#------------------------------------------------------------------------------ #$Date: 2020-07-06 05:06:13 +0300 (Mon, 06 Jul 2020) $ #$Revision: 253827 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/65/7126512.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_7126512 loop_ _publ_author_name 'Fujii, Toshiki' 'Tanaka, Susumu' 'Hayashi, Shotaro' 'Imoto, Hiroaki' 'Naka, Kensuke' _publ_section_title ; Dipyridinoarsole: a new class of stable and modifiable heteroatom-bridged bipyridines. ; _journal_issue 45 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 6035 _journal_page_last 6038 _journal_paper_doi 10.1039/d0cc02389b _journal_volume 56 _journal_year 2020 _chemical_formula_moiety 'C16 H11 N2 P' _chemical_formula_sum 'C16 H11 N2 P' _chemical_formula_weight 262.25 _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 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_update_record ; 2020-04-02 deposited with the CCDC. 2020-05-11 downloaded from the CCDC. ; _cell_angle_alpha 90.0000 _cell_angle_beta 103.655(14) _cell_angle_gamma 90.0000 _cell_formula_units_Z 4 _cell_length_a 13.597(4) _cell_length_b 11.204(3) _cell_length_c 8.645(2) _cell_measurement_reflns_used 1844 _cell_measurement_temperature 273 _cell_measurement_theta_max 27.49 _cell_measurement_theta_min 3.03 _cell_volume 1279.8(6) _computing_cell_refinement DTREK _computing_data_collection DTREK _computing_data_reduction DTREK _computing_molecular_graphics 'CrystalStructure 4.1' _computing_publication_material 'CrystalStructure 4.1 (Rigaku, 2014)' _computing_structure_refinement 'SHELXL2013 (Sheldrick, 2008)' _computing_structure_solution 'SIR2011 (Burla, et al., 2012)' _diffrn_ambient_temperature 273 _diffrn_detector_area_resol_mean 13.653 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Rigaku XtaLAB mini' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0642 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 13536 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.676 _diffrn_reflns_theta_min 3.031 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.200 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_correction_T_min 0.928 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_description chip _exptl_crystal_F_000 544.00 _exptl_crystal_size_max 0.550 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.060 _refine_diff_density_max 0.32 _refine_diff_density_min -0.30 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 172 _refine_ls_number_reflns 2995 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1272 _refine_ls_R_factor_gt 0.0666 _refine_ls_shift/su_max 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0799P)^2^+0.5683P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1523 _refine_ls_wR_factor_ref 0.1913 _reflns_number_gt 1660 _reflns_number_total 2995 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file d0cc02389b2.cif _cod_data_source_block DPP_5 _cod_depositor_comments 'Adding full bibliography for 7126511--7126515.cif.' _cod_database_code 7126512 _shelxl_res_file ; shelxl.res created by SHELXL-2014/7 TITL DIpyridinophosphole_01 CELL 0.71075 13.59740 11.20450 8.64470 90.00000 103.65500 90.00000 ZERR 4 0.00409 0.00304 0.00247 0.00000 0.01370 0.00000 LATT 1 SYMM -X, .50+Y, .50-Z SFAC C H N P UNIT 64 44 8 4 L.S. 5 FMAP 2 PLAN -25 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP 0.0 ACTA SIZE 0.060 0.550 0.080 WGHT 0.079900 0.568300 FVAR 1.18905 P1 4 0.677827 0.996399 0.494002 11.00000 0.05701 0.05185 = 0.05531 -0.00018 0.01377 0.00972 N7 3 0.928160 0.951784 0.311805 11.00000 0.06855 0.08264 = 0.06647 -0.00365 0.02773 -0.00359 N19 3 0.554599 0.687092 0.622801 11.00000 0.06052 0.07958 = 0.07665 0.00187 0.01963 -0.01193 C1 1 0.792147 0.817206 0.432105 11.00000 0.04566 0.05257 = 0.04339 -0.00193 0.00860 0.00330 C2 1 0.785945 0.941785 0.429156 11.00000 0.05798 0.05050 = 0.04715 0.00022 0.01462 0.00050 C3 1 0.650173 0.844718 0.543232 11.00000 0.04179 0.05589 = 0.04834 -0.00002 0.00589 0.00080 C4 1 0.666253 1.121879 0.761342 11.00000 0.05689 0.04813 = 0.06452 -0.00179 0.01584 0.00499 AFIX 43 H4 2 0.597982 1.126825 0.710625 11.00000 -1.20000 AFIX 0 C5 1 0.834090 1.058930 0.763460 11.00000 0.05810 0.04637 = 0.06136 0.00409 0.02051 -0.00033 AFIX 43 H5 2 0.879604 1.020403 0.715241 11.00000 -1.20000 AFIX 0 C8 1 0.700696 1.173458 0.909108 11.00000 0.07679 0.04702 = 0.07377 -0.01093 0.02902 0.00333 AFIX 43 H8 2 0.655778 1.211562 0.958918 11.00000 -1.20000 AFIX 0 C9 1 0.856332 1.002737 0.367258 11.00000 0.07270 0.06079 = 0.05998 -0.00087 0.02470 -0.00379 AFIX 43 H9 2 0.852654 1.085620 0.364627 11.00000 -1.20000 AFIX 0 C10 1 0.867442 0.762851 0.375957 11.00000 0.06000 0.05760 = 0.05915 -0.00873 0.01592 0.00766 AFIX 43 H10 2 0.874076 0.680221 0.377682 11.00000 -1.20000 AFIX 0 C11 1 0.571830 0.802982 0.606340 11.00000 0.04870 0.07483 = 0.06230 -0.00226 0.01070 0.00205 AFIX 43 H11 2 0.529583 0.858164 0.638493 11.00000 -1.20000 AFIX 0 C12 1 0.695385 0.642316 0.512591 11.00000 0.05968 0.05101 = 0.05958 -0.00381 0.01111 -0.00297 AFIX 43 H12 2 0.736205 0.584708 0.481860 11.00000 -1.20000 AFIX 0 C13 1 0.867699 1.111939 0.909571 11.00000 0.05526 0.05755 = 0.06582 -0.00450 0.01076 -0.00980 AFIX 43 H13 2 0.936193 1.109465 0.959566 11.00000 -1.20000 AFIX 0 C14 1 0.932371 0.833454 0.317468 11.00000 0.05798 0.08309 = 0.07166 -0.00623 0.02429 0.00365 AFIX 43 H14 2 0.982864 0.796024 0.279088 11.00000 -1.20000 AFIX 0 C15 1 0.802037 1.168022 0.982075 11.00000 0.08513 0.05207 = 0.06266 -0.00911 0.02102 -0.00600 AFIX 43 H15 2 0.825805 1.202877 1.081525 11.00000 -1.20000 AFIX 0 C16 1 0.615814 0.611008 0.574800 11.00000 0.07149 0.06116 = 0.06979 0.00160 0.01323 -0.01051 AFIX 43 H16 2 0.603551 0.529996 0.584278 11.00000 -1.20000 AFIX 0 C17 1 0.732066 1.062949 0.687857 11.00000 0.05606 0.03753 = 0.05770 0.00436 0.02091 0.00793 C18 1 0.713267 0.762032 0.496803 11.00000 0.04490 0.05093 = 0.04250 -0.00226 0.00404 0.00431 HKLF 4 REM DIpyridinophosphole_01 REM R1 = 0.0666 for 1660 Fo > 4sig(Fo) and 0.1272 for all 2995 data REM 172 parameters refined using 0 restraints END WGHT 0.0799 0.5683 REM Instructions for potential hydrogen bonds EQIV $1 -x+2, -y+2, -z+1 HTAB C5 N7_$1 REM Highest difference peak 0.319, deepest hole -0.304, 1-sigma level 0.053 Q1 1 0.5990 1.0499 0.3973 11.00000 0.05 0.32 Q2 1 0.7224 0.9340 0.6790 11.00000 0.05 0.24 Q3 1 1.0365 1.0088 0.4853 11.00000 0.05 0.23 Q4 1 0.8404 0.9325 0.7497 11.00000 0.05 0.20 Q5 1 0.8673 0.6149 0.3971 11.00000 0.05 0.19 Q6 1 0.8071 0.9568 0.4003 11.00000 0.05 0.18 Q7 1 0.8741 1.2614 0.9083 11.00000 0.05 0.18 Q8 1 0.6294 0.8243 0.5531 11.00000 0.05 0.18 Q9 1 0.5644 1.1065 0.6700 11.00000 0.05 0.18 Q10 1 0.7210 1.0379 0.6403 11.00000 0.05 0.18 Q11 1 0.7844 0.6037 0.5977 11.00000 0.05 0.17 Q12 1 0.7482 0.7796 0.4783 11.00000 0.05 0.16 Q13 1 0.6853 1.0095 0.3208 11.00000 0.05 0.16 Q14 1 0.6980 1.1340 1.0262 11.00000 0.05 0.16 Q15 1 0.6560 0.8957 0.5059 11.00000 0.05 0.16 Q16 1 0.4980 0.8446 0.6793 11.00000 0.05 0.16 Q17 1 0.5569 0.9253 0.8287 11.00000 0.05 0.16 Q18 1 0.6447 1.1791 0.5428 11.00000 0.05 0.15 Q19 1 1.0793 0.7247 0.3510 11.00000 0.05 0.15 Q20 1 0.7402 1.0924 0.6789 11.00000 0.05 0.15 Q21 1 0.7054 1.2481 1.0085 11.00000 0.05 0.15 Q22 1 0.7830 0.9797 0.4905 11.00000 0.05 0.15 Q23 1 0.6931 1.1077 0.5569 11.00000 0.05 0.15 Q24 1 0.6161 0.9397 0.3638 11.00000 0.05 0.15 Q25 1 0.6452 0.5039 0.6638 11.00000 0.05 0.15 ; _shelxl_hkl_file ; 0 0 212340.45 134.24 0 0 212423.24 133.76 0 0 212384.97 135.44 0 0 3 -1.11 6.02 0 0 3 3.60 5.78 0 0 3 -7.89 5.23 0 0 4 686.83 21.66 0 0 4 696.10 21.83 0 0 4 669.03 21.83 0 0 5 -5.75 6.72 0 0 5 -9.33 6.22 0 0 5 5.92 7.06 0 0 6 131.82 15.87 0 0 6 129.75 14.71 0 0 6 116.28 33.08 0 0 7 7.44 9.37 0 0 7 10.95 12.77 0 0 7 13.86 10.85 0 0 8 178.12 23.95 0 0 8 207.45 24.77 0 0 -8 224.75 24.24 0 0 9 -5.55 10.47 0 0 -9 12.85 9.80 0 0 9 12.08 11.08 0 0 -10 61.49 17.50 0 0 -10 154.91 39.72 0 0 10 61.27 21.31 0 1 1 4681.67 53.01 0 1 -1 4820.15 51.87 0 -1 1 4889.09 57.24 0 1 2 1033.47 19.74 0 1 2 1044.50 20.24 0 1 -2 1008.09 20.17 0 1 2 1048.38 23.70 0 -1 2 1035.42 23.16 0 -1 2 1049.02 18.58 0 1 -3 125.95 11.19 0 1 3 106.33 9.89 0 1 3 103.62 9.71 0 1 3 111.45 12.61 0 -1 3 131.76 10.86 0 -1 3 98.25 12.49 0 1 -4 1592.55 31.71 0 1 4 1510.67 33.06 0 1 4 1523.86 29.51 0 1 4 1598.39 32.41 0 -1 4 1583.78 34.68 0 -1 4 1550.64 30.33 0 1 5 1518.88 46.68 0 1 5 1507.24 42.37 0 1 5 1492.09 44.31 0 1 -5 1497.23 42.75 0 -1 5 1466.21 42.54 0 -1 5 1439.88 44.64 0 1 6 -0.47 8.75 0 1 6 7.62 7.42 0 1 6 20.17 11.14 0 1 -6 33.94 13.52 0 -1 6 -5.46 8.47 0 -1 6 22.31 10.85 0 1 7 195.13 20.38 0 1 7 189.47 22.27 0 1 -7 205.25 19.66 0 1 7 179.58 16.97 0 -1 7 226.81 21.37 0 -1 7 177.24 20.64 0 1 -8 20.76 12.63 0 1 8 5.72 11.08 0 1 8 -6.74 9.42 0 -1 8 5.65 9.46 0 -1 -8 0.83 7.95 0 -1 8 27.58 14.58 0 1 -9 9.79 7.18 0 1 9 16.81 13.39 0 -1 9 7.17 10.43 0 -1 9 -4.03 10.05 0 -1 -9 22.09 19.17 0 1 10 -5.52 12.15 0 -1 10 0.33 9.71 0 -1 -10 13.01 10.16 0 -1 10 33.70 20.55 0 -1 -10 5.28 9.96 0 2 0 216.20 11.25 0 -2 0 252.86 14.26 0 -2 0 224.68 10.04 0 2 117820.86 190.28 0 2 117602.33 186.54 0 2 -117922.76 190.75 0 2 -117636.26 181.53 0 -2 117844.77 189.95 0 -2 -117493.04 181.03 0 -2 118041.96 185.68 0 2 2 715.34 18.48 0 2 2 700.64 22.38 0 2 -2 673.76 18.50 0 -2 2 686.66 19.89 0 -2 -2 713.51 15.12 0 -2 2 681.59 13.42 0 2 3 301.48 15.56 0 2 -3 320.92 17.52 0 2 3 315.61 19.48 0 -2 3 359.51 20.89 0 -2 -3 277.87 21.72 0 -2 3 342.05 15.61 0 2 -4 1603.72 34.77 0 2 4 1655.40 37.88 0 2 4 1519.08 30.39 0 -2 4 1615.66 37.36 0 -2 4 1616.66 29.01 0 -2 -4 1597.14 31.36 0 2 5 439.52 25.38 0 2 -5 434.11 31.81 0 2 5 467.92 21.08 0 -2 5 489.36 21.71 0 -2 -5 487.82 21.82 0 -2 5 492.45 25.68 0 2 -6 300.50 57.50 0 2 6 301.50 18.61 0 2 6 281.31 23.40 0 -2 -6 308.24 20.79 0 -2 6 285.37 22.52 0 -2 6 309.93 19.16 0 2 7 1.48 7.94 0 2 -7 10.07 5.35 0 2 7 -1.58 10.61 0 -2 7 10.15 10.92 0 -2 7 5.04 7.20 0 -2 -7 5.88 8.02 0 2 -8 27.78 9.73 0 2 8 10.68 15.39 0 2 8 17.39 16.24 0 -2 8 20.64 16.18 0 -2 -8 5.21 5.60 0 -2 8 12.65 12.83 0 2 -9 10.81 9.26 0 2 9 19.49 19.65 0 2 9 26.02 16.36 0 -2 -9 11.20 11.08 0 -2 9 19.47 13.15 0 -2 9 32.07 17.30 0 2 10 1.94 11.64 0 2 -10 -5.12 10.10 0 -2 -10 -1.99 6.13 0 -2 10 12.98 13.47 0 3 0 28.43 14.76 0 -3 0 -7.06 4.65 0 -3 0 8.76 6.11 0 3 110930.93 124.97 0 3 110579.75 120.90 0 3 -110730.05 123.69 0 -3 110881.25 123.95 0 -3 110901.63 117.27 0 -3 -110812.32 117.13 0 3 -2 70.46 16.54 0 3 2 38.40 12.76 0 3 2 21.73 8.23 0 -3 2 23.68 13.39 0 -3 -2 23.35 7.77 0 -3 2 30.77 5.39 0 3 3 933.04 27.61 0 3 -3 938.05 25.10 0 3 3 916.95 23.18 0 -3 3 936.79 18.78 0 -3 -3 914.70 27.15 0 -3 3 949.18 28.45 0 3 -4 453.94 28.36 0 3 4 501.29 23.76 0 3 4 466.50 17.85 0 -3 4 470.10 15.12 0 -3 -4 448.74 15.63 0 -3 4 469.68 22.34 0 3 5 502.17 25.72 0 3 5 487.21 21.65 0 3 -5 553.22 26.67 0 -3 5 523.07 25.33 0 -3 5 495.77 17.43 0 -3 -5 478.35 47.49 0 3 6 11.55 8.64 0 3 6 17.70 11.87 0 -3 6 4.03 9.94 0 -3 -6 13.81 5.76 0 -3 6 3.18 5.50 0 3 7 561.26 47.01 0 3 -7 478.03 95.94 0 3 7 534.65 40.29 0 -3 -7 455.80 67.41 0 -3 7 495.55 42.05 0 -3 7 536.21 39.78 0 3 8 14.84 13.25 0 3 -8 12.01 7.83 0 3 8 4.66 12.09 0 -3 8 0.74 10.33 0 -3 8 -6.83 7.32 0 -3 -8 -15.16 7.42 0 3 -9 178.59 45.22 0 3 9 232.80 43.17 0 3 9 203.50 41.75 0 -3 9 214.49 45.00 0 -3 9 185.44 35.45 0 -3 -9 148.02 36.71 0 3 -10 14.62 10.71 0 3 10 4.42 13.54 0 -3 10 4.24 13.41 0 -3 -10 9.55 7.39 0 4 0 97.46 21.07 0 -4 0 56.66 8.98 0 -4 0 52.52 9.13 0 4 1 713.50 25.06 0 4 -1 708.38 25.99 0 -4 1 711.17 18.48 0 -4 1 731.27 21.12 0 -4 -1 719.95 22.13 0 -4 -1 754.30 19.87 0 4 2 456.30 17.54 0 4 2 469.65 22.73 0 -4 2 502.20 14.25 0 -4 -2 443.14 19.02 0 4 -3 374.14 20.50 0 4 3 363.81 44.12 0 4 3 349.67 41.79 0 -4 3 379.23 11.90 0 -4 3 349.91 43.06 0 -4 -3 392.15 15.36 0 4 -4 41.79 12.09 0 4 4 61.63 12.29 0 4 4 57.69 14.82 0 -4 -4 47.10 10.93 0 -4 4 48.06 9.36 0 4 5 106.04 19.62 0 4 5 93.64 22.15 0 4 -5 102.42 20.99 0 -4 5 101.25 17.82 0 -4 5 66.35 19.86 0 -4 -5 78.29 20.59 0 4 -6 939.35 93.80 0 4 6 944.66 44.84 0 4 6 906.69 49.67 0 -4 6 932.66 41.79 0 -4 -6 962.66 44.49 0 -4 6 913.83 48.90 0 4 7 -11.86 8.41 0 4 7 -2.82 12.15 0 4 -7 12.24 8.48 0 -4 -7 -3.63 7.92 0 -4 7 -5.81 5.67 0 -4 7 31.41 17.35 0 4 -8 260.49 62.43 0 4 8 333.19 35.97 0 4 8 452.20 49.66 0 -4 -8 234.72 48.83 0 -4 8 318.87 33.22 0 -4 8 423.99 48.43 0 4 9 15.53 13.67 0 4 -9 9.93 10.38 0 4 9 -19.47 14.20 0 -4 -9 9.44 8.80 0 -4 9 19.50 19.84 0 4 10 34.85 24.90 0 4 -10 24.87 18.78 0 -4 10 56.60 29.41 0 5 0 -7.22 13.43 0 -5 0 -6.92 6.69 0 -5 0 -0.48 5.80 0 5 -1 4749.28 65.39 0 5 1 4756.28 65.55 0 -5 -1 4790.91 108.42 0 -5 1 4806.17 55.23 0 -5 1 4924.37 61.75 0 -5 -1 4757.63 54.60 0 5 2 2481.47 45.33 0 5 -2 2574.65 49.84 0 -5 2 2496.95 44.45 0 -5 -2 2548.89 36.84 0 -5 -2 2550.86 45.86 0 -5 2 2555.93 34.70 0 5 3 776.47 30.02 0 5 -3 705.42 26.81 0 5 3 777.66 27.52 0 -5 3 752.68 17.02 0 -5 3 748.33 26.62 0 -5 -3 752.09 20.73 0 5 4 245.40 18.27 0 5 -4 239.52 20.42 0 5 4 225.38 21.10 0 -5 4 203.26 10.36 0 -5 -4 262.50 16.54 0 -5 4 242.77 21.37 0 5 5 221.76 19.59 0 5 5 218.10 25.46 0 5 -5 205.44 20.94 0 -5 5 200.94 13.08 0 -5 -5 224.08 15.67 0 -5 5 202.75 22.05 0 5 6 46.89 24.53 0 5 -6 25.73 21.51 0 5 6 60.81 24.62 0 -5 -6 49.10 19.31 0 -5 6 25.07 15.09 0 5 7 91.48 21.77 0 5 7 67.86 13.33 0 5 -7 86.38 16.94 0 -5 -7 102.46 15.03 0 -5 7 50.40 11.14 0 -5 7 62.00 16.85 0 5 8 1.22 14.25 0 5 8 -10.05 9.94 0 5 -8 -9.28 12.14 0 -5 -8 6.21 9.23 0 -5 8 40.24 18.16 0 5 -9 46.26 22.47 0 5 9 15.55 16.46 0 5 9 50.04 19.65 0 -5 9 81.54 25.95 0 5 -10 -9.68 13.28 0 -5 10 -16.07 14.13 0 -5 -10 -12.05 14.07 0 6 0 2990.84 56.67 0 -6 0 2942.21 50.24 0 -6 0 3022.20 45.51 0 6 -1 342.91 46.14 0 6 1 334.28 21.17 0 -6 -1 333.35 53.44 0 -6 1 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-14 9 2 13.73 15.18 14 -9 -2 27.82 32.15 -14 -9 2 2.64 17.15 -15 0 7 3.68 15.31 -15 0 6 36.52 19.05 15 0 -6 -8.24 12.60 -15 0 6 34.64 20.17 -15 0 5 11.46 14.33 -15 0 5 7.97 13.14 15 0 -5 -21.08 12.89 -15 0 4 -4.94 12.07 15 0 -4 3.81 13.85 -15 0 4 11.96 10.75 -15 0 3 -4.55 13.36 15 0 -3 8.64 13.69 -15 0 3 -5.19 7.85 15 0 -2 15.26 16.64 -15 0 2 11.35 18.00 -15 0 1 -20.96 17.05 15 0 -1 25.30 22.66 15 0 0 61.69 21.12 -15 0 0 62.48 27.21 -15 0 -1 -26.72 18.77 15 0 1 -1.67 14.99 15 0 2 0.71 18.42 -15 0 -2 62.69 35.38 15 0 3 8.13 19.09 -15 0 -3 14.63 21.85 15 1 -8 -6.09 13.66 -15 1 8 -14.30 16.31 15 1 -7 4.15 14.03 -15 1 7 -16.63 14.57 -15 -1 7 16.39 19.75 15 -1 -7 -11.34 14.21 15 1 -6 -6.81 12.29 -15 1 6 16.51 14.75 -15 -1 6 -9.75 11.59 15 -1 -6 -16.43 13.49 15 1 -5 13.13 12.91 -15 1 5 5.66 12.34 15 1 -5 18.08 17.50 -15 1 5 54.41 19.61 -15 -1 5 52.49 23.42 15 -1 -5 -11.24 14.86 15 1 -4 37.21 20.63 15 1 -4 20.52 13.19 -15 1 4 14.05 14.27 -15 1 4 23.66 15.99 15 -1 -4 -19.12 13.67 -15 -1 4 -2.14 12.89 15 1 -3 4.53 9.13 -15 1 3 7.84 11.70 15 1 -3 -2.14 13.12 -15 1 3 4.71 13.15 -15 -1 3 2.22 15.50 15 -1 -3 -18.00 16.04 15 1 -2 5.11 13.45 -15 1 2 -4.21 14.38 15 -1 -2 -3.75 14.68 -15 -1 2 -11.36 16.03 -15 1 1 16.95 19.58 15 1 -1 37.36 18.76 -15 -1 1 38.98 28.24 15 -1 -1 26.20 22.90 -15 1 0 -0.60 18.16 15 1 0 -8.04 11.92 15 -1 0 10.83 17.26 -15 -1 0 67.50 32.35 -15 1 -1 0.38 17.21 15 1 1 17.32 16.74 15 -1 1 8.79 19.54 -15 -1 -1 32.68 23.60 -15 1 -2 171.24 127.80 -15 -1 -2 63.03 32.49 15 -1 2 33.78 20.76 -15 1 -3 17.34 21.17 15 1 3 6.63 16.22 -15 -1 -3 20.51 24.16 15 -1 3 17.05 19.56 -15 2 7 43.88 27.10 15 2 -7 23.63 19.35 -15 -2 7 25.72 20.88 15 -2 -7 -11.29 14.82 15 2 -6 6.45 13.27 -15 2 6 20.60 14.37 -15 -2 6 65.05 29.43 15 -2 -6 18.95 24.41 -15 2 5 -5.96 10.83 15 2 -5 -13.62 11.42 15 2 -5 8.39 11.00 -15 -2 5 24.37 18.20 15 -2 -5 0.71 14.87 -15 2 4 -24.93 11.34 15 2 -4 22.99 19.58 -15 2 4 -13.06 9.50 15 2 -4 -19.05 10.47 15 -2 -4 -19.24 16.41 -15 -2 4 3.25 15.01 -15 2 3 10.29 12.18 15 2 -3 -5.00 13.41 -15 2 3 4.87 14.49 15 2 -3 -7.36 10.82 15 -2 -3 8.99 17.01 -15 -2 3 -1.17 14.49 15 2 -2 33.60 19.99 -15 2 2 35.23 12.65 -15 2 2 15.97 17.21 -15 -2 2 38.75 20.38 15 -2 -2 57.87 22.61 15 2 -1 3.27 13.09 -15 2 1 21.83 22.85 -15 -2 1 20.07 22.79 15 -2 -1 27.07 25.13 15 2 0 38.70 21.68 -15 2 0 16.34 20.01 15 -2 0 12.86 19.86 -15 -2 0 -21.55 20.60 -15 2 -1 139.96 40.79 -15 -2 -1 91.33 33.78 15 -2 1 117.11 35.02 15 2 2 -31.36 13.81 -15 2 -2 7.38 17.26 15 -2 2 -4.02 18.14 -15 -2 -2 43.60 35.89 -15 2 -3 -16.36 18.21 15 2 3 -8.02 14.99 -15 -2 -3 22.25 22.08 15 -2 3 1.38 17.08 15 3 -7 -15.26 14.13 -15 3 7 28.42 23.61 15 -3 -7 -8.67 16.13 -15 -3 7 42.09 24.93 15 3 -6 23.16 13.46 -15 3 6 61.35 27.22 15 -3 -6 11.32 18.64 -15 -3 6 39.74 22.66 15 3 -5 14.36 11.14 -15 3 5 7.94 12.50 15 -3 -5 0.17 17.10 -15 -3 5 7.63 15.08 15 3 -4 -11.45 10.66 15 3 -4 -0.99 12.87 -15 3 4 2.85 10.42 15 -3 -4 10.38 16.46 -15 -3 4 -4.56 15.62 -15 3 3 32.65 13.30 15 3 -3 31.79 8.80 -15 3 3 25.88 21.94 15 3 -3 30.77 15.17 -15 -3 3 38.85 25.53 15 -3 -3 -5.67 14.88 -15 3 2 11.52 16.27 -15 3 2 16.36 13.65 15 3 -2 -1.34 12.92 15 -3 -2 13.74 18.76 -15 -3 2 -1.57 19.80 -15 3 1 9.61 17.24 15 3 -1 12.33 14.27 15 -3 -1 5.90 18.97 -15 -3 1 9.56 20.31 -15 3 0 2.33 13.07 15 3 0 31.89 21.33 15 -3 0 3.69 17.78 -15 -3 0 9.65 19.92 15 3 1 -8.82 14.86 -15 3 -1 -21.84 14.29 -15 -3 -1 -1.64 23.04 15 -3 1 12.19 19.13 -15 3 -2 8.78 18.75 15 3 2 4.05 15.24 15 -3 2 29.93 21.33 -15 -3 -2 49.32 35.68 -15 3 -3 -28.63 17.26 15 3 3 21.31 19.32 15 -3 3 -1.49 15.32 -15 -3 -3 26.51 25.91 15 4 -7 6.99 17.83 -15 4 7 -6.58 15.06 15 -4 -7 74.03 34.72 -15 -4 7 21.99 16.25 -15 4 6 15.16 16.33 15 4 -6 -6.24 14.74 15 -4 -6 43.15 22.73 -15 -4 6 15.35 17.46 15 4 -5 -4.63 9.01 -15 4 5 14.18 15.23 -15 -4 5 4.81 14.11 15 -4 -5 52.10 30.70 -15 4 4 -16.53 10.68 15 4 -4 14.47 11.16 15 -4 -4 -0.50 16.71 -15 -4 4 10.19 16.31 -15 4 3 -1.64 9.33 15 4 -3 2.73 11.26 15 4 -3 4.21 8.09 15 -4 -3 28.21 25.21 -15 -4 3 -14.73 16.61 -15 4 2 18.91 13.29 -15 4 2 36.66 19.36 15 4 -2 32.14 16.47 -15 -4 2 17.93 21.05 15 -4 -2 28.78 19.57 -15 4 1 10.28 14.96 15 4 -1 -3.08 13.07 -15 -4 1 -0.17 18.12 15 -4 -1 16.02 19.53 -15 4 0 -5.76 15.18 15 4 0 6.28 13.98 15 -4 0 10.29 19.62 -15 -4 0 8.90 24.49 -15 4 -1 3.68 15.24 15 4 1 16.85 18.46 -15 -4 -1 21.20 24.58 15 -4 1 8.04 18.87 -15 4 -2 -8.97 15.28 15 4 2 19.27 18.80 -15 -4 -2 -0.20 24.76 15 -4 2 20.30 20.69 -15 5 6 15.67 16.86 15 5 -6 -22.54 14.59 15 -5 -6 35.54 23.57 -15 -5 6 -7.63 15.84 15 5 -5 11.16 8.76 -15 5 5 3.45 14.15 -15 -5 5 -17.44 15.80 15 -5 -5 -2.57 18.45 -15 5 4 33.65 15.61 15 5 -4 15.54 9.84 -15 -5 4 27.62 28.14 15 -5 -4 -5.96 17.16 -15 5 3 26.70 13.50 15 5 -3 11.83 16.00 15 -5 -3 -9.82 21.45 -15 -5 3 16.13 20.16 -15 5 2 29.30 18.41 15 5 -2 2.23 11.28 -15 -5 2 -3.35 17.51 15 -5 -2 -25.38 19.82 -15 5 1 9.60 12.52 15 5 -1 14.94 18.47 15 -5 -1 24.42 21.04 -15 -5 1 25.87 23.80 15 5 0 8.95 14.43 -15 5 0 16.46 21.07 15 -5 0 -15.93 18.74 -15 -5 0 37.54 26.14 -15 5 -1 -4.02 13.50 15 5 1 7.65 15.52 15 -5 1 42.27 31.88 -15 -5 -1 -13.46 26.56 -15 5 -2 -3.33 14.19 15 5 2 24.79 18.12 15 -5 2 5.23 15.62 -15 -5 -2 6.20 23.17 -15 6 6 13.51 21.24 15 6 -6 -4.65 15.17 -15 -6 6 -10.04 16.46 15 -6 -6 34.70 30.74 -15 6 5 4.47 13.97 15 6 -5 26.43 11.40 15 -6 -5 5.98 19.39 -15 -6 5 -8.22 16.17 -15 6 4 8.22 14.19 15 6 -4 14.18 15.92 -15 -6 4 26.81 25.53 15 -6 -4 22.91 30.47 -15 6 3 39.10 21.51 15 -6 -3 76.01 39.53 -15 -6 3 -13.52 15.83 -15 6 2 -1.60 10.26 15 -6 -2 15.91 23.19 -15 -6 2 31.36 23.83 15 6 -1 12.11 14.48 -15 -6 1 0.07 20.91 15 -6 -1 -13.84 19.28 15 6 0 9.61 14.78 -15 -6 0 -3.87 24.55 15 -6 0 -23.26 19.32 -15 6 -1 -4.25 13.20 15 6 1 -13.13 14.32 15 -6 1 -6.57 14.93 -15 -6 -1 3.43 21.99 -15 7 4 10.13 14.38 15 7 -4 -10.28 13.86 -15 -7 4 -15.68 18.37 15 -7 -4 46.44 25.34 -15 7 3 1.11 12.22 -15 -7 3 7.72 18.13 15 -7 -3 -8.33 22.18 -15 7 2 38.67 22.00 -15 -7 2 44.58 25.75 15 -7 -2 -7.99 19.76 -15 -7 1 -16.35 21.62 15 -7 -1 34.56 24.58 15 7 0 22.92 20.90 15 -7 0 -14.39 16.00 -15 -7 0 66.52 35.23 -16 0 7 20.53 22.77 16 0 -6 44.35 22.66 -16 0 6 55.86 32.28 16 0 -5 39.48 22.19 -16 0 5 -7.16 11.67 -16 0 5 1.43 11.26 -16 0 4 -4.82 13.32 -16 0 4 8.34 10.86 16 0 -4 24.90 16.79 -16 0 3 -16.88 14.59 16 0 -3 -8.03 12.92 16 0 -2 34.99 18.13 -16 0 2 34.79 19.13 16 0 -1 -11.31 14.48 16 0 0 44.35 19.73 -16 0 0 69.12 32.87 16 0 1 17.96 20.06 -16 0 -1 -19.63 20.18 -16 0 -2 0.07 19.23 16 0 2 16.85 17.80 -16 1 7 7.89 15.42 16 1 -7 -7.24 12.36 16 1 -6 37.18 25.80 -16 1 6 32.89 19.70 16 -1 -6 39.82 21.50 -16 -1 6 3.51 13.26 16 1 -5 46.30 27.09 16 1 -5 15.65 15.01 -16 1 5 38.37 17.22 -16 -1 5 31.78 20.06 16 1 -4 7.05 10.71 16 1 -4 34.54 20.24 -16 1 4 -16.60 11.19 -16 1 4 -2.00 10.24 16 -1 -4 2.64 14.33 -16 -1 4 9.29 14.91 -16 1 3 20.35 22.91 16 1 -3 29.96 16.73 -16 -1 3 29.49 16.93 16 -1 -3 10.04 17.28 16 1 -2 38.54 20.95 -16 1 2 -2.59 16.39 -16 -1 2 -11.46 18.00 16 -1 -2 21.20 18.66 -16 1 1 -15.15 16.73 16 1 -1 12.11 16.36 -16 -1 1 26.00 19.55 16 -1 -1 55.34 26.54 16 1 0 -13.08 15.09 -16 1 0 4.24 19.09 16 -1 0 30.98 24.13 -16 -1 0 -1.05 19.94 16 1 1 -4.99 15.63 -16 1 -1 10.70 21.13 16 -1 1 -8.61 16.68 -16 -1 -1 73.61 41.33 -16 1 -2 46.07 31.54 16 1 2 -4.17 15.92 -16 -1 -2 36.00 25.37 16 -1 2 40.98 28.71 -16 2 6 53.51 29.13 16 2 -6 18.86 16.66 16 -2 -6 31.96 20.78 -16 -2 6 25.90 17.14 16 2 -5 -1.42 10.63 -16 2 5 24.37 14.81 -16 -2 5 -1.08 12.80 16 -2 -5 2.57 16.15 16 2 -4 19.03 19.87 16 2 -4 44.53 15.34 -16 2 4 8.43 11.37 -16 -2 4 56.84 24.49 16 -2 -4 69.78 30.69 -16 2 3 -0.44 9.35 -16 2 3 20.97 17.27 16 2 -3 -2.06 12.71 -16 -2 3 -9.48 16.50 16 -2 -3 25.86 18.45 -16 2 2 37.84 24.07 16 2 -2 17.40 16.55 -16 -2 2 10.57 17.35 16 -2 -2 23.66 23.53 16 2 -1 -3.43 13.19 -16 2 1 -18.64 16.64 16 -2 -1 -1.83 16.87 -16 -2 1 1.70 19.32 -16 2 0 41.05 28.03 16 2 0 16.36 18.86 16 -2 0 18.79 20.78 -16 -2 0 -21.41 24.33 16 2 1 18.64 19.57 -16 2 -1 -24.44 18.50 16 -2 1 7.05 17.54 -16 -2 -1 -1.07 21.60 16 2 2 37.26 27.22 -16 2 -2 -3.44 18.79 16 -2 2 60.89 30.65 -16 -2 -2 47.33 28.50 16 3 -6 -3.54 15.57 -16 3 6 -34.46 13.44 -16 -3 6 14.41 15.67 16 -3 -6 4.03 16.82 16 3 -5 8.73 7.10 -16 3 5 9.24 13.68 16 -3 -5 -6.61 17.13 -16 -3 5 26.13 21.74 16 3 -4 3.53 12.27 16 3 -4 12.75 15.20 -16 3 4 14.29 14.16 16 -3 -4 21.15 19.64 16 3 -3 31.74 20.06 -16 3 3 -0.84 9.87 -16 -3 3 10.17 16.63 16 -3 -3 20.25 22.19 16 3 -2 1.88 12.69 -16 3 2 4.48 13.11 -16 -3 2 1.74 19.56 16 -3 -2 -5.07 15.94 16 3 -1 21.42 16.17 -16 3 1 36.09 23.97 -16 -3 1 87.90 47.73 16 -3 -1 25.22 29.59 16 3 0 55.91 28.00 -16 3 0 -18.37 16.88 16 -3 0 2.29 18.89 -16 -3 0 13.41 22.60 -16 3 -1 13.41 19.04 16 3 1 16.11 18.12 16 -3 1 37.37 32.05 -16 -3 -1 55.18 41.78 -16 4 6 13.13 15.27 16 4 -6 18.75 13.56 16 -4 -6 -11.80 18.32 -16 -4 6 27.90 23.81 16 4 -5 48.19 21.02 -16 4 5 9.76 15.15 16 -4 -5 30.26 28.10 -16 -4 5 -7.70 15.07 -16 4 4 12.71 18.06 16 4 -4 39.79 19.51 -16 -4 4 21.64 18.36 16 -4 -4 7.39 18.57 16 4 -3 -6.47 11.93 -16 4 3 -0.34 9.99 16 -4 -3 6.98 18.29 -16 -4 3 50.38 31.73 16 4 -2 -11.84 12.94 16 -4 -2 11.50 21.67 -16 -4 2 5.51 22.62 -16 4 1 11.78 16.29 16 4 -1 32.96 22.17 16 -4 -1 14.31 21.06 -16 -4 1 2.72 19.57 -16 4 0 -4.39 13.88 16 4 0 -23.83 14.81 16 -4 0 41.10 25.80 -16 -4 0 -20.61 23.33 16 4 1 5.46 16.19 -16 4 -1 7.91 15.88 -16 -4 -1 49.16 27.53 16 -4 1 14.68 24.41 16 5 -5 -9.10 14.13 -16 5 5 12.12 15.31 16 -5 -5 89.57 44.34 -16 -5 5 3.86 15.92 -16 5 4 5.66 12.98 -16 -5 4 46.19 35.25 16 -5 -4 29.30 30.90 -16 5 3 49.92 26.66 -16 -5 3 16.82 20.94 16 -5 -3 16.53 20.92 16 5 -2 34.44 22.30 -16 -5 2 2.70 18.24 16 -5 -2 8.48 18.75 16 5 -1 17.52 16.23 -16 -5 1 51.62 31.20 16 -5 -1 69.24 39.79 16 5 0 9.58 14.95 16 -5 0 1.84 16.79 -16 -5 0 12.42 21.36 -16 6 4 33.21 21.77 16 -6 -4 32.78 28.01 -16 -6 4 41.81 28.40 -16 -6 3 81.36 37.01 16 -6 -3 15.31 19.62 -16 -6 2 0.68 19.68 16 -6 -2 -16.14 19.31 -16 -6 1 -0.69 18.85 16 -6 -1 -0.18 17.65 17 0 -5 -10.04 13.53 -17 0 4 11.17 15.82 17 0 -4 29.79 24.22 17 0 -3 -18.20 15.87 -17 0 3 14.85 17.09 17 0 -2 29.42 19.42 -17 0 2 20.49 21.14 -17 0 1 -21.35 19.18 17 0 -1 -0.73 15.90 -17 0 0 8.17 20.27 17 0 0 39.99 21.94 17 1 -5 6.16 12.07 -17 1 5 16.43 19.52 17 -1 -5 32.65 22.68 -17 -1 5 29.47 21.57 17 1 -4 -6.17 13.89 -17 -1 4 30.56 23.62 17 -1 -4 38.89 27.85 17 1 -3 104.00 78.22 -17 1 3 110.52 81.68 -17 -1 3 34.00 22.54 17 -1 -3 47.65 25.07 -17 1 2 30.60 20.78 17 1 -2 -4.32 14.75 17 -1 -2 54.50 31.69 -17 -1 2 33.15 28.21 17 1 -1 5.08 15.67 -17 1 1 -17.26 17.69 17 -1 -1 24.02 21.65 -17 -1 1 40.63 33.76 17 1 0 -14.03 15.19 -17 1 0 1.53 20.01 -17 -1 0 1.66 20.98 17 -1 0 38.68 26.35 -17 2 5 -18.01 12.69 17 -2 -5 -1.22 16.10 -17 -2 5 -5.45 13.90 17 2 -4 4.69 13.52 -17 -2 4 40.15 22.81 17 -2 -4 17.60 18.91 17 2 -3 -1.45 13.61 17 -2 -3 -0.73 16.61 -17 -2 3 -28.45 16.61 17 2 -2 29.87 19.18 -17 2 2 31.20 19.70 -17 -2 2 -17.19 20.11 17 -2 -2 42.55 25.11 17 2 -1 -9.65 13.96 -17 2 1 7.57 17.03 -17 -2 1 -4.49 21.09 17 -2 -1 11.68 19.54 -17 2 0 5.71 17.83 17 2 0 40.49 21.17 -17 -2 0 114.93 51.66 17 -2 0 13.10 17.74 17 -3 -4 -17.96 17.18 -17 -3 4 13.41 17.74 17 3 -3 35.13 24.32 17 -3 -3 18.05 20.15 -17 -3 3 4.22 18.91 17 3 -2 6.17 14.93 -17 -3 2 14.81 21.05 17 -3 -2 63.28 32.72 -17 3 1 40.53 24.79 17 3 -1 -5.91 14.14 -17 -3 1 59.80 34.71 17 -4 -3 -7.73 18.51 -17 -4 3 30.70 27.26 17 4 -2 31.24 23.08 17 -4 -2 -12.97 17.53 -17 -4 2 9.11 18.22 ; loop_ _symmetry_equiv_pos_site_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +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_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.67783(7) 0.99640(8) 0.49400(10) 0.0546(3) Uani 1 4 d . . . N1 N 0.5546(2) 0.6871(3) 0.6228(4) 0.0717(9) Uani 1 4 d . . . N2 N 0.9282(2) 0.9518(3) 0.3118(4) 0.0706(9) Uani 1 4 d . . . C1 C 0.6502(2) 0.8447(3) 0.5432(4) 0.0495(8) Uani 1 4 d . . . C2 C 0.7133(2) 0.7620(3) 0.4968(3) 0.0472(7) Uani 1 4 d . . . C3 C 0.7922(2) 0.8172(3) 0.4321(4) 0.0475(7) Uani 1 4 d . . . C4 C 0.7859(2) 0.9418(3) 0.4292(4) 0.0515(8) Uani 1 4 d . . . C5 C 0.7321(2) 1.0630(3) 0.6879(4) 0.0492(7) Uani 1 4 d . . . C6 C 0.5718(3) 0.8030(4) 0.6063(4) 0.0623(9) Uani 1 4 d . . . C7 C 0.6158(3) 0.6110(4) 0.5748(5) 0.0681(10) Uani 1 4 d . . . C8 C 0.6954(3) 0.6423(3) 0.5126(4) 0.0573(9) Uani 1 4 d . . . C9 C 0.8563(3) 1.0027(4) 0.3673(4) 0.0630(9) Uani 1 4 d . . . C10 C 0.9324(3) 0.8335(4) 0.3175(5) 0.0694(10) Uani 1 4 d . . . C11 C 0.8674(3) 0.7629(3) 0.3760(4) 0.0586(9) Uani 1 4 d . . . C12 C 0.6663(3) 1.1219(3) 0.7613(4) 0.0563(9) Uani 1 4 d . . . C13 C 0.7007(3) 1.1735(3) 0.9091(5) 0.0640(10) Uani 1 4 d . . . C14 C 0.8020(3) 1.1680(3) 0.9821(5) 0.0660(10) Uani 1 4 d . . . C15 C 0.8677(3) 1.1119(3) 0.9096(4) 0.0601(9) Uani 1 4 d . . . C16 C 0.8341(3) 1.0589(3) 0.7635(4) 0.0542(8) Uani 1 4 d . . . H6 H 0.52958 0.85816 0.63849 0.0748 Uiso 1 4 calc R . . H7 H 0.60355 0.53 0.58428 0.0817 Uiso 1 4 calc R . . H8 H 0.73621 0.58471 0.48186 0.0687 Uiso 1 4 calc R . . H9 H 0.85265 1.08562 0.36463 0.0756 Uiso 1 4 calc R . . H10 H 0.98286 0.79602 0.27909 0.0833 Uiso 1 4 calc R . . H11 H 0.87408 0.68022 0.37768 0.0703 Uiso 1 4 calc R . . H12 H 0.59798 1.12682 0.71063 0.0675 Uiso 1 4 calc R . . H13 H 0.65578 1.21156 0.95892 0.0768 Uiso 1 4 calc R . . H14 H 0.8258 1.20288 1.08153 0.0792 Uiso 1 4 calc R . . H15 H 0.93619 1.10947 0.95957 0.0722 Uiso 1 4 calc R . . H16 H 0.8796 1.0204 0.71524 0.0650 Uiso 1 4 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 P1 0.0570(5) 0.0519(5) 0.0553(5) 0.0097(4) 0.0138(4) -0.0002(4) N1 0.0605(19) 0.080(2) 0.077(2) -0.0119(17) 0.0196(17) 0.0019(19) N2 0.069(2) 0.083(2) 0.0665(19) -0.0036(18) 0.0277(16) -0.0037(18) C1 0.0418(17) 0.056(2) 0.0483(17) 0.0008(14) 0.0059(14) -0.0000(15) C2 0.0449(17) 0.0509(18) 0.0425(16) 0.0043(14) 0.0040(14) -0.0023(14) C3 0.0457(17) 0.0526(19) 0.0434(16) 0.0033(14) 0.0086(14) -0.0019(14) C4 0.058(2) 0.0505(19) 0.0471(16) 0.0005(16) 0.0146(15) 0.0002(15) C5 0.0561(19) 0.0375(17) 0.0577(18) 0.0079(14) 0.0209(16) 0.0044(14) C6 0.049(2) 0.075(3) 0.062(2) 0.0021(18) 0.0107(17) -0.0023(19) C7 0.071(3) 0.061(2) 0.070(2) -0.011(2) 0.013(2) 0.0016(19) C8 0.060(2) 0.051(2) 0.060(2) -0.0030(16) 0.0111(17) -0.0038(16) C9 0.073(2) 0.061(2) 0.060(2) -0.0038(19) 0.0247(18) -0.0009(18) C10 0.058(2) 0.083(3) 0.072(2) 0.004(2) 0.024(2) -0.006(2) C11 0.060(2) 0.058(2) 0.059(2) 0.0077(17) 0.0159(17) -0.0087(17) C12 0.057(2) 0.0481(19) 0.065(2) 0.0050(15) 0.0158(18) -0.0018(16) C13 0.077(3) 0.047(2) 0.074(2) 0.0033(18) 0.029(2) -0.0109(18) C14 0.085(3) 0.052(2) 0.063(2) -0.0060(19) 0.021(2) -0.0091(18) C15 0.055(2) 0.058(2) 0.066(2) -0.0098(17) 0.0108(18) -0.0045(17) C16 0.058(2) 0.0464(19) 0.061(2) -0.0003(15) 0.0205(17) 0.0041(16) 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 for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.1023 0.0942 ; International Tables for Crystallography (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_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C1 P1 C4 89.10(16) yes . . . C1 P1 C5 103.23(14) yes . . . C4 P1 C5 104.03(15) yes . . . C6 N1 C7 117.0(4) yes . . . C9 N2 C10 116.7(4) yes . . . P1 C1 C2 112.5(3) yes . . . P1 C1 C6 129.0(3) yes . . . C2 C1 C6 118.3(3) yes . . . C1 C2 C3 112.9(3) yes . . . C1 C2 C8 119.2(3) yes . . . C3 C2 C8 127.9(3) yes . . . C2 C3 C4 112.5(3) yes . . . C2 C3 C11 128.6(3) yes . . . C4 C3 C11 118.9(3) yes . . . P1 C4 C3 112.6(3) yes . . . P1 C4 C9 130.1(3) yes . . . C3 C4 C9 117.1(3) yes . . . P1 C5 C12 116.9(2) yes . . . P1 C5 C16 124.2(3) yes . . . C12 C5 C16 118.9(3) yes . . . N1 C6 C1 122.7(4) yes . . . N1 C7 C8 125.0(4) yes . . . C2 C8 C7 117.7(3) yes . . . N2 C9 C4 124.6(4) yes . . . N2 C10 C11 124.4(4) yes . . . C3 C11 C10 118.3(4) yes . . . C5 C12 C13 120.7(3) yes . . . C12 C13 C14 119.4(4) yes . . . C13 C14 C15 120.3(3) yes . . . C14 C15 C16 120.8(3) yes . . . C5 C16 C15 119.9(3) yes . . . N1 C6 H6 118.629 no . . . C1 C6 H6 118.629 no . . . N1 C7 H7 117.487 no . . . C8 C7 H7 117.483 no . . . C2 C8 H8 121.132 no . . . C7 C8 H8 121.130 no . . . N2 C9 H9 117.695 no . . . C4 C9 H9 117.691 no . . . N2 C10 H10 117.795 no . . . C11 C10 H10 117.793 no . . . C3 C11 H11 120.869 no . . . C10 C11 H11 120.853 no . . . C5 C12 H12 119.643 no . . . C13 C12 H12 119.641 no . . . C12 C13 H13 120.300 no . . . C14 C13 H13 120.309 no . . . C13 C14 H14 119.822 no . . . C15 C14 H14 119.840 no . . . C14 C15 H15 119.602 no . . . C16 C15 H15 119.611 no . . . C5 C16 H16 120.065 no . . . C15 C16 H16 120.070 no . . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 P1 C1 1.813(4) yes . . P1 C4 1.800(4) yes . . P1 C5 1.823(3) yes . . N1 C6 1.333(5) yes . . N1 C7 1.325(6) yes . . N2 C9 1.316(5) yes . . N2 C10 1.327(6) yes . . C1 C2 1.385(5) yes . . C1 C6 1.388(5) yes . . C2 C3 1.459(5) yes . . C2 C8 1.376(5) yes . . C3 C4 1.398(5) yes . . C3 C11 1.375(5) yes . . C4 C9 1.382(5) yes . . C5 C12 1.382(5) yes . . C5 C16 1.388(4) yes . . C7 C8 1.363(6) yes . . C10 C11 1.368(6) yes . . C12 C13 1.379(5) yes . . C13 C14 1.375(6) yes . . C14 C15 1.360(6) yes . . C15 C16 1.373(5) yes . . C6 H6 0.930 no . . C7 H7 0.930 no . . C8 H8 0.930 no . . C9 H9 0.930 no . . C10 H10 0.930 no . . C11 H11 0.930 no . . C12 H12 0.930 no . . C13 H13 0.930 no . . C14 H14 0.930 no . . C15 H15 0.930 no . . C16 H16 0.930 no . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 N1 C2 2.767(5) no . . N2 C3 2.772(5) no . . C1 C7 2.685(5) no . . C4 C10 2.698(6) no . . C4 C16 3.100(5) no . . C5 C14 2.760(5) no . . C6 C8 2.713(5) no . . C8 C11 3.162(6) no . . C9 C11 2.692(5) no . . C9 C16 3.565(5) no . . C12 C15 2.739(5) no . . C13 C16 2.757(6) no . . N1 C1 3.577(5) no . 4_565 N1 C2 3.484(4) no . 4_565 N1 C12 3.460(5) no . 2_646 N1 C13 3.420(5) no . 2_646 N2 N2 3.545(4) no . 3_776 N2 C9 3.564(4) no . 3_776 N2 C16 3.447(5) no . 3_776 C1 N1 3.577(5) no . 4_564 C2 N1 3.484(4) no . 4_564 C2 C6 3.544(4) no . 4_564 C2 C11 3.460(4) no . 4_565 C3 C7 3.527(5) no . 4_564 C3 C8 3.583(5) no . 4_564 C4 C7 3.426(5) no . 4_564 C6 C2 3.544(4) no . 4_565 C6 C8 3.570(5) no . 4_565 C7 C3 3.527(5) no . 4_565 C7 C4 3.426(5) no . 4_565 C8 C3 3.583(5) no . 4_565 C8 C6 3.570(5) no . 4_564 C9 N2 3.564(4) no . 3_776 C11 C2 3.460(4) no . 4_564 C12 N1 3.460(5) no . 2_656 C13 N1 3.420(5) no . 2_656 C16 N2 3.447(5) no . 3_776 P1 H6 3.0351 no . . P1 H9 3.0259 no . . P1 H12 2.7895 no . . P1 H16 2.9631 no . . N1 H8 3.2123 no . . N2 H11 3.2126 no . . C1 H8 3.2296 no . . C2 H6 3.2161 no . . C2 H7 3.1764 no . . C2 H11 2.7830 no . . C3 H8 2.7757 no . . C3 H9 3.2075 no . . C3 H10 3.1860 no . . C3 H16 3.3487 no . . C4 H11 3.2365 no . . C4 H16 2.6508 no . . C5 H6 3.5317 no . . C5 H9 3.5670 no . . C5 H13 3.2384 no . . C5 H15 3.2271 no . . C6 H7 3.1010 no . . C7 H6 3.1066 no . . C8 H11 2.9634 no . . C9 H10 3.0862 no . . C9 H16 2.9562 no . . C10 H9 3.0876 no . . C11 H8 2.9627 no . . C12 H6 3.5186 no . . C12 H14 3.2182 no . . C12 H16 3.2270 no . . C13 H15 3.2090 no . . C14 H12 3.2162 no . . C14 H16 3.2120 no . . C15 H13 3.2112 no . . C16 H9 3.5286 no . . C16 H12 3.2252 no . . C16 H14 3.2126 no . . H6 H12 3.1688 no . . H7 H8 2.2732 no . . H8 H11 2.5036 no . . H9 H16 3.0546 no . . H10 H11 2.2788 no . . H12 H13 2.3086 no . . H13 H14 2.3066 no . . H14 H15 2.2819 no . . H15 H16 2.2982 no . . P1 H6 3.2243 no . 3_676 P1 H7 3.4589 no . 4_564 P1 H13 3.2933 no . 4_574 N1 H7 3.4537 no . 3_666 N1 H12 2.8713 no . 2_646 N1 H13 2.7934 no . 2_646 N2 H8 3.4059 no . 4_564 N2 H9 3.5981 no . 3_776 N2 H14 3.5366 no . 1_554 N2 H15 3.5444 no . 1_554 N2 H15 3.3793 no . 3_776 N2 H16 2.6969 no . 3_776 C1 H12 3.5786 no . 3_676 C2 H11 3.5555 no . 4_565 C4 H7 3.4129 no . 4_564 C5 H8 3.0220 no . 4_565 C5 H11 3.5141 no . 4_565 C5 H13 3.2260 no . 4_574 C5 H14 3.1475 no . 4_574 C6 H12 3.2359 no . 3_676 C6 H13 3.1814 no . 2_646 C7 H7 3.3686 no . 3_666 C8 H6 3.4784 no . 4_564 C9 H8 3.4869 no . 4_564 C9 H14 3.2891 no . 1_554 C10 H8 3.5663 no . 4_564 C10 H14 3.5156 no . 2_746 C10 H15 3.4031 no . 2_746 C10 H15 3.3704 no . 3_776 C10 H16 3.1048 no . 3_776 C11 H10 3.5300 no . 4_565 C11 H15 3.2112 no . 2_746 C11 H16 3.4840 no . 4_564 C12 H7 3.5412 no . 4_565 C12 H8 3.0068 no . 4_565 C12 H13 3.1878 no . 4_574 C12 H14 3.5454 no . 4_574 C13 H7 3.1905 no . 4_565 C13 H8 2.9754 no . 4_565 C13 H9 3.4754 no . 4_575 C14 H8 2.9697 no . 4_565 C14 H9 3.3449 no . 1_556 C14 H9 3.0747 no . 4_575 C14 H10 3.4674 no . 2_756 C15 H8 2.9949 no . 4_565 C15 H9 3.4115 no . 4_575 C15 H10 3.0687 no . 3_776 C15 H11 3.2880 no . 4_565 C15 H14 3.4509 no . 4_574 C16 H8 3.0187 no . 4_565 C16 H10 3.0666 no . 3_776 C16 H11 2.8631 no . 4_565 C16 H14 3.0863 no . 4_574 H6 P1 3.2243 no . 3_676 H6 C8 3.4784 no . 4_565 H6 H12 3.5350 no . 2_646 H6 H12 3.1103 no . 3_676 H6 H13 2.9593 no . 2_646 H7 P1 3.4589 no . 4_565 H7 N1 3.4537 no . 3_666 H7 C4 3.4129 no . 4_565 H7 C7 3.3686 no . 3_666 H7 C12 3.5412 no . 4_564 H7 C13 3.1905 no . 4_564 H7 H7 2.9271 no . 3_666 H7 H13 3.0607 no . 4_564 H8 N2 3.4059 no . 4_565 H8 C5 3.0220 no . 4_564 H8 C9 3.4869 no . 4_565 H8 C10 3.5663 no . 4_565 H8 C12 3.0068 no . 4_564 H8 C13 2.9754 no . 4_564 H8 C14 2.9697 no . 4_564 H8 C15 2.9949 no . 4_564 H8 C16 3.0187 no . 4_564 H8 H12 3.5450 no . 4_564 H8 H13 3.4860 no . 4_564 H8 H14 3.4805 no . 4_564 H8 H15 3.5231 no . 4_564 H8 H16 3.5528 no . 4_564 H9 N2 3.5981 no . 3_776 H9 C13 3.4754 no . 4_574 H9 C14 3.3449 no . 1_554 H9 C14 3.0747 no . 4_574 H9 C15 3.4115 no . 4_574 H9 H14 2.7252 no . 1_554 H9 H14 3.0964 no . 4_574 H10 C11 3.5300 no . 4_564 H10 C14 3.4674 no . 2_746 H10 C15 3.0687 no . 3_776 H10 C16 3.0666 no . 3_776 H10 H11 3.4463 no . 4_564 H10 H14 2.7982 no . 2_746 H10 H15 3.0839 no . 2_746 H10 H15 2.7680 no . 3_776 H10 H16 2.7727 no . 3_776 H11 C2 3.5555 no . 4_564 H11 C5 3.5141 no . 4_564 H11 C15 3.2880 no . 4_564 H11 C16 2.8631 no . 4_564 H11 H10 3.4463 no . 4_565 H11 H15 2.7477 no . 2_746 H11 H15 3.3864 no . 4_564 H11 H16 2.6608 no . 4_564 H12 N1 2.8713 no . 2_656 H12 C1 3.5786 no . 3_676 H12 C6 3.2359 no . 3_676 H12 H6 3.5350 no . 2_656 H12 H6 3.1103 no . 3_676 H12 H8 3.5450 no . 4_565 H12 H13 3.0723 no . 4_574 H13 P1 3.2933 no . 4_575 H13 N1 2.7934 no . 2_656 H13 C5 3.2260 no . 4_575 H13 C6 3.1814 no . 2_656 H13 C12 3.1878 no . 4_575 H13 H6 2.9593 no . 2_656 H13 H7 3.0607 no . 4_565 H13 H8 3.4860 no . 4_565 H13 H12 3.0723 no . 4_575 H14 N2 3.5366 no . 1_556 H14 C5 3.1475 no . 4_575 H14 C9 3.2891 no . 1_556 H14 C10 3.5156 no . 2_756 H14 C12 3.5454 no . 4_575 H14 C15 3.4509 no . 4_575 H14 C16 3.0863 no . 4_575 H14 H8 3.4805 no . 4_565 H14 H9 2.7252 no . 1_556 H14 H9 3.0964 no . 4_575 H14 H10 2.7982 no . 2_756 H14 H16 3.3294 no . 4_575 H15 N2 3.5444 no . 1_556 H15 N2 3.3793 no . 3_776 H15 C10 3.4031 no . 2_756 H15 C10 3.3704 no . 3_776 H15 C11 3.2112 no . 2_756 H15 H8 3.5231 no . 4_565 H15 H10 3.0839 no . 2_756 H15 H10 2.7680 no . 3_776 H15 H11 2.7477 no . 2_756 H15 H11 3.3864 no . 4_565 H15 H15 2.9908 no . 3_777 H16 N2 2.6969 no . 3_776 H16 C10 3.1048 no . 3_776 H16 C11 3.4840 no . 4_565 H16 H8 3.5528 no . 4_565 H16 H10 2.7727 no . 3_776 H16 H11 2.6608 no . 4_565 H16 H14 3.3294 no . 4_574 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C1 P1 C4 C3 5.39(19) no . . . . C1 P1 C4 C9 179.7(2) no . . . . C4 P1 C1 C2 -5.86(19) no . . . . C4 P1 C1 C6 180.0(2) no . . . . C1 P1 C5 C12 -92.9(2) no . . . . C1 P1 C5 C16 87.9(3) no . . . . C5 P1 C1 C2 -110.1(2) no . . . . C5 P1 C1 C6 75.8(3) no . . . . C4 P1 C5 C12 174.7(2) no . . . . C4 P1 C5 C16 -4.5(3) no . . . . C5 P1 C4 C3 108.81(19) no . . . . C5 P1 C4 C9 -76.8(3) no . . . . C6 N1 C7 C8 1.1(5) no . . . . C7 N1 C6 C1 -0.4(5) no . . . . C9 N2 C10 C11 0.2(5) no . . . . C10 N2 C9 C4 -0.3(5) no . . . . P1 C1 C2 C3 4.9(3) no . . . . P1 C1 C2 C8 -173.95(17) no . . . . P1 C1 C6 N1 173.4(2) no . . . . C2 C1 C6 N1 -0.5(4) no . . . . C6 C1 C2 C3 179.8(2) no . . . . C6 C1 C2 C8 0.9(4) no . . . . C1 C2 C3 C4 -0.8(3) no . . . . C1 C2 C3 C11 179.6(2) no . . . . C1 C2 C8 C7 -0.4(4) no . . . . C3 C2 C8 C7 -179.1(2) no . . . . C8 C2 C3 C4 178.0(3) no . . . . C8 C2 C3 C11 -1.6(5) no . . . . C2 C3 C4 P1 -3.7(3) no . . . . C2 C3 C4 C9 -178.9(2) no . . . . C2 C3 C11 C10 178.7(2) no . . . . C4 C3 C11 C10 -0.9(4) no . . . . C11 C3 C4 P1 175.9(2) no . . . . C11 C3 C4 C9 0.8(4) no . . . . P1 C4 C9 N2 -174.3(2) no . . . . C3 C4 C9 N2 -0.1(4) no . . . . P1 C5 C12 C13 179.2(2) no . . . . P1 C5 C16 C15 179.9(2) no . . . . C12 C5 C16 C15 0.7(5) no . . . . C16 C5 C12 C13 -1.6(5) no . . . . N1 C7 C8 C2 -0.6(5) no . . . . N2 C10 C11 C3 0.4(5) no . . . . C5 C12 C13 C14 1.3(5) no . . . . C12 C13 C14 C15 -0.2(5) no . . . . C13 C14 C15 C16 -0.6(5) no . . . . C14 C15 C16 C5 0.4(5) no . . . .