#------------------------------------------------------------------------------ #$Date: 2019-11-08 04:08:20 +0200 (Fri, 08 Nov 2019) $ #$Revision: 225303 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/66/7156618.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7156618 loop_ _publ_author_name 'Shen, Jiabin' 'Xu, Jun' 'Cai, Heng' 'Shen, Chao' 'Zhang, Pengfei' _publ_section_title ; Platinum(ii)-catalyzed selective para C-H alkoxylation of arylamines through a coordinating activation strategy. ; _journal_issue 3 _journal_name_full 'Organic & biomolecular chemistry' _journal_page_first 490 _journal_page_last 497 _journal_paper_doi 10.1039/c8ob02942c _journal_volume 17 _journal_year 2019 _chemical_formula_moiety 'C21 H16 N2 O2' _chemical_formula_sum 'C21 H16 N2 O2' _chemical_formula_weight 328.36 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2018-07-21 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2018-08-01 deposited with the CCDC. 2018-12-12 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 99.193(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.1601(7) _cell_length_b 16.0224(18) _cell_length_c 16.6437(19) _cell_measurement_reflns_used 3047 _cell_measurement_temperature 273.15 _cell_measurement_theta_max 26.333 _cell_measurement_theta_min 2.542 _cell_volume 1621.6(3) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 273.15 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'Bruker P4' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_unetI/netI 0.0284 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 9560 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.491 _diffrn_reflns_theta_min 1.775 _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6873 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2014/3 (Bruker,2014/3) was used for absorption correction. wR2(int) was 0.0565 before and 0.0355 after correction. The Ratio of minimum to maximum transmission is 0.9218. The \l/2 correction factor is 0.00150.' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.345 _exptl_crystal_description block _exptl_crystal_F_000 688 _refine_diff_density_max 0.238 _refine_diff_density_min -0.166 _refine_diff_density_rms 0.045 _refine_ls_extinction_coef 0.0182(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 228 _refine_ls_number_reflns 3656 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.017 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0432 _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^)+(0.0524P)^2^+0.3199P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1025 _refine_ls_wR_factor_ref 0.1175 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2614 _reflns_number_total 3656 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8ob02942c2.cif _cod_data_source_block 180717xj _cod_depositor_comments 'Adding full bibliography for 7156618.cif.' _cod_database_code 7156618 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: N1(H1), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21) 2.b Idealised Me refined as rotating group: C6(H6A,H6B,H6C) ; _shelx_res_file ; TITL 180717xj_0P 1 21/c 1 R = 0.09 180717xj.res created by SHELXL-2018/3 at 10:14:42 on 21-Jul-2018 CELL 0.71073 6.1601 16.0224 16.6437 90 99.193 90 ZERR 4 0.0007 0.0018 0.0019 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C 2.310 20.844 1.02 10.208 1.589 0.569 0.865 51.651 0.216 0.003 0.002 = 11.5 0.68 12.01 SFAC H SFAC N 12.213 0.006 3.132 9.893 2.013 28.998 1.166 0.583 -11.529 0.006 = 0.003 19.6 0.68 14.01 SFAC O 3.049 13.277 2.287 5.701 1.546 0.324 0.867 32.909 0.251 0.011 0.006 = 32.5 0.68 16 UNIT 84 64 8 8 L.S. 5 PLAN -20 TEMP 0 CONF fmap 2 acta OMIT 0 0 2 REM REM REM WGHT 0.052400 0.319900 EXTI 0.018151 FVAR 0.49532 O1 4 0.379224 0.490807 0.645989 11.00000 0.06495 0.05174 = 0.05906 -0.01307 -0.00504 0.00981 O2 4 -0.545938 0.693515 0.532126 11.00000 0.04795 0.07126 = 0.04566 -0.00651 -0.00896 0.00659 N1 3 0.273488 0.607873 0.708919 11.00000 0.04016 0.04469 = 0.04432 -0.00465 0.00214 0.00093 AFIX 43 H1 2 0.317053 0.640777 0.749087 11.00000 -1.20000 AFIX 0 N2 3 0.620921 0.595118 0.825354 11.00000 0.04089 0.03863 = 0.04181 0.00172 0.00966 0.00224 C1 1 0.409696 0.543622 0.700094 11.00000 0.04259 0.03706 = 0.04341 0.00302 0.01022 -0.00212 C2 1 0.069816 0.628599 0.661515 11.00000 0.03606 0.04221 = 0.03921 0.00273 0.00517 -0.00178 C3 1 -0.059399 0.693113 0.691101 11.00000 0.03862 0.03462 = 0.03479 0.00543 0.00555 -0.00567 C4 1 -0.269810 0.712152 0.645602 11.00000 0.03940 0.03705 = 0.03390 0.00655 0.00364 -0.00500 C5 1 -0.343456 0.669269 0.571305 11.00000 0.04049 0.04779 = 0.03736 0.00436 0.00107 -0.00235 C6 1 -0.630496 0.652738 0.457776 11.00000 0.05996 0.09720 = 0.04989 -0.01537 -0.01421 0.00274 AFIX 137 H6A 2 -0.534406 0.662680 0.418705 11.00000 -1.50000 H6B 2 -0.774202 0.674187 0.437286 11.00000 -1.50000 H6C 2 -0.639945 0.593828 0.467161 11.00000 -1.50000 AFIX 0 C7 1 -0.214883 0.609466 0.543865 11.00000 0.05221 0.05595 = 0.03774 -0.00649 0.00082 -0.00153 AFIX 43 H7 2 -0.263195 0.582304 0.494889 11.00000 -1.20000 AFIX 0 C8 1 -0.009475 0.588959 0.589653 11.00000 0.04947 0.05350 = 0.04435 -0.00688 0.00636 0.00623 AFIX 43 H8 2 0.074874 0.547411 0.570709 11.00000 -1.20000 AFIX 0 C9 1 -0.403390 0.772918 0.675896 11.00000 0.04193 0.04161 = 0.04567 0.00627 0.00165 0.00263 AFIX 43 H9 2 -0.541906 0.784711 0.646918 11.00000 -1.20000 AFIX 0 C10 1 -0.332193 0.814343 0.746782 11.00000 0.05268 0.03888 = 0.05058 -0.00018 0.00731 0.00598 AFIX 43 H10 2 -0.422041 0.853848 0.765931 11.00000 -1.20000 AFIX 0 C11 1 -0.123034 0.797241 0.790786 11.00000 0.05615 0.04270 = 0.04308 -0.00431 -0.00072 -0.00189 AFIX 43 H11 2 -0.074092 0.826214 0.838675 11.00000 -1.20000 AFIX 0 C12 1 0.009447 0.738481 0.764023 11.00000 0.04300 0.04005 = 0.04190 0.00123 -0.00138 -0.00110 AFIX 43 H12 2 0.147339 0.727997 0.794136 11.00000 -1.20000 AFIX 0 C13 1 0.611954 0.541710 0.764407 11.00000 0.03971 0.03480 = 0.04231 0.00382 0.01033 -0.00111 C14 1 0.807616 0.596549 0.882299 11.00000 0.04178 0.03695 = 0.04039 0.00300 0.01020 0.00027 C15 1 0.989039 0.543280 0.877365 11.00000 0.03991 0.03972 = 0.04499 0.00282 0.00985 -0.00027 C16 1 0.967737 0.485891 0.812499 11.00000 0.04220 0.04427 = 0.05792 -0.00387 0.01173 0.00820 AFIX 43 H16 2 1.081355 0.448798 0.808086 11.00000 -1.20000 AFIX 0 C17 1 0.781351 0.484570 0.756263 11.00000 0.04576 0.04165 = 0.04962 -0.00840 0.00884 0.00125 AFIX 43 H17 2 0.765927 0.446767 0.713327 11.00000 -1.20000 AFIX 0 C18 1 1.181461 0.551219 0.936074 11.00000 0.04103 0.05919 = 0.05734 -0.00117 0.00637 0.00407 AFIX 43 H18 2 1.301782 0.516983 0.933016 11.00000 -1.20000 AFIX 0 C19 1 1.191751 0.608333 0.996724 11.00000 0.05232 0.07117 = 0.05530 -0.00563 -0.00390 -0.00354 AFIX 43 H19 2 1.319653 0.613417 1.034528 11.00000 -1.20000 AFIX 0 C20 1 1.010420 0.659911 1.002850 11.00000 0.06872 0.06012 = 0.05017 -0.01289 0.00490 0.00029 AFIX 43 H20 2 1.018997 0.698338 1.045119 11.00000 -1.20000 AFIX 0 C21 1 0.822142 0.654244 0.947540 11.00000 0.05521 0.05061 = 0.04920 -0.00596 0.00909 0.00761 AFIX 43 H21 2 0.702893 0.688329 0.952626 11.00000 -1.20000 AFIX 0 HKLF 4 REM 180717xj_0P 1 21/c 1 R = 0.09 REM wR2 = 0.1175, GooF = S = 1.017, Restrained GooF = 1.017 for all data REM R1 = 0.0432 for 2614 Fo > 4sig(Fo) and 0.0662 for all 3656 data REM 228 parameters refined using 0 restraints END WGHT 0.0524 0.3199 REM Highest difference peak 0.238, deepest hole -0.166, 1-sigma level 0.045 Q1 1 0.6638 0.5030 0.7620 11.00000 0.05 0.24 Q2 1 0.9601 0.5024 0.8616 11.00000 0.05 0.19 Q3 1 0.9293 0.5775 0.8697 11.00000 0.05 0.17 Q4 1 -0.2587 0.6603 0.5499 11.00000 0.05 0.17 Q5 1 0.5133 0.6409 0.8271 11.00000 0.05 0.17 Q6 1 0.3478 0.4968 0.6861 11.00000 0.05 0.17 Q7 1 -0.1241 0.8045 0.8601 11.00000 0.05 0.16 Q8 1 -0.1917 0.8172 0.7524 11.00000 0.05 0.16 Q9 1 -0.0424 0.7855 0.7648 11.00000 0.05 0.16 Q10 1 -0.3140 0.7552 0.6498 11.00000 0.05 0.16 Q11 1 -0.7629 0.7040 0.4291 11.00000 0.05 0.16 Q12 1 -0.3438 0.8161 0.6971 11.00000 0.05 0.16 Q13 1 -0.3494 0.8361 0.7501 11.00000 0.05 0.15 Q14 1 -0.3074 0.6218 0.5699 11.00000 0.05 0.15 Q15 1 -0.0072 0.6684 0.6736 11.00000 0.05 0.15 Q16 1 -0.3038 0.7015 0.6037 11.00000 0.05 0.15 Q17 1 0.7411 0.4633 0.6847 11.00000 0.05 0.14 Q18 1 1.2820 0.4803 0.9370 11.00000 0.05 0.14 Q19 1 -0.3203 0.6799 0.6191 11.00000 0.05 0.14 Q20 1 0.3536 0.5214 0.6091 11.00000 0.05 0.14 ; _shelx_res_checksum 12656 _shelx_hkl_file ; -1 0 0 245.59 4.62 -2 0 0 26.06 0.88 -3 0 0 755.95 14.25 -4 0 0 -0.24 0.41 -5 0 0 474.99 9.89 6 0 0 5.15 0.94 7 0 0 0.75 0.73 0 1 0 -0.01 0.02 1 1 0 900.71 15.95 -1 1 0 869.62 15.99 -2 -1 0 3.34 0.35 -2 1 0 3.89 0.39 -3 -1 0 0.00 0.30 -3 1 0 -0.48 0.24 -4 -1 0 25.17 1.25 -4 1 0 23.13 1.22 -5 1 0 52.93 2.13 5 1 0 50.31 2.10 -6 1 0 7.95 1.10 6 1 0 7.81 1.03 7 -1 0 3.82 1.01 7 1 0 3.69 0.94 -1 2 0 5.32 0.33 1 2 0 5.08 0.30 2 -2 0 108.28 2.33 -2 2 0 106.02 2.49 2 2 0 109.42 2.41 3 -2 0 1.57 0.31 3 2 0 1.19 0.32 -3 2 0 1.62 0.41 4 -2 0 0.78 0.37 -4 2 0 1.27 0.53 4 2 0 1.60 0.46 5 -2 0 142.60 3.73 5 2 0 147.86 3.90 -5 2 0 152.88 4.10 -6 2 0 0.77 0.74 6 2 0 0.48 0.63 7 2 0 3.13 0.99 -7 2 0 3.28 0.95 7 2 0 2.75 0.92 0 3 0 -0.20 0.12 1 -3 0 455.33 8.19 1 3 0 423.68 8.24 -1 3 0 438.37 8.21 1 3 0 437.19 8.09 2 -3 0 42.47 1.12 -2 3 0 40.80 1.28 2 3 0 41.93 1.19 3 -3 0 17.26 0.79 3 3 0 17.45 0.84 -3 3 0 17.69 0.94 4 -3 0 49.75 1.63 -4 3 0 46.68 1.84 4 3 0 52.12 1.78 -5 3 0 7.33 1.00 5 3 0 7.49 0.91 6 3 0 16.02 1.41 -6 3 0 13.99 1.42 -7 3 0 1.54 0.92 7 3 0 1.78 0.99 0 4 0 50.40 1.22 0 4 0 50.25 1.18 1 -4 0 59.43 1.38 -1 4 0 60.62 1.51 -1 4 0 59.84 1.32 1 4 0 60.70 1.43 1 4 0 57.46 1.54 2 -4 0 502.99 9.11 2 4 0 475.86 9.46 -2 4 0 483.03 9.11 -2 4 0 487.27 9.38 2 4 0 490.78 9.20 3 -4 0 44.56 1.34 3 4 0 42.99 1.43 -3 4 0 46.53 1.60 4 -4 0 1.29 0.38 -4 4 0 -0.36 0.46 4 4 0 -0.38 0.38 5 4 0 8.52 0.98 -5 4 0 8.15 1.05 6 4 0 4.08 0.90 6 4 0 5.30 1.03 -6 4 0 3.53 0.90 -7 4 0 14.44 1.63 7 4 0 13.97 1.76 0 5 0 0.08 0.18 -1 5 0 20.97 0.64 1 5 0 20.18 0.81 1 5 0 21.93 0.78 -1 5 0 19.92 0.79 2 -5 0 202.05 4.14 -2 5 0 209.85 4.46 2 5 0 210.85 4.57 2 5 0 207.00 4.26 -2 5 0 207.63 4.14 3 -5 0 88.92 2.21 -3 5 0 92.89 2.58 3 5 0 96.60 2.69 3 5 0 90.86 2.36 4 -5 0 25.72 1.11 4 5 0 26.58 1.49 -4 5 0 30.17 1.48 4 5 0 28.50 1.28 5 5 0 5.55 0.97 -5 5 0 6.03 0.95 5 5 0 6.50 0.91 6 5 0 -1.49 0.69 6 5 0 -0.75 0.49 -6 5 0 -0.09 0.69 7 5 0 12.99 1.66 -7 5 0 14.89 1.74 0 6 0 214.89 4.78 0 6 0 280.74 4.98 1 6 0 57.93 1.53 1 6 0 57.05 1.61 -1 6 0 57.81 1.39 -1 6 0 59.43 1.62 2 -6 0 52.02 1.40 -2 6 0 51.49 1.64 -2 6 0 50.80 1.35 2 6 0 53.71 1.73 2 6 0 51.11 1.49 3 -6 0 40.49 1.29 3 6 0 42.46 1.71 -3 6 0 42.52 1.61 3 6 0 40.25 1.42 4 -6 0 32.42 1.88 4 6 0 30.25 1.64 4 6 0 32.62 1.44 -4 6 0 29.95 1.55 5 6 0 16.14 1.16 -5 6 0 13.09 1.30 5 6 0 14.62 1.43 -6 6 0 0.12 0.67 6 6 0 0.87 0.84 -7 6 0 9.23 1.43 7 6 0 7.06 1.40 0 7 0 0.18 0.24 0 7 0 -0.05 0.19 1 7 0 26.14 1.04 1 7 0 25.14 0.97 -1 7 0 25.31 0.82 -1 7 0 26.15 1.02 2 -7 0 1.79 0.34 2 7 0 1.28 0.37 2 7 0 1.56 0.42 -2 7 0 1.53 0.39 -2 7 0 1.57 0.27 3 -7 0 0.59 0.32 3 7 0 0.49 0.40 -3 7 0 0.66 0.39 3 7 0 1.23 0.51 -3 7 0 0.53 0.30 -4 7 0 254.90 6.00 4 7 0 255.87 6.14 4 7 0 259.15 5.65 5 7 0 7.00 1.12 -5 7 0 7.39 1.04 5 7 0 7.97 0.94 -6 7 0 3.68 0.98 6 7 0 4.07 1.05 -7 7 0 0.68 0.97 7 7 0 0.94 1.06 0 8 0 10.62 0.62 0 8 0 11.07 0.67 1 8 0 32.69 1.17 1 8 0 31.65 1.21 -1 8 0 34.59 1.04 -1 8 0 33.65 1.24 2 8 0 52.86 1.64 2 8 0 55.59 1.86 -2 8 0 50.33 1.74 -2 8 0 52.05 1.42 3 -8 0 1.38 0.39 -3 8 0 1.67 0.36 3 8 0 1.85 0.57 -3 8 0 0.21 0.41 3 8 0 0.20 0.39 -4 8 0 14.94 1.26 4 8 0 13.64 1.12 4 8 0 15.57 1.37 -5 8 0 12.23 1.28 5 8 0 9.69 1.02 5 8 0 8.50 1.21 6 8 0 1.26 0.89 -6 8 0 2.84 0.97 7 8 0 0.29 0.97 -7 8 0 2.04 1.00 0 9 0 0.46 0.32 0 9 0 -0.07 0.24 1 9 0 240.04 5.03 -1 9 0 234.76 5.13 -1 9 0 239.16 4.81 1 9 0 241.42 5.12 2 9 0 73.09 2.26 -2 9 0 69.23 2.18 2 9 0 67.72 2.01 -2 9 0 69.62 1.78 3 -9 0 7.75 0.68 3 9 0 8.79 0.97 -3 9 0 8.35 0.89 3 9 0 9.39 0.87 4 9 0 58.25 2.44 4 9 0 61.84 2.14 -4 9 0 63.65 2.46 -5 9 0 2.44 0.80 5 9 0 2.84 0.90 6 9 0 15.18 1.70 -6 9 0 20.05 1.73 7 9 0 0.34 1.03 0 10 0 290.78 5.91 0 10 0 289.40 6.06 -1 10 0 7.95 0.58 -1 10 0 8.59 0.75 1 10 0 8.25 0.75 1 10 0 8.85 0.74 2 10 0 94.43 2.53 -2 10 0 93.86 2.72 2 10 0 93.19 2.73 -2 10 0 92.32 2.31 3 10 0 5.72 0.87 -3 10 0 7.17 0.90 3 10 0 6.90 0.84 4 10 0 7.41 0.92 -4 10 0 8.33 1.05 4 10 0 6.93 1.07 5 10 0 10.72 1.37 -5 10 0 12.78 1.39 6 10 0 7.22 1.39 -6 10 0 4.82 1.11 0 11 0 0.04 0.40 0 11 0 0.03 0.32 -1 11 0 0.83 0.32 -1 11 0 3.82 0.61 1 11 0 0.31 0.45 1 11 0 1.33 0.46 2 11 0 2.66 0.62 -2 11 0 2.32 0.59 2 11 0 1.79 0.61 3 11 0 5.98 0.84 -3 11 0 6.94 0.92 3 11 0 6.91 1.02 -4 11 0 2.13 0.73 4 11 0 3.31 0.86 4 11 0 1.12 0.65 5 11 0 4.87 1.18 -5 11 0 5.27 1.06 6 11 0 2.40 1.14 -6 11 0 3.12 1.08 0 12 0 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1.16 1 -5 -18 0.15 0.73 1 5 -18 0.08 0.68 0 5 -18 29.13 1.91 -1 5 -18 1.16 0.97 1 5 18 0.44 0.81 -2 5 -18 -1.96 0.75 2 5 18 -0.19 0.83 4 -6 -18 1.13 1.00 4 6 -18 0.89 0.84 4 6 -18 0.98 0.80 3 -6 -18 -0.53 0.91 3 6 -18 -0.35 0.75 3 6 -18 1.67 0.79 2 -6 -18 4.02 1.12 2 6 -18 4.32 0.93 1 -6 -18 0.70 0.80 1 6 -18 0.62 0.77 0 6 18 12.30 1.40 0 6 -18 12.37 1.44 1 6 18 19.50 1.84 -1 6 -18 16.76 1.75 2 6 18 0.85 0.92 -2 6 -18 0.79 1.02 4 -7 -18 -1.68 0.87 4 7 -18 -0.14 0.91 4 7 -18 0.45 0.83 3 -7 -18 2.00 1.02 3 7 -18 2.40 0.92 2 -7 -18 1.02 0.87 2 7 -18 3.26 0.89 1 -7 -18 2.36 0.89 1 7 -18 2.19 0.91 0 7 18 29.01 2.05 0 7 -18 29.52 2.01 1 7 18 9.87 1.51 -1 7 -18 8.89 1.44 2 7 18 8.68 1.73 -2 7 -18 12.34 1.72 4 -8 -18 2.13 1.21 4 8 -18 2.12 1.00 4 8 -18 3.13 1.00 3 -8 -18 -1.42 0.88 3 8 -18 -0.13 0.69 2 -8 -18 0.98 1.01 2 8 -18 3.44 1.03 1 -8 -18 0.20 0.75 1 8 -18 0.25 0.75 0 8 -18 6.66 1.22 0 8 18 8.79 1.37 -1 8 -18 3.24 1.14 1 8 18 1.72 1.09 -2 8 -18 -0.21 0.87 3 -9 -18 -0.61 0.87 3 9 -18 1.48 0.82 2 -9 -18 3.77 1.12 2 9 -18 2.83 1.04 1 -9 -18 -0.92 0.73 -1 9 18 0.02 0.80 1 9 -18 -0.26 0.75 0 9 18 1.69 0.94 0 9 -18 1.47 0.89 -1 9 -18 8.62 1.42 1 9 18 9.06 1.52 3 -10 -18 7.46 1.43 3 10 -18 8.32 1.36 2 -10 -18 0.60 0.95 2 10 -18 2.13 1.00 -1 10 18 1.57 0.89 1 10 -18 0.28 0.83 0 10 -18 12.39 1.64 0 10 18 10.42 1.46 -1 10 -18 6.27 1.29 2 -11 -18 2.47 1.15 2 11 -18 3.69 1.09 1 11 -18 0.99 0.89 -1 11 18 0.16 0.88 0 11 -18 3.72 1.21 4 0 -19 0.63 0.99 3 0 -19 -1.30 0.76 2 0 -19 -0.27 0.64 0 0 -19 -0.69 0.64 -1 0 -19 0.45 0.84 4 -1 -19 0.30 0.92 4 1 -19 1.40 1.10 3 -1 -19 -0.92 0.69 3 1 -19 0.14 0.83 2 -1 -19 16.76 1.60 2 1 -19 16.27 2.31 1 1 -19 0.99 0.71 0 -1 -19 8.83 1.26 0 1 -19 12.09 1.45 -1 -1 -19 -0.57 0.64 -1 1 -19 -0.40 0.77 -2 1 -19 11.24 1.55 4 -2 -19 29.91 2.43 4 2 -19 29.25 2.36 3 -2 -19 -0.32 0.90 3 2 -19 1.52 0.83 2 -2 -19 6.15 1.11 1 2 -19 3.56 0.99 0 2 -19 3.04 0.94 -1 2 -19 0.10 0.81 -2 2 -19 1.00 0.86 2 2 19 -1.75 1.27 4 -3 -19 0.12 0.98 4 3 -19 2.02 1.09 3 -3 -19 0.04 0.86 3 3 -19 0.95 0.80 2 -3 -19 2.85 0.92 2 3 -19 4.13 0.94 1 -3 -19 0.12 0.78 1 3 -19 0.53 0.75 0 3 -19 12.33 1.43 -1 3 -19 -1.08 0.78 -2 3 -19 0.43 0.86 2 3 19 0.90 0.99 4 -4 -19 1.36 1.03 4 4 -19 2.95 1.12 3 -4 -19 0.13 0.95 3 4 -19 0.03 0.81 2 -4 -19 0.09 0.82 2 4 -19 0.41 0.66 1 -4 -19 3.28 0.90 1 4 -19 5.69 1.12 0 4 -19 4.84 1.09 -1 4 -19 4.24 1.15 2 4 19 -0.63 0.83 -2 4 -19 -1.20 0.86 4 -5 -19 -0.70 0.87 4 5 -19 -0.36 0.89 3 -5 -19 0.24 0.91 3 5 -19 1.76 0.83 2 -5 -19 1.29 0.84 2 5 -19 0.87 0.80 1 -5 -19 3.20 0.93 1 5 -19 5.06 1.00 0 5 -19 2.16 0.98 1 5 19 -0.87 0.76 -1 5 -19 0.69 0.98 -2 5 -19 0.93 1.08 2 5 19 -0.22 0.93 4 -6 -19 2.38 1.18 4 6 -19 1.03 0.92 3 -6 -19 -0.02 0.99 3 6 -19 1.31 0.85 2 -6 -19 2.52 1.02 2 6 -19 1.67 0.90 1 -6 -19 16.98 1.64 1 6 -19 20.22 1.78 0 6 -19 4.47 1.11 -1 6 -19 0.76 0.99 1 6 19 0.73 0.92 3 -7 -19 -0.70 0.84 3 7 -19 0.14 0.77 2 -7 -19 1.26 0.99 2 7 -19 2.85 0.97 1 -7 -19 0.60 0.88 1 7 -19 -0.08 0.74 0 7 -19 2.38 1.06 1 7 19 0.26 0.92 -1 7 -19 1.14 1.05 3 -8 -19 2.95 1.14 3 8 -19 2.19 0.91 2 -8 -19 1.42 0.94 2 8 -19 0.58 0.77 1 -8 -19 0.33 0.89 1 8 -19 1.27 0.94 0 8 -19 13.00 1.59 0 8 19 11.33 1.54 1 8 19 5.24 1.50 -1 8 -19 6.04 1.33 2 -9 -19 1.29 0.98 2 9 -19 1.28 0.87 1 9 -19 14.77 1.65 0 9 -19 8.19 1.45 0 9 19 11.09 1.53 4 0 -20 15.78 1.89 3 0 -20 1.39 0.94 0 0 -20 8.88 1.34 -1 0 -20 0.37 0.76 4 -1 -20 -0.09 0.87 4 1 -20 -0.94 0.94 3 -1 -20 0.40 0.86 3 1 -20 -0.01 0.88 2 -1 -20 8.92 1.34 1 1 -20 1.86 1.45 0 1 -20 3.72 1.08 -1 -1 -20 0.77 0.89 -1 1 -20 -0.26 0.85 4 -2 -20 1.26 1.05 4 2 -20 3.29 1.25 3 -2 -20 2.75 1.02 3 2 -20 5.73 1.24 2 -2 -20 -0.86 0.81 1 2 -20 34.32 2.14 0 2 -20 -0.06 0.84 -1 2 -20 -0.18 0.83 3 -3 -20 -1.08 0.86 3 3 -20 1.45 1.14 2 -3 -20 0.67 0.87 2 3 -20 0.85 1.23 1 3 -20 30.76 2.07 0 3 -20 0.14 0.86 -1 3 -20 -0.09 0.85 3 -4 -20 1.01 0.95 2 -4 -20 1.18 0.86 2 4 -20 2.62 0.90 1 4 -20 26.34 1.98 0 4 -20 1.06 0.92 -1 4 -20 2.77 1.05 3 -5 -20 0.97 0.98 2 -5 -20 -0.46 0.80 2 5 -20 -0.05 0.68 1 -5 -20 2.16 0.94 1 5 -20 2.41 0.91 0 5 -20 2.45 1.09 -1 5 -20 -0.42 0.93 3 -6 -20 0.33 0.87 3 6 -20 0.98 0.86 2 -6 -20 0.66 0.90 2 6 -20 0.98 0.80 1 -6 -20 2.18 0.95 1 6 -20 3.13 1.04 0 6 -20 9.30 1.42 2 -7 -20 0.00 0.95 2 7 -20 2.08 0.89 1 -7 -20 0.26 0.84 1 7 -20 3.26 1.00 0 7 -20 4.69 1.19 3 0 -21 -0.43 0.93 0 0 -21 -0.18 1.19 3 -1 -21 1.06 1.00 3 1 -21 2.29 1.04 0 1 -21 0.15 0.74 1 2 -21 6.03 1.41 0 2 -21 0.84 0.89 2 -3 -21 -0.42 0.75 1 3 -21 0.32 0.73 0 3 -21 1.88 1.01 2 -4 -21 0.26 0.81 2 4 -21 0.49 0.92 1 4 -21 1.81 0.98 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 60964 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn O1 O 0.3792(2) 0.49081(7) 0.64599(7) 0.0602(3) Uani 1 1 d . O2 O -0.54594(18) 0.69352(8) 0.53213(6) 0.0568(3) Uani 1 1 d . N1 N 0.2735(2) 0.60787(8) 0.70892(7) 0.0436(3) Uani 1 1 d . H1 H 0.317053 0.640777 0.749087 0.052 Uiso 1 1 calc R N2 N 0.62092(19) 0.59512(7) 0.82535(7) 0.0401(3) Uani 1 1 d . C1 C 0.4097(2) 0.54362(9) 0.70009(9) 0.0407(3) Uani 1 1 d . C2 C 0.0698(2) 0.62860(9) 0.66151(8) 0.0393(3) Uani 1 1 d . C3 C -0.0594(2) 0.69311(8) 0.69110(8) 0.0360(3) Uani 1 1 d . C4 C -0.2698(2) 0.71215(8) 0.64560(8) 0.0370(3) Uani 1 1 d . C5 C -0.3435(2) 0.66927(10) 0.57131(9) 0.0424(4) Uani 1 1 d . C6 C -0.6305(3) 0.65274(14) 0.45778(11) 0.0715(6) Uani 1 1 d . H6A H -0.534406 0.662680 0.418705 0.107 Uiso 1 1 calc GR H6B H -0.774202 0.674187 0.437286 0.107 Uiso 1 1 calc GR H6C H -0.639945 0.593828 0.467161 0.107 Uiso 1 1 calc GR C7 C -0.2149(3) 0.60947(10) 0.54386(9) 0.0493(4) Uani 1 1 d . H7 H -0.263195 0.582304 0.494889 0.059 Uiso 1 1 calc R C8 C -0.0095(3) 0.58896(10) 0.58965(9) 0.0492(4) Uani 1 1 d . H8 H 0.074874 0.547411 0.570709 0.059 Uiso 1 1 calc R C9 C -0.4034(2) 0.77292(9) 0.67590(9) 0.0437(4) Uani 1 1 d . H9 H -0.541906 0.784711 0.646918 0.052 Uiso 1 1 calc R C10 C -0.3322(3) 0.81434(10) 0.74678(9) 0.0475(4) Uani 1 1 d . H10 H -0.422041 0.853848 0.765931 0.057 Uiso 1 1 calc R C11 C -0.1230(3) 0.79724(10) 0.79079(9) 0.0483(4) Uani 1 1 d . H11 H -0.074092 0.826214 0.838675 0.058 Uiso 1 1 calc R C12 C 0.0094(2) 0.73848(9) 0.76402(9) 0.0425(3) Uani 1 1 d . H12 H 0.147339 0.727997 0.794136 0.051 Uiso 1 1 calc R C13 C 0.6120(2) 0.54171(9) 0.76441(9) 0.0385(3) Uani 1 1 d . C14 C 0.8076(2) 0.59655(9) 0.88230(8) 0.0393(3) Uani 1 1 d . C15 C 0.9890(2) 0.54328(9) 0.87736(9) 0.0412(3) Uani 1 1 d . C16 C 0.9677(3) 0.48589(10) 0.81250(10) 0.0477(4) Uani 1 1 d . H16 H 1.081355 0.448798 0.808086 0.057 Uiso 1 1 calc R C17 C 0.7814(2) 0.48457(10) 0.75626(9) 0.0455(4) Uani 1 1 d . H17 H 0.765927 0.446767 0.713327 0.055 Uiso 1 1 calc R C18 C 1.1815(3) 0.55122(11) 0.93607(10) 0.0527(4) Uani 1 1 d . H18 H 1.301782 0.516983 0.933016 0.063 Uiso 1 1 calc R C19 C 1.1918(3) 0.60833(12) 0.99672(11) 0.0610(5) Uani 1 1 d . H19 H 1.319653 0.613417 1.034528 0.073 Uiso 1 1 calc R C20 C 1.0104(3) 0.65991(12) 1.00285(10) 0.0602(5) Uani 1 1 d . H20 H 1.018997 0.698338 1.045119 0.072 Uiso 1 1 calc R C21 C 0.8221(3) 0.65424(10) 0.94754(10) 0.0516(4) Uani 1 1 d . H21 H 0.702893 0.688329 0.952626 0.062 Uiso 1 1 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0649(8) 0.0517(7) 0.0591(7) -0.0131(6) -0.0050(6) 0.0098(6) O2 0.0480(7) 0.0713(8) 0.0457(6) -0.0065(6) -0.0090(5) 0.0066(5) N1 0.0402(7) 0.0447(7) 0.0443(7) -0.0047(5) 0.0021(5) 0.0009(5) N2 0.0409(7) 0.0386(6) 0.0418(7) 0.0017(5) 0.0097(5) 0.0022(5) C1 0.0426(8) 0.0371(8) 0.0434(8) 0.0030(6) 0.0102(6) -0.0021(6) C2 0.0361(8) 0.0422(8) 0.0392(8) 0.0027(6) 0.0052(6) -0.0018(6) C3 0.0386(8) 0.0346(7) 0.0348(7) 0.0054(6) 0.0055(6) -0.0057(6) C4 0.0394(8) 0.0370(7) 0.0339(7) 0.0066(6) 0.0036(6) -0.0050(6) C5 0.0405(8) 0.0478(9) 0.0374(7) 0.0044(6) 0.0011(6) -0.0024(7) C6 0.0600(11) 0.0972(16) 0.0499(10) -0.0154(10) -0.0142(9) 0.0027(11) C7 0.0522(9) 0.0560(10) 0.0377(8) -0.0065(7) 0.0008(7) -0.0015(7) C8 0.0495(9) 0.0535(9) 0.0444(9) -0.0069(7) 0.0064(7) 0.0062(7) C9 0.0419(8) 0.0416(8) 0.0457(8) 0.0063(6) 0.0016(7) 0.0026(6) C10 0.0527(9) 0.0389(8) 0.0506(9) -0.0002(7) 0.0073(7) 0.0060(7) C11 0.0561(10) 0.0427(9) 0.0431(8) -0.0043(7) -0.0007(7) -0.0019(7) C12 0.0430(8) 0.0400(8) 0.0419(8) 0.0012(6) -0.0014(6) -0.0011(6) C13 0.0397(8) 0.0348(7) 0.0423(8) 0.0038(6) 0.0103(6) -0.0011(6) C14 0.0418(8) 0.0369(7) 0.0404(8) 0.0030(6) 0.0102(6) 0.0003(6) C15 0.0399(8) 0.0397(8) 0.0450(8) 0.0028(6) 0.0099(6) -0.0003(6) C16 0.0422(9) 0.0443(9) 0.0579(10) -0.0039(7) 0.0117(7) 0.0082(7) C17 0.0458(9) 0.0417(8) 0.0496(9) -0.0084(7) 0.0088(7) 0.0012(6) C18 0.0410(9) 0.0592(10) 0.0573(10) -0.0012(8) 0.0064(7) 0.0041(7) C19 0.0523(10) 0.0712(12) 0.0553(10) -0.0056(9) -0.0039(8) -0.0035(9) C20 0.0687(12) 0.0601(11) 0.0502(10) -0.0129(8) 0.0049(8) 0.0003(9) C21 0.0552(10) 0.0506(9) 0.0492(9) -0.0060(7) 0.0091(8) 0.0076(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 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 C5 O2 C6 117.61(13) C1 N1 C2 129.12(13) C13 N2 C14 118.02(12) O1 C1 N1 125.45(14) O1 C1 C13 121.25(13) N1 C1 C13 113.30(12) N1 C2 C3 117.96(12) C8 C2 N1 122.61(14) C8 C2 C3 119.42(13) C4 C3 C2 118.53(12) C12 C3 C2 123.66(13) C12 C3 C4 117.80(13) C5 C4 C3 119.63(13) C9 C4 C3 119.20(13) C9 C4 C5 121.16(13) O2 C5 C4 114.62(13) C7 C5 O2 124.92(13) C7 C5 C4 120.46(14) C5 C7 C8 120.08(14) C2 C8 C7 121.83(14) C10 C9 C4 121.13(14) C9 C10 C11 119.87(15) C12 C11 C10 120.71(14) C11 C12 C3 121.26(14) N2 C13 C1 117.41(12) N2 C13 C17 123.58(14) C17 C13 C1 119.01(13) N2 C14 C15 122.16(13) N2 C14 C21 118.98(13) C21 C14 C15 118.85(14) C16 C15 C14 117.34(14) C16 C15 C18 123.56(14) C18 C15 C14 119.09(14) C17 C16 C15 120.17(14) C16 C17 C13 118.66(14) C19 C18 C15 120.56(16) C18 C19 C20 120.48(17) C21 C20 C19 120.78(16) C20 C21 C14 120.21(15) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C1 1.2281(17) O2 C5 1.3682(18) O2 C6 1.423(2) N1 C1 1.3508(18) N1 C2 1.4109(18) N2 C13 1.3215(18) N2 C14 1.3686(18) C1 C13 1.508(2) C2 C3 1.439(2) C2 C8 1.373(2) C3 C4 1.4258(19) C3 C12 1.4202(19) C4 C5 1.424(2) C4 C9 1.418(2) C5 C7 1.367(2) C7 C8 1.408(2) C9 C10 1.364(2) C10 C11 1.404(2) C11 C12 1.366(2) C13 C17 1.411(2) C14 C15 1.419(2) C14 C21 1.418(2) C15 C16 1.408(2) C15 C18 1.416(2) C16 C17 1.361(2) C18 C19 1.356(2) C19 C20 1.406(3) C20 C21 1.364(2) 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 O1 C1 C13 N2 -172.81(13) O1 C1 C13 C17 8.0(2) O2 C5 C7 C8 -179.45(14) N1 C1 C13 N2 7.46(18) N1 C1 C13 C17 -171.76(13) N1 C2 C3 C4 -177.30(12) N1 C2 C3 C12 1.8(2) N1 C2 C8 C7 178.86(14) N2 C13 C17 C16 -2.2(2) N2 C14 C15 C16 -2.2(2) N2 C14 C15 C18 176.68(13) N2 C14 C21 C20 -176.71(15) C1 N1 C2 C3 170.65(13) C1 N1 C2 C8 -8.4(2) C1 C13 C17 C16 176.96(13) C2 N1 C1 O1 1.3(2) C2 N1 C1 C13 -178.96(13) C2 C3 C4 C5 -2.04(19) C2 C3 C4 C9 177.15(12) C2 C3 C12 C11 -177.76(14) C3 C2 C8 C7 -0.2(2) C3 C4 C5 O2 -178.95(12) C3 C4 C5 C7 0.7(2) C3 C4 C9 C10 1.2(2) C4 C3 C12 C11 1.4(2) C4 C5 C7 C8 0.9(2) C4 C9 C10 C11 0.3(2) C5 C4 C9 C10 -179.58(14) C5 C7 C8 C2 -1.2(2) C6 O2 C5 C4 -179.51(14) C6 O2 C5 C7 0.9(2) C8 C2 C3 C4 1.8(2) C8 C2 C3 C12 -179.10(14) C9 C4 C5 O2 1.88(19) C9 C4 C5 C7 -178.47(14) C9 C10 C11 C12 -1.0(2) C10 C11 C12 C3 0.1(2) C12 C3 C4 C5 178.80(12) C12 C3 C4 C9 -2.02(19) C13 N2 C14 C15 0.3(2) C13 N2 C14 C21 179.05(13) C14 N2 C13 C1 -177.23(12) C14 N2 C13 C17 2.0(2) C14 C15 C16 C17 1.9(2) C14 C15 C18 C19 0.7(2) C15 C14 C21 C20 2.1(2) C15 C16 C17 C13 0.2(2) C15 C18 C19 C20 0.8(3) C16 C15 C18 C19 179.46(16) C18 C15 C16 C17 -176.93(15) C18 C19 C20 C21 -0.8(3) C19 C20 C21 C14 -0.7(3) C21 C14 C15 C16 179.06(14) C21 C14 C15 C18 -2.1(2)