 1 1 calc R U . . . H5B H 0.1876 0.5067 0.9004 0.021 Uiso 1 1 calc R U . . . N6 N 0.2017(6) 0.6071(6) 1.2004(9) 0.0176(15) Uani 1 1 d . . . . . H6A H 0.2003 0.6064 1.3067 0.021 Uiso 1 1 calc R U . . . H6B H 0.1320 0.5756 1.1654 0.021 Uiso 1 1 calc R U . . . N7 N 0.0000 0.0000 0.0023(14) 0.018(2) Uani 1 3 d S T P . . H7A H -0.0087 -0.0642 -0.0332 0.027 Uiso 0.3333 1 calc R U P . . H7B H 0.0642 0.0555 -0.0332 0.027 Uiso 0.3333 1 calc R U P . . H7C H -0.0555 0.0087 -0.0332 0.027 Uiso 0.3333 1 calc R U P . . N8 N 0.2691(6) 0.1384(5) 0.5484(8) 0.0180(13) Uani 1 1 d . . . . . H8A H 0.2971 0.2112 0.5371 0.027 Uiso 1 1 calc R U . . . H8B H 0.3097 0.1171 0.4925 0.027 Uiso 1 1 calc R U . . . H8C H 0.2702 0.1225 0.6511 0.027 Uiso 1 1 calc R U . . . N9 N 0.6667 0.3333 0.3151(15) 0.018(2) Uani 1 3 d S T P . . H9A H 0.6587 0.3893 0.2797 0.026 Uiso 0.3333 1 calc R U P . . H9B H 0.6107 0.2694 0.2797 0.026 Uiso 0.3333 1 calc R U P . . H9C H 0.7306 0.3413 0.2797 0.026 Uiso 0.3333 1 calc R U P . . N10 N 0.5309(6) 0.4670(6) 0.8594(9) 0.0211(14) Uani 1 1 d . . . . . H10A H 0.4584 0.4260 0.8398 0.032 Uiso 1 1 calc R U . . . H10B H 0.5580 0.5321 0.8099 0.032 Uiso 1 1 calc R U . . . H10C H 0.5418 0.4781 0.9642 0.032 Uiso 1 1 calc R U . . . N11 N 0.3333 0.6667 0.6584(14) 0.015(2) Uani 1 3 d S T P . . H11A H 0.2984 0.5970 0.6229 0.022 Uiso 0.3333 1 calc R U P . . H11B H 0.4030 0.7014 0.6229 0.022 Uiso 0.3333 1 calc R U P . . H11C H 0.2986 0.7016 0.6229 0.022 Uiso 0.3333 1 calc R U P . . N12 N 0.1866(6) 0.3980(6) 1.2061(9) 0.0192(13) Uani 1 1 d . . . . . H12A H 0.2031 0.3967 1.3085 0.029 Uiso 1 1 calc R U . . . H12B H 0.2050 0.3552 1.1498 0.029 Uiso 1 1 calc R U . . . H12C H 0.1141 0.3727 1.1963 0.029 Uiso 1 1 calc R U . . . N13 N 0.0626(9) 0.4206(7) 0.5925(14) 0.023(2) Uani 1 1 d . . . . . N14 N -0.0113(11) 0.2384(9) 0.8711(13) 0.0251(19) Uani 1 1 d . . . . . N15 N 0.2272(9) 0.2310(8) 0.9258(12) 0.0260(19) Uani 1 1 d . . . . . N16 N 0.4055(13) 0.3467(8) 1.2122(15) 0.031(2) Uani 1 1 d . . . . . Be1 Be 0.0000 0.0000 0.2106(19) 0.016(3) Uani 1 3 d S T P . . Be2 Be 0.1326(8) 0.0686(8) 0.4787(11) 0.0151(17) Uani 1 1 d . . . . . Be3 Be 0.6667 0.3333 0.523(2) 0.018(3) Uani 1 3 d S T P . . Be4 Be 0.5987(8) 0.3973(8) 0.7893(13) 0.020(2) Uani 1 1 d . . . . . Be5 Be 0.3333 0.6667 0.868(2) 0.017(3) Uani 1 3 d S T P . . Be6 Be 0.2607(8) 0.5345(8) 1.1346(12) 0.0173(18) Uani 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 Br1 0.0186(5) 0.0152(5) 0.0214(5) -0.0003(3) 0.0000(3) 0.0085(3) Br2 0.0220(5) 0.0188(5) 0.0197(5) 0.0006(3) 0.0006(3) 0.0113(4) N1 0.017(4) 0.014(3) 0.019(4) 0.002(3) 0.001(3) 0.006(3) N2 0.014(3) 0.016(3) 0.015(4) -0.002(3) 0.001(2) 0.005(3) N3 0.015(3) 0.015(3) 0.021(4) 0.004(3) 0.004(3) 0.007(3) N4 0.015(3) 0.016(3) 0.019(4) 0.006(3) 0.004(3) 0.007(3) N5 0.015(3) 0.014(3) 0.023(4) -0.002(3) 0.002(3) 0.008(3) N6 0.016(3) 0.020(4) 0.018(3) 0.003(3) 0.002(2) 0.009(3) N7 0.023(3) 0.023(3) 0.010(6) 0.000 0.000 0.0113(17) N8 0.016(3) 0.014(3) 0.024(4) -0.004(3) -0.003(3) 0.008(3) N9 0.019(3) 0.019(3) 0.015(6) 0.000 0.000 0.0096(17) N10 0.023(3) 0.028(4) 0.019(3) 0.000(3) 0.005(3) 0.017(3) N11 0.014(3) 0.014(3) 0.015(5) 0.000 0.000 0.0072(15) N12 0.016(3) 0.019(3) 0.024(3) 0.002(3) 0.001(3) 0.009(3) N13 0.022(4) 0.028(5) 0.021(5) 0.001(3) -0.001(3) 0.014(3) N14 0.029(5) 0.026(4) 0.023(5) -0.004(3) 0.002(4) 0.015(4) N15 0.025(4) 0.032(5) 0.025(5) 0.009(3) 0.007(4) 0.017(4) N16 0.051(6) 0.027(5) 0.027(5) 0.000(3) 0.003(5) 0.027(4) Be1 0.019(5) 0.019(5) 0.010(8) 0.000 0.000 0.009(2) Be2 0.019(4) 0.017(4) 0.011(4) -0.001(3) -0.003(3) 0.010(4) Be3 0.021(5) 0.021(5) 0.011(8) 0.000 0.000 0.010(2) Be4 0.017(4) 0.019(5) 0.024(5) 0.000(4) 0.001(4) 0.010(4) Be5 0.017(5) 0.017(5) 0.015(8) 0.000 0.000 0.009(2) Be6 0.014(4) 0.019(4) 0.021(5) 0.003(4) 0.006(3) 0.009(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Be Be 0.0038 0.0014 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 '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 Be2 110.6(8) . . ? Be1 N1 H1A 109.5 . . ? Be2 N1 H1A 109.5 . . ? Be1 N1 H1B 109.5 . . ? Be2 N1 H1B 109.5 . . ? H1A N1 H1B 108.1 . . ? Be2 N2 Be2 110.3(7) . 2 ? Be2 N2 H2A 109.6 . . ? Be2 N2 H2A 109.6 2 . ? Be2 N2 H2B 109.6 . . ? Be2 N2 H2B 109.6 2 . ? H2A N2 H2B 108.1 . . ? Be4 N3 Be3 109.3(8) . . ? Be4 N3 H3A 109.8 . . ? Be3 N3 H3A 109.8 . . ? Be4 N3 H3B 109.8 . . ? Be3 N3 H3B 109.8 . . ? H3A N3 H3B 108.3 . . ? Be4 N4 Be4 109.2(8) 2_655 . ? Be4 N4 H4A 109.8 2_655 . ? Be4 N4 H4A 109.8 . . ? Be4 N4 H4B 109.8 2_655 . ? Be4 N4 H4B 109.8 . . ? H4A N4 H4B 108.3 . . ? Be5 N5 Be6 109.4(8) . . ? Be5 N5 H5A 109.8 . . ? Be6 N5 H5A 109.8 . . ? Be5 N5 H5B 109.8 . . ? Be6 N5 H5B 109.8 . . ? H5A N5 H5B 108.2 . . ? Be6 N6 Be6 110.2(8) . 3_565 ? Be6 N6 H6A 109.6 . . ? Be6 N6 H6A 109.6 3_565 . ? Be6 N6 H6B 109.6 . . ? Be6 N6 H6B 109.6 3_565 . ? H6A N6 H6B 108.1 . . ? Be1 N7 H7A 109.5 . . ? Be1 N7 H7B 109.5 . . ? H7A N7 H7B 109.5 . . ? Be1 N7 H7C 109.5 . . ? H7A N7 H7C 109.5 . . ? H7B N7 H7C 109.5 . . ? Be2 N8 H8A 109.5 . . ? Be2 N8 H8B 109.5 . . ? H8A N8 H8B 109.5 . . ? Be2 N8 H8C 109.5 . . ? H8A N8 H8C 109.5 . . ? H8B N8 H8C 109.5 . . ? Be3 N9 H9A 109.5 . . ? Be3 N9 H9B 109.5 . . ? H9A N9 H9B 109.5 . . ? Be3 N9 H9C 109.5 . . ? H9A N9 H9C 109.5 . . ? H9B N9 H9C 109.5 . . ? Be4 N10 H10A 109.5 . . ? Be4 N10 H10B 109.5 . . ? H10A N10 H10B 109.5 . . ? Be4 N10 H10C 109.5 . . ? H10A N10 H10C 109.5 . . ? H10B N10 H10C 109.5 . . ? Be5 N11 H11A 109.5 . . ? Be5 N11 H11B 109.5 . . ? H11A N11 H11B 109.5 . . ? Be5 N11 H11C 109.5 . . ? H11A N11 H11C 109.5 . . ? H11B N11 H11C 109.5 . . ? Be6 N12 H12A 109.5 . . ? Be6 N12 H12B 109.5 . . ? H12A N12 H12B 109.5 . . ? Be6 N12 H12C 109.5 . . ? H12A N12 H12C 109.5 . . ? H12B N12 H12C 109.5 . . ? N1 Be1 N1 109.1(6) 3 2 ? N1 Be1 N1 109.1(6) 3 . ? N1 Be1 N1 109.1(6) 2 . ? N1 Be1 N7 109.9(6) 3 . ? N1 Be1 N7 109.9(6) 2 . ? N1 Be1 N7 109.8(6) . . ? N1 Be2 N2 109.0(6) . . ? N1 Be2 N2 109.5(6) . 3 ? N2 Be2 N2 108.3(7) . 3 ? N1 Be2 N8 110.3(6) . . ? N2 Be2 N8 110.1(6) . . ? N2 Be2 N8 109.6(6) 3 . ? N3 Be3 N3 109.7(6) . 3_665 ? N3 Be3 N3 109.7(6) . 2_655 ? N3 Be3 N3 109.7(6) 3_665 2_655 ? N3 Be3 N9 109.2(6) . . ? N3 Be3 N9 109.2(6) 3_665 . ? N3 Be3 N9 109.2(6) 2_655 . ? N3 Be4 N4 109.9(7) . 3_665 ? N3 Be4 N4 108.5(7) . . ? N4 Be4 N4 110.1(7) 3_665 . ? N3 Be4 N10 109.7(7) . . ? N4 Be4 N10 108.0(6) 3_665 . ? N4 Be4 N10 110.6(7) . . ? N5 Be5 N5 109.8(6) . 3_565 ? N5 Be5 N5 109.8(6) . 2_665 ? N5 Be5 N5 109.8(6) 3_565 2_665 ? N5 Be5 N11 109.2(6) . . ? N5 Be5 N11 109.2(6) 3_565 . ? N5 Be5 N11 109.2(6) 2_665 . ? N6 Be6 N5 107.4(7) . . ? N6 Be6 N6 109.5(8) . 2_665 ? N5 Be6 N6 110.5(6) . 2_665 ? N6 Be6 N12 109.8(6) . . ? N5 Be6 N12 110.3(7) . . ? N6 Be6 N12 109.3(7) 2_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 Be1 1.712(9) . ? N1 Be2 1.714(12) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N2 Be2 1.721(12) . ? N2 Be2 1.726(12) 2 ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N3 Be4 1.712(13) . ? N3 Be3 1.718(10) . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N4 Be4 1.722(13) 2_655 ? N4 Be4 1.730(13) . ? N4 H4A 0.9100 . ? N4 H4B 0.9100 . ? N5 Be5 1.716(10) . ? N5 Be6 1.719(13) . ? N5 H5A 0.9100 . ? N5 H5B 0.9100 . ? N6 Be6 1.718(13) . ? N6 Be6 1.725(12) 3_565 ? N6 H6A 0.9100 . ? N6 H6B 0.9100 . ? N7 Be1 1.78(2) . ? N7 H7A 0.9100 . ? N7 H7B 0.9100 . ? N7 H7C 0.9100 . ? N8 Be2 1.783(12) . ? N8 H8A 0.9100 . ? N8 H8B 0.9100 . ? N8 H8C 0.9100 . ? N9 Be3 1.78(2) . ? N9 H9A 0.9100 . ? N9 H9B 0.9100 . ? N9 H9C 0.9100 . ? N10 Be4 1.797(12) . ? N10 H10A 0.9100 . ? N10 H10B 0.9100 . ? N10 H10C 0.9100 . ? N11 Be5 1.79(2) . ? N11 H11A 0.9100 . ? N11 H11B 0.9100 . ? N11 H11C 0.9100 . ? N12 Be6 1.791(12) . ? N12 H12A 0.9100 . ? N12 H12B 0.9100 . ? N12 H12C 0.9100 . ? Be1 N1 1.712(9) 3 ? Be1 N1 1.712(9) 2 ? Be2 N2 1.726(12) 3 ? Be3 N3 1.718(10) 3_665 ? Be3 N3 1.718(10) 2_655 ? Be4 N4 1.722(13) 3_665 ? Be5 N5 1.716(10) 3_565 ? Be5 N5 1.716(10) 2_665 ? Be6 N6 1.725(12) 2_665 ? 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 N2 H2A Br1 0.91 3.04 3.753(7) 136.8 . N4 H4A Br2 0.91 3.13 3.854(8) 137.4 2_655 N5 H5A Br1 0.91 3.06 3.799(8) 139.1 . N7 H7A N15 0.91 2.44 3.323(10) 164.7 3_554 N7 H7B N15 0.91 2.44 3.323(10) 164.7 1_554 N7 H7C N15 0.91 2.44 3.323(10) 164.7 2_554 N8 H8A Br1 0.91 2.73 3.580(7) 156.6 . N8 H8B Br2 0.91 2.81 3.668(7) 157.0 2_654 N8 H8C N14 0.91 2.38 3.236(14) 156.5 3 N9 H9A Br2 0.91 2.70 3.588(3) 164.5 1_554 N9 H9B Br2 0.91 2.70 3.588(3) 164.5 2_654 N9 H9C Br2 0.91 2.70 3.588(3) 164.5 3_664 N10 H10A Br1 0.91 2.98 3.689(8) 135.8 . N10 H10B N13 0.91 2.35 3.190(14) 153.3 2_665 N10 H10C Br2 0.91 2.88 3.706(8) 151.2 . N11 H11A Br1 0.91 2.81 3.595(3) 145.7 . N11 H11B Br1 0.91 2.81 3.595(3) 145.7 2_665 N11 H11C Br1 0.91 2.81 3.595(3) 145.7 3_565 N12 H12A Br1 0.91 2.74 3.621(8) 163.2 1_556 N12 H12C Br2 0.91 2.67 3.563(7) 167.4 3_565