#------------------------------------------------------------------------------ #$Date: 2017-07-25 11:41:50 +0300 (Tue, 25 Jul 2017) $ #$Revision: 199047 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/80/2108057.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_2108057 loop_ _publ_author_name 'Chia, Tze Shyang' 'Quah, Ching Kheng' _publ_section_title ; Temperature-induced first-order displacive phase transition of isonicotinamide-4-methoxybenzoic acid co-crystal ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 285 _journal_page_last 295 _journal_paper_doi 10.1107/S2052520616019405 _journal_volume 73 _journal_year 2017 _chemical_formula_moiety 'C8 H8 O3, C6 H6 N2 O' _chemical_formula_sum 'C14 H14 N2 O4' _chemical_formula_weight 274.27 _chemical_name_systematic ; Isonicotinamide 4-methoxybenzoic acid ; _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-I 2ya' _space_group_name_H-M_alt 'I 1 2/a 1' _symmetry_space_group_name_Hall '-I 2ya' _symmetry_space_group_name_H-M 'I 1 2/a 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 90.95(2) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 20.296(7) _cell_length_b 5.1263(18) _cell_length_c 25.005(9) _cell_measurement_reflns_used 3184 _cell_measurement_temperature 142.00(10) _cell_measurement_theta_max 28.67 _cell_measurement_theta_min 2.56 _cell_volume 2601.2(16) _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_molecular_graphics ; SHELXTL (Sheldrick, 2008), Mercury (Macrae, 2006) ; _computing_publication_material ; PLATON (Spek, 2009) ; _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2008)' _diffrn_ambient_temperature 142.00(10) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Bruker APEX Duo CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_number 14782 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.829 _diffrn_reflns_theta_min 1.629 _exptl_absorpt_coefficient_mu 0.104 _exptl_absorpt_correction_T_max 0.9686 _exptl_absorpt_correction_T_min 0.7685 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2009)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.401 _exptl_crystal_description block _exptl_crystal_F_000 1152 _exptl_crystal_size_max 0.808 _exptl_crystal_size_mid 0.126 _exptl_crystal_size_min 0.046 _refine_diff_density_max 0.314 _refine_diff_density_min -0.240 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 194 _refine_ls_number_reflns 3363 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.040 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_gt 0.0462 _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^)+(0.0729P)^2^+0.7112P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1197 _refine_ls_wR_factor_ref 0.1333 _reflns_number_gt 2502 _reflns_number_total 3363 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file gw5049sup1.cif _cod_data_source_block mo_in4meo142_0m _cod_database_code 2108057 _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 0.921 _shelx_estimated_absorpt_t_max 0.995 _shelx_hkl_file ; -2 0 0 297.538 10.0304 1 2 0 0 313.051 10.0425 1 -2 0 0 316.798 10.0201 3 -2 0 0 316.640 10.0300 2 2 0 0 299.693 10.0205 2 4 0 0 247.269 8.40547 1 -4 0 0 260.447 8.37086 3 4 0 0 257.939 8.37030 2 4 0 0 251.624 8.42126 2 -4 0 0 250.260 8.38669 2 -6 0 0 8.86142 0.61781 3 6 0 0 9.89692 0.67131 1 6 0 0 10.2002 0.62192 2 8 0 0 35.9302 1.70466 1 -8 0 0 37.2874 1.62802 3 8 0 0 38.1910 1.63067 2 10 0 0 10.7761 0.75897 2 -10 0 0 10.1814 0.78969 3 10 0 0 10.3464 0.87923 1 12 0 0 669.661 21.7992 2 -12 0 0 653.294 21.8108 3 12 0 0 652.865 22.0614 1 14 0 0 0.54647 0.29123 2 14 0 0 0.13499 0.34518 1 -14 0 0 0.35751 0.33655 3 16 0 0 15.1384 1.08657 2 16 0 0 12.9205 1.51394 1 -16 0 0 14.5538 1.12122 3 -18 0 0 181.616 6.92174 3 18 0 0 189.914 6.86042 2 18 0 0 184.401 7.42286 1 20 0 0 72.4125 3.20409 2 -20 0 0 72.4422 3.32815 3 20 0 0 71.3315 3.81055 1 22 0 0 0.18807 0.39219 2 -22 0 0 0.94364 0.52515 3 22 0 0 0.58235 0.76549 1 24 0 0 2.15157 1.02261 1 -24 0 0 0.52752 0.55925 3 -26 0 0 2.25436 0.74863 3 26 0 0 2.17859 1.15786 1 -28 0 0 1.29914 0.82549 3 28 0 0 0.64111 1.26380 1 30 0 0 112.505 6.42264 1 32 0 0 -0.1043 1.59327 1 -32 0 0 0.70850 0.89373 3 1 -1 0 96.6922 3.54349 1 -1 -1 0 98.2648 3.50949 3 -1 -1 0 99.9050 3.69604 2 1 -1 0 95.3663 3.55375 3 1 -1 0 95.6574 3.56406 2 -1 -1 0 95.7072 3.46015 1 1 1 0 94.7579 3.44458 1 3 -1 0 207.322 7.22787 3 -3 -1 0 189.625 7.35455 2 3 -1 0 222.044 7.28548 1 3 -1 0 205.933 7.06134 2 -3 -1 0 218.053 7.06700 3 -3 1 0 211.939 7.19013 3 3 1 0 201.591 6.95750 1 3 1 0 210.474 7.34339 2 -5 -1 0 399.674 12.9904 3 -5 -1 0 395.806 13.4569 2 5 -1 0 392.879 13.2471 3 5 -1 0 398.530 13.3204 1 5 -1 0 386.876 12.9213 2 -5 1 0 403.530 12.8442 2 5 1 0 410.820 13.4185 2 5 1 0 373.227 12.8783 1 -5 1 0 375.295 13.1501 3 7 -1 0 389.003 13.4170 2 7 -1 0 431.678 14.0730 1 -7 -1 0 424.527 13.6205 3 -7 -1 0 415.357 14.1656 2 -7 1 0 396.412 13.4251 2 7 1 0 406.097 13.5237 1 7 1 0 416.489 14.0673 2 -7 1 0 408.082 13.8316 3 9 -1 0 166.393 5.92697 2 -9 -1 0 189.819 6.23592 3 9 -1 0 176.025 6.66996 1 -9 -1 0 182.499 6.80474 2 9 1 0 177.849 6.16314 1 -9 1 0 171.604 6.40289 3 9 1 0 176.153 6.64567 2 -11 -1 0 188.136 6.52062 3 11 -1 0 183.325 6.18110 2 -11 -1 0 184.891 7.09256 2 11 -1 0 180.848 7.00681 1 -11 1 0 177.708 6.69806 3 11 1 0 184.373 6.96135 2 11 1 0 182.285 6.50467 1 13 -1 0 1.28079 0.32789 2 13 -1 0 1.98469 0.66826 1 -13 -1 0 1.32866 0.45119 3 13 1 0 1.90821 0.61062 2 -13 1 0 0.95923 0.43894 3 13 1 0 1.38058 0.42948 1 15 -1 0 4.66777 1.05028 1 -15 -1 0 3.81626 0.69308 3 15 -1 0 3.90515 0.53567 2 15 1 0 3.71615 0.71006 1 15 1 0 4.55045 0.88515 2 -15 1 0 2.13835 0.63926 3 17 -1 0 0.54560 0.55047 1 -17 -1 0 0.61865 0.44345 3 17 -1 0 0.11670 0.38306 2 17 1 0 0.25273 0.38174 2 -17 1 0 0.09462 0.36732 3 17 1 0 0.23407 0.47577 1 -19 -1 0 35.4513 2.09153 3 19 -1 0 38.9721 2.69998 1 -19 1 0 38.5192 2.26938 3 19 1 0 36.1310 2.35255 2 19 1 0 39.0127 2.36640 1 21 -1 0 2.22798 0.99461 1 -21 -1 0 1.07123 0.52967 3 21 1 0 0.66941 0.59361 2 -21 1 0 1.26972 0.65813 3 21 1 0 1.82737 0.79900 1 -23 -1 0 17.9396 1.83311 3 23 -1 0 16.8044 2.37364 1 23 1 0 21.4451 2.27466 1 -23 1 0 20.6661 1.74112 3 23 1 0 17.6820 1.67343 2 25 -1 0 6.95914 1.73529 1 -25 -1 0 4.07311 0.97402 3 25 1 0 4.98116 1.13662 2 -25 1 0 4.07996 1.00049 3 25 1 0 3.26115 1.22570 1 27 -1 0 4.00671 1.53546 1 -27 -1 0 2.26231 0.93343 3 -27 1 0 2.28025 0.85000 3 27 1 0 2.65898 1.33512 1 -29 -1 0 1.40917 0.91112 3 29 -1 0 3.08717 1.48593 1 -29 1 0 2.95555 1.05915 3 29 1 0 0.26880 1.26414 1 31 -1 0 0.08713 1.34725 1 -31 1 0 0.00167 0.83790 3 33 -1 0 0.75792 1.90904 1 -33 1 0 -0.0976 0.83296 3 0 -2 0 854.291 28.1187 2 0 -2 0 833.711 27.8533 3 0 -2 0 838.004 27.8266 1 2 -2 0 131.969 5.18173 2 -2 -2 0 137.146 5.07696 3 2 -2 0 136.609 5.15915 1 2 -2 0 129.263 5.11285 3 -2 -2 0 135.935 5.40992 2 -2 -2 0 128.991 4.93559 1 2 2 0 137.299 4.95664 1 2 2 0 125.236 5.25467 2 4 -2 0 18.4554 1.23367 2 4 -2 0 15.5319 1.29795 3 -4 -2 0 20.6142 1.29374 3 4 -2 0 17.1811 1.33652 1 -4 -2 0 19.3455 1.54452 2 4 2 0 17.0407 1.05443 1 4 2 0 17.2840 1.36801 2 -4 2 0 18.9485 1.28346 3 6 -2 0 1.13077 0.53714 3 -6 -2 0 0.13079 0.36697 2 -6 -2 0 0.17537 0.34996 3 6 -2 0 0.09517 0.26420 2 6 -2 0 0.20470 0.38371 1 -6 2 0 0.26951 0.36017 3 6 2 0 -0.0726 0.18217 1 6 2 0 0.08476 0.36757 2 -8 -2 0 7.83017 0.90793 3 8 -2 0 6.58442 0.75864 2 8 -2 0 6.61751 1.06891 1 8 -2 0 8.58435 1.17018 3 -8 -2 0 7.02225 1.17807 2 8 2 0 5.88075 1.07301 2 -8 2 0 6.96608 0.96243 3 10 -2 0 78.7972 3.14627 2 -10 -2 0 83.6002 3.37652 3 -10 -2 0 80.3685 4.06061 2 10 -2 0 77.4007 3.83507 1 10 2 0 78.5523 3.88115 2 10 2 0 82.3554 3.12401 1 -10 2 0 77.6070 3.56581 3 -12 -2 0 10.7371 1.52851 2 -12 -2 0 11.2465 1.17735 3 12 -2 0 14.7055 1.80691 1 12 -2 0 10.2041 0.81365 2 12 2 0 12.1791 1.53932 2 12 2 0 10.9392 0.86387 1 -12 2 0 10.3690 1.23245 3 -14 -2 0 8.71945 1.52872 2 -14 -2 0 11.5296 1.25081 3 14 -2 0 8.95939 0.74727 2 14 -2 0 10.9949 1.58697 1 14 2 0 8.12825 1.34612 2 -14 2 0 10.6549 1.38251 3 14 2 0 9.79470 1.01611 1 -16 -2 0 0.23482 0.44571 3 16 -2 0 -0.2101 0.52151 1 16 2 0 -0.1325 0.37183 1 16 2 0 0.38183 0.59230 2 -16 2 0 -0.0179 0.47771 3 -18 -2 0 37.4121 2.30587 3 18 -2 0 38.3858 2.87941 1 18 2 0 40.4805 2.76895 2 18 2 0 40.9734 2.27176 1 -18 2 0 37.8783 2.45331 3 20 -2 0 22.6353 2.59426 1 -20 -2 0 21.2145 2.00409 3 20 2 0 21.2157 2.42943 2 20 2 0 20.0282 1.74410 1 -20 2 0 21.1150 2.08714 3 22 -2 0 2.99003 1.14946 1 -22 -2 0 0.82761 0.71228 3 22 2 0 1.22870 0.76257 2 -22 2 0 3.06652 1.04624 3 22 2 0 3.49404 1.04043 1 -24 -2 0 0.95817 0.73410 3 24 -2 0 -0.5776 0.92690 1 -24 2 0 0.44440 0.65304 3 24 2 0 -1.5231 0.73991 1 24 2 0 0.20880 0.83264 2 26 -2 0 2.74031 1.39889 1 26 2 0 -0.1446 0.73596 2 -26 2 0 1.38095 0.94043 3 28 -2 0 1.35478 1.44587 1 28 2 0 -0.2858 0.80183 2 -28 2 0 -0.0045 0.84951 3 30 -2 0 28.8628 3.88843 1 -30 2 0 18.6538 2.35517 3 32 -2 0 1.95959 1.75274 1 -32 2 0 0.40504 1.03143 3 1 -3 0 18.3668 1.51892 3 -1 -3 0 17.0560 1.38414 1 -1 -3 0 16.7329 1.58681 2 1 -3 0 15.9931 1.52026 2 1 -3 0 17.3317 1.41237 1 -1 -3 0 17.3346 1.46235 3 -1 3 0 14.2122 1.53451 1 -1 3 0 17.5034 1.52440 2 1 3 0 14.9237 1.73462 2 1 3 0 15.5898 1.32061 1 3 -3 0 87.5520 4.08234 2 3 -3 0 86.1332 4.02241 3 3 -3 0 85.9262 4.01852 1 -3 -3 0 85.2239 3.88195 3 -3 -3 0 87.3372 3.75216 1 -3 -3 0 95.6536 4.48294 2 3 3 0 85.6984 3.71756 1 3 3 0 86.0018 4.23304 2 -3 3 0 87.0547 3.92356 3 5 -3 0 73.7531 3.68167 1 5 -3 0 72.1948 3.53741 2 -5 -3 0 81.1561 3.54278 3 5 -3 0 72.4716 3.65243 3 -5 -3 0 79.2511 4.08725 2 5 3 0 73.5047 3.21127 1 5 3 0 76.2623 3.91113 2 -5 3 0 71.6388 3.53338 3 7 -3 0 19.5333 1.97539 1 7 -3 0 17.8811 1.45093 2 7 -3 0 19.7375 2.00800 3 -7 -3 0 15.0755 1.87836 2 -7 -3 0 18.2141 1.48829 3 7 3 0 19.1163 1.78451 2 -7 3 0 18.1451 1.52496 3 7 3 0 17.1324 1.17275 1 9 -3 0 1.59194 0.54158 2 -9 -3 0 0.46719 0.71833 2 9 -3 0 2.52470 0.85766 3 9 -3 0 0.95841 0.68112 1 -9 -3 0 0.47244 0.50118 3 -9 3 0 0.96514 0.56765 3 9 3 0 0.72807 0.38418 1 9 3 0 0.75433 0.57269 2 -11 -3 0 27.6981 2.41459 2 11 -3 0 22.8149 1.57016 2 -11 -3 0 23.9925 1.77106 3 11 -3 0 28.2115 2.24249 1 11 3 0 22.9627 2.11265 2 11 3 0 27.6374 1.50695 1 -11 3 0 28.5588 2.02538 3 13 -3 0 4.63961 1.29510 1 -13 -3 0 6.09848 1.00238 3 -13 -3 0 6.04598 1.46282 2 13 3 0 4.85984 0.75563 1 13 3 0 4.99224 1.19447 2 -13 3 0 4.08482 0.96884 3 -15 -3 0 9.21126 1.32804 3 -15 -3 0 8.55799 1.65649 2 15 -3 0 9.47888 1.86850 1 15 3 0 9.35712 1.06199 1 15 3 0 8.00051 1.65354 2 -15 3 0 6.84976 1.21299 3 17 -3 0 68.0354 4.21784 1 -17 -3 0 71.8243 3.57382 3 17 3 0 66.0938 4.15862 2 17 3 0 68.7081 3.17899 1 -17 3 0 74.3359 3.86932 3 -19 -3 0 77.9158 3.98659 3 19 -3 0 75.8527 4.64731 1 -19 3 0 72.7426 4.07200 3 19 3 0 80.5020 4.62089 2 21 -3 0 0.65200 0.85789 1 21 3 0 0.93305 0.90658 2 -21 3 0 1.48422 0.90026 3 23 -3 0 1.77497 1.24269 1 23 3 0 0.13186 0.83581 2 -23 3 0 0.02024 0.80720 3 25 -3 0 0.44668 1.11915 1 -25 3 0 0.76908 0.95917 3 25 3 0 0.84986 0.96284 2 27 -3 0 9.27990 2.18017 1 27 3 0 8.54999 1.93652 2 -27 3 0 9.91775 1.87662 3 29 -3 0 3.20270 1.91339 1 -29 3 0 0.43874 1.07118 3 29 3 0 1.81886 1.32641 2 0 -4 0 19.2250 2.39279 2 0 -4 0 22.8574 2.25884 3 0 -4 0 20.5259 2.06287 1 0 4 0 19.9457 2.06200 1 0 4 0 23.8647 2.08640 2 -2 -4 0 2.88840 1.08809 2 -2 -4 0 2.02201 0.77719 3 2 -4 0 3.55204 0.98143 1 2 -4 0 4.35438 1.09726 3 -2 -4 0 4.30637 0.90999 1 2 -4 0 3.02475 1.01873 2 2 4 0 2.66154 0.82594 1 -2 4 0 3.32149 0.86989 3 -2 4 0 4.15184 1.04600 2 -2 4 0 3.51569 0.96243 1 2 4 0 3.33219 1.02782 2 4 -4 0 114.164 5.38900 3 4 -4 0 120.681 5.44362 1 -4 -4 0 114.653 5.81883 2 4 -4 0 117.853 5.50381 2 -4 -4 0 110.709 5.16115 3 -4 4 0 124.692 5.47142 2 4 4 0 122.324 5.02736 1 4 4 0 116.393 5.71008 2 -4 4 0 107.126 5.16276 3 6 -4 0 3.57388 1.00398 1 6 -4 0 5.70623 1.24266 2 -6 -4 0 2.81032 1.00758 2 -6 -4 0 4.92005 1.12268 3 6 -4 0 3.51440 1.04532 3 -6 4 0 4.38510 1.01956 2 6 4 0 4.27299 0.83649 1 6 4 0 5.10582 1.29809 2 -6 4 0 4.24723 1.02757 3 8 -4 0 324.287 12.6733 1 -8 -4 0 337.949 12.2095 3 8 -4 0 361.661 12.7001 3 8 -4 0 321.568 12.1980 2 -8 -4 0 329.695 13.2401 2 -8 4 0 323.866 12.3236 3 8 4 0 318.835 11.6003 1 -8 4 0 328.368 12.1612 2 8 4 0 323.314 12.9331 2 -10 -4 0 0.39459 0.82340 2 10 -4 0 -0.2956 0.65716 3 -10 -4 0 -0.4181 0.65973 3 10 -4 0 0.19081 0.66051 1 10 4 0 -0.3271 0.40227 1 -10 4 0 0.57862 0.65572 3 10 4 0 -0.1147 0.61780 2 -12 -4 0 15.3930 2.29583 2 12 -4 0 28.9334 3.10991 1 -12 -4 0 24.1846 2.27353 3 12 4 0 20.4036 2.61583 2 -12 4 0 25.2021 2.48336 3 -14 -4 0 18.9762 2.69326 2 14 -4 0 20.3003 2.78452 1 -14 4 0 19.0306 2.24638 3 14 4 0 18.6806 2.55792 2 -16 -4 0 9.82682 1.95287 2 16 -4 0 13.6748 2.38653 1 16 4 0 10.5227 1.96146 2 -16 4 0 13.1737 1.91245 3 18 -4 0 1.92859 1.16811 1 18 4 0 0.60473 0.95158 2 -18 4 0 0.15580 0.83999 3 20 -4 0 4.25692 1.67435 1 20 4 0 3.89557 1.37814 2 -20 4 0 5.41659 1.27724 3 22 -4 0 37.8811 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1.86542 3 -22 4 22 0.35262 1.08071 1 -20 -4 22 18.6416 3.47228 3 -20 4 22 16.2619 3.11718 1 -18 -4 22 8.14896 2.69848 3 -40 0 23 -0.3908 1.45001 3 40 0 -23 2.25902 1.07727 2 -38 0 23 0.83606 1.41495 3 38 0 -23 2.09823 0.96605 2 -36 0 23 0.60032 1.33178 3 36 0 -23 1.07387 0.98721 2 34 0 -23 1.03821 0.94279 2 -34 0 23 0.21938 1.24376 3 -32 0 23 -0.1169 1.19398 3 32 0 -23 0.81241 0.93613 2 -30 0 23 1.19172 1.26460 3 30 0 -23 0.30321 0.89152 2 28 0 -23 1.69152 0.98438 2 -28 0 23 2.53805 1.25998 3 -26 0 23 0.86982 1.18824 3 26 0 -23 0.22043 0.84225 2 24 0 -23 0.33967 0.96155 2 -24 0 23 1.02100 1.92092 3 22 0 -23 -0.6042 1.03899 2 -22 0 23 -0.7378 0.52766 1 20 0 -23 -0.3820 1.06922 2 -20 0 23 -0.7138 0.56863 1 18 0 -23 1.07502 1.05986 2 -18 0 23 -0.1921 0.59035 1 -16 0 23 0.59559 0.67302 1 16 0 -23 -0.0144 1.11506 2 14 0 -23 0.44187 1.37624 2 -14 0 23 0.09270 0.69618 1 -12 0 23 0.47853 0.74298 1 -10 0 23 1.43305 0.92574 1 -8 0 23 1.28610 0.87819 1 -6 0 23 -0.3843 1.02531 1 -4 0 23 -2.2585 1.02443 1 -39 -1 23 4.47125 2.07651 3 39 -1 -23 3.51634 1.57286 2 -39 1 23 2.04026 1.69931 3 39 1 -23 8.29505 1.71870 2 -37 -1 23 0.88737 1.54730 3 37 -1 -23 2.60777 1.34849 2 -37 1 23 2.14129 1.55810 3 37 1 -23 4.76279 1.21315 2 -35 -1 23 -0.9311 1.25275 3 35 -1 -23 0.03867 0.89135 2 -35 1 23 -0.0205 1.30577 3 35 1 -23 3.63980 1.11117 2 -33 -1 23 2.12434 1.51266 3 33 -1 -23 2.61651 1.34802 2 33 1 -23 6.16510 1.34742 2 -33 1 23 3.90548 1.53561 3 31 -1 -23 2.88705 1.29322 2 -31 -1 23 2.69743 1.53265 3 31 1 -23 4.42409 1.22519 2 -31 1 23 2.64403 1.79844 3 -29 -1 23 6.86536 1.86696 3 29 -1 -23 12.1637 2.24741 2 29 1 -23 11.6271 1.83526 2 27 -1 -23 5.27361 1.70730 2 -27 -1 23 3.34817 1.75517 3 -27 1 23 2.73523 0.93669 1 27 1 -23 4.93710 1.20695 2 25 -1 -23 59.5669 4.43299 2 -25 -1 23 62.1399 4.48489 3 25 1 -23 58.1740 3.82150 2 23 -1 -23 7.89169 1.81860 2 -23 -1 23 6.04286 1.79688 3 23 1 -23 9.42401 1.82671 2 -23 1 23 8.00677 1.36198 1 -21 -1 23 7.25390 1.96521 3 21 -1 -23 9.52443 2.15904 2 21 1 -23 11.8464 2.07334 2 -21 1 23 8.26789 1.41338 1 19 -1 -23 1.63857 1.18652 2 -19 -1 23 -0.0040 1.18076 3 19 1 -23 0.58130 1.12147 2 -19 1 23 0.77367 0.78488 1 17 -1 -23 46.5612 4.09846 2 17 1 -23 43.5574 3.56786 2 -17 1 23 45.0972 3.02908 1 15 -1 -23 -0.1477 1.27129 2 -15 -1 23 0.39897 0.81076 1 -15 1 23 0.09783 0.68376 1 13 -1 -23 3.84661 1.80561 2 -13 -1 23 1.99546 1.05637 1 -13 1 23 2.69154 1.05771 1 -11 -1 23 44.9068 3.39005 1 11 -1 -23 54.2759 4.67715 2 -11 1 23 46.6860 3.25955 1 -9 -1 23 2.33904 1.32403 1 -9 1 23 4.06609 1.27039 1 -7 -1 23 4.06282 1.45491 1 -7 1 23 7.86009 1.66523 1 -5 -1 23 43.0428 3.61980 1 -5 1 23 33.6316 4.49243 1 38 -2 -23 8.67627 2.49139 2 -36 -2 23 71.1879 5.46292 3 36 -2 -23 62.1520 4.93241 2 36 2 -23 66.5276 4.58352 2 -34 -2 23 -0.6251 1.46384 3 34 -2 -23 0.22808 1.16775 2 34 2 -23 2.30156 1.49467 2 -32 -2 23 2.89028 1.70005 3 32 -2 -23 0.92685 1.38636 2 32 2 -23 1.28669 1.11801 2 -32 2 23 1.37302 0.96135 1 -30 -2 23 1.12682 1.58227 3 30 -2 -23 1.42819 1.02850 2 30 2 -23 1.53731 1.07269 2 -30 2 23 1.01453 0.79439 1 28 -2 -23 -0.0977 1.18422 2 -28 -2 23 1.42966 1.62059 3 -28 2 23 1.06848 0.86334 1 28 2 -23 4.17097 1.11501 2 -26 -2 23 0.69057 1.48519 3 26 -2 -23 0.39500 1.10857 2 -26 2 23 -0.8603 0.65776 1 24 -2 -23 31.4007 3.91735 2 -24 -2 23 26.3383 3.67556 3 24 2 -23 28.7797 2.50875 2 -24 2 23 25.2057 2.66873 1 22 -2 -23 1.05098 1.29800 2 -22 -2 23 1.65401 1.55739 3 22 2 -23 3.63892 1.13608 2 -22 2 23 2.39917 0.96050 1 -20 -2 23 21.1711 3.15265 3 20 -2 -23 25.4286 3.74338 2 20 2 -23 23.6162 2.68305 2 -18 -2 23 1.21722 1.58043 3 18 -2 -23 2.11867 1.50173 2 -18 2 23 0.33133 0.69912 1 16 -2 -23 28.0774 4.03407 2 -16 -2 23 19.9259 3.02948 3 -16 2 23 22.9460 2.55780 1 -14 -2 23 6.64448 2.05559 3 14 -2 -23 5.54723 2.13123 2 -14 2 23 8.74249 1.67244 1 12 -2 -23 3.84822 1.92843 2 -12 2 23 3.74006 1.13431 1 10 -2 -23 1.09368 1.73561 2 -10 2 23 1.21491 0.94617 1 8 -2 -23 5.05237 2.21142 2 -8 2 23 4.95239 1.45640 1 33 -3 -23 3.80741 2.07855 2 33 3 -23 2.59200 1.55650 2 -33 3 23 3.03342 1.21837 1 -31 -3 23 5.45035 2.26464 3 31 -3 -23 2.96162 1.59385 2 31 3 -23 3.37715 1.63820 2 -31 3 23 3.05927 1.21580 1 -29 -3 23 13.8722 2.95267 3 29 -3 -23 17.7003 3.06722 2 -29 3 23 13.5090 2.11754 1 29 3 -23 17.2651 2.57000 2 27 -3 -23 1.54351 1.61460 2 -27 -3 23 2.50032 1.97207 3 -27 3 23 2.52567 1.02500 1 27 3 -23 2.49880 1.18640 2 25 -3 -23 7.97663 2.27663 2 -25 -3 23 1.09737 1.60568 3 -25 3 23 2.49238 1.13776 1 25 3 -23 5.19597 1.41917 2 -23 -3 23 0.95416 1.46154 3 23 -3 -23 4.10857 1.90835 2 -23 3 23 3.82542 1.28286 1 23 3 -23 6.05909 1.20708 2 -21 -3 23 -0.1871 1.60811 3 21 -3 -23 1.90033 1.58225 2 -21 3 23 0.08837 0.76240 1 19 -3 -23 2.21670 1.77548 2 -19 -3 23 2.75695 1.84640 3 -19 3 23 1.06272 0.89284 1 -17 -3 23 33.2077 4.09922 3 17 -3 -23 37.3449 4.73652 2 15 -3 -23 0.40153 1.55815 2 -15 -3 23 0.62502 1.66368 3 -15 3 23 0.95754 1.03316 1 -13 -3 23 12.1732 2.80656 3 13 -3 -23 15.7724 3.33480 2 -13 3 23 8.08642 1.70764 1 38 0 -24 8.76796 1.81646 2 -38 0 24 7.64232 2.16971 3 -36 0 24 3.47286 1.65520 3 36 0 -24 1.68117 1.08150 2 -34 0 24 1.14100 1.41081 3 34 0 -24 1.20019 1.02863 2 32 0 -24 18.8342 2.70200 2 -32 0 24 20.1268 2.98807 3 -30 0 24 1.86800 1.29268 3 30 0 -24 1.62487 1.12879 2 -28 0 24 9.11491 2.11272 3 28 0 -24 13.6013 2.22165 2 26 0 -24 7.27717 1.77958 2 24 0 -24 1.62762 1.30488 2 22 0 -24 1.12227 1.21179 2 20 0 -24 5.14347 1.71964 2 -20 0 24 3.77097 1.06513 1 -18 0 24 0.94210 0.77237 1 18 0 -24 0.29020 1.36376 2 -16 0 24 12.4736 1.82892 1 16 0 -24 17.3014 2.89111 2 -14 0 24 0.06116 0.83055 1 14 0 -24 0.52231 1.63209 2 -12 0 24 37.7012 3.02432 1 -10 0 24 2.05061 1.08229 1 -8 0 24 2.18011 1.14853 1 -39 -1 24 0.79652 1.64879 3 -39 1 24 0.31070 1.47394 3 37 -1 -24 16.2061 2.67742 2 -37 -1 24 15.1375 2.97432 3 -37 1 24 16.6257 2.65893 3 37 1 -24 20.3701 2.52733 2 -35 -1 24 -0.1511 1.32719 3 35 -1 -24 1.82638 1.28809 2 -35 1 24 0.54267 1.29979 3 35 1 -24 2.70914 1.14501 2 33 -1 -24 7.86444 1.95520 2 -33 -1 24 5.91095 1.94371 3 33 1 -24 9.27290 1.80487 2 31 -1 -24 1.72037 1.29542 2 -31 -1 24 4.50242 1.87638 3 31 1 -24 5.43737 1.39465 2 -29 -1 24 3.81633 1.99317 3 29 -1 -24 6.62008 1.87487 2 29 1 -24 7.55811 1.52844 2 27 -1 -24 -0.1524 1.17694 2 -27 -1 24 -0.6281 1.24710 3 27 1 -24 0.76411 0.86692 2 -27 1 24 -0.5181 0.73968 1 25 -1 -24 2.81816 1.43823 2 -25 -1 24 1.94174 1.53907 3 25 1 -24 1.24961 1.05065 2 -25 1 24 0.01695 0.65604 1 23 -1 -24 4.87968 1.86365 2 -23 -1 24 9.38952 2.21431 3 23 1 -24 7.33146 1.81082 2 -23 1 24 6.57703 1.32215 1 21 -1 -24 0.12167 1.23514 2 -21 -1 24 -0.2346 1.37478 3 -21 1 24 -0.1988 0.69529 1 21 1 -24 0.26967 0.93082 2 19 -1 -24 0.83184 1.30232 2 -19 1 24 0.05445 0.67040 1 19 1 -24 0.40090 1.24122 2 17 -1 -24 7.26498 2.20486 2 -17 1 24 6.99173 1.45921 1 15 -1 -24 1.57622 1.65224 2 -15 1 24 -0.6570 0.62915 1 -13 -1 24 1.60432 1.19212 1 13 -1 -24 2.07195 1.93143 2 -13 1 24 0.37083 0.78741 1 11 -1 -24 1.26226 2.25740 2 -11 -1 24 2.16291 1.25248 1 -11 1 24 3.08398 1.15355 1 -9 -1 24 2.15524 1.24698 1 -9 1 24 2.15768 1.14217 1 36 -2 -24 9.13135 3.32284 2 -36 -2 24 9.45190 2.56124 3 36 2 -24 6.93795 2.37920 2 34 -2 -24 -0.7769 1.25068 2 -34 -2 24 -0.8802 1.72471 3 34 2 -24 2.59889 1.27621 2 32 -2 -24 2.70772 1.41464 2 -32 -2 24 -1.5765 1.46373 3 -32 2 24 1.98656 0.97131 1 32 2 -24 2.92894 1.10198 2 -30 -2 24 1.05251 1.69253 3 30 -2 -24 0.79349 1.39619 2 30 2 -24 2.14525 0.89643 2 -30 2 24 0.06335 0.81075 1 -28 -2 24 -0.5873 1.44205 3 28 -2 -24 -0.0847 1.33649 2 28 2 -24 3.03060 0.95853 2 -28 2 24 -0.4391 0.70857 1 -26 -2 24 11.4163 2.63615 3 26 -2 -24 9.24158 2.31126 2 -26 2 24 8.15087 1.55962 1 26 2 -24 14.4240 2.06786 2 24 -2 -24 20.7877 3.36370 2 -24 -2 24 14.2494 2.75675 3 -24 2 24 11.5480 1.77934 1 24 2 -24 12.6297 1.97050 2 22 -2 -24 9.70309 2.53267 2 -22 -2 24 11.3338 2.62234 3 22 2 -24 8.44680 1.75203 2 -20 -2 24 0.85389 1.54185 3 20 -2 -24 1.35000 1.48543 2 -20 2 24 0.82930 0.81254 1 18 -2 -24 9.13796 2.39041 2 -18 -2 24 7.91832 2.24268 3 -18 2 24 6.92695 1.42479 1 -16 -2 24 0.90248 1.57850 3 16 -2 -24 2.49971 1.99185 2 -16 2 24 1.71046 1.12870 1 14 -2 -24 7.07184 2.32803 2 -14 2 24 6.48352 1.55502 1 12 -2 -24 0.79718 1.69093 2 -12 2 24 -0.7460 0.84707 1 -31 3 24 22.3639 2.76071 1 31 3 -24 20.1187 2.90115 2 -29 -3 24 14.7261 3.19605 3 29 3 -24 13.9182 2.26646 2 -29 3 24 11.3327 2.05116 1 27 -3 -24 2.94417 1.98009 2 -27 -3 24 6.14524 2.35978 3 -27 3 24 1.88247 1.07732 1 27 3 -24 6.59703 1.45626 2 25 -3 -24 2.32883 1.61930 2 -25 -3 24 0.96268 1.80415 3 25 3 -24 6.30149 1.27736 2 -25 3 24 2.54928 1.24919 1 -23 -3 24 -0.1695 1.59766 3 23 -3 -24 1.98052 1.78740 2 -23 3 24 0.38059 0.83180 1 -21 -3 24 2.10592 2.05766 3 21 -3 -24 3.29335 1.92580 2 -21 3 24 2.17233 1.03143 1 -19 -3 24 -0.9900 1.62836 3 19 -3 -24 -1.6581 1.26662 2 -19 3 24 0.84367 0.89138 1 17 -3 -24 33.0837 4.87717 2 -17 -3 24 17.2390 3.29133 3 -38 0 25 -0.5299 1.52885 3 36 0 -25 0.58792 1.19864 2 -36 0 25 0.02574 1.46236 3 -34 0 25 0.01615 1.54101 3 34 0 -25 0.33947 1.12763 2 -32 0 25 0.73478 1.40318 3 32 0 -25 0.65543 1.19665 2 30 0 -25 0.29372 1.09457 2 28 0 -25 1.17914 1.18823 2 26 0 -25 -0.0758 1.21228 2 24 0 -25 2.08293 1.37832 2 22 0 -25 -0.2036 1.35066 2 20 0 -25 -0.3026 1.39579 2 -20 0 25 0.30653 0.88514 1 18 0 -25 0.14236 1.33837 2 -18 0 25 0.75507 0.79256 1 -16 0 25 0.74408 0.85866 1 16 0 -25 0.03626 1.33857 2 -14 0 25 -0.4160 0.85598 1 -12 0 25 0.93396 0.91621 1 -37 -1 25 9.79690 2.61184 3 -35 -1 25 10.0522 2.35677 3 35 -1 -25 7.84222 2.06399 2 35 1 -25 10.0611 1.91150 2 33 -1 -25 9.28182 2.29559 2 -33 -1 25 8.03043 2.34127 3 33 1 -25 13.6573 2.21834 2 31 -1 -25 5.31553 1.92032 2 -31 -1 25 0.39094 1.67390 3 31 1 -25 5.73667 1.47813 2 29 -1 -25 3.38138 1.72573 2 -29 -1 25 2.25753 1.67365 3 29 1 -25 5.83041 1.59269 2 -27 -1 25 4.80261 1.93569 3 27 -1 -25 3.91230 1.65806 2 27 1 -25 4.44119 1.51599 2 25 -1 -25 6.28433 1.95524 2 -25 -1 25 9.84650 2.40731 3 -25 1 25 6.65012 1.40657 1 25 1 -25 15.0158 2.38173 2 23 -1 -25 54.8904 4.46490 2 23 1 -25 50.3294 3.90690 2 -23 1 25 49.9378 3.32866 1 21 -1 -25 1.00890 1.36311 2 -21 1 25 0.62385 0.81874 1 21 1 -25 -0.1473 1.21582 2 19 -1 -25 10.8022 2.63597 2 19 1 -25 7.68697 2.20651 2 -19 1 25 9.06760 1.55507 1 17 -1 -25 8.81431 2.50614 2 -17 1 25 7.49558 1.54093 1 15 -1 -25 1.39575 1.70084 2 -15 1 25 0.54101 0.78318 1 13 -1 -25 -1.1895 1.62211 2 -13 1 25 -0.1355 0.78477 1 -34 -2 25 23.6847 3.89687 3 34 2 -25 33.3763 2.95196 2 -32 -2 25 2.66788 1.98781 3 32 -2 -25 4.01959 1.93348 2 32 2 -25 9.00381 1.64713 2 -30 -2 25 0.82149 1.77245 3 30 -2 -25 -0.3570 1.38214 2 -30 2 25 1.01086 0.89416 1 30 2 -25 2.62926 1.13883 2 -28 -2 25 7.89643 2.43675 3 28 -2 -25 6.67524 2.21123 2 -28 2 25 6.40961 1.45583 1 28 2 -25 11.0914 1.90298 2 -26 -2 25 12.6014 2.82298 3 26 -2 -25 17.1425 3.15972 2 -26 2 25 7.86128 1.60317 1 26 2 -25 13.7645 2.09243 2 24 -2 -25 4.68489 2.11536 2 -24 -2 25 2.12472 1.81018 3 24 2 -25 5.64985 1.48892 2 -24 2 25 3.09448 1.05076 1 -22 -2 25 -0.8450 1.61439 3 22 -2 -25 -0.0152 1.44386 2 -22 2 25 0.31594 0.81203 1 -20 -2 25 1.16506 1.70580 3 20 -2 -25 1.78974 1.70533 2 -20 2 25 0.61889 0.77855 1 18 -2 -25 9.83322 2.68885 2 -18 2 25 8.32469 1.73163 1 16 -2 -25 3.83892 2.13760 2 -16 2 25 2.68030 1.20755 1 -36 0 26 13.4502 2.82717 3 -34 0 26 19.0978 3.96307 3 34 0 -26 19.8646 2.89963 2 32 0 -26 1.97022 1.29389 2 30 0 -26 8.98938 2.13007 2 28 0 -26 0.75492 1.27184 2 26 0 -26 1.30512 1.50936 2 24 0 -26 19.3032 3.01617 2 22 0 -26 0.28711 1.39722 2 20 0 -26 1.86013 1.51895 2 -18 0 26 12.3309 2.10227 1 18 0 -26 21.2921 3.32296 2 -16 0 26 39.8035 3.19286 1 -35 -1 26 56.6889 5.44824 3 33 -1 -26 2.14893 1.65930 2 -33 -1 26 1.98862 1.99586 3 33 1 -26 2.90856 1.41196 2 -31 -1 26 3.29566 1.99067 3 31 -1 -26 1.35443 1.65364 2 31 1 -26 3.46834 1.41156 2 29 -1 -26 1.78859 1.59359 2 -29 -1 26 3.36278 1.92113 3 29 1 -26 2.95003 1.46964 2 27 -1 -26 1.69970 1.59246 2 27 1 -26 2.14971 1.28607 2 25 -1 -26 0.26692 1.37658 2 -25 1 26 -0.5210 0.88539 1 25 1 -26 0.93291 1.30235 2 23 -1 -26 11.5259 2.56865 2 23 1 -26 9.28529 2.19465 2 -23 1 26 7.83222 1.47832 1 21 -1 -26 3.09986 2.01199 2 21 1 -26 1.50851 1.55146 2 -21 1 26 -0.2295 0.82996 1 19 -1 -26 -0.1387 1.59698 2 -19 1 26 0.37840 0.87000 1 17 -1 -26 1.39878 1.67673 2 -17 1 26 1.31660 1.00754 1 -30 -2 26 -0.3337 1.64726 3 30 2 -26 2.61544 1.20326 2 -30 2 26 0.27734 0.90650 1 -28 -2 26 20.8791 3.44332 3 28 2 -26 20.0041 2.58828 2 26 -2 -26 10.3435 3.28614 2 -26 -2 26 4.36673 2.16594 3 26 2 -26 6.86449 1.66487 2 -26 2 26 2.63980 1.05065 1 -24 -2 26 37.1154 4.49298 3 24 -2 -26 49.7680 6.03016 2 -22 -2 26 3.00817 2.08449 3 22 -2 -26 4.83194 2.28757 2 -22 2 26 4.81382 1.36093 1 -20 2 26 0.62559 1.01453 1 32 0 -27 0.98229 2.03756 2 30 0 -27 0.79838 1.57888 2 28 0 -27 1.79812 1.64102 2 26 0 -27 0.08226 1.58214 2 24 0 -27 1.41458 1.63898 2 22 0 -27 0.19896 1.53251 2 20 0 -27 0.25981 1.62001 2 31 1 -27 2.92533 1.52098 2 29 -1 -27 4.08935 2.84410 2 29 1 -27 5.12880 1.69837 2 27 -1 -27 0.01824 1.71441 2 27 1 -27 0.71182 1.38521 2 25 -1 -27 2.56114 1.90841 2 25 1 -27 5.84644 1.88923 2 23 -1 -27 0.44885 1.66560 2 -23 1 27 1.71687 1.10340 1 23 1 -27 2.36046 1.84873 2 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.9686 _exptl_absorpt_correction_T_min 0.7685 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71098 32.282 5.172 20.512 89.936 128.550 90.060 ) ; _shelx_hkl_checksum 17396 _shelx_res_file ; mo_in4meo142_0m.res created by SHELXL-2014/7 TITL mo_in4meo142_0m in I2/a (142K) CELL 0.71073 20.2960 5.1263 25.0050 90.000 90.950 90.000 ZERR 8 0.0070 0.0018 0.0090 0.000 0.020 0.000 LATT 2 SYMM 0.50000 - X , Y , - Z SFAC C H N O UNIT 112 112 16 32 TEMP -131.000 SIZE 0.046 0.126 0.808 L.S. 10 BOND $H FMAP 2 2 60 PLAN 20 ACTA CONF WGHT 0.072900 0.711200 FVAR 0.20486 O1 4 0.998421 1.243070 0.544469 11.00000 0.02092 0.02397 = 0.02706 0.00244 -0.00556 -0.00489 O2 4 0.778375 0.163945 0.645360 11.00000 0.02110 0.02484 = 0.02474 0.00418 -0.00482 -0.00564 O3 4 0.705144 0.227697 0.579014 11.00000 0.02350 0.02568 = 0.02266 0.00530 -0.00329 -0.00222 O4 4 0.561367 -0.660055 0.709952 11.00000 0.02491 0.02880 = 0.02957 0.00812 -0.00060 -0.00686 N1 3 0.839757 0.561950 0.599667 11.00000 0.02216 0.02107 = 0.02564 0.00163 0.00058 -0.00158 N2 3 0.917266 1.324251 0.484314 11.00000 0.02005 0.01950 = 0.02292 0.00330 -0.00318 -0.00307 C1 1 0.933030 0.844222 0.592993 11.00000 0.01904 0.02785 = 0.02653 0.00506 -0.00530 -0.00309 AFIX 43 H1A 2 0.975232 0.894802 0.606323 11.00000 -1.20000 AFIX 0 C2 1 0.899039 0.642499 0.616747 11.00000 0.02502 0.02769 = 0.02690 0.00791 -0.00368 -0.00007 AFIX 43 H2A 2 0.918810 0.557065 0.646664 11.00000 -1.20000 AFIX 0 C3 1 0.812699 0.686137 0.557846 11.00000 0.01991 0.02464 = 0.02514 0.00021 -0.00188 -0.00260 AFIX 43 H3A 2 0.770500 0.631185 0.545295 11.00000 -1.20000 AFIX 0 C4 1 0.843029 0.891268 0.531778 11.00000 0.02148 0.02279 = 0.02155 0.00202 -0.00301 -0.00092 AFIX 43 H4A 2 0.821857 0.975148 0.502296 11.00000 -1.20000 AFIX 0 C5 1 0.904725 0.971503 0.549518 11.00000 0.01938 0.01702 = 0.01888 -0.00154 0.00058 -0.00004 C6 1 0.943488 1.191600 0.525094 11.00000 0.01836 0.01786 = 0.01914 -0.00234 -0.00066 -0.00023 C7 1 0.682982 -0.099716 0.643995 11.00000 0.01958 0.02018 = 0.01914 -0.00130 -0.00109 -0.00194 C8 1 0.707119 -0.252769 0.685666 11.00000 0.02127 0.02345 = 0.02331 0.00115 -0.00391 -0.00223 AFIX 43 H8A 2 0.750882 -0.225925 0.698573 11.00000 -1.20000 AFIX 0 C9 1 0.668496 -0.445028 0.708975 11.00000 0.02423 0.02281 = 0.02352 0.00374 -0.00453 -0.00119 AFIX 43 H9A 2 0.685620 -0.548356 0.737517 11.00000 -1.20000 AFIX 0 C10 1 0.604548 -0.483434 0.689858 11.00000 0.02254 0.02063 = 0.02182 -0.00019 0.00174 -0.00291 C11 1 0.580368 -0.334235 0.647273 11.00000 0.01859 0.02946 = 0.02571 0.00313 -0.00391 -0.00410 AFIX 43 H11A 2 0.536909 -0.363045 0.633860 11.00000 -1.20000 AFIX 0 C12 1 0.619055 -0.145788 0.624607 11.00000 0.02155 0.02619 = 0.02163 0.00355 -0.00325 -0.00098 AFIX 43 H12A 2 0.602204 -0.045772 0.595467 11.00000 -1.20000 AFIX 0 C13 1 0.722628 0.111456 0.619587 11.00000 0.01892 0.02062 = 0.02051 -0.00142 -0.00119 -0.00002 C14 1 0.581937 -0.807794 0.755482 11.00000 0.03343 0.03110 = 0.02967 0.01080 0.00146 -0.00639 AFIX 137 H14A 2 0.546120 -0.923648 0.766269 11.00000 -1.50000 H14B 2 0.593180 -0.689185 0.784985 11.00000 -1.50000 H14C 2 0.620666 -0.912212 0.746524 11.00000 -1.50000 AFIX 0 H1N2 2 0.941694 1.462573 0.471282 11.00000 0.03919 H2N2 2 0.876395 1.280189 0.470389 11.00000 0.03870 H1O2 2 0.801256 0.309400 0.628134 11.00000 0.06814 HKLF 4 1 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 0.0000 1.0000 REM mo_in4meo142_0m in I2/a (142K) REM R1 = 0.0462 for 2502 Fo > 4sig(Fo) and 0.0646 for all 3363 data REM 194 parameters refined using 0 restraints END WGHT 0.0728 0.7193 REM Highest difference peak 0.314, deepest hole -0.240, 1-sigma level 0.053 Q1 1 0.6797 -0.3160 0.7027 11.00000 0.05 0.31 Q2 1 0.6606 -0.1093 0.6378 11.00000 0.05 0.31 Q3 1 0.8804 0.9412 0.5390 11.00000 0.05 0.30 Q4 1 0.6391 -0.4744 0.7001 11.00000 0.05 0.27 Q5 1 0.9206 1.0426 0.5375 11.00000 0.05 0.26 Q6 1 0.6978 0.0210 0.6380 11.00000 0.05 0.24 Q7 1 0.6026 -0.4317 0.6644 11.00000 0.05 0.22 Q8 1 0.8392 0.7576 0.5361 11.00000 0.05 0.21 Q9 1 0.8629 0.6386 0.6144 11.00000 0.05 0.20 Q10 1 0.9008 0.7844 0.6151 11.00000 0.05 0.19 Q11 1 0.9212 0.6945 0.5971 11.00000 0.05 0.19 Q12 1 0.7026 -0.2241 0.6741 11.00000 0.05 0.17 Q13 1 0.7949 0.6981 0.5600 11.00000 0.05 0.17 Q14 1 0.5198 -0.6416 0.7175 11.00000 0.05 0.16 Q15 1 0.5386 -0.8202 0.7789 11.00000 0.05 0.16 Q16 1 0.5357 -0.8906 0.7392 11.00000 0.05 0.15 Q17 1 0.5990 -0.2305 0.6393 11.00000 0.05 0.15 Q18 1 0.8217 0.8509 0.5569 11.00000 0.05 0.15 Q19 1 0.5821 -0.5861 0.7005 11.00000 0.05 0.14 Q20 1 0.9222 0.8919 0.5644 11.00000 0.05 0.14 ; _shelx_res_checksum 90854 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' 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 O O1 0.99842(5) 1.24307(18) 0.54447(4) 0.0241(2) Uani d 1 O O2 0.77837(5) 0.16395(19) 0.64536(4) 0.0236(2) Uani d 1 O O3 0.70514(5) 0.22770(19) 0.57901(4) 0.0240(2) Uani d 1 O O4 0.56137(5) -0.66005(19) 0.70995(4) 0.0278(3) Uani d 1 N N1 0.83976(5) 0.5619(2) 0.59967(4) 0.0230(3) Uani d 1 N N2 0.91727(6) 1.3243(2) 0.48431(4) 0.0209(3) Uani d 1 C C1 0.93303(7) 0.8442(3) 0.59299(5) 0.0245(3) Uani d 1 H H1A 0.9752 0.8948 0.6063 0.029 Uiso calc 1 C C2 0.89904(7) 0.6425(3) 0.61675(6) 0.0266(3) Uani d 1 H H2A 0.9188 0.5571 0.6467 0.032 Uiso calc 1 C C3 0.81270(7) 0.6861(3) 0.55785(6) 0.0233(3) Uani d 1 H H3A 0.7705 0.6312 0.5453 0.028 Uiso calc 1 C C4 0.84303(6) 0.8913(3) 0.53178(5) 0.0220(3) Uani d 1 H H4A 0.8219 0.9751 0.5023 0.026 Uiso calc 1 C C5 0.90473(6) 0.9715(2) 0.54952(5) 0.0184(3) Uani d 1 C C6 0.94349(6) 1.1916(2) 0.52509(5) 0.0185(3) Uani d 1 C C7 0.68298(6) -0.0997(3) 0.64400(5) 0.0197(3) Uani d 1 C C8 0.70712(7) -0.2528(3) 0.68567(5) 0.0227(3) Uani d 1 H H8A 0.7509 -0.2259 0.6986 0.027 Uiso calc 1 C C9 0.66850(6) -0.4450(3) 0.70898(5) 0.0236(3) Uani d 1 H H9A 0.6856 -0.5484 0.7375 0.028 Uiso calc 1 C C10 0.60455(6) -0.4834(3) 0.68986(5) 0.0216(3) Uani d 1 C C11 0.58037(7) -0.3342(3) 0.64727(5) 0.0246(3) Uani d 1 H H11A 0.5369 -0.3630 0.6339 0.030 Uiso calc 1 C C12 0.61906(7) -0.1458(3) 0.62461(5) 0.0232(3) Uani d 1 H H12A 0.6022 -0.0458 0.5955 0.028 Uiso calc 1 C C13 0.72263(6) 0.1115(3) 0.61959(5) 0.0200(3) Uani d 1 C C14 0.58194(8) -0.8078(3) 0.75548(6) 0.0314(3) Uani d 1 H H14A 0.5461 -0.9236 0.7663 0.047 Uiso calc 1 H H14B 0.5932 -0.6892 0.7850 0.047 Uiso calc 1 H H14C 0.6207 -0.9122 0.7465 0.047 Uiso calc 1 H H1N2 0.9417(8) 1.463(4) 0.4713(7) 0.039(5) Uiso d 1 H H2N2 0.8764(9) 1.280(4) 0.4704(7) 0.039(5) Uiso d 1 H H1O2 0.8013(11) 0.309(4) 0.6281(8) 0.068(7) 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 O1 0.0209(5) 0.0240(5) 0.0271(5) -0.0049(4) -0.0056(4) 0.0024(4) O2 0.0211(5) 0.0248(5) 0.0247(5) -0.0056(4) -0.0048(4) 0.0042(4) O3 0.0235(5) 0.0257(5) 0.0227(5) -0.0022(4) -0.0033(4) 0.0053(4) O4 0.0249(5) 0.0288(5) 0.0296(6) -0.0069(4) -0.0006(4) 0.0081(4) N1 0.0222(6) 0.0211(6) 0.0256(6) -0.0016(5) 0.0006(4) 0.0016(5) N2 0.0200(6) 0.0195(6) 0.0229(6) -0.0031(4) -0.0032(4) 0.0033(4) C1 0.0190(6) 0.0278(7) 0.0265(7) -0.0031(5) -0.0053(5) 0.0051(6) C2 0.0250(7) 0.0277(7) 0.0269(7) -0.0001(6) -0.0037(6) 0.0079(6) C3 0.0199(6) 0.0246(7) 0.0251(7) -0.0026(5) -0.0019(5) 0.0002(5) C4 0.0215(6) 0.0228(7) 0.0215(7) -0.0009(5) -0.0030(5) 0.0020(5) C5 0.0194(6) 0.0170(6) 0.0189(6) 0.0000(5) 0.0006(5) -0.0015(5) C6 0.0184(6) 0.0179(6) 0.0191(6) -0.0002(5) -0.0007(5) -0.0023(5) C7 0.0196(6) 0.0202(6) 0.0191(6) -0.0019(5) -0.0011(5) -0.0013(5) C8 0.0213(7) 0.0235(7) 0.0233(7) -0.0022(5) -0.0039(5) 0.0011(5) C9 0.0242(7) 0.0228(7) 0.0235(7) -0.0012(5) -0.0045(5) 0.0037(5) C10 0.0225(7) 0.0206(6) 0.0218(7) -0.0029(5) 0.0017(5) -0.0002(5) C11 0.0186(6) 0.0295(7) 0.0257(7) -0.0041(5) -0.0039(5) 0.0031(6) C12 0.0215(6) 0.0262(7) 0.0216(7) -0.0010(5) -0.0032(5) 0.0035(5) C13 0.0189(6) 0.0206(6) 0.0205(6) 0.0000(5) -0.0012(5) -0.0014(5) C14 0.0334(8) 0.0311(8) 0.0297(8) -0.0064(6) 0.0015(6) 0.0108(6) 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 C13 O2 H1O2 110.4(13) C10 O4 C14 117.81(11) C3 N1 C2 117.38(12) C6 N2 H1N2 116.8(11) C6 N2 H2N2 120.7(11) H1N2 N2 H2N2 122.5(15) C2 C1 C5 119.10(12) C2 C1 H1A 120.5 C5 C1 H1A 120.5 N1 C2 C1 123.17(13) N1 C2 H2A 118.4 C1 C2 H2A 118.4 N1 C3 C4 123.36(12) N1 C3 H3A 118.3 C4 C3 H3A 118.3 C5 C4 C3 118.75(12) C5 C4 H4A 120.6 C3 C4 H4A 120.6 C4 C5 C1 118.23(12) C4 C5 C6 124.54(11) C1 C5 C6 117.22(11) O1 C6 N2 122.56(12) O1 C6 C5 118.25(11) N2 C6 C5 119.19(11) C8 C7 C12 118.63(12) C8 C7 C13 122.25(12) C12 C7 C13 119.11(12) C7 C8 C9 121.35(12) C7 C8 H8A 119.3 C9 C8 H8A 119.3 C10 C9 C8 119.02(12) C10 C9 H9A 120.5 C8 C9 H9A 120.5 O4 C10 C9 124.77(12) O4 C10 C11 115.22(12) C9 C10 C11 120.01(12) C12 C11 C10 120.33(12) C12 C11 H11A 119.8 C10 C11 H11A 119.8 C11 C12 C7 120.64(12) C11 C12 H12A 119.7 C7 C12 H12A 119.7 O3 C13 O2 122.65(12) O3 C13 C7 122.93(12) O2 C13 C7 114.42(11) O4 C14 H14A 109.5 O4 C14 H14B 109.5 H14A C14 H14B 109.5 O4 C14 H14C 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C6 1.2367(16) O2 C13 1.3205(16) O2 H1O2 0.98(2) O3 C13 1.2241(16) O4 C10 1.3619(16) O4 C14 1.4242(17) N1 C3 1.3347(18) N1 C2 1.3355(18) N2 C6 1.3294(17) N2 H1N2 0.927(19) N2 H2N2 0.92(2) C1 C2 1.3826(19) C1 C5 1.3845(18) C1 H1A 0.9500 C2 H2A 0.9500 C3 C4 1.3867(19) C3 H3A 0.9500 C4 C5 1.3840(18) C4 H4A 0.9500 C5 C6 1.5103(18) C7 C8 1.3872(18) C7 C12 1.3976(18) C7 C13 1.4860(18) C8 C9 1.3931(19) C8 H8A 0.9500 C9 C10 1.3897(19) C9 H9A 0.9500 C10 C11 1.3937(19) C11 C12 1.3732(19) C11 H11A 0.9500 C12 H12A 0.9500 C14 H14A 0.9800 C14 H14B 0.9800 C14 H14C 0.9800 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 N2 H1N2 O1 5_786 0.929(19) 1.980(19) 2.8992(18) 170.3(15) yes N2 H2N2 O3 2_666 0.923(18) 2.066(18) 2.9655(19) 164.5(16) yes O2 H1O2 N1 . 0.98(2) 1.68(2) 2.6583(17) 178.6(17) yes C4 H4A O3 2_666 0.9500 2.4600 3.393(2) 166.00 yes C11 H11A O1 6_565 0.9500 2.4400 3.074(2) 124.00 yes C14 H14A O4 4_546 0.9800 2.5700 3.543(2) 170.00 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 C3 N1 C2 C1 -0.5(2) C5 C1 C2 N1 0.3(2) C2 N1 C3 C4 0.1(2) N1 C3 C4 C5 0.5(2) C3 C4 C5 C1 -0.7(2) C3 C4 C5 C6 -179.96(12) C2 C1 C5 C4 0.3(2) C2 C1 C5 C6 179.65(12) C4 C5 C6 O1 -179.50(13) C1 C5 C6 O1 1.20(18) C4 C5 C6 N2 1.34(19) C1 C5 C6 N2 -177.97(12) C12 C7 C8 C9 -1.5(2) C13 C7 C8 C9 178.21(12) C7 C8 C9 C10 0.1(2) C14 O4 C10 C9 3.2(2) C14 O4 C10 C11 -176.46(12) C8 C9 C10 O4 -178.35(12) C8 C9 C10 C11 1.3(2) O4 C10 C11 C12 178.52(12) C9 C10 C11 C12 -1.1(2) C10 C11 C12 C7 -0.3(2) C8 C7 C12 C11 1.6(2) C13 C7 C12 C11 -178.08(12) C8 C7 C13 O3 171.32(13) C12 C7 C13 O3 -9.0(2) C8 C7 C13 O2 -8.79(19) C12 C7 C13 O2 170.93(12) _cod_database_fobs_code 2108057