#------------------------------------------------------------------------------ #$Date: 2019-12-06 11:07:57 +0200 (Fri, 06 Dec 2019) $ #$Revision: 244926 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/64/1556429.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_1556429 loop_ _publ_author_name 'Rungthanaphatsophon, P.' 'Fajen, O.J.' 'Kelley, S.P.' 'Walensky, J.R.' _publ_section_title ; Thorium(IV) and Uranium(IV) Phosphaazaallenes ; _journal_name_full Inorganics _journal_page_first 105 _journal_paper_doi 10.3390/inorganics7090105 _journal_volume 7 _journal_year 2019 _chemical_formula_sum 'C36 H53 N2 P U' _chemical_formula_weight 782.80 _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 iterative _atom_sites_solution_secondary difmap _cell_angle_alpha 90 _cell_angle_beta 107.4770(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.0337(4) _cell_length_b 33.6762(14) _cell_length_c 10.7644(4) _cell_measurement_reflns_used 9968 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.44 _cell_measurement_theta_min 2.21 _cell_volume 3469.4(2) _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-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_unetI/netI 0.0315 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 63680 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.482 _diffrn_reflns_theta_min 2.212 _exptl_absorpt_coefficient_mu 4.750 _exptl_absorpt_correction_T_max 0.5624 _exptl_absorpt_correction_T_min 0.4798 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker AXScale' _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1560 _exptl_crystal_size_max 0.110 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.010 _refine_diff_density_max 0.995 _refine_diff_density_min -1.731 _refine_diff_density_rms 0.099 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 377 _refine_ls_number_reflns 7159 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.062 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0264 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0098P)^2^+6.5497P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.0459 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6047 _reflns_number_total 7159 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file Complex4_CIF.cif _cod_data_source_block s1_a _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1556429 _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 0.623 _shelx_estimated_absorpt_t_max 0.954 _shelx_res_file ; TITL s1_a.res in P2(1)/c s1_a.res created by SHELXL-2017/1 at 14:52:06 on 24-Jan-2018 REM Old TITL s1 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.061, Rweak 0.006, Alpha 0.130, Orientation as input REM Formula found by SHELXT: C34 N4 P U CELL 0.71073 10.0337 33.6762 10.7644 90.000 107.477 90.000 ZERR 4.000 0.0004 0.0014 0.0004 0.000 0.001 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N P U UNIT 144 212 8 4 4 TEMP -173 SIZE 0.01 0.04 0.11 L.S. 16 ACTA LIST 6 FMAP 2 PLAN 20 OMIT 0 4 0 OMIT 0 2 1 WGHT 0.009800 6.549700 FVAR 0.23573 U1 5 0.630772 0.615326 0.340546 11.00000 0.01226 0.01036 = 0.01305 0.00164 0.00463 0.00071 P1 4 0.252542 0.664074 0.158427 11.00000 0.01691 0.01875 = 0.01807 -0.00289 0.00230 0.00325 N1 3 0.912844 0.665872 0.596793 11.00000 0.01694 0.01526 = 0.02060 0.00377 0.00792 0.00187 N2 3 0.518746 0.674256 0.335396 11.00000 0.01831 0.01167 = 0.01414 0.00079 0.00609 0.00210 C1 1 0.634470 0.587228 0.582918 11.00000 0.01875 0.01888 = 0.01690 0.00733 0.00653 -0.00229 C2 1 0.700239 0.557042 0.529919 11.00000 0.01862 0.01543 = 0.01922 0.00910 0.00553 0.00335 C3 1 0.596830 0.539484 0.423545 11.00000 0.02272 0.01275 = 0.01886 0.00682 0.00746 -0.00068 C4 1 0.468412 0.559368 0.410869 11.00000 0.02286 0.01659 = 0.01817 0.00878 0.00456 -0.00511 C5 1 0.492239 0.588702 0.509459 11.00000 0.01828 0.01728 = 0.02217 0.00726 0.00986 -0.00243 C6 1 0.698054 0.608752 0.709620 11.00000 0.03045 0.02873 = 0.01917 -0.00029 0.00989 -0.00623 AFIX 137 H6A 2 0.667644 0.596132 0.778557 11.00000 -1.50000 H6B 2 0.667719 0.636546 0.700366 11.00000 -1.50000 H6C 2 0.800156 0.607580 0.732349 11.00000 -1.50000 AFIX 0 C7 1 0.849686 0.543956 0.587694 11.00000 0.02158 0.02702 = 0.02573 0.00932 0.00481 0.00605 AFIX 137 H7A 2 0.863503 0.534089 0.676324 11.00000 -1.50000 H7B 2 0.912118 0.566523 0.590243 11.00000 -1.50000 H7C 2 0.870659 0.522742 0.534099 11.00000 -1.50000 AFIX 0 C8 1 0.609899 0.502474 0.350115 11.00000 0.03534 0.01640 = 0.02543 0.00270 0.01277 -0.00317 AFIX 137 H8A 2 0.553939 0.481232 0.371818 11.00000 -1.50000 H8B 2 0.708084 0.494281 0.374308 11.00000 -1.50000 H8C 2 0.576196 0.507772 0.256324 11.00000 -1.50000 AFIX 0 C9 1 0.326900 0.546925 0.323713 11.00000 0.02615 0.02911 = 0.02715 0.01010 0.00261 -0.00853 AFIX 137 H9A 2 0.280558 0.530283 0.373031 11.00000 -1.50000 H9B 2 0.338151 0.531834 0.249666 11.00000 -1.50000 H9C 2 0.269978 0.570568 0.291773 11.00000 -1.50000 AFIX 0 C10 1 0.381415 0.613347 0.540074 11.00000 0.02137 0.02894 = 0.03210 0.00775 0.01514 0.00061 AFIX 137 H10A 2 0.321222 0.596167 0.573577 11.00000 -1.50000 H10B 2 0.325089 0.626681 0.460742 11.00000 -1.50000 H10C 2 0.425593 0.633281 0.605888 11.00000 -1.50000 AFIX 0 C11 1 0.877640 0.616536 0.274158 11.00000 0.01241 0.02140 = 0.01665 0.00087 0.00903 0.00253 C12 1 0.793298 0.647690 0.203336 11.00000 0.01551 0.01620 = 0.01500 0.00260 0.01029 -0.00119 C13 1 0.678597 0.630387 0.105820 11.00000 0.01721 0.01588 = 0.01440 0.00063 0.00876 0.00053 C14 1 0.692672 0.588460 0.118333 11.00000 0.01602 0.01621 = 0.01718 -0.00109 0.00897 -0.00039 C15 1 0.815309 0.580015 0.222471 11.00000 0.01784 0.01698 = 0.01742 0.00229 0.00968 0.00293 C16 1 1.021492 0.620102 0.367884 11.00000 0.01581 0.02604 = 0.02251 -0.00209 0.00689 0.00052 AFIX 137 H16A 2 1.090622 0.613200 0.323639 11.00000 -1.50000 H16B 2 1.030899 0.601988 0.441281 11.00000 -1.50000 H16C 2 1.037129 0.647451 0.400091 11.00000 -1.50000 AFIX 0 C17 1 0.830538 0.691089 0.215895 11.00000 0.02457 0.01699 = 0.02454 0.00015 0.00942 -0.00243 AFIX 137 H17A 2 0.883141 0.697807 0.155392 11.00000 -1.50000 H17B 2 0.887861 0.696734 0.305285 11.00000 -1.50000 H17C 2 0.744870 0.706995 0.195190 11.00000 -1.50000 AFIX 0 C18 1 0.575483 0.653719 0.000477 11.00000 0.02310 0.01786 = 0.01803 0.00339 0.00531 0.00117 AFIX 137 H18A 2 0.624516 0.666866 -0.054328 11.00000 -1.50000 H18B 2 0.530351 0.673760 0.040258 11.00000 -1.50000 H18C 2 0.504498 0.635712 -0.053035 11.00000 -1.50000 AFIX 0 C19 1 0.606842 0.557844 0.025304 11.00000 0.02286 0.01720 = 0.02052 -0.00364 0.01165 0.00194 AFIX 137 H19A 2 0.668382 0.541818 -0.010205 11.00000 -1.50000 H19B 2 0.537248 0.571302 -0.046015 11.00000 -1.50000 H19C 2 0.559306 0.540582 0.071878 11.00000 -1.50000 AFIX 0 C20 1 0.886516 0.540480 0.254857 11.00000 0.02457 0.01739 = 0.02710 0.00160 0.01116 0.00620 AFIX 137 H20A 2 0.963033 0.538730 0.216025 11.00000 -1.50000 H20B 2 0.818982 0.519204 0.220057 11.00000 -1.50000 H20C 2 0.924003 0.537704 0.349626 11.00000 -1.50000 AFIX 0 C21 1 0.821663 0.651505 0.517720 11.00000 0.02002 0.01266 = 0.01957 0.00160 0.00807 0.00075 C22 1 1.026526 0.685699 0.696194 11.00000 0.01922 0.02539 = 0.02262 -0.00596 0.00068 -0.00553 C23 1 0.967538 0.699175 0.804291 11.00000 0.03328 0.03376 = 0.02793 -0.01141 0.00293 0.00407 AFIX 137 H23A 2 0.932300 0.676092 0.840163 11.00000 -1.50000 H23B 2 0.891041 0.717991 0.768824 11.00000 -1.50000 H23C 2 1.041354 0.712106 0.873379 11.00000 -1.50000 AFIX 0 C24 1 1.142895 0.655453 0.745780 11.00000 0.02471 0.05009 = 0.02956 -0.00542 -0.00284 0.01249 AFIX 137 H24A 2 1.105852 0.631877 0.777401 11.00000 -1.50000 H24B 2 1.217673 0.667107 0.817104 11.00000 -1.50000 H24C 2 1.180174 0.647880 0.674800 11.00000 -1.50000 AFIX 0 C25 1 1.072196 0.720977 0.629802 11.00000 0.03358 0.03362 = 0.04560 -0.00685 0.00684 -0.01339 AFIX 137 H25A 2 1.108999 0.711368 0.560644 11.00000 -1.50000 H25B 2 1.145066 0.735868 0.694027 11.00000 -1.50000 H25C 2 0.991849 0.738350 0.592101 11.00000 -1.50000 AFIX 0 C26 1 0.422631 0.652570 0.247961 11.00000 0.01694 0.01688 = 0.00960 0.00206 0.00713 0.00107 C27 1 0.500675 0.716089 0.373922 11.00000 0.02322 0.01473 = 0.01624 -0.00113 0.00458 0.00531 C28 1 0.474197 0.743235 0.255131 11.00000 0.02904 0.01354 = 0.02461 0.00154 0.00713 0.00449 AFIX 137 H28A 2 0.553954 0.741872 0.220521 11.00000 -1.50000 H28B 2 0.462252 0.770623 0.280667 11.00000 -1.50000 H28C 2 0.389412 0.734611 0.188060 11.00000 -1.50000 AFIX 0 C29 1 0.635685 0.728962 0.475115 11.00000 0.02574 0.01564 = 0.02768 -0.00681 0.00204 0.00277 AFIX 137 H29A 2 0.713441 0.726820 0.438023 11.00000 -1.50000 H29B 2 0.653593 0.711790 0.551884 11.00000 -1.50000 H29C 2 0.626827 0.756551 0.500498 11.00000 -1.50000 AFIX 0 C30 1 0.379595 0.719090 0.432517 11.00000 0.03031 0.02269 = 0.01863 -0.00357 0.00896 0.00644 AFIX 137 H30A 2 0.293431 0.709729 0.368872 11.00000 -1.50000 H30B 2 0.367920 0.746800 0.455038 11.00000 -1.50000 H30C 2 0.399935 0.702660 0.511145 11.00000 -1.50000 AFIX 0 C31 1 0.192603 0.617770 0.071556 11.00000 0.01854 0.02107 = 0.00780 0.00129 0.00160 0.00118 C32 1 0.276920 0.590749 0.031543 11.00000 0.01552 0.02272 = 0.02241 -0.00265 0.00479 0.00048 AFIX 43 H32A 2 0.373635 0.596344 0.049215 11.00000 -1.20000 AFIX 0 C33 1 0.223619 0.556107 -0.033026 11.00000 0.02526 0.02560 = 0.02708 -0.00775 0.00924 0.00260 AFIX 43 H33A 2 0.283503 0.538455 -0.059901 11.00000 -1.20000 AFIX 0 C34 1 0.082726 0.546908 -0.058946 11.00000 0.02962 0.02457 = 0.02289 -0.00860 0.00336 -0.00417 AFIX 43 H34A 2 0.046454 0.522667 -0.100682 11.00000 -1.20000 AFIX 0 C35 1 -0.003340 0.573519 -0.023114 11.00000 0.01585 0.03565 = 0.02031 -0.00110 0.00271 -0.00691 AFIX 43 H35A 2 -0.100115 0.567843 -0.041819 11.00000 -1.20000 AFIX 0 C36 1 0.050214 0.608472 0.039960 11.00000 0.01785 0.02587 = 0.01557 0.00378 0.00303 0.00370 AFIX 43 H36A 2 -0.011225 0.626642 0.062425 11.00000 -1.20000 AFIX 0 HKLF 4 REM s1_a.res in P2(1)/c REM R1 = 0.0264 for 6047 Fo > 4sig(Fo) and 0.0376 for all 7159 data REM 377 parameters refined using 0 restraints END WGHT 0.0071 6.7432 REM Highest difference peak 0.995, deepest hole -1.731, 1-sigma level 0.099 Q1 1 0.7156 0.6143 0.4008 11.00000 0.05 0.99 Q2 1 0.6339 0.5959 0.2887 11.00000 0.05 0.83 Q3 1 1.1520 0.6160 0.7068 11.00000 0.05 0.71 Q4 1 0.5577 0.5957 0.2962 11.00000 0.05 0.51 Q5 1 0.1262 0.6265 0.0356 11.00000 0.05 0.44 Q6 1 0.5087 0.6946 0.3549 11.00000 0.05 0.44 Q7 1 0.2163 0.6399 0.1079 11.00000 0.05 0.42 Q8 1 0.0462 0.6015 -0.0322 11.00000 0.05 0.40 Q9 1 0.5037 0.6367 0.1832 11.00000 0.05 0.40 Q10 1 0.6003 0.6643 0.3397 11.00000 0.05 0.39 Q11 1 0.9592 0.6777 0.6550 11.00000 0.05 0.39 Q12 1 0.6016 0.6122 0.2389 11.00000 0.05 0.39 Q13 1 0.2196 0.5819 -0.0374 11.00000 0.05 0.38 Q14 1 0.4788 0.6540 0.3645 11.00000 0.05 0.38 Q15 1 0.4780 0.5778 0.4595 11.00000 0.05 0.38 Q16 1 0.8190 0.6279 0.4331 11.00000 0.05 0.37 Q17 1 0.5712 0.7159 0.4228 11.00000 0.05 0.37 Q18 1 0.7854 0.6304 0.4849 11.00000 0.05 0.37 Q19 1 0.4336 0.5878 0.5430 11.00000 0.05 0.37 Q20 1 0.9571 0.5642 0.4643 11.00000 0.05 0.37 ; _shelx_res_checksum 58424 _shelx_hkl_file ; 2 0 0 13.50 6.00 -2 0 0 30.90 9.40 2 0 0 20.80 8.00 -2 0 0 27.50 6.20 2 0 0 -2.10 9.80 -2 0 0 4.10 10.30 3 0 0 3183.88 98.69 -3 0 0 3206.68 95.59 3 0 0 3256.87 95.69 -3 0 0 3286.27 100.09 -3 0 0 3359.96 100.59 -3 0 0 3153.88 98.69 3 0 0 3081.99 100.29 4 0 0 3480.35 114.19 -4 0 0 3687.03 112.89 4 0 0 3660.73 108.29 -4 0 0 3757.72 107.99 4 0 0 3614.24 111.99 -4 0 0 3642.84 114.09 -4 0 0 3405.56 117.79 -5 0 0 921.01 33.10 -5 0 0 1002.50 42.20 -5 0 0 897.81 41.00 5 0 0 901.11 33.80 5 0 0 929.81 38.40 5 0 0 847.62 43.60 -5 0 0 934.81 43.50 6 0 0 221.68 21.30 -6 0 0 222.28 28.00 -6 0 0 229.48 26.70 -6 0 0 274.07 27.90 6 0 0 200.98 24.30 7 0 0 1553.24 69.99 7 0 0 1598.64 62.19 -7 0 0 1728.73 67.39 -7 0 0 1623.44 67.19 -7 0 0 1650.63 55.39 7 0 0 1668.33 57.29 -7 0 0 1590.54 68.99 8 0 0 1972.50 75.99 8 0 0 2032.30 85.69 -8 0 0 2050.99 67.29 8 0 0 1886.71 68.59 -8 0 0 2103.29 81.39 -8 0 0 1923.51 79.69 -9 0 0 588.84 49.60 9 0 0 542.65 51.79 9 0 0 572.64 34.40 -9 0 0 493.75 29.00 -9 0 0 485.55 46.10 10 0 0 64.59 18.60 -10 0 0 26.40 14.90 -10 0 0 18.90 26.60 -10 0 0 58.49 30.70 10 0 0 72.09 41.50 -11 0 0 753.82 61.39 11 0 0 674.93 40.70 11 0 0 675.03 68.39 -11 0 0 743.63 61.39 1 1 0 1804.72 54.89 1 1 0 1674.83 53.79 2 -1 0 1956.20 61.59 2 -1 0 1976.30 65.19 2 -1 0 2065.99 63.79 -2 -1 0 2101.89 61.99 -2 -1 0 2083.99 64.99 -2 -1 0 2227.08 66.29 -2 1 0 2042.40 64.19 2 1 0 2082.69 64.69 2 1 0 2046.90 62.09 2 1 0 1943.21 65.29 -2 1 0 2107.39 61.69 -2 1 0 2144.49 65.39 3 -1 0 988.00 32.50 3 -1 0 1033.90 35.50 -3 -1 0 940.61 36.50 -3 -1 0 1008.00 32.70 -3 -1 0 1015.80 38.30 -3 -1 0 946.91 36.40 3 -1 0 1013.10 37.80 -3 1 0 943.91 37.60 -3 1 0 993.70 32.30 -3 1 0 985.60 36.00 3 1 0 952.00 32.60 -3 1 0 1016.30 38.20 3 1 0 1001.60 36.20 3 1 0 934.71 37.90 4 -1 0 10.40 9.40 4 -1 0 8.90 12.70 4 -1 0 19.30 7.20 -4 -1 0 35.20 12.80 -4 -1 0 21.20 10.10 -4 -1 0 24.90 11.90 -4 -1 0 26.10 7.50 4 1 0 23.40 13.50 4 1 0 26.20 7.40 -4 1 0 18.10 12.70 -4 1 0 26.20 12.40 -4 1 0 12.10 13.30 4 1 0 21.90 10.50 -4 1 0 22.80 6.80 -5 -1 0 2317.17 79.39 5 -1 0 2361.86 77.39 -5 -1 0 2349.86 79.49 -5 -1 0 2388.16 72.69 5 -1 0 2316.87 72.69 5 -1 0 2161.18 80.39 -5 -1 0 2402.76 81.89 -5 1 0 2429.56 81.49 -5 1 0 2231.88 78.49 5 1 0 2369.06 78.09 5 1 0 2196.38 81.49 -5 1 0 2367.16 72.29 5 1 0 2345.87 73.19 -5 1 0 2182.48 79.69 -6 -1 0 813.32 40.70 -6 -1 0 811.22 42.20 6 -1 0 787.12 43.60 -6 -1 0 779.02 33.80 6 -1 0 843.82 37.10 -6 -1 0 827.42 43.40 -6 1 0 788.02 41.20 -6 1 0 801.12 42.10 -6 1 0 768.32 31.70 6 1 0 793.72 44.60 6 1 0 830.42 33.70 6 1 0 877.21 38.00 -6 1 0 834.32 42.10 7 -1 0 51.29 23.10 -7 -1 0 76.79 19.70 -7 -1 0 52.69 19.40 7 -1 0 79.09 13.80 -7 -1 0 66.19 21.20 -7 -1 0 51.09 11.30 7 -1 0 74.39 15.10 7 1 0 46.60 14.90 -7 1 0 59.99 11.10 -7 1 0 76.99 20.50 7 1 0 64.29 14.00 -7 1 0 70.99 21.50 7 1 0 47.20 21.20 -7 1 0 85.39 22.50 -8 -1 0 119.79 14.90 8 -1 0 106.89 19.60 -8 -1 0 122.59 24.20 8 -1 0 134.39 17.90 -8 -1 0 109.79 26.50 8 -1 0 119.69 29.60 8 1 0 105.99 29.10 8 1 0 133.89 17.40 -8 1 0 128.79 26.70 -8 1 0 131.49 27.80 8 1 0 54.19 18.10 -8 1 0 90.29 14.10 -9 -1 0 198.48 22.00 9 -1 0 202.98 36.30 -9 -1 0 230.98 33.40 9 -1 0 185.08 20.50 -9 -1 0 229.38 32.70 -9 1 0 212.08 33.00 -9 1 0 176.88 17.50 9 1 0 193.98 21.70 9 1 0 188.18 35.90 -9 1 0 177.78 32.40 -10 -1 0 409.76 47.20 -10 -1 0 416.66 44.20 10 -1 0 341.27 48.70 10 -1 0 348.97 31.60 -10 -1 0 393.96 27.70 -10 1 0 361.76 27.20 -10 1 0 389.36 46.30 10 1 0 450.25 64.49 -10 1 0 369.16 41.00 10 1 0 390.36 32.50 -11 -1 0 93.79 34.30 11 -1 0 147.89 40.90 -11 -1 0 155.88 39.60 11 -1 0 139.69 21.00 11 1 0 103.59 22.40 11 1 0 144.79 43.70 -1 -2 0 64.89 6.40 1 -2 0 62.59 6.30 -1 -2 0 59.99 6.90 1 -2 0 60.79 4.90 1 -2 0 64.79 4.40 1 2 0 53.49 6.40 1 2 0 68.29 7.50 1 2 0 63.89 5.00 -1 2 0 57.59 4.50 -2 -2 0 298.37 14.00 -2 -2 0 302.87 19.40 2 -2 0 262.27 13.00 -2 -2 0 298.77 19.20 2 -2 0 291.67 15.40 2 -2 0 253.47 18.60 2 2 0 276.47 21.10 2 2 0 319.37 18.60 2 2 0 295.97 14.50 -2 2 0 267.87 13.00 -2 2 0 247.58 18.70 -2 2 0 293.87 16.70 3 -2 0 229.58 12.30 -3 -2 0 261.77 20.40 3 -2 0 211.88 18.10 -3 -2 0 221.78 16.40 -3 -2 0 252.67 18.40 3 -2 0 262.47 15.40 -3 -2 0 247.08 13.00 3 2 0 235.88 19.70 -3 2 0 238.78 16.70 -3 2 0 285.57 20.10 -3 2 0 232.18 12.40 -3 2 0 233.68 17.80 3 2 0 255.77 17.50 3 2 0 249.18 13.80 4 -2 0 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708.13 60.09 -4 -6 13 81.89 42.20 4 -6 -13 159.58 37.30 4 -6 -13 101.69 30.90 -4 6 13 164.78 49.80 4 6 -13 168.98 41.20 4 6 -13 152.78 34.40 -3 -6 13 47.40 39.80 3 -6 -13 -16.20 30.50 3 -6 -13 39.30 33.90 -3 6 13 -22.90 41.90 3 6 -13 -37.80 30.00 3 6 -13 70.39 36.80 2 -6 -13 383.06 42.50 -2 -6 13 327.07 56.19 2 -6 -13 449.16 56.79 -2 6 13 392.36 54.99 2 6 -13 404.96 49.50 2 6 -13 472.35 51.59 1 -6 -13 703.63 64.39 1 6 -13 729.83 55.19 1 6 -13 813.22 66.29 -1 6 13 869.61 77.39 -6 -7 13 93.49 46.00 6 -7 -13 102.29 38.90 6 7 -13 -9.10 34.80 6 7 -13 -4.00 40.50 -6 7 13 3.10 42.80 -6 7 13 68.99 29.30 -5 -7 13 65.99 44.90 5 -7 -13 14.00 26.80 5 -7 -13 44.20 38.40 5 7 -13 14.60 38.50 -5 7 13 -35.70 25.80 5 7 -13 -29.30 35.90 -5 7 13 27.50 46.80 4 -7 -13 74.99 35.60 -4 -7 13 152.38 43.10 4 -7 -13 7.10 27.70 4 7 -13 61.09 36.70 -4 7 13 65.89 45.30 4 7 -13 21.90 31.10 3 -7 -13 1.10 30.90 -3 -7 13 34.90 35.20 3 -7 -13 61.39 35.10 -3 7 13 -6.50 38.60 3 7 -13 31.10 30.40 3 7 -13 63.89 34.60 2 -7 -13 -29.30 31.30 2 -7 -13 10.80 30.40 -2 7 13 -30.20 43.90 2 7 -13 52.49 34.60 2 7 -13 51.39 30.00 5 -8 -13 251.67 43.90 -5 -8 13 271.67 49.40 5 8 -13 267.97 45.50 -5 8 13 301.07 52.29 -5 8 13 176.68 31.50 5 8 -13 266.87 37.60 4 -8 -13 54.39 28.50 -4 -8 13 104.39 45.60 4 -8 -13 140.19 38.40 4 8 -13 48.90 33.00 -4 8 13 176.78 47.80 -4 8 13 15.00 25.40 4 8 -13 37.10 36.90 -3 -8 13 22.60 36.70 3 -8 -13 58.19 34.90 3 -8 -13 57.29 31.40 3 8 -13 -6.70 33.50 3 8 -13 43.00 33.30 -3 8 13 114.99 43.00 2 -8 -13 55.69 35.10 2 -8 -13 57.49 33.30 -2 8 13 113.69 48.20 2 8 -13 123.99 37.50 2 8 -13 104.89 34.00 -5 -9 13 37.20 44.10 5 -9 -13 41.80 38.90 -5 9 13 -50.59 24.90 5 9 -13 21.10 39.70 5 9 -13 42.30 32.40 -5 9 13 -19.70 40.90 4 -9 -13 325.97 36.70 -4 -9 13 260.67 51.49 4 -9 -13 369.96 46.80 4 9 -13 265.17 40.40 -4 9 13 239.98 33.10 -4 9 13 333.77 54.29 4 9 -13 335.77 45.60 3 -9 -13 822.92 64.19 3 -9 -13 736.93 58.89 -3 -9 13 717.23 72.39 3 9 -13 802.82 63.39 3 9 -13 638.24 62.59 -3 9 13 790.32 74.59 2 -9 -13 250.17 39.70 2 -9 -13 245.28 42.90 -2 9 13 281.57 51.09 2 9 -13 227.28 40.20 2 9 -13 279.07 37.40 -5 -10 13 428.86 54.39 -5 10 13 417.76 47.40 5 10 -13 513.95 55.79 -5 10 13 496.55 58.69 -4 -10 13 211.48 47.30 4 -10 -13 114.49 37.30 4 -10 -13 147.19 32.70 -4 10 13 108.59 28.80 4 10 -13 201.38 42.40 -4 10 13 128.89 49.70 4 10 -13 194.48 36.60 3 -10 -13 52.59 36.50 -3 -10 13 20.80 40.90 3 -10 -13 -23.10 29.00 -3 10 13 36.20 42.30 3 10 -13 33.20 31.90 3 10 -13 11.90 35.10 -4 -11 13 10.00 42.00 -4 11 13 -45.80 27.40 -4 11 13 -24.40 42.90 4 11 -13 42.30 34.60 3 11 -13 15.10 34.90 -3 11 13 44.60 43.90 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 77872 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.63077(2) 0.61533(2) 0.34055(2) 0.01171(4) Uani 1 1 d . . . . . P1 P 0.25254(9) 0.66407(3) 0.15843(8) 0.01856(19) Uani 1 1 d . . . . . N1 N 0.9128(3) 0.66587(8) 0.5968(3) 0.0171(6) Uani 1 1 d . . . . . N2 N 0.5187(3) 0.67426(7) 0.3354(2) 0.0144(6) Uani 1 1 d . . . . . C1 C 0.6345(3) 0.58723(10) 0.5829(3) 0.0179(7) Uani 1 1 d . . . . . C2 C 0.7002(3) 0.55704(9) 0.5299(3) 0.0178(7) Uani 1 1 d . . . . . C3 C 0.5968(3) 0.53948(9) 0.4235(3) 0.0178(7) Uani 1 1 d . . . . . C4 C 0.4684(4) 0.55937(10) 0.4109(3) 0.0196(7) Uani 1 1 d . . . . . C5 C 0.4922(3) 0.58870(10) 0.5095(3) 0.0184(7) Uani 1 1 d . . . . . C6 C 0.6981(4) 0.60875(11) 0.7096(3) 0.0256(8) Uani 1 1 d . . . . . H6A H 0.667644 0.596132 0.778557 0.038 Uiso 1 1 calc R U . . . H6B H 0.667719 0.636546 0.700366 0.038 Uiso 1 1 calc R U . . . H6C H 0.800156 0.607580 0.732349 0.038 Uiso 1 1 calc R U . . . C7 C 0.8497(4) 0.54396(11) 0.5877(3) 0.0253(8) Uani 1 1 d . . . . . H7A H 0.863503 0.534089 0.676324 0.038 Uiso 1 1 calc R U . . . H7B H 0.912118 0.566523 0.590243 0.038 Uiso 1 1 calc R U . . . H7C H 0.870659 0.522742 0.534099 0.038 Uiso 1 1 calc R U . . . C8 C 0.6099(4) 0.50247(10) 0.3501(3) 0.0249(8) Uani 1 1 d . . . . . H8A H 0.553939 0.481232 0.371818 0.037 Uiso 1 1 calc R U . . . H8B H 0.708084 0.494281 0.374308 0.037 Uiso 1 1 calc R U . . . H8C H 0.576196 0.507772 0.256324 0.037 Uiso 1 1 calc R U . . . C9 C 0.3269(4) 0.54693(11) 0.3237(4) 0.0287(9) Uani 1 1 d . . . . . H9A H 0.280558 0.530283 0.373031 0.043 Uiso 1 1 calc R U . . . H9B H 0.338151 0.531834 0.249666 0.043 Uiso 1 1 calc R U . . . H9C H 0.269978 0.570568 0.291773 0.043 Uiso 1 1 calc R U . . . C10 C 0.3814(3) 0.61335(11) 0.5401(3) 0.0259(8) Uani 1 1 d . . . . . H10A H 0.321222 0.596167 0.573577 0.039 Uiso 1 1 calc R U . . . H10B H 0.325089 0.626681 0.460742 0.039 Uiso 1 1 calc R U . . . H10C H 0.425593 0.633281 0.605888 0.039 Uiso 1 1 calc R U . . . C11 C 0.8776(3) 0.61654(10) 0.2742(3) 0.0158(6) Uani 1 1 d . . . . . C12 C 0.7933(3) 0.64769(9) 0.2033(3) 0.0143(7) Uani 1 1 d . . . . . C13 C 0.6786(3) 0.63039(9) 0.1058(3) 0.0149(7) Uani 1 1 d . . . . . C14 C 0.6927(3) 0.58846(9) 0.1183(3) 0.0156(7) Uani 1 1 d . . . . . C15 C 0.8153(3) 0.58002(9) 0.2225(3) 0.0164(7) Uani 1 1 d . . . . . C16 C 1.0215(3) 0.62010(10) 0.3679(3) 0.0212(7) Uani 1 1 d . . . . . H16A H 1.090622 0.613200 0.323639 0.032 Uiso 1 1 calc R U . . . H16B H 1.030899 0.601988 0.441281 0.032 Uiso 1 1 calc R U . . . H16C H 1.037129 0.647451 0.400091 0.032 Uiso 1 1 calc R U . . . C17 C 0.8305(4) 0.69109(10) 0.2159(3) 0.0216(8) Uani 1 1 d . . . . . H17A H 0.883141 0.697807 0.155392 0.032 Uiso 1 1 calc R U . . . H17B H 0.887861 0.696734 0.305285 0.032 Uiso 1 1 calc R U . . . H17C H 0.744870 0.706995 0.195190 0.032 Uiso 1 1 calc R U . . . C18 C 0.5755(3) 0.65372(10) 0.0005(3) 0.0199(7) Uani 1 1 d . . . . . H18A H 0.624516 0.666866 -0.054328 0.030 Uiso 1 1 calc R U . . . H18B H 0.530351 0.673760 0.040258 0.030 Uiso 1 1 calc R U . . . H18C H 0.504498 0.635712 -0.053035 0.030 Uiso 1 1 calc R U . . . C19 C 0.6068(4) 0.55784(10) 0.0253(3) 0.0191(7) Uani 1 1 d . . . . . H19A H 0.668382 0.541818 -0.010205 0.029 Uiso 1 1 calc R U . . . H19B H 0.537248 0.571302 -0.046015 0.029 Uiso 1 1 calc R U . . . H19C H 0.559306 0.540582 0.071878 0.029 Uiso 1 1 calc R U . . . C20 C 0.8865(4) 0.54048(10) 0.2549(3) 0.0223(8) Uani 1 1 d . . . . . H20A H 0.963033 0.538730 0.216025 0.033 Uiso 1 1 calc R U . . . H20B H 0.818982 0.519204 0.220057 0.033 Uiso 1 1 calc R U . . . H20C H 0.924003 0.537704 0.349626 0.033 Uiso 1 1 calc R U . . . C21 C 0.8217(3) 0.65150(9) 0.5177(3) 0.0169(7) Uani 1 1 d . . . . . C22 C 1.0265(4) 0.68570(10) 0.6962(3) 0.0236(8) Uani 1 1 d . . . . . C23 C 0.9675(4) 0.69918(12) 0.8043(4) 0.0330(9) Uani 1 1 d . . . . . H23A H 0.932300 0.676092 0.840163 0.050 Uiso 1 1 calc R U . . . H23B H 0.891041 0.717991 0.768824 0.050 Uiso 1 1 calc R U . . . H23C H 1.041354 0.712106 0.873379 0.050 Uiso 1 1 calc R U . . . C24 C 1.1429(4) 0.65545(13) 0.7458(4) 0.0372(10) Uani 1 1 d . . . . . H24A H 1.105852 0.631877 0.777401 0.056 Uiso 1 1 calc R U . . . H24B H 1.217673 0.667107 0.817104 0.056 Uiso 1 1 calc R U . . . H24C H 1.180174 0.647880 0.674800 0.056 Uiso 1 1 calc R U . . . C25 C 1.0722(4) 0.72098(12) 0.6298(4) 0.0387(10) Uani 1 1 d . . . . . H25A H 1.108999 0.711368 0.560644 0.058 Uiso 1 1 calc R U . . . H25B H 1.145066 0.735868 0.694027 0.058 Uiso 1 1 calc R U . . . H25C H 0.991849 0.738350 0.592101 0.058 Uiso 1 1 calc R U . . . C26 C 0.4226(3) 0.65257(9) 0.2480(3) 0.0138(7) Uani 1 1 d . . . . . C27 C 0.5007(3) 0.71609(9) 0.3739(3) 0.0184(7) Uani 1 1 d . . . . . C28 C 0.4742(4) 0.74324(10) 0.2551(3) 0.0226(8) Uani 1 1 d . . . . . H28A H 0.553954 0.741872 0.220521 0.034 Uiso 1 1 calc R U . . . H28B H 0.462252 0.770623 0.280667 0.034 Uiso 1 1 calc R U . . . H28C H 0.389412 0.734611 0.188060 0.034 Uiso 1 1 calc R U . . . C29 C 0.6357(4) 0.72896(10) 0.4751(3) 0.0243(8) Uani 1 1 d . . . . . H29A H 0.713441 0.726820 0.438023 0.037 Uiso 1 1 calc R U . . . H29B H 0.653593 0.711790 0.551884 0.037 Uiso 1 1 calc R U . . . H29C H 0.626827 0.756551 0.500498 0.037 Uiso 1 1 calc R U . . . C30 C 0.3796(4) 0.71909(10) 0.4325(3) 0.0235(8) Uani 1 1 d . . . . . H30A H 0.293431 0.709729 0.368872 0.035 Uiso 1 1 calc R U . . . H30B H 0.367920 0.746800 0.455038 0.035 Uiso 1 1 calc R U . . . H30C H 0.399935 0.702660 0.511145 0.035 Uiso 1 1 calc R U . . . C31 C 0.1926(3) 0.61777(10) 0.0716(3) 0.0163(7) Uani 1 1 d . . . . . C32 C 0.2769(4) 0.59075(10) 0.0315(3) 0.0204(7) Uani 1 1 d . . . . . H32A H 0.373635 0.596344 0.049215 0.024 Uiso 1 1 calc R U . . . C33 C 0.2236(4) 0.55611(11) -0.0330(3) 0.0257(8) Uani 1 1 d . . . . . H33A H 0.283503 0.538455 -0.059901 0.031 Uiso 1 1 calc R U . . . C34 C 0.0827(4) 0.54691(11) -0.0589(3) 0.0267(8) Uani 1 1 d . . . . . H34A H 0.046454 0.522667 -0.100682 0.032 Uiso 1 1 calc R U . . . C35 C -0.0033(4) 0.57352(11) -0.0231(3) 0.0245(8) Uani 1 1 d . . . . . H35A H -0.100115 0.567843 -0.041819 0.029 Uiso 1 1 calc R U . . . C36 C 0.0502(3) 0.60847(10) 0.0400(3) 0.0202(7) Uani 1 1 d . . . . . H36A H -0.011225 0.626642 0.062425 0.024 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 U1 0.01226(6) 0.01036(6) 0.01305(6) 0.00164(5) 0.00463(4) 0.00071(6) P1 0.0169(5) 0.0187(5) 0.0181(4) -0.0029(3) 0.0023(4) 0.0033(4) N1 0.0169(15) 0.0153(14) 0.0206(15) 0.0038(12) 0.0079(13) 0.0019(12) N2 0.0183(14) 0.0117(13) 0.0141(14) 0.0008(11) 0.0061(12) 0.0021(11) C1 0.0188(18) 0.0189(17) 0.0169(17) 0.0073(14) 0.0065(15) -0.0023(14) C2 0.0186(18) 0.0154(17) 0.0192(18) 0.0091(14) 0.0055(15) 0.0034(14) C3 0.0227(18) 0.0128(16) 0.0189(17) 0.0068(13) 0.0075(15) -0.0007(14) C4 0.0229(19) 0.0166(17) 0.0182(18) 0.0088(14) 0.0046(15) -0.0051(14) C5 0.0183(18) 0.0173(17) 0.0222(18) 0.0073(14) 0.0099(15) -0.0024(14) C6 0.030(2) 0.029(2) 0.0192(18) -0.0003(15) 0.0099(16) -0.0062(16) C7 0.0216(19) 0.027(2) 0.026(2) 0.0093(16) 0.0048(16) 0.0060(16) C8 0.035(2) 0.0164(17) 0.025(2) 0.0027(15) 0.0128(17) -0.0032(16) C9 0.026(2) 0.029(2) 0.027(2) 0.0101(16) 0.0026(17) -0.0085(17) C10 0.0214(18) 0.0289(19) 0.032(2) 0.0077(18) 0.0151(16) 0.0006(17) C11 0.0124(15) 0.0214(17) 0.0167(16) 0.0009(15) 0.0090(13) 0.0025(15) C12 0.0155(16) 0.0162(17) 0.0150(16) 0.0026(13) 0.0103(14) -0.0012(13) C13 0.0172(17) 0.0159(16) 0.0144(16) 0.0006(13) 0.0088(14) 0.0005(13) C14 0.0160(17) 0.0162(17) 0.0172(17) -0.0011(13) 0.0090(15) -0.0004(14) C15 0.0178(17) 0.0170(17) 0.0174(17) 0.0023(14) 0.0097(15) 0.0029(14) C16 0.0158(16) 0.0260(19) 0.0225(18) -0.0021(15) 0.0069(14) 0.0005(15) C17 0.0246(19) 0.0170(18) 0.0245(19) 0.0001(14) 0.0094(16) -0.0024(15) C18 0.0231(18) 0.0179(17) 0.0180(17) 0.0034(14) 0.0053(15) 0.0012(15) C19 0.0229(19) 0.0172(17) 0.0205(18) -0.0036(14) 0.0116(15) 0.0019(14) C20 0.0246(19) 0.0174(18) 0.027(2) 0.0016(15) 0.0112(16) 0.0062(15) C21 0.0200(18) 0.0127(16) 0.0196(18) 0.0016(14) 0.0081(16) 0.0008(14) C22 0.0192(18) 0.0254(19) 0.0226(19) -0.0060(15) 0.0007(16) -0.0055(15) C23 0.033(2) 0.034(2) 0.028(2) -0.0114(17) 0.0029(18) 0.0041(18) C24 0.025(2) 0.050(3) 0.030(2) -0.005(2) -0.0028(18) 0.0125(19) C25 0.034(2) 0.034(2) 0.046(3) -0.0068(19) 0.007(2) -0.0134(19) C26 0.0169(16) 0.0169(16) 0.0096(15) 0.0021(13) 0.0071(13) 0.0011(13) C27 0.0232(19) 0.0147(17) 0.0162(17) -0.0011(13) 0.0046(15) 0.0053(14) C28 0.029(2) 0.0135(17) 0.0246(19) 0.0015(14) 0.0071(16) 0.0045(15) C29 0.026(2) 0.0156(17) 0.028(2) -0.0068(15) 0.0020(16) 0.0028(15) C30 0.030(2) 0.0227(19) 0.0186(18) -0.0036(15) 0.0090(16) 0.0064(16) C31 0.0185(16) 0.0211(17) 0.0078(14) 0.0013(14) 0.0016(13) 0.0012(15) C32 0.0155(17) 0.0227(19) 0.0224(19) -0.0027(15) 0.0048(15) 0.0005(14) C33 0.025(2) 0.026(2) 0.027(2) -0.0077(16) 0.0092(17) 0.0026(16) C34 0.030(2) 0.025(2) 0.0229(19) -0.0086(15) 0.0034(17) -0.0042(16) C35 0.0158(18) 0.036(2) 0.0203(19) -0.0011(16) 0.0027(15) -0.0069(16) C36 0.0179(17) 0.026(2) 0.0156(17) 0.0038(14) 0.0030(14) 0.0037(14) 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 N2 U1 C26 33.43(10) . . N2 U1 C21 81.78(10) . . C26 U1 C21 115.18(10) . . N2 U1 C12 90.55(9) . . C26 U1 C12 98.87(10) . . C21 U1 C12 77.25(10) . . N2 U1 C4 106.04(10) . . C26 U1 C4 87.62(10) . . C21 U1 C4 119.57(10) . . C12 U1 C4 157.41(10) . . N2 U1 C5 87.50(9) . . C26 U1 C5 83.95(10) . . C21 U1 C5 94.36(10) . . C12 U1 C5 171.58(10) . . C4 U1 C5 29.90(10) . . N2 U1 C13 92.17(9) . . C26 U1 C13 83.79(10) . . C21 U1 C13 107.28(10) . . C12 U1 C13 30.15(9) . . C4 U1 C13 131.36(10) . . C5 U1 C13 158.09(10) . . N2 U1 C3 135.03(10) . . C26 U1 C3 116.39(10) . . C21 U1 C3 109.61(10) . . C12 U1 C3 134.05(10) . . C4 U1 C3 29.95(10) . . C5 U1 C3 49.33(10) . . C13 U1 C3 122.63(9) . . N2 U1 C2 130.63(9) . . C26 U1 C2 132.64(10) . . C21 U1 C2 79.78(10) . . C12 U1 C2 128.48(10) . . C4 U1 C2 49.27(10) . . C5 U1 C2 49.18(10) . . C13 U1 C2 137.04(10) . . C3 U1 C2 29.84(10) . . N2 U1 C1 100.85(9) . . C26 U1 C1 109.66(10) . . C21 U1 C1 70.49(10) . . C12 U1 C1 143.61(10) . . C4 U1 C1 49.08(10) . . C5 U1 C1 29.61(10) . . C13 U1 C1 166.18(10) . . C3 U1 C1 49.15(10) . . C2 U1 C1 29.79(10) . . N2 U1 C11 116.98(10) . . C26 U1 C11 128.47(10) . . C21 U1 C11 70.14(10) . . C12 U1 C11 29.81(9) . . C4 U1 C11 136.97(10) . . C5 U1 C11 147.37(10) . . C13 U1 C11 49.25(9) . . C3 U1 C11 107.65(10) . . C2 U1 C11 98.82(10) . . C1 U1 C11 119.18(9) . . N2 U1 C14 119.79(9) . . C26 U1 C14 101.80(10) . . C21 U1 C14 118.75(10) . . C12 U1 C14 49.09(9) . . C4 U1 C14 108.47(10) . . C5 U1 C14 138.29(10) . . C13 U1 C14 29.65(9) . . C3 U1 C14 93.34(9) . . C2 U1 C14 109.24(9) . . C1 U1 C14 138.85(9) . . C11 U1 C14 48.71(9) . . C26 P1 C31 102.23(15) . . C21 N1 C22 177.8(3) . . C26 N2 C27 125.8(3) . . C26 N2 U1 77.77(17) . . C27 N2 U1 156.4(2) . . C5 C1 C2 108.3(3) . . C5 C1 C6 125.0(3) . . C2 C1 C6 125.9(3) . . C5 C1 U1 74.58(18) . . C2 C1 U1 75.07(18) . . C6 C1 U1 124.9(2) . . C1 C2 C3 107.8(3) . . C1 C2 C7 124.6(3) . . C3 C2 C7 127.3(3) . . C1 C2 U1 75.14(18) . . C3 C2 U1 74.94(17) . . C7 C2 U1 120.8(2) . . C4 C3 C2 107.6(3) . . C4 C3 C8 124.0(3) . . C2 C3 C8 127.6(3) . . C4 C3 U1 74.31(18) . . C2 C3 U1 75.22(18) . . C8 C3 U1 123.9(2) . . C5 C4 C3 108.2(3) . . C5 C4 C9 125.1(3) . . C3 C4 C9 125.9(3) . . C5 C4 U1 75.34(18) . . C3 C4 U1 75.74(18) . . C9 C4 U1 123.1(2) . . C1 C5 C4 108.1(3) . . C1 C5 C10 126.0(3) . . C4 C5 C10 125.5(3) . . C1 C5 U1 75.80(18) . . C4 C5 U1 74.76(18) . . C10 C5 U1 121.3(2) . . C15 C11 C12 108.0(3) . . C15 C11 C16 123.9(3) . . C12 C11 C16 127.0(3) . . C15 C11 U1 76.44(18) . . C12 C11 U1 73.43(17) . . C16 C11 U1 125.6(2) . . C11 C12 C13 108.2(3) . . C11 C12 C17 125.3(3) . . C13 C12 C17 125.9(3) . . C11 C12 U1 76.77(17) . . C13 C12 U1 75.80(17) . . C17 C12 U1 120.7(2) . . C14 C13 C12 107.5(3) . . C14 C13 C18 128.0(3) . . C12 C13 C18 124.1(3) . . C14 C13 U1 76.71(18) . . C12 C13 U1 74.05(17) . . C18 C13 U1 121.1(2) . . C13 C14 C15 108.1(3) . . C13 C14 C19 126.4(3) . . C15 C14 C19 124.8(3) . . C13 C14 U1 73.64(18) . . C15 C14 U1 75.66(18) . . C19 C14 U1 123.9(2) . . C11 C15 C14 108.2(3) . . C11 C15 C20 123.8(3) . . C14 C15 C20 126.8(3) . . C11 C15 U1 74.19(17) . . C14 C15 U1 74.92(18) . . C20 C15 U1 127.1(2) . . N1 C21 U1 175.8(3) . . N1 C22 C24 107.3(3) . . N1 C22 C23 107.3(3) . . C24 C22 C23 111.4(3) . . N1 C22 C25 106.8(3) . . C24 C22 C25 112.3(3) . . C23 C22 C25 111.5(3) . . N2 C26 P1 130.4(2) . . N2 C26 U1 68.80(17) . . P1 C26 U1 160.61(18) . . N2 C27 C29 108.1(3) . . N2 C27 C28 109.7(3) . . C29 C27 C28 108.8(3) . . N2 C27 C30 110.7(3) . . C29 C27 C30 109.4(3) . . C28 C27 C30 110.2(3) . . C32 C31 C36 116.6(3) . . C32 C31 P1 125.3(2) . . C36 C31 P1 118.1(2) . . C33 C32 C31 121.8(3) . . C32 C33 C34 120.4(3) . . C35 C34 C33 118.9(3) . . C34 C35 C36 120.5(3) . . C35 C36 C31 121.8(3) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 U1 N2 2.273(2) . U1 C26 2.383(3) . U1 C21 2.568(3) . U1 C12 2.734(3) . U1 C4 2.742(3) . U1 C5 2.750(3) . U1 C13 2.757(3) . U1 C3 2.760(3) . U1 C2 2.764(3) . U1 C1 2.765(3) . U1 C11 2.777(3) . U1 C14 2.796(3) . P1 C26 1.733(3) . P1 C31 1.825(3) . N1 C21 1.152(4) . N1 C22 1.469(4) . N2 C26 1.343(4) . N2 C27 1.495(4) . C1 C5 1.409(5) . C1 C2 1.421(5) . C1 C6 1.507(5) . C2 C3 1.423(5) . C2 C7 1.506(5) . C3 C4 1.422(5) . C3 C8 1.503(5) . C4 C5 1.417(5) . C4 C9 1.507(5) . C5 C10 1.501(5) . C11 C15 1.416(5) . C11 C12 1.418(4) . C11 C16 1.497(4) . C12 C13 1.428(4) . C12 C17 1.505(4) . C13 C14 1.421(4) . C13 C18 1.506(4) . C14 C15 1.422(5) . C14 C19 1.513(4) . C15 C20 1.502(4) . C22 C24 1.520(5) . C22 C23 1.524(5) . C22 C25 1.526(5) . C27 C29 1.524(5) . C27 C28 1.529(4) . C27 C30 1.531(5) . C31 C32 1.396(5) . C31 C36 1.401(4) . C32 C33 1.381(5) . C33 C34 1.391(5) . C34 C35 1.378(5) . C35 C36 1.384(5) .