#------------------------------------------------------------------------------ #$Date: 2020-06-05 13:22:57 +0300 (Fri, 05 Jun 2020) $ #$Revision: 252747 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/80/1558013.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_1558013 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_paper_doi 10.1039/D0SC01112F _journal_volume 11 _journal_year 2020 _chemical_formula_sum 'Be4 H51 I2 N19' _chemical_formula_weight 607.43 _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 1 _cell_length_a 9.77560(10) _cell_length_b 9.77560(10) _cell_length_c 8.7186(2) _cell_measurement_reflns_used 9830 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 154.18 _cell_measurement_theta_min 10.15 _cell_volume 721.55(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 1.000 _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 0.0166 _diffrn_reflns_av_unetI/netI 0.0155 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 4283 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.982 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 75.826 _diffrn_reflns_theta_min 5.073 _diffrn_source 'GeniX 3D HF Cu' _exptl_absorpt_coefficient_mu 17.294 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.398 _exptl_crystal_description block _exptl_crystal_F_000 306 _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_transmission_factor_max 0.1060 _exptl_transmission_factor_min 0.0301 _refine_diff_density_max 0.972 _refine_diff_density_min -0.830 _refine_diff_density_rms 0.182 _refine_ls_abs_structure_details ; Flack x determined using 751 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.413(17) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.164 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 79 _refine_ls_number_reflns 1779 _refine_ls_number_restraints 13 _refine_ls_restrained_S_all 1.160 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0447 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.003 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0903P)^2^+2.1179P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1274 _refine_ls_wR_factor_ref 0.1277 _reflns_Friedel_coverage 0.964 _reflns_Friedel_fraction_full 0.981 _reflns_Friedel_fraction_max 0.964 _reflns_number_gt 1767 _reflns_number_total 1779 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc01112f2.cif _cod_data_source_block 5 _cod_depositor_comments 'Adding full bibliography for 1558013--1558021.cif.' _cod_database_code 1558013 _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 P3 REM SHELXT solution in P3 REM R1 0.175, Rweak 0.041, Alpha 0.021, Orientation as input REM Flack x = 0.488 ( 0.019 ) from Parsons' quotients REM Formula found by SHELXT: N15 I CELL 1.54178 9.7756 9.7756 8.7186 90.000 90.000 120.000 ZERR 1.000 0.0001 0.0001 0.0002 0.000 0.000 0.000 LATT -1 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SFAC BE H N I UNIT 4 51 19 2 L.S. 7 BOND $H LIST 4 TWIN -1 0 0 0 -1 0 0 0 1 ACTA TEMP -173.15 FMAP 2 PLAN 50 ISOR 0.01 $Be rem EXTI 0.001024 WGHT 0.090300 2.117900 BASF 0.19745 FVAR 0.61958 I1 4 0.333333 0.666667 0.190970 10.33333 0.02895 0.02895 = 0.02036 0.00000 0.00000 0.01448 I2 4 0.000000 0.000000 0.840220 10.33333 0.01733 0.01733 = 0.02492 0.00000 0.00000 0.00866 N1 3 0.843890 0.478288 1.140337 11.00000 0.04026 0.01471 = 0.03791 -0.01356 -0.01558 0.00817 AFIX 23 H1A 2 0.863481 0.574530 1.174060 11.00000 -1.20000 H1B 2 0.923560 0.463733 1.174837 11.00000 -1.20000 AFIX 0 N2 3 0.816478 0.300990 0.879106 11.00000 0.03062 0.01445 = 0.01715 0.00020 -0.00971 0.01223 AFIX 23 H2A 2 0.895982 0.283126 0.906689 11.00000 -1.20000 H2B 2 0.811789 0.302426 0.774917 11.00000 -1.20000 AFIX 0 N3 3 0.666667 0.333333 1.427909 10.33333 0.03190 0.03190 = 0.01843 0.00000 0.00000 0.01595 AFIX 137 H3A 2 0.565642 0.275872 1.462700 10.33333 -1.50000 H3B 2 0.710230 0.434358 1.462701 10.33333 -1.50000 H3C 2 0.724128 0.289771 1.462700 10.33333 -1.50000 AFIX 0 N4 3 1.037821 0.629282 0.883783 11.00000 0.03150 0.03876 = 0.03017 0.00253 -0.00188 0.01673 AFIX 137 H4A 2 1.037019 0.720882 0.867885 11.00000 -1.50000 H4B 2 1.057987 0.595719 0.793696 11.00000 -1.50000 H4C 2 1.114192 0.646115 0.953219 11.00000 -1.50000 AFIX 0 N5 3 0.529388 0.547543 0.511307 11.00000 0.05924 0.05265 = 0.02866 -0.00110 0.00527 0.04091 N7 3 0.942557 0.770683 1.459988 11.00000 0.04510 0.04713 = 0.05020 -0.00957 -0.00444 0.02653 N6 3 0.786982 0.811934 1.228462 11.00000 0.03977 0.05130 = 0.04903 -0.00833 -0.00330 0.01461 BE1 1 0.847715 0.480616 0.956356 11.00000 0.03027 0.03600 = 0.01504 -0.00171 0.00205 0.01520 BE2 1 0.666667 0.333333 1.222065 10.33333 0.02670 0.02670 = 0.01197 0.00000 0.00000 0.01335 HKLF 4 REM 1_b.res in P3 REM R1 = 0.0447 for 1767 Fo > 4sig(Fo) and 0.0450 for all 1779 data REM 79 parameters refined using 13 restraints END WGHT 0.0932 2.1175 REM Highest difference peak 0.972, deepest hole -0.830, 1-sigma level 0.182 Q1 1 1.2952 0.8184 0.8878 11.00000 0.05 0.97 Q2 1 0.9661 0.8174 1.5473 11.00000 0.05 0.91 Q3 1 0.6227 0.4838 0.5566 11.00000 0.05 0.90 Q4 1 0.9021 0.6817 1.5356 11.00000 0.05 0.89 Q5 1 0.5174 0.6243 0.5873 11.00000 0.05 0.88 Q6 1 0.8040 0.9556 1.1461 11.00000 0.05 0.80 Q7 1 0.3063 0.7300 0.1934 11.00000 0.05 0.74 Q8 1 0.6067 0.6310 0.5518 11.00000 0.05 0.72 Q9 1 0.4748 0.6256 0.4845 11.00000 0.05 0.71 Q10 1 0.6900 0.1770 0.8075 11.00000 0.05 0.71 Q11 1 0.0284 0.0733 0.8470 11.00000 0.05 0.70 Q12 1 1.1452 0.6341 1.1418 11.00000 0.05 0.69 Q13 1 1.1409 0.6968 0.8026 11.00000 0.05 0.69 Q14 1 0.7338 0.6952 1.1406 11.00000 0.05 0.67 Q15 1 0.9715 0.1572 0.8898 11.00000 0.05 0.61 Q16 1 0.7162 0.1817 1.4758 11.00000 0.05 0.60 Q17 1 0.8454 0.3563 1.2166 11.00000 0.05 0.58 Q18 1 1.0449 0.7481 1.5428 11.00000 0.05 0.52 Q19 1 0.5511 0.7316 0.5794 11.00000 0.05 0.48 Q20 1 0.8123 0.6848 1.1588 11.00000 0.05 0.47 Q21 1 1.0232 0.5495 1.1777 11.00000 0.05 0.47 Q22 1 0.6667 0.3333 0.8099 10.33333 0.05 0.45 Q23 1 0.0000 0.0000 0.6281 10.33333 0.05 0.42 Q24 1 1.1201 0.8070 1.5948 11.00000 0.05 0.40 Q25 1 0.6771 0.7643 1.1466 11.00000 0.05 0.40 Q26 1 0.9029 0.5348 1.0602 11.00000 0.05 0.40 Q27 1 0.6667 0.3333 1.6081 10.33333 0.05 0.39 Q28 1 0.6167 0.7221 0.5113 11.00000 0.05 0.39 Q29 1 0.7364 0.7196 1.3207 11.00000 0.05 0.38 Q30 1 0.8892 0.1967 0.8479 11.00000 0.05 0.38 Q31 1 0.4987 0.7430 0.4891 11.00000 0.05 0.37 Q32 1 0.3333 0.6667 0.3866 10.33333 0.05 0.36 Q33 1 0.8629 0.8221 1.1060 11.00000 0.05 0.36 Q34 1 1.0582 0.6594 0.6980 11.00000 0.05 0.35 Q35 1 0.0000 0.0000 1.0455 10.33333 0.05 0.34 Q36 1 0.9494 0.6124 0.9176 11.00000 0.05 0.34 Q37 1 0.3333 0.6667 0.5065 10.33333 0.05 0.33 Q38 1 1.1069 0.7590 1.1255 11.00000 0.05 0.33 Q39 1 0.6667 0.3333 1.1243 10.33333 0.05 0.33 Q40 1 1.0000 1.0000 1.5283 10.33333 0.05 0.33 Q41 1 0.7669 0.9140 1.2458 11.00000 0.05 0.32 Q42 1 0.7651 0.5042 1.0713 11.00000 0.05 0.32 Q43 1 0.7638 0.3958 1.5248 11.00000 0.05 0.31 Q44 1 0.8085 0.2911 1.0545 11.00000 0.05 0.31 Q45 1 0.7424 0.2342 0.9404 11.00000 0.05 0.30 Q46 1 0.8680 0.4294 1.0695 11.00000 0.05 0.29 Q47 1 0.0388 0.0771 0.9942 11.00000 0.05 0.29 Q48 1 0.9179 0.6948 1.2347 11.00000 0.05 0.28 Q49 1 0.9345 0.3620 0.7290 11.00000 0.05 0.28 Q50 1 0.6658 0.7901 1.0355 11.00000 0.05 0.28 ; _shelx_res_checksum 29904 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 I1 I 0.3333 0.6667 0.19097(19) 0.0261(7) Uani 1 3 d S T P . . I2 I 0.0000 0.0000 0.84022(10) 0.0199(5) Uani 1 3 d S T P . . N1 N 0.844(3) 0.478(2) 1.140(2) 0.033(5) Uani 1 1 d . . . . . H1A H 0.8635 0.5745 1.1741 0.040 Uiso 1 1 calc R U . . . H1B H 0.9236 0.4637 1.1748 0.040 Uiso 1 1 calc R U . . . N2 N 0.816(2) 0.3010(19) 0.8791(19) 0.020(3) Uani 1 1 d . . . . . H2A H 0.8960 0.2831 0.9067 0.024 Uiso 1 1 calc R U . . . H2B H 0.8118 0.3024 0.7749 0.024 Uiso 1 1 calc R U . . . N3 N 0.6667 0.3333 1.428(2) 0.027(4) Uani 1 3 d S T P . . H3A H 0.5656 0.2759 1.4627 0.041 Uiso 0.3333 1 calc R U P . . H3B H 0.7102 0.4344 1.4627 0.041 Uiso 0.3333 1 calc R U P . . H3C H 0.7241 0.2898 1.4627 0.041 Uiso 0.3333 1 calc R U P . . N4 N 1.0378(16) 0.6293(17) 0.8838(16) 0.034(3) Uani 1 1 d . . . . . H4A H 1.0370 0.7209 0.8679 0.051 Uiso 1 1 calc R U . . . H4B H 1.0580 0.5957 0.7937 0.051 Uiso 1 1 calc R U . . . H4C H 1.1142 0.6461 0.9532 0.051 Uiso 1 1 calc R U . . . N5 N 0.529(2) 0.5475(19) 0.5113(19) 0.041(3) Uani 1 1 d . . . . . N7 N 0.943(2) 0.771(2) 1.460(2) 0.046(4) Uani 1 1 d . . . . . N6 N 0.787(2) 0.812(2) 1.228(2) 0.050(4) Uani 1 1 d . . . . . Be1 Be 0.848(2) 0.481(2) 0.956(2) 0.028(4) Uani 1 1 d . U . . . Be2 Be 0.6667 0.3333 1.222(3) 0.022(6) Uani 1 3 d S TU P . . 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 I1 0.0290(11) 0.0290(11) 0.0204(11) 0.000 0.000 0.0145(5) I2 0.0173(6) 0.0173(6) 0.0249(11) 0.000 0.000 0.0087(3) N1 0.040(11) 0.015(8) 0.038(10) -0.014(7) -0.016(8) 0.008(7) N2 0.031(9) 0.014(7) 0.017(7) 0.000(5) -0.010(6) 0.012(6) N3 0.032(7) 0.032(7) 0.018(11) 0.000 0.000 0.016(3) N4 0.031(6) 0.039(7) 0.030(6) 0.003(5) -0.002(5) 0.017(6) N5 0.059(10) 0.053(9) 0.029(7) -0.001(6) 0.005(7) 0.041(8) N7 0.045(9) 0.047(10) 0.050(9) -0.010(8) -0.004(7) 0.027(8) N6 0.040(8) 0.051(10) 0.049(10) -0.008(8) -0.003(7) 0.015(7) Be1 0.030(8) 0.036(8) 0.015(6) -0.002(6) 0.002(6) 0.015(6) Be2 0.027(7) 0.027(7) 0.012(10) 0.000 0.000 0.013(3) 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' I I -0.3257 6.8362 '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 115.2(16) . . ? Be1 N1 H1A 108.5 . . ? Be2 N1 H1A 108.5 . . ? Be1 N1 H1B 108.5 . . ? Be2 N1 H1B 108.5 . . ? H1A N1 H1B 107.5 . . ? Be1 N2 Be1 105.7(16) . 3_665 ? Be1 N2 H2A 110.6 . . ? Be1 N2 H2A 110.6 3_665 . ? Be1 N2 H2B 110.6 . . ? Be1 N2 H2B 110.6 3_665 . ? H2A N2 H2B 108.7 . . ? Be2 N3 H3A 109.5 . . ? Be2 N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? Be2 N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? Be1 N4 H4A 109.5 . . ? Be1 N4 H4B 109.5 . . ? H4A N4 H4B 109.5 . . ? Be1 N4 H4C 109.5 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? N1 Be1 N2 112.2(14) . . ? N1 Be1 N2 111.4(14) . 2_655 ? N2 Be1 N2 107.2(15) . 2_655 ? N1 Be1 N4 111.6(14) . . ? N2 Be1 N4 105.3(12) . . ? N2 Be1 N4 108.8(13) 2_655 . ? N1 Be2 N1 104.6(12) 3_665 . ? N1 Be2 N1 104.6(12) 3_665 2_655 ? N1 Be2 N1 104.6(12) . 2_655 ? N1 Be2 N3 114.0(10) 3_665 . ? N1 Be2 N3 114.0(10) . . ? N1 Be2 N3 114.0(10) 2_655 . ? 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 1.60(3) . ? N1 Be2 1.75(2) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N2 Be1 1.76(3) . ? N2 Be1 1.78(3) 3_665 ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N3 Be2 1.79(3) . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N3 H3C 0.9100 . ? N4 Be1 1.81(2) . ? N4 H4A 0.9100 . ? N4 H4B 0.9100 . ? N4 H4C 0.9100 . ? Be1 N2 1.78(3) 2_655 ? Be2 N1 1.75(2) 3_665 ? Be2 N1 1.75(2) 2_655 ?