#------------------------------------------------------------------------------ #$Date: 2022-11-10 02:38:44 +0000 (Thu, 10 Nov 2022) $ #$Revision: 279168 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/90/2109079.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2109079 loop_ _publ_author_name 'Bujak, Maciej' 'Olejniczak, Anna' 'Podsiad\/lo, Marcin' _publ_section_title ; Evolution of intermolecular contacts with temperature and pressure in bromoethane and iodoethane -- a comparative study ; _journal_coeditor_code AW5073 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first ; ; _journal_paper_doi 10.1107/S2052520622010149 _journal_volume 78 _journal_year 2022 _chemical_formula_moiety 'C2 H5 Br' _chemical_formula_sum 'C2 H5 Br' _chemical_formula_weight 108.96 _chemical_name_systematic bromoethane _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 100.379(8) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.5087(4) _cell_length_b 9.8814(8) _cell_length_c 6.9315(6) _cell_measurement_reflns_used 2450 _cell_measurement_temperature 100.0(1) _cell_measurement_theta_max 30.55 _cell_measurement_theta_min 3.63 _cell_volume 371.13(5) _computing_cell_refinement 'CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)' _computing_molecular_graphics 'Mercury (Macrae at al., 2020)' _computing_publication_material 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXS-2013/1 (Sheldrick, 2013)' _diffrn_ambient_temperature 100.0(1) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'KUMA KM4-CCD, Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_unetI/netI 0.0277 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 5716 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.492 _diffrn_reflns_theta_min 3.631 _exptl_absorpt_coefficient_mu 10.806 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.054 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.950 _exptl_crystal_description irregular _exptl_crystal_F_000 208 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.703 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.095 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 29 _refine_ls_number_reflns 850 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.082 _refine_ls_R_factor_all 0.0252 _refine_ls_R_factor_gt 0.0211 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0195P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.0484 _reflns_Friedel_coverage 0.000 _reflns_number_gt 770 _reflns_number_total 850 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file aw5073sup1.cif _cod_data_source_block MBE_100K _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2109079 _publcif_datablock.id {be0415f6-7ab7-42a7-9df3-75ce0baafac1} _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_estimated_absorpt_t_min 0.411 _shelx_estimated_absorpt_t_max 0.411 _shelx_res_file ; TITL MBE_100K in P2(1)/n mbe_100k.res created by SHELXL-2018/3 at 17:46:57 on 11-Oct-2021 REM P2(1)/n (#14 in standard setting) CELL 0.71073 5.508735 9.881412 6.931473 90.0000 100.3787 90.0000 ZERR 4.00 0.000422 0.000830 0.000591 0.0000 0.0082 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H Br UNIT 8.00 20.00 4.00 L.S. 50 BOND $H FMAP 2 PLAN 100 OMIT 0 55 ACTA SIZE 0.1 0.1 0.1 HTAB WGHT 0.019500 FVAR 9.45464 BR1 3 0.224799 0.941845 0.810281 11.00000 0.01560 0.02502 = 0.03239 -0.00231 0.00546 -0.00434 C1 1 -0.100361 0.862723 0.709403 11.00000 0.01421 0.02601 = 0.03067 0.00235 0.00006 -0.00139 AFIX 23 H11 2 -0.226595 0.931305 0.708255 11.00000 -1.20000 H12 2 -0.105678 0.832564 0.575534 11.00000 -1.20000 AFIX 0 C2 1 -0.153416 0.745969 0.831836 11.00000 0.01892 0.01893 = 0.03403 0.00027 -0.00069 -0.00146 AFIX 137 H21 2 -0.311771 0.708441 0.777618 11.00000 -1.50000 H22 2 -0.154132 0.776292 0.963312 11.00000 -1.50000 H23 2 -0.028481 0.678048 0.833356 11.00000 -1.50000 AFIX 0 HKLF 4 REM MBE_100K in P2(1)/n REM wR2 = 0.0484, GooF = S = 1.082, Restrained GooF = 1.082 for all data REM R1 = 0.0211 for 770 Fo > 4sig(Fo) and 0.0252 for all 850 data REM 29 parameters refined using 0 restraints END WGHT 0.0195 0.0000 REM Instructions for potential hydrogen bonds HTAB C2 Br1_$13 REM Highest difference peak 0.703, deepest hole -0.544, 1-sigma level 0.095 Q1 1 0.2439 0.9409 0.9431 11.00000 0.05 0.70 Q2 1 0.2026 0.9451 0.6786 11.00000 0.05 0.45 Q3 1 0.1112 1.0225 0.9139 11.00000 0.05 0.29 Q4 1 -0.2723 0.9729 0.7884 11.00000 0.05 0.28 Q5 1 0.2049 1.0850 0.7404 11.00000 0.05 0.27 Q6 1 -0.1740 0.9390 0.6267 11.00000 0.05 0.26 Q7 1 0.1551 1.0528 0.7352 11.00000 0.05 0.26 Q8 1 0.2609 0.7328 0.7795 11.00000 0.05 0.26 Q9 1 -0.0077 0.9139 1.0626 11.00000 0.05 0.26 Q10 1 0.2387 1.0195 1.0421 11.00000 0.05 0.26 Q11 1 0.1472 0.8180 0.7868 11.00000 0.05 0.24 Q12 1 -0.2632 1.0619 0.4798 11.00000 0.05 0.24 Q13 1 0.3278 0.8770 0.8102 11.00000 0.05 0.24 Q14 1 -0.0071 0.7835 0.5416 11.00000 0.05 0.24 Q15 1 0.2723 0.7971 0.8980 11.00000 0.05 0.23 Q16 1 0.3466 0.8467 0.8517 11.00000 0.05 0.23 Q17 1 -0.0320 0.8058 1.0601 11.00000 0.05 0.22 Q18 1 -0.1759 0.9512 0.7132 11.00000 0.05 0.22 Q19 1 0.0028 0.9728 0.9744 11.00000 0.05 0.22 Q20 1 -0.0029 0.9562 0.8604 11.00000 0.05 0.22 ... ; _shelx_res_checksum 98719 _shelx_hkl_file ; 0 0 -2 949487. 7200.77 1 0 0 2 944453. 6950.48 1 0 0 3 384.288 176.051 1 0 0 -3 372.034 156.716 1 0 0 -4 3764.13 936.058 2 0 0 -4 4083.08 920.410 13 0 0 4 4698.96 951.822 12 0 0 5 5299.70 1722.58 5 0 0 -5 1485.01 1341.89 13 0 0 -5 636.330 1612.97 2 0 0 -6 115481. 6304.33 13 0 0 6 97939.1 5997.38 5 0 0 -6 119985. 6793.30 2 0 0 -7-80.4658 376.676 2 0 0 -7-987.648 673.824 13 0 0 7 482.249 215.037 10 0 0 7-853.601 732.615 5 0 0 -8 81485.6 6495.21 13 0 0 8 77869.8 7018.58 10 0 0 8 71290.3 6456.54 5 0 0 8 75357.2 6413.29 14 0 0 9 1813.03 1336.10 14 0 0 -9-578.028 684.573 13 0 0 9 748.046 1201.88 10 0 1 1 133331. 2660.68 1 0 -1 1 129935. 2628.86 1 0 -1 -2 119662. 2885.09 1 0 -1 2 125147. 3155.83 1 0 1 2 124008. 2969.37 1 0 1 3 448200. 8842.94 10 0 1 3 449068. 6448.83 1 0 -1 3 430304. 6463.80 1 0 -1 -3 450533. 8277.34 13 0 -1 -3 440191. 6417.54 1 0 -1 3 446924. 6186.53 1 0 -1 -4 93920.6 4514.27 2 0 -1 -4 86323.0 4303.07 13 0 -1 -4 88340.0 4302.70 15 0 1 4 76389.1 3906.20 5 0 1 -4 86802.8 4699.46 9 0 1 -4 83931.1 4598.81 2 0 1 4 80659.0 4447.46 10 0 1 -4 82814.8 4206.30 13 0 -1 4 78343.2 4339.23 5 0 -1 4 82569.9 4321.85 12 0 1 -5 232976. 8876.12 9 0 1 -5 226260. 8646.76 2 0 -1 5 230442. 8194.51 12 0 -1 -5 233926. 7892.03 15 0 -1 -5 222176. 7825.98 13 0 1 5 217714. 7613.62 12 0 1 5 212172. 7644.46 5 0 -1 5 217107. 8343.60 5 0 1 5 228753. 8631.99 10 0 -1 -5 234691. 8126.24 2 0 1 -5 228047. 7947.67 13 0 1 -6 11535.2 2173.34 2 0 -1 6 9370.94 1928.53 5 0 1 6 9503.72 1929.61 10 0 -1 -6 8881.26 1662.28 13 0 1 6 9606.22 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-1 29260.4 4674.22 17 7 3 1 36088.3 6043.60 11 -7 3 -1 42762.5 6683.18 7 -7 -3 -1 37180.3 6295.43 7 -7 -3 -2 5055.35 2456.60 7 -7 3 -2 2781.75 1208.67 17 7 -3 2 1963.11 1961.91 6 -7 -3 -2 2059.25 1147.33 17 7 3 2 3719.80 1481.57 11 7 -4 -5 4575.65 3200.95 13 7 -4 -5-3516.18 3900.39 6 -7 -4 5-2547.19 1794.29 16 7 4 -5-172.983 1828.12 6 7 -4 -4 67162.6 12421.8 6 7 4 -4 44522.4 6390.69 6 -7 4 4 43586.1 6508.16 16 -7 -4 4 51949.9 6339.93 16 7 -4 -4 68468.0 15109.3 13 -7 -4 4 56042.3 6864.95 7 -7 -4 3 972.708 1235.02 7 7 -4 -3 1903.77 1995.97 6 -7 4 3 3401.40 1817.49 16 7 4 -3-988.697 1153.20 6 7 4 -3 3757.07 2532.70 8 -7 4 2 5229.09 2451.55 7 -7 -4 2 4064.75 2233.59 7 7 -4 -2 7263.29 3091.56 6 -7 4 2 3975.91 1285.16 16 7 4 -2 10923.8 4485.20 8 -7 4 1-70.3701 487.644 7 -7 -4 1 1715.88 1177.98 7 7 -4 -1 1080.83 462.106 6 7 4 -1 1956.18 2124.23 11 7 4 -1 3658.53 3128.35 8 -7 4 0 20665.5 4355.81 7 -7 -4 0 18436.6 4211.58 7 -7 4 0 16743.8 3611.31 17 7 -4 0 23650.7 5141.45 6 7 4 0 23018.0 4836.81 11 -7 -4 0 21810.8 5101.83 14 -7 -4 -1 2617.54 1966.51 7 -7 4 -1 2105.41 1886.68 17 7 -4 1 1913.75 797.332 6 7 4 1-166.984 1406.51 11 -7 -4 -2 60218.6 8782.03 7 7 -5 -4 3506.03 2912.48 6 -7 -5 4 3843.07 1566.83 16 7 5 -4 1481.40 1013.16 6 -7 5 3 36305.8 6073.22 16 7 -5 -3 51345.2 10031.5 6 -7 -5 3 35187.2 5655.04 7 -7 -5 2 5997.86 2257.84 7 7 -5 -2 7350.15 3202.02 6 -7 5 2 10775.8 3535.26 16 7 5 -2 14864.0 4526.08 8 -7 -5 1 56805.3 7292.23 7 7 -5 -1 78043.0 10263.0 6 -7 5 1 63745.9 8094.56 16 -7 -5 1 68025.2 8603.94 14 7 5 -1 71551.4 9598.28 8 -7 5 0 4352.88 2723.30 7 -7 -5 0-12.5639 1009.06 7 -7 5 0 2774.41 1655.62 17 7 -5 0 1721.21 917.499 6 7 5 0 1543.80 1048.82 11 -7 -5 0-700.644 2115.03 14 -7 -5 -1 22464.1 4838.29 7 -7 5 -1 20397.4 4262.61 17 7 5 1 20232.8 4309.88 11 -7 -6 3 2098.21 1881.92 7 7 -6 -3 3395.38 2626.36 6 7 -6 -3 7225.13 4663.54 15 -7 -6 3 6197.25 2730.63 14 -7 -6 2 3773.84 1551.00 7 7 -6 -2 4332.64 3103.96 6 -7 6 2 941.204 1039.28 16 7 -6 -2 2969.60 2882.08 15 -7 -6 2 3217.83 2166.38 14 7 6 -2 10092.3 3965.70 8 -7 -6 1 4576.05 2730.80 7 7 -6 -1 4115.32 1956.28 6 -7 6 1 6666.27 2926.87 16 -7 -6 1 1983.89 2102.94 14 7 6 -1 487.475 1475.15 8 -7 6 0 6594.78 2769.75 7 -7 6 0 8071.50 2680.08 17 7 6 0 10720.7 3027.47 11 -7 -6 0 12717.6 4373.62 14 7 -7 -2 53674.5 10026.7 6 8 0 -2 37025.6 8654.66 8 0 0 0 0.00 0.00 0 TITL MBE_100K in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 0.71073 5.508735 9.881412 6.931473 90.0000 100.3787 90.0000 ZERR 8.00 0.000422 0.000830 0.000591 0.0000 0.0082 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H Br UNIT 16.00 40.00 8.00 TREF HKLF 4 END ; _shelx_hkl_checksum 83073 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 0.22480(4) 0.94184(2) 0.81028(4) 0.02419(11) Uani 1 1 d . . . . . C1 C -0.1004(5) 0.8627(3) 0.7094(4) 0.0241(5) Uani 1 1 d . . . . . H11 H -0.226595 0.931305 0.708255 0.029 Uiso 1 1 calc R U . . . H12 H -0.105678 0.832564 0.575534 0.029 Uiso 1 1 calc R U . . . C2 C -0.1534(5) 0.7460(3) 0.8318(4) 0.0246(5) Uani 1 1 d . . . . . H21 H -0.311771 0.708441 0.777618 0.037 Uiso 1 1 calc R U . . . H22 H -0.154132 0.776292 0.963312 0.037 Uiso 1 1 calc R U . . . H23 H -0.028481 0.678048 0.833356 0.037 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 Br1 0.01560(16) 0.02502(16) 0.03239(16) -0.00231(9) 0.00546(11) -0.00434(10) C1 0.0142(12) 0.0260(14) 0.0307(13) 0.0023(10) 0.0001(10) -0.0014(11) C2 0.0189(12) 0.0189(12) 0.0340(13) 0.0003(10) -0.0007(10) -0.0015(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' Br Br -0.2901 2.4595 '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 C2 C1 Br1 111.40(17) . . ? C2 C1 H11 109.3 . . ? Br1 C1 H11 109.3 . . ? C2 C1 H12 109.3 . . ? Br1 C1 H12 109.3 . . ? H11 C1 H12 108.0 . . ? C1 C2 H21 109.5 . . ? C1 C2 H22 109.5 . . ? H21 C2 H22 109.5 . . ? C1 C2 H23 109.5 . . ? H21 C2 H23 109.5 . . ? H22 C2 H23 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 Br1 C1 1.964(3) . ? C1 C2 1.492(3) . ? C1 H11 0.9700 . ? C1 H12 0.9700 . ? C2 H21 0.9600 . ? C2 H22 0.9600 . ? C2 H23 0.9600 . ? _cod_database_fobs_code 2109079