#------------------------------------------------------------------------------ #$Date: 2020-02-04 22:09:40 +0200 (Tue, 04 Feb 2020) $ #$Revision: 247617 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125677.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_7125677 loop_ _publ_author_name 'Livshits-Kritsman, Yulia' 'Tumanskii, Boris' 'M\'enard, Gabriel' 'Dobrovetsky, Roman' _publ_section_title ; Isolable cyclic (alkyl)(amino)carbene-phosphonyl radical adducts. ; _journal_issue 9 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 1341 _journal_page_last 1344 _journal_paper_doi 10.1039/c9cc09244g _journal_volume 56 _journal_year 2020 _chemical_formula_moiety '2(C23 H38 N O3 P), C6 H6' _chemical_formula_sum 'C52 H82 N2 O6 P2' _chemical_formula_weight 893.13 _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_creation_method SHELXL-2018/1 _audit_update_record ; 2019-11-21 deposited with the CCDC. 2019-12-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 95.0850(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 18.3588(5) _cell_length_b 15.6255(3) _cell_length_c 17.7751(5) _cell_measurement_reflns_used 46348 _cell_measurement_temperature 110(2) _cell_measurement_theta_max 28.326 _cell_measurement_theta_min 1.714 _cell_volume 5079.0(2) _computing_cell_refinement 'Saint, Bruker-AXS' _computing_data_collection 'Apex2, Bruker-AXS' _computing_data_reduction 'Saint, Bruker-AXS' _computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 110(2) _diffrn_detector_area_resol_mean 1.75 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'ApexDuo, Bruker-AXS' _diffrn_measurement_method '0.5 deg. \f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_unetI/netI 0.0566 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 46348 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.326 _diffrn_reflns_theta_min 1.714 _diffrn_source 'ImuS micro-focus' _exptl_absorpt_coefficient_mu 0.134 _exptl_absorpt_correction_T_max 0.995 _exptl_absorpt_correction_T_min 0.993 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Sadabs, Bruker-AXS' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.168 _exptl_crystal_description needle _exptl_crystal_F_000 1944 _exptl_crystal_size_max 0.292 _exptl_crystal_size_mid 0.043 _exptl_crystal_size_min 0.035 _refine_diff_density_max 0.361 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.054 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 579 _refine_ls_number_reflns 12634 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.009 _refine_ls_R_factor_all 0.0780 _refine_ls_R_factor_gt 0.0457 _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^)+(0.0464P)^2^+1.6797P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0999 _refine_ls_wR_factor_ref 0.1133 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8894 _reflns_number_total 12634 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc09244g2.cif _cod_data_source_block rom62a _cod_depositor_comments 'Adding full bibliography for 7125674--7125677.cif.' _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7125677 _shelx_shelxl_version_number 2018/1 _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 0.962 _shelx_estimated_absorpt_t_max 0.995 _shelx_res_file ; TITL mo_rom62a_0ma_a.res in P2(1)/c rom62a.res created by SHELXL-2018/1 at 12:32:37 on 31-Mar-2019 REM Old TITL mo_rom62a_0ma in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.141, Rweak 0.005, Alpha 0.035, Orientation as input REM Formula found by SHELXT: C52 N2 O6 P2 CELL 0.71073 18.3588 15.6255 17.7751 90.000 95.085 90.000 ZERR 4.000 0.0005 0.0003 0.0005 0.000 0.001 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O P UNIT 208 328 8 24 8 TEMP -163.000 SIZE 0.035 0.043 0.292 ACTA L.S. 10 BOND $H LIST 6 FMAP 2 PLAN 20 OMIT 1 0 0 WGHT 0.046400 1.679700 FVAR 0.22883 P1 5 0.543906 0.362957 0.661445 11.00000 0.01410 0.01005 = 0.01708 -0.00245 0.00380 -0.00040 P2 5 -0.031184 0.385553 0.339519 11.00000 0.01881 0.01090 = 0.01584 0.00326 0.00626 0.00333 O3 4 0.530421 0.294761 0.715360 11.00000 0.02958 0.01116 = 0.02855 0.00148 0.01255 -0.00081 O4 4 0.511742 0.361798 0.582185 11.00000 0.01861 0.02072 = 0.02115 -0.00769 -0.00020 0.00021 O5 4 0.630024 0.384047 0.666232 11.00000 0.01473 0.01819 = 0.01593 -0.00284 0.00369 0.00071 C6 1 0.673149 0.369412 0.603014 11.00000 0.01730 0.02269 = 0.01650 -0.00187 0.00430 0.00218 AFIX 13 H6 2 0.647973 0.395696 0.556433 11.00000 -1.20000 AFIX 0 C7 1 0.682031 0.274524 0.590886 11.00000 0.02939 0.02423 = 0.03753 -0.00840 0.01386 0.00314 AFIX 137 H7A 2 0.633795 0.248199 0.580017 11.00000 -1.50000 H7B 2 0.706665 0.248743 0.636543 11.00000 -1.50000 H7C 2 0.711400 0.265014 0.548222 11.00000 -1.50000 AFIX 0 C8 1 0.745543 0.413330 0.622116 11.00000 0.02067 0.03636 = 0.03266 -0.00529 0.00969 -0.00453 AFIX 137 H8A 2 0.776421 0.405935 0.580352 11.00000 -1.50000 H8B 2 0.769916 0.388123 0.668164 11.00000 -1.50000 H8C 2 0.737352 0.474482 0.630249 11.00000 -1.50000 AFIX 0 C9 1 0.518172 0.467867 0.701920 11.00000 0.00903 0.01167 = 0.01465 0.00012 -0.00059 -0.00170 C10 1 0.513058 0.549701 0.656197 11.00000 0.01976 0.01107 = 0.01366 0.00116 0.00212 0.00123 C11 1 0.576180 0.562363 0.606539 11.00000 0.02911 0.01500 = 0.02200 0.00282 0.00949 -0.00032 AFIX 137 H11A 2 0.575431 0.516450 0.568919 11.00000 -1.50000 H11B 2 0.622724 0.560985 0.638102 11.00000 -1.50000 H11C 2 0.570802 0.617763 0.580800 11.00000 -1.50000 AFIX 0 C12 1 0.440766 0.546966 0.604566 11.00000 0.02555 0.02128 = 0.01759 0.00278 -0.00210 0.00561 AFIX 137 H12A 2 0.435573 0.599844 0.574928 11.00000 -1.50000 H12B 2 0.399515 0.541506 0.635657 11.00000 -1.50000 H12C 2 0.441378 0.497815 0.570382 11.00000 -1.50000 AFIX 0 C13 1 0.513156 0.618950 0.717378 11.00000 0.02526 0.01086 = 0.01715 -0.00061 0.00524 -0.00002 AFIX 23 H13A 2 0.562945 0.642762 0.728270 11.00000 -1.20000 H13B 2 0.479642 0.666111 0.700360 11.00000 -1.20000 AFIX 0 C14 1 0.487638 0.576410 0.788116 11.00000 0.02260 0.00945 = 0.01590 -0.00249 0.00319 0.00088 C15 1 0.407128 0.591354 0.798573 11.00000 0.02714 0.01553 = 0.03064 -0.00131 0.01017 0.00413 AFIX 137 H15A 2 0.377103 0.571245 0.753717 11.00000 -1.50000 H15B 2 0.398592 0.652616 0.805688 11.00000 -1.50000 H15C 2 0.393918 0.559812 0.843038 11.00000 -1.50000 AFIX 0 C16 1 0.532998 0.604454 0.859595 11.00000 0.03781 0.01576 = 0.01897 -0.00408 0.00003 -0.00227 AFIX 137 H16A 2 0.584878 0.593899 0.854099 11.00000 -1.50000 H16B 2 0.518014 0.571881 0.902745 11.00000 -1.50000 H16C 2 0.525337 0.665656 0.868009 11.00000 -1.50000 AFIX 0 N17 3 0.501917 0.480955 0.770446 11.00000 0.01274 0.01011 = 0.01319 0.00057 0.00016 0.00009 C18 1 0.494149 0.415585 0.828483 11.00000 0.01866 0.01093 = 0.01167 0.00027 0.00389 -0.00011 C19 1 0.554990 0.395279 0.878757 11.00000 0.01850 0.01601 = 0.01563 0.00139 -0.00032 -0.00068 C20 1 0.544278 0.337805 0.936546 11.00000 0.02345 0.02253 = 0.01540 0.00509 -0.00311 -0.00051 AFIX 43 H20 2 0.584498 0.323662 0.971688 11.00000 -1.20000 AFIX 0 C21 1 0.477226 0.300663 0.944537 11.00000 0.03061 0.01975 = 0.01580 0.00493 0.00487 -0.00444 AFIX 43 H21 2 0.471077 0.262708 0.985243 11.00000 -1.20000 AFIX 0 C22 1 0.419081 0.319624 0.892264 11.00000 0.01982 0.01753 = 0.01842 -0.00077 0.00807 -0.00476 AFIX 43 H22 2 0.373183 0.292981 0.896910 11.00000 -1.20000 AFIX 0 C23 1 0.425863 0.376669 0.832984 11.00000 0.01694 0.01274 = 0.01452 -0.00300 0.00479 0.00051 C24 1 0.632925 0.425474 0.870571 11.00000 0.01709 0.02771 = 0.02323 0.00907 -0.00318 -0.00343 AFIX 13 H24 2 0.631619 0.468486 0.828815 11.00000 -1.20000 AFIX 0 C25 1 0.679600 0.349262 0.849467 11.00000 0.01806 0.03878 = 0.03650 0.01357 0.00164 0.00449 AFIX 137 H25A 2 0.656699 0.321965 0.803681 11.00000 -1.50000 H25B 2 0.683344 0.307757 0.890964 11.00000 -1.50000 H25C 2 0.728596 0.369344 0.840266 11.00000 -1.50000 AFIX 0 C26 1 0.666992 0.467800 0.943465 11.00000 0.02867 0.04191 = 0.02862 0.00994 -0.01310 -0.01394 AFIX 137 H26A 2 0.713563 0.494555 0.933904 11.00000 -1.50000 H26B 2 0.675542 0.424318 0.982994 11.00000 -1.50000 H26C 2 0.633587 0.511508 0.959962 11.00000 -1.50000 AFIX 0 C27 1 0.360177 0.387116 0.774840 11.00000 0.01504 0.01868 = 0.02170 0.00166 0.00319 -0.00259 AFIX 13 H27 2 0.372240 0.432011 0.737821 11.00000 -1.20000 AFIX 0 C28 1 0.345243 0.302911 0.731725 11.00000 0.02196 0.02747 = 0.02196 -0.00098 -0.00007 -0.00722 AFIX 137 H28A 2 0.305257 0.311304 0.692105 11.00000 -1.50000 H28B 2 0.331520 0.258548 0.766794 11.00000 -1.50000 H28C 2 0.389417 0.285124 0.708751 11.00000 -1.50000 AFIX 0 C29 1 0.291467 0.415355 0.811004 11.00000 0.01562 0.03189 = 0.03868 0.00155 0.00600 0.00159 AFIX 137 H29A 2 0.252777 0.429253 0.771321 11.00000 -1.50000 H29B 2 0.302656 0.466006 0.842437 11.00000 -1.50000 H29C 2 0.274975 0.368888 0.842407 11.00000 -1.50000 AFIX 0 O30 4 -0.045254 0.319273 0.281039 11.00000 0.02691 0.01079 = 0.02205 0.00055 0.00848 0.00046 O31 4 0.031670 0.380595 0.397004 11.00000 0.02811 0.02395 = 0.02077 0.00560 -0.00052 0.00833 O32 4 -0.105266 0.408479 0.376765 11.00000 0.02312 0.01223 = 0.03075 0.00008 0.01485 -0.00020 C33 1 -0.163991 0.346700 0.376843 11.00000 0.01692 0.01649 = 0.02387 0.00394 0.00517 -0.00101 AFIX 13 H33 2 -0.166852 0.313122 0.328779 11.00000 -1.20000 AFIX 0 C34 1 -0.148032 0.286878 0.442936 11.00000 0.02506 0.02167 = 0.02520 0.00497 0.00651 -0.00341 AFIX 137 H34A 2 -0.187055 0.244103 0.443115 11.00000 -1.50000 H34B 2 -0.145476 0.319662 0.490098 11.00000 -1.50000 H34C 2 -0.101206 0.258034 0.438503 11.00000 -1.50000 AFIX 0 C35 1 -0.234219 0.396584 0.381055 11.00000 0.02272 0.02909 = 0.06254 0.00724 0.00809 0.00631 AFIX 137 H35A 2 -0.242062 0.434069 0.336877 11.00000 -1.50000 H35B 2 -0.230725 0.431292 0.427155 11.00000 -1.50000 H35C 2 -0.275323 0.356677 0.381859 11.00000 -1.50000 AFIX 0 C36 1 -0.016330 0.492068 0.297015 11.00000 0.01061 0.01220 = 0.01294 -0.00061 -0.00089 0.00185 C37 1 -0.025261 0.576771 0.337214 11.00000 0.02288 0.01150 = 0.01359 -0.00112 0.00276 -0.00004 C38 1 0.001162 0.574556 0.421163 11.00000 0.03926 0.01947 = 0.01367 -0.00154 -0.00013 -0.00183 AFIX 137 H38A 2 0.051254 0.552350 0.427478 11.00000 -1.50000 H38B 2 -0.030963 0.537338 0.447837 11.00000 -1.50000 H38C 2 0.000142 0.632560 0.442015 11.00000 -1.50000 AFIX 0 C39 1 -0.107144 0.601292 0.328319 11.00000 0.02596 0.01448 = 0.02513 -0.00025 0.00784 0.00331 AFIX 137 H39A 2 -0.124396 0.602880 0.274560 11.00000 -1.50000 H39B 2 -0.113605 0.657783 0.350735 11.00000 -1.50000 H39C 2 -0.135342 0.558757 0.354022 11.00000 -1.50000 AFIX 0 C40 1 0.020942 0.637617 0.293063 11.00000 0.02615 0.01232 = 0.01542 -0.00037 0.00018 -0.00315 AFIX 23 H40A 2 -0.002615 0.694571 0.288071 11.00000 -1.20000 H40B 2 0.070225 0.644598 0.319795 11.00000 -1.20000 AFIX 0 C41 1 0.026702 0.598243 0.215185 11.00000 0.01982 0.00806 = 0.01422 0.00127 0.00176 -0.00283 C42 1 0.103289 0.606725 0.189825 11.00000 0.02197 0.01618 = 0.02738 0.00262 0.00399 -0.00522 AFIX 137 H42A 2 0.105841 0.576555 0.141795 11.00000 -1.50000 H42B 2 0.138699 0.581710 0.228125 11.00000 -1.50000 H42C 2 0.114710 0.667378 0.183204 11.00000 -1.50000 AFIX 0 C43 1 -0.027932 0.633353 0.153215 11.00000 0.02475 0.01286 = 0.01661 0.00285 -0.00005 -0.00220 AFIX 137 H43A 2 -0.024038 0.600970 0.106526 11.00000 -1.50000 H43B 2 -0.017271 0.693821 0.144498 11.00000 -1.50000 H43C 2 -0.077604 0.627837 0.168788 11.00000 -1.50000 AFIX 0 N44 3 0.009093 0.503610 0.232065 11.00000 0.01435 0.00943 = 0.01218 -0.00037 0.00007 -0.00117 C45 1 0.018974 0.437887 0.175125 11.00000 0.01857 0.00870 = 0.01052 0.00108 0.00558 -0.00160 C46 1 -0.040025 0.419875 0.121468 11.00000 0.01873 0.01188 = 0.01451 0.00113 0.00275 -0.00140 C47 1 -0.027141 0.363326 0.063813 11.00000 0.02456 0.01652 = 0.01463 -0.00201 -0.00110 -0.00175 AFIX 43 H47 2 -0.065648 0.350973 0.026096 11.00000 -1.20000 AFIX 0 C48 1 0.039958 0.324546 0.059699 11.00000 0.03070 0.01479 = 0.01476 -0.00262 0.00661 0.00152 AFIX 43 H48 2 0.047723 0.287368 0.018883 11.00000 -1.20000 AFIX 0 C49 1 0.095767 0.340233 0.115438 11.00000 0.02241 0.01453 = 0.01771 0.00277 0.00695 0.00292 AFIX 43 H49 2 0.141259 0.311751 0.113342 11.00000 -1.20000 AFIX 0 C50 1 0.087008 0.396765 0.174635 11.00000 0.01961 0.01116 = 0.01337 0.00373 0.00541 -0.00130 C51 1 -0.117952 0.452015 0.125630 11.00000 0.01666 0.01549 = 0.01864 -0.00354 -0.00105 0.00012 AFIX 13 H51 2 -0.117710 0.495278 0.167107 11.00000 -1.20000 AFIX 0 C52 1 -0.167390 0.377425 0.144618 11.00000 0.01999 0.02380 = 0.02938 -0.00040 0.00039 -0.00328 AFIX 137 H52A 2 -0.170055 0.335616 0.103369 11.00000 -1.50000 H52B 2 -0.216535 0.399046 0.151173 11.00000 -1.50000 H52C 2 -0.147182 0.349931 0.191450 11.00000 -1.50000 AFIX 0 C53 1 -0.148845 0.494411 0.051882 11.00000 0.02347 0.02222 = 0.02581 0.00043 -0.00506 0.00280 AFIX 137 H53A 2 -0.154472 0.451326 0.011722 11.00000 -1.50000 H53B 2 -0.115246 0.539222 0.037834 11.00000 -1.50000 H53C 2 -0.196577 0.519805 0.058914 11.00000 -1.50000 AFIX 0 C54 1 0.149075 0.404216 0.237051 11.00000 0.01467 0.01825 = 0.02011 -0.00161 0.00298 0.00046 AFIX 13 H54 2 0.136013 0.449285 0.273468 11.00000 -1.20000 AFIX 0 C55 1 0.221743 0.429198 0.206042 11.00000 0.01786 0.02796 = 0.03496 -0.00183 0.00494 -0.00218 AFIX 137 H55A 2 0.237422 0.383175 0.173674 11.00000 -1.50000 H55B 2 0.259093 0.438316 0.248178 11.00000 -1.50000 H55C 2 0.215009 0.482020 0.176519 11.00000 -1.50000 AFIX 0 C56 1 0.158724 0.318754 0.279441 11.00000 0.02113 0.02458 = 0.02006 0.00331 0.00083 0.00688 AFIX 137 H56A 2 0.172091 0.274058 0.244515 11.00000 -1.50000 H56B 2 0.112770 0.303236 0.300105 11.00000 -1.50000 H56C 2 0.197467 0.324436 0.320751 11.00000 -1.50000 AFIX 0 C57 1 0.183690 0.303463 0.478449 11.00000 0.01991 0.06138 = 0.02118 0.00944 0.00283 -0.01096 AFIX 43 H57 2 0.134144 0.296276 0.459134 11.00000 -1.20000 AFIX 0 C58 1 0.212140 0.384073 0.489252 11.00000 0.02508 0.03839 = 0.04288 0.01554 0.01076 0.00781 AFIX 43 H58 2 0.182074 0.432709 0.478029 11.00000 -1.20000 AFIX 0 C59 1 0.283553 0.394664 0.516089 11.00000 0.02754 0.02621 = 0.04146 -0.00297 0.01251 -0.00550 AFIX 43 H59 2 0.303060 0.450815 0.522022 11.00000 -1.20000 AFIX 0 C60 1 0.327839 0.325227 0.534729 11.00000 0.01880 0.04453 = 0.02012 -0.00350 0.00226 -0.00219 AFIX 43 H60 2 0.377329 0.333218 0.553919 11.00000 -1.20000 AFIX 0 C61 1 0.299170 0.243938 0.525081 11.00000 0.03494 0.03374 = 0.02733 0.00637 0.01529 0.01052 AFIX 43 H61 2 0.328774 0.195509 0.538584 11.00000 -1.20000 AFIX 0 C62 1 0.227060 0.232684 0.495645 11.00000 0.04110 0.03125 = 0.02919 -0.00459 0.01833 -0.01421 AFIX 43 H62 2 0.207776 0.176708 0.487427 11.00000 -1.20000 AFIX 0 HKLF 4 REM mo_rom62a_0ma_a.res in P2(1)/c REM R1 = 0.0457 for 8894 Fo > 4sig(Fo) and 0.0780 for all 12634 data REM 579 parameters refined using 0 restraints END WGHT 0.0464 1.6797 REM Highest difference peak 0.361, deepest hole -0.367, 1-sigma level 0.054 Q1 1 0.5086 0.5844 0.6836 11.00000 0.05 0.36 Q2 1 -0.0269 0.4415 0.3105 11.00000 0.05 0.34 Q3 1 0.4978 0.4460 0.7997 11.00000 0.05 0.33 Q4 1 -0.0162 0.5753 0.3745 11.00000 0.05 0.32 Q5 1 0.1158 0.4026 0.2107 11.00000 0.05 0.32 Q6 1 0.5123 0.5110 0.6736 11.00000 0.05 0.31 Q7 1 0.2089 0.3420 0.4729 11.00000 0.05 0.31 Q8 1 -0.0799 0.4351 0.1263 11.00000 0.05 0.30 Q9 1 0.0241 0.6121 0.2568 11.00000 0.05 0.30 Q10 1 -0.0282 0.5362 0.3223 11.00000 0.05 0.29 Q11 1 0.3918 0.3875 0.8056 11.00000 0.05 0.29 Q12 1 0.2085 0.2208 0.4598 11.00000 0.05 0.29 Q13 1 0.1473 0.3639 0.2593 11.00000 0.05 0.29 Q14 1 -0.0192 0.4154 0.1610 11.00000 0.05 0.28 Q15 1 -0.2005 0.3613 0.3846 11.00000 0.05 0.28 Q16 1 0.0483 0.4086 0.1849 11.00000 0.05 0.28 Q17 1 0.5279 0.4224 0.6776 11.00000 0.05 0.28 Q18 1 -0.0617 0.5857 0.3403 11.00000 0.05 0.28 Q19 1 -0.1405 0.4130 0.1363 11.00000 0.05 0.27 Q20 1 0.5499 0.3562 0.8981 11.00000 0.05 0.27 ; _shelx_res_checksum 46665 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 P1 P 0.54391(2) 0.36296(2) 0.66145(2) 0.01360(9) Uani 1 1 d . . P2 P -0.03118(2) 0.38555(2) 0.33952(2) 0.01490(10) Uani 1 1 d . . O3 O 0.53042(7) 0.29476(7) 0.71536(7) 0.0225(3) Uani 1 1 d . . O4 O 0.51174(6) 0.36180(7) 0.58219(7) 0.0203(3) Uani 1 1 d . . O5 O 0.63002(6) 0.38405(7) 0.66623(6) 0.0161(2) Uani 1 1 d . . C6 C 0.67315(9) 0.36941(10) 0.60301(9) 0.0187(3) Uani 1 1 d . . H6 H 0.647973 0.395696 0.556433 0.022 Uiso 1 1 calc R U C7 C 0.68203(10) 0.27452(11) 0.59089(12) 0.0297(4) Uani 1 1 d . . H7A H 0.633795 0.248199 0.580017 0.045 Uiso 1 1 calc R U H7B H 0.706665 0.248743 0.636543 0.045 Uiso 1 1 calc R U H7C H 0.711400 0.265014 0.548222 0.045 Uiso 1 1 calc R U C8 C 0.74554(10) 0.41333(12) 0.62212(11) 0.0295(4) Uani 1 1 d . . H8A H 0.776421 0.405935 0.580352 0.044 Uiso 1 1 calc R U H8B H 0.769916 0.388123 0.668164 0.044 Uiso 1 1 calc R U H8C H 0.737352 0.474482 0.630249 0.044 Uiso 1 1 calc R U C9 C 0.51817(8) 0.46787(9) 0.70192(9) 0.0119(3) Uani 1 1 d . . C10 C 0.51306(9) 0.54970(9) 0.65620(9) 0.0148(3) Uani 1 1 d . . C11 C 0.57618(10) 0.56236(10) 0.60654(10) 0.0216(4) Uani 1 1 d . . H11A H 0.575431 0.516450 0.568919 0.032 Uiso 1 1 calc R U H11B H 0.622724 0.560985 0.638102 0.032 Uiso 1 1 calc R U H11C H 0.570802 0.617763 0.580800 0.032 Uiso 1 1 calc R U C12 C 0.44077(9) 0.54697(11) 0.60457(10) 0.0217(4) Uani 1 1 d . . H12A H 0.435573 0.599844 0.574928 0.033 Uiso 1 1 calc R U H12B H 0.399515 0.541506 0.635657 0.033 Uiso 1 1 calc R U H12C H 0.441378 0.497815 0.570382 0.033 Uiso 1 1 calc R U C13 C 0.51316(9) 0.61895(10) 0.71738(9) 0.0176(3) Uani 1 1 d . . H13A H 0.562945 0.642762 0.728270 0.021 Uiso 1 1 calc R U H13B H 0.479642 0.666111 0.700360 0.021 Uiso 1 1 calc R U C14 C 0.48764(9) 0.57641(9) 0.78812(9) 0.0159(3) Uani 1 1 d . . C15 C 0.40713(10) 0.59135(11) 0.79857(11) 0.0240(4) Uani 1 1 d . . H15A H 0.377103 0.571245 0.753717 0.036 Uiso 1 1 calc R U H15B H 0.398592 0.652616 0.805688 0.036 Uiso 1 1 calc R U H15C H 0.393918 0.559812 0.843038 0.036 Uiso 1 1 calc R U C16 C 0.53300(10) 0.60445(11) 0.85960(10) 0.0243(4) Uani 1 1 d . . H16A H 0.584878 0.593899 0.854099 0.036 Uiso 1 1 calc R U H16B H 0.518014 0.571881 0.902745 0.036 Uiso 1 1 calc R U H16C H 0.525337 0.665656 0.868009 0.036 Uiso 1 1 calc R U N17 N 0.50192(7) 0.48095(8) 0.77045(7) 0.0121(3) Uani 1 1 d . . C18 C 0.49415(9) 0.41559(9) 0.82848(9) 0.0136(3) Uani 1 1 d . . C19 C 0.55499(9) 0.39528(10) 0.87876(9) 0.0168(3) Uani 1 1 d . . C20 C 0.54428(9) 0.33781(11) 0.93655(9) 0.0207(4) Uani 1 1 d . . H20 H 0.584498 0.323662 0.971688 0.025 Uiso 1 1 calc R U C21 C 0.47723(10) 0.30066(11) 0.94454(10) 0.0219(4) Uani 1 1 d . . H21 H 0.471077 0.262708 0.985243 0.026 Uiso 1 1 calc R U C22 C 0.41908(9) 0.31962(10) 0.89226(9) 0.0182(3) Uani 1 1 d . . H22 H 0.373183 0.292981 0.896910 0.022 Uiso 1 1 calc R U C23 C 0.42586(9) 0.37667(9) 0.83298(9) 0.0145(3) Uani 1 1 d . . C24 C 0.63293(9) 0.42547(11) 0.87057(10) 0.0230(4) Uani 1 1 d . . H24 H 0.631619 0.468486 0.828815 0.028 Uiso 1 1 calc R U C25 C 0.67960(10) 0.34926(13) 0.84947(12) 0.0312(4) Uani 1 1 d . . H25A H 0.656699 0.321965 0.803681 0.047 Uiso 1 1 calc R U H25B H 0.683344 0.307757 0.890964 0.047 Uiso 1 1 calc R U H25C H 0.728596 0.369344 0.840266 0.047 Uiso 1 1 calc R U C26 C 0.66699(11) 0.46780(13) 0.94347(11) 0.0340(5) Uani 1 1 d . . H26A H 0.713563 0.494555 0.933904 0.051 Uiso 1 1 calc R U H26B H 0.675542 0.424318 0.982994 0.051 Uiso 1 1 calc R U H26C H 0.633587 0.511508 0.959962 0.051 Uiso 1 1 calc R U C27 C 0.36018(9) 0.38712(10) 0.77484(10) 0.0184(3) Uani 1 1 d . . H27 H 0.372240 0.432011 0.737821 0.022 Uiso 1 1 calc R U C28 C 0.34524(10) 0.30291(11) 0.73172(10) 0.0239(4) Uani 1 1 d . . H28A H 0.305257 0.311304 0.692105 0.036 Uiso 1 1 calc R U H28B H 0.331520 0.258548 0.766794 0.036 Uiso 1 1 calc R U H28C H 0.389417 0.285124 0.708751 0.036 Uiso 1 1 calc R U C29 C 0.29147(9) 0.41536(12) 0.81100(11) 0.0285(4) Uani 1 1 d . . H29A H 0.252777 0.429253 0.771321 0.043 Uiso 1 1 calc R U H29B H 0.302656 0.466006 0.842437 0.043 Uiso 1 1 calc R U H29C H 0.274975 0.368888 0.842407 0.043 Uiso 1 1 calc R U O30 O -0.04525(6) 0.31927(7) 0.28104(7) 0.0195(3) Uani 1 1 d . . O31 O 0.03167(7) 0.38060(7) 0.39700(7) 0.0244(3) Uani 1 1 d . . O32 O -0.10527(6) 0.40848(7) 0.37676(7) 0.0213(3) Uani 1 1 d . . C33 C -0.16399(9) 0.34670(10) 0.37684(10) 0.0189(4) Uani 1 1 d . . H33 H -0.166852 0.313122 0.328779 0.023 Uiso 1 1 calc R U C34 C -0.14803(10) 0.28688(11) 0.44294(10) 0.0237(4) Uani 1 1 d . . H34A H -0.187055 0.244103 0.443115 0.036 Uiso 1 1 calc R U H34B H -0.145476 0.319662 0.490098 0.036 Uiso 1 1 calc R U H34C H -0.101206 0.258034 0.438503 0.036 Uiso 1 1 calc R U C35 C -0.23422(10) 0.39658(13) 0.38106(14) 0.0379(5) Uani 1 1 d . . H35A H -0.242062 0.434069 0.336877 0.057 Uiso 1 1 calc R U H35B H -0.230725 0.431292 0.427155 0.057 Uiso 1 1 calc R U H35C H -0.275323 0.356677 0.381859 0.057 Uiso 1 1 calc R U C36 C -0.01633(8) 0.49207(9) 0.29701(9) 0.0120(3) Uani 1 1 d . . C37 C -0.02526(9) 0.57677(9) 0.33721(9) 0.0159(3) Uani 1 1 d . . C38 C 0.00116(11) 0.57456(11) 0.42116(9) 0.0243(4) Uani 1 1 d . . H38A H 0.051254 0.552350 0.427478 0.036 Uiso 1 1 calc R U H38B H -0.030963 0.537338 0.447837 0.036 Uiso 1 1 calc R U H38C H 0.000142 0.632560 0.442015 0.036 Uiso 1 1 calc R U C39 C -0.10714(9) 0.60129(10) 0.32832(10) 0.0215(4) Uani 1 1 d . . H39A H -0.124396 0.602880 0.274560 0.032 Uiso 1 1 calc R U H39B H -0.113605 0.657783 0.350735 0.032 Uiso 1 1 calc R U H39C H -0.135342 0.558757 0.354022 0.032 Uiso 1 1 calc R U C40 C 0.02094(9) 0.63762(10) 0.29306(9) 0.0181(3) Uani 1 1 d . . H40A H -0.002615 0.694571 0.288071 0.022 Uiso 1 1 calc R U H40B H 0.070225 0.644598 0.319795 0.022 Uiso 1 1 calc R U C41 C 0.02670(9) 0.59824(9) 0.21519(9) 0.0140(3) Uani 1 1 d . . C42 C 0.10329(9) 0.60672(10) 0.18983(10) 0.0217(4) Uani 1 1 d . . H42A H 0.105841 0.576555 0.141795 0.033 Uiso 1 1 calc R U H42B H 0.138699 0.581710 0.228125 0.033 Uiso 1 1 calc R U H42C H 0.114710 0.667378 0.183204 0.033 Uiso 1 1 calc R U C43 C -0.02793(9) 0.63335(10) 0.15322(9) 0.0182(3) Uani 1 1 d . . H43A H -0.024038 0.600970 0.106526 0.027 Uiso 1 1 calc R U H43B H -0.017271 0.693821 0.144498 0.027 Uiso 1 1 calc R U H43C H -0.077604 0.627837 0.168788 0.027 Uiso 1 1 calc R U N44 N 0.00909(7) 0.50361(8) 0.23207(7) 0.0121(3) Uani 1 1 d . . C45 C 0.01897(9) 0.43789(9) 0.17512(9) 0.0123(3) Uani 1 1 d . . C46 C -0.04002(9) 0.41988(9) 0.12147(9) 0.0150(3) Uani 1 1 d . . C47 C -0.02714(9) 0.36333(10) 0.06381(9) 0.0187(4) Uani 1 1 d . . H47 H -0.065648 0.350973 0.026096 0.022 Uiso 1 1 calc R U C48 C 0.03996(10) 0.32455(10) 0.05970(10) 0.0198(4) Uani 1 1 d . . H48 H 0.047723 0.287368 0.018883 0.024 Uiso 1 1 calc R U C49 C 0.09577(9) 0.34023(10) 0.11544(9) 0.0179(3) Uani 1 1 d . . H49 H 0.141259 0.311751 0.113342 0.021 Uiso 1 1 calc R U C50 C 0.08701(9) 0.39676(9) 0.17463(9) 0.0145(3) Uani 1 1 d . . C51 C -0.11795(9) 0.45201(10) 0.12563(9) 0.0171(3) Uani 1 1 d . . H51 H -0.117710 0.495278 0.167107 0.021 Uiso 1 1 calc R U C52 C -0.16739(9) 0.37742(11) 0.14462(11) 0.0245(4) Uani 1 1 d . . H52A H -0.170055 0.335616 0.103369 0.037 Uiso 1 1 calc R U H52B H -0.216535 0.399046 0.151173 0.037 Uiso 1 1 calc R U H52C H -0.147182 0.349931 0.191450 0.037 Uiso 1 1 calc R U C53 C -0.14884(10) 0.49441(11) 0.05188(10) 0.0243(4) Uani 1 1 d . . H53A H -0.154472 0.451326 0.011722 0.036 Uiso 1 1 calc R U H53B H -0.115246 0.539222 0.037834 0.036 Uiso 1 1 calc R U H53C H -0.196577 0.519805 0.058914 0.036 Uiso 1 1 calc R U C54 C 0.14908(9) 0.40422(10) 0.23705(9) 0.0176(3) Uani 1 1 d . . H54 H 0.136013 0.449285 0.273468 0.021 Uiso 1 1 calc R U C55 C 0.22174(9) 0.42920(12) 0.20604(11) 0.0268(4) Uani 1 1 d . . H55A H 0.237422 0.383175 0.173674 0.040 Uiso 1 1 calc R U H55B H 0.259093 0.438316 0.248178 0.040 Uiso 1 1 calc R U H55C H 0.215009 0.482020 0.176519 0.040 Uiso 1 1 calc R U C56 C 0.15872(10) 0.31875(11) 0.27944(10) 0.0220(4) Uani 1 1 d . . H56A H 0.172091 0.274058 0.244515 0.033 Uiso 1 1 calc R U H56B H 0.112770 0.303236 0.300105 0.033 Uiso 1 1 calc R U H56C H 0.197467 0.324436 0.320751 0.033 Uiso 1 1 calc R U C57 C 0.18369(10) 0.30346(14) 0.47845(11) 0.0341(5) Uani 1 1 d . . H57 H 0.134144 0.296276 0.459134 0.041 Uiso 1 1 calc R U C58 C 0.21214(11) 0.38407(13) 0.48925(12) 0.0350(5) Uani 1 1 d . . H58 H 0.182074 0.432709 0.478029 0.042 Uiso 1 1 calc R U C59 C 0.28355(10) 0.39466(12) 0.51609(12) 0.0312(4) Uani 1 1 d . . H59 H 0.303060 0.450815 0.522022 0.037 Uiso 1 1 calc R U C60 C 0.32784(10) 0.32523(13) 0.53473(10) 0.0278(4) Uani 1 1 d . . H60 H 0.377329 0.333218 0.553919 0.033 Uiso 1 1 calc R U C61 C 0.29917(11) 0.24394(13) 0.52508(11) 0.0313(5) Uani 1 1 d . . H61 H 0.328774 0.195509 0.538584 0.038 Uiso 1 1 calc R U C62 C 0.22706(11) 0.23268(13) 0.49565(11) 0.0329(5) Uani 1 1 d . . H62 H 0.207776 0.176708 0.487427 0.040 Uiso 1 1 calc R U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0141(2) 0.01005(18) 0.0171(2) -0.00245(16) 0.00380(16) -0.00040(15) P2 0.0188(2) 0.01090(19) 0.0158(2) 0.00326(16) 0.00626(17) 0.00333(16) O3 0.0296(7) 0.0112(5) 0.0286(7) 0.0015(5) 0.0126(6) -0.0008(5) O4 0.0186(6) 0.0207(6) 0.0211(6) -0.0077(5) -0.0002(5) 0.0002(5) O5 0.0147(6) 0.0182(5) 0.0159(6) -0.0028(5) 0.0037(5) 0.0007(4) C6 0.0173(8) 0.0227(8) 0.0165(8) -0.0019(7) 0.0043(7) 0.0022(7) C7 0.0294(10) 0.0242(9) 0.0375(12) -0.0084(8) 0.0139(9) 0.0031(8) C8 0.0207(9) 0.0364(11) 0.0327(11) -0.0053(9) 0.0097(8) -0.0045(8) C9 0.0090(7) 0.0117(7) 0.0147(8) 0.0001(6) -0.0006(6) -0.0017(6) C10 0.0198(8) 0.0111(7) 0.0137(8) 0.0012(6) 0.0021(6) 0.0012(6) C11 0.0291(10) 0.0150(8) 0.0220(9) 0.0028(7) 0.0095(8) -0.0003(7) C12 0.0256(9) 0.0213(8) 0.0176(9) 0.0028(7) -0.0021(7) 0.0056(7) C13 0.0253(9) 0.0109(7) 0.0172(8) -0.0006(6) 0.0052(7) 0.0000(6) C14 0.0226(9) 0.0095(7) 0.0159(8) -0.0025(6) 0.0032(7) 0.0009(6) C15 0.0271(10) 0.0155(8) 0.0306(10) -0.0013(7) 0.0102(8) 0.0041(7) C16 0.0378(11) 0.0158(8) 0.0190(9) -0.0041(7) 0.0000(8) -0.0023(7) N17 0.0127(6) 0.0101(6) 0.0132(7) 0.0006(5) 0.0002(5) 0.0001(5) C18 0.0187(8) 0.0109(7) 0.0117(8) 0.0003(6) 0.0039(6) -0.0001(6) C19 0.0185(8) 0.0160(8) 0.0156(8) 0.0014(6) -0.0003(7) -0.0007(6) C20 0.0234(9) 0.0225(8) 0.0154(9) 0.0051(7) -0.0031(7) -0.0005(7) C21 0.0306(10) 0.0197(8) 0.0158(9) 0.0049(7) 0.0049(7) -0.0044(7) C22 0.0198(8) 0.0175(8) 0.0184(9) -0.0008(7) 0.0081(7) -0.0048(7) C23 0.0169(8) 0.0127(7) 0.0145(8) -0.0030(6) 0.0048(6) 0.0005(6) C24 0.0171(9) 0.0277(9) 0.0232(10) 0.0091(8) -0.0032(7) -0.0034(7) C25 0.0181(9) 0.0388(11) 0.0365(12) 0.0136(9) 0.0016(8) 0.0045(8) C26 0.0287(11) 0.0419(11) 0.0286(11) 0.0099(9) -0.0131(9) -0.0139(9) C27 0.0150(8) 0.0187(8) 0.0217(9) 0.0017(7) 0.0032(7) -0.0026(6) C28 0.0220(9) 0.0275(9) 0.0220(10) -0.0010(7) -0.0001(7) -0.0072(7) C29 0.0156(9) 0.0319(10) 0.0387(12) 0.0016(9) 0.0060(8) 0.0016(7) O30 0.0269(7) 0.0108(5) 0.0221(7) 0.0005(5) 0.0085(5) 0.0005(5) O31 0.0281(7) 0.0240(6) 0.0208(7) 0.0056(5) -0.0005(5) 0.0083(5) O32 0.0231(6) 0.0122(5) 0.0308(7) 0.0001(5) 0.0149(5) -0.0002(5) C33 0.0169(8) 0.0165(8) 0.0239(9) 0.0039(7) 0.0052(7) -0.0010(6) C34 0.0251(9) 0.0217(8) 0.0252(10) 0.0050(7) 0.0065(8) -0.0034(7) C35 0.0227(10) 0.0291(10) 0.0625(15) 0.0072(10) 0.0081(10) 0.0063(8) C36 0.0106(7) 0.0122(7) 0.0129(8) -0.0006(6) -0.0009(6) 0.0019(6) C37 0.0229(9) 0.0115(7) 0.0136(8) -0.0011(6) 0.0028(7) 0.0000(6) C38 0.0393(11) 0.0195(8) 0.0137(9) -0.0015(7) -0.0001(8) -0.0018(8) C39 0.0260(9) 0.0145(8) 0.0251(10) -0.0002(7) 0.0078(7) 0.0033(7) C40 0.0262(9) 0.0123(7) 0.0154(8) -0.0004(6) 0.0002(7) -0.0032(7) C41 0.0198(8) 0.0081(7) 0.0142(8) 0.0013(6) 0.0018(6) -0.0028(6) C42 0.0220(9) 0.0162(8) 0.0274(10) 0.0026(7) 0.0040(7) -0.0052(7) C43 0.0247(9) 0.0129(7) 0.0166(8) 0.0029(6) 0.0000(7) -0.0022(7) N44 0.0144(7) 0.0094(6) 0.0122(7) -0.0004(5) 0.0001(5) -0.0012(5) C45 0.0186(8) 0.0087(7) 0.0105(8) 0.0011(6) 0.0056(6) -0.0016(6) C46 0.0187(8) 0.0119(7) 0.0145(8) 0.0011(6) 0.0028(6) -0.0014(6) C47 0.0246(9) 0.0165(8) 0.0146(8) -0.0020(7) -0.0011(7) -0.0018(7) C48 0.0307(10) 0.0148(8) 0.0148(8) -0.0026(7) 0.0066(7) 0.0015(7) C49 0.0224(9) 0.0145(8) 0.0177(9) 0.0028(7) 0.0070(7) 0.0029(6) C50 0.0196(8) 0.0112(7) 0.0134(8) 0.0037(6) 0.0054(6) -0.0013(6) C51 0.0167(8) 0.0155(8) 0.0186(9) -0.0035(7) -0.0011(7) 0.0001(6) C52 0.0200(9) 0.0238(9) 0.0294(10) -0.0004(8) 0.0004(7) -0.0033(7) C53 0.0235(9) 0.0222(9) 0.0258(10) 0.0004(8) -0.0051(8) 0.0028(7) C54 0.0147(8) 0.0182(8) 0.0201(9) -0.0016(7) 0.0030(7) 0.0005(6) C55 0.0179(9) 0.0280(9) 0.0350(11) -0.0018(8) 0.0049(8) -0.0022(7) C56 0.0211(9) 0.0246(9) 0.0201(9) 0.0033(7) 0.0008(7) 0.0069(7) C57 0.0199(10) 0.0614(14) 0.0212(10) 0.0094(10) 0.0028(8) -0.0110(9) C58 0.0251(10) 0.0384(11) 0.0429(13) 0.0155(10) 0.0108(9) 0.0078(9) C59 0.0275(10) 0.0262(10) 0.0415(12) -0.0030(9) 0.0125(9) -0.0055(8) C60 0.0188(9) 0.0445(11) 0.0201(10) -0.0035(8) 0.0023(7) -0.0022(8) C61 0.0349(11) 0.0337(10) 0.0273(11) 0.0064(9) 0.0153(9) 0.0105(9) C62 0.0411(12) 0.0312(10) 0.0292(11) -0.0046(9) 0.0183(9) -0.0142(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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 O3 P1 O4 122.45(7) O3 P1 O5 109.61(7) O4 P1 O5 111.12(6) O3 P1 C9 108.81(7) O4 P1 C9 106.53(7) O5 P1 C9 94.63(6) O30 P2 O31 121.97(7) O30 P2 O32 110.23(7) O31 P2 O32 111.45(7) O30 P2 C36 111.44(7) O31 P2 C36 101.24(7) O32 P2 C36 97.36(6) C6 O5 P1 121.89(10) O5 C6 C8 106.55(13) O5 C6 C7 109.83(14) C8 C6 C7 112.03(15) O5 C6 H6 109.5 C8 C6 H6 109.5 C7 C6 H6 109.5 C6 C7 H7A 109.5 C6 C7 H7B 109.5 H7A C7 H7B 109.5 C6 C7 H7C 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 C6 C8 H8A 109.5 C6 C8 H8B 109.5 H8A C8 H8B 109.5 C6 C8 H8C 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 N17 C9 C10 111.28(13) N17 C9 P1 126.00(11) C10 C9 P1 122.71(11) C9 C10 C11 113.88(13) C9 C10 C13 102.66(13) C11 C10 C13 111.36(13) C9 C10 C12 107.73(13) C11 C10 C12 108.38(14) C13 C10 C12 112.79(13) C10 C11 H11A 109.5 C10 C11 H11B 109.5 H11A C11 H11B 109.5 C10 C11 H11C 109.5 H11A C11 H11C 109.5 H11B C11 H11C 109.5 C10 C12 H12A 109.5 C10 C12 H12B 109.5 H12A C12 H12B 109.5 C10 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 C14 C13 C10 107.13(12) C14 C13 H13A 110.3 C10 C13 H13A 110.3 C14 C13 H13B 110.3 C10 C13 H13B 110.3 H13A C13 H13B 108.5 C16 C14 C15 108.61(14) C16 C14 C13 112.09(14) C15 C14 C13 113.83(14) C16 C14 N17 110.88(13) C15 C14 N17 110.80(12) C13 C14 N17 100.46(12) C14 C15 H15A 109.5 C14 C15 H15B 109.5 H15A C15 H15B 109.5 C14 C15 H15C 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 C14 C16 H16A 109.5 C14 C16 H16B 109.5 H16A C16 H16B 109.5 C14 C16 H16C 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 C9 N17 C18 126.57(13) C9 N17 C14 113.53(12) C18 N17 C14 119.88(12) C23 C18 C19 122.06(14) C23 C18 N17 119.02(13) C19 C18 N17 118.91(14) C20 C19 C18 117.35(15) C20 C19 C24 117.72(14) C18 C19 C24 124.71(14) C21 C20 C19 122.23(15) C21 C20 H20 118.9 C19 C20 H20 118.9 C20 C21 C22 118.89(15) C20 C21 H21 120.6 C22 C21 H21 120.6 C21 C22 C23 121.95(15) C21 C22 H22 119.0 C23 C22 H22 119.0 C22 C23 C18 117.43(14) C22 C23 C27 117.53(14) C18 C23 C27 124.89(14) C19 C24 C25 109.41(14) C19 C24 C26 111.56(15) C25 C24 C26 110.24(15) C19 C24 H24 108.5 C25 C24 H24 108.5 C26 C24 H24 108.5 C24 C25 H25A 109.5 C24 C25 H25B 109.5 H25A C25 H25B 109.5 C24 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 C24 C26 H26A 109.5 C24 C26 H26B 109.5 H26A C26 H26B 109.5 C24 C26 H26C 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 C23 C27 C29 112.19(14) C23 C27 C28 109.99(13) C29 C27 C28 109.84(14) C23 C27 H27 108.2 C29 C27 H27 108.2 C28 C27 H27 108.2 C27 C28 H28A 109.5 C27 C28 H28B 109.5 H28A C28 H28B 109.5 C27 C28 H28C 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 C27 C29 H29A 109.5 C27 C29 H29B 109.5 H29A C29 H29B 109.5 C27 C29 H29C 109.5 H29A C29 H29C 109.5 H29B C29 H29C 109.5 C33 O32 P2 120.67(10) O32 C33 C34 108.70(14) O32 C33 C35 107.12(13) C34 C33 C35 112.81(15) O32 C33 H33 109.4 C34 C33 H33 109.4 C35 C33 H33 109.4 C33 C34 H34A 109.5 C33 C34 H34B 109.5 H34A C34 H34B 109.5 C33 C34 H34C 109.5 H34A C34 H34C 109.5 H34B C34 H34C 109.5 C33 C35 H35A 109.5 C33 C35 H35B 109.5 H35A C35 H35B 109.5 C33 C35 H35C 109.5 H35A C35 H35C 109.5 H35B C35 H35C 109.5 N44 C36 C37 111.11(13) N44 C36 P2 124.37(11) C37 C36 P2 124.27(11) C36 C37 C38 113.66(13) C36 C37 C40 102.21(13) C38 C37 C40 111.79(13) C36 C37 C39 108.19(13) C38 C37 C39 109.10(14) C40 C37 C39 111.75(13) C37 C38 H38A 109.5 C37 C38 H38B 109.5 H38A C38 H38B 109.5 C37 C38 H38C 109.5 H38A C38 H38C 109.5 H38B C38 H38C 109.5 C37 C39 H39A 109.5 C37 C39 H39B 109.5 H39A C39 H39B 109.5 C37 C39 H39C 109.5 H39A C39 H39C 109.5 H39B C39 H39C 109.5 C41 C40 C37 107.44(12) C41 C40 H40A 110.2 C37 C40 H40A 110.2 C41 C40 H40B 110.2 C37 C40 H40B 110.2 H40A C40 H40B 108.5 C42 C41 C43 108.72(13) C42 C41 C40 111.96(13) C43 C41 C40 114.58(13) C42 C41 N44 110.81(12) C43 C41 N44 110.38(12) C40 C41 N44 100.17(12) C41 C42 H42A 109.5 C41 C42 H42B 109.5 H42A C42 H42B 109.5 C41 C42 H42C 109.5 H42A C42 H42C 109.5 H42B C42 H42C 109.5 C41 C43 H43A 109.5 C41 C43 H43B 109.5 H43A C43 H43B 109.5 C41 C43 H43C 109.5 H43A C43 H43C 109.5 H43B C43 H43C 109.5 C36 N44 C45 126.49(12) C36 N44 C41 113.79(12) C45 N44 C41 119.66(12) C50 C45 C46 122.39(14) C50 C45 N44 119.31(13) C46 C45 N44 118.28(13) C47 C46 C45 117.14(15) C47 C46 C51 117.86(14) C45 C46 C51 124.81(14) C48 C47 C46 121.96(15) C48 C47 H47 119.0 C46 C47 H47 119.0 C47 C48 C49 119.49(15) C47 C48 H48 120.3 C49 C48 H48 120.3 C48 C49 C50 121.70(15) C48 C49 H49 119.1 C50 C49 H49 119.1 C49 C50 C45 117.16(15) C49 C50 C54 118.00(14) C45 C50 C54 124.65(14) C46 C51 C53 112.26(14) C46 C51 C52 109.68(13) C53 C51 C52 109.61(14) C46 C51 H51 108.4 C53 C51 H51 108.4 C52 C51 H51 108.4 C51 C52 H52A 109.5 C51 C52 H52B 109.5 H52A C52 H52B 109.5 C51 C52 H52C 109.5 H52A C52 H52C 109.5 H52B C52 H52C 109.5 C51 C53 H53A 109.5 C51 C53 H53B 109.5 H53A C53 H53B 109.5 C51 C53 H53C 109.5 H53A C53 H53C 109.5 H53B C53 H53C 109.5 C50 C54 C56 109.71(13) C50 C54 C55 112.03(14) C56 C54 C55 109.30(14) C50 C54 H54 108.6 C56 C54 H54 108.6 C55 C54 H54 108.6 C54 C55 H55A 109.5 C54 C55 H55B 109.5 H55A C55 H55B 109.5 C54 C55 H55C 109.5 H55A C55 H55C 109.5 H55B C55 H55C 109.5 C54 C56 H56A 109.5 C54 C56 H56B 109.5 H56A C56 H56B 109.5 C54 C56 H56C 109.5 H56A C56 H56C 109.5 H56B C56 H56C 109.5 C58 C57 C62 119.99(18) C58 C57 H57 120.0 C62 C57 H57 120.0 C59 C58 C57 120.18(18) C59 C58 H58 119.9 C57 C58 H58 119.9 C58 C59 C60 121.09(18) C58 C59 H59 119.5 C60 C59 H59 119.5 C59 C60 C61 118.97(18) C59 C60 H60 120.5 C61 C60 H60 120.5 C60 C61 C62 120.20(18) C60 C61 H61 119.9 C62 C61 H61 119.9 C57 C62 C61 119.53(18) C57 C62 H62 120.2 C61 C62 H62 120.2 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance P1 O3 1.4688(12) P1 O4 1.4786(12) P1 O5 1.6099(11) P1 C9 1.8677(15) P2 O30 1.4739(12) P2 O31 1.4740(12) P2 O32 1.6050(12) P2 C36 1.8579(15) O5 C6 1.4490(19) C6 C8 1.508(2) C6 C7 1.509(2) C6 H6 1.0000 C7 H7A 0.9800 C7 H7B 0.9800 C7 H7C 0.9800 C8 H8A 0.9800 C8 H8B 0.9800 C8 H8C 0.9800 C9 N17 1.296(2) C9 C10 1.514(2) C10 C11 1.531(2) C10 C13 1.534(2) C10 C12 1.546(2) C11 H11A 0.9800 C11 H11B 0.9800 C11 H11C 0.9800 C12 H12A 0.9800 C12 H12B 0.9800 C12 H12C 0.9800 C13 C14 1.532(2) C13 H13A 0.9900 C13 H13B 0.9900 C14 C16 1.521(2) C14 C15 1.524(2) C14 N17 1.5513(19) C15 H15A 0.9800 C15 H15B 0.9800 C15 H15C 0.9800 C16 H16A 0.9800 C16 H16B 0.9800 C16 H16C 0.9800 N17 C18 1.4676(19) C18 C23 1.402(2) C18 C19 1.404(2) C19 C20 1.391(2) C19 C24 1.526(2) C20 C21 1.380(2) C20 H20 0.9500 C21 C22 1.384(2) C21 H21 0.9500 C22 C23 1.394(2) C22 H22 0.9500 C23 C27 1.526(2) C24 C25 1.533(3) C24 C26 1.537(2) C24 H24 1.0000 C25 H25A 0.9800 C25 H25B 0.9800 C25 H25C 0.9800 C26 H26A 0.9800 C26 H26B 0.9800 C26 H26C 0.9800 C27 C29 1.531(2) C27 C28 1.535(2) C27 H27 1.0000 C28 H28A 0.9800 C28 H28B 0.9800 C28 H28C 0.9800 C29 H29A 0.9800 C29 H29B 0.9800 C29 H29C 0.9800 O32 C33 1.4472(19) C33 C34 1.510(2) C33 C35 1.514(2) C33 H33 1.0000 C34 H34A 0.9800 C34 H34B 0.9800 C34 H34C 0.9800 C35 H35A 0.9800 C35 H35B 0.9800 C35 H35C 0.9800 C36 N44 1.296(2) C36 C37 1.520(2) C37 C38 1.528(2) C37 C40 1.535(2) C37 C39 1.546(2) C38 H38A 0.9800 C38 H38B 0.9800 C38 H38C 0.9800 C39 H39A 0.9800 C39 H39B 0.9800 C39 H39C 0.9800 C40 C41 1.527(2) C40 H40A 0.9900 C40 H40B 0.9900 C41 C42 1.520(2) C41 C43 1.525(2) C41 N44 1.5486(19) C42 H42A 0.9800 C42 H42B 0.9800 C42 H42C 0.9800 C43 H43A 0.9800 C43 H43B 0.9800 C43 H43C 0.9800 N44 C45 1.4644(19) C45 C50 1.405(2) C45 C46 1.407(2) C46 C47 1.389(2) C46 C51 1.524(2) C47 C48 1.381(2) C47 H47 0.9500 C48 C49 1.383(2) C48 H48 0.9500 C49 C50 1.394(2) C49 H49 0.9500 C50 C54 1.523(2) C51 C53 1.532(2) C51 C52 1.533(2) C51 H51 1.0000 C52 H52A 0.9800 C52 H52B 0.9800 C52 H52C 0.9800 C53 H53A 0.9800 C53 H53B 0.9800 C53 H53C 0.9800 C54 C56 1.536(2) C54 C55 1.538(2) C54 H54 1.0000 C55 H55A 0.9800 C55 H55B 0.9800 C55 H55C 0.9800 C56 H56A 0.9800 C56 H56B 0.9800 C56 H56C 0.9800 C57 C58 1.371(3) C57 C62 1.381(3) C57 H57 0.9500 C58 C59 1.365(3) C58 H58 0.9500 C59 C60 1.379(3) C59 H59 0.9500 C60 C61 1.380(3) C60 H60 0.9500 C61 C62 1.391(3) C61 H61 0.9500 C62 H62 0.9500