#------------------------------------------------------------------------------ #$Date: 2024-09-17 04:14:26 +0300 (Tue, 17 Sep 2024) $ #$Revision: 294770 $ #$URL: file:///home/coder/svn-repositories/cod/cif/3/00/04/3000473.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_3000473 loop_ _publ_author_name 'Deka, Poonam' 'Jaiswal, Shilpi' 'Sarma, Parishmita' 'Bora, Debajit' 'Nakane, Takanori' 'Kawamoto, Akihiro' 'Kurisu, Genji' 'Mahanta, Sanjeev Pran' 'Patra, Abhijit' 'Ichiyanagi, Kouhei' 'Sasaki, Toshiyuki' 'Thakuria, Ranjit' _publ_section_title ; Analysis of Solid-State Emission of the p-Bis(2,2-dicyanovinyl)benzene Analogue through Combined X-ray, Synchrotron, and Microcrystal Electron Diffraction ; _journal_name_full 'Crystal Growth & Design' _journal_page_first 7222 _journal_page_last 7234 _journal_paper_doi 10.1021/acs.cgd.4c00856 _journal_volume 24 _journal_year 2024 _chemical_formula_sum 'C14 H6 N4' _chemical_formula_weight 230.23 _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' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2016/6 _cell_angle_alpha 90 _cell_angle_beta 99.465(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.1560(3) _cell_length_b 12.5164(5) _cell_length_c 13.2162(6) _cell_measurement_reflns_used 6316 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 26.36 _cell_measurement_theta_min 2.26 _cell_volume 1167.62(9) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_unetI/netI 0.0214 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 10004 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.404 _diffrn_reflns_theta_min 3.313 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_T_max 0.987 _exptl_absorpt_correction_T_min 0.982 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker AXS SADABS program' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.310 _exptl_crystal_description block _exptl_crystal_F_000 472 _exptl_crystal_size_max 0.210 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.150 _refine_diff_density_max 0.284 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.080 _refine_ls_extinction_coef 0.55(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)' _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 164 _refine_ls_number_reflns 2380 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.132 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0586 _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^)+(0.0815P)^2^+0.2211P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1415 _refine_ls_wR_factor_ref 0.1484 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2070 _reflns_number_total 2380 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file IP-1_SCXRD.cif _cod_data_source_block IP-1 _cod_depositor_comments 'Releasing structure 3000473 into public domain as published material.' _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 3000473 _shelx_shelxl_version_number 2016/6 _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 0.983 _shelx_estimated_absorpt_t_max 0.988 _exptl_absorpt_special_details 'Sheldrick,G.M.,2015,University of gottingen' _shelx_res_file ; TITL RT_PS32_IP1_0m_a.res in P2(1)/c rt_ps32_ip1_0m_a.res created by SHELXL-2016/6 at 16:15:28 on 08-May-2019 CELL 0.71073 7.1560 12.5164 13.2162 90.000 99.465 90.000 ZERR 4.000 0.0003 0.0005 0.0006 0.000 0.002 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N UNIT 56 24 16 L.S. 10 ACTA BOND $H FMAP 2 PLAN 3 LIST 6 SIZE 0.15 0.17 0.21 TEMP 23.000 WGHT 0.081500 0.221100 EXTI 0.552978 FVAR 1.73429 N1 3 0.480153 0.212095 0.331509 11.00000 0.12322 0.05495 = 0.03822 -0.00095 0.00997 0.01151 N2 3 0.588203 0.048083 0.627049 11.00000 0.19305 0.05444 = 0.05937 0.01693 -0.01396 0.01104 N3 3 0.062903 0.319433 0.203522 11.00000 0.11051 0.04964 = 0.05493 -0.00128 -0.00193 -0.01131 N4 3 0.025357 0.634956 0.055953 11.00000 0.14127 0.07891 = 0.06687 0.03114 -0.00983 -0.00594 C1 1 0.317549 0.398594 0.540095 11.00000 0.03838 0.04569 = 0.03528 -0.00291 0.00670 -0.00706 C2 1 0.271000 0.431063 0.438024 11.00000 0.04193 0.04008 = 0.03530 -0.00359 0.00388 -0.00171 AFIX 43 H2 2 0.284323 0.383458 0.385653 11.00000 -1.20000 AFIX 0 C3 1 0.204743 0.534160 0.413863 11.00000 0.03770 0.03887 = 0.04635 -0.00328 0.00542 -0.00356 C4 1 0.187296 0.605252 0.493678 11.00000 0.04208 0.04155 = 0.06243 -0.01134 0.01206 -0.00294 AFIX 43 H4 2 0.145201 0.674601 0.478407 11.00000 -1.20000 AFIX 0 C5 1 0.231847 0.573454 0.594451 11.00000 0.05109 0.05869 = 0.05342 -0.02111 0.01728 -0.00616 AFIX 43 H5 2 0.218655 0.621123 0.646792 11.00000 -1.20000 AFIX 0 C6 1 0.295813 0.471393 0.617967 11.00000 0.04600 0.06285 = 0.03767 -0.00972 0.01145 -0.00842 AFIX 43 H6 2 0.324970 0.450429 0.686252 11.00000 -1.20000 AFIX 0 C7 1 0.390678 0.294132 0.574040 11.00000 0.05355 0.05009 = 0.02780 0.00394 0.00251 -0.00951 AFIX 43 H7 2 0.393804 0.281199 0.643592 11.00000 -1.20000 AFIX 0 C8 1 0.454613 0.212854 0.522872 11.00000 0.06517 0.03881 = 0.03116 0.00464 -0.00193 -0.00804 C9 1 0.465974 0.212014 0.415658 11.00000 0.07814 0.03459 = 0.03529 0.00074 0.00068 0.00244 C10 1 0.528128 0.119371 0.579285 11.00000 0.10726 0.04405 = 0.03854 0.00522 -0.00420 -0.00447 C11 1 0.154097 0.574866 0.309860 11.00000 0.05114 0.03499 = 0.05656 0.00411 0.00398 0.00159 AFIX 43 H11 2 0.156963 0.648888 0.304204 11.00000 -1.20000 AFIX 0 C12 1 0.104042 0.522940 0.221007 11.00000 0.05416 0.04168 = 0.04593 0.00926 0.00491 0.00065 C13 1 0.082899 0.409410 0.211141 11.00000 0.06638 0.04789 = 0.03594 0.00360 0.00223 -0.00399 C14 1 0.058761 0.583651 0.127689 11.00000 0.08458 0.05266 = 0.05432 0.01326 -0.00050 -0.00392 HKLF 4 REM RT_PS32_IP1_0m_a.res in P2(1)/c REM R1 = 0.0586 for 2070 Fo > 4sig(Fo) and 0.0645 for all 2380 data REM 164 parameters refined using 0 restraints END WGHT 0.0815 0.2211 REM Highest difference peak 0.284, deepest hole -0.342, 1-sigma level 0.080 Q1 1 0.5403 0.4426 0.6927 11.00000 0.05 0.28 Q2 1 -0.0945 0.6724 0.3977 11.00000 0.05 0.23 Q3 1 0.3432 0.4247 0.7083 11.00000 0.05 0.21 ; _shelx_res_checksum 68973 _shelx_hkl_file ; -2 0 0 2131.19 51.29 3 0 0 1668.63 39.40 -3 0 0 1648.24 39.50 4 0 0 592.44 15.10 -4 0 0 603.94 15.30 5 0 0 249.58 7.40 -5 0 0 251.27 7.60 -6 0 0 2.90 1.70 6 0 0 8.90 1.90 7 0 0 15.40 2.40 -7 0 0 17.70 2.30 -7 0 0 11.80 2.40 -8 0 0 69.49 4.60 -8 0 0 61.79 4.90 8 0 0 73.59 4.60 0 -1 0 0.00 0.10 0 -1 0 0.00 0.10 0 -1 0 0.00 0.10 0 1 0 -0.10 0.10 0 1 0 -0.10 0.10 -1 -1 0 343.07 9.20 -1 1 0 408.26 9.20 -2 -1 0 4298.77 106.39 -2 -1 0 4542.75 106.89 -2 1 0 4880.21 106.49 2 1 0 4205.98 119.49 -2 1 0 4384.16 107.39 -3 -1 0 2308.77 54.59 3 -1 0 2274.57 57.29 3 1 0 2305.57 54.29 -4 -1 0 284.87 8.00 4 -1 0 297.97 7.90 4 1 0 282.67 8.00 5 -1 0 265.47 7.70 -5 -1 0 262.37 7.90 -5 1 0 267.57 8.20 -5 1 0 265.57 8.10 5 1 0 268.57 7.90 6 -1 0 221.68 7.00 -6 -1 0 223.08 7.20 6 1 0 229.78 7.20 -6 1 0 209.78 7.30 -6 1 0 197.28 7.40 7 -1 0 3.10 1.80 -7 -1 0 -1.60 1.50 7 1 0 -1.40 1.80 -7 1 0 1.20 1.70 -7 1 0 2.10 1.90 -8 -1 0 0.30 2.30 -8 -1 0 -1.00 1.90 -8 1 0 0.50 2.10 -8 1 0 0.40 2.00 8 1 0 1.00 2.30 -1 -2 0 2655.63 72.39 -2 -2 0 5763.32 155.28 -2 2 0 4966.70 144.59 -2 2 0 6694.33 139.79 -3 -2 0 221.58 6.20 3 -2 0 230.28 6.00 3 2 0 230.38 6.30 3 2 0 220.28 6.30 -3 2 0 234.38 6.10 -3 2 0 227.18 6.20 -3 2 0 214.48 6.40 -4 -2 0 9.70 1.60 -4 2 0 10.90 1.90 -4 2 0 16.10 1.90 4 2 0 17.30 2.00 -5 -2 0 67.09 3.30 5 -2 0 71.19 3.30 5 2 0 71.79 3.60 -5 2 0 62.69 3.40 -5 2 0 65.29 3.70 -6 -2 0 12.50 2.00 6 -2 0 24.70 2.70 -6 2 0 16.90 2.30 -6 2 0 15.90 2.30 6 2 0 25.30 2.60 -7 -2 0 -0.30 1.70 7 2 0 -0.20 1.90 -7 2 0 0.70 1.80 -7 2 0 0.80 1.70 -8 -2 0 14.30 2.50 8 2 0 21.10 3.10 -8 2 0 14.20 2.60 -8 2 0 17.40 2.80 0 -3 0 -3.70 0.40 0 3 0 -4.00 0.30 -1 -3 0 3056.19 69.69 -1 -3 0 2759.02 69.19 -1 -3 0 3024.50 69.69 -1 3 0 2539.35 73.79 1 3 0 3080.99 69.59 2 -3 0 1337.47 31.90 -2 -3 0 1375.16 31.50 2 -3 0 1308.67 31.40 -2 -3 0 1326.97 31.50 2 -3 0 1353.86 31.50 -2 3 0 1293.87 31.80 -2 3 0 1362.76 31.60 -2 3 0 1334.47 31.30 2 3 0 1351.46 31.70 2 3 0 1243.38 31.50 -3 -3 0 3496.85 86.99 3 3 0 3599.34 87.29 -3 3 0 3468.25 86.39 -3 3 0 3677.73 85.49 -3 3 0 3698.93 85.39 3 3 0 3784.92 85.89 -4 -3 0 5543.25 138.09 4 3 0 6061.69 137.09 -4 3 0 5736.13 137.39 -4 3 0 5798.32 137.09 4 3 0 5794.02 136.89 -5 -3 0 124.09 4.50 5 3 0 116.69 4.60 -5 3 0 129.19 4.60 -6 -3 0 339.67 9.80 6 3 0 345.57 10.10 -6 3 0 333.77 10.00 -7 -3 0 19.40 2.40 7 3 0 28.20 3.10 -7 3 0 22.60 2.60 -7 3 0 26.60 2.90 -8 -3 0 23.60 2.70 -8 -3 0 26.40 2.90 -8 3 0 25.00 3.00 -8 3 0 24.00 3.00 8 3 0 22.20 3.00 0 -4 0 1021.60 23.00 0 -4 0 908.41 22.70 0 -4 0 984.20 22.70 0 4 0 981.20 22.70 0 4 0 880.51 22.90 1 -4 0 3769.12 104.89 -1 -4 0 4329.37 104.59 1 -4 0 4501.55 103.59 -1 -4 0 4806.82 104.19 -1 -4 0 4523.65 103.69 1 4 0 4367.76 104.39 1 4 0 3691.93 103.49 -1 4 0 4842.32 105.19 2 -4 0 60.79 2.00 2 -4 0 60.99 2.60 -2 -4 0 62.59 2.20 -2 -4 0 60.99 2.20 2 -4 0 60.49 2.10 2 4 0 58.69 2.30 -2 4 0 61.69 2.00 -2 4 0 63.89 2.60 2 4 0 57.19 2.40 3 -4 0 354.56 9.70 -3 -4 0 359.76 9.10 -3 -4 0 356.26 9.10 -3 4 0 339.57 9.50 -3 4 0 353.46 9.00 3 4 0 342.97 9.30 3 4 0 347.07 9.20 -3 4 0 347.37 8.90 -4 -4 0 37.40 2.40 -4 -4 0 36.50 2.20 4 4 0 36.50 2.60 -4 4 0 25.10 2.80 -4 4 0 33.40 2.30 4 4 0 38.70 2.90 -5 -4 0 19.10 1.90 -5 -4 0 14.70 1.70 5 4 0 12.20 2.10 -5 4 0 13.30 1.70 5 4 0 16.20 1.90 -6 -4 0 84.09 4.20 -6 -4 0 86.19 4.10 6 4 0 85.19 4.40 -6 4 0 88.99 4.30 -7 -4 0 2.50 2.00 -7 -4 0 1.10 1.70 7 4 0 0.90 2.30 -7 4 0 4.30 1.90 -8 -4 0 23.20 3.20 -8 -4 0 25.60 2.90 -8 4 0 25.60 3.20 -8 4 0 24.30 3.00 8 4 0 22.10 3.30 0 -5 0 2.60 0.80 0 -5 0 -1.30 0.40 0 -5 0 -1.00 0.50 0 5 0 1.90 0.60 0 5 0 -1.70 0.50 1 -5 0 285.57 7.40 -1 -5 0 285.87 7.40 -1 -5 0 289.47 7.60 1 -5 0 291.77 7.80 -1 -5 0 295.67 7.80 1 -5 0 293.17 7.20 -1 5 0 287.37 7.20 1 5 0 293.77 7.60 -1 5 0 283.87 7.70 1 5 0 293.47 7.50 2 -5 0 1684.53 41.00 2 -5 0 1727.33 40.70 -2 -5 0 1716.33 40.50 2 -5 0 1762.82 40.40 -2 -5 0 1708.63 40.60 2 5 0 1697.53 40.60 -2 5 0 1727.53 40.20 2 5 0 1670.73 40.60 -2 5 0 1679.13 40.80 -3 -5 0 96.29 3.30 3 -5 0 90.49 3.90 -3 -5 0 99.19 3.40 3 -5 0 100.19 3.30 -3 5 0 92.89 3.00 -3 5 0 100.19 3.20 3 5 0 95.89 3.60 3 5 0 98.39 3.50 -3 5 0 90.19 3.80 -4 -5 0 142.19 4.70 -4 -5 0 150.78 4.70 4 5 0 139.39 5.10 4 5 0 146.69 5.00 -4 5 0 144.19 4.50 -5 -5 0 96.09 3.80 -5 -5 0 97.49 3.90 -5 5 0 97.39 3.90 5 5 0 94.79 4.30 -6 -5 0 253.77 7.80 -6 -5 0 264.17 8.00 -6 5 0 267.07 8.10 6 5 0 268.77 8.70 -7 -5 0 7.60 2.00 -7 -5 0 7.90 2.10 7 5 0 11.10 2.80 -7 5 0 10.30 2.10 -8 -5 0 36.10 3.50 8 5 0 46.00 5.00 -8 5 0 47.90 4.20 -8 5 0 49.60 4.60 0 -6 0 3783.42 98.39 0 -6 0 4574.74 99.99 0 -6 0 4367.36 97.99 0 6 0 4235.28 99.79 0 6 0 3641.14 97.99 -1 -6 0 133.99 4.20 1 -6 0 133.29 3.70 -1 -6 0 135.49 4.00 1 -6 0 138.99 4.00 1 -6 0 134.59 4.40 -1 6 0 134.89 3.70 1 6 0 132.59 4.10 -1 6 0 139.19 4.30 1 6 0 136.29 4.00 -2 -6 0 660.43 16.70 2 -6 0 688.33 16.50 2 -6 0 690.03 17.40 2 -6 0 682.73 16.70 -2 -6 0 674.63 16.90 -2 6 0 686.23 17.20 2 6 0 694.23 16.90 2 6 0 679.23 16.90 -2 6 0 682.83 16.40 3 -6 0 162.08 5.70 3 -6 0 163.28 4.70 3 -6 0 165.28 5.00 -3 -6 0 168.78 5.10 -3 -6 0 165.18 5.10 3 6 0 168.28 5.20 -3 6 0 161.78 4.60 3 6 0 166.38 5.30 -3 6 0 163.18 4.70 -3 6 0 178.68 6.30 -4 -6 0 42.10 2.40 4 -6 0 38.20 3.10 -4 -6 0 39.20 2.50 -4 6 0 40.40 2.30 4 6 0 42.30 2.60 4 6 0 38.70 2.90 -5 -6 0 2.90 1.50 -5 -6 0 2.40 1.30 5 6 0 2.30 1.90 -5 6 0 1.80 1.30 -6 -6 0 -0.40 1.70 -6 -6 0 1.70 1.40 -6 6 0 0.90 1.50 6 6 0 0.20 1.90 -7 -6 0 0.50 1.60 -7 -6 0 3.50 2.20 7 6 0 0.80 2.30 -7 6 0 1.70 1.80 -8 -6 0 11.80 2.60 8 6 0 11.20 3.30 0 -7 0 0.00 0.80 0 -7 0 -0.60 0.70 0 7 0 -0.90 0.60 0 7 0 -0.20 0.80 -1 -7 0 3.40 1.00 1 -7 0 3.10 1.10 -1 -7 0 3.30 0.80 1 -7 0 4.00 0.90 1 -7 0 2.90 0.70 1 7 0 4.00 0.90 1 7 0 3.80 1.00 -1 7 0 4.00 1.20 -1 7 0 2.40 0.70 2 -7 0 1.70 1.20 2 -7 0 1.00 0.90 2 -7 0 1.20 0.60 -2 -7 0 2.20 1.00 -2 -7 0 2.50 1.00 2 7 0 2.00 1.00 -2 7 0 0.70 1.40 -2 7 0 1.90 0.80 2 7 0 2.90 1.00 -3 -7 0 -0.30 1.00 3 -7 0 4.30 1.40 3 -7 0 0.50 0.90 3 -7 0 0.30 0.70 -3 7 0 0.50 0.80 -3 7 0 0.30 0.70 3 7 0 1.00 1.00 3 7 0 0.60 1.30 4 -7 0 7.80 1.40 4 -7 0 7.00 1.70 -4 -7 0 13.60 1.60 -4 -7 0 9.90 1.60 -4 7 0 8.50 1.20 4 7 0 9.40 1.90 -5 -7 0 55.49 3.40 -5 -7 0 51.19 3.20 -5 7 0 48.00 2.80 5 7 0 44.80 3.70 -6 -7 0 0.50 1.90 -6 -7 0 1.20 1.60 -6 7 0 2.70 1.60 6 7 0 1.20 2.30 -7 -7 0 30.70 3.20 -7 -7 0 28.50 3.10 7 7 0 23.20 3.30 0 -8 0 1819.32 43.20 0 -8 0 1822.12 42.60 0 8 0 1743.63 43.30 0 8 0 1778.32 42.40 1 -8 0 11.50 1.60 -1 -8 0 14.30 1.40 -1 -8 0 14.80 1.50 1 -8 0 13.80 1.40 1 8 0 12.20 1.30 -1 8 0 11.60 1.30 1 8 0 10.40 1.30 -2 -8 0 31.80 2.30 2 -8 0 34.20 1.70 -2 -8 0 33.50 2.20 2 -8 0 33.50 2.10 2 -8 0 33.90 2.70 2 8 0 32.00 2.20 -2 8 0 34.50 1.70 2 8 0 36.30 3.10 3 -8 0 2.70 1.30 -3 -8 0 1.70 1.20 3 -8 0 2.70 1.40 3 -8 0 0.60 1.00 -3 -8 0 3.20 1.20 3 8 0 1.40 1.30 -3 8 0 2.20 0.90 -4 -8 0 0.50 1.30 -4 -8 0 0.00 1.40 4 -8 0 0.10 1.30 4 -8 0 1.30 1.50 -4 8 0 -0.10 1.00 4 8 0 0.60 1.50 -5 -8 0 1.70 1.50 -5 -8 0 0.20 1.60 5 8 0 -0.70 2.00 -5 8 0 1.70 1.30 -6 -8 0 61.49 3.80 -6 -8 0 67.69 4.10 6 8 0 57.19 4.20 -7 -8 0 1.20 1.90 -7 -8 0 4.40 2.30 7 8 0 0.80 2.30 0 -9 0 -1.70 1.00 0 -9 0 0.70 1.10 0 9 0 -0.60 0.90 -1 -9 0 268.07 7.50 -1 -9 0 261.67 7.80 1 -9 0 267.27 7.40 1 -9 0 268.17 8.10 -1 9 0 257.77 7.00 1 9 0 263.77 7.40 2 -9 0 46.90 2.60 -2 -9 0 48.30 2.50 -2 -9 0 46.70 3.00 2 -9 0 48.20 3.30 2 9 0 49.10 2.90 -2 9 0 47.70 2.10 -3 -9 0 614.34 15.80 3 -9 0 603.44 15.50 -3 -9 0 605.54 15.60 3 -9 0 596.84 16.60 -3 9 0 599.84 14.90 3 9 0 609.04 15.90 4 -9 0 5.10 1.90 -4 -9 0 3.00 1.70 -4 -9 0 4.20 1.60 4 -9 0 4.90 1.50 4 9 0 2.70 1.90 -4 9 0 4.10 1.20 -5 -9 0 99.59 4.60 -5 -9 0 96.79 4.50 5 9 0 100.89 5.20 -6 -9 0 6.00 1.80 -6 -9 0 2.30 2.00 6 9 0 2.00 2.40 -7 -9 0 6.70 2.30 7 9 0 7.40 2.90 0 -10 0 1075.29 26.50 0 -10 0 1076.59 27.20 0 10 0 1098.19 26.30 -1 -10 0 124.39 4.40 1 -10 0 128.69 5.30 -1 -10 0 132.69 5.00 1 -10 0 132.19 4.60 -1 10 0 125.69 4.10 1 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13 1.70 1.90 -3 0 13 -4.60 2.00 -3 0 13 2.50 1.70 -2 0 13 -1.60 1.70 -2 0 13 0.40 1.40 -1 0 13 0.20 1.70 -1 0 13 0.60 1.20 0 0 13 -2.60 1.60 1 0 13 4.30 1.70 2 0 13 -0.50 1.50 3 0 13 0.10 1.70 4 0 13 1.30 1.90 -6 -1 13 49.50 5.40 -6 1 13 49.99 5.40 -5 -1 13 615.34 17.60 -5 -1 13 639.14 17.60 -5 1 13 611.94 17.60 -5 1 13 610.04 17.70 -4 -1 13 166.98 7.00 -4 -1 13 166.28 6.50 -4 1 13 154.58 7.10 -4 1 13 167.68 6.60 -3 -1 13 -2.30 1.50 -3 -1 13 0.20 1.90 -3 1 13 -3.90 2.10 -3 1 13 0.40 1.60 -2 -1 13 115.09 4.50 -2 -1 13 113.39 5.10 -2 1 13 106.49 5.00 -2 1 13 110.89 4.60 -1 -1 13 171.18 5.50 -1 -1 13 175.78 6.30 -1 1 13 166.08 5.40 -1 1 13 172.58 6.50 0 -1 13 30.40 3.20 0 1 13 36.00 3.40 1 -1 13 1.90 1.50 1 1 13 0.80 1.60 2 -1 13 84.89 4.10 2 1 13 81.19 4.40 3 -1 13 18.40 2.20 3 1 13 15.30 2.30 4 1 13 76.09 4.60 -6 -2 13 2.00 2.80 -6 2 13 -0.30 2.90 -5 -2 13 21.60 3.10 -5 -2 13 14.00 2.60 -5 2 13 17.40 3.30 -5 2 13 9.20 2.70 -4 -2 13 7.70 2.00 -4 -2 13 8.90 2.40 -4 2 13 1.20 2.60 -4 2 13 3.80 2.00 -3 -2 13 182.78 6.80 -3 -2 13 178.58 6.30 -3 2 13 162.88 7.10 -3 2 13 185.08 6.60 -2 -2 13 15.70 2.30 -2 -2 13 17.60 1.90 -2 2 13 16.90 2.00 -2 2 13 16.30 2.70 1 -2 -13 21.90 2.10 -1 -2 13 20.10 2.30 -1 -2 13 18.90 2.30 -1 2 13 17.20 1.80 -1 2 13 17.70 2.50 0 -2 -13 34.40 2.40 0 -2 13 31.30 3.00 0 2 13 28.70 2.90 1 -2 13 18.80 2.10 1 2 13 19.40 2.40 2 -2 13 -0.20 1.30 2 2 13 1.40 1.80 3 2 13 4.90 2.00 4 2 13 29.30 3.00 -6 -3 13 4.10 2.70 -6 3 13 2.40 2.80 -5 -3 13 1.50 2.20 -5 -3 13 1.00 2.30 -5 3 13 -5.40 2.40 -5 3 13 -4.80 2.10 -4 -3 13 39.50 3.70 -4 -3 13 45.60 4.10 -4 3 13 44.00 3.90 -4 3 13 41.60 3.90 -3 -3 13 74.39 4.10 -3 -3 13 72.69 4.30 -3 3 13 67.99 4.90 -3 3 13 76.09 4.30 -2 -3 13 15.00 2.20 -2 -3 13 12.60 1.80 -2 3 13 8.80 2.60 -2 3 13 11.70 1.90 -1 -3 13 44.50 3.40 1 -3 -13 46.00 3.00 -1 -3 13 50.39 2.90 -1 3 13 47.20 3.60 0 -3 13 5.80 1.50 0 -3 13 5.60 1.60 0 -3 -13 5.30 1.40 0 3 13 6.50 2.10 1 -3 13 62.29 3.40 -1 -3 -13 65.49 3.00 1 3 13 61.89 4.10 2 3 13 12.40 2.20 3 3 13 14.10 2.50 4 3 13 46.20 4.30 -6 -4 13 18.00 3.30 -6 4 13 23.60 3.70 -5 -4 13 0.60 2.30 -5 4 13 -3.70 2.10 -5 4 13 -1.50 2.20 -4 -4 13 3.60 2.20 -4 -4 13 2.70 1.80 -4 4 13 1.40 2.30 -4 4 13 2.70 2.00 -3 -4 13 6.80 1.80 -3 -4 13 4.80 2.00 -3 4 13 1.00 2.30 -3 4 13 3.50 1.90 -2 -4 13 138.49 5.30 -2 -4 13 136.99 5.50 2 -4 -13 131.89 5.30 -2 4 13 149.79 5.50 -2 4 13 132.89 6.20 -1 -4 13 37.90 3.00 -1 -4 13 40.80 2.90 1 -4 -13 42.70 3.00 -1 4 13 33.00 3.40 0 -4 -13 8.50 1.60 0 -4 13 6.90 1.60 0 -4 13 6.40 1.40 0 4 13 6.00 2.10 -1 -4 -13 124.19 4.60 1 4 13 126.89 5.70 2 4 13 6.80 2.20 3 4 13 0.90 2.10 -5 -5 13 11.90 2.70 -5 5 13 10.70 3.40 -5 5 13 14.60 3.10 -4 -5 13 93.19 5.00 -4 -5 13 96.99 5.30 -4 5 13 96.99 5.80 -4 5 13 96.29 5.40 3 -5 -13 42.30 3.50 -3 -5 13 43.30 3.60 -3 -5 13 36.00 3.70 -3 5 13 40.90 3.90 -3 5 13 39.30 3.80 -2 -5 13 -0.40 1.50 2 -5 -13 0.10 1.70 -2 -5 13 0.40 1.50 -2 5 13 -1.40 1.40 -2 5 13 -2.00 2.10 -1 -5 13 165.98 5.80 -1 -5 13 166.28 5.90 1 -5 -13 170.08 6.00 -1 5 13 168.58 6.90 0 -5 13 22.00 2.60 0 -5 -13 24.30 2.30 0 5 13 22.30 2.90 -1 -5 -13 10.10 1.80 1 5 13 6.30 2.00 -2 -5 -13 -0.60 1.40 2 5 13 1.30 1.90 3 5 13 3.30 2.20 -5 -6 13 19.70 3.10 -5 6 13 20.90 3.40 -4 -6 13 8.50 2.30 -4 6 13 12.20 2.60 -4 6 13 11.20 2.80 3 -6 -13 10.80 2.30 -3 -6 13 14.70 2.30 -3 -6 13 7.60 2.00 -3 6 13 11.70 2.80 -3 6 13 13.00 2.40 -2 -6 13 8.50 1.80 -2 -6 13 12.50 2.00 2 -6 -13 8.80 2.10 -2 6 13 11.10 2.70 -1 -6 13 48.70 3.50 1 -6 -13 49.90 3.50 -1 6 13 49.50 4.30 0 -6 -13 55.19 3.50 0 -6 13 50.69 3.30 0 6 13 53.09 4.40 -1 -6 -13 1.60 1.60 1 6 13 2.20 2.10 -2 -6 -13 27.80 2.50 2 6 13 17.70 2.60 3 6 13 10.30 2.70 -4 -7 13 0.80 2.00 4 -7 -13 -0.10 2.10 -4 7 13 0.70 2.30 -4 7 13 0.00 2.20 3 -7 -13 2.20 2.10 -3 -7 13 -1.20 1.60 -3 -7 13 -0.90 1.80 -3 7 13 1.50 2.00 -3 7 13 -0.50 2.10 -2 -7 13 10.00 2.00 2 -7 -13 7.60 2.20 -2 7 13 9.40 2.60 -1 -7 13 22.30 2.40 1 -7 -13 24.40 2.60 -1 7 13 24.20 3.00 0 -7 -13 16.90 2.40 0 -7 13 16.10 2.20 0 7 13 19.50 2.90 -1 -7 -13 28.10 2.70 1 7 13 28.10 3.20 -2 -7 -13 10.20 2.10 2 7 13 14.20 2.90 4 -8 -13 4.50 2.30 -4 -8 13 2.00 2.10 -4 8 13 4.80 2.70 -4 8 13 5.30 2.70 3 -8 -13 0.30 2.10 -3 8 13 0.30 2.40 -3 8 13 0.70 2.90 2 -8 -13 68.89 4.40 -2 -8 13 59.89 4.10 -2 8 13 67.79 5.00 1 -8 -13 0.20 2.00 -1 -8 13 -0.50 1.70 -1 8 13 0.80 2.30 0 -8 13 8.00 2.00 0 8 13 7.50 2.60 -1 -8 -13 14.00 2.40 1 8 13 13.40 2.90 3 -9 -13 8.40 2.60 -3 9 13 5.90 2.80 2 -9 -13 1.60 2.20 -1 -9 13 13.80 2.50 1 -9 -13 15.40 2.60 -1 9 13 17.60 3.10 0 -9 13 21.20 2.60 0 -9 -13 25.20 2.90 0 9 13 23.60 3.10 -5 0 14 20.80 3.50 -5 0 14 20.10 3.50 -4 0 14 128.49 6.40 -4 0 14 132.99 6.00 -3 0 14 26.50 3.00 -3 0 14 36.20 3.30 -2 0 14 26.40 2.90 -2 0 14 29.80 2.70 -1 0 14 31.90 3.40 0 0 14 178.88 6.70 1 0 14 77.39 4.30 2 0 14 122.39 5.20 3 0 14 -0.10 1.80 -5 -1 14 19.20 3.30 -5 1 14 15.30 3.30 -5 1 14 18.00 3.10 -4 -1 14 2.30 2.50 -4 -1 14 3.30 1.90 -4 1 14 -1.10 2.40 -4 1 14 1.40 2.00 -3 -1 14 5.20 2.10 -3 -1 14 4.80 1.70 -3 1 14 3.00 1.90 -3 1 14 0.70 2.10 -2 -1 14 4.20 2.00 -2 -1 14 3.30 1.40 -2 1 14 4.60 1.50 -2 1 14 5.70 2.30 -1 -1 14 0.10 1.70 -1 1 14 -0.70 1.90 0 -1 14 8.70 2.00 0 1 14 7.70 2.10 1 -1 14 9.10 1.90 1 1 14 9.50 2.10 2 -1 14 -1.20 1.50 2 1 14 0.30 1.70 3 1 14 21.00 2.70 -5 -2 14 12.00 2.90 -5 2 14 2.70 2.90 -5 2 14 9.30 3.10 -4 -2 14 1.30 2.20 -4 -2 14 1.30 1.80 -4 2 14 0.70 2.00 -4 2 14 -3.60 2.40 -3 -2 14 26.70 3.10 -3 -2 14 23.50 2.80 -3 2 14 26.10 3.20 -3 2 14 24.00 2.50 -2 -2 14 56.29 3.40 -2 -2 14 52.59 4.00 -2 2 14 54.39 4.40 -2 2 14 52.49 3.90 -1 -2 14 6.60 1.90 -1 2 14 10.30 2.40 0 -2 -14 -1.70 1.80 0 -2 14 1.30 1.70 0 2 14 -0.70 1.70 1 -2 14 8.80 1.80 1 2 14 9.00 2.10 2 2 14 1.60 1.90 3 2 14 92.49 5.20 -5 -3 14 23.20 3.20 -5 3 14 22.30 3.50 -4 -3 14 46.80 3.70 -4 -3 14 49.10 4.30 -4 3 14 45.70 4.10 -4 3 14 38.00 4.20 -3 -3 14 2.60 1.70 -3 -3 14 0.90 1.80 -3 3 14 -0.40 1.70 -3 3 14 -3.30 2.30 -2 -3 14 -1.10 1.70 -2 -3 14 2.50 1.50 -2 3 14 1.40 2.20 1 -3 -14 15.60 2.00 -1 -3 14 17.40 2.10 -1 -3 14 18.30 2.30 -1 3 14 15.30 2.60 0 -3 14 4.30 1.70 0 -3 -14 4.50 1.40 0 3 14 6.50 2.20 1 -3 14 0.80 2.30 1 3 14 1.40 2.00 2 3 14 181.88 7.10 3 3 14 17.40 2.80 -5 -4 14 0.10 2.40 -5 4 14 0.10 2.70 -4 -4 14 21.60 3.00 -4 -4 14 21.20 2.60 -4 4 14 20.80 2.80 -4 4 14 16.00 2.90 -3 -4 14 200.78 7.50 -3 -4 14 198.98 7.20 -3 4 14 202.48 8.10 -3 4 14 209.98 7.40 -2 -4 14 11.10 2.10 -2 -4 14 9.30 1.90 2 -4 -14 14.40 2.30 -2 4 14 13.50 2.80 -1 -4 14 0.30 1.60 1 -4 -14 2.00 1.60 -1 -4 14 0.50 1.40 -1 4 14 -0.20 2.10 0 -4 14 14.40 2.90 0 -4 -14 15.80 1.90 0 4 14 14.80 2.70 1 4 14 6.40 2.30 2 4 14 26.10 3.10 -5 -5 14 2.80 2.50 -5 5 14 0.70 2.70 -4 -5 14 1.10 2.20 -4 5 14 0.30 2.40 -4 5 14 2.30 2.10 -3 -5 14 24.10 2.70 -3 -5 14 19.20 2.50 -3 5 14 21.30 3.40 -3 5 14 24.40 3.30 -2 -5 14 10.50 2.00 2 -5 -14 6.90 2.10 -2 -5 14 6.40 1.90 -2 5 14 5.00 2.50 -1 -5 14 0.00 2.80 1 -5 -14 0.50 1.70 -1 -5 14 -0.40 1.40 -1 5 14 -0.70 2.20 0 -5 -14 50.09 3.40 0 5 14 48.90 4.30 -1 -5 -14 49.40 3.30 1 5 14 49.80 4.30 2 5 14 17.30 2.80 -4 -6 14 1.90 2.20 -4 6 14 2.00 2.70 -4 6 14 2.30 2.20 -3 -6 14 57.29 4.10 -3 -6 14 63.19 4.30 3 -6 -14 64.69 4.50 -3 6 14 58.29 5.00 -2 -6 14 0.40 1.70 2 -6 -14 -0.90 1.80 -2 6 14 1.10 2.40 1 -6 -14 30.10 2.90 -1 -6 14 29.10 3.10 -1 6 14 31.10 3.50 0 -6 -14 1.10 1.70 0 6 14 -1.50 2.20 -1 -6 -14 53.09 3.60 1 6 14 56.69 4.70 2 6 14 -1.20 2.30 3 -7 -14 1.00 2.10 -3 7 14 -0.10 2.50 2 -7 -14 1.80 2.00 -2 -7 14 0.90 1.70 -2 7 14 -0.40 2.40 -1 -7 14 13.20 2.20 1 -7 -14 16.70 2.50 -1 7 14 18.00 3.10 0 -7 -14 43.10 3.50 0 7 14 41.40 4.50 -1 -7 -14 6.20 2.10 1 7 14 8.90 2.80 2 -8 -14 13.30 2.70 -2 8 14 11.90 3.00 -1 -8 14 30.80 3.60 1 -8 -14 29.60 3.00 -1 8 14 19.70 3.00 0 -8 -14 6.60 2.20 0 8 14 9.50 2.90 -5 0 15 -1.10 2.50 -4 0 15 0.00 2.30 -4 0 15 -0.70 1.80 -3 0 15 1.50 2.20 -3 0 15 0.00 1.50 -2 0 15 0.20 2.10 -1 0 15 0.00 2.00 0 0 15 -0.80 1.80 1 0 15 0.00 1.70 2 0 15 -2.90 1.70 -5 -1 15 3.80 2.70 -5 1 15 3.60 2.70 -4 -1 15 42.20 3.80 -4 -1 15 41.90 4.40 -4 1 15 46.40 4.70 -4 1 15 46.50 4.20 -3 -1 15 9.90 1.90 -3 -1 15 13.00 2.60 -3 1 15 13.30 2.70 -3 1 15 10.20 2.20 -2 -1 15 25.90 3.00 -2 1 15 23.80 3.10 -1 -1 15 113.99 5.40 -1 1 15 120.59 6.00 0 -1 15 7.30 2.20 0 1 15 8.60 2.30 1 -1 15 33.40 3.50 1 1 15 34.10 3.60 2 -1 15 -1.40 3.20 2 1 15 4.50 2.10 -4 -2 15 2.40 1.90 -4 -2 15 6.00 2.40 -4 2 15 1.30 2.30 -4 2 15 2.40 2.10 -3 -2 15 0.70 2.10 -3 -2 15 3.60 1.70 -3 2 15 -0.40 2.40 -2 -2 15 1.50 2.00 -2 2 15 0.60 2.20 -1 -2 15 17.90 2.50 -1 2 15 14.70 2.70 0 -2 15 123.19 5.30 0 2 15 117.39 5.80 1 -2 15 0.70 1.90 1 2 15 -0.30 2.00 2 2 15 134.39 6.30 -4 -3 15 -0.50 2.10 -4 -3 15 0.90 2.20 -4 3 15 -1.40 2.00 -4 3 15 -1.20 2.60 -3 -3 15 13.90 2.20 -3 -3 15 15.30 2.60 -3 3 15 13.60 3.00 -2 -3 15 -2.60 1.80 -2 3 15 -0.80 2.10 -1 -3 15 4.70 1.90 -1 3 15 6.60 2.40 0 -3 15 4.80 1.90 0 3 15 3.40 2.40 1 3 15 301.27 10.20 -4 -4 15 -0.50 2.20 -4 4 15 0.40 2.30 -4 4 15 3.00 2.50 -3 -4 15 28.90 3.50 -3 -4 15 21.40 2.80 -3 4 15 24.60 3.40 -2 -4 15 11.20 2.30 -2 -4 15 13.90 2.30 -2 4 15 13.50 2.90 -1 -4 15 3.00 1.90 1 -4 -15 3.20 1.80 -1 4 15 3.00 2.30 0 4 15 39.50 4.30 1 4 15 3.70 2.40 -3 -5 15 20.40 2.60 -3 -5 15 19.70 2.70 -3 5 15 18.70 3.30 -2 -5 15 13.10 2.20 -2 -5 15 11.20 2.60 2 -5 -15 13.00 2.40 -2 5 15 12.30 2.80 1 -5 -15 216.38 7.50 -1 5 15 215.98 8.50 0 -5 -15 142.49 5.70 0 5 15 152.18 6.90 1 5 15 41.10 4.30 2 -6 -15 142.59 6.30 -2 -6 15 175.18 6.50 -2 6 15 151.08 7.30 1 -6 -15 156.78 6.20 -1 6 15 154.28 7.20 0 -6 -15 106.89 5.10 0 6 15 117.09 6.30 -3 0 16 351.16 11.50 -2 0 16 50.09 4.50 -1 0 16 6.10 2.50 0 0 16 2.90 2.30 -3 -1 16 5.60 2.50 -3 1 16 4.30 2.60 -2 -1 16 90.99 5.50 -2 1 16 92.99 5.60 -1 -1 16 14.60 2.80 -1 1 16 15.40 2.90 0 -1 16 191.28 7.40 0 1 16 187.28 7.50 -3 -2 16 2.50 2.40 -3 2 16 -0.40 2.50 -2 -2 16 57.99 4.70 -2 2 16 50.99 4.80 -1 -2 16 339.77 10.80 -1 2 16 345.27 11.30 0 -2 16 29.20 3.10 0 2 16 42.20 4.40 -2 -3 16 34.00 3.80 -2 3 16 28.00 3.70 -1 -3 16 27.00 3.00 -1 3 16 24.80 3.30 0 3 16 1.60 2.50 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 60945 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 _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.4802(3) 0.21209(13) 0.33151(11) 0.0725(5) Uani 1 1 d . . . . . N2 N 0.5882(4) 0.04808(15) 0.62705(15) 0.1062(9) Uani 1 1 d . . . . . N3 N 0.0629(3) 0.31943(13) 0.20352(12) 0.0734(5) Uani 1 1 d . . . . . N4 N 0.0254(4) 0.63496(17) 0.05595(15) 0.0987(7) Uani 1 1 d . . . . . C1 C 0.31755(19) 0.39859(11) 0.54009(10) 0.0397(4) Uani 1 1 d . . . . . C2 C 0.27100(19) 0.43106(11) 0.43802(10) 0.0394(4) Uani 1 1 d . . . . . H2 H 0.284323 0.383458 0.385653 0.047 Uiso 1 1 calc R U . . . C3 C 0.20474(19) 0.53416(11) 0.41386(11) 0.0411(4) Uani 1 1 d . . . . . C4 C 0.1873(2) 0.60525(13) 0.49368(13) 0.0483(4) Uani 1 1 d . . . . . H4 H 0.145201 0.674601 0.478407 0.058 Uiso 1 1 calc R U . . . C5 C 0.2318(2) 0.57345(14) 0.59445(13) 0.0534(4) Uani 1 1 d . . . . . H5 H 0.218655 0.621123 0.646792 0.064 Uiso 1 1 calc R U . . . C6 C 0.2958(2) 0.47139(13) 0.61797(12) 0.0483(4) Uani 1 1 d . . . . . H6 H 0.324970 0.450429 0.686252 0.058 Uiso 1 1 calc R U . . . C7 C 0.3907(2) 0.29413(12) 0.57404(10) 0.0443(4) Uani 1 1 d . . . . . H7 H 0.393804 0.281199 0.643592 0.053 Uiso 1 1 calc R U . . . C8 C 0.4546(2) 0.21285(11) 0.52287(11) 0.0462(4) Uani 1 1 d . . . . . C9 C 0.4660(3) 0.21201(11) 0.41566(11) 0.0503(4) Uani 1 1 d . . . . . C10 C 0.5281(3) 0.11937(14) 0.57928(13) 0.0651(6) Uani 1 1 d . . . . . C11 C 0.1541(2) 0.57487(11) 0.30986(12) 0.0481(4) Uani 1 1 d . . . . . H11 H 0.156963 0.648888 0.304204 0.058 Uiso 1 1 calc R U . . . C12 C 0.1040(2) 0.52294(12) 0.22101(12) 0.0476(4) Uani 1 1 d . . . . . C13 C 0.0829(2) 0.40941(13) 0.21114(11) 0.0508(4) Uani 1 1 d . . . . . C14 C 0.0588(3) 0.58365(15) 0.12769(14) 0.0652(5) Uani 1 1 d . . . . . 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 N1 0.1232(15) 0.0550(9) 0.0382(8) -0.0009(6) 0.0100(8) 0.0115(9) N2 0.193(3) 0.0544(10) 0.0594(11) 0.0169(8) -0.0140(13) 0.0110(12) N3 0.1105(14) 0.0496(9) 0.0549(9) -0.0013(7) -0.0019(9) -0.0113(8) N4 0.141(2) 0.0789(13) 0.0669(11) 0.0311(10) -0.0098(12) -0.0059(12) C1 0.0384(7) 0.0457(8) 0.0353(7) -0.0029(5) 0.0067(5) -0.0071(6) C2 0.0419(7) 0.0401(7) 0.0353(7) -0.0036(5) 0.0039(5) -0.0017(5) C3 0.0377(7) 0.0389(7) 0.0464(8) -0.0033(6) 0.0054(6) -0.0036(5) C4 0.0421(7) 0.0416(8) 0.0624(10) -0.0113(7) 0.0121(7) -0.0029(6) C5 0.0511(9) 0.0587(10) 0.0534(9) -0.0211(7) 0.0173(7) -0.0062(7) C6 0.0460(8) 0.0629(10) 0.0377(8) -0.0097(6) 0.0114(6) -0.0084(7) C7 0.0536(8) 0.0501(8) 0.0278(7) 0.0039(5) 0.0025(6) -0.0095(6) C8 0.0652(10) 0.0388(8) 0.0312(7) 0.0046(5) -0.0019(6) -0.0080(6) C9 0.0781(11) 0.0346(7) 0.0353(8) 0.0007(5) 0.0007(7) 0.0024(7) C10 0.1073(15) 0.0441(9) 0.0385(8) 0.0052(7) -0.0042(9) -0.0045(9) C11 0.0511(9) 0.0350(7) 0.0566(10) 0.0041(6) 0.0040(7) 0.0016(6) C12 0.0542(9) 0.0417(8) 0.0459(9) 0.0093(6) 0.0049(7) 0.0006(6) C13 0.0664(10) 0.0479(9) 0.0359(8) 0.0036(6) 0.0022(7) -0.0040(7) C14 0.0846(13) 0.0527(10) 0.0543(10) 0.0133(8) -0.0005(9) -0.0039(9) 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 C2 C1 C6 118.85(14) . . C2 C1 C7 125.28(13) . . C6 C1 C7 115.87(13) . . C3 C2 C1 120.61(13) . . C3 C2 H2 119.7 . . C1 C2 H2 119.7 . . C2 C3 C4 118.99(14) . . C2 C3 C11 124.28(13) . . C4 C3 C11 116.72(14) . . C5 C4 C3 120.65(15) . . C5 C4 H4 119.7 . . C3 C4 H4 119.7 . . C6 C5 C4 120.19(14) . . C6 C5 H5 119.9 . . C4 C5 H5 119.9 . . C5 C6 C1 120.71(15) . . C5 C6 H6 119.6 . . C1 C6 H6 119.6 . . C8 C7 C1 131.46(13) . . C8 C7 H7 114.3 . . C1 C7 H7 114.3 . . C7 C8 C9 125.67(14) . . C7 C8 C10 118.73(14) . . C9 C8 C10 115.53(14) . . N1 C9 C8 178.1(2) . . N2 C10 C8 177.3(2) . . C12 C11 C3 130.39(14) . . C12 C11 H11 114.8 . . C3 C11 H11 114.8 . . C11 C12 C13 124.79(14) . . C11 C12 C14 119.04(15) . . C13 C12 C14 116.11(15) . . N3 C13 C12 178.8(2) . . N4 C14 C12 177.4(2) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 N1 C9 1.133(2) . N2 C10 1.136(2) . N3 C13 1.138(2) . N4 C14 1.137(2) . C1 C2 1.3957(19) . C1 C6 1.402(2) . C1 C7 1.452(2) . C2 C3 1.3936(19) . C2 H2 0.9300 . C3 C4 1.401(2) . C3 C11 1.455(2) . C4 C5 1.376(2) . C4 H4 0.9300 . C5 C6 1.375(2) . C5 H5 0.9300 . C6 H6 0.9300 . C7 C8 1.343(2) . C7 H7 0.9300 . C8 C9 1.433(2) . C8 C10 1.440(2) . C11 C12 1.338(2) . C11 H11 0.9300 . C12 C13 1.433(2) . C12 C14 1.439(2) .