#------------------------------------------------------------------------------ #$Date: 2022-10-29 14:07:13 +0200 (Sat, 29 Oct 2022) $ #$Revision: 278875 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/26/2022690.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_2022690 loop_ _publ_author_name 'Allen, Caleb J.' 'Olden, Alex M.' 'Yates, James L.' 'Wheeler, Kraig A.' 'Abbey, Eric R.' _publ_section_title ; Synthesis, crystal structure and Hirshfeld analysis of triphenylphosphine--(4-bromophenyl)borane ; _journal_coeditor_code ZO3028 _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229622010002 _journal_volume 78 _journal_year 2022 _chemical_formula_iupac 'C24 H21 B Br P' _chemical_formula_moiety 'C24 H21 B Br P' _chemical_formula_sum 'C24 H21 B Br P' _chemical_formula_weight 431.10 _chemical_name_systematic ; (4-Bromophenyl)(triphenylphosphanyl)borane ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 81.515(2) _cell_angle_beta 74.038(2) _cell_angle_gamma 67.798(2) _cell_formula_units_Z 2 _cell_length_a 9.4920(6) _cell_length_b 10.0234(7) _cell_length_c 12.0606(8) _cell_measurement_reflns_used 9941 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 72.10 _cell_measurement_theta_min 3.84 _cell_volume 1020.21(12) _computing_cell_refinement ; SAINT (Bruker, 2017) ; _computing_data_collection ; APEX3 (Bruker, 2018) ; _computing_data_reduction ; SAINT (Bruker, 2017) ; _computing_molecular_graphics ; XSEED (Barbour, 2001) ; _computing_publication_material ; XSEED (Barbour, 2001) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015a) ; _computing_structure_solution ; SHELXT2018 (Sheldrick, 2015b) ; _diffrn_ambient_temperature 100(2) _diffrn_detector 'Bruker Photon II CPAD' _diffrn_detector_area_resol_mean 7.9 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device 'Kappa Four-Circle Diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'Double Bounce Multilayer Mirrors' _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_unetI/netI 0.0219 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 6803 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 72.306 _diffrn_reflns_theta_min 3.817 _diffrn_source 'Microsource IuS Incoatec 3.0' _exptl_absorpt_coefficient_mu 3.508 _exptl_absorpt_correction_T_max 0.7535 _exptl_absorpt_correction_T_min 0.6440 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2016) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.403 _exptl_crystal_description plate _exptl_crystal_F_000 440 _exptl_crystal_size_max 0.238 _exptl_crystal_size_mid 0.207 _exptl_crystal_size_min 0.034 _refine_diff_density_max 0.410 _refine_diff_density_min -0.531 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 250 _refine_ls_number_reflns 3986 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.049 _refine_ls_R_factor_all 0.0257 _refine_ls_R_factor_gt 0.0252 _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^)+(0.0215P)^2^+0.9841P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.0632 _reflns_number_gt 3904 _reflns_number_total 3986 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file zo3028sup1.cif _cod_data_source_block I _cod_database_code 2022690 _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_hkl_file ; -1 0 0 204.27 6.41 1 0 0 210.19 6.43 -3 0 0 180.10 5.59 3 0 0 176.79 5.65 -4 0 0 41.25 1.40 4 0 0 40.58 1.47 -5 0 0 77.91 2.58 5 0 0 77.04 2.68 -6 0 0 83.50 2.75 -6 0 0 80.82 2.55 -6 0 0 80.52 2.60 -6 0 0 81.67 2.64 6 0 0 80.84 2.58 6 0 0 79.26 2.54 6 0 0 81.91 2.87 6 0 0 79.34 2.60 -7 0 0 0.14 0.09 -7 0 0 0.14 0.13 -7 0 0 0.20 0.24 -7 0 0 0.07 0.10 7 0 0 -0.06 0.11 7 0 0 0.19 0.08 7 0 0 0.34 0.10 7 0 0 0.19 0.30 -8 0 0 20.65 1.10 -8 0 0 21.92 0.82 -8 0 0 23.00 0.79 8 0 0 18.61 1.25 8 0 0 22.40 0.78 8 0 0 22.05 0.75 -9 0 0 58.85 1.90 -9 0 0 60.08 1.94 9 0 0 59.87 1.91 9 0 0 57.35 1.88 -10 0 0 5.77 0.27 -10 0 0 5.26 0.25 10 0 0 5.44 0.28 10 0 0 5.79 0.24 10 -1 0 12.92 0.45 -10 1 0 13.02 0.44 -10 1 0 12.82 0.46 9 -1 0 0.09 0.07 9 -1 0 0.19 0.07 -9 1 0 0.17 0.08 -9 1 0 0.21 0.11 8 -1 0 19.68 0.68 8 -1 0 20.00 0.71 -8 1 0 18.63 1.08 -8 1 0 20.31 0.72 -8 1 0 19.64 0.76 -8 1 0 19.80 0.66 7 -1 0 3.82 0.70 7 -1 0 3.41 0.20 7 -1 0 3.34 0.24 -7 1 0 3.20 0.24 -7 1 0 3.12 0.18 -7 1 0 3.28 0.45 -7 1 0 3.44 0.32 6 -1 0 93.33 2.97 6 -1 0 95.54 3.03 6 -1 0 93.15 3.31 6 -1 0 94.69 3.00 -6 1 0 95.27 2.99 -6 1 0 97.41 3.21 -6 1 0 95.68 3.08 -6 1 0 94.67 3.04 5 -1 0 19.69 0.72 5 -1 0 21.40 0.94 5 -1 0 20.84 0.75 -5 1 0 21.22 0.85 -5 1 0 20.43 0.71 4 -1 0 210.23 6.80 -4 1 0 216.23 6.73 3 -1 0 244.31 7.84 -3 1 0 253.85 7.78 2 -1 0 191.04 5.98 -2 1 0 190.31 5.94 1 -1 0 316.26 9.79 0 1 0 193.41 6.13 0 1 0 204.49 6.13 -1 -1 0 117.51 3.63 -1 -1 0 114.59 3.68 1 1 0 120.07 3.64 -3 -1 0 25.93 0.90 3 1 0 26.88 0.96 -4 -1 0 32.26 1.13 4 1 0 32.76 1.21 -5 -1 0 230.82 7.21 5 1 0 225.71 7.31 -6 -1 0 6.56 0.42 -6 -1 0 6.54 0.29 -6 -1 0 6.14 0.34 -6 -1 0 5.87 0.37 6 1 0 6.27 0.31 6 1 0 6.34 0.38 6 1 0 6.45 0.27 -7 -1 0 92.50 3.14 -7 -1 0 93.40 3.08 7 1 0 94.71 2.94 7 1 0 90.68 2.95 7 1 0 91.76 2.91 7 1 0 90.67 3.29 -8 -1 0 11.30 0.46 -8 -1 0 11.14 0.50 -8 -1 0 10.69 0.81 8 1 0 11.41 0.44 8 1 0 11.29 0.47 8 1 0 11.40 0.41 8 1 0 11.12 0.88 -9 -1 0 0.15 0.10 -9 -1 0 0.14 0.10 9 1 0 0.18 0.10 9 1 0 0.16 0.06 -10 -1 0 6.47 0.29 -10 -1 0 6.48 0.33 10 1 0 6.78 0.26 10 1 0 6.90 0.29 9 -2 0 19.67 0.66 -9 2 0 18.98 0.70 -9 2 0 19.35 0.67 8 -2 0 5.47 0.25 8 -2 0 5.55 0.27 -8 2 0 5.80 0.28 -8 2 0 5.44 0.35 -8 2 0 5.67 0.23 7 -2 0 2.19 0.19 7 -2 0 2.12 0.17 -7 2 0 1.95 0.15 -7 2 0 2.53 0.39 -7 2 0 2.41 0.27 -7 2 0 2.22 0.21 6 -2 0 43.64 1.77 6 -2 0 44.12 1.44 6 -2 0 44.79 1.47 -6 2 0 43.85 1.49 -6 2 0 44.11 1.66 -6 2 0 43.59 1.53 -6 2 0 43.91 1.43 5 -2 0 0.38 0.23 5 -2 0 0.33 0.11 5 -2 0 0.31 0.12 -5 2 0 0.56 0.17 -5 2 0 0.82 0.30 -5 2 0 0.19 0.10 4 -2 0 38.30 1.42 -4 2 0 37.63 1.35 3 -2 0 1.89 0.22 -3 2 0 1.97 0.18 2 -2 0 321.96 10.18 -2 2 0 332.01 10.16 1 -2 0 4.40 0.21 -1 2 0 4.12 0.19 0 2 0 38.14 1.22 0 2 0 39.50 1.25 -1 -2 0 43.21 1.31 -1 -2 0 40.15 1.38 1 2 0 39.57 1.30 1 2 0 43.80 1.30 -2 -2 0 242.25 7.57 2 2 0 247.69 7.61 3 2 0 133.29 4.24 -4 -2 0 0.45 0.10 4 2 0 0.35 0.12 -5 -2 0 37.16 1.35 5 2 0 40.08 1.46 -6 -2 0 7.57 0.40 -6 -2 0 8.28 0.39 -6 -2 0 7.61 0.45 6 2 0 7.51 0.32 6 2 0 8.48 0.60 -7 -2 0 4.13 0.28 -7 -2 0 4.06 0.30 -7 -2 0 3.96 0.47 7 2 0 3.87 0.22 7 2 0 3.90 0.25 7 2 0 4.34 0.34 7 2 0 4.57 0.51 -8 -2 0 -0.03 0.12 -8 -2 0 0.66 0.14 -8 -2 0 -0.58 0.48 8 2 0 0.18 0.07 8 2 0 0.33 0.09 8 2 0 -0.12 0.31 8 2 0 0.17 0.15 -9 -2 0 0.14 0.12 -9 -2 0 0.08 0.10 9 2 0 -0.24 0.12 9 2 0 0.24 0.07 9 2 0 0.30 0.08 10 2 0 4.30 0.24 -11 -2 0 4.88 0.20 11 2 0 4.72 0.19 9 -3 0 2.19 0.12 -9 3 0 2.43 0.14 8 -3 0 7.14 0.29 -8 3 0 7.34 0.32 -8 3 0 6.79 0.29 -8 3 0 7.16 0.41 7 -3 0 5.88 0.29 -7 3 0 6.05 0.32 -7 3 0 6.08 0.26 -7 3 0 6.43 0.65 -7 3 0 6.26 0.44 6 -3 0 51.48 1.68 6 -3 0 53.25 1.72 -6 3 0 54.42 1.76 -6 3 0 50.97 1.80 -6 3 0 52.54 1.96 -6 3 0 52.54 1.70 5 -3 0 121.15 3.86 5 -3 0 119.86 3.82 -5 3 0 120.83 3.85 -5 3 0 127.82 4.06 4 -3 0 0.05 0.22 4 -3 0 0.38 0.12 -4 3 0 0.25 0.14 -4 3 0 0.06 0.12 3 -3 0 308.55 9.80 -3 3 0 316.94 9.79 2 -3 0 150.50 4.88 -2 3 0 150.49 4.75 1 -3 0 150.36 4.76 -1 3 0 155.92 4.79 0 3 0 55.80 1.76 -1 -3 0 29.38 1.09 -1 -3 0 32.06 0.99 -2 -3 0 1.62 0.18 -2 -3 0 1.75 0.09 2 3 0 1.54 0.12 -3 -3 0 237.13 7.42 3 3 0 242.19 7.50 -4 -3 0 19.82 0.83 4 3 0 24.34 0.88 -5 -3 0 184.37 5.90 5 3 0 190.52 6.04 -6 -3 0 97.22 3.24 -6 -3 0 103.54 3.28 -6 -3 0 97.67 3.18 6 3 0 92.09 3.16 6 3 0 112.88 3.88 6 3 0 97.20 3.16 -7 -3 0 6.40 0.39 -7 -3 0 7.32 0.37 -7 -3 0 7.52 0.40 7 3 0 7.93 0.60 7 3 0 7.61 0.34 7 3 0 7.55 0.32 -8 -3 0 13.56 0.56 -8 -3 0 13.88 0.55 8 3 0 13.46 0.51 8 3 0 12.83 0.59 8 3 0 13.95 0.49 8 3 0 12.78 0.90 -9 -3 0 3.73 0.24 9 3 0 3.68 0.30 9 3 0 3.60 0.67 9 3 0 3.57 0.19 9 3 0 3.57 0.20 -10 -3 0 5.59 0.26 10 3 0 5.11 0.23 10 3 0 5.55 0.24 10 3 0 5.53 0.32 -11 -3 0 0.44 0.07 11 3 0 0.48 0.09 8 -4 0 1.78 0.11 -8 4 0 1.83 0.14 -8 4 0 1.86 0.11 7 -4 0 6.54 0.28 -7 4 0 6.45 0.27 -7 4 0 6.50 0.31 6 -4 0 0.75 0.17 -6 4 0 0.89 0.32 -6 4 0 1.22 0.18 5 -4 0 10.82 0.56 5 -4 0 11.26 0.45 -5 4 0 11.56 0.65 -5 4 0 11.02 0.50 -5 4 0 11.45 0.45 4 -4 0 16.07 0.59 4 -4 0 15.62 0.61 -4 4 0 14.93 0.62 -4 4 0 16.22 0.73 3 -4 0 110.45 3.55 3 -4 0 110.16 3.56 3 -4 0 109.90 3.76 -3 4 0 120.72 3.68 -2 4 0 111.05 3.56 -1 4 0 466.39 14.54 0 4 0 605.70 18.69 -1 -4 0 8.88 0.45 -2 -4 0 333.26 10.75 -2 -4 0 364.06 10.58 2 4 0 328.80 10.55 -3 -4 0 93.10 2.95 3 4 0 95.83 3.02 -4 -4 0 74.00 2.38 4 4 0 76.83 2.51 5 4 0 109.19 3.62 -6 -4 0 108.85 3.39 -6 -4 0 103.38 3.34 6 4 0 115.94 3.66 6 4 0 97.43 3.32 6 4 0 102.27 3.33 -7 -4 0 12.65 0.52 7 4 0 13.00 0.50 7 4 0 12.13 0.47 7 4 0 12.61 0.79 -8 -4 0 65.21 2.10 8 4 0 63.35 2.08 8 4 0 65.26 2.50 8 4 0 64.50 2.06 -9 -4 0 42.55 1.39 9 4 0 42.41 1.36 9 4 0 42.29 1.37 9 4 0 39.01 1.86 -10 -4 0 0.56 0.09 10 4 0 0.52 0.08 10 4 0 0.39 0.07 -11 -4 0 1.68 0.18 11 4 0 1.47 0.10 7 -5 0 2.10 0.12 -7 5 0 1.79 0.12 -7 5 0 1.90 0.16 6 -5 0 17.91 0.62 -6 5 0 17.87 0.63 -6 5 0 18.01 0.67 5 -5 0 1.16 0.19 5 -5 0 1.07 0.12 -5 5 0 0.99 0.12 -5 5 0 0.93 0.31 -5 5 0 1.30 0.18 4 -5 0 113.35 3.67 4 -5 0 114.02 3.65 -4 5 0 120.31 3.86 3 -5 0 52.17 1.76 3 -5 0 49.53 1.62 3 -5 0 50.41 1.65 -3 5 0 47.09 1.67 -3 5 0 51.85 1.78 2 -5 0 7.95 0.44 2 -5 0 8.39 0.52 2 -5 0 7.53 0.35 -2 5 0 7.96 0.41 -1 5 0 76.08 2.46 0 5 0 129.36 4.06 -1 -5 0 6.07 0.41 -2 -5 0 114.66 3.82 -3 -5 0 120.93 4.28 3 5 0 137.83 4.10 -4 -5 0 0.69 0.09 4 5 0 1.07 0.18 -5 -5 0 80.32 2.70 -5 -5 0 83.98 2.65 -5 -5 0 82.27 2.72 5 5 0 88.61 2.84 -6 -5 0 40.93 1.34 -6 -5 0 41.08 1.40 -6 -5 0 42.08 1.35 -6 -5 0 41.49 1.38 -6 -5 0 41.19 1.38 6 5 0 38.30 1.38 6 5 0 38.20 1.38 6 5 0 43.57 1.60 -7 -5 0 26.93 0.95 -7 -5 0 26.64 0.98 -7 -5 0 26.58 0.91 7 5 0 26.61 1.21 7 5 0 25.09 1.04 -8 -5 0 55.27 1.78 -8 -5 0 54.14 1.79 8 5 0 54.98 1.77 8 5 0 55.28 2.18 8 5 0 53.56 1.76 -9 -5 0 1.24 0.13 9 5 0 1.33 0.13 9 5 0 1.35 0.15 -10 -5 0 27.65 0.99 10 5 0 29.40 0.94 -11 -5 0 51.13 1.62 11 5 0 53.01 1.63 -7 6 0 5.19 0.23 6 -6 0 1.88 0.12 -6 6 0 1.97 0.18 -6 6 0 1.81 0.18 5 -6 0 1.63 0.13 5 -6 0 1.47 0.18 -5 6 0 1.47 0.15 -5 6 0 1.37 0.17 4 -6 0 0.95 0.18 4 -6 0 1.10 0.12 4 -6 0 0.93 0.14 -4 6 0 0.90 0.29 -4 6 0 1.10 0.14 -4 6 0 0.76 0.17 3 -6 0 0.31 0.10 3 -6 0 0.45 0.12 -3 6 0 0.14 0.21 -3 6 0 0.66 0.18 2 -6 0 9.29 0.50 2 -6 0 9.13 0.42 2 -6 0 9.87 0.38 -2 6 0 9.95 0.50 1 -6 0 10.18 0.45 1 -6 0 10.92 0.52 1 -6 0 10.15 0.46 -1 6 0 10.65 0.48 0 -6 0 24.91 0.88 0 6 0 23.79 0.84 -1 -6 0 6.40 0.48 -2 -6 0 120.05 4.07 -3 -6 0 6.17 0.48 -4 -6 0 28.59 1.06 4 6 0 32.43 1.12 -5 -6 0 8.78 0.42 -5 -6 0 9.35 0.39 -5 -6 0 8.98 0.42 -5 -6 0 9.12 0.54 5 6 0 9.78 0.55 -6 -6 0 2.63 0.23 -6 -6 0 1.97 0.25 -6 -6 0 2.43 0.23 -6 -6 0 2.61 0.24 6 6 0 2.65 0.42 -7 -6 0 46.05 1.55 -7 -6 0 45.74 1.52 -7 -6 0 45.34 1.46 7 6 0 44.41 1.79 7 6 0 45.14 1.48 7 6 0 44.12 1.47 -8 -6 0 69.11 2.25 -8 -6 0 71.50 2.21 8 6 0 69.15 2.22 8 6 0 67.95 2.60 8 6 0 69.33 2.22 -9 -6 0 13.32 0.48 -9 -6 0 13.24 0.52 9 6 0 13.78 0.49 9 6 0 13.55 0.49 -10 -6 0 10.43 0.36 10 6 0 10.33 0.38 10 6 0 10.44 0.38 11 6 0 0.37 0.06 11 6 0 0.40 0.06 -6 7 0 22.21 0.71 -6 7 0 21.56 0.73 5 -7 0 14.55 0.55 -5 7 0 15.14 0.58 -5 7 0 14.36 0.55 4 -7 0 9.48 0.43 -4 7 0 10.28 0.45 -4 7 0 9.77 0.40 3 -7 0 9.76 0.48 3 -7 0 9.88 0.43 -3 7 0 9.41 0.67 2 -7 0 3.71 0.26 2 -7 0 3.66 0.32 -2 7 0 2.59 0.51 -2 7 0 3.91 0.42 1 -7 0 3.05 0.25 1 -7 0 2.88 0.25 1 -7 0 2.59 0.28 -1 7 0 3.57 0.35 0 -7 0 26.83 0.97 0 -7 0 25.92 0.95 0 -7 0 26.67 1.02 0 -7 0 26.52 1.27 0 -7 0 26.49 0.94 -1 -7 0 5.37 0.40 -1 -7 0 6.02 0.38 -1 -7 0 5.14 0.32 -1 -7 0 4.87 0.32 -1 -7 0 5.16 0.51 -2 -7 0 0.80 0.28 -2 -7 0 0.91 0.18 -2 -7 0 0.71 0.16 -2 -7 0 0.83 0.17 -2 -7 0 0.67 0.13 -3 -7 0 31.57 1.07 -3 -7 0 30.17 1.08 -3 -7 0 32.08 1.09 -3 -7 0 29.60 1.36 -3 -7 0 28.98 1.06 -4 -7 0 5.78 0.37 -4 -7 0 6.14 0.34 -4 -7 0 6.47 0.36 -5 -7 0 31.72 1.09 -5 -7 0 29.98 1.10 -6 -7 0 23.29 0.83 -6 -7 0 23.23 0.83 -6 -7 0 22.09 0.85 6 7 0 21.43 1.02 -7 -7 0 9.85 0.43 -7 -7 0 8.86 0.45 7 7 0 9.84 0.78 7 7 0 9.54 0.41 -8 -7 0 20.65 0.74 8 7 0 21.14 1.22 8 7 0 19.98 0.70 8 7 0 19.14 0.70 -9 -7 0 38.31 1.26 9 7 0 38.02 1.24 10 7 0 0.83 0.10 10 7 0 0.75 0.09 -5 8 0 3.41 0.16 4 -8 0 10.70 0.43 -4 8 0 11.51 0.42 3 -8 0 20.49 0.77 3 -8 0 21.09 0.74 -3 8 0 20.67 0.73 2 -8 0 6.07 0.31 2 -8 0 5.69 0.34 2 -8 0 5.52 0.82 -2 8 0 5.55 0.40 1 -8 0 8.95 0.40 1 -8 0 7.90 0.80 1 -8 0 9.03 0.49 0 -8 0 76.50 2.49 0 -8 0 78.48 2.48 0 -8 0 75.90 2.57 0 -8 0 73.72 2.96 -1 -8 0 3.21 0.28 -1 -8 0 2.99 0.26 -1 -8 0 3.39 0.29 -1 -8 0 2.87 0.26 -1 -8 0 3.30 0.32 -1 -8 0 3.26 0.54 -2 -8 0 91.21 2.91 -2 -8 0 89.65 2.91 -2 -8 0 92.61 3.00 -2 -8 0 90.87 2.96 -2 -8 0 85.93 3.31 -2 -8 0 92.34 2.89 -2 -8 0 88.47 2.92 -3 -8 0 53.76 1.78 -3 -8 0 51.06 2.15 -3 -8 0 53.42 1.75 -3 -8 0 52.31 1.74 -3 -8 0 54.25 1.77 -3 -8 0 51.64 1.73 -4 -8 0 4.30 0.56 -4 -8 0 5.63 0.32 -4 -8 0 5.75 0.35 -5 -8 0 167.92 5.36 -5 -8 0 169.71 5.36 -5 -8 0 172.05 5.37 -6 -8 0 127.39 4.07 -6 -8 0 124.59 4.08 -6 -8 0 132.59 4.09 -7 -8 0 21.24 0.82 -7 -8 0 23.45 0.83 7 8 0 21.97 0.78 -8 -8 0 98.17 3.14 8 8 0 98.61 3.10 -9 -8 0 15.85 0.57 9 8 0 15.88 0.55 10 8 0 31.56 1.02 4 -9 0 22.91 0.82 -4 9 0 26.04 0.79 3 -9 0 11.38 0.46 3 -9 0 12.00 0.46 -3 9 0 12.11 0.43 2 -9 0 25.58 0.90 2 -9 0 25.94 0.92 2 -9 0 25.39 0.89 -2 9 0 26.19 0.89 1 -9 0 41.91 1.50 1 -9 0 42.95 1.45 1 -9 0 45.06 1.56 1 -9 0 44.28 1.47 0 -9 0 15.04 1.14 0 -9 0 15.98 0.61 0 -9 0 15.46 0.70 0 -9 0 15.84 0.63 -1 -9 0 3.22 0.62 -1 -9 0 3.29 0.41 -1 -9 0 3.07 0.25 -1 -9 0 3.16 0.24 -2 -9 0 191.68 6.25 -2 -9 0 206.76 6.29 -2 -9 0 203.68 6.29 -2 -9 0 206.58 6.31 -2 -9 0 187.78 6.77 -2 -9 0 210.69 6.40 -2 -9 0 200.81 6.27 -2 -9 0 193.02 6.25 -3 -9 0 82.77 2.66 -3 -9 0 80.14 2.64 -3 -9 0 82.33 2.65 -3 -9 0 84.47 2.69 -3 -9 0 81.11 2.68 -3 -9 0 81.43 2.66 -3 -9 0 84.00 2.76 -3 -9 0 80.33 2.63 -3 -9 0 83.52 2.65 -4 -9 0 31.32 1.06 -4 -9 0 29.81 1.06 -4 -9 0 29.92 1.08 -4 -9 0 30.05 1.09 -4 -9 0 30.49 1.06 -4 -9 0 30.17 1.09 -5 -9 0 109.81 3.57 -5 -9 0 111.06 3.55 -5 -9 0 111.81 3.54 -6 -9 0 15.07 0.59 -6 -9 0 15.48 0.60 -6 -9 0 15.07 0.59 -7 -9 0 51.71 1.71 -7 -9 0 52.19 1.71 -8 -9 0 35.73 1.19 -8 -9 0 35.08 1.19 8 9 0 35.41 1.16 -9 -9 0 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17.43 0.63 1 5 12 17.41 0.66 1 5 12 17.20 0.61 -2 -5 -12 10.18 0.43 2 5 12 10.73 0.41 2 5 12 10.19 0.44 -3 -5 -12 0.37 0.13 3 5 12 0.45 0.09 3 5 12 0.29 0.12 -4 -5 -12 27.05 0.98 4 5 12 28.39 0.99 4 5 12 28.57 0.96 -5 -5 -12 62.61 2.10 5 5 12 65.61 2.12 5 5 12 65.30 2.08 -6 -5 -12 4.08 0.33 6 5 12 4.24 0.28 6 5 12 4.16 0.23 -7 -5 -12 104.62 3.32 7 5 12 102.91 3.31 7 5 12 107.72 3.35 -8 -5 -12 18.57 0.67 8 5 12 20.12 0.66 8 5 12 19.62 0.70 9 5 12 0.58 0.09 9 5 12 0.74 0.09 0 6 12 0.33 0.06 0 6 12 0.20 0.09 1 6 12 56.26 1.81 2 6 12 16.95 0.65 2 6 12 18.38 0.63 3 6 12 47.48 1.57 3 6 12 47.57 1.54 4 6 12 150.62 4.74 4 6 12 150.48 4.71 5 6 12 15.99 0.58 5 6 12 15.78 0.62 6 6 12 92.88 3.02 6 6 12 96.27 3.03 7 6 12 115.24 3.79 7 6 12 124.80 3.77 8 6 12 0.15 0.06 8 6 12 0.07 0.17 1 7 12 65.49 2.06 2 7 12 2.51 0.23 2 7 12 2.46 0.16 3 7 12 8.21 0.33 -4 -7 -12 12.90 0.52 4 7 12 13.75 0.49 4 7 12 13.80 0.55 -5 -7 -12 0.23 0.14 5 7 12 -0.11 0.17 5 7 12 0.13 0.08 -6 -7 -12 52.24 1.73 -6 -7 -12 51.85 1.73 6 7 12 55.22 1.73 6 7 12 56.79 1.77 -7 -7 -12 2.35 0.31 7 7 12 3.07 0.18 7 7 12 3.00 0.26 8 7 12 26.30 0.92 8 7 12 28.01 0.94 2 8 12 0.30 0.06 3 8 12 0.20 0.07 4 8 12 0.25 0.07 -5 -8 -12 0.08 0.14 -5 -8 -12 0.40 0.11 5 8 12 0.12 0.08 -6 -8 -12 3.78 0.29 -6 -8 -12 3.99 0.22 7 8 12 2.42 0.15 0 4 -13 25.18 0.85 0 -4 13 25.31 0.83 1 -4 13 3.72 0.21 -2 4 -13 38.66 1.26 2 -4 13 38.88 1.25 1 3 -13 18.90 0.65 -1 -3 13 18.53 0.64 0 3 -13 13.36 0.49 0 -3 13 12.93 0.49 -1 3 -13 2.56 0.29 -1 3 -13 3.24 0.20 1 -3 13 3.11 0.19 -2 3 -13 40.49 1.47 -2 3 -13 44.19 1.41 2 -3 13 44.84 1.42 -3 3 -13 10.04 0.54 -3 3 -13 10.82 0.41 3 -3 13 11.23 0.42 -4 3 -13 5.99 0.31 4 -3 13 5.19 0.26 2 2 -13 5.91 0.25 1 2 -13 3.13 0.26 1 2 -13 2.61 0.18 -1 -2 13 2.66 0.18 0 2 -13 5.84 0.35 0 2 -13 6.18 0.29 0 -2 13 6.50 0.30 -1 2 -13 27.15 0.93 -1 2 -13 25.88 0.96 1 -2 13 28.19 0.94 -2 2 -13 0.07 0.17 -2 2 -13 0.12 0.09 2 -2 13 0.00 0.09 -3 2 -13 33.94 1.20 -3 2 -13 34.54 1.16 3 -2 13 35.35 1.17 -4 2 -13 0.42 0.19 -4 2 -13 0.20 0.08 4 -2 13 0.01 0.09 -5 2 -13 23.42 0.85 5 -2 13 24.10 0.81 2 1 -13 20.87 0.73 2 1 -13 19.67 0.69 -2 -1 13 22.26 0.75 1 1 -13 51.92 1.68 1 1 -13 51.33 1.65 -1 -1 13 49.34 1.63 -1 -1 13 52.40 1.67 0 1 -13 80.15 2.57 0 1 -13 80.17 2.60 0 -1 13 79.75 2.55 0 -1 13 82.61 2.59 -1 1 -13 2.51 0.20 -1 1 -13 2.18 0.24 1 -1 13 2.14 0.20 1 -1 13 2.07 0.20 -2 1 -13 84.59 2.68 -2 1 -13 81.68 2.72 2 -1 13 85.78 2.72 2 -1 13 83.56 2.66 -3 1 -13 25.30 0.94 -3 1 -13 26.57 0.90 3 -1 13 25.27 0.91 3 -1 13 26.08 0.88 -4 1 -13 1.69 0.20 -4 1 -13 2.03 0.18 4 -1 13 1.95 0.20 4 -1 13 2.02 0.19 -5 1 -13 43.73 1.43 -5 1 -13 44.36 1.49 5 -1 13 43.13 1.41 5 -1 13 46.08 1.47 -6 1 -13 17.14 0.64 2 0 -13 7.34 0.33 -2 0 13 6.90 0.30 -2 0 13 6.90 0.29 1 0 -13 92.37 2.95 -1 0 13 93.83 2.91 -1 0 13 91.21 2.93 0 0 -13 21.01 0.78 0 0 -13 20.84 0.74 0 0 13 21.52 0.74 0 0 13 21.82 0.77 -1 0 -13 20.10 0.85 -1 0 -13 16.38 0.63 1 0 13 17.24 0.66 1 0 13 16.34 0.74 -2 0 -13 158.30 5.07 -2 0 -13 158.93 5.10 2 0 13 163.32 5.03 -3 0 -13 22.47 0.79 -3 0 -13 22.10 0.84 3 0 13 22.77 0.80 -4 0 -13 39.77 1.33 -4 0 -13 39.17 1.41 4 0 13 40.65 1.37 4 0 13 41.56 1.34 -5 0 -13 31.15 1.10 -5 0 -13 30.95 1.04 5 0 13 32.04 1.05 5 0 13 31.70 1.09 -6 0 -13 9.69 0.44 6 0 13 10.22 0.39 6 0 13 10.24 0.42 -7 0 -13 15.24 0.57 7 0 13 15.63 0.55 2 -1 -13 5.39 0.25 -2 1 13 5.50 0.28 -2 1 13 5.19 0.23 1 -1 -13 58.77 1.91 -1 1 13 57.36 1.89 -1 1 13 59.99 1.88 0 -1 -13 3.79 0.24 0 -1 -13 3.03 0.26 0 1 13 3.68 0.22 0 1 13 3.59 0.26 -1 -1 -13 48.88 1.64 -1 -1 -13 47.62 1.59 1 1 13 49.75 1.64 1 1 13 50.36 1.62 -2 -1 -13 59.85 1.95 -2 -1 -13 59.82 2.00 2 1 13 61.37 1.98 2 1 13 61.47 2.03 -3 -1 -13 0.82 0.16 -3 -1 -13 0.69 0.15 3 1 13 0.93 0.29 3 1 13 0.84 0.13 -4 -1 -13 131.34 4.13 -4 -1 -13 128.16 4.20 4 1 13 135.09 4.17 4 1 13 133.82 4.20 -5 -1 -13 46.92 1.69 5 1 13 47.70 1.62 5 1 13 50.54 1.65 -6 -1 -13 11.13 0.48 6 1 13 10.72 0.48 6 1 13 11.67 0.44 -7 -1 -13 15.38 0.58 7 1 13 15.52 0.58 7 1 13 15.77 0.55 2 -2 -13 0.25 0.08 -2 2 13 0.31 0.07 1 -2 -13 6.15 0.28 -1 2 13 5.83 0.26 -1 2 13 5.32 0.36 0 -2 -13 16.77 0.64 0 2 13 17.56 0.63 0 2 13 18.04 0.73 -1 -2 -13 0.13 0.10 1 2 13 0.01 0.09 1 2 13 0.03 0.21 -2 -2 -13 5.28 0.30 2 2 13 5.55 0.29 2 2 13 5.78 0.41 -3 -2 -13 7.90 0.38 3 2 13 7.60 0.45 3 2 13 7.93 0.36 3 2 13 6.79 0.39 -4 -2 -13 16.05 0.63 4 2 13 15.85 0.68 4 2 13 15.59 0.60 -5 -2 -13 20.29 0.77 5 2 13 21.52 0.82 5 2 13 20.30 0.75 -6 -2 -13 15.79 0.62 6 2 13 16.30 0.60 -7 -2 -13 0.10 0.10 7 2 13 0.11 0.23 7 2 13 0.17 0.08 -8 -2 -13 10.88 0.41 8 2 13 10.85 0.39 1 -3 -13 61.77 1.95 -1 3 13 60.35 1.94 0 -3 -13 21.32 0.75 0 3 13 21.23 0.74 -1 -3 -13 6.78 0.35 1 3 13 7.32 0.45 1 3 13 6.57 0.28 -2 -3 -13 33.70 1.16 2 3 13 33.05 1.18 2 3 13 34.72 1.15 -3 -3 -13 31.67 1.12 3 3 13 32.84 1.11 -4 -3 -13 1.79 0.21 4 3 13 2.17 0.20 4 3 13 2.11 0.16 -5 -3 -13 37.34 1.29 5 3 13 38.04 1.27 5 3 13 37.28 1.22 -6 -3 -13 0.13 0.10 6 3 13 0.06 0.07 6 3 13 0.21 0.10 -7 -3 -13 10.00 0.41 7 3 13 9.78 0.40 -8 -3 -13 19.36 0.66 8 3 13 18.74 0.71 1 -4 -13 53.85 1.72 -1 4 13 56.00 1.74 0 -4 -13 7.34 0.31 0 4 13 6.99 0.31 0 4 13 7.89 0.30 -1 -4 -13 27.57 0.95 1 4 13 28.04 0.92 1 4 13 28.75 0.96 -2 -4 -13 107.59 3.47 2 4 13 109.81 3.47 2 4 13 111.45 3.44 -3 -4 -13 10.44 0.56 3 4 13 10.30 0.41 3 4 13 10.55 0.55 -4 -4 -13 65.71 2.20 4 4 13 64.32 2.10 4 4 13 60.97 2.03 -5 -4 -13 55.26 1.84 5 4 13 58.63 1.86 5 4 13 55.11 1.83 -6 -4 -13 7.32 0.35 6 4 13 7.44 0.30 6 4 13 8.00 0.35 -7 -4 -13 35.71 1.18 7 4 13 36.85 1.19 7 4 13 34.72 1.14 -8 -4 -13 23.32 0.76 8 4 13 22.91 0.87 0 5 13 3.96 0.20 0 5 13 4.10 0.17 -1 -5 -13 28.00 0.94 1 5 13 29.17 0.94 1 5 13 30.25 0.97 -2 -5 -13 45.97 1.51 2 5 13 47.29 1.50 2 5 13 47.53 1.53 -3 -5 -13 20.09 0.71 3 5 13 20.71 0.70 3 5 13 20.28 0.73 -4 -5 -13 103.05 3.29 4 5 13 105.98 3.31 4 5 13 103.88 3.28 -5 -5 -13 2.16 0.20 5 5 13 2.85 0.21 5 5 13 2.32 0.16 -6 -5 -13 1.33 0.14 6 5 13 1.56 0.13 6 5 13 1.35 0.15 7 5 13 8.07 0.31 7 5 13 8.68 0.35 8 5 13 7.37 0.27 8 5 13 8.36 0.32 1 6 13 1.86 0.16 1 6 13 1.65 0.12 2 6 13 15.18 0.54 2 6 13 15.24 0.52 3 6 13 3.56 0.18 3 6 13 3.10 0.21 4 6 13 34.40 1.12 4 6 13 34.04 1.14 5 6 13 10.51 0.39 5 6 13 10.37 0.42 6 6 13 1.29 0.22 6 6 13 0.95 0.11 7 6 13 0.84 0.10 7 6 13 0.84 0.12 3 7 13 2.30 0.15 4 7 13 0.42 0.07 4 7 13 0.27 0.15 5 7 13 11.63 0.49 5 7 13 12.86 0.44 -1 2 -14 15.03 0.59 -1 2 -14 15.82 0.54 1 -2 14 16.27 0.55 -2 2 -14 11.89 0.43 -2 2 -14 12.00 0.53 2 -2 14 12.07 0.44 -3 2 -14 38.44 1.34 -3 2 -14 40.21 1.27 3 -2 14 40.41 1.29 0 1 -14 36.38 1.22 0 -1 14 37.85 1.21 -1 1 -14 2.20 0.18 -1 1 -14 1.82 0.21 1 -1 14 2.31 0.18 -2 1 -14 73.44 2.27 -2 1 -14 63.28 2.11 2 -1 14 65.05 2.14 -3 1 -14 52.07 1.67 -3 1 -14 52.64 1.72 3 -1 14 53.55 1.70 -4 1 -14 0.42 0.13 4 -1 14 0.36 0.10 0 0 -14 6.96 0.33 0 0 14 6.75 0.30 0 0 14 6.32 0.28 -1 0 -14 1.55 0.17 1 0 14 2.32 0.25 1 0 14 1.41 0.15 -2 0 -14 6.34 0.31 -2 0 -14 7.11 0.34 2 0 14 7.06 0.29 2 0 14 7.19 0.33 -3 0 -14 9.08 0.40 -3 0 -14 8.37 0.37 3 0 14 9.78 0.36 3 0 14 9.48 0.39 -4 0 -14 0.05 0.11 4 0 14 0.26 0.13 4 0 14 -0.01 0.09 -5 0 -14 11.44 0.45 5 0 14 9.82 0.39 5 0 14 11.05 0.42 0 -1 -14 30.32 1.00 0 1 14 29.67 0.97 0 1 14 29.39 0.99 -1 -1 -14 24.12 0.84 1 1 14 24.18 0.81 1 1 14 24.00 0.84 -2 -1 -14 11.47 0.47 2 1 14 11.46 0.63 2 1 14 11.95 0.44 -3 -1 -14 31.78 1.11 3 1 14 32.68 1.09 3 1 14 33.75 1.14 -4 -1 -14 3.84 0.25 4 1 14 4.17 0.22 4 1 14 4.27 0.29 -5 -1 -14 4.78 0.26 5 1 14 4.53 0.23 5 1 14 5.25 0.29 -6 -1 -14 28.84 0.97 6 1 14 29.15 0.94 6 1 14 28.64 0.97 0 2 14 27.59 0.92 -1 -2 -14 0.29 0.10 1 2 14 0.59 0.25 1 2 14 0.32 0.08 -2 -2 -14 26.06 0.89 2 2 14 24.64 0.91 2 2 14 25.96 0.87 -3 -2 -14 31.43 1.09 3 2 14 33.66 1.08 3 2 14 31.50 1.11 -4 -2 -14 0.66 0.12 4 2 14 0.72 0.11 4 2 14 0.48 0.21 -5 -2 -14 0.72 0.12 5 2 14 0.61 0.10 -6 -2 -14 46.68 1.54 6 2 14 48.02 1.54 -1 -3 -14 9.66 0.38 1 3 14 9.64 0.37 -2 -3 -14 50.57 1.68 2 3 14 52.87 1.67 -3 -3 -14 26.93 0.93 3 3 14 27.66 0.93 -4 -3 -14 12.67 0.50 4 3 14 12.99 0.49 -5 -3 -14 75.63 2.43 5 3 14 76.93 2.43 -6 -3 -14 13.92 0.51 6 3 14 13.79 0.50 -1 -4 -14 5.83 0.25 1 4 14 6.27 0.26 2 4 14 11.48 0.43 -3 -4 -14 3.86 0.21 3 4 14 3.83 0.21 -4 -4 -14 11.60 0.44 4 4 14 11.60 0.44 -5 -4 -14 21.60 0.73 5 4 14 20.54 0.69 5 4 14 21.91 0.74 -6 -4 -14 0.76 0.10 6 4 14 0.91 0.11 2 5 14 2.51 0.16 3 5 14 28.99 0.96 5 5 14 10.71 0.43 6 5 14 1.72 0.12 6 5 14 1.76 0.15 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 92167 _shelx_res_file ; TITL cu_20ERA01_0m in P-1 C:\frames\guest\20ERA01\work\cu_20ERA01_0m.res created by SHELXL-2018/3 at 08:06:11 on 01-Jun-2020 CELL 1.54178 9.4920 10.0234 12.0606 81.515 74.038 67.798 ZERR 2.0000 0.0006 0.0007 0.0008 0.002 0.002 0.002 LATT 1 SFAC C H B P BR UNIT 48 42 2 2 2 BOND $h conf ACTA FMAP 2 1 53 PLAN 20 0 0 TEMP -173 L.S. 10 WGHT 0.021500 0.984100 FVAR 0.28156 BR1 5 0.323277 0.484898 0.105904 11.00000 0.04593 0.03054 = 0.01421 0.00151 -0.00767 -0.02059 P1 4 0.333169 0.250849 0.716491 11.00000 0.01051 0.01121 = 0.01213 -0.00028 -0.00335 -0.00479 C1 1 0.274234 0.268880 0.482687 11.00000 0.01682 0.01192 = 0.01623 -0.00394 -0.00534 -0.00673 C2 1 0.143692 0.346704 0.437275 11.00000 0.01548 0.01510 = 0.01941 -0.00365 -0.00475 -0.00664 AFIX 43 H2 2 0.042212 0.357635 0.484672 11.00000 -1.20000 AFIX 0 C3 1 0.156527 0.408645 0.325627 11.00000 0.02155 0.01683 = 0.02141 -0.00004 -0.01127 -0.00774 AFIX 43 H3 2 0.065679 0.459834 0.297054 11.00000 -1.20000 AFIX 0 C4 1 0.303944 0.394322 0.257032 11.00000 0.02951 0.01625 = 0.01398 -0.00141 -0.00693 -0.01200 C5 1 0.437968 0.318445 0.296914 11.00000 0.01955 0.01888 = 0.01852 -0.00566 -0.00071 -0.00951 AFIX 43 H5 2 0.538792 0.308835 0.248898 11.00000 -1.20000 AFIX 0 C6 1 0.421566 0.256692 0.408784 11.00000 0.01572 0.01599 = 0.02044 -0.00337 -0.00607 -0.00493 AFIX 43 H6 2 0.513121 0.204428 0.436253 11.00000 -1.20000 AFIX 0 C7 1 0.248676 0.443822 0.736703 11.00000 0.01057 0.01282 = 0.01712 -0.00008 -0.00623 -0.00386 C8 1 0.269359 0.536911 0.639638 11.00000 0.01590 0.01838 = 0.01466 -0.00043 -0.00502 -0.00661 AFIX 43 H8 2 0.329205 0.498154 0.566921 11.00000 -1.20000 AFIX 0 C9 1 0.202677 0.685617 0.649376 11.00000 0.02043 0.01673 = 0.02000 0.00464 -0.00967 -0.00855 AFIX 43 H9 2 0.217521 0.748213 0.583525 11.00000 -1.20000 AFIX 0 C10 1 0.114354 0.742557 0.755454 11.00000 0.01885 0.01300 = 0.02677 -0.00107 -0.00962 -0.00140 AFIX 43 H10 2 0.068703 0.844141 0.762101 11.00000 -1.20000 AFIX 0 C11 1 0.092718 0.651227 0.851745 11.00000 0.01870 0.01889 = 0.01925 -0.00436 -0.00354 -0.00023 AFIX 43 H11 2 0.032144 0.690538 0.924145 11.00000 -1.20000 AFIX 0 C12 1 0.159343 0.502373 0.842703 11.00000 0.01542 0.01681 = 0.01621 0.00138 -0.00500 -0.00318 AFIX 43 H12 2 0.143978 0.440397 0.908890 11.00000 -1.20000 AFIX 0 C13 1 0.544779 0.204549 0.677988 11.00000 0.01185 0.01296 = 0.01067 0.00002 -0.00345 -0.00500 C14 1 0.636502 0.064844 0.641571 11.00000 0.01621 0.01266 = 0.01554 -0.00107 -0.00483 -0.00677 AFIX 43 H14 2 0.587565 0.001074 0.633363 11.00000 -1.20000 AFIX 0 C15 1 0.798730 0.019383 0.617454 11.00000 0.01513 0.01191 = 0.01571 -0.00216 -0.00267 -0.00289 AFIX 43 H15 2 0.860611 -0.075613 0.593161 11.00000 -1.20000 AFIX 0 C16 1 0.870926 0.112665 0.628784 11.00000 0.01169 0.01689 = 0.01276 0.00056 -0.00251 -0.00509 AFIX 43 H16 2 0.981988 0.081366 0.612318 11.00000 -1.20000 AFIX 0 C17 1 0.780676 0.251229 0.664101 11.00000 0.01575 0.01623 = 0.01672 -0.00032 -0.00336 -0.00977 AFIX 43 H17 2 0.830186 0.314913 0.671449 11.00000 -1.20000 AFIX 0 C18 1 0.617548 0.297782 0.688935 11.00000 0.01441 0.01164 = 0.01632 -0.00202 -0.00338 -0.00445 AFIX 43 H18 2 0.556163 0.392851 0.713263 11.00000 -1.20000 AFIX 0 C19 1 0.296364 0.158591 0.856806 11.00000 0.01202 0.01413 = 0.01451 0.00132 -0.00249 -0.00235 C20 1 0.225642 0.056048 0.872696 11.00000 0.02674 0.02713 = 0.02268 0.00463 -0.00714 -0.01584 AFIX 43 H20 2 0.190504 0.038696 0.811541 11.00000 -1.20000 AFIX 0 C21 1 0.206300 -0.021306 0.978384 11.00000 0.02932 0.02817 = 0.02941 0.01046 -0.00404 -0.01645 AFIX 43 H21 2 0.160281 -0.092902 0.988478 11.00000 -1.20000 AFIX 0 C22 1 0.253957 0.006023 1.068425 11.00000 0.02237 0.02490 = 0.01845 0.00819 0.00017 -0.00164 AFIX 43 H22 2 0.240089 -0.046403 1.140437 11.00000 -1.20000 AFIX 0 C23 1 0.321827 0.109635 1.053790 11.00000 0.02166 0.02169 = 0.01578 -0.00009 -0.00441 0.00204 AFIX 43 H23 2 0.352238 0.129765 1.116371 11.00000 -1.20000 AFIX 0 C24 1 0.345671 0.184358 0.947888 11.00000 0.01625 0.01491 = 0.01712 -0.00096 -0.00414 -0.00100 AFIX 43 H24 2 0.395575 0.253059 0.937423 11.00000 -1.20000 AFIX 0 B1 3 0.251041 0.190645 0.609361 11.00000 0.01704 0.01744 = 0.01801 -0.00108 -0.00735 -0.00906 H1A 2 0.314820 0.070612 0.611033 11.00000 -1.20000 H1B 2 0.123435 0.219233 0.658877 11.00000 -1.20000 HKLF 4 REM cu_20ERA01_0m in P-1 REM wR2 = 0.0632, GooF = S = 1.049, Restrained GooF = 1.049 for all data REM R1 = 0.0252 for 3904 Fo > 4sig(Fo) and 0.0257 for all 3986 data REM 250 parameters refined using 0 restraints END WGHT 0.0215 0.9841 REM Highest difference peak 0.410, deepest hole -0.531, 1-sigma level 0.055 Q1 1 0.1398 -0.1242 1.1267 11.00000 0.05 0.41 Q2 1 0.2828 0.3620 0.7262 11.00000 0.05 0.37 Q3 1 0.4479 0.2267 0.6989 11.00000 0.05 0.36 Q4 1 0.2752 0.2250 0.5434 11.00000 0.05 0.33 Q5 1 0.3207 0.4294 0.2033 11.00000 0.05 0.33 Q6 1 0.4098 0.4173 0.0985 11.00000 0.05 0.33 Q7 1 0.3100 0.1981 0.7950 11.00000 0.05 0.32 Q8 1 0.3396 0.2993 0.5929 11.00000 0.05 0.32 Q9 1 0.6999 0.2647 0.6795 11.00000 0.05 0.32 Q10 1 0.5776 0.2504 0.6782 11.00000 0.05 0.31 Q11 1 0.3732 0.3459 0.2759 11.00000 0.05 0.31 Q12 1 0.2235 0.3918 0.2810 11.00000 0.05 0.31 Q13 1 0.7265 0.0500 0.6296 11.00000 0.05 0.31 Q14 1 0.2461 0.4898 0.6859 11.00000 0.05 0.30 Q15 1 0.3289 0.1679 0.9013 11.00000 0.05 0.30 Q16 1 0.8267 0.0745 0.6194 11.00000 0.05 0.30 Q17 1 0.1941 0.4731 0.7826 11.00000 0.05 0.29 Q18 1 0.2998 0.2245 0.6606 11.00000 0.05 0.29 Q19 1 0.4209 0.4750 0.0610 11.00000 0.05 0.28 Q20 1 0.1303 0.5781 0.8449 11.00000 0.05 0.27 ; _shelx_res_checksum 71654 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br Br1 0.32328(2) 0.48490(2) 0.10590(2) 0.02829(7) Uani d 1 . . P P1 0.33317(4) 0.25085(4) 0.71649(3) 0.01089(9) Uani d 1 . . C C1 0.27423(18) 0.26888(16) 0.48269(13) 0.0138(3) Uani d 1 . . C C2 0.14369(18) 0.34670(17) 0.43727(14) 0.0159(3) Uani d 1 . . H H2 0.042212 0.357635 0.484672 0.019 Uiso calc 1 . . C C3 0.15653(19) 0.40865(17) 0.32563(14) 0.0184(3) Uani d 1 . . H H3 0.065679 0.459834 0.297054 0.022 Uiso calc 1 . . C C4 0.3039(2) 0.39432(17) 0.25703(14) 0.0183(3) Uani d 1 . . C C5 0.43797(19) 0.31845(17) 0.29691(14) 0.0185(3) Uani d 1 . . H H5 0.538792 0.308835 0.248898 0.022 Uiso calc 1 . . C C6 0.42157(18) 0.25669(17) 0.40878(14) 0.0170(3) Uani d 1 . . H H6 0.513121 0.204428 0.436253 0.020 Uiso calc 1 . . C C7 0.24868(17) 0.44382(16) 0.73670(13) 0.0130(3) Uani d 1 . . C C8 0.26936(18) 0.53691(17) 0.63964(13) 0.0159(3) Uani d 1 . . H H8 0.329205 0.498154 0.566921 0.019 Uiso calc 1 . . C C9 0.20268(19) 0.68562(17) 0.64938(14) 0.0180(3) Uani d 1 . . H H9 0.217521 0.748213 0.583525 0.022 Uiso calc 1 . . C C10 0.11435(19) 0.74256(17) 0.75545(15) 0.0199(3) Uani d 1 . . H H10 0.068703 0.844141 0.762101 0.024 Uiso calc 1 . . C C11 0.09272(19) 0.65123(18) 0.85174(15) 0.0207(3) Uani d 1 . . H H11 0.032144 0.690538 0.924145 0.025 Uiso calc 1 . . C C12 0.15934(18) 0.50237(17) 0.84270(14) 0.0169(3) Uani d 1 . . H H12 0.143978 0.440397 0.908890 0.020 Uiso calc 1 . . C C13 0.54478(17) 0.20455(16) 0.67799(12) 0.0116(3) Uani d 1 . . C C14 0.63650(18) 0.06484(16) 0.64157(13) 0.0140(3) Uani d 1 . . H H14 0.587565 0.001074 0.633363 0.017 Uiso calc 1 . . C C15 0.79873(18) 0.01938(16) 0.61745(13) 0.0149(3) Uani d 1 . . H H15 0.860611 -0.075613 0.593161 0.018 Uiso calc 1 . . C C16 0.87093(17) 0.11267(17) 0.62878(13) 0.0140(3) Uani d 1 . . H H16 0.981988 0.081366 0.612318 0.017 Uiso calc 1 . . C C17 0.78068(18) 0.25123(17) 0.66410(13) 0.0152(3) Uani d 1 . . H H17 0.830186 0.314913 0.671449 0.018 Uiso calc 1 . . C C18 0.61755(18) 0.29778(16) 0.68893(13) 0.0141(3) Uani d 1 . . H H18 0.556163 0.392851 0.713263 0.017 Uiso calc 1 . . C C19 0.29636(17) 0.15859(16) 0.85681(13) 0.0146(3) Uani d 1 . . C C20 0.2256(2) 0.0560(2) 0.87270(15) 0.0240(4) Uani d 1 . . H H20 0.190504 0.038696 0.811541 0.029 Uiso calc 1 . . C C21 0.2063(2) -0.0213(2) 0.97838(17) 0.0290(4) Uani d 1 . . H H21 0.160281 -0.092902 0.988478 0.035 Uiso calc 1 . . C C22 0.2540(2) 0.0060(2) 1.06842(15) 0.0261(4) Uani d 1 . . H H22 0.240089 -0.046403 1.140437 0.031 Uiso calc 1 . . C C23 0.3218(2) 0.10963(19) 1.05379(14) 0.0228(4) Uani d 1 . . H H23 0.352238 0.129765 1.116371 0.027 Uiso calc 1 . . C C24 0.34567(18) 0.18436(17) 0.94789(14) 0.0174(3) Uani d 1 . . H H24 0.395575 0.253059 0.937423 0.021 Uiso calc 1 . . B B1 0.2510(2) 0.19065(19) 0.60936(16) 0.0159(3) Uani d 1 . . H H1A 0.315(2) 0.071(2) 0.6110(17) 0.019 Uiso d 1 . . H H1B 0.123(2) 0.219(2) 0.6589(17) 0.019 Uiso d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br1 0.04593(13) 0.03054(12) 0.01421(10) -0.02059(9) -0.00767(8) 0.00151(7) P1 0.01051(17) 0.01121(17) 0.01213(18) -0.00479(13) -0.00335(13) -0.00028(13) C1 0.0168(7) 0.0119(7) 0.0162(7) -0.0067(6) -0.0053(6) -0.0039(6) C2 0.0155(7) 0.0151(7) 0.0194(8) -0.0066(6) -0.0048(6) -0.0037(6) C3 0.0216(8) 0.0168(8) 0.0214(8) -0.0077(6) -0.0113(6) 0.0000(6) C4 0.0295(9) 0.0163(7) 0.0140(7) -0.0120(7) -0.0069(6) -0.0014(6) C5 0.0195(8) 0.0189(8) 0.0185(8) -0.0095(6) -0.0007(6) -0.0057(6) C6 0.0157(7) 0.0160(7) 0.0204(8) -0.0049(6) -0.0061(6) -0.0034(6) C7 0.0106(6) 0.0128(7) 0.0171(7) -0.0039(5) -0.0062(6) -0.0001(6) C8 0.0159(7) 0.0184(8) 0.0147(7) -0.0066(6) -0.0050(6) -0.0004(6) C9 0.0204(8) 0.0167(8) 0.0200(8) -0.0086(6) -0.0097(6) 0.0046(6) C10 0.0188(8) 0.0130(7) 0.0268(9) -0.0014(6) -0.0096(7) -0.0011(6) C11 0.0187(8) 0.0189(8) 0.0192(8) -0.0002(6) -0.0035(6) -0.0044(6) C12 0.0154(7) 0.0168(8) 0.0162(8) -0.0032(6) -0.0050(6) 0.0014(6) C13 0.0119(7) 0.0130(7) 0.0107(7) -0.0050(5) -0.0035(5) 0.0000(5) C14 0.0162(7) 0.0127(7) 0.0155(7) -0.0068(6) -0.0048(6) -0.0011(6) C15 0.0151(7) 0.0119(7) 0.0157(7) -0.0029(6) -0.0027(6) -0.0022(6) C16 0.0117(7) 0.0169(7) 0.0128(7) -0.0051(6) -0.0025(5) 0.0006(6) C17 0.0157(7) 0.0162(7) 0.0167(7) -0.0098(6) -0.0034(6) -0.0003(6) C18 0.0144(7) 0.0116(7) 0.0163(7) -0.0045(6) -0.0034(6) -0.0020(6) C19 0.0120(7) 0.0141(7) 0.0145(7) -0.0023(6) -0.0025(6) 0.0013(6) C20 0.0267(9) 0.0271(9) 0.0227(9) -0.0158(7) -0.0071(7) 0.0046(7) C21 0.0293(9) 0.0282(9) 0.0294(10) -0.0165(8) -0.0040(8) 0.0105(8) C22 0.0224(8) 0.0249(9) 0.0185(8) -0.0016(7) 0.0002(7) 0.0082(7) C23 0.0217(8) 0.0217(8) 0.0158(8) 0.0020(7) -0.0044(6) -0.0001(6) C24 0.0162(7) 0.0149(7) 0.0171(8) -0.0010(6) -0.0041(6) -0.0010(6) B1 0.0170(8) 0.0174(8) 0.0180(8) -0.0091(7) -0.0073(7) -0.0011(7) 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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C19 P1 C7 . . 107.96(7) ? C19 P1 C13 . . 103.51(7) ? C7 P1 C13 . . 106.24(7) ? C19 P1 B1 . . 110.16(8) ? C7 P1 B1 . . 113.37(7) ? C13 P1 B1 . . 114.93(7) ? C2 C1 C6 . . 116.19(14) ? C2 C1 B1 . . 119.85(14) ? C6 C1 B1 . . 123.81(14) ? C3 C2 C1 . . 122.68(15) ? C3 C2 H2 . . 118.7 ? C1 C2 H2 . . 118.7 ? C4 C3 C2 . . 118.74(15) ? C4 C3 H3 . . 120.6 ? C2 C3 H3 . . 120.6 ? C3 C4 C5 . . 121.38(15) ? C3 C4 Br1 . . 119.30(13) ? C5 C4 Br1 . . 119.30(13) ? C4 C5 C6 . . 118.60(15) ? C4 C5 H5 . . 120.7 ? C6 C5 H5 . . 120.7 ? C5 C6 C1 . . 122.40(15) ? C5 C6 H6 . . 118.8 ? C1 C6 H6 . . 118.8 ? C12 C7 C8 . . 119.17(14) ? C12 C7 P1 . . 122.87(12) ? C8 C7 P1 . . 117.90(12) ? C9 C8 C7 . . 120.32(14) ? C9 C8 H8 . . 119.8 ? C7 C8 H8 . . 119.8 ? C10 C9 C8 . . 119.95(15) ? C10 C9 H9 . . 120.0 ? C8 C9 H9 . . 120.0 ? C11 C10 C9 . . 120.08(15) ? C11 C10 H10 . . 120.0 ? C9 C10 H10 . . 120.0 ? C10 C11 C12 . . 120.29(15) ? C10 C11 H11 . . 119.9 ? C12 C11 H11 . . 119.9 ? C11 C12 C7 . . 120.19(15) ? C11 C12 H12 . . 119.9 ? C7 C12 H12 . . 119.9 ? C18 C13 C14 . . 119.56(13) ? C18 C13 P1 . . 123.29(11) ? C14 C13 P1 . . 117.06(11) ? C15 C14 C13 . . 120.13(14) ? C15 C14 H14 . . 119.9 ? C13 C14 H14 . . 119.9 ? C14 C15 C16 . . 120.13(14) ? C14 C15 H15 . . 119.9 ? C16 C15 H15 . . 119.9 ? C17 C16 C15 . . 119.93(14) ? C17 C16 H16 . . 120.0 ? C15 C16 H16 . . 120.0 ? C16 C17 C18 . . 120.38(14) ? C16 C17 H17 . . 119.8 ? C18 C17 H17 . . 119.8 ? C13 C18 C17 . . 119.86(14) ? C13 C18 H18 . . 120.1 ? C17 C18 H18 . . 120.1 ? C20 C19 C24 . . 119.39(15) ? C20 C19 P1 . . 120.06(12) ? C24 C19 P1 . . 120.46(12) ? C19 C20 C21 . . 120.05(17) ? C19 C20 H20 . . 120.0 ? C21 C20 H20 . . 120.0 ? C22 C21 C20 . . 120.14(17) ? C22 C21 H21 . . 119.9 ? C20 C21 H21 . . 119.9 ? C21 C22 C23 . . 120.07(16) ? C21 C22 H22 . . 120.0 ? C23 C22 H22 . . 120.0 ? C22 C23 C24 . . 120.23(17) ? C22 C23 H23 . . 119.9 ? C24 C23 H23 . . 119.9 ? C23 C24 C19 . . 120.08(16) ? C23 C24 H24 . . 120.0 ? C19 C24 H24 . . 120.0 ? C1 B1 P1 . . 114.22(11) ? C1 B1 H1A . . 114.2(10) ? P1 B1 H1A . . 102.0(10) ? C1 B1 H1B . . 113.8(10) ? P1 B1 H1B . . 100.0(10) ? H1A B1 H1B . . 111.2(14) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Br1 C4 . 1.9062(16) ? P1 C19 . 1.8161(16) ? P1 C7 . 1.8175(15) ? P1 C13 . 1.8198(15) ? P1 B1 . 1.9444(18) ? C1 C2 . 1.400(2) ? C1 C6 . 1.408(2) ? C1 B1 . 1.609(2) ? C2 C3 . 1.391(2) ? C2 H2 . 0.9500 ? C3 C4 . 1.382(2) ? C3 H3 . 0.9500 ? C4 C5 . 1.388(2) ? C5 C6 . 1.392(2) ? C5 H5 . 0.9500 ? C6 H6 . 0.9500 ? C7 C12 . 1.395(2) ? C7 C8 . 1.403(2) ? C8 C9 . 1.391(2) ? C8 H8 . 0.9500 ? C9 C10 . 1.389(2) ? C9 H9 . 0.9500 ? C10 C11 . 1.388(2) ? C10 H10 . 0.9500 ? C11 C12 . 1.391(2) ? C11 H11 . 0.9500 ? C12 H12 . 0.9500 ? C13 C18 . 1.394(2) ? C13 C14 . 1.401(2) ? C14 C15 . 1.388(2) ? C14 H14 . 0.9500 ? C15 C16 . 1.391(2) ? C15 H15 . 0.9500 ? C16 C17 . 1.385(2) ? C16 H16 . 0.9500 ? C17 C18 . 1.395(2) ? C17 H17 . 0.9500 ? C18 H18 . 0.9500 ? C19 C20 . 1.392(2) ? C19 C24 . 1.397(2) ? C20 C21 . 1.395(2) ? C20 H20 . 0.9500 ? C21 C22 . 1.382(3) ? C21 H21 . 0.9500 ? C22 C23 . 1.383(3) ? C22 H22 . 0.9500 ? C23 C24 . 1.389(2) ? C23 H23 . 0.9500 ? C24 H24 . 0.9500 ? B1 H1A . 1.12(2) ? B1 H1B . 1.14(2) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C14 H14 Cg1 2_656 0.95 3.096 3.786 130.8 yes C15 H15 Cg1 2_656 0.95 3.305 3.890 121.8 yes C17 H17 Cg1 2_666 0.95 3.284 3.947 128.6 yes C18 H18 Cg1 2_666 0.95 3.486 4.047 120.1 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C6 C1 C2 C3 . . . . 0.3(2) ? B1 C1 C2 C3 . . . . -175.62(14) ? C1 C2 C3 C4 . . . . -0.8(2) ? C2 C3 C4 C5 . . . . 0.8(2) ? C2 C3 C4 Br1 . . . . -177.57(11) ? C3 C4 C5 C6 . . . . -0.3(2) ? Br1 C4 C5 C6 . . . . 178.03(11) ? C4 C5 C6 C1 . . . . -0.2(2) ? C2 C1 C6 C5 . . . . 0.2(2) ? B1 C1 C6 C5 . . . . 175.92(14) ? C19 P1 C7 C12 . . . . -5.66(15) ? C13 P1 C7 C12 . . . . -116.17(13) ? B1 P1 C7 C12 . . . . 116.67(13) ? C19 P1 C7 C8 . . . . 177.19(11) ? C13 P1 C7 C8 . . . . 66.69(13) ? B1 P1 C7 C8 . . . . -60.48(14) ? C12 C7 C8 C9 . . . . 0.5(2) ? P1 C7 C8 C9 . . . . 177.80(12) ? C7 C8 C9 C10 . . . . -0.4(2) ? C8 C9 C10 C11 . . . . 0.1(2) ? C9 C10 C11 C12 . . . . 0.1(2) ? C10 C11 C12 C7 . . . . 0.1(2) ? C8 C7 C12 C11 . . . . -0.4(2) ? P1 C7 C12 C11 . . . . -177.52(12) ? C19 P1 C13 C18 . . . . -101.16(13) ? C7 P1 C13 C18 . . . . 12.44(15) ? B1 P1 C13 C18 . . . . 138.67(13) ? C19 P1 C13 C14 . . . . 75.38(13) ? C7 P1 C13 C14 . . . . -171.02(11) ? B1 P1 C13 C14 . . . . -44.80(14) ? C18 C13 C14 C15 . . . . 0.5(2) ? P1 C13 C14 C15 . . . . -176.17(12) ? C13 C14 C15 C16 . . . . -0.3(2) ? C14 C15 C16 C17 . . . . -0.1(2) ? C15 C16 C17 C18 . . . . 0.3(2) ? C14 C13 C18 C17 . . . . -0.3(2) ? P1 C13 C18 C17 . . . . 176.18(12) ? C16 C17 C18 C13 . . . . -0.1(2) ? C7 P1 C19 C20 . . . . 127.27(13) ? C13 P1 C19 C20 . . . . -120.37(14) ? B1 P1 C19 C20 . . . . 2.99(16) ? C7 P1 C19 C24 . . . . -55.97(14) ? C13 P1 C19 C24 . . . . 56.38(14) ? B1 P1 C19 C24 . . . . 179.75(12) ? C24 C19 C20 C21 . . . . -0.8(3) ? P1 C19 C20 C21 . . . . 175.98(14) ? C19 C20 C21 C22 . . . . 1.5(3) ? C20 C21 C22 C23 . . . . -0.4(3) ? C21 C22 C23 C24 . . . . -1.5(3) ? C22 C23 C24 C19 . . . . 2.2(2) ? C20 C19 C24 C23 . . . . -1.0(2) ? P1 C19 C24 C23 . . . . -177.78(12) ? C2 C1 B1 P1 . . . . -122.51(13) ? C6 C1 B1 P1 . . . . 61.93(18) ? _cod_database_fobs_code 2022690