#------------------------------------------------------------------------------ #$Date: 2019-11-04 18:09:09 +0200 (Mon, 04 Nov 2019) $ #$Revision: 223212 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/12/72/4127280.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_4127280 loop_ _publ_author_name 'Devannah, Vijayarajan' 'Sharma, Rajgopal' 'Watson, Donald A.' _publ_section_title ; Nickel-Catalyzed Asymmetric C-Alkylation of Nitroalkanes: Synthesis of Enantioenriched \b-Nitroamides. ; _journal_issue 21 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 8436 _journal_page_last 8440 _journal_paper_doi 10.1021/jacs.9b04175 _journal_volume 141 _journal_year 2019 _chemical_absolute_configuration ad _chemical_formula_sum 'C21 H24 N2 O5' _chemical_formula_weight 384.42 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.7516(3) _cell_length_b 13.2713(4) _cell_length_c 15.4202(5) _cell_measurement_reflns_used 9955 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 74.96 _cell_measurement_theta_min 3.33 _cell_volume 1995.63(11) _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-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 200(2) _diffrn_detector_area_resol_mean 8.33 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type 'Bruker AXS APEX diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0949 _diffrn_reflns_av_unetI/netI 0.0549 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 15610 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.983 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 74.955 _diffrn_reflns_theta_min 4.395 _exptl_absorpt_coefficient_mu 0.756 _exptl_absorpt_correction_T_max 0.7539 _exptl_absorpt_correction_T_min 0.6748 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'APEX3 (Bruker, 2015)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.279 _exptl_crystal_description block _exptl_crystal_F_000 816 _exptl_crystal_size_max 0.424 _exptl_crystal_size_mid 0.412 _exptl_crystal_size_min 0.202 _refine_diff_density_max 0.210 _refine_diff_density_min -0.209 _refine_diff_density_rms 0.051 _refine_ls_abs_structure_details ; Flack x determined using 1697 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.05(9) _refine_ls_extinction_coef 0.0212(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 256 _refine_ls_number_reflns 4057 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.020 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0415 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0743P)^2^+0.2160P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1138 _refine_ls_wR_factor_ref 0.1145 _reflns_Friedel_coverage 0.751 _reflns_Friedel_fraction_full 0.997 _reflns_Friedel_fraction_max 0.981 _reflns_number_gt 3993 _reflns_number_total 4057 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja9b04175_si_003.cif _cod_data_source_block donw063 _cod_depositor_comments 'Adding full bibliography for 4127279--4127281.cif.' _cod_database_code 4127280 _shelx_shelxl_version_number 2014/7 _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 0.740 _shelx_estimated_absorpt_t_max 0.862 _shelx_res_file ; donw063.res created by SHELXL-2014/7 TITL donw063 in P2(1)2(1)2(1) CELL 1.54178 9.7516 13.2713 15.4202 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0004 0.0005 0.000 0.000 0.000 LATT -1 SYMM x+1/2, -y+1/2, -z SYMM -x, y+1/2, -z+1/2 SYMM -x+1/2, -y, z+1/2 SFAC C H N O UNIT 84 96 8 20 L.S. 20 ACTA BOND $H FMAP 2 PLAN 10 HTAB SIZE 0.202 0.412 0.424 TEMP -73.150 WGHT 0.074300 0.216000 EXTI 0.021210 FVAR 0.44595 C1 1 0.463884 0.765083 0.938343 11.00000 0.03936 0.03720 = 0.04414 -0.00723 0.00425 -0.00469 AFIX 43 H1 2 0.538375 0.791837 0.970687 11.00000 -1.20000 AFIX 0 C2 1 0.369538 0.829940 0.900839 11.00000 0.04832 0.03412 = 0.05692 -0.00426 0.00830 0.00153 AFIX 43 H2 2 0.379455 0.900674 0.907924 11.00000 -1.20000 AFIX 0 C3 1 0.260561 0.791918 0.852943 11.00000 0.03998 0.04537 = 0.04852 0.00141 0.00566 0.00896 AFIX 43 H3 2 0.196336 0.836419 0.826886 11.00000 -1.20000 AFIX 0 C4 1 0.246200 0.688857 0.843452 11.00000 0.03535 0.04928 = 0.04284 -0.00436 0.00110 0.00033 AFIX 43 H4 2 0.171807 0.662439 0.810813 11.00000 -1.20000 AFIX 0 C5 1 0.340268 0.623795 0.881518 11.00000 0.04111 0.03446 = 0.04171 -0.00493 0.00104 -0.00291 AFIX 43 H5 2 0.329261 0.553069 0.875041 11.00000 -1.20000 AFIX 0 C6 1 0.450699 0.661284 0.929145 11.00000 0.03558 0.03671 = 0.03309 -0.00460 0.00455 0.00005 C7 1 0.551290 0.591947 0.973615 11.00000 0.04781 0.03814 = 0.03522 -0.00844 -0.00573 0.00289 AFIX 23 H7A 2 0.634873 0.630826 0.988050 11.00000 -1.20000 H7B 2 0.510342 0.568578 1.028813 11.00000 -1.20000 AFIX 0 C8 1 0.656619 0.555428 0.775479 11.00000 0.05387 0.03639 = 0.04106 0.00373 0.00032 0.00556 AFIX 43 H8 2 0.563084 0.569046 0.762856 11.00000 -1.20000 AFIX 0 C9 1 0.756696 0.572083 0.713190 11.00000 0.07981 0.03895 = 0.04416 0.00717 0.01047 -0.00065 AFIX 43 H9 2 0.731535 0.597844 0.657956 11.00000 -1.20000 AFIX 0 C10 1 0.892680 0.551477 0.730903 11.00000 0.06547 0.04197 = 0.06046 0.00026 0.02350 -0.01330 AFIX 43 H10 2 0.960701 0.563132 0.687956 11.00000 -1.20000 AFIX 0 C11 1 0.929563 0.514074 0.810759 11.00000 0.04365 0.05041 = 0.06684 -0.00037 0.00730 -0.01234 AFIX 43 H11 2 1.022873 0.498644 0.822469 11.00000 -1.20000 AFIX 0 C12 1 0.830701 0.498772 0.874407 11.00000 0.03946 0.04496 = 0.04694 0.00272 -0.00136 -0.00792 AFIX 43 H12 2 0.856571 0.474723 0.930080 11.00000 -1.20000 AFIX 0 C13 1 0.693930 0.518843 0.856135 11.00000 0.04187 0.02859 = 0.03827 -0.00038 0.00313 -0.00279 C14 1 0.540855 0.411518 0.943357 11.00000 0.02892 0.03822 = 0.03265 0.00026 -0.00291 0.00363 C15 1 0.580596 0.323836 0.884573 11.00000 0.02716 0.03398 = 0.03166 0.00014 -0.00058 -0.00132 AFIX 13 H15 2 0.671355 0.338235 0.857046 11.00000 -1.20000 AFIX 0 C16 1 0.589367 0.225148 0.935228 11.00000 0.02723 0.03702 = 0.03279 -0.00004 -0.00083 -0.00259 AFIX 13 H16 2 0.494906 0.198863 0.946423 11.00000 -1.20000 AFIX 0 C17 1 0.672223 0.146514 0.885019 11.00000 0.03242 0.03352 = 0.03459 0.00149 -0.00137 -0.00057 AFIX 23 H17A 2 0.637796 0.144481 0.824647 11.00000 -1.20000 H17B 2 0.768990 0.168935 0.882862 11.00000 -1.20000 AFIX 0 C18 1 0.668324 0.040313 0.921578 11.00000 0.03648 0.03468 = 0.04216 0.00174 0.00068 -0.00387 AFIX 23 H18A 2 0.714850 0.038996 0.978629 11.00000 -1.20000 H18B 2 0.571863 0.019335 0.930225 11.00000 -1.20000 AFIX 0 C19 1 0.738556 -0.032369 0.860477 11.00000 0.03233 0.03154 = 0.04223 0.00021 -0.00610 -0.00337 C20 1 0.827489 -0.196236 0.843931 11.00000 0.05971 0.03503 = 0.06249 -0.00560 -0.01423 0.00720 AFIX 137 H20A 2 0.766579 -0.212772 0.795426 11.00000 -1.50000 H20B 2 0.844553 -0.256956 0.878451 11.00000 -1.50000 H20C 2 0.914618 -0.170374 0.821401 11.00000 -1.50000 AFIX 0 C21 1 0.469894 0.315362 0.813444 11.00000 0.03698 0.04313 = 0.03566 0.00258 -0.00588 0.00001 AFIX 137 H21A 2 0.379903 0.305759 0.840500 11.00000 -1.50000 H21B 2 0.490481 0.257722 0.775914 11.00000 -1.50000 H21C 2 0.468990 0.377224 0.778745 11.00000 -1.50000 AFIX 0 N1 3 0.591355 0.503226 0.922212 11.00000 0.03787 0.03457 = 0.03307 -0.00222 0.00057 0.00144 N2 3 0.662403 0.242141 1.020478 11.00000 0.04112 0.04152 = 0.03300 -0.00092 -0.00238 0.00760 O1 4 0.461204 0.398761 1.003943 11.00000 0.04063 0.04614 = 0.04175 -0.00021 0.01151 0.00272 O2 4 0.754591 0.304040 1.022686 11.00000 0.04173 0.04855 = 0.04676 -0.00853 -0.01337 0.00266 O3 4 0.628193 0.189913 1.082201 11.00000 0.08230 0.07158 = 0.03449 0.01483 -0.00010 -0.00131 O4 4 0.763565 -0.120333 0.897861 11.00000 0.05963 0.03200 = 0.05128 0.00256 -0.00331 0.00331 O5 4 0.766720 -0.013963 0.786833 11.00000 0.10407 0.04534 = 0.04907 0.00497 0.01606 0.02164 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM donw063 in P2(1)2(1)2(1) REM R1 = 0.0415 for 3993 Fo > 4sig(Fo) and 0.0431 for all 4057 data REM 256 parameters refined using 0 restraints END WGHT 0.0784 0.1883 REM Instructions for potential hydrogen bonds EQIV $1 x-1/2, -y+1/2, -z+2 HTAB C16 O2_$1 EQIV $2 x+1/2, -y+1/2, -z+2 HTAB C18 O1_$2 REM Highest difference peak 0.210, deepest hole -0.209, 1-sigma level 0.051 Q1 1 0.5999 0.2798 0.9060 11.00000 0.05 0.21 Q2 1 0.5652 0.3559 0.9100 11.00000 0.05 0.18 Q3 1 0.7319 0.0349 0.7819 11.00000 0.05 0.15 Q4 1 0.4549 0.7176 0.9379 11.00000 0.05 0.15 Q5 1 0.6327 0.1868 0.9074 11.00000 0.05 0.14 Q6 1 0.6864 0.3005 0.8406 11.00000 0.05 0.14 Q7 1 0.5857 0.4572 0.9387 11.00000 0.05 0.13 Q8 1 0.6588 0.0824 0.9153 11.00000 0.05 0.13 Q9 1 1.1069 0.4701 0.8644 11.00000 0.05 0.13 Q10 1 0.4140 0.2678 0.8122 11.00000 0.05 0.13 ; _shelx_res_checksum 41123 _shelx_hkl_file ; 0 0 -1 0.02 0.01 0 0 1 0.22 0.01 0 0 -2 509.54 6.77 0 0 2 452.03 6.32 0 0 -3 0.16 0.03 0 0 3 0.06 0.02 0 0 -4 808.88 3.03 0 0 4 621.50 2.63 0 0 -5 0.00 0.03 0 0 5 0.15 0.03 0 0 -6 98.44 0.50 0 0 6 71.45 0.43 0 0 6 93.05 0.56 0 0 7 -0.02 0.04 0 0 8 13.81 0.26 0 0 8 15.74 0.28 0 0 9 0.20 0.06 0 0 9 0.13 0.06 0 0 10 64.00 0.64 0 0 10 71.19 0.69 0 0 11 0.00 0.07 0 0 11 0.01 0.06 0 0 12 1.37 0.15 0 0 -14 124.38 1.16 0 0 -15 0.02 0.10 0 0 -16 -0.09 0.09 0 0 -17 -0.06 0.08 0 0 -18 -0.02 0.07 0 0 -19 0.04 0.05 0 -1 0 0.60 0.02 0 1 0 0.01 0.01 0 -1 -1 204.24 1.04 0 -1 1 169.49 0.82 0 1 -1 172.31 0.84 0 1 1 210.85 1.06 0 -1 -2 137.71 0.83 0 -1 2 105.96 0.62 0 1 -2 103.63 0.61 0 1 -2 98.37 0.59 0 1 2 129.23 3.18 0 -1 -3 932.30 12.58 0 -1 3 636.85 8.63 0 1 -3 660.13 9.01 0 1 -3 750.72 2.44 0 1 3 854.92 11.90 0 -1 -4 120.56 0.48 0 -1 4 83.82 0.36 0 1 -4 92.92 0.38 0 1 4 96.25 0.43 0 -1 -5 429.08 8.34 0 -1 5 292.08 1.55 0 -1 5 373.28 1.06 0 1 -5 291.70 1.54 0 1 -5 344.43 6.34 0 1 5 326.72 1.52 0 -1 -6 20.61 0.25 0 -1 6 12.87 0.18 0 -1 6 17.12 0.25 0 1 -6 13.17 0.18 0 1 -6 16.52 0.20 0 1 6 13.46 0.20 0 1 6 16.01 0.23 0 -1 -7 48.26 0.41 0 -1 7 43.55 0.44 0 1 7 43.92 0.41 0 -1 8 116.78 0.77 0 -1 8 127.04 0.81 0 1 8 125.12 0.75 0 -1 9 81.84 0.70 0 -1 9 88.70 0.74 0 1 9 86.46 0.68 0 -1 10 65.62 0.67 0 -1 10 70.98 0.71 0 1 10 67.17 0.65 0 -1 11 51.68 0.64 0 -1 11 56.75 0.68 0 -1 12 7.97 0.28 0 -1 12 7.94 0.28 0 -1 13 12.94 0.36 0 -1 13 12.95 0.37 0 -1 -14 16.72 0.45 0 -1 14 18.83 0.45 0 -1 14 16.44 0.42 0 1 -14 17.40 0.47 0 1 -14 18.60 0.44 0 -1 -15 6.42 0.30 0 -1 15 7.14 0.30 0 1 -15 6.78 0.31 0 1 -15 7.12 0.30 0 -1 -16 0.03 0.09 0 1 -16 -0.03 0.10 0 -1 -17 8.68 0.29 0 1 -17 7.92 0.28 0 -1 -18 18.75 0.34 0 1 -18 18.17 0.35 0 -1 -19 9.46 0.20 0 1 -19 9.88 0.21 0 -2 0 40.94 0.22 0 2 0 46.04 0.24 0 -2 -1 20.07 0.17 0 -2 1 17.60 0.14 0 2 -1 19.26 0.15 0 -2 -2 1155.00 14.82 0 -2 2 757.92 10.36 0 2 -2 888.93 11.18 0 2 -2 840.28 10.78 0 2 2 1171.00 15.01 0 -2 -3 314.97 1.41 0 2 -3 124.90 0.88 0 2 -3 224.25 1.27 0 2 3 312.47 1.80 0 -2 -4 158.02 0.61 0 2 -4 118.76 0.45 0 2 -4 111.06 0.44 0 2 4 139.17 0.58 0 -2 -5 240.23 3.79 0 -2 5 180.98 0.61 0 -2 5 220.95 0.85 0 2 -5 181.78 0.62 0 2 -5 178.97 0.61 0 2 5 198.09 0.75 0 -2 -6 128.80 0.66 0 -2 6 126.74 0.72 0 2 -6 104.08 0.66 0 -2 -7 73.72 0.54 0 -2 7 62.47 0.54 0 -2 7 70.29 0.58 0 2 7 63.62 0.48 0 -2 -8 20.19 0.31 0 -2 8 17.57 0.32 0 -2 8 19.35 0.33 0 -2 9 144.17 0.96 0 -2 9 157.81 1.01 0 -2 10 24.62 0.43 0 -2 10 28.39 0.47 0 -2 11 23.78 0.45 0 -2 11 25.78 0.47 0 -2 12 50.15 0.68 0 -2 12 52.69 0.71 0 -2 13 0.99 0.15 0 -2 13 0.86 0.14 0 -2 -14 51.52 0.73 0 -2 14 59.08 0.78 0 -2 14 58.20 0.84 0 2 -14 53.57 0.77 0 2 -14 57.42 0.77 0 2 14 57.47 0.78 0 -2 -15 15.21 0.41 0 -2 15 17.00 0.43 0 2 -15 15.23 0.43 0 2 -15 17.20 0.43 0 -2 -16 0.39 0.12 0 2 -16 0.33 0.11 0 2 -16 0.43 0.13 0 -2 -17 3.52 0.21 0 2 -17 3.59 0.21 0 2 -17 3.80 0.19 0 -2 -18 0.53 0.09 0 2 -18 0.40 0.09 0 2 -19 17.99 0.26 0 -3 0 0.14 0.04 0 3 0 0.08 0.04 0 -3 -1 156.18 0.98 0 -3 1 137.31 0.49 0 3 -1 161.01 0.99 0 3 1 171.78 0.90 0 -3 -2 184.80 1.11 0 -3 2 147.37 1.93 0 3 -2 184.22 1.05 0 3 2 207.59 1.29 0 -3 -3 34.45 0.30 0 -3 3 24.54 0.22 0 3 -3 30.04 0.24 0 3 -3 25.14 0.22 0 3 3 34.33 0.30 0 -3 -4 76.15 0.48 0 -3 -4 80.38 0.49 0 -3 4 64.75 0.44 0 3 -4 62.61 0.36 0 3 -4 51.77 0.33 0 3 4 69.05 0.45 0 -3 -5 47.95 0.41 0 -3 5 46.88 0.42 0 3 -5 42.22 0.32 0 3 -5 35.80 0.29 0 -3 -6 212.22 0.91 0 -3 6 204.75 0.95 0 -3 -7 3.39 0.14 0 -3 7 3.30 0.15 0 -3 7 3.05 0.14 0 -3 -8 108.39 0.74 0 -3 8 91.36 0.74 0 -3 8 101.78 0.79 0 -3 -9 90.37 1.07 0 -3 9 71.22 0.70 0 -3 9 81.20 0.76 0 -3 10 14.22 0.35 0 -3 10 16.47 0.38 0 -3 11 0.70 0.12 0 -3 11 1.00 0.14 0 -3 12 14.19 0.39 0 -3 12 13.08 0.38 0 -3 13 49.65 0.71 0 -3 13 52.79 0.74 0 -3 -14 1.93 0.20 0 -3 14 2.07 0.20 0 -3 14 2.20 0.21 0 3 -14 1.70 0.21 0 3 -14 1.94 0.20 0 -3 -15 25.52 0.50 0 -3 15 22.30 0.48 0 3 -15 26.04 0.53 0 3 -15 27.87 0.54 0 -3 -16 1.19 0.15 0 3 -16 0.84 0.12 0 3 -16 1.10 0.15 0 -3 -17 13.61 0.31 0 3 -17 13.64 0.34 0 3 -17 15.14 0.34 0 3 -18 0.60 0.09 0 3 -18 0.64 0.09 0 -4 0 589.25 3.06 0 4 0 657.52 12.45 0 -4 -1 1299.00 19.21 0 -4 1 1116.00 4.35 0 4 -1 1370.00 4.90 0 4 1 1394.00 4.87 0 -4 -2 211.45 0.80 0 -4 -2 217.16 1.04 0 -4 2 173.87 0.85 0 4 -2 213.93 0.73 0 4 2 -0.02 0.02 0 -4 -3 50.21 0.41 0 -4 3 38.39 0.31 0 4 -3 50.63 0.36 0 4 -3 39.28 0.32 0 -4 -4 14.47 0.23 0 -4 4 12.43 0.18 0 -4 4 13.78 0.22 0 4 -4 13.56 0.19 0 4 -4 12.33 0.18 0 -4 -5 9.20 0.21 0 -4 5 8.13 0.19 0 -4 -6 6.05 0.18 0 -4 6 5.26 0.17 0 -4 6 6.16 0.18 0 -4 -7 88.03 0.67 0 -4 7 78.24 0.67 0 -4 7 84.70 0.69 0 -4 -8 210.50 1.10 0 -4 8 183.94 1.10 0 -4 8 193.81 1.13 0 -4 -9 50.42 0.57 0 -4 9 44.30 0.58 0 -4 9 47.94 0.60 0 -4 10 132.75 1.06 0 -4 10 138.75 1.09 0 -4 11 5.20 0.25 0 -4 11 4.99 0.25 0 -4 12 0.41 0.11 0 -4 12 0.09 0.09 0 -4 13 13.09 0.39 0 -4 13 13.43 0.40 0 4 -13 18.80 0.64 0 -4 -14 77.76 0.87 0 -4 14 97.57 1.00 0 -4 14 113.73 1.10 0 4 -14 101.90 1.03 0 4 -14 110.85 1.08 0 -4 -15 11.12 0.33 0 4 -15 15.72 0.41 0 4 -15 17.21 0.43 0 4 -16 2.45 0.19 0 4 -16 2.75 0.21 0 4 -17 0.17 0.08 0 4 -17 0.19 0.09 0 4 -18 36.24 0.41 0 4 -18 38.54 0.42 0 -5 0 0.02 0.03 0 -5 -1 84.18 0.54 0 -5 1 73.74 0.49 0 5 -1 98.34 0.69 0 -5 -2 172.30 0.80 0 -5 2 139.89 0.67 0 5 -2 189.07 0.81 0 -5 -3 267.06 1.37 0 -5 3 198.19 0.80 0 -5 3 251.38 0.91 0 -5 -4 45.87 0.45 0 -5 4 29.72 0.32 0 -5 4 41.86 0.41 0 -5 -5 20.99 0.33 0 -5 5 16.82 0.29 0 -5 5 19.22 0.30 0 -5 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6 2 7.24 0.25 -10 6 2 8.56 0.29 -10 6 2 7.63 0.27 -10 6 -3 6.48 0.24 -10 6 -3 7.95 0.27 -10 6 -3 7.25 0.25 -10 6 3 7.24 0.24 -10 6 3 8.40 0.28 -10 6 3 7.36 0.26 -10 6 -4 9.31 0.27 -10 6 -4 11.90 0.31 -10 6 -4 11.16 0.29 -10 6 4 9.80 0.26 -10 6 4 12.43 0.31 -10 6 4 11.07 0.29 -10 6 -5 6.44 0.22 -10 6 -5 7.35 0.25 -10 6 -5 7.18 0.23 -10 6 -5 7.01 0.22 -10 6 5 6.22 0.20 -10 6 5 7.90 0.25 -10 6 5 7.36 0.24 10 -6 -5 5.43 0.19 10 -6 5 6.42 0.21 -10 -6 -6 1.41 0.12 -10 -6 6 2.10 0.14 -10 6 -6 1.98 0.14 -10 6 -6 2.09 0.16 -10 6 -6 2.29 0.15 -10 6 -6 1.90 0.15 -10 6 6 2.39 0.16 -10 6 6 2.04 0.15 10 -6 6 1.99 0.14 -10 -6 -7 1.64 0.12 -10 -6 -7 1.66 0.12 -10 -6 7 2.15 0.13 -10 6 -7 2.02 0.12 -10 6 -7 2.40 0.14 -10 6 -7 2.19 0.12 -10 6 -7 2.11 0.13 -10 6 7 2.45 0.14 -10 6 7 2.33 0.13 10 -6 7 2.20 0.13 -10 -6 -8 0.65 0.08 -10 6 -8 0.63 0.08 -10 6 -8 0.84 0.10 -10 6 -8 0.97 0.11 -10 6 -8 0.72 0.07 -10 6 8 0.88 0.10 -10 6 8 0.78 0.09 10 -6 8 0.71 0.08 -10 7 0 9.47 0.27 -10 7 0 11.44 0.30 -10 7 0 10.62 0.29 -10 7 -1 5.24 0.21 -10 7 -1 6.77 0.25 -10 7 -1 6.30 0.24 -10 7 1 5.88 0.22 -10 7 1 7.23 0.25 -10 7 1 6.65 0.24 -10 7 -2 2.11 0.16 -10 7 -2 2.41 0.18 -10 7 -2 2.46 0.17 -10 7 2 2.25 0.16 -10 7 2 2.58 0.17 -10 7 2 2.37 0.17 -10 7 -3 2.77 0.16 -10 7 -3 3.30 0.19 -10 7 -3 3.25 0.18 -10 7 3 2.95 0.16 -10 7 3 3.49 0.18 -10 7 3 3.05 0.17 -10 7 -4 9.84 0.25 -10 7 -4 11.41 0.27 -10 7 -4 11.00 0.27 -10 7 4 9.66 0.24 -10 7 4 12.40 0.28 -10 7 4 11.45 0.26 -10 7 -5 7.91 0.22 -10 7 -5 9.66 0.24 -10 7 -5 8.60 0.23 -10 7 -5 8.87 0.21 -10 7 5 8.27 0.21 -10 7 5 10.42 0.25 -10 7 5 9.86 0.23 10 -7 -5 7.67 0.19 10 -7 5 9.10 0.21 -10 -7 -6 0.46 0.07 -10 -7 6 0.48 0.07 -10 7 -6 0.57 0.08 -10 7 -6 0.56 0.08 -10 7 -6 0.66 0.09 -10 7 -6 0.51 0.07 -10 7 6 0.52 0.07 -10 7 6 0.84 0.09 -10 7 6 0.63 0.08 10 -7 -6 0.56 0.07 10 -7 6 0.54 0.07 -10 7 -7 4.36 0.15 -10 7 -7 4.21 0.14 -10 7 7 4.54 0.18 -10 8 0 4.76 0.18 -10 8 0 6.40 0.21 -10 8 0 5.57 0.19 -10 8 -1 0.26 0.08 -10 8 -1 0.42 0.08 -10 8 -1 0.32 0.08 -10 8 1 0.26 0.07 -10 8 1 0.28 0.08 -10 8 1 0.22 0.08 -10 8 -2 0.27 0.08 -10 8 -2 0.46 0.09 -10 8 -2 0.47 0.09 -10 8 2 0.43 0.08 -10 8 2 0.42 0.08 -10 8 2 0.34 0.08 -10 8 -3 13.28 0.26 -10 8 -3 15.43 0.28 -10 8 -3 14.75 0.28 -10 8 3 12.40 0.25 -10 8 3 15.47 0.27 -10 8 3 14.32 0.26 -10 8 -4 0.04 0.06 -10 8 -4 0.00 0.06 -10 8 -4 0.02 0.06 -10 8 4 0.02 0.05 -10 8 4 0.00 0.07 -10 8 4 0.01 0.05 10 -8 -4 0.00 0.05 -10 8 -5 7.62 0.17 -10 8 -5 8.40 0.19 -10 8 -5 8.14 0.19 -10 8 5 6.00 0.16 -10 8 5 7.45 0.24 10 -8 -5 5.78 0.15 -10 8 -6 5.62 0.21 -10 9 0 2.49 0.12 -10 9 0 2.46 0.12 -10 9 -1 7.83 0.19 -10 9 -1 7.89 0.18 -10 9 1 7.78 0.19 -10 9 1 8.05 0.18 -10 9 -2 0.53 0.07 -10 9 -2 0.38 0.06 -10 9 2 0.50 0.07 10 -9 -2 0.45 0.06 -10 9 -3 1.86 0.10 -10 9 3 1.58 0.09 10 -9 -3 1.27 0.09 -11 0 -5 0.15 0.07 -11 0 5 0.16 0.08 -11 0 -6 0.17 0.07 -11 0 6 0.23 0.07 -11 0 -7 9.17 0.20 -11 0 -7 10.55 0.23 -11 0 7 11.33 0.22 -11 1 2 28.79 0.44 -11 1 2 27.26 0.41 -11 1 -3 6.38 0.21 -11 1 3 7.74 0.24 -11 1 3 7.72 0.23 -11 1 -4 19.71 0.34 -11 1 4 25.80 0.38 -11 1 4 23.52 0.37 -11 1 -5 21.11 0.34 -11 1 5 26.70 0.37 -11 1 5 24.74 0.37 -11 1 -6 3.53 0.16 -11 1 6 4.55 0.16 -11 1 6 4.33 0.17 -11 -1 -7 6.95 0.17 -11 1 -7 8.50 0.20 -11 1 -7 9.04 0.21 -11 1 7 9.04 0.28 -11 1 7 10.54 0.22 -11 1 -8 1.76 0.12 -11 2 0 7.35 0.25 -11 2 0 7.00 0.23 -11 2 -1 7.23 0.32 -11 2 -1 8.37 0.25 -11 2 1 8.82 0.26 -11 2 1 8.45 0.25 -11 2 -2 3.78 0.18 -11 2 -2 4.68 0.20 -11 2 2 4.44 0.21 -11 2 2 4.55 0.20 -11 2 -3 2.30 0.15 -11 2 -3 2.79 0.16 -11 2 3 3.31 0.19 -11 2 3 3.11 0.18 -11 2 -4 0.87 0.10 -11 2 -4 1.13 0.14 -11 2 4 1.27 0.14 -11 2 4 1.18 0.13 -11 2 -5 0.03 0.07 -11 2 -5 0.08 0.07 -11 2 5 0.08 0.07 -11 2 5 0.10 0.08 -11 2 -6 1.58 0.12 -11 2 6 2.19 0.13 -11 2 6 2.06 0.14 -11 2 -7 3.51 0.14 -11 2 7 4.12 0.14 -11 2 7 4.34 0.15 -11 2 -8 2.26 0.13 -11 3 0 0.10 0.08 -11 3 0 0.02 0.08 -11 3 0 0.09 0.08 -11 3 -1 2.33 0.16 -11 3 -1 2.87 0.18 -11 3 -1 2.72 0.17 -11 3 1 3.08 0.19 -11 3 1 2.84 0.18 -11 3 -2 4.49 0.19 -11 3 -2 5.46 0.22 -11 3 -2 5.25 0.19 -11 3 2 6.12 0.22 -11 3 2 5.77 0.22 -11 3 -3 3.20 0.17 -11 3 -3 3.66 0.19 -11 3 -3 3.60 0.17 -11 3 3 3.83 0.19 -11 3 3 3.96 0.19 -11 3 -4 8.07 0.23 -11 3 -4 9.58 0.25 -11 3 4 10.44 0.26 -11 3 4 9.71 0.25 -11 3 -5 1.77 0.13 -11 3 -5 1.82 0.13 -11 3 5 2.15 0.14 -11 3 5 2.05 0.14 -11 3 -6 0.77 0.09 -11 3 -6 0.87 0.11 -11 3 6 0.91 0.11 -11 3 6 0.84 0.10 -11 3 -7 1.60 0.10 -11 3 7 1.93 0.11 -11 3 7 2.00 0.11 -11 4 0 0.30 0.08 -11 4 0 0.44 0.09 -11 4 0 0.48 0.10 -11 4 -1 7.97 0.23 -11 4 -1 9.28 0.26 -11 4 -1 8.42 0.24 -11 4 1 7.67 0.22 -11 4 1 9.76 0.27 -11 4 1 8.71 0.25 -11 4 -2 5.67 0.20 -11 4 -2 7.03 0.23 -11 4 -2 6.60 0.21 -11 4 2 6.76 0.23 -11 4 2 6.71 0.22 -11 4 -3 2.30 0.15 -11 4 -3 2.59 0.16 -11 4 -3 2.63 0.15 -11 4 3 3.00 0.17 -11 4 3 2.51 0.16 -11 4 -4 0.20 0.07 -11 4 -4 0.10 0.07 -11 4 -4 0.21 0.07 -11 4 4 0.17 0.07 -11 4 4 0.17 0.08 -11 4 -5 12.18 0.25 -11 4 -5 14.10 0.26 -11 4 5 15.07 0.28 -11 4 5 13.48 0.26 -11 4 -6 0.89 0.09 -11 4 -6 0.86 0.10 -11 4 6 1.06 0.10 -11 4 6 1.05 0.10 -11 4 -7 9.59 0.26 -11 4 7 9.47 0.25 -11 5 0 3.61 0.16 -11 5 0 4.49 0.19 -11 5 0 4.27 0.18 -11 5 -1 35.38 0.42 -11 5 -1 41.00 0.47 -11 5 -1 37.39 0.45 -11 5 1 32.00 0.39 -11 5 1 42.42 0.48 -11 5 1 40.14 0.46 -11 5 -2 0.31 0.08 -11 5 -2 0.20 0.07 -11 5 -2 0.24 0.07 -11 5 2 0.31 0.07 -11 5 2 0.22 0.08 -11 5 2 0.36 0.09 -11 5 -3 0.51 0.08 -11 5 -3 0.66 0.09 -11 5 -3 0.63 0.09 -11 5 3 0.60 0.09 -11 5 3 0.63 0.09 -11 5 -4 1.67 0.11 -11 5 -4 1.99 0.13 -11 5 -4 1.80 0.11 -11 5 4 1.88 0.13 -11 5 4 1.90 0.12 -11 5 -5 0.38 0.06 -11 5 -5 0.36 0.07 -11 5 5 0.49 0.08 -11 5 5 0.51 0.07 -11 5 -6 3.06 0.16 -11 5 6 3.52 0.15 -11 6 0 6.21 0.18 -11 6 0 7.77 0.21 -11 6 0 6.89 0.19 -11 6 -1 0.58 0.08 -11 6 -1 0.67 0.08 -11 6 -1 0.68 0.08 -11 6 1 0.58 0.08 -11 6 1 0.88 0.11 -11 6 1 0.77 0.09 -11 6 -2 4.93 0.16 -11 6 -2 6.15 0.19 -11 6 -2 5.75 0.17 -11 6 2 4.63 0.15 -11 6 2 6.09 0.18 -11 6 2 5.76 0.18 -11 6 -3 2.82 0.13 -11 6 -3 3.23 0.14 -11 6 -3 2.73 0.13 -11 6 3 3.36 0.14 -11 6 3 3.32 0.14 -11 6 -4 7.14 0.17 -11 6 -4 9.15 0.19 -11 6 -4 7.55 0.23 -11 6 4 9.50 0.20 -11 6 4 8.28 0.18 -11 7 0 1.97 0.10 -11 7 0 2.17 0.11 -11 7 0 2.09 0.11 -11 7 -1 2.54 0.11 -11 7 -1 2.77 0.14 -11 7 -1 2.99 0.12 -11 7 1 2.66 0.15 -11 7 1 2.61 0.12 -11 7 -2 8.34 0.21 -11 7 -2 8.80 0.26 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 30088 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, 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 C1 C 0.4639(2) 0.76508(16) 0.93834(14) 0.0402(4) Uani 1 1 d . . H1 H 0.5384 0.7918 0.9707 0.048 Uiso 1 1 calc R U C2 C 0.3695(2) 0.82994(17) 0.90084(16) 0.0465(5) Uani 1 1 d . . H2 H 0.3795 0.9007 0.9079 0.056 Uiso 1 1 calc R U C3 C 0.2606(2) 0.79192(17) 0.85294(15) 0.0446(5) Uani 1 1 d . . H3 H 0.1963 0.8364 0.8269 0.054 Uiso 1 1 calc R U C4 C 0.2462(2) 0.68886(18) 0.84345(14) 0.0425(5) Uani 1 1 d . . H4 H 0.1718 0.6624 0.8108 0.051 Uiso 1 1 calc R U C5 C 0.3403(2) 0.62379(15) 0.88152(13) 0.0391(4) Uani 1 1 d . . H5 H 0.3293 0.5531 0.8750 0.047 Uiso 1 1 calc R U C6 C 0.4507(2) 0.66128(15) 0.92914(12) 0.0351(4) Uani 1 1 d . . C7 C 0.5513(2) 0.59195(16) 0.97362(13) 0.0404(5) Uani 1 1 d . . H7A H 0.6349 0.6308 0.9881 0.048 Uiso 1 1 calc R U H7B H 0.5103 0.5686 1.0288 0.048 Uiso 1 1 calc R U C8 C 0.6566(3) 0.55543(16) 0.77548(14) 0.0438(5) Uani 1 1 d . . H8 H 0.5631 0.5690 0.7629 0.053 Uiso 1 1 calc R U C9 C 0.7567(3) 0.57208(18) 0.71319(16) 0.0543(6) Uani 1 1 d . . H9 H 0.7315 0.5978 0.6580 0.065 Uiso 1 1 calc R U C10 C 0.8927(3) 0.55148(19) 0.73090(18) 0.0560(6) Uani 1 1 d . . H10 H 0.9607 0.5631 0.6880 0.067 Uiso 1 1 calc R U C11 C 0.9296(3) 0.5141(2) 0.81076(19) 0.0536(6) Uani 1 1 d . . H11 H 1.0229 0.4986 0.8225 0.064 Uiso 1 1 calc R U C12 C 0.8307(2) 0.49877(17) 0.87441(15) 0.0438(5) Uani 1 1 d . . H12 H 0.8566 0.4747 0.9301 0.053 Uiso 1 1 calc R U C13 C 0.6939(2) 0.51884(14) 0.85613(13) 0.0362(4) Uani 1 1 d . . C14 C 0.54085(18) 0.41152(15) 0.94336(12) 0.0333(4) Uani 1 1 d . . C15 C 0.58060(18) 0.32384(14) 0.88457(11) 0.0309(4) Uani 1 1 d . . H15 H 0.6714 0.3382 0.8570 0.037 Uiso 1 1 calc R U C16 C 0.58937(18) 0.22515(15) 0.93523(12) 0.0323(4) Uani 1 1 d . . H16 H 0.4949 0.1989 0.9464 0.039 Uiso 1 1 calc R U C17 C 0.67222(19) 0.14651(14) 0.88502(12) 0.0335(4) Uani 1 1 d . . H17A H 0.6378 0.1445 0.8246 0.040 Uiso 1 1 calc R U H17B H 0.7690 0.1689 0.8829 0.040 Uiso 1 1 calc R U C18 C 0.6683(2) 0.04031(15) 0.92158(13) 0.0378(4) Uani 1 1 d . . H18A H 0.7149 0.0390 0.9786 0.045 Uiso 1 1 calc R U H18B H 0.5719 0.0193 0.9302 0.045 Uiso 1 1 calc R U C19 C 0.73856(19) -0.03237(14) 0.86048(13) 0.0354(4) Uani 1 1 d . . C20 C 0.8275(3) -0.19624(17) 0.84393(18) 0.0524(6) Uani 1 1 d . . H20A H 0.7666 -0.2128 0.7954 0.079 Uiso 1 1 calc R U H20B H 0.8446 -0.2570 0.8785 0.079 Uiso 1 1 calc R U H20C H 0.9146 -0.1704 0.8214 0.079 Uiso 1 1 calc R U C21 C 0.4699(2) 0.31536(17) 0.81344(13) 0.0386(4) Uani 1 1 d . . H21A H 0.3799 0.3058 0.8405 0.058 Uiso 1 1 calc R U H21B H 0.4905 0.2577 0.7759 0.058 Uiso 1 1 calc R U H21C H 0.4690 0.3772 0.7787 0.058 Uiso 1 1 calc R U N1 N 0.59136(17) 0.50323(13) 0.92221(10) 0.0352(4) Uani 1 1 d . . N2 N 0.66240(19) 0.24214(13) 1.02048(10) 0.0385(4) Uani 1 1 d . . O1 O 0.46120(15) 0.39876(12) 1.00394(10) 0.0428(4) Uani 1 1 d . . O2 O 0.75459(16) 0.30404(13) 1.02269(10) 0.0457(4) Uani 1 1 d . . O3 O 0.6282(2) 0.18991(17) 1.08220(11) 0.0628(5) Uani 1 1 d . . O4 O 0.76356(19) -0.12033(12) 0.89786(11) 0.0476(4) Uani 1 1 d . . O5 O 0.7667(3) -0.01396(14) 0.78683(12) 0.0662(6) 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 C1 0.0394(10) 0.0372(10) 0.0441(10) -0.0072(8) 0.0042(8) -0.0047(8) C2 0.0483(12) 0.0341(10) 0.0569(12) -0.0043(9) 0.0083(10) 0.0015(8) C3 0.0400(10) 0.0454(11) 0.0485(11) 0.0014(9) 0.0057(9) 0.0090(9) C4 0.0353(10) 0.0493(11) 0.0428(10) -0.0044(9) 0.0011(8) 0.0003(9) C5 0.0411(10) 0.0345(9) 0.0417(10) -0.0049(8) 0.0010(8) -0.0029(8) C6 0.0356(9) 0.0367(9) 0.0331(9) -0.0046(7) 0.0046(7) 0.0000(7) C7 0.0478(11) 0.0381(9) 0.0352(9) -0.0084(8) -0.0057(8) 0.0029(9) C8 0.0539(12) 0.0364(9) 0.0411(10) 0.0037(8) 0.0003(9) 0.0056(9) C9 0.0798(17) 0.0390(10) 0.0442(11) 0.0072(9) 0.0105(12) -0.0006(11) C10 0.0655(15) 0.0420(11) 0.0605(14) 0.0003(10) 0.0235(12) -0.0133(11) C11 0.0436(11) 0.0504(13) 0.0668(14) -0.0004(11) 0.0073(11) -0.0123(10) C12 0.0395(10) 0.0450(11) 0.0469(11) 0.0027(9) -0.0014(8) -0.0079(9) C13 0.0419(10) 0.0286(7) 0.0383(10) -0.0004(7) 0.0031(8) -0.0028(7) C14 0.0289(8) 0.0382(9) 0.0327(8) 0.0003(7) -0.0029(7) 0.0036(7) C15 0.0272(8) 0.0340(9) 0.0317(8) 0.0001(7) -0.0006(6) -0.0013(7) C16 0.0272(8) 0.0370(9) 0.0328(8) 0.0000(7) -0.0008(7) -0.0026(7) C17 0.0324(8) 0.0335(9) 0.0346(9) 0.0015(7) -0.0014(7) -0.0006(7) C18 0.0365(9) 0.0347(9) 0.0422(10) 0.0017(8) 0.0007(7) -0.0039(8) C19 0.0323(8) 0.0315(8) 0.0422(10) 0.0002(7) -0.0061(7) -0.0034(7) C20 0.0597(13) 0.0350(10) 0.0625(14) -0.0056(10) -0.0142(11) 0.0072(10) C21 0.0370(10) 0.0431(10) 0.0357(9) 0.0026(8) -0.0059(7) 0.0000(8) N1 0.0379(8) 0.0346(8) 0.0331(8) -0.0022(6) 0.0006(6) 0.0014(7) N2 0.0411(9) 0.0415(9) 0.0330(8) -0.0009(7) -0.0024(7) 0.0076(7) O1 0.0406(7) 0.0461(8) 0.0417(8) -0.0002(6) 0.0115(6) 0.0027(6) O2 0.0417(8) 0.0486(8) 0.0468(8) -0.0085(7) -0.0134(6) 0.0027(7) O3 0.0823(13) 0.0716(12) 0.0345(8) 0.0148(8) -0.0001(8) -0.0013(11) O4 0.0596(9) 0.0320(7) 0.0513(9) 0.0026(6) -0.0033(7) 0.0033(7) O5 0.1041(15) 0.0453(9) 0.0491(10) 0.0050(8) 0.0161(10) 0.0216(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 C2 C1 C6 120.7(2) C2 C1 H1 119.6 C6 C1 H1 119.6 C1 C2 C3 120.3(2) C1 C2 H2 119.9 C3 C2 H2 119.9 C4 C3 C2 119.5(2) C4 C3 H3 120.2 C2 C3 H3 120.2 C3 C4 C5 120.2(2) C3 C4 H4 119.9 C5 C4 H4 119.9 C4 C5 C6 120.7(2) C4 C5 H5 119.7 C6 C5 H5 119.7 C1 C6 C5 118.6(2) C1 C6 C7 119.82(18) C5 C6 C7 121.55(19) N1 C7 C6 114.54(16) N1 C7 H7A 108.6 C6 C7 H7A 108.6 N1 C7 H7B 108.6 C6 C7 H7B 108.6 H7A C7 H7B 107.6 C13 C8 C9 119.6(2) C13 C8 H8 120.2 C9 C8 H8 120.2 C10 C9 C8 120.5(2) C10 C9 H9 119.8 C8 C9 H9 119.8 C11 C10 C9 120.0(2) C11 C10 H10 120.0 C9 C10 H10 120.0 C10 C11 C12 120.2(2) C10 C11 H11 119.9 C12 C11 H11 119.9 C13 C12 C11 119.6(2) C13 C12 H12 120.2 C11 C12 H12 120.2 C8 C13 C12 120.1(2) C8 C13 N1 120.19(19) C12 C13 N1 119.66(18) O1 C14 N1 122.56(18) O1 C14 C15 120.55(18) N1 C14 C15 116.79(16) C14 C15 C16 111.38(15) C14 C15 C21 107.48(15) C16 C15 C21 109.89(15) C14 C15 H15 109.4 C16 C15 H15 109.4 C21 C15 H15 109.4 N2 C16 C15 110.07(15) N2 C16 C17 107.03(15) C15 C16 C17 110.83(15) N2 C16 H16 109.6 C15 C16 H16 109.6 C17 C16 H16 109.6 C18 C17 C16 115.59(16) C18 C17 H17A 108.4 C16 C17 H17A 108.4 C18 C17 H17B 108.4 C16 C17 H17B 108.4 H17A C17 H17B 107.4 C19 C18 C17 110.45(16) C19 C18 H18A 109.6 C17 C18 H18A 109.6 C19 C18 H18B 109.6 C17 C18 H18B 109.6 H18A C18 H18B 108.1 O5 C19 O4 123.5(2) O5 C19 C18 124.50(19) O4 C19 C18 111.98(17) O4 C20 H20A 109.5 O4 C20 H20B 109.5 H20A C20 H20B 109.5 O4 C20 H20C 109.5 H20A C20 H20C 109.5 H20B C20 H20C 109.5 C15 C21 H21A 109.5 C15 C21 H21B 109.5 H21A C21 H21B 109.5 C15 C21 H21C 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 C14 N1 C13 123.49(16) C14 N1 C7 119.55(16) C13 N1 C7 116.70(16) O2 N2 O3 124.15(19) O2 N2 C16 118.19(16) O3 N2 C16 117.60(18) C19 O4 C20 116.27(18) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.386(3) C1 C6 1.391(3) C1 H1 0.9500 C2 C3 1.389(4) C2 H2 0.9500 C3 C4 1.383(3) C3 H3 0.9500 C4 C5 1.390(3) C4 H4 0.9500 C5 C6 1.395(3) C5 H5 0.9500 C6 C7 1.510(3) C7 N1 1.472(2) C7 H7A 0.9900 C7 H7B 0.9900 C8 C13 1.384(3) C8 C9 1.387(3) C8 H8 0.9500 C9 C10 1.381(4) C9 H9 0.9500 C10 C11 1.376(4) C10 H10 0.9500 C11 C12 1.391(3) C11 H11 0.9500 C12 C13 1.389(3) C12 H12 0.9500 C13 N1 1.443(3) C14 O1 1.227(2) C14 N1 1.353(3) C14 C15 1.525(3) C15 C16 1.527(3) C15 C21 1.543(2) C15 H15 1.0000 C16 N2 1.512(2) C16 C17 1.530(3) C16 H16 1.0000 C17 C18 1.518(3) C17 H17A 0.9900 C17 H17B 0.9900 C18 C19 1.512(3) C18 H18A 0.9900 C18 H18B 0.9900 C19 O5 1.194(3) C19 O4 1.325(2) C20 O4 1.447(3) C20 H20A 0.9800 C20 H20B 0.9800 C20 H20C 0.9800 C21 H21A 0.9800 C21 H21B 0.9800 C21 H21C 0.9800 N2 O2 1.218(3) N2 O3 1.224(2)