#------------------------------------------------------------------------------ #$Date: 2020-06-05 13:22:57 +0300 (Fri, 05 Jun 2020) $ #$Revision: 252747 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/80/1558019.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_1558019 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 'C8 H16 Be N6' _chemical_formula_weight 205.28 _space_group_crystal_system tetragonal _space_group_IT_number 94 _space_group_name_Hall 'P 4n 2n' _space_group_name_H-M_alt 'P 42 21 2' _atom_sites_solution_hydrogens mixed _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 90 _cell_formula_units_Z 2 _cell_length_a 9.9478(3) _cell_length_b 9.9478(3) _cell_length_c 5.4077(3) _cell_measurement_reflns_used 4208 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 151.23 _cell_measurement_theta_min 12.58 _cell_volume 535.14(4) _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 0.989 _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 0.0413 _diffrn_reflns_av_unetI/netI 0.0231 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_number 3136 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 75.716 _diffrn_reflns_theta_min 6.292 _diffrn_source 'GeniX 3D HF Cu' _exptl_absorpt_coefficient_mu 0.667 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.274 _exptl_crystal_description block _exptl_crystal_F_000 220 _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.148 _refine_diff_density_min -0.147 _refine_diff_density_rms 0.039 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.2(11) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 42 _refine_ls_number_reflns 555 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.083 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0369 _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^)+(0.0651P)^2^+0.0470P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0954 _refine_ls_wR_factor_ref 0.0996 _reflns_Friedel_coverage 0.552 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.995 _reflns_number_gt 484 _reflns_number_total 555 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc01112f2.cif _cod_data_source_block 4 _cod_depositor_comments 'Adding full bibliography for 1558013--1558021.cif.' _cod_database_code 1558019 _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 ; 4.res created by SHELXL-2014/7 TITL 1_a.res in P4(2)2(1)2 REM Old TITL 1 in P4(2)2(1)2 REM SHELXT solution in P4(2)2(1)2 REM R1 0.101, Rweak 0.011, Alpha 0.002, Orientation as input REM Flack x = 0.406 ( 0.972 ) from Parsons' quotients REM Formula found by SHELXT: C8 Be N6 CELL 1.54178 9.9478 9.9478 5.4077 90.000 90.000 90.000 ZERR 2.000 0.0003 0.0003 0.0003 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, Z SYMM 1/2-Y, 1/2+X, 1/2+Z SYMM 1/2+Y, 1/2-X, 1/2+Z SYMM 1/2-X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, 1/2-Z SYMM Y, X, -Z SYMM -Y, -X, -Z SFAC C H BE N UNIT 16 32 2 12 L.S. 10 BOND $H LIST 4 ACTA TEMP -173.15 FMAP 2 PLAN 20 REM EXTI 0.000000 TWIN HTAB WGHT 0.065100 0.047000 BASF 0.19878 FVAR 2.03515 N1 4 0.358585 0.515315 0.329207 11.00000 0.02348 0.02299 = 0.01927 -0.00119 -0.00030 -0.00149 H1 2 0.336494 0.454976 0.215490 11.00000 0.03079 BE1 3 0.500000 0.500000 0.500000 10.25000 0.02084 0.02084 = 0.01971 0.00000 0.00000 0.00027 C1 1 0.272805 0.614127 0.341450 11.00000 0.02006 0.02270 = 0.01915 0.00583 0.00422 -0.00383 N2 4 0.280014 0.719986 0.500000 10.50000 0.02157 0.02157 = 0.02456 0.00320 0.00320 0.00111 C2 1 0.153524 0.615766 0.170325 11.00000 0.02146 0.02973 = 0.02874 0.00389 -0.00051 -0.00039 AFIX 137 H2A 2 0.085784 0.678390 0.233904 11.00000 -1.50000 H2B 2 0.114879 0.525311 0.160312 11.00000 -1.50000 H2C 2 0.182230 0.644663 0.005317 11.00000 -1.50000 REM ##### AFIX 0 HKLF 4 REM 1_a.res in P4(2)2(1)2 REM R1 = 0.0369 for 484 Fo > 4sig(Fo) and 0.0443 for all 555 data REM 42 parameters refined using 0 restraints END WGHT 0.0651 0.0470 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.148, deepest hole -0.147, 1-sigma level 0.039 Q1 1 0.2974 0.5512 0.4156 11.00000 0.05 0.15 Q2 1 0.4245 0.4997 0.4252 11.00000 0.05 0.14 Q3 1 0.3084 0.7091 0.5561 11.00000 0.05 0.14 Q4 1 0.1012 0.7076 0.1303 11.00000 0.05 0.13 Q5 1 0.1745 0.6912 0.5734 11.00000 0.05 0.13 Q6 1 0.2085 0.7780 0.5548 11.00000 0.05 0.12 Q7 1 0.2055 0.6166 0.2545 11.00000 0.05 0.11 Q8 1 0.0773 0.6323 0.2524 11.00000 0.05 0.10 Q9 1 0.1380 0.5164 0.0424 11.00000 0.05 0.10 Q10 1 0.1581 0.7473 -0.0295 11.00000 0.05 0.10 Q11 1 0.4479 0.5521 0.0000 10.50000 0.05 0.10 Q12 1 0.2243 0.3599 0.1545 11.00000 0.05 0.09 Q13 1 0.3453 0.5841 0.2561 11.00000 0.05 0.09 Q14 1 0.0358 0.7317 0.3739 11.00000 0.05 0.09 Q15 1 0.2866 0.4184 -0.0067 11.00000 0.05 0.09 Q16 1 0.2030 0.5866 0.0260 11.00000 0.05 0.09 Q17 1 0.2976 0.3165 0.3070 11.00000 0.05 0.09 Q18 1 0.3527 0.3603 0.0935 11.00000 0.05 0.08 Q19 1 0.1310 0.7967 0.0816 11.00000 0.05 0.07 Q20 1 0.3576 0.7767 0.5115 11.00000 0.05 0.07 ; _shelx_res_checksum 5535 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y, x, -z' '-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 0.35858(15) 0.51531(17) 0.3292(3) 0.0219(5) Uani 1 1 d . . . . . H1 H 0.336(3) 0.455(3) 0.215(5) 0.031(7) Uiso 1 1 d . . . . . Be1 Be 0.5000 0.5000 0.5000 0.0205(10) Uani 1 4 d S T P . . C1 C 0.27281(19) 0.61413(18) 0.3414(4) 0.0206(5) Uani 1 1 d . . . . . N2 N 0.28001(16) 0.71999(16) 0.5000 0.0226(6) Uani 1 2 d S T P . . C2 C 0.1535(2) 0.6158(2) 0.1703(5) 0.0266(5) Uani 1 1 d . . . . . H2A H 0.0858 0.6784 0.2339 0.040 Uiso 1 1 calc R U . . . H2B H 0.1149 0.5253 0.1603 0.040 Uiso 1 1 calc R U . . . H2C H 0.1822 0.6447 0.0053 0.040 Uiso 1 1 calc R U . . . 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 0.0235(9) 0.0230(9) 0.0193(9) -0.0012(8) -0.0003(8) -0.0015(6) Be1 0.0208(14) 0.0208(14) 0.020(2) 0.000 0.000 0.0003(19) C1 0.0201(9) 0.0227(9) 0.0191(9) 0.0058(8) 0.0042(9) -0.0038(7) N2 0.0216(7) 0.0216(7) 0.0246(12) 0.0032(7) 0.0032(7) 0.0011(9) C2 0.0215(10) 0.0297(10) 0.0287(11) 0.0039(11) -0.0005(11) -0.0004(8) 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 C1 N1 Be1 125.82(15) . . ? C1 N1 H1 112.5(17) . . ? Be1 N1 H1 121.6(17) . . ? N1 Be1 N1 98.55(12) . 8_666 ? N1 Be1 N1 113.73(12) . 2_665 ? N1 Be1 N1 116.67(11) 8_666 2_665 ? N1 Be1 N1 116.67(11) . 7_556 ? N1 Be1 N1 113.73(12) 8_666 7_556 ? N1 Be1 N1 98.55(12) 2_665 7_556 ? N1 C1 N2 125.56(19) . . ? N1 C1 C2 119.55(19) . . ? N2 C1 C2 114.89(18) . . ? C1 N2 C1 118.6(2) 8_666 . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? 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 C1 1.303(2) . ? N1 Be1 1.6897(17) . ? N1 H1 0.89(3) . ? Be1 N1 1.6898(17) 8_666 ? Be1 N1 1.6898(17) 2_665 ? Be1 N1 1.6898(17) 7_556 ? C1 N2 1.360(2) . ? C1 C2 1.505(3) . ? N2 C1 1.360(2) 8_666 ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ?