#------------------------------------------------------------------------------ #$Date: 2021-10-14 05:28:04 +0300 (Thu, 14 Oct 2021) $ #$Revision: 269937 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/39/2243934.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_2243934 loop_ _publ_author_name 'Poirot, Alexandre' 'Saffon-Merceron, Nathalie' 'Leygue, Nadine' 'Benoist, Eric' 'Fery-Forgues, Suzanne' _publ_section_title ; Crystal structure of methyl 1,3-benzoxazole-2-carboxylate ; _journal_coeditor_code DJ2033 _journal_issue 11 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first ; ; _journal_paper_doi 10.1107/S2056989021010094 _journal_volume 77 _journal_year 2021 _chemical_formula_iupac 'C9 H7 N O3' _chemical_formula_moiety 'C9 H7 N O3' _chemical_formula_sum 'C9 H7 N O3' _chemical_formula_weight 177.16 _chemical_name_systematic ; Methyl 1,3-benzoxazole-2-carboxylate ; _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 95.1319(16) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 6.8165(3) _cell_length_b 4.4676(2) _cell_length_c 13.2879(6) _cell_measurement_reflns_used 6695 _cell_measurement_temperature 193(2) _cell_measurement_theta_max 28.20 _cell_measurement_theta_min 3.25 _cell_volume 403.04(3) _computing_cell_refinement ; SAINT (Bruker, 2018) ; _computing_data_collection ; APEX3 (Bruker, 2018) ; _computing_data_reduction ; SAINT (Bruker, 2018) ; _computing_molecular_graphics ; SHELXTL (Sheldrick, 2008) and Mercury (Macrae et al, 2020) ; _computing_publication_material ; Platon (Spek 2020) and publCIF (Westrip 2010) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 193(2) _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'Bruker D8-Venture Photon III detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_unetI/netI 0.0176 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 9084 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.285 _diffrn_reflns_theta_min 3.248 _diffrn_source 'Fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.112 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6976 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.460 _exptl_crystal_description plate _exptl_crystal_F_000 184 _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.196 _refine_diff_density_min -0.156 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 119 _refine_ls_number_reflns 1954 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.099 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0299 _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^)+(0.0432P)^2^+0.0403P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0749 _refine_ls_wR_factor_ref 0.0767 _reflns_number_gt 1860 _reflns_number_total 1954 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL ALP078Pdep_a.res in P2(1) ALP078Pdep_a.res created by SHELXL-2018/3 at 10:57:09 on 17-Dec-2020 CELL 0.71073 6.81650 4.46760 13.28790 90.0000 95.1319 90.0000 ZERR 2.00 0.00030 0.00020 0.00060 0.0000 0.0016 0.0000 LATT -1 SYMM -X, 1/2+Y, -Z SFAC C H N O UNIT 18 14 2 6 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 CONF SIZE 0.10 0.30 0.40 TEMP -80.150 WGHT 0.043200 0.040300 FVAR 0.99898 O1 4 0.252546 0.388465 0.699334 11.00000 0.02589 0.03617 = 0.03589 0.00011 -0.00132 -0.00641 O2 4 0.439814 -0.000355 0.579929 11.00000 0.04056 0.03487 = 0.03798 -0.00349 -0.00237 -0.00870 O3 4 0.732199 0.201715 0.638332 11.00000 0.03154 0.03415 = 0.03636 -0.00613 0.00089 -0.00249 N1 3 0.545407 0.549335 0.771768 11.00000 0.02409 0.02741 = 0.03118 0.00016 0.00078 -0.00170 C1 1 0.452771 0.378886 0.704732 11.00000 0.02876 0.02860 = 0.03112 0.00484 0.00068 -0.00478 C2 1 0.537799 0.170273 0.632943 11.00000 0.03289 0.02642 = 0.02916 0.00388 -0.00062 -0.00419 C3 1 0.831903 0.012452 0.570154 11.00000 0.03841 0.03805 = 0.03812 -0.00421 0.00468 0.00300 AFIX 137 H3A 2 0.794777 -0.196824 0.579791 11.00000 -1.50000 H3B 2 0.974729 0.034297 0.584461 11.00000 -1.50000 H3C 2 0.793506 0.072127 0.500188 11.00000 -1.50000 AFIX 0 C4 1 0.214894 0.591900 0.772642 11.00000 0.02587 0.03046 = 0.03077 0.00626 0.00105 -0.00494 C5 1 0.394738 0.691909 0.817788 11.00000 0.02326 0.02784 = 0.03057 0.00570 0.00128 -0.00192 C6 1 0.401375 0.900864 0.896072 11.00000 0.03108 0.03566 = 0.03658 -0.00138 -0.00060 -0.00299 AFIX 43 H6 2 0.522730 0.971603 0.928121 11.00000 -1.20000 AFIX 0 C7 1 0.222035 0.999823 0.924649 11.00000 0.04378 0.03699 = 0.04073 -0.00147 0.00963 0.00195 AFIX 43 H7 2 0.220300 1.141802 0.977785 11.00000 -1.20000 AFIX 0 C8 1 0.042899 0.895914 0.877195 11.00000 0.03018 0.04310 = 0.05050 0.01073 0.01457 0.00398 AFIX 43 H8 2 -0.076652 0.971435 0.898830 11.00000 -1.20000 AFIX 0 C9 1 0.034154 0.687837 0.800181 11.00000 0.02199 0.04290 = 0.04607 0.01036 0.00315 -0.00350 AFIX 43 H9 2 -0.087048 0.615698 0.768384 11.00000 -1.20000 AFIX 0 HKLF 4 REM ALP078Pdep_a.res in P2(1) REM wR2 = 0.076735, GooF = S = 1.09961, Restrained GooF = 1.09931 for all data REM R1 = 0.029859 for 1860 Fo > 4sig(Fo) and 0.031945 for all 1954 data REM 119 parameters refined using 1 restraints END WGHT 0.0432 0.0403 REM Highest difference peak 0.196, deepest hole -0.156, 1-sigma level 0.029 Q1 1 0.4932 0.3102 0.6637 11.00000 0.05 0.20 Q2 1 0.2940 0.6651 0.8043 11.00000 0.05 0.19 Q3 1 0.5154 0.5114 0.7206 11.00000 0.05 0.16 Q4 1 0.3956 0.8163 0.8448 11.00000 0.05 0.15 Q5 1 0.1320 0.7085 0.7804 11.00000 0.05 0.13 Q6 1 0.4820 0.6297 0.7967 11.00000 0.05 0.13 Q7 1 0.5020 0.4015 0.7545 11.00000 0.05 0.13 Q8 1 0.0423 0.7268 0.8612 11.00000 0.05 0.13 Q9 1 0.1290 0.5946 0.7988 11.00000 0.05 0.12 Q10 1 0.1363 0.9628 0.8842 11.00000 0.05 0.11 Q11 1 0.4969 0.0182 0.6336 11.00000 0.05 0.11 Q12 1 0.3715 0.3867 0.6945 11.00000 0.05 0.11 Q13 1 0.3021 0.9033 0.9183 11.00000 0.05 0.10 Q14 1 0.4818 0.1639 0.5835 11.00000 0.05 0.10 Q15 1 0.3157 0.9904 0.8985 11.00000 0.05 0.10 Q16 1 0.6403 0.2491 0.6229 11.00000 0.05 0.10 Q17 1 0.7653 0.2148 0.6987 11.00000 0.05 0.10 Q18 1 0.8413 0.1041 0.5105 11.00000 0.05 0.10 Q19 1 0.6033 0.4888 0.7994 11.00000 0.05 0.10 Q20 1 0.0562 0.8800 0.8084 11.00000 0.05 0.08 ; _cod_data_source_file dj2033sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 2243934 _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 0.957 _shelx_estimated_absorpt_t_max 0.989 _shelx_hkl_file ; 2 0 0 63.86 1.38 2 0 0 62.05 1.37 2 0 0 62.52 1.42 -2 0 0 59.70 1.38 -2 0 0 63.14 1.42 -2 0 0 60.78 1.37 3 0 0 214.91 4.54 -3 0 0 218.40 4.61 3 0 0 212.64 4.62 -3 0 0 217.56 4.53 3 0 0 215.77 4.54 3 0 0 215.41 4.60 -3 0 0 217.78 4.54 4 0 0 529.81 10.99 4 0 0 525.54 11.01 4 0 0 527.84 10.89 -4 0 0 526.79 10.89 5 0 0 113.76 2.67 5 0 0 112.36 2.55 -5 0 0 111.68 2.54 -5 0 0 106.74 2.81 5 0 0 114.96 2.57 5 0 0 113.28 2.71 -5 0 0 114.99 2.54 6 0 0 124.04 2.86 -6 0 0 122.29 2.84 -6 0 0 124.87 3.01 6 0 0 126.07 3.01 6 0 0 126.07 3.07 -6 0 0 127.48 2.84 -7 0 0 8.91 0.51 -7 0 0 8.73 0.50 7 0 0 8.25 0.66 -7 0 0 8.72 0.68 7 0 0 7.80 0.54 7 0 0 8.66 0.73 -8 0 0 1.95 0.43 8 0 0 2.64 0.36 8 0 0 1.73 0.48 8 0 0 2.16 0.48 9 0 0 0.34 0.36 9 0 0 0.33 0.27 9 0 0 0.31 0.44 0 -1 0 0.37 0.14 0 -1 0 0.14 0.12 0 -1 0 0.26 0.14 0 -1 0 0.19 0.14 0 1 0 0.28 0.14 0 1 0 0.67 0.14 0 1 0 0.17 0.13 0 1 0 0.11 0.13 -2 -1 0 237.92 5.16 -2 -1 0 246.54 5.17 2 -1 0 246.65 5.07 2 1 0 235.93 5.01 -3 -1 0 438.60 9.12 3 -1 0 434.26 9.05 3 1 0 429.69 8.99 -4 -1 0 20.95 0.76 4 -1 0 19.45 0.67 -4 -1 0 21.75 0.77 4 -1 0 21.30 0.85 4 1 0 21.28 0.78 4 1 0 21.16 0.80 4 1 0 20.72 0.76 4 1 0 21.13 0.79 -5 -1 0 22.06 0.80 -5 -1 0 20.42 0.86 -5 -1 0 18.82 0.80 5 -1 0 21.62 0.83 5 1 0 21.68 0.87 5 1 0 20.35 0.83 5 1 0 21.51 0.87 5 1 0 19.74 0.91 6 -1 0 33.97 1.09 -6 -1 0 34.53 1.23 6 -1 0 35.40 1.19 -6 -1 0 31.25 1.12 6 1 0 33.09 1.21 6 1 0 33.87 1.14 6 1 0 32.88 1.20 6 1 0 33.53 1.15 -7 -1 0 1.84 0.40 -7 -1 0 1.96 0.48 -7 -1 0 2.80 0.41 7 -1 0 3.28 0.52 7 -1 0 1.69 0.35 7 -1 0 2.10 0.45 7 1 0 2.42 0.41 7 1 0 1.38 0.42 7 1 0 2.70 0.45 7 1 0 3.16 0.50 -8 -1 0 21.36 0.91 8 -1 0 21.18 1.06 8 -1 0 18.76 1.05 8 -1 0 20.29 0.91 8 1 0 19.98 1.10 8 1 0 20.03 0.93 8 1 0 20.68 1.06 0 -2 0 313.52 6.51 0 -2 0 308.54 6.47 0 -2 0 303.38 6.50 0 2 0 313.21 6.52 0 2 0 306.21 6.52 -1 -2 0 37.30 1.06 1 -2 0 37.65 0.97 1 -2 0 37.20 0.98 -1 -2 0 39.20 1.09 -1 -2 0 38.22 1.09 1 -2 0 39.43 1.04 -1 -2 0 37.88 1.09 1 -2 0 37.26 0.98 1 2 0 38.75 0.93 -1 2 0 39.19 1.05 1 2 0 37.44 1.10 1 2 0 37.85 1.07 -1 2 0 38.61 1.00 1 2 0 37.17 1.08 -1 2 0 39.18 1.00 1 2 0 39.81 1.10 -2 -2 0 9.12 0.53 2 -2 0 9.20 0.37 2 -2 0 9.59 0.38 -2 -2 0 10.28 0.56 2 -2 0 10.04 0.48 -2 -2 0 9.21 0.55 2 2 0 9.92 0.56 -2 2 0 9.17 0.48 2 2 0 9.57 0.45 2 2 0 9.89 0.55 2 2 0 9.85 0.55 -3 -2 0 210.03 4.74 3 -2 0 220.24 4.51 3 -2 0 214.99 4.66 -3 -2 0 207.96 4.74 -3 -2 0 213.16 4.74 3 2 0 215.47 4.71 3 2 0 207.89 4.67 3 2 0 202.41 4.73 3 2 0 213.88 4.68 3 2 0 212.06 4.71 4 -2 0 0.57 0.19 4 -2 0 0.50 0.25 4 -2 0 0.45 0.21 -4 -2 0 0.24 0.28 -4 -2 0 0.22 0.28 -4 -2 0 0.79 0.30 4 2 0 0.62 0.31 4 2 0 0.36 0.28 4 2 0 0.19 0.28 4 2 0 0.42 0.26 4 2 0 0.20 0.28 -5 -2 0 17.21 0.91 5 -2 0 19.81 0.77 5 -2 0 19.67 0.70 -5 -2 0 18.32 0.89 -5 -2 0 19.35 0.90 5 -2 0 20.04 0.86 5 2 0 17.39 0.90 5 2 0 20.19 0.92 5 2 0 18.13 0.90 5 2 0 21.03 0.89 5 2 0 18.14 0.88 -6 -2 0 5.80 0.72 -6 -2 0 5.52 0.58 -6 -2 0 5.27 0.57 6 -2 0 5.61 0.51 6 -2 0 5.59 0.45 6 -2 0 6.36 0.62 6 2 0 5.67 0.58 6 2 0 5.70 0.61 6 2 0 5.98 0.61 6 2 0 5.37 0.64 6 2 0 5.64 0.59 7 -2 0 1.55 0.50 -7 -2 0 1.21 0.39 7 -2 0 1.86 0.42 7 -2 0 1.28 0.30 7 2 0 1.19 0.42 7 2 0 1.55 0.45 7 2 0 1.46 0.44 7 2 0 1.39 0.45 8 -2 0 12.49 0.88 8 -2 0 12.63 0.68 8 -2 0 14.30 0.88 -8 -2 0 13.41 0.83 8 2 0 12.08 0.92 8 2 0 14.56 0.87 8 2 0 13.66 0.94 8 2 0 12.78 0.89 0 -3 0 0.15 0.22 0 -3 0 -0.10 0.22 0 -3 0 0.13 0.24 0 -3 0 -0.13 0.22 0 3 0 0.14 0.23 0 3 0 -0.01 0.22 0 3 0 0.06 0.22 -1 -3 0 194.31 4.35 -1 -3 0 196.04 4.39 1 -3 0 196.08 4.34 1 -3 0 196.38 4.26 -1 -3 0 192.83 4.39 1 -3 0 189.88 4.28 1 -3 0 194.02 4.28 -1 -3 0 198.56 4.39 1 3 0 197.80 4.44 1 3 0 201.80 4.41 -1 3 0 195.76 4.32 -1 3 0 200.30 4.40 1 3 0 195.82 4.44 1 3 0 193.00 4.43 2 -3 0 149.85 3.31 -2 -3 0 146.43 3.49 -2 -3 0 146.67 3.53 -2 -3 0 147.90 3.54 2 -3 0 152.17 3.32 2 -3 0 154.66 3.45 2 -3 0 151.89 3.33 2 3 0 148.90 3.27 2 3 0 149.88 3.52 -2 3 0 150.72 3.29 -2 3 0 148.81 3.46 -2 3 0 146.82 3.27 2 3 0 149.27 3.52 2 3 0 146.18 3.52 2 3 0 153.40 3.50 -3 -3 0 11.72 0.70 -3 -3 0 11.38 0.73 3 -3 0 9.94 0.60 -3 -3 0 11.03 0.72 -3 3 0 10.20 0.62 3 3 0 10.76 0.71 3 3 0 9.69 0.68 3 3 0 11.29 0.58 3 3 0 11.71 0.71 3 3 0 11.06 0.73 4 -3 0 38.09 1.07 4 -3 0 38.37 1.24 -4 -3 0 39.48 1.37 -4 -3 0 35.83 1.32 -4 -3 0 37.03 1.36 4 3 0 38.69 1.35 4 3 0 37.56 1.19 4 3 0 36.54 1.52 4 3 0 37.81 1.36 4 3 0 36.16 1.32 -5 -3 0 172.57 4.18 -5 -3 0 172.16 4.17 5 -3 0 170.24 4.02 -5 -3 0 166.04 4.15 5 3 0 169.84 4.07 5 3 0 144.33 4.84 5 3 0 174.45 4.83 5 3 0 159.72 4.06 5 3 0 174.71 3.91 6 -3 0 42.72 1.47 -6 -3 0 41.93 1.99 6 -3 0 42.14 1.21 -6 -3 0 43.40 1.65 6 -3 0 43.80 1.28 6 3 0 42.14 1.46 6 3 0 41.70 1.58 6 3 0 41.37 1.57 7 -3 0 0.53 0.30 -7 -3 0 1.10 0.47 7 -3 0 0.55 0.34 7 3 0 0.21 0.37 7 3 0 0.93 0.47 7 3 0 1.17 0.83 7 3 0 0.21 0.38 0 -4 0 63.73 1.81 0 -4 0 61.24 1.79 0 -4 0 61.72 1.79 0 -4 0 61.75 1.74 0 4 0 65.62 1.83 0 4 0 62.09 1.80 0 4 0 62.29 1.82 -1 -4 0 0.82 0.38 1 -4 0 0.79 0.31 1 -4 0 1.58 0.40 -1 -4 0 1.50 0.41 -1 -4 0 1.27 0.36 -1 -4 0 1.22 0.39 1 -4 0 0.77 0.31 1 -4 0 1.08 0.34 -1 4 0 1.19 0.34 1 4 0 0.97 0.37 1 4 0 1.09 0.39 1 4 0 0.76 0.36 -1 4 0 0.87 0.33 2 -4 0 4.63 0.45 -2 -4 0 3.38 0.49 2 -4 0 4.04 0.48 2 -4 0 3.89 0.43 -2 -4 0 3.88 0.54 2 -4 0 4.18 0.42 -2 -4 0 3.34 0.50 2 4 0 3.64 0.53 2 4 0 3.01 0.45 -2 4 0 4.25 0.42 2 4 0 3.29 0.49 -2 4 0 4.08 0.40 2 4 0 2.16 0.89 -2 4 0 3.80 0.46 -3 -4 0 24.65 1.16 -3 -4 0 24.12 1.14 3 -4 0 22.83 0.83 3 -4 0 23.67 0.84 3 -4 0 22.41 1.07 -3 -4 0 25.73 1.19 3 -4 0 22.20 0.98 3 4 0 23.12 1.11 -3 4 0 24.66 1.02 3 4 0 25.24 1.17 3 4 0 20.11 1.70 3 4 0 25.14 0.88 3 4 0 25.03 1.15 -4 -4 0 4.59 0.71 4 -4 0 5.70 0.60 -4 -4 0 6.16 0.69 -4 -4 0 4.06 0.64 4 4 0 4.59 0.64 4 4 0 5.41 0.65 4 4 0 5.15 0.68 4 4 0 5.46 0.52 4 4 0 5.45 0.70 -5 -4 0 0.77 0.46 -5 -4 0 0.71 0.45 5 -4 0 0.86 0.38 5 4 0 0.99 0.40 5 4 0 1.13 0.46 5 4 0 0.99 0.48 5 4 0 1.49 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12.22 1.02 4 0 15 12.41 1.03 4 0 15 12.32 1.00 -4 0 -15 13.46 0.72 5 -1 -15 2.38 0.51 -5 -1 15 2.19 0.54 5 -1 -15 1.71 0.52 5 1 -15 2.14 0.51 -5 1 15 2.46 0.59 5 1 -15 2.09 0.42 -4 -1 15 6.33 0.74 4 -1 -15 4.89 0.67 4 -1 -15 6.28 0.68 -4 1 15 5.15 0.63 4 1 -15 8.29 0.67 4 1 -15 5.81 0.72 4 1 -15 6.90 0.73 -3 -1 15 16.64 1.13 3 -1 -15 17.90 1.03 -3 -1 15 19.67 0.94 3 -1 -15 16.96 1.06 3 1 -15 17.74 1.03 3 1 -15 18.00 1.09 3 1 -15 19.12 0.91 -3 1 15 19.13 1.07 -2 -1 15 0.35 0.50 -2 -1 15 1.72 0.43 2 -1 -15 0.70 0.43 2 1 -15 0.50 0.35 2 1 -15 0.60 0.43 2 1 -15 0.46 0.35 -1 -1 15 10.43 0.87 -1 -1 15 8.19 0.82 -1 -1 15 8.89 0.77 1 -1 -15 9.27 0.84 1 1 -15 7.63 0.87 1 1 -15 8.69 0.75 1 1 -15 8.87 0.70 0 -1 15 4.94 0.73 0 -1 15 5.77 0.66 0 -1 -15 5.35 0.68 0 -1 15 6.13 0.87 0 1 -15 5.61 0.73 0 1 15 5.43 0.83 0 1 -15 4.86 0.52 0 1 15 6.42 0.58 1 -1 15 21.46 1.14 -1 -1 -15 19.48 1.45 1 -1 15 26.28 1.26 1 1 15 23.78 1.25 -1 1 -15 24.40 0.96 1 1 15 23.77 1.02 -1 1 -15 23.39 1.22 1 1 15 22.21 1.15 2 -1 15 12.98 1.02 2 -1 15 15.01 1.00 2 -1 15 11.67 0.93 -2 -1 -15 14.11 1.04 -2 -1 -15 15.04 0.89 -2 1 -15 12.63 0.99 2 1 15 18.87 1.09 2 1 15 14.46 0.91 -2 1 -15 13.00 0.70 2 1 15 14.39 0.99 -2 1 -15 13.63 0.70 -3 -1 -15 13.76 0.96 3 -1 15 13.53 0.98 -3 -1 -15 15.30 1.08 3 -1 15 12.79 0.96 3 -1 15 13.58 1.02 -3 1 -15 14.16 1.03 3 1 15 15.18 1.08 3 1 15 14.51 0.95 3 1 15 12.25 0.97 -4 -2 15 6.26 0.83 4 -2 -15 5.66 0.74 -4 -2 15 5.41 0.67 4 -2 -15 5.54 0.66 4 2 -15 4.61 0.67 4 2 -15 5.65 0.68 -4 2 15 5.22 0.75 -3 -2 15 6.36 0.75 -3 -2 15 6.00 0.69 3 -2 -15 4.91 0.63 3 2 -15 4.51 0.63 3 2 -15 6.15 0.76 -2 -2 15 2.43 0.59 -2 -2 15 3.73 0.69 2 -2 -15 2.56 0.50 2 2 -15 3.15 0.51 2 2 -15 2.00 0.56 -1 -2 15 4.46 0.99 -1 -2 15 3.94 0.64 -1 -2 15 5.58 0.73 1 -2 -15 4.11 0.61 1 2 -15 4.81 0.68 1 2 -15 4.69 0.53 0 -2 15 1.74 0.57 0 -2 15 1.62 0.55 0 -2 -15 1.11 0.47 0 -2 15 1.44 0.54 0 2 -15 2.08 0.54 0 2 -15 2.08 0.40 -1 -2 -15 2.00 0.51 1 -2 15 1.33 0.51 -1 -2 -15 0.76 0.46 1 -2 15 1.20 0.55 1 -2 15 1.73 0.52 -1 2 -15 0.75 0.44 -2 -2 -15 11.39 0.97 2 -2 15 9.66 0.96 -2 -2 -15 10.44 0.90 2 -2 15 10.38 0.97 2 -2 15 9.72 0.90 2 2 15 12.65 0.80 -2 2 -15 12.53 0.96 2 2 15 10.67 0.90 3 -2 15 2.38 0.61 -3 -2 -15 3.02 0.62 3 -2 15 1.55 0.93 3 -2 15 1.51 0.73 3 -2 15 1.07 0.52 -3 2 -15 2.97 0.57 3 2 15 1.02 0.50 3 2 15 1.53 0.81 -2 -3 15 11.28 1.06 2 -3 -15 11.45 0.88 -2 -3 15 10.83 0.97 2 3 -15 10.94 0.99 2 3 -15 11.76 0.80 -1 -3 15 -0.63 0.44 -1 -3 15 -0.93 0.43 1 -3 -15 -0.17 0.38 -1 -3 15 -0.47 0.43 1 3 -15 -0.67 0.66 1 3 -15 0.05 0.32 0 -3 -15 0.95 0.48 0 -3 15 0.51 0.50 0 -3 -15 0.51 0.44 0 -3 15 0.98 0.55 0 -3 15 0.23 0.77 0 3 -15 0.91 0.49 4 0 -16 0.77 0.44 4 0 -16 0.51 0.38 -4 0 16 1.01 0.48 3 0 -16 5.52 0.70 -3 0 16 5.79 0.76 3 0 -16 6.15 0.72 -2 0 16 6.94 0.56 2 0 -16 5.74 0.65 -2 0 16 7.88 0.81 2 0 -16 7.12 0.78 1 0 -16 0.80 0.40 1 0 -16 0.65 0.46 -1 0 16 1.96 0.45 0 0 -16 5.35 0.75 0 0 -16 4.61 0.58 0 0 16 5.30 0.61 1 0 16 0.60 0.51 1 0 16 0.20 0.43 -2 0 -16 6.46 0.85 2 0 16 5.61 0.69 -2 0 -16 5.16 0.70 2 0 16 6.07 0.70 2 0 16 6.04 0.74 3 0 16 0.71 0.52 -3 0 -16 0.35 0.48 3 0 16 0.63 0.46 -3 0 -16 0.06 0.40 3 0 16 -0.04 0.50 4 -1 -16 20.22 1.55 4 -1 -16 23.24 1.23 -4 -1 16 26.52 1.32 4 1 -16 24.15 1.33 4 1 -16 28.97 1.07 4 1 -16 25.13 1.27 -4 1 16 25.08 1.20 3 -1 -16 11.27 0.92 -3 -1 16 12.07 0.80 3 -1 -16 11.54 0.92 -3 -1 16 13.06 1.03 -3 1 16 11.44 0.90 3 1 -16 14.14 0.79 3 1 -16 12.10 0.90 3 1 -16 11.57 0.95 -2 -1 16 1.29 0.44 2 -1 -16 1.15 0.47 2 -1 -16 1.13 0.44 -2 -1 16 0.11 0.48 2 1 -16 1.61 0.41 2 1 -16 0.82 0.40 2 1 -16 0.90 0.45 -1 -1 16 1.41 0.48 -1 -1 16 2.38 0.61 1 -1 -16 1.32 0.49 1 1 -16 1.49 0.52 1 1 -16 1.74 0.43 0 -1 16 6.96 1.23 0 -1 -16 6.19 0.77 0 -1 16 7.24 0.77 0 -1 16 8.50 0.80 0 1 -16 6.92 0.66 0 1 16 7.46 0.62 1 -1 16 2.27 0.62 -1 -1 -16 0.22 0.44 1 -1 16 0.12 0.51 1 -1 16 0.04 0.45 -1 1 -16 0.43 0.33 1 1 16 0.60 0.41 -1 1 -16 0.63 0.48 2 -1 16 12.64 1.01 2 -1 16 12.39 0.99 -2 -1 -16 13.52 1.07 2 1 16 9.57 1.26 2 1 16 11.86 0.97 -2 1 -16 10.19 0.97 -2 1 -16 12.76 0.68 -2 1 -16 12.53 0.66 -3 -2 16 2.38 0.52 -3 -2 16 0.97 0.57 3 -2 -16 2.16 0.53 3 -2 -16 1.58 0.53 3 2 -16 1.84 0.49 3 2 -16 1.64 0.55 2 -2 -16 14.64 1.02 -2 -2 16 14.07 1.00 -2 -2 16 13.60 1.75 2 2 -16 15.08 1.09 2 2 -16 14.64 0.92 1 -2 -16 23.55 1.28 -1 -2 16 26.30 1.28 -1 -2 16 25.79 1.38 1 2 -16 24.54 1.09 1 2 -16 22.48 1.28 0 -2 16 4.07 0.60 0 -2 -16 3.70 0.57 0 -2 16 2.49 0.60 0 -2 -16 2.62 0.56 0 -2 16 2.14 0.65 0 2 -16 3.71 0.44 0 2 -16 2.48 0.63 -1 -2 -16 2.52 0.57 -1 -2 -16 1.74 0.55 1 -2 16 3.65 0.97 1 -2 16 1.94 0.57 1 -2 16 1.63 0.61 -1 2 -16 1.11 0.51 3 0 -17 1.60 0.50 -3 0 17 3.23 0.62 3 0 -17 2.09 0.57 2 0 -17 1.02 0.49 2 0 -17 1.09 0.43 -2 0 17 1.29 0.56 -1 0 17 9.99 0.73 1 0 -17 7.07 0.80 -1 0 17 11.23 1.00 1 0 -17 8.42 0.78 0 0 17 32.11 1.28 0 0 -17 32.04 1.50 0 0 -17 31.88 1.32 -1 0 -17 16.77 1.16 1 0 17 19.73 1.05 -1 0 -17 16.52 0.95 -2 -1 17 1.75 0.68 2 -1 -17 0.59 0.42 -2 -1 17 0.14 0.52 2 -1 -17 0.91 0.47 2 1 -17 0.08 0.42 2 1 -17 1.02 0.40 1 -1 -17 7.14 0.78 -1 -1 17 8.59 0.83 -1 -1 17 8.69 1.27 1 1 -17 8.47 0.74 1 1 -17 8.89 0.89 0 -1 17 16.93 1.22 0 -1 -17 17.94 1.15 0 -1 17 16.88 1.04 0 1 -17 16.44 1.14 0 1 -17 16.33 0.91 1 -1 17 2.44 0.60 1 -1 17 2.12 0.65 -1 -1 -17 2.45 0.58 1 1 17 2.26 0.48 -1 1 -17 2.66 0.61 -1 1 -17 2.12 0.40 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 38264 _shelx_res_file ; TITL ALP078Pdep_a.res in P2(1) ALP078Pdep_a.res created by SHELXL-2018/3 at 10:57:09 on 17-Dec-2020 CELL 0.71073 6.81650 4.46760 13.28790 90.0000 95.1319 90.0000 ZERR 2.00 0.00030 0.00020 0.00060 0.0000 0.0016 0.0000 LATT -1 SYMM -X, 1/2+Y, -Z SFAC C H N O UNIT 18 14 2 6 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 CONF SIZE 0.10 0.30 0.40 TEMP -80.150 WGHT 0.043200 0.040300 FVAR 0.99898 O1 4 0.252546 0.388465 0.699334 11.00000 0.02589 0.03617 = 0.03589 0.00011 -0.00132 -0.00641 O2 4 0.439814 -0.000355 0.579929 11.00000 0.04056 0.03487 = 0.03798 -0.00349 -0.00237 -0.00870 O3 4 0.732199 0.201715 0.638332 11.00000 0.03154 0.03415 = 0.03636 -0.00613 0.00089 -0.00249 N1 3 0.545407 0.549335 0.771768 11.00000 0.02409 0.02741 = 0.03118 0.00016 0.00078 -0.00170 C1 1 0.452771 0.378886 0.704732 11.00000 0.02876 0.02860 = 0.03112 0.00484 0.00068 -0.00478 C2 1 0.537799 0.170273 0.632943 11.00000 0.03289 0.02642 = 0.02916 0.00388 -0.00062 -0.00419 C3 1 0.831903 0.012452 0.570154 11.00000 0.03841 0.03805 = 0.03812 -0.00421 0.00468 0.00300 AFIX 137 H3A 2 0.794777 -0.196824 0.579791 11.00000 -1.50000 H3B 2 0.974729 0.034297 0.584461 11.00000 -1.50000 H3C 2 0.793506 0.072127 0.500188 11.00000 -1.50000 AFIX 0 C4 1 0.214894 0.591900 0.772642 11.00000 0.02587 0.03046 = 0.03077 0.00626 0.00105 -0.00494 C5 1 0.394738 0.691909 0.817788 11.00000 0.02326 0.02784 = 0.03057 0.00570 0.00128 -0.00192 C6 1 0.401375 0.900864 0.896072 11.00000 0.03108 0.03566 = 0.03658 -0.00138 -0.00060 -0.00299 AFIX 43 H6 2 0.522730 0.971603 0.928121 11.00000 -1.20000 AFIX 0 C7 1 0.222035 0.999823 0.924649 11.00000 0.04378 0.03699 = 0.04073 -0.00147 0.00963 0.00195 AFIX 43 H7 2 0.220300 1.141802 0.977785 11.00000 -1.20000 AFIX 0 C8 1 0.042899 0.895914 0.877195 11.00000 0.03018 0.04310 = 0.05050 0.01073 0.01457 0.00398 AFIX 43 H8 2 -0.076652 0.971435 0.898830 11.00000 -1.20000 AFIX 0 C9 1 0.034154 0.687837 0.800181 11.00000 0.02199 0.04290 = 0.04607 0.01036 0.00315 -0.00350 AFIX 43 H9 2 -0.087048 0.615698 0.768384 11.00000 -1.20000 AFIX 0 HKLF 4 REM ALP078Pdep_a.res in P2(1) REM wR2 = 0.076735, GooF = S = 1.09961, Restrained GooF = 1.09931 for all data REM R1 = 0.029859 for 1860 Fo > 4sig(Fo) and 0.031945 for all 1954 data REM 119 parameters refined using 1 restraints END WGHT 0.0432 0.0403 REM Highest difference peak 0.196, deepest hole -0.156, 1-sigma level 0.029 Q1 1 0.4932 0.3102 0.6637 11.00000 0.05 0.20 Q2 1 0.2940 0.6651 0.8043 11.00000 0.05 0.19 Q3 1 0.5154 0.5114 0.7206 11.00000 0.05 0.16 Q4 1 0.3956 0.8163 0.8448 11.00000 0.05 0.15 Q5 1 0.1320 0.7085 0.7804 11.00000 0.05 0.13 Q6 1 0.4820 0.6297 0.7967 11.00000 0.05 0.13 Q7 1 0.5020 0.4015 0.7545 11.00000 0.05 0.13 Q8 1 0.0423 0.7268 0.8612 11.00000 0.05 0.13 Q9 1 0.1290 0.5946 0.7988 11.00000 0.05 0.12 Q10 1 0.1363 0.9628 0.8842 11.00000 0.05 0.11 Q11 1 0.4969 0.0182 0.6336 11.00000 0.05 0.11 Q12 1 0.3715 0.3867 0.6945 11.00000 0.05 0.11 Q13 1 0.3021 0.9033 0.9183 11.00000 0.05 0.10 Q14 1 0.4818 0.1639 0.5835 11.00000 0.05 0.10 Q15 1 0.3157 0.9904 0.8985 11.00000 0.05 0.10 Q16 1 0.6403 0.2491 0.6229 11.00000 0.05 0.10 Q17 1 0.7653 0.2148 0.6987 11.00000 0.05 0.10 Q18 1 0.8413 0.1041 0.5105 11.00000 0.05 0.10 Q19 1 0.6033 0.4888 0.7994 11.00000 0.05 0.10 Q20 1 0.0562 0.8800 0.8084 11.00000 0.05 0.08 ; _shelx_res_checksum 92588 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -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 O O1 0.25255(16) 0.3885(3) 0.69933(9) 0.0329(3) Uani d 1 . . O O2 0.43981(19) -0.0004(3) 0.57993(9) 0.0382(3) Uani d 1 . . O O3 0.73220(17) 0.2017(3) 0.63833(9) 0.0341(3) Uani d 1 . . N N1 0.54541(19) 0.5493(3) 0.77177(10) 0.0277(3) Uani d 1 . . C C1 0.4528(2) 0.3789(4) 0.70473(12) 0.0296(3) Uani d 1 . . C C2 0.5378(2) 0.1703(4) 0.63294(12) 0.0297(3) Uani d 1 . . C C3 0.8319(3) 0.0125(4) 0.57015(13) 0.0381(4) Uani d 1 . . H H3A 0.794777 -0.196824 0.579791 0.057 Uiso calc 1 . . H H3B 0.974729 0.034297 0.584461 0.057 Uiso calc 1 . . H H3C 0.793506 0.072127 0.500188 0.057 Uiso calc 1 . . C C4 0.2149(2) 0.5919(4) 0.77264(12) 0.0291(3) Uani d 1 . . C C5 0.3947(2) 0.6919(4) 0.81779(11) 0.0273(3) Uani d 1 . . C C6 0.4014(2) 0.9009(4) 0.89607(13) 0.0347(4) Uani d 1 . . H H6 0.522730 0.971603 0.928121 0.042 Uiso calc 1 . . C C7 0.2220(3) 0.9998(4) 0.92465(14) 0.0401(4) Uani d 1 . . H H7 0.220300 1.141802 0.977785 0.048 Uiso calc 1 . . C C8 0.0429(3) 0.8959(5) 0.87719(15) 0.0406(4) Uani d 1 . . H H8 -0.076652 0.971435 0.898830 0.049 Uiso calc 1 . . C C9 0.0342(2) 0.6878(5) 0.80018(14) 0.0370(4) Uani d 1 . . H H9 -0.087048 0.615698 0.768384 0.044 Uiso calc 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 O1 0.0259(5) 0.0362(6) 0.0359(6) -0.0064(5) -0.0013(4) 0.0001(5) O2 0.0406(6) 0.0349(6) 0.0380(6) -0.0087(5) -0.0024(5) -0.0035(5) O3 0.0315(6) 0.0342(6) 0.0364(6) -0.0025(5) 0.0009(4) -0.0061(5) N1 0.0241(6) 0.0274(6) 0.0312(6) -0.0017(5) 0.0008(4) 0.0002(5) C1 0.0288(7) 0.0286(7) 0.0311(7) -0.0048(6) 0.0007(6) 0.0048(6) C2 0.0329(8) 0.0264(7) 0.0292(7) -0.0042(6) -0.0006(6) 0.0039(6) C3 0.0384(9) 0.0380(10) 0.0381(8) 0.0030(8) 0.0047(7) -0.0042(8) C4 0.0259(7) 0.0305(8) 0.0308(7) -0.0049(6) 0.0010(5) 0.0063(6) C5 0.0233(7) 0.0278(7) 0.0306(7) -0.0019(6) 0.0013(5) 0.0057(6) C6 0.0311(8) 0.0357(8) 0.0366(8) -0.0030(7) -0.0006(6) -0.0014(7) C7 0.0438(10) 0.0370(9) 0.0407(9) 0.0020(8) 0.0096(7) -0.0015(8) C8 0.0302(8) 0.0431(10) 0.0505(10) 0.0040(8) 0.0146(7) 0.0107(9) C9 0.0220(7) 0.0429(9) 0.0461(9) -0.0035(7) 0.0032(6) 0.0104(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 C1 O1 C4 . . 103.51(12) ? C2 O3 C3 . . 115.17(14) ? C1 N1 C5 . . 103.74(13) ? N1 C1 O1 . . 116.33(15) ? N1 C1 C2 . . 128.06(14) ? O1 C1 C2 . . 115.61(13) ? O2 C2 O3 . . 126.82(17) ? O2 C2 C1 . . 123.11(16) ? O3 C2 C1 . . 110.07(14) ? O3 C3 H3A . . 109.5 ? O3 C3 H3B . . 109.5 ? H3A C3 H3B . . 109.5 ? O3 C3 H3C . . 109.5 ? H3A C3 H3C . . 109.5 ? H3B C3 H3C . . 109.5 ? O1 C4 C9 . . 128.30(15) ? O1 C4 C5 . . 107.78(14) ? C9 C4 C5 . . 123.92(17) ? C4 C5 N1 . . 108.64(15) ? C4 C5 C6 . . 120.36(15) ? N1 C5 C6 . . 131.00(14) ? C7 C6 C5 . . 116.58(16) ? C7 C6 H6 . . 121.7 ? C5 C6 H6 . . 121.7 ? C6 C7 C8 . . 121.71(18) ? C6 C7 H7 . . 119.1 ? C8 C7 H7 . . 119.1 ? C9 C8 C7 . . 122.32(17) ? C9 C8 H8 . . 118.8 ? C7 C8 H8 . . 118.8 ? C8 C9 C4 . . 115.10(16) ? C8 C9 H9 . . 122.4 ? C4 C9 H9 . . 122.4 ? 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 O1 C1 . 1.3610(19) ? O1 C4 . 1.373(2) ? O2 C2 . 1.200(2) ? O3 C2 . 1.3281(19) ? O3 C3 . 1.452(2) ? N1 C1 . 1.293(2) ? N1 C5 . 1.395(2) ? C1 C2 . 1.488(2) ? C3 H3A . 0.9800 ? C3 H3B . 0.9800 ? C3 H3C . 0.9800 ? C4 C9 . 1.384(2) ? C4 C5 . 1.390(2) ? C5 C6 . 1.395(2) ? C6 C7 . 1.385(3) ? C6 H6 . 0.9500 ? C7 C8 . 1.402(3) ? C7 H7 . 0.9500 ? C8 C9 . 1.380(3) ? C8 H8 . 0.9500 ? C9 H9 . 0.9500 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _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 C9 H9 N1 1_555 1_555 1_455 0.95 2.53 3.377(2) 149 yes C3 H3C O2 1_555 1_555 2_656 0.98 2.65 3.389(2) 133 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 C5 N1 C1 O1 . . . . 0.05(19) ? C5 N1 C1 C2 . . . . -179.34(15) ? C4 O1 C1 N1 . . . . 0.03(18) ? C4 O1 C1 C2 . . . . 179.50(13) ? C3 O3 C2 O2 . . . . 1.7(2) ? C3 O3 C2 C1 . . . . -178.99(13) ? N1 C1 C2 O2 . . . . 172.61(18) ? O1 C1 C2 O2 . . . . -6.8(2) ? N1 C1 C2 O3 . . . . -6.7(2) ? O1 C1 C2 O3 . . . . 173.92(14) ? C1 O1 C4 C9 . . . . -179.89(17) ? C1 O1 C4 C5 . . . . -0.10(16) ? O1 C4 C5 N1 . . . . 0.14(17) ? C9 C4 C5 N1 . . . . 179.93(15) ? O1 C4 C5 C6 . . . . -179.61(14) ? C9 C4 C5 C6 . . . . 0.2(2) ? C1 N1 C5 C4 . . . . -0.11(17) ? C1 N1 C5 C6 . . . . 179.60(17) ? C4 C5 C6 C7 . . . . -0.2(2) ? N1 C5 C6 C7 . . . . -179.92(16) ? C5 C6 C7 C8 . . . . -0.1(3) ? C6 C7 C8 C9 . . . . 0.6(3) ? C7 C8 C9 C4 . . . . -0.6(3) ? O1 C4 C9 C8 . . . . 180.00(16) ? C5 C4 C9 C8 . . . . 0.2(3) ? _cod_database_fobs_code 2243934