#------------------------------------------------------------------------------ #$Date: 2016-08-05 06:37:12 +0300 (Fri, 05 Aug 2016) $ #$Revision: 184958 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/32/1543270.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_1543270 loop_ _publ_author_name 'Ho, Hon Eong' 'Oniwa, Kazuaki' 'Yamamoto, Yoshinori' 'Jin, Tienan' _publ_section_title ; N-Methyl Transfer Induced Copper-Mediated Oxidative Diamination of Alkynes. ; _journal_issue 10 _journal_name_full 'Organic letters' _journal_page_first 2487 _journal_page_last 2490 _journal_paper_doi 10.1021/acs.orglett.6b01067 _journal_volume 18 _journal_year 2016 _chemical_formula_moiety 'C16 H14 N2' _chemical_formula_sum 'C16 H14 N2' _chemical_formula_weight 234.29 _chemical_name_common 5,10-dimethyl-5,10-dihydroindolo[3,2-b]indole _chemical_name_systematic ;Indoloindole; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/a 1' _symmetry_space_group_name_Hall '-P 2yab' _symmetry_space_group_name_H-M 'P 1 21/a 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014 _cell_angle_alpha 90 _cell_angle_beta 113.4303(14) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.8715(6) _cell_length_b 5.5938(2) _cell_length_c 17.2693(10) _cell_measurement_reflns_used 126 _cell_measurement_temperature 300 _cell_measurement_theta_max 54.91 _cell_measurement_theta_min 8.91 _cell_volume 1229.51(10) _computing_cell_refinement 'RAPID AUTO' _computing_data_collection 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_molecular_graphics 'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)' _computing_publication_material 'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _diffrn_ambient_temperature 300 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Rigaku RAPID-S' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_unetI/netI 0.0229 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 11442 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.479 _diffrn_reflns_theta_min 3.201 _diffrn_source 'sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_T_max 0.970 _exptl_absorpt_correction_T_min 0.947 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_crystal_colour white _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_description cubic _exptl_crystal_F_000 496 _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.4 _refine_diff_density_max 0.486 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.039 _refine_ls_extinction_coef 0.030(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 166 _refine_ls_number_reflns 2819 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.067 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0588 _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^)+(0.1039P)^2^+0.2359P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1768 _refine_ls_wR_factor_ref 0.1908 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2086 _reflns_number_total 2819 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ol6b01067_si_002.cif _cod_data_source_block Indoloindole _cod_depositor_comments 'Adding full bibliography for 1543270.cif.' _cod_database_code 1543270 _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 0.942 _shelx_estimated_absorpt_t_max 0.985 _shelxl_version_number 2014-3 _shelx_res_file ; TITL REM Yadorkari-X generated CELL 0.71075 13.8715 5.5938 17.2693 90.0000 113.4303 90.0000 ZERR 4.0 0.0006 0.0002 0.0010 0.0000 0.0014 0.0000 LATT 1 SYMM 1/2-X, 1/2+Y, -Z REM SPGR P21/a monoclinic SFAC C H N UNIT 64 56 8 SIZE 0.80 0.50 0.20 TEMP 23.0 L.S. 20 FMAP 2 PLAN -25 ACTA CONF HTAB LIST 4 BOND $H MERG 2 OMIT -10.000000 55.000000 OMIT 1 1 6 WGHT 0.103900 0.235900 EXTI 0.029810 FVAR 5.10685 C1 1 0.484495 0.438922 0.463126 11.00000 0.05254 0.05523 = 0.05794 -0.00864 0.00804 0.00167 N1 3 0.419218 0.254594 0.461046 11.00000 0.06319 0.06320 = 0.07655 -0.01298 0.01142 -0.00881 C2 1 0.407630 0.261823 0.536706 11.00000 0.05347 0.06857 = 0.07409 0.00621 0.01917 0.01132 C3 1 0.348481 0.105699 0.564568 11.00000 0.06484 0.07483 = 0.15203 0.02262 0.03339 0.00657 AFIX 43 H1 2 0.309643 -0.019551 0.531311 11.00000 -1.20000 AFIX 0 C4 1 0.351577 0.150145 0.645362 11.00000 0.09754 0.13120 = 0.16843 0.08154 0.08530 0.04776 AFIX 43 H2 2 0.313618 0.051791 0.666442 11.00000 -1.20000 AFIX 0 C5 1 0.408614 0.333276 0.693749 11.00000 0.12116 0.14826 = 0.11070 0.05981 0.07215 0.07310 AFIX 43 H3 2 0.408740 0.355618 0.747153 11.00000 -1.20000 AFIX 0 C6 1 0.464318 0.481840 0.667436 11.00000 0.08895 0.10451 = 0.06463 0.01204 0.02898 0.04117 AFIX 43 H4 2 0.501853 0.606235 0.702036 11.00000 -1.20000 AFIX 0 C7 1 0.466324 0.450979 0.588460 11.00000 0.05554 0.06521 = 0.06323 0.00574 0.01697 0.01539 C8 1 0.367540 0.094354 0.390076 11.00000 0.07873 0.08218 = 0.11084 -0.03996 -0.00147 -0.00889 AFIX 137 H5 2 0.398515 0.112753 0.349635 11.00000 -1.50000 H6 2 0.294091 0.132542 0.363994 11.00000 -1.50000 H7 2 0.375946 -0.067866 0.409814 11.00000 -1.50000 AFIX 0 C9 1 0.528555 0.444617 1.037380 11.00000 0.04686 0.03902 = 0.05155 0.00323 0.02388 0.00346 N2 3 0.474271 0.249835 1.048320 11.00000 0.04722 0.04237 = 0.05482 0.00708 0.02370 0.00036 C10 1 0.380500 0.239352 0.978457 11.00000 0.04598 0.04403 = 0.05527 -0.00360 0.02727 0.00078 C11 1 0.299975 0.072924 0.959473 11.00000 0.05700 0.04978 = 0.06964 -0.00380 0.03451 -0.00707 AFIX 43 H8 2 0.303901 -0.051171 0.996448 11.00000 -1.20000 AFIX 0 C12 1 0.214127 0.097625 0.884120 11.00000 0.05193 0.06625 = 0.07591 -0.01507 0.02925 -0.01614 AFIX 43 H9 2 0.159835 -0.013174 0.870097 11.00000 -1.20000 AFIX 0 C13 1 0.206277 0.283692 0.828334 11.00000 0.04878 0.07920 = 0.06059 -0.00842 0.01718 -0.00950 AFIX 43 H10 2 0.146938 0.295300 0.778183 11.00000 -1.20000 AFIX 0 C14 1 0.285016 0.450369 0.846380 11.00000 0.05096 0.06027 = 0.05463 0.00148 0.02139 0.00060 AFIX 43 H11 2 0.279206 0.574584 0.808987 11.00000 -1.20000 AFIX 0 C15 1 0.374446 0.430189 0.922215 11.00000 0.04267 0.04444 = 0.05326 -0.00466 0.02446 0.00043 C16 1 0.505833 0.097424 1.122509 11.00000 0.06570 0.05114 = 0.06002 0.01354 0.03327 0.00705 AFIX 137 H12 2 0.580998 0.098872 1.151112 11.00000 -1.50000 H13 2 0.482256 -0.063004 1.105601 11.00000 -1.50000 H14 2 0.475085 0.155769 1.159800 11.00000 -1.50000 AFIX 0 HKLF 4 1 -1 0 0 0 -1 0 1 0 1 REM REM R1 = 0.0588 for 2086 Fo > 4sig(Fo) and 0.0754 for all 2819 data REM 166 parameters refined using 0 restraints END WGHT 0.1036 0.2387 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.486, deepest hole -0.207, 1-sigma level 0.039 Q1 1 0.4665 0.3742 0.3994 11.00000 0.05 0.49 Q2 1 0.4042 0.2155 0.3327 11.00000 0.05 0.30 Q3 1 0.5431 0.2138 1.1785 11.00000 0.05 0.19 Q4 1 0.3343 0.2180 0.3300 11.00000 0.05 0.19 Q5 1 0.3134 0.1189 0.5886 11.00000 0.05 0.18 Q6 1 0.6404 0.6587 1.0485 11.00000 0.05 0.18 Q7 1 0.6610 0.5373 1.1113 11.00000 0.05 0.17 Q8 1 0.4386 0.0495 1.1319 11.00000 0.05 0.16 Q9 1 0.5732 -0.0155 1.1252 11.00000 0.05 0.16 Q10 1 0.5580 0.3467 1.0929 11.00000 0.05 0.16 Q11 1 0.3435 0.1417 0.5151 11.00000 0.05 0.15 Q12 1 0.4181 0.4960 0.9316 11.00000 0.05 0.15 Q13 1 0.4575 0.4326 0.6210 11.00000 0.05 0.14 Q14 1 0.2680 -0.0435 0.6217 11.00000 0.05 0.14 Q15 1 0.3346 0.1838 0.9690 11.00000 0.05 0.13 Q16 1 0.5490 0.6409 0.4300 11.00000 0.05 0.13 Q17 1 0.2955 0.0032 0.4124 11.00000 0.05 0.11 Q18 1 0.4277 -0.0052 0.3714 11.00000 0.05 0.11 Q19 1 0.2584 0.3146 0.8217 11.00000 0.05 0.10 Q20 1 0.2502 0.1357 0.9277 11.00000 0.05 0.08 Q21 1 0.4895 0.1799 1.0863 11.00000 0.05 0.08 Q22 1 0.1617 -0.0890 0.9087 11.00000 0.05 0.08 Q23 1 0.2658 0.0265 0.9127 11.00000 0.05 0.08 Q24 1 0.4853 0.5784 1.0310 11.00000 0.05 0.08 Q25 1 0.3275 -0.1413 1.0311 11.00000 0.05 0.07 ; _shelx_res_checksum 63474 _shelx_hkl_file ; 0 0 3 1820.88 33.01 0 0 -3 1867.35 33.59 0 0 441087.99 858.86 0 0 -438440.41 794.22 0 0 5 515.27 26.08 0 0 -5 505.95 32.24 0 0 614864.92 295.60 0 0 -613558.92 259.82 0 0 711088.38 226.97 0 0 -711194.61 224.08 0 0 815763.64 319.89 0 0 -815904.11 317.48 0 0 9 40.34 25.12 0 0 -9 41.94 24.14 0 0 1016203.16 358.69 0 0 -1016914.84 359.22 0 0 11 2643.29 98.18 0 0 -11 2657.30 79.80 0 0 12 5373.29 160.90 0 0 -12 5578.24 157.64 0 0 13 -24.09 23.47 0 0 -13 3.34 21.87 0 0 14 8374.27 249.15 0 0 -14 8684.22 243.43 0 0 15 280.50 57.30 0 0 -15 263.12 53.43 0 0 16 2371.61 101.52 0 0 -16 2399.62 95.23 0 0 17 291.30 68.20 0 0 -17 345.95 47.49 0 0 18 -42.87 39.91 0 0 -18 25.02 37.37 0 0 19 54.49 52.00 0 0 -19 31.07 48.25 0 0 20 71.98 42.27 0 0 -20 15.55 39.22 0 1 0 12.30 9.73 0 -1 144597.97 913.05 0 1 -145113.62 924.43 0 -1 2 170.67 14.50 0 1 -2 211.80 14.98 0 -1 -2 165.62 15.29 0 1 3 737.47 28.74 0 -1 3 725.63 26.09 0 1 -3 717.68 26.18 0 -1 -3 776.33 29.39 0 1 4 139.90 29.92 0 -1 4 158.33 19.06 0 1 -4 150.44 18.90 0 -1 -4 136.87 21.18 0 -1 5 7891.77 147.73 0 1 5 7938.63 160.23 0 1 -5 7854.06 146.88 0 -1 -5 8026.11 168.13 0 1 6 613.15 33.37 0 -1 6 625.07 30.69 0 1 -6 691.75 29.64 0 -1 -6 687.02 31.54 0 -1 7 1439.79 45.98 0 1 7 1441.49 50.19 0 -1 -7 1662.53 60.60 0 1 -7 1502.62 38.95 0 1 8 844.16 52.90 0 -1 8 876.85 40.55 0 -1 -8 835.29 39.31 0 1 -8 800.19 38.05 0 -1 9 2247.05 70.46 0 1 9 2189.73 86.97 0 1 -9 2216.46 67.69 0 -1 -9 2199.17 67.91 0 -1 10 746.11 46.73 0 1 10 775.67 48.20 0 -1 -10 769.97 44.77 0 1 -10 741.45 44.76 0 -1 11 456.66 33.66 0 1 11 498.08 45.49 0 -1 -11 534.29 42.28 0 1 -11 460.61 42.70 0 1 12 1472.47 73.04 0 -1 12 1485.99 59.21 0 1 -12 1438.70 55.72 0 -1 -12 1594.28 68.35 0 1 13 2588.65 127.74 0 -1 13 2714.04 105.23 0 1 -13 2659.02 99.19 0 -1 -13 2698.37 99.51 0 1 14 1685.20 104.86 0 -1 14 1625.90 85.55 0 1 -14 1728.69 66.05 0 -1 -14 1810.89 99.05 0 -1 15 1435.92 85.13 0 1 15 1499.07 105.72 0 1 -15 1499.85 65.85 0 -1 -15 1504.71 97.58 0 -1 16 26.42 34.47 0 1 16 -7.05 45.47 0 1 -16 22.18 25.34 0 -1 -16 10.93 30.81 0 -1 17 282.08 61.38 0 1 17 292.25 59.99 0 1 -17 434.73 45.56 0 -1 -17 409.34 56.51 0 -1 18 78.56 38.61 0 1 18 77.21 39.58 0 1 18 141.62 47.36 0 1 -18 97.47 47.75 0 -1 -18 103.61 43.18 0 1 19 84.23 46.66 0 -1 19 236.94 60.28 0 1 19 190.42 72.53 0 1 -19 152.71 55.39 0 -1 -19 259.16 66.77 0 1 20 16.23 38.15 0 -1 20 39.14 48.62 0 1 20 84.86 58.76 0 -1 -20 103.21 56.03 0 1 -20 -6.12 35.18 0 -2 0 6443.17 125.07 0 -2 1 649.18 37.04 0 2 -1 688.66 27.24 0 -2 -1 633.50 41.95 0 -2 2 610.43 26.14 0 2 -2 556.81 31.48 0 -2 3 244.60 18.52 0 2 -3 288.36 23.93 0 -2 -3 260.59 24.24 0 -2 -3 267.23 8.30 0 -2 446140.96 1025.36 0 2 -446702.94 1019.57 0 -2 -446545.71 1059.11 0 -2 5 206.72 22.61 0 2 -5 211.88 23.37 0 -2 -5 212.93 25.82 0 -2 610723.37 212.13 0 -2 -610887.05 227.08 0 2 -610853.75 212.68 0 -2 7 524.21 30.59 0 -2 -7 498.64 36.98 0 2 -7 486.29 30.97 0 2 8 2163.93 35.85 0 -2 8 2231.89 64.78 0 -2 -8 2356.58 75.00 0 2 -8 2220.21 54.76 0 2 9 14.75 8.89 0 2 9 32.63 24.79 0 -2 9 0.69 19.79 0 -2 -9 16.98 23.27 0 2 -9 18.01 19.20 0 2 10 1246.15 32.10 0 -2 10 1308.90 56.24 0 2 10 1492.27 86.52 0 -2 -10 1345.66 64.43 0 2 -10 1386.34 56.53 0 2 11 2083.27 56.63 0 2 11 2280.28 94.85 0 -2 11 2356.96 80.82 0 -2 -11 2586.67 89.85 0 2 -11 2313.00 78.27 0 -2 12 831.66 55.19 0 2 12 712.87 31.84 0 2 12 764.94 64.58 0 2 -12 925.68 52.87 0 -2 -12 773.27 60.75 0 2 13 177.19 22.93 0 2 13 224.19 64.25 0 -2 13 293.44 41.16 0 2 -13 263.46 29.39 0 -2 -13 340.94 44.82 0 -2 14 286.45 41.63 0 2 14 183.48 50.90 0 2 14 227.38 23.68 0 -2 -14 223.73 47.54 0 2 -14 225.40 40.64 0 -2 15 90.41 34.36 0 2 15 14.36 22.50 0 2 15 10.13 38.19 0 -2 -15 11.50 35.49 0 2 -15 47.83 31.20 0 -2 16 132.39 44.83 0 2 16 118.18 32.15 0 2 16 136.40 26.02 0 -2 -16 163.57 46.69 0 2 -16 141.46 41.24 0 -2 17 155.36 45.88 0 2 17 38.16 27.43 0 2 -17 198.93 43.47 0 -2 -17 333.27 64.13 0 2 18 -5.77 20.74 0 -2 18 20.18 34.39 0 -2 -18 33.35 36.97 0 2 -18 21.48 33.17 0 -2 19 9.18 39.90 0 2 -19 1.92 38.58 0 -2 -19 66.18 43.69 0 -3 0 -6.63 19.84 0 -3 1 1519.72 57.75 0 -3 -1 1518.43 51.73 0 -3 2 922.94 36.45 0 -3 -2 904.20 30.58 0 -3 -2 868.92 43.01 0 3 -2 944.04 35.60 0 -3 311248.88 241.54 0 3 -310990.86 220.10 0 -3 -311128.49 258.83 0 -3 -311159.50 237.28 0 -3 -311001.19 187.02 0 -3 4 4279.78 105.13 0 3 -4 4337.41 104.48 0 -3 -4 4454.96 125.80 0 -3 -4 4207.11 61.96 0 -3 5 3907.77 96.43 0 3 -5 4077.57 100.74 0 -3 -5 4118.61 107.65 0 -3 6 123.27 25.71 0 3 -6 103.14 25.89 0 -3 -6 103.94 39.30 0 -3 7 521.47 36.88 0 3 -7 485.57 38.09 0 -3 -7 508.97 44.78 0 -3 8 6.18 19.69 0 -3 -8 -9.93 32.50 0 3 -8 21.84 20.33 0 -3 9 2740.09 82.98 0 3 -9 2821.55 84.98 0 -3 -9 2903.83 99.40 0 -3 10 127.46 30.61 0 3 -10 138.21 31.71 0 -3 -10 148.21 40.31 0 -3 11 5044.30 137.64 0 -3 -11 5012.45 182.24 0 3 -11 4859.96 133.65 0 -3 12 426.30 45.98 0 3 -12 472.74 43.44 0 -3 -12 475.38 75.17 0 -3 13 1388.84 69.10 0 -3 -13 1337.02 80.74 0 3 -13 1208.36 64.90 0 -3 14 151.72 40.07 0 3 -14 201.31 38.63 0 -3 -14 172.76 48.45 0 -3 15 41.16 26.77 0 -3 -15 92.70 58.70 0 3 -15 92.58 34.67 0 -3 16 220.74 44.65 0 3 -16 248.31 45.53 0 -3 -16 179.87 57.39 0 -3 17 28.78 34.73 0 3 -17 20.22 34.37 0 -3 -17 30.86 44.70 0 -3 18 299.21 52.42 0 -3 -18 214.27 86.71 0 3 -18 191.18 53.36 0 -4 0 3854.26 108.11 0 -4 1 264.40 31.70 0 -4 -1 172.77 34.44 0 -4 2 5388.84 131.64 0 -4 -2 5424.19 111.08 0 -4 -2 5400.14 163.10 0 -4 3 171.72 36.67 0 -4 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49.34 54.65 -15 -2 15 30.00 69.85 -15 2 15 24.16 55.82 -15 2 15 181.45 60.58 15 2 -14 120.61 54.98 15 -2 -14 116.82 55.35 -15 -2 14 21.58 57.24 -15 -2 14 123.36 54.48 -15 2 14 77.79 44.58 -15 2 14 99.92 49.84 15 2 -13 220.33 60.07 15 -2 -13 179.37 57.88 -15 -2 13 40.06 82.72 -15 -2 13 196.00 61.12 -15 2 13 139.79 62.22 -15 2 13 250.60 56.25 15 2 -12 575.64 74.39 15 -2 -12 484.85 68.62 -15 -2 12 530.81 78.64 -15 -2 12 760.91 97.26 -15 2 12 590.96 73.29 -15 2 12 575.67 93.44 15 2 -11 26.84 45.92 15 -2 -11 -15.02 30.75 -15 -2 11 13.33 48.44 -15 -2 11 -0.85 34.71 -15 2 11 2.16 32.80 -15 2 11 36.10 46.36 15 2 -10 39.09 34.43 15 -2 -10 -27.34 30.24 -15 -2 10 -5.11 35.62 -15 -2 10 -2.11 49.09 -15 2 10 13.60 31.27 -15 2 10 72.29 48.49 15 2 -9 451.65 65.19 15 -2 -9 492.09 52.46 -15 -2 9 311.47 68.59 -15 -2 9 650.65 85.47 -15 2 9 515.50 55.06 -15 2 9 613.03 94.31 15 2 -8 727.04 70.59 15 -2 -8 750.39 57.51 -15 -2 8 889.57 98.90 -15 -2 8 708.85 92.25 -15 2 8 860.37 81.18 -15 2 8 679.51 56.05 15 2 -7 69.81 59.81 15 -2 -7 117.86 33.80 -15 -2 7 207.62 65.14 -15 -2 7 116.18 46.73 -15 2 7 126.61 54.93 -15 2 7 149.92 34.33 15 2 -6 70.85 39.88 15 -2 -6 -2.93 21.78 -15 -2 6 267.13 40.68 -15 -2 6 127.40 56.75 -15 2 6 83.91 66.50 -15 2 6 44.01 26.36 15 2 -5 -37.46 30.46 -15 -2 5 17.34 41.44 -15 -2 5 -28.46 42.70 -15 2 5 -2.93 17.42 -15 2 5 5.19 39.96 15 2 -4 29.66 35.59 -15 -2 4 63.36 48.35 -15 -2 4 39.30 38.93 -15 2 4 14.54 62.71 15 2 -3 13.31 33.87 -15 -2 3 32.32 47.35 -15 -2 3 126.85 50.48 -15 2 3 -0.54 48.57 15 -2 -2 13.25 85.97 -15 -2 2 639.08 76.52 -15 -2 2 666.52 62.51 -15 2 2 472.53 106.61 15 -2 -1 168.42 46.64 -15 -2 1 -16.77 54.34 -15 -2 1 43.55 50.07 -15 2 1 29.28 54.73 15 -2 0 49.12 52.76 -15 -2 0 8.38 42.10 -15 -2 0 10.41 45.89 -15 2 0 2.34 46.87 15 -2 1 52.42 53.47 -15 -2 -1 182.78 55.75 -15 -2 -1 129.73 60.49 15 -2 2 33.46 46.42 -15 -2 -2 86.37 47.10 -15 -2 -2 7.11 51.42 15 3 -15 -7.59 50.73 15 -3 -15 48.90 36.56 -15 -3 15 16.76 66.58 -15 3 15 1.06 37.76 -15 3 15 23.18 51.89 15 3 -14 -2.84 49.09 15 -3 -14 31.92 44.50 -15 -3 14 18.74 48.66 -15 3 14 38.41 35.07 -15 3 14 -7.39 39.66 15 3 -13 36.32 57.00 15 -3 -13 -9.47 28.32 -15 -3 13 20.96 43.83 -15 3 13 2.84 29.64 -15 3 13 25.81 48.51 15 3 -12 0.88 46.38 15 -3 -12 26.07 29.25 -15 -3 12 -2.02 46.23 -15 -3 12 10.52 60.79 -15 3 12 -29.53 54.02 -15 3 12 61.28 39.90 15 3 -11 104.37 44.52 15 -3 -11 -3.47 34.92 -15 -3 11 -4.93 42.81 -15 -3 11 1.35 43.91 -15 3 11 22.38 36.74 -15 3 11 -6.74 41.03 15 3 -10 77.71 70.80 15 -3 -10 82.42 40.00 -15 -3 10 84.89 67.00 -15 -3 10 81.71 72.42 -15 3 10 97.09 41.53 -15 3 10 95.03 51.68 15 3 -9 72.01 50.14 15 -3 -9 102.91 34.41 -15 -3 9 56.82 48.41 -15 -3 9 66.93 69.65 -15 3 9 82.32 44.44 -15 3 9 51.38 50.92 15 3 -8 32.23 39.61 15 -3 -8 3.76 24.51 -15 -3 8 27.19 41.04 -15 -3 8 73.54 49.48 -15 3 8 15.69 42.07 -15 3 8 -7.13 26.01 15 3 -7 46.46 44.81 -15 -3 7 4.08 46.21 -15 -3 7 74.98 54.45 -15 3 7 46.51 48.66 15 3 -6 95.89 44.87 -15 -3 6 11.17 63.04 -15 -3 6 78.24 53.92 -15 3 6 3.24 52.21 15 3 -5 87.22 46.92 -15 -3 5 135.69 64.15 -15 -3 5 43.12 56.71 -15 3 5 61.99 55.79 15 3 -4 76.41 55.66 15 -3 -4 -3.32 45.30 -15 -3 4 -8.43 59.13 -15 -3 4 21.98 38.53 -15 3 4 151.56 51.76 15 3 -3 70.53 57.54 15 -3 -3 23.55 63.29 -15 -3 3 90.40 58.97 -15 -3 3 36.46 51.40 -15 3 3 37.65 72.94 15 -3 -2 127.63 74.02 -15 -3 2 174.37 67.28 -15 -3 2 76.86 57.13 -15 3 2 79.03 63.10 15 -3 -1 3.29 45.96 -15 -3 1 -58.78 40.54 -15 -3 1 -2.97 45.11 15 4 -8 7.24 69.73 -15 -4 8 -5.21 54.89 -15 -4 8 20.94 56.65 -15 4 8 104.05 50.34 -15 -4 7 91.39 76.50 -15 -4 7 73.26 60.23 -15 4 7 39.10 54.90 16 0 -17 320.89 72.74 -16 0 17 100.94 78.74 -16 0 17 53.99 23.98 16 0 -16 675.84 76.83 -16 0 16 662.98 111.95 -16 0 16 416.44 53.72 16 0 -15 169.29 62.46 -16 0 15 38.72 55.26 -16 0 15 18.13 62.53 16 0 -14 -4.25 46.60 -16 0 14 20.50 42.75 -16 0 14 -35.05 37.26 16 0 -13 26.97 53.72 -16 0 13 78.37 55.67 -16 0 13 39.02 66.53 16 0 -12 426.69 57.64 -16 0 12 333.09 78.37 -16 0 12 517.72 73.88 16 0 -11 120.99 54.31 -16 0 11 91.56 54.13 -16 0 11 108.47 41.59 16 0 -10 -2.31 27.53 -16 0 10 20.91 51.12 -16 0 10 11.27 37.26 16 0 -9 412.35 69.23 -16 0 9 557.79 74.60 -16 0 9 581.76 67.52 16 0 -8 435.51 65.44 -16 0 8 368.12 72.98 -16 0 8 506.61 62.28 16 0 -7 52.59 34.29 -16 0 7 120.59 42.85 -16 0 7 144.06 52.51 16 0 -6 1422.28 86.00 -16 0 6 1673.12 87.18 -16 0 6 1627.61 136.58 16 0 -5 87.35 43.75 -16 0 5 108.70 55.44 -16 0 5 181.72 41.02 16 0 -4 123.91 42.71 -16 0 4 281.16 42.06 -16 0 4 221.82 61.14 16 0 -3 -0.61 30.32 -16 0 3 4.93 43.83 -16 0 3 72.37 29.14 -16 0 2 140.09 34.48 -16 0 2 61.55 56.19 -16 0 1 146.20 59.04 -16 0 0 -0.26 33.14 -16 0 -1 105.78 74.27 16 1 -17 123.18 64.74 16 -1 -17 258.38 76.11 -16 -1 17 92.70 68.44 -16 -1 17 96.08 50.42 -16 1 17 149.05 37.89 -16 1 17 158.99 61.28 16 1 -16 4.90 63.49 16 -1 -16 5.12 41.48 -16 -1 16 -6.14 67.35 -16 -1 16 49.52 59.19 -16 1 16 72.86 56.41 -16 1 16 34.23 47.66 16 1 -15 -14.21 44.33 16 -1 -15 24.32 50.14 -16 -1 15 15.66 49.63 -16 -1 15 45.23 61.68 -16 1 15 -15.30 60.15 -16 1 15 52.22 40.19 16 1 -14 28.17 38.75 16 -1 -14 9.14 32.76 -16 -1 14 38.61 51.43 -16 -1 14 -25.66 55.81 -16 1 14 12.10 39.35 -16 1 14 8.89 40.59 -16 1 14 -15.89 34.56 16 1 -13 8.31 36.80 16 -1 -13 -4.65 39.99 -16 -1 13 -27.78 41.00 -16 -1 13 -33.80 48.67 -16 1 13 -4.96 40.29 -16 1 13 2.81 41.78 16 1 -12 318.77 83.54 16 -1 -12 267.49 68.47 -16 -1 12 473.48 76.63 -16 -1 12 428.55 83.73 -16 1 12 439.54 94.77 -16 1 12 513.38 70.20 16 1 -11 771.85 74.67 16 -1 -11 779.44 79.05 -16 -1 11 724.89 89.73 -16 -1 11 891.38 94.76 -16 1 11 839.06 112.50 -16 1 11 815.57 82.10 16 1 -10 1807.82 99.57 16 -1 -10 1733.91 83.89 -16 -1 10 1837.61 120.18 -16 -1 10 1861.86 145.84 -16 1 10 1835.08 102.39 -16 1 10 1893.25 148.96 16 1 -9 774.56 89.84 16 -1 -9 716.45 69.51 -16 -1 9 850.84 83.41 -16 -1 9 725.03 87.13 -16 1 9 723.93 70.16 -16 1 9 778.02 86.05 16 1 -8 659.61 82.66 16 -1 -8 613.02 63.68 -16 -1 8 743.82 81.21 -16 -1 8 678.68 81.24 -16 1 8 746.58 63.15 -16 1 8 771.38 85.92 16 1 -7 51.02 49.65 16 -1 -7 10.51 37.26 -16 -1 7 118.94 48.93 -16 -1 7 180.86 49.47 -16 1 7 80.18 36.04 -16 1 7 66.98 70.32 16 1 -6 585.98 75.72 16 -1 -6 554.47 54.27 -16 -1 6 654.09 73.97 -16 -1 6 690.38 72.92 -16 1 6 656.23 80.74 -16 1 6 647.51 52.66 16 1 -5 -26.07 36.73 16 -1 -5 8.50 24.99 -16 -1 5 -28.87 50.52 -16 -1 5 15.46 27.48 -16 1 5 39.02 55.38 -16 1 5 25.24 23.57 16 1 -4 291.48 43.80 -16 -1 4 271.74 83.30 -16 -1 4 317.44 58.42 -16 1 4 357.19 70.77 -16 1 4 296.45 43.42 16 1 -3 -20.37 30.14 -16 -1 3 -5.64 31.04 -16 -1 3 2.86 34.10 -16 1 3 21.54 38.31 -16 -1 2 16.74 35.81 -16 -1 2 9.12 32.20 -16 1 2 -10.15 41.88 -16 -1 1 -0.90 28.13 -16 1 1 41.20 49.28 -16 -1 1 -25.96 43.29 -16 -1 0 97.57 46.70 -16 -1 0 152.24 53.66 -16 1 0 136.79 82.13 16 2 -15 38.68 67.04 16 -2 -15 93.88 50.52 -16 -2 15 -6.48 55.22 -16 -2 15 16.64 50.34 -16 2 15 -1.47 54.84 -16 2 15 31.08 44.75 16 2 -14 255.37 95.32 16 -2 -14 346.07 70.71 -16 -2 14 211.06 101.62 -16 -2 14 217.10 71.55 -16 2 14 406.26 58.46 -16 2 14 274.63 90.98 16 2 -13 7.24 60.86 16 -2 -13 94.03 42.66 -16 -2 13 -23.26 48.87 -16 -2 13 43.41 59.32 -16 2 13 19.88 45.93 -16 2 13 -10.26 44.85 16 2 -12 18.31 50.28 16 -2 -12 105.23 34.78 -16 -2 12 109.81 64.86 -16 -2 12 6.72 52.87 -16 2 12 29.65 47.82 -16 2 12 72.92 51.73 16 2 -11 19.72 60.56 16 -2 -11 25.21 39.57 -16 -2 11 66.25 50.55 -16 -2 11 73.73 59.55 -16 2 11 21.47 42.42 -16 2 11 78.82 65.15 16 2 -10 21.97 35.64 16 -2 -10 -15.47 30.55 -16 -2 10 17.30 38.95 -16 -2 10 -12.11 35.05 -16 2 10 17.58 31.08 -16 2 10 25.33 52.94 16 2 -9 -22.93 34.54 16 -2 -9 10.81 27.92 -16 -2 9 -11.63 37.81 -16 -2 9 16.17 34.14 -16 2 9 -9.85 52.06 -16 2 9 -22.48 28.70 16 2 -8 13.86 37.42 16 -2 -8 42.69 28.85 -16 -2 8 12.55 36.92 -16 -2 8 12.24 40.97 -16 2 8 -11.29 45.17 -16 2 8 12.73 28.57 16 2 -7 135.67 47.59 -16 -2 7 -1.77 39.48 -16 -2 7 -8.60 35.76 -16 2 7 -3.21 45.18 -16 2 7 1.63 30.63 16 2 -6 14.06 32.74 -16 -2 6 1.64 36.46 -16 -2 6 13.35 33.22 -16 2 6 8.44 58.01 16 2 -5 129.95 64.09 -16 -2 5 241.42 51.70 -16 -2 5 247.08 55.63 -16 2 5 182.48 67.61 16 2 -4 48.40 48.78 -16 -2 4 59.20 38.30 -16 -2 4 34.63 42.74 -16 2 4 5.27 53.66 16 2 -3 184.76 48.40 -16 -2 3 266.76 66.14 -16 -2 3 184.45 72.89 -16 2 3 228.33 92.46 -16 -2 2 39.32 49.80 -16 -2 2 32.74 41.88 -16 2 2 48.19 55.20 16 -2 -1 85.32 45.11 -16 -2 1 18.62 49.80 -16 -2 1 15.03 55.32 -16 2 1 30.47 75.28 16 3 -12 37.41 50.02 16 -3 -12 -3.55 40.01 -16 -3 12 5.01 48.56 -16 -3 12 -2.19 64.95 -16 3 12 76.19 42.04 -16 3 12 17.62 46.81 16 3 -11 -41.70 59.28 16 -3 -11 59.29 34.28 -16 -3 11 -25.26 43.72 -16 -3 11 -34.97 46.17 -16 3 11 53.57 35.89 -16 3 11 -22.58 59.35 16 3 -10 81.31 46.11 16 -3 -10 3.43 32.66 -16 -3 10 -10.95 57.69 -16 -3 10 -20.09 47.08 -16 3 10 35.62 33.56 -16 3 10 14.86 61.90 16 3 -9 108.92 58.40 -16 -3 9 -36.95 41.70 -16 -3 9 11.29 44.04 -16 3 9 24.43 45.62 16 3 -8 130.31 56.48 -16 -3 8 117.91 57.91 -16 -3 8 124.55 69.58 -16 3 8 75.64 60.09 16 3 -7 6.13 50.01 -16 -3 7 181.20 67.75 -16 -3 7 102.32 46.87 -16 3 7 16.16 56.51 16 3 -6 452.00 98.69 -16 -3 6 630.53 102.21 -16 -3 6 569.68 73.18 -16 3 6 690.07 90.06 16 3 -5 260.89 81.36 -16 -3 5 244.14 65.72 -16 -3 5 387.29 78.05 -16 3 5 251.97 76.29 16 3 -4 135.95 52.55 -16 -3 4 61.36 54.42 -16 3 4 227.89 88.18 17 0 -15 11.42 43.89 -17 0 15 54.25 40.98 -17 0 15 10.44 51.59 17 0 -14 22.64 42.76 -17 0 14 90.41 57.61 -17 0 14 28.89 53.08 17 0 -13 -22.18 50.68 -17 0 13 38.03 63.35 -17 0 13 39.31 38.67 17 0 -12 12.19 35.17 -17 0 12 -11.53 61.56 -17 0 12 43.40 47.02 17 0 -11 3.33 25.59 -17 0 11 -4.61 46.45 -17 0 11 -2.26 25.27 17 0 -10 16.54 39.03 -17 0 10 7.01 54.91 -17 0 10 -3.17 38.66 17 0 -9 -8.30 27.46 -17 0 9 -6.02 42.68 -17 0 9 0.98 35.70 17 0 -8 -16.29 25.83 -17 0 8 8.97 24.86 -17 0 8 -10.00 39.74 17 0 -7 -8.13 36.43 -17 0 7 -31.87 34.86 -17 0 7 14.54 58.50 17 0 -6 12.51 33.48 -17 0 6 23.09 42.35 -17 0 6 -2.79 31.44 17 0 -5 -3.28 28.74 -17 0 5 20.63 37.82 -17 0 5 -3.16 26.51 17 0 -4 24.49 27.98 -17 0 4 0.80 51.87 -17 0 4 -13.21 26.52 -17 0 3 4.06 53.06 -17 0 2 1.57 37.87 17 1 -14 -22.69 39.55 17 -1 -14 17.26 43.66 -17 -1 14 0.08 46.34 -17 -1 14 -4.89 40.40 -17 1 14 57.40 43.61 -17 1 14 5.05 45.47 17 1 -13 157.64 78.00 17 -1 -13 92.05 64.75 -17 -1 13 220.59 92.53 -17 -1 13 278.63 78.41 -17 1 13 258.14 87.34 -17 1 13 208.43 66.75 17 1 -12 22.03 40.56 17 -1 -12 84.66 42.78 -17 -1 12 33.54 52.80 -17 -1 12 -22.87 64.38 -17 1 12 -30.28 43.65 -17 1 12 12.53 47.62 17 1 -11 32.71 51.00 17 -1 -11 2.55 40.69 -17 -1 11 4.86 49.49 -17 -1 11 36.23 62.56 -17 1 11 46.30 41.32 -17 1 11 -2.93 47.68 17 1 -10 893.29 101.08 17 -1 -10 795.58 79.70 -17 -1 10 932.25 123.56 -17 -1 10 910.39 75.28 -17 1 10 862.61 80.90 -17 1 10 918.77 97.90 17 1 -9 477.93 63.86 17 -1 -9 503.24 63.94 -17 -1 9 589.52 78.98 -17 -1 9 537.68 79.03 -17 1 9 446.97 64.64 -17 1 9 398.13 82.37 17 1 -8 170.83 70.31 17 -1 -8 424.97 56.22 -17 -1 8 308.04 91.03 -17 -1 8 318.95 68.55 -17 1 8 255.87 53.62 -17 1 8 295.49 96.62 17 1 -7 178.73 49.67 17 -1 -7 -7.06 29.90 -17 -1 7 66.01 50.40 -17 -1 7 71.89 48.24 -17 1 7 36.03 54.62 -17 1 7 59.74 35.59 17 1 -6 202.88 61.65 -17 -1 6 289.92 85.17 -17 -1 6 269.90 60.19 -17 1 6 190.58 71.03 -17 1 6 191.61 41.70 17 1 -5 16.57 39.60 -17 -1 5 181.93 76.32 -17 -1 5 262.64 52.69 -17 1 5 203.20 65.83 17 1 -4 207.86 51.09 -17 -1 4 137.69 38.47 -17 -1 4 40.77 73.95 -17 1 4 49.79 64.50 -17 -1 3 173.81 85.19 -17 -1 3 279.29 56.12 -17 1 3 243.31 73.16 17 2 -12 618.32 104.73 17 -2 -12 529.00 73.34 -17 -2 12 469.62 114.93 -17 -2 12 478.28 103.34 -17 2 12 521.60 77.14 -17 2 12 677.39 87.59 17 2 -11 245.68 68.01 17 -2 -11 203.51 59.31 -17 -2 11 341.00 98.35 -17 -2 11 368.07 85.05 -17 2 11 232.29 60.93 -17 2 11 500.98 74.73 17 2 -10 138.31 57.01 17 -2 -10 100.42 47.78 -17 -2 10 200.19 62.63 -17 -2 10 212.29 72.99 -17 2 10 171.45 66.51 -17 2 10 114.21 48.40 17 2 -9 -58.80 37.09 -17 -2 9 -5.46 41.84 -17 -2 9 1.42 48.32 -17 2 9 25.15 45.10 -17 2 9 4.49 30.54 17 2 -8 57.77 40.03 -17 -2 8 25.84 45.63 -17 -2 8 -11.32 40.29 -17 2 8 19.68 51.66 17 2 -7 -25.78 45.80 -17 -2 7 7.02 51.94 -17 -2 7 24.82 34.17 -17 2 7 7.13 45.27 17 2 -6 253.16 57.93 -17 -2 6 457.03 66.92 -17 -2 6 179.03 75.41 -17 2 6 277.29 78.27 17 2 -5 70.94 58.28 -17 -2 5 113.86 52.76 -17 -2 5 77.15 59.30 -17 2 5 114.79 83.92 18 0 -9 29.33 46.06 -18 0 9 36.87 45.35 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 65069 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp C1 C 0.48450(15) 0.4389(3) 0.46313(12) 0.0596(5) Uani 1 1 d . . N1 N 0.41922(14) 0.2546(3) 0.46105(12) 0.0728(5) Uani 1 1 d . . C2 C 0.40763(16) 0.2618(4) 0.53671(14) 0.0673(6) Uani 1 1 d . . C3 C 0.3485(2) 0.1057(5) 0.5646(3) 0.1003(10) Uani 1 1 d . . H1 H 0.3096 -0.0196 0.5313 0.120 Uiso 1 1 calc R U C4 C 0.3516(3) 0.1501(8) 0.6454(3) 0.1222(15) Uani 1 1 d . . H2 H 0.3136 0.0518 0.6664 0.147 Uiso 1 1 calc R U C5 C 0.4086(3) 0.3333(9) 0.6937(2) 0.1185(13) Uani 1 1 d . . H3 H 0.4087 0.3556 0.7472 0.142 Uiso 1 1 calc R U C6 C 0.4643(2) 0.4818(5) 0.66744(16) 0.0865(8) Uani 1 1 d . . H4 H 0.5019 0.6062 0.7020 0.104 Uiso 1 1 calc R U C7 C 0.46632(16) 0.4510(4) 0.58846(13) 0.0634(5) Uani 1 1 d . . C8 C 0.3675(2) 0.0944(5) 0.39008(19) 0.1029(10) Uani 1 1 d . . H5 H 0.3985 0.1128 0.3496 0.154 Uiso 1 1 calc R U H6 H 0.2941 0.1325 0.3640 0.154 Uiso 1 1 calc R U H7 H 0.3759 -0.0679 0.4098 0.154 Uiso 1 1 calc R U C9 C 0.52856(13) 0.4446(3) 1.03738(10) 0.0445(4) Uani 1 1 d . . N2 N 0.47427(11) 0.2498(2) 1.04832(9) 0.0471(4) Uani 1 1 d . . C10 C 0.38050(13) 0.2394(3) 0.97846(11) 0.0462(4) Uani 1 1 d . . C11 C 0.29997(15) 0.0729(3) 0.95947(13) 0.0559(5) Uani 1 1 d . . H8 H 0.3039 -0.0512 0.9964 0.067 Uiso 1 1 calc R U C12 C 0.21413(15) 0.0976(4) 0.88412(14) 0.0635(5) Uani 1 1 d . . H9 H 0.1598 -0.0132 0.8701 0.076 Uiso 1 1 calc R U C13 C 0.20628(15) 0.2837(4) 0.82833(13) 0.0643(5) Uani 1 1 d . . H10 H 0.1469 0.2953 0.7782 0.077 Uiso 1 1 calc R U C14 C 0.28502(14) 0.4504(3) 0.84638(12) 0.0552(5) Uani 1 1 d . . H11 H 0.2792 0.5746 0.8090 0.066 Uiso 1 1 calc R U C15 C 0.37445(13) 0.4302(3) 0.92222(11) 0.0451(4) Uani 1 1 d . . C16 C 0.50583(16) 0.0974(3) 1.12251(12) 0.0563(5) Uani 1 1 d . . H12 H 0.5810 0.0989 1.1511 0.085 Uiso 1 1 calc R U H13 H 0.4823 -0.0630 1.1056 0.085 Uiso 1 1 calc R U H14 H 0.4751 0.1558 1.1598 0.085 Uiso 1 1 calc R U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0525(10) 0.0552(10) 0.0579(11) -0.0086(8) 0.0080(8) 0.0017(8) N1 0.0632(10) 0.0632(11) 0.0766(12) -0.0130(9) 0.0114(9) -0.0088(8) C2 0.0535(11) 0.0686(13) 0.0741(13) 0.0062(10) 0.0192(10) 0.0113(9) C3 0.0648(15) 0.0748(16) 0.152(3) 0.0226(18) 0.0334(17) 0.0066(12) C4 0.098(2) 0.131(3) 0.168(4) 0.082(3) 0.085(3) 0.048(2) C5 0.121(3) 0.148(3) 0.111(3) 0.060(3) 0.072(2) 0.073(3) C6 0.0890(17) 0.1045(18) 0.0646(14) 0.0120(13) 0.0290(13) 0.0412(16) C7 0.0555(11) 0.0652(12) 0.0632(12) 0.0057(9) 0.0170(9) 0.0154(9) C8 0.0787(16) 0.0822(17) 0.111(2) -0.0400(15) -0.0015(15) -0.0089(13) C9 0.0469(8) 0.0390(8) 0.0516(9) 0.0032(6) 0.0239(7) 0.0035(6) N2 0.0472(8) 0.0424(7) 0.0548(8) 0.0071(6) 0.0237(6) 0.0004(6) C10 0.0460(8) 0.0440(8) 0.0553(9) -0.0036(7) 0.0273(7) 0.0008(6) C11 0.0570(10) 0.0498(10) 0.0696(12) -0.0038(8) 0.0345(10) -0.0071(8) C12 0.0519(10) 0.0662(12) 0.0759(13) -0.0151(10) 0.0293(10) -0.0161(9) C13 0.0488(10) 0.0792(13) 0.0606(11) -0.0084(10) 0.0172(9) -0.0095(9) C14 0.0510(10) 0.0603(11) 0.0546(10) 0.0015(8) 0.0214(8) 0.0006(8) C15 0.0427(8) 0.0444(8) 0.0533(9) -0.0047(7) 0.0245(7) 0.0004(6) C16 0.0657(11) 0.0511(10) 0.0600(11) 0.0135(8) 0.0333(9) 0.0071(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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 C1 C1 N1 111.4(2) 3_666 . C1 C1 C7 108.1(2) 3_666 3_666 N1 C1 C7 140.48(18) . 3_666 C1 N1 C2 106.22(17) . . C1 N1 C8 126.0(2) . . C2 N1 C8 127.7(2) . . N1 C2 C3 127.5(2) . . N1 C2 C7 111.46(19) . . C3 C2 C7 121.0(3) . . C4 C3 C2 116.0(3) . . C4 C3 H1 122.0 . . C2 C3 H1 122.0 . . C5 C4 C3 121.7(3) . . C5 C4 H2 119.1 . . C3 C4 H2 119.1 . . C6 C5 C4 122.4(3) . . C6 C5 H3 118.8 . . C4 C5 H3 118.8 . . C5 C6 C7 120.0(3) . . C5 C6 H4 120.0 . . C7 C6 H4 120.0 . . C6 C7 C2 118.9(2) . . C6 C7 C1 138.3(2) . 3_666 C2 C7 C1 102.81(18) . 3_666 N1 C8 H5 109.5 . . N1 C8 H6 109.5 . . H5 C8 H6 109.5 . . N1 C8 H7 109.5 . . H5 C8 H7 109.5 . . H6 C8 H7 109.5 . . C9 C9 N2 110.17(19) 3_667 . C9 C9 C15 108.60(18) 3_667 3_667 N2 C9 C15 141.23(16) . 3_667 C10 N2 C9 106.86(13) . . C10 N2 C16 126.48(14) . . C9 N2 C16 126.46(15) . . N2 C10 C11 128.67(16) . . N2 C10 C15 110.14(14) . . C11 C10 C15 121.19(17) . . C12 C11 C10 117.87(18) . . C12 C11 H8 121.1 . . C10 C11 H8 121.1 . . C11 C12 C13 121.92(18) . . C11 C12 H9 119.0 . . C13 C12 H9 119.0 . . C14 C13 C12 120.91(19) . . C14 C13 H10 119.5 . . C12 C13 H10 119.5 . . C13 C14 C15 118.97(18) . . C13 C14 H11 120.5 . . C15 C14 H11 120.5 . . C14 C15 C10 119.14(16) . . C14 C15 C9 136.61(16) . 3_667 C10 C15 C9 104.23(15) . 3_667 N2 C16 H12 109.5 . . N2 C16 H13 109.5 . . H12 C16 H13 109.5 . . N2 C16 H14 109.5 . . H12 C16 H14 109.5 . . H13 C16 H14 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 C1 1.356(4) 3_666 C1 N1 1.363(3) . C1 C7 1.457(3) 3_666 N1 C2 1.379(3) . N1 C8 1.456(3) . C2 C3 1.408(3) . C2 C7 1.415(3) . C3 C4 1.401(5) . C3 H1 0.9300 . C4 C5 1.359(6) . C4 H2 0.9300 . C5 C6 1.332(5) . C5 H3 0.9300 . C6 C7 1.386(3) . C6 H4 0.9300 . C7 C1 1.457(3) 3_666 C8 H5 0.9600 . C8 H6 0.9600 . C8 H7 0.9600 . C9 C9 1.366(3) 3_667 C9 N2 1.379(2) . C9 C15 1.429(2) 3_667 N2 C10 1.379(2) . N2 C16 1.454(2) . C10 C11 1.389(2) . C10 C15 1.423(2) . C11 C12 1.378(3) . C11 H8 0.9300 . C12 C13 1.393(3) . C12 H9 0.9300 . C13 C14 1.374(3) . C13 H10 0.9300 . C14 C15 1.405(3) . C14 H11 0.9300 . C15 C9 1.429(2) 3_667 C16 H12 0.9600 . C16 H13 0.9600 . C16 H14 0.9600 . 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 C1 C1 N1 C2 0.6(3) 3_666 . C7 C1 N1 C2 179.8(2) 3_666 . C1 C1 N1 C8 176.9(2) 3_666 . C7 C1 N1 C8 -3.8(4) 3_666 . C1 N1 C2 C3 -179.2(2) . . C8 N1 C2 C3 4.5(4) . . C1 N1 C2 C7 -0.4(2) . . C8 N1 C2 C7 -176.7(2) . . N1 C2 C3 C4 178.8(2) . . C7 C2 C3 C4 0.1(3) . . C2 C3 C4 C5 -0.1(4) . . C3 C4 C5 C6 0.4(5) . . C4 C5 C6 C7 -0.7(4) . . C5 C6 C7 C2 0.7(3) . . C5 C6 C7 C1 -178.4(2) . 3_666 N1 C2 C7 C6 -179.26(18) . . C3 C2 C7 C6 -0.4(3) . . N1 C2 C7 C1 0.1(2) . 3_666 C3 C2 C7 C1 178.98(19) . 3_666 C9 C9 N2 C10 -0.2(2) 3_667 . C15 C9 N2 C10 -179.4(2) 3_667 . C9 C9 N2 C16 -175.35(17) 3_667 . C15 C9 N2 C16 5.4(3) 3_667 . C9 N2 C10 C11 178.83(16) . . C16 N2 C10 C11 -6.0(3) . . C9 N2 C10 C15 -0.21(17) . . C16 N2 C10 C15 174.97(14) . . N2 C10 C11 C12 -178.60(17) . . C15 C10 C11 C12 0.4(2) . . C10 C11 C12 C13 -0.7(3) . . C11 C12 C13 C14 0.4(3) . . C12 C13 C14 C15 0.3(3) . . C13 C14 C15 C10 -0.6(3) . . C13 C14 C15 C9 177.90(18) . 3_667 N2 C10 C15 C14 179.41(15) . . C11 C10 C15 C14 0.3(2) . . N2 C10 C15 C9 0.48(17) . 3_667 C11 C10 C15 C9 -178.65(15) . 3_667