#------------------------------------------------------------------------------ #$Date: 2020-05-06 02:26:44 +0300 (Wed, 06 May 2020) $ #$Revision: 251788 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/80/1558016.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_1558016 loop_ _publ_author_name 'M\"uller, Matthias' 'Karttunen, Antti J.' 'Buchner, Magnus Richard' _publ_section_title ; Speciation of Be2+ in acidic liquid ammonia and formation of tetra- and octanuclear beryllium amido clusters ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D0SC01112F _journal_year 2020 _chemical_formula_sum 'Be4 Cl2 H36 N14' _chemical_formula_weight 339.37 _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 difmap _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 13.93420(10) _cell_length_b 13.93420(10) _cell_length_c 8.37270(10) _cell_measurement_reflns_used 25538 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 150.10 _cell_measurement_theta_min 7.04 _cell_volume 1407.86(2) _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 1.000 _diffrn_measured_fraction_theta_max 0.998 _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 0.0198 _diffrn_reflns_av_unetI/netI 0.0173 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 19167 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 78.738 _diffrn_reflns_theta_min 3.663 _diffrn_source 'GeniX 3D HF Cu' _exptl_absorpt_coefficient_mu 3.195 _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 1.201 _exptl_crystal_description block _exptl_crystal_F_000 552 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max 0.3535 _exptl_transmission_factor_min 0.0892 _refine_diff_density_max 0.178 _refine_diff_density_min -0.120 _refine_diff_density_rms 0.032 _refine_ls_abs_structure_details ; Flack x determined using 1127 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.126(8) _refine_ls_extinction_coef 0.00106(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 327 _refine_ls_number_reflns 3314 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.028 _refine_ls_R_factor_all 0.0189 _refine_ls_R_factor_gt 0.0175 _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^)+(0.0258P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0395 _reflns_Friedel_coverage 0.993 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.991 _reflns_number_gt 3183 _reflns_number_total 3314 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc01112f2.cif _cod_data_source_block 11 _cod_original_cell_volume 1407.86(3) _cod_original_formula_sum 'Be4 H36 Cl2 N14' _cod_database_code 1558016 _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 ; 11.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 0.071, Rweak 0.022, Alpha 0.013, Orientation as input REM Flack x = 0.182 ( 0.008 ) from Parsons' quotients REM Formula found by SHELXT: Be2 N7 Cl CELL 1.54178 13.9342 13.9342 8.3727 90.000 90.000 120.000 ZERR 3.000 0.0001 0.0001 0.0001 0.000 0.000 0.000 LATT -1 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SFAC BE H N CL UNIT 12 108 42 6 L.S. 10 BOND $H LIST 4 ACTA TEMP -173.15 TWIN 0 1 0 1 0 0 0 0 -1 FMAP 2 PLAN 40 HTAB EQIV $1 -x+y+1, -x+1, z HTAB N3 Cl2_$1 EQIV $2 x, y, z+1 HTAB N6 Cl1_$2 HTAB N7 Cl1_$2 HTAB N5 Cl2_$1 EQIV $3 x, y+1, z HTAB N9 Cl2_$3 HTAB N8 N16 HTAB N8 N15 EQIV $4 -y, x-y, z HTAB N8 Cl2_$4 EQIV $5 -y+1, x-y, z+1 HTAB N11 N13_$5 EQIV $6 -x+y+1, -x+1, z-1 HTAB N10 Cl2_$6 HTAB N10 Cl1 HTAB N10 N13_$1 HTAB N12 N14 HTAB N12 Cl2 HTAB N12 Cl1_$2 EQIV $7 -x+y, -x, z HTAB N13 N16_$7 HTAB N13 Cl2 HTAB N13 N14 HTAB N14 N15 HTAB N14 Cl1 HTAB N15 Cl1_$2 HTAB N15 Cl2_$1 HTAB N15 Cl2_$4 EQIV $8 -y, x-y, z-1 HTAB N16 Cl2_$8 HTAB N16 Cl1 HTAB N16 Cl1_$4 WGHT 0.025800 EXTI 0.001059 BASF 0.03669 FVAR 0.41533 CL1 4 0.254215 0.233664 -0.122490 11.00000 0.01542 0.01511 = 0.01785 -0.00010 -0.00157 0.00581 CL2 4 0.358518 -0.076443 0.540949 11.00000 0.01619 0.01339 = 0.01643 -0.00047 -0.00020 0.00770 N1 3 0.057518 0.133115 0.527026 11.00000 0.01442 0.01308 = 0.01397 -0.00094 -0.00135 0.00735 N2 3 0.134121 0.074253 0.255761 11.00000 0.01416 0.01699 = 0.01250 0.00213 0.00181 0.00685 N3 3 0.386815 0.586725 0.186386 11.00000 0.01433 0.01292 = 0.01238 0.00106 -0.00043 0.00780 N4 3 0.255957 0.533040 -0.085548 11.00000 0.01238 0.01172 = 0.01288 -0.00081 -0.00090 0.00518 N5 3 0.594623 0.394581 0.568027 11.00000 0.01376 0.01483 = 0.01437 0.00046 0.00045 0.00847 N6 3 0.532919 0.259755 0.842004 11.00000 0.01191 0.01337 = 0.01427 0.00195 0.00212 0.00639 N7 3 0.000000 0.000000 0.809290 10.33333 0.01408 0.01408 = 0.01332 0.00000 0.00000 0.00704 N8 3 0.123571 0.274295 0.253287 11.00000 0.02807 0.01509 = 0.01998 0.00234 -0.00411 0.00695 N9 3 0.333333 0.666667 0.468647 10.33333 0.01313 0.01313 = 0.01250 0.00000 0.00000 0.00656 N10 3 0.449438 0.509618 -0.094278 11.00000 0.01562 0.01484 = 0.01480 -0.00077 -0.00025 0.00852 N11 3 0.666667 0.333333 1.123879 10.33333 0.01778 0.01778 = 0.01442 0.00000 0.00000 0.00889 N12 3 0.392088 0.184839 0.567634 11.00000 0.01309 0.01374 = 0.01698 -0.00011 -0.00016 0.00646 N13 3 0.439139 0.091882 0.187456 11.00000 0.01974 0.02321 = 0.02160 0.00550 0.00394 0.01071 N14 3 0.408130 0.312792 0.235455 11.00000 0.02062 0.02083 = 0.02067 0.00110 -0.00134 0.01046 N15 3 0.308395 0.395699 0.521845 11.00000 0.01989 0.01733 = 0.01948 0.00074 -0.00230 0.00812 N16 3 0.022290 0.275361 -0.101835 11.00000 0.02313 0.01914 = 0.02055 -0.00196 0.00059 0.00598 BE1 1 0.000000 0.000000 0.595018 10.33333 0.01356 0.01356 = 0.01155 0.00000 0.00000 0.00678 BE2 1 0.059386 0.133667 0.322823 11.00000 0.01588 0.01274 = 0.01439 0.00150 -0.00055 0.00603 BE3 1 0.333333 0.666667 0.253256 10.33333 0.01241 0.01241 = 0.01110 0.00000 0.00000 0.00621 BE4 1 0.389210 0.589191 -0.018740 11.00000 0.01393 0.01283 = 0.01322 -0.00112 0.00034 0.00799 BE5 1 0.532611 0.260902 0.636912 11.00000 0.01123 0.01358 = 0.01524 -0.00066 -0.00139 0.00620 BE6 1 0.666667 0.333333 0.908634 10.33333 0.01395 0.01395 = 0.01390 0.00000 0.00000 0.00698 H1A 2 0.022386 0.161605 0.564742 11.00000 0.02897 H1B 2 0.122946 0.173957 0.570839 11.00000 0.02903 H2A 2 0.141193 0.076230 0.162369 11.00000 0.03920 H2B 2 0.199920 0.110225 0.281945 11.00000 0.03412 H3A 2 0.343712 0.516467 0.223784 11.00000 0.02910 H3B 2 0.452033 0.608973 0.233949 11.00000 0.02066 H4A 2 0.255120 0.531427 -0.188113 11.00000 0.02861 H4B 2 0.218687 0.467995 -0.055042 11.00000 0.02349 H6A 2 0.504774 0.192101 0.876164 11.00000 0.03234 H6B 2 0.487196 0.281955 0.876739 11.00000 0.03186 H7 2 0.061582 0.056750 0.849644 11.00000 0.02543 H5A 2 0.558892 0.429026 0.589035 11.00000 0.02538 H5B 2 0.591924 0.392472 0.471670 11.00000 0.02637 H9 2 0.338430 0.729708 0.506499 11.00000 0.01947 H8A 2 0.115609 0.280157 0.164628 11.00000 0.08185 H8B 2 0.189689 0.310275 0.284130 11.00000 0.04990 H8C 2 0.093953 0.313265 0.299504 11.00000 0.06965 H11 2 0.732496 0.342979 1.157461 11.00000 0.03944 H10A 2 0.477245 0.534661 -0.190718 11.00000 0.03669 H10B 2 0.396156 0.435606 -0.102912 11.00000 0.03237 H10C 2 0.501990 0.512821 -0.038378 11.00000 0.02348 H12A 2 0.387186 0.209770 0.467394 11.00000 0.03669 H12B 2 0.374009 0.116686 0.561968 11.00000 0.03429 H12C 2 0.348928 0.195254 0.636899 11.00000 0.02572 H13A 2 0.387104 0.053620 0.123690 11.00000 0.03872 H13B 2 0.426295 0.055549 0.268480 11.00000 0.02841 H13C 2 0.424781 0.150018 0.212577 11.00000 0.03396 H14A 2 0.463528 0.361782 0.210414 11.00000 0.01557 H14B 2 0.372908 0.333472 0.306696 11.00000 0.03957 H14C 2 0.361570 0.291011 0.138360 11.00000 0.03569 H15A 2 0.304979 0.355416 0.588647 11.00000 0.04243 H15B 2 0.373633 0.462927 0.518528 11.00000 0.03975 H15C 2 0.249882 0.409877 0.528558 11.00000 0.03535 H16A 2 0.025798 0.311620 -0.199005 11.00000 0.02887 H16B 2 0.066943 0.255738 -0.117680 11.00000 0.04023 H16C 2 -0.040199 0.216298 -0.117200 11.00000 0.02224 HKLF 4 REM 1_b.res in P3 REM R1 = 0.0175 for 3183 Fo > 4sig(Fo) and 0.0189 for all 3314 data REM 327 parameters refined using 1 restraints END WGHT 0.0258 0.0000 REM Instructions for potential hydrogen bonds HTAB N3 Cl2_$1 HTAB N6 Cl1_$2 HTAB N7 Cl1_$2 HTAB N5 Cl2_$1 HTAB N9 Cl2_$3 HTAB N8 N16 HTAB N8 N15 HTAB N8 Cl2_$4 HTAB N11 N13_$5 HTAB N10 Cl2_$6 HTAB N10 Cl1 HTAB N10 N13_$1 HTAB N12 N14 HTAB N12 Cl2 HTAB N12 Cl1_$2 HTAB N13 N16_$7 HTAB N13 Cl2 HTAB N13 N14 HTAB N14 N15 HTAB N14 Cl1 HTAB N15 Cl1_$2 HTAB N15 Cl2_$1 HTAB N15 Cl2_$4 HTAB N16 Cl2_$8 HTAB N16 Cl1 HTAB N16 Cl1_$4 REM Highest difference peak 0.178, deepest hole -0.120, 1-sigma level 0.032 Q1 1 0.3787 0.5854 0.0991 11.00000 0.05 0.18 Q2 1 0.5282 0.2598 0.7471 11.00000 0.05 0.16 Q3 1 0.3162 0.5636 -0.0411 11.00000 0.05 0.16 Q4 1 0.0999 0.0118 0.2935 11.00000 0.05 0.15 Q5 1 0.0402 0.1189 0.4351 11.00000 0.05 0.15 Q6 1 0.5953 0.2999 0.8641 11.00000 0.05 0.15 Q7 1 0.5710 0.2310 0.6119 11.00000 0.05 0.15 Q8 1 0.1851 0.2165 -0.1659 11.00000 0.05 0.14 Q9 1 0.0909 0.0888 0.2843 11.00000 0.05 0.14 Q10 1 0.3619 -0.1359 0.4952 11.00000 0.05 0.14 Q11 1 0.2293 0.5694 -0.0508 11.00000 0.05 0.14 Q12 1 0.2997 -0.0944 0.5001 11.00000 0.05 0.13 Q13 1 0.3569 -0.0230 0.5798 11.00000 0.05 0.13 Q14 1 0.0000 0.0000 0.7237 10.33333 0.05 0.13 Q15 1 0.2532 0.2405 0.0059 11.00000 0.05 0.13 Q16 1 0.3061 0.3593 0.4439 11.00000 0.05 0.12 Q17 1 0.6667 0.3333 1.0281 10.33333 0.05 0.12 Q18 1 0.2421 0.2841 -0.0924 11.00000 0.05 0.12 Q19 1 0.2906 0.3017 -0.1983 11.00000 0.05 0.12 Q20 1 0.5718 0.3431 0.6240 11.00000 0.05 0.12 Q21 1 0.4431 0.2797 0.2884 11.00000 0.05 0.12 Q22 1 0.3530 0.6202 0.2198 11.00000 0.05 0.12 Q23 1 0.2961 -0.1424 0.5671 11.00000 0.05 0.11 Q24 1 0.0249 0.0653 0.5513 11.00000 0.05 0.11 Q25 1 0.0056 0.3087 -0.0216 11.00000 0.05 0.11 Q26 1 0.3536 -0.1028 0.6538 11.00000 0.05 0.10 Q27 1 0.4547 0.2154 0.6119 11.00000 0.05 0.10 Q28 1 0.3595 -0.0652 0.6821 11.00000 0.05 0.10 Q29 1 0.4901 0.0785 0.1400 11.00000 0.05 0.10 Q30 1 0.1830 0.1809 -0.1001 11.00000 0.05 0.10 Q31 1 0.3333 0.6667 0.3811 10.33333 0.05 0.10 Q32 1 0.2703 0.2439 -0.2569 11.00000 0.05 0.10 Q33 1 0.5021 0.1327 0.1513 11.00000 0.05 0.10 Q34 1 0.4742 0.6221 0.3806 11.00000 0.05 0.09 Q35 1 0.4195 -0.0810 0.5846 11.00000 0.05 0.09 Q36 1 0.1663 0.2809 0.1329 11.00000 0.05 0.09 Q37 1 0.3773 -0.0637 0.4146 11.00000 0.05 0.09 Q38 1 0.1561 0.4676 -0.2975 11.00000 0.05 0.08 Q39 1 0.4262 0.5468 -0.0619 11.00000 0.05 0.08 Q40 1 0.4162 -0.0153 0.5021 11.00000 0.05 0.08 ; _shelx_res_checksum 11863 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 Cl1 Cl 0.25422(4) 0.23366(4) -0.12249(4) 0.01694(12) Uani 1 1 d . . . . . Cl2 Cl 0.35852(4) -0.07644(4) 0.54095(4) 0.01520(11) Uani 1 1 d . . . . . N1 N 0.05752(16) 0.13311(16) 0.5270(2) 0.0136(3) Uani 1 1 d . . . . . N2 N 0.13412(17) 0.07425(16) 0.2558(2) 0.0150(3) Uani 1 1 d . . . . . N3 N 0.38682(15) 0.58672(15) 0.1864(2) 0.0128(3) Uani 1 1 d . . . . . N4 N 0.25596(15) 0.53304(16) -0.0855(2) 0.0127(3) Uani 1 1 d . . . . . N5 N 0.59462(16) 0.39458(17) 0.5680(2) 0.0137(4) Uani 1 1 d . . . . . N6 N 0.53292(18) 0.25976(17) 0.8420(2) 0.0132(4) Uani 1 1 d . . . . . N7 N 0.0000 0.0000 0.8093(3) 0.0138(5) Uani 1 3 d S T P . . N8 N 0.12357(16) 0.27429(13) 0.2533(2) 0.0227(3) Uani 1 1 d . . . . . N9 N 0.3333 0.6667 0.4686(3) 0.0129(4) Uani 1 3 d S T P . . N10 N 0.44944(12) 0.50962(12) -0.09428(18) 0.0147(3) Uani 1 1 d . . . . . N11 N 0.6667 0.3333 1.1239(3) 0.0167(5) Uani 1 3 d S T P . . N12 N 0.39209(12) 0.18484(12) 0.56763(18) 0.0147(3) Uani 1 1 d . . . . . N13 N 0.43914(18) 0.0919(2) 0.1875(3) 0.0215(4) Uani 1 1 d . . . . . N14 N 0.4081(2) 0.3128(2) 0.2355(3) 0.0207(4) Uani 1 1 d . . . . . N15 N 0.30839(18) 0.3957(2) 0.5218(3) 0.0194(5) Uani 1 1 d . . . . . N16 N 0.0223(2) 0.2754(2) -0.1018(3) 0.0230(5) Uani 1 1 d . . . . . Be1 Be 0.0000 0.0000 0.5950(4) 0.0129(6) Uani 1 3 d S T P . . Be2 Be 0.05939(18) 0.13367(18) 0.3228(3) 0.0148(4) Uani 1 1 d . . . . . Be3 Be 0.3333 0.6667 0.2533(4) 0.0120(6) Uani 1 3 d S T P . . Be4 Be 0.38921(17) 0.58919(16) -0.0187(3) 0.0128(4) Uani 1 1 d . . . . . Be5 Be 0.53261(17) 0.26090(16) 0.6369(3) 0.0134(4) Uani 1 1 d . . . . . Be6 Be 0.6667 0.3333 0.9086(4) 0.0139(6) Uani 1 3 d S T P . . H1A H 0.022(2) 0.162(2) 0.565(3) 0.029(7) Uiso 1 1 d . . . . . H1B H 0.123(2) 0.174(2) 0.571(3) 0.029(7) Uiso 1 1 d . . . . . H2A H 0.141(3) 0.076(3) 0.162(4) 0.039(9) Uiso 1 1 d . . . . . H2B H 0.200(2) 0.110(2) 0.282(3) 0.034(7) Uiso 1 1 d . . . . . H3A H 0.344(2) 0.516(2) 0.224(3) 0.029(6) Uiso 1 1 d . . . . . H3B H 0.452(2) 0.609(2) 0.234(3) 0.021(6) Uiso 1 1 d . . . . . H4A H 0.255(2) 0.531(2) -0.188(3) 0.029(7) Uiso 1 1 d . . . . . H4B H 0.2187(19) 0.468(2) -0.055(3) 0.023(6) Uiso 1 1 d . . . . . H6A H 0.505(2) 0.192(2) 0.876(3) 0.032(7) Uiso 1 1 d . . . . . H6B H 0.487(2) 0.282(2) 0.877(3) 0.032(7) Uiso 1 1 d . . . . . H7 H 0.062(2) 0.057(2) 0.850(3) 0.025(7) Uiso 1 1 d . . . . . H5A H 0.559(2) 0.429(2) 0.589(3) 0.025(6) Uiso 1 1 d . . . . . H5B H 0.592(2) 0.392(2) 0.472(3) 0.026(6) Uiso 1 1 d . . . . . H9 H 0.338(2) 0.7297(19) 0.506(3) 0.019(6) Uiso 1 1 d . . . . . H8A H 0.116(3) 0.280(4) 0.165(5) 0.082(13) Uiso 1 1 d . . . . . H8B H 0.190(3) 0.310(3) 0.284(4) 0.050(9) Uiso 1 1 d . . . . . H8C H 0.094(3) 0.313(3) 0.300(4) 0.070(10) Uiso 1 1 d . . . . . H11 H 0.7325(19) 0.343(3) 1.157(3) 0.039(7) Uiso 1 1 d . . . . . H10A H 0.477(2) 0.535(2) -0.191(3) 0.037(7) Uiso 1 1 d . . . . . H10B H 0.396(2) 0.436(2) -0.103(3) 0.032(6) Uiso 1 1 d . . . . . H10C H 0.502(2) 0.513(2) -0.038(3) 0.023(6) Uiso 1 1 d . . . . . H12A H 0.387(2) 0.210(2) 0.467(3) 0.037(7) Uiso 1 1 d . . . . . H12B H 0.374(2) 0.117(2) 0.562(3) 0.034(7) Uiso 1 1 d . . . . . H12C H 0.349(2) 0.1953(19) 0.637(3) 0.026(6) Uiso 1 1 d . . . . . H13A H 0.387(3) 0.054(3) 0.124(4) 0.039(9) Uiso 1 1 d . . . . . H13B H 0.426(2) 0.056(3) 0.268(4) 0.028(7) Uiso 1 1 d . . . . . H13C H 0.425(2) 0.150(3) 0.213(3) 0.034(9) Uiso 1 1 d . . . . . H14A H 0.464(2) 0.362(2) 0.210(3) 0.016(7) Uiso 1 1 d . . . . . H14B H 0.373(3) 0.333(3) 0.307(4) 0.040(9) Uiso 1 1 d . . . . . H14C H 0.362(2) 0.291(2) 0.138(4) 0.036(8) Uiso 1 1 d . . . . . H15A H 0.305(3) 0.355(3) 0.589(4) 0.042(10) Uiso 1 1 d . . . . . H15B H 0.374(3) 0.463(3) 0.519(4) 0.040(10) Uiso 1 1 d . . . . . H15C H 0.250(3) 0.410(3) 0.529(4) 0.035(9) Uiso 1 1 d . . . . . H16A H 0.026(2) 0.312(2) -0.199(3) 0.029(8) Uiso 1 1 d . . . . . H16B H 0.067(3) 0.256(3) -0.118(4) 0.040(10) Uiso 1 1 d . . . . . H16C H -0.040(3) 0.216(3) -0.117(4) 0.022(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 Cl1 0.0154(2) 0.0151(2) 0.0178(3) -0.00010(17) -0.00157(18) 0.00581(18) Cl2 0.0162(2) 0.0134(2) 0.0164(3) -0.00047(16) -0.00020(17) 0.00770(18) N1 0.0144(7) 0.0131(7) 0.0140(7) -0.0009(6) -0.0014(6) 0.0074(6) N2 0.0142(7) 0.0170(8) 0.0125(7) 0.0021(6) 0.0018(6) 0.0069(6) N3 0.0143(8) 0.0129(8) 0.0124(8) 0.0011(6) -0.0004(6) 0.0078(6) N4 0.0124(7) 0.0117(7) 0.0129(7) -0.0008(5) -0.0009(6) 0.0052(6) N5 0.0138(9) 0.0148(9) 0.0144(10) 0.0005(6) 0.0005(7) 0.0085(8) N6 0.0119(8) 0.0134(9) 0.0143(9) 0.0020(6) 0.0021(6) 0.0064(7) N7 0.0141(7) 0.0141(7) 0.0133(12) 0.000 0.000 0.0070(3) N8 0.0281(9) 0.0151(7) 0.0200(8) 0.0023(6) -0.0041(7) 0.0070(7) N9 0.0131(7) 0.0131(7) 0.0125(11) 0.000 0.000 0.0066(3) N10 0.0156(7) 0.0148(7) 0.0148(6) -0.0008(5) -0.0002(6) 0.0085(6) N11 0.0178(7) 0.0178(7) 0.0144(13) 0.000 0.000 0.0089(4) N12 0.0131(7) 0.0137(7) 0.0170(7) -0.0001(5) -0.0002(5) 0.0065(6) N13 0.0197(9) 0.0232(10) 0.0216(10) 0.0055(8) 0.0039(7) 0.0107(8) N14 0.0206(10) 0.0208(10) 0.0207(10) 0.0011(7) -0.0013(7) 0.0105(8) N15 0.0199(11) 0.0173(10) 0.0195(11) 0.0007(8) -0.0023(7) 0.0081(8) N16 0.0231(12) 0.0191(10) 0.0205(12) -0.0020(8) 0.0006(8) 0.0060(9) Be1 0.0136(9) 0.0136(9) 0.0115(15) 0.000 0.000 0.0068(5) Be2 0.0159(9) 0.0127(9) 0.0144(9) 0.0015(7) -0.0005(7) 0.0060(8) Be3 0.0124(9) 0.0124(9) 0.0111(15) 0.000 0.000 0.0062(5) Be4 0.0139(9) 0.0128(9) 0.0132(9) -0.0011(7) 0.0003(7) 0.0080(7) Be5 0.0112(8) 0.0136(9) 0.0152(9) -0.0007(7) -0.0014(7) 0.0062(8) Be6 0.0140(9) 0.0140(9) 0.0139(16) 0.000 0.000 0.0070(5) 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' Cl Cl 0.3639 0.7018 '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 109.62(17) . . ? Be1 N1 H1A 108.9(17) . . ? Be2 N1 H1A 112.9(17) . . ? Be1 N1 H1B 109.6(17) . . ? Be2 N1 H1B 114.0(18) . . ? H1A N1 H1B 102(2) . . ? Be2 N2 Be2 109.55(17) 3 . ? Be2 N2 H2A 110(2) 3 . ? Be2 N2 H2A 114(2) . . ? Be2 N2 H2B 111.3(18) 3 . ? Be2 N2 H2B 112.2(18) . . ? H2A N2 H2B 99(3) . . ? Be3 N3 Be4 108.90(16) . . ? Be3 N3 H3A 108.6(15) . . ? Be4 N3 H3A 111.2(15) . . ? Be3 N3 H3B 109.0(16) . . ? Be4 N3 H3B 115.6(17) . . ? H3A N3 H3B 103(2) . . ? Be4 N4 Be4 109.71(16) . 3_565 ? Be4 N4 H4A 109.7(18) . . ? Be4 N4 H4A 109.8(18) 3_565 . ? Be4 N4 H4B 110.1(17) . . ? Be4 N4 H4B 110.9(16) 3_565 . ? H4A N4 H4B 107(2) . . ? Be5 N5 Be5 109.75(17) . 3_665 ? Be5 N5 H5A 114.7(16) . . ? Be5 N5 H5A 111.1(16) 3_665 . ? Be5 N5 H5B 107.9(18) . . ? Be5 N5 H5B 112.0(17) 3_665 . ? H5A N5 H5B 101(2) . . ? Be6 N6 Be5 109.13(18) . . ? Be6 N6 H6A 108.0(17) . . ? Be5 N6 H6A 109.7(16) . . ? Be6 N6 H6B 116.3(17) . . ? Be5 N6 H6B 108.6(16) . . ? H6A N6 H6B 105(2) . . ? Be1 N7 H7 112.2(15) . . ? Be2 N8 H8A 114(3) . . ? Be2 N8 H8B 111(2) . . ? H8A N8 H8B 114(4) . . ? Be2 N8 H8C 113(2) . . ? H8A N8 H8C 102(4) . . ? H8B N8 H8C 102(3) . . ? Be3 N9 H9 110.6(14) . . ? Be4 N10 H10A 108.8(18) . . ? Be4 N10 H10B 110.6(15) . . ? H10A N10 H10B 108(2) . . ? Be4 N10 H10C 115.3(17) . . ? H10A N10 H10C 107(2) . . ? H10B N10 H10C 107(2) . . ? Be6 N11 H11 108.1(15) . . ? Be5 N12 H12A 109.6(17) . . ? Be5 N12 H12B 107.6(17) . . ? H12A N12 H12B 109(2) . . ? Be5 N12 H12C 108.5(16) . . ? H12A N12 H12C 110(2) . . ? H12B N12 H12C 112(2) . . ? H13A N13 H13B 106(3) . . ? H13A N13 H13C 101(3) . . ? H13B N13 H13C 106(3) . . ? H14A N14 H14B 111(3) . . ? H14A N14 H14C 105(3) . . ? H14B N14 H14C 105(3) . . ? H15A N15 H15B 115(3) . . ? H15A N15 H15C 111(3) . . ? H15B N15 H15C 108(3) . . ? H16A N16 H16B 101(3) . . ? H16A N16 H16C 98(3) . . ? H16B N16 H16C 104(3) . . ? N1 Be1 N1 109.48(12) . 2 ? N1 Be1 N1 109.48(12) . 3 ? N1 Be1 N1 109.48(12) 2 3 ? N1 Be1 N7 109.46(12) . . ? N1 Be1 N7 109.46(12) 2 . ? N1 Be1 N7 109.46(12) 3 . ? N1 Be2 N2 108.42(15) . 2 ? N1 Be2 N2 109.66(14) . . ? N2 Be2 N2 110.08(18) 2 . ? N1 Be2 N8 109.10(14) . . ? N2 Be2 N8 110.37(14) 2 . ? N2 Be2 N8 109.20(14) . . ? N3 Be3 N3 109.88(12) . 3_565 ? N3 Be3 N3 109.88(12) . 2_665 ? N3 Be3 N3 109.88(12) 3_565 2_665 ? N3 Be3 N9 109.06(12) . . ? N3 Be3 N9 109.06(12) 3_565 . ? N3 Be3 N9 109.06(12) 2_665 . ? N4 Be4 N4 110.02(17) . 2_665 ? N4 Be4 N3 108.20(14) . . ? N4 Be4 N3 110.08(14) 2_665 . ? N4 Be4 N10 109.65(13) . . ? N4 Be4 N10 108.53(13) 2_665 . ? N3 Be4 N10 110.37(13) . . ? N5 Be5 N5 108.82(18) . 2_655 ? N5 Be5 N6 110.14(14) . . ? N5 Be5 N6 109.08(14) 2_655 . ? N5 Be5 N12 109.96(13) . . ? N5 Be5 N12 109.87(14) 2_655 . ? N6 Be5 N12 108.96(14) . . ? N6 Be6 N6 109.90(13) 2_655 3_665 ? N6 Be6 N6 109.90(13) 2_655 . ? N6 Be6 N6 109.90(13) 3_665 . ? N6 Be6 N11 109.04(13) 2_655 . ? N6 Be6 N11 109.04(13) 3_665 . ? N6 Be6 N11 109.04(13) . . ? 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 1.709(2) . ? N1 Be2 1.710(3) . ? N1 H1A 0.83(3) . ? N1 H1B 0.88(3) . ? N2 Be2 1.710(3) 3 ? N2 Be2 1.717(3) . ? N2 H2A 0.79(3) . ? N2 H2B 0.82(3) . ? N3 Be3 1.715(2) . ? N3 Be4 1.718(3) . ? N3 H3A 0.91(3) . ? N3 H3B 0.89(3) . ? N4 Be4 1.709(3) . ? N4 Be4 1.715(3) 3_565 ? N4 H4A 0.86(3) . ? N4 H4B 0.83(2) . ? N5 Be5 1.714(3) . ? N5 Be5 1.715(3) 3_665 ? N5 H5A 0.86(3) . ? N5 H5B 0.81(3) . ? N6 Be6 1.710(2) . ? N6 Be5 1.717(3) . ? N6 H6A 0.87(3) . ? N6 H6B 0.89(3) . ? N7 Be1 1.794(4) . ? N7 H7 0.89(2) . ? N8 Be2 1.796(3) . ? N8 H8A 0.76(4) . ? N8 H8B 0.84(4) . ? N8 H8C 0.92(4) . ? N9 Be3 1.803(4) . ? N9 H9 0.90(2) . ? N10 Be4 1.807(2) . ? N10 H10A 0.89(3) . ? N10 H10B 0.92(2) . ? N10 H10C 0.85(3) . ? N11 Be6 1.802(4) . ? N11 H11 0.90(2) . ? N12 Be5 1.794(3) . ? N12 H12A 0.92(3) . ? N12 H12B 0.85(3) . ? N12 H12C 0.90(3) . ? N13 H13A 0.84(3) . ? N13 H13B 0.81(3) . ? N13 H13C 0.95(3) . ? N14 H14A 0.76(3) . ? N14 H14B 0.91(3) . ? N14 H14C 0.99(3) . ? N15 H15A 0.78(4) . ? N15 H15B 0.92(4) . ? N15 H15C 0.93(3) . ? N16 H16A 0.95(3) . ? N16 H16B 0.81(4) . ? N16 H16C 0.86(3) . ? Be1 N1 1.709(2) 2 ? Be1 N1 1.709(2) 3 ? Be2 N2 1.710(3) 2 ? Be3 N3 1.715(2) 3_565 ? Be3 N3 1.715(2) 2_665 ? Be4 N4 1.715(3) 2_665 ? Be5 N5 1.715(3) 2_655 ? Be6 N6 1.710(2) 2_655 ? Be6 N6 1.710(2) 3_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 N3 H3B Cl2 0.89(3) 2.93(3) 3.6970(18) 145(2) 3_665 N6 H6B Cl1 0.89(3) 2.97(3) 3.727(2) 145(2) 1_556 N7 H7 Cl1 0.89(2) 2.59(2) 3.4557(7) 163(2) 1_556 N5 H5A Cl2 0.86(3) 2.95(2) 3.671(2) 143(2) 3_665 N9 H9 Cl2 0.90(2) 2.59(2) 3.4708(7) 165.8(19) 1_565 N8 H8A N16 0.76(4) 2.57(4) 3.294(3) 161(4) . N8 H8B N15 0.84(4) 2.48(3) 3.193(3) 143(3) . N8 H8C Cl2 0.92(4) 2.73(4) 3.5657(19) 153(3) 2 N11 H11 N13 0.90(2) 2.43(2) 3.315(2) 166(2) 2_656 N10 H10A Cl2 0.89(3) 2.63(3) 3.5127(16) 170(2) 3_664 N10 H10B Cl1 0.92(2) 2.51(3) 3.4324(16) 179(2) . N10 H10C N13 0.85(3) 2.65(3) 3.475(3) 163(2) 3_665 N12 H12A N14 0.92(3) 2.34(3) 3.250(3) 167(2) . N12 H12B Cl2 0.85(3) 2.60(3) 3.4381(15) 169(2) . N12 H12C Cl1 0.90(3) 2.61(3) 3.4917(15) 169(2) 1_556 N13 H13A N16 0.84(3) 2.49(4) 3.316(4) 167(3) 3 N13 H13B Cl2 0.81(3) 2.78(3) 3.590(2) 174(3) . N13 H13C N14 0.95(3) 2.40(3) 3.340(4) 170(2) . N14 H14B N15 0.91(3) 2.36(3) 3.259(3) 170(3) . N14 H14C Cl1 0.99(3) 2.54(3) 3.526(2) 175(2) . N15 H15A Cl1 0.78(4) 2.83(3) 3.582(3) 163(3) 1_556 N15 H15B Cl2 0.92(4) 2.59(4) 3.507(2) 172(3) 3_665 N15 H15C Cl2 0.93(3) 2.61(3) 3.541(2) 176(3) 2 N16 H16A Cl2 0.95(3) 2.64(3) 3.575(3) 169(2) 2_554 N16 H16B Cl1 0.81(4) 2.78(4) 3.562(3) 165(3) . N16 H16C Cl1 0.86(3) 2.71(3) 3.563(2) 172(3) 2