#------------------------------------------------------------------------------ #$Date: 2019-12-24 04:17:23 +0200 (Tue, 24 Dec 2019) $ #$Revision: 245548 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125690.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_7125690 loop_ _publ_author_name 'Mei, Ruhuai' 'Fang, Xin-Yue' 'He, Liang' 'Sun, Junmei' 'Zou, Liang' 'Ma, Wenbo' 'Ackermann, Lutz' _publ_section_title ; Cobaltaelectro-Catalyzed Oxidative Allene Annulation by Electro-Removable Hydrazides ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C9CC09076B _journal_year 2020 _chemical_formula_sum 'C28 H24 N3 O2 P' _chemical_formula_weight 465.47 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-11-06 deposited with the CCDC. 2019-12-23 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 110.736(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.7656(3) _cell_length_b 22.5128(5) _cell_length_c 11.5704(3) _cell_measurement_temperature 293(2) _cell_volume 2378.98(12) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.978 _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_unetI/netI 0.0392 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.978 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 13259 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.978 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 71.900 _diffrn_reflns_theta_min 3.927 _exptl_absorpt_coefficient_mu 1.268 _exptl_crystal_density_diffrn 1.300 _exptl_crystal_F_000 976 _refine_diff_density_max 0.329 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.067 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 308 _refine_ls_number_reflns 4561 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.016 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0618 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1220P)^2^+0.3630P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1683 _refine_ls_wR_factor_ref 0.1834 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3742 _reflns_number_total 4561 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc09076b2.cif _cod_data_source_block cd-meh-hl-rmc87b _cod_original_cell_volume 2379.00(11) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7125690 _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_res_file ; cd-meh-hl-rmc87b.res created by SHELXL-2014/7 TITL cd-meh-hl-rmc87b_a.res in P2(1)/c REM Old TITL cd-meh-hl-rmc87b in P21/c #14 REM SHELXT solution in P2(1)/c REM R1 0.176, Rweak 0.067, Alpha 0.033, Orientation as input REM Formula found by SHELXT: C28 N3 O2 Cl CELL 1.54184 9.765604 22.512788 11.570433 90 110.7356 90 ZERR 4 0.000253 0.000535 0.000297 0 0.0029 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O P UNIT 112 96 12 8 4 L.S. 10 PLAN 20 BOND $H LIST 6 fmap 2 ACTA REM REM REM WGHT 0.122000 0.363000 FVAR 0.52238 P01 5 0.659526 0.261685 0.589190 11.00000 0.04393 0.03074 = 0.04344 0.00150 0.00383 0.00033 O002 4 0.878315 0.501719 0.668284 11.00000 0.04697 0.04336 = 0.07623 0.00184 0.01338 -0.01315 O003 4 0.679733 0.287426 0.478537 11.00000 0.06820 0.04594 = 0.05160 0.00731 0.01288 0.00180 N004 3 0.803386 0.408990 0.694881 11.00000 0.03120 0.03552 = 0.04708 -0.00397 0.00821 -0.00066 N005 3 0.942187 0.387348 0.706792 11.00000 0.03389 0.04651 = 0.04911 -0.00698 0.01028 0.00105 N006 3 1.189360 0.402398 0.812268 11.00000 0.03738 0.06331 = 0.05324 0.00501 0.01416 0.00424 C007 1 1.055409 0.403632 0.815962 11.00000 0.03498 0.03526 = 0.04884 0.00220 0.01105 0.00102 C008 1 0.634860 0.491087 0.665037 11.00000 0.04426 0.03968 = 0.03503 -0.00585 0.00600 0.00191 C009 1 0.780162 0.469972 0.674774 11.00000 0.04127 0.03468 = 0.04320 -0.00480 0.00567 -0.00545 C00A 1 0.734601 0.188061 0.624509 11.00000 0.03785 0.03420 = 0.04784 0.00200 0.01059 -0.00040 C00B 1 0.531431 0.451699 0.679107 11.00000 0.04311 0.04833 = 0.03206 -0.00176 0.00912 0.00600 C00C 1 0.699785 0.369232 0.708988 11.00000 0.03943 0.03454 = 0.03871 -0.00237 0.00804 -0.00424 C00D 1 0.567985 0.390444 0.701991 11.00000 0.03940 0.04534 = 0.04282 0.00044 0.01167 -0.00568 AFIX 43 H00D 2 0.499185 0.364465 0.712354 11.00000 -1.20000 AFIX 0 C00E 1 1.027454 0.417413 0.923467 11.00000 0.04082 0.05370 = 0.05104 -0.00139 0.01562 0.00097 AFIX 43 H00E 2 0.932322 0.417532 0.923703 11.00000 -1.20000 AFIX 0 C00F 1 0.468373 0.253762 0.568747 11.00000 0.04407 0.03778 = 0.05343 -0.00199 0.00246 0.00187 C00G 1 0.678238 0.145845 0.532426 11.00000 0.04962 0.04668 = 0.05328 -0.00142 0.00644 0.00523 AFIX 43 H00G 2 0.604297 0.156412 0.459034 11.00000 -1.20000 AFIX 0 C00H 1 0.742087 0.305086 0.730096 11.00000 0.04572 0.03582 = 0.04580 0.00100 0.00526 -0.00305 AFIX 23 H00A 2 0.710465 0.289388 0.794622 11.00000 -1.20000 H00B 2 0.847818 0.301575 0.757653 11.00000 -1.20000 AFIX 0 C00I 1 1.143674 0.430712 1.028251 11.00000 0.05869 0.06464 = 0.04640 0.00143 0.01448 0.00198 AFIX 43 H00I 2 1.128385 0.440403 1.100878 11.00000 -1.20000 AFIX 0 C00J 1 0.600220 0.551147 0.639826 11.00000 0.06667 0.04014 = 0.04381 -0.00239 0.00856 0.00716 AFIX 43 H00J 2 0.669559 0.576955 0.629832 11.00000 -1.20000 AFIX 0 C00K 1 0.392552 0.473932 0.668311 11.00000 0.05048 0.07774 = 0.04671 0.00568 0.02161 0.01430 AFIX 43 H00K 2 0.322172 0.448525 0.677785 11.00000 -1.20000 AFIX 0 C00L 1 1.284237 0.429630 1.025332 11.00000 0.04528 0.07373 = 0.05058 0.00799 -0.00262 -0.00299 AFIX 43 H00L 2 1.365036 0.438296 1.095397 11.00000 -1.20000 AFIX 0 C00M 1 0.842432 0.072766 0.656116 11.00000 0.05107 0.03999 = 0.06909 0.00464 0.02486 0.01034 AFIX 43 H00M 2 0.878643 0.034157 0.666686 11.00000 -1.20000 AFIX 0 C00N 1 0.844769 0.171471 0.732745 11.00000 0.05757 0.04064 = 0.05822 -0.00268 -0.00071 0.00361 AFIX 43 H00N 2 0.882117 0.198925 0.796230 11.00000 -1.20000 AFIX 0 C00O 1 1.299932 0.415513 0.916889 11.00000 0.03533 0.07750 = 0.06296 0.00848 0.00857 0.00156 AFIX 43 H00O 2 1.394323 0.414885 0.914965 11.00000 -1.20000 AFIX 0 C00P 1 0.730566 0.088509 0.548523 11.00000 0.05859 0.04171 = 0.06862 -0.00978 0.01468 0.00346 AFIX 43 H00P 2 0.690557 0.060372 0.486909 11.00000 -1.20000 AFIX 0 C00Q 1 0.361040 0.532987 0.643852 11.00000 0.06244 0.07963 = 0.05199 0.00570 0.02143 0.03295 AFIX 43 H00Q 2 0.268912 0.547200 0.636509 11.00000 -1.20000 AFIX 0 C00R 1 0.899852 0.114064 0.747084 11.00000 0.05316 0.05133 = 0.06041 0.00874 0.00415 0.01210 AFIX 43 H00R 2 0.976277 0.103611 0.818990 11.00000 -1.20000 AFIX 0 C00S 1 0.464994 0.572162 0.629779 11.00000 0.08177 0.05450 = 0.04745 0.00013 0.01533 0.02986 AFIX 43 H00S 2 0.442489 0.612164 0.613726 11.00000 -1.20000 AFIX 0 C00T 1 0.969328 0.384210 0.590354 11.00000 0.05207 0.07595 = 0.05222 -0.01409 0.01761 -0.00030 AFIX 137 H00C 2 0.888301 0.364944 0.528882 11.00000 -1.50000 H00F 2 1.057252 0.361983 0.602591 11.00000 -1.50000 H00H 2 0.980228 0.423644 0.563234 11.00000 -1.50000 AFIX 0 C00U 1 0.421272 0.224707 0.650382 11.00000 0.05090 0.10497 = 0.07868 0.02669 0.00820 -0.00413 AFIX 43 H00U 2 0.489358 0.208421 0.721404 11.00000 -1.20000 AFIX 0 C00V 1 0.172641 0.242478 0.528508 11.00000 0.04426 0.09846 = 0.10880 -0.00872 0.01259 0.00159 AFIX 43 H00V 2 0.073362 0.239329 0.515628 11.00000 -1.20000 AFIX 0 C00W 1 0.273537 0.218955 0.629533 11.00000 0.06391 0.12184 = 0.09366 0.00948 0.02778 -0.01329 AFIX 43 H00W 2 0.243596 0.198499 0.686295 11.00000 -1.20000 AFIX 0 C00X 1 0.366233 0.276751 0.465291 11.00000 0.05249 0.15938 = 0.09015 0.05328 0.00251 0.01251 AFIX 43 H00X 2 0.395703 0.296488 0.407430 11.00000 -1.20000 AFIX 0 C00Y 1 0.218771 0.270899 0.445789 11.00000 0.04959 0.22120 = 0.12287 0.06949 -0.00716 0.01789 AFIX 43 H00Y 2 0.150056 0.286763 0.374602 11.00000 -1.20000 AFIX 0 HKLF 4 REM cd-meh-hl-rmc87b_a.res in P2(1)/c REM R1 = 0.0618 for 3742 Fo > 4sig(Fo) and 0.0710 for all 4561 data REM 308 parameters refined using 0 restraints END WGHT 0.1219 0.3631 REM Highest difference peak 0.329, deepest hole -0.399, 1-sigma level 0.067 Q1 1 0.6896 0.2208 0.6052 11.00000 0.05 0.33 Q2 1 0.7268 0.2806 0.6700 11.00000 0.05 0.29 Q3 1 0.5643 0.2630 0.5904 11.00000 0.05 0.23 Q4 1 0.6597 0.1575 0.5987 11.00000 0.05 0.23 Q5 1 0.6051 0.2822 0.4990 11.00000 0.05 0.22 Q6 1 0.6471 0.3797 0.7629 11.00000 0.05 0.22 Q7 1 0.6042 0.2961 0.3982 11.00000 0.05 0.21 Q8 1 0.8474 0.1859 0.6614 11.00000 0.05 0.20 Q9 1 0.4255 0.5504 0.6339 11.00000 0.05 0.20 Q10 1 0.7268 0.3316 0.7158 11.00000 0.05 0.19 Q11 1 0.7771 0.3185 0.5069 11.00000 0.05 0.19 Q12 1 0.2313 0.2822 0.5165 11.00000 0.05 0.19 Q13 1 0.7558 0.1802 0.6819 11.00000 0.05 0.19 Q14 1 0.4154 0.2877 0.5270 11.00000 0.05 0.19 Q15 1 0.6325 0.5354 0.6830 11.00000 0.05 0.19 Q16 1 0.9446 0.1332 0.6944 11.00000 0.05 0.19 Q17 1 0.7771 0.2883 0.8004 11.00000 0.05 0.18 Q18 1 0.5810 0.3196 0.4354 11.00000 0.05 0.18 Q19 1 0.4432 0.6569 0.5053 11.00000 0.05 0.18 Q20 1 1.0595 0.5063 0.9974 11.00000 0.05 0.18 ; _shelx_res_checksum 51696 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 P01 P 0.65953(6) 0.26168(2) 0.58919(5) 0.0425(2) Uani 1 1 d . . O002 O 0.87832(18) 0.50172(8) 0.66828(18) 0.0578(5) Uani 1 1 d . . O003 O 0.6797(2) 0.28743(8) 0.47854(16) 0.0575(4) Uani 1 1 d . . N004 N 0.80339(18) 0.40899(8) 0.69488(16) 0.0395(4) Uani 1 1 d . . N005 N 0.94219(18) 0.38735(9) 0.70679(17) 0.0444(4) Uani 1 1 d . . N006 N 1.1894(2) 0.40240(10) 0.81227(19) 0.0518(5) Uani 1 1 d . . C007 C 1.0554(2) 0.40363(9) 0.8160(2) 0.0407(5) Uani 1 1 d . . C008 C 0.6349(2) 0.49109(10) 0.66504(18) 0.0418(5) Uani 1 1 d . . C009 C 0.7802(2) 0.46997(10) 0.67477(19) 0.0422(5) Uani 1 1 d . . C00A C 0.7346(2) 0.18806(9) 0.6245(2) 0.0412(5) Uani 1 1 d . . C00B C 0.5314(2) 0.45170(10) 0.67911(18) 0.0423(5) Uani 1 1 d . . C00C C 0.6998(2) 0.36923(9) 0.70899(18) 0.0391(4) Uani 1 1 d . . C00D C 0.5680(2) 0.39044(10) 0.70199(19) 0.0433(5) Uani 1 1 d . . H00D H 0.4992 0.3645 0.7124 0.052 Uiso 1 1 calc R U C00E C 1.0275(2) 0.41741(11) 0.9235(2) 0.0487(5) Uani 1 1 d . . H00E H 0.9323 0.4175 0.9237 0.058 Uiso 1 1 calc R U C00F C 0.4684(3) 0.25376(10) 0.5687(2) 0.0491(5) Uani 1 1 d . . C00G C 0.6782(3) 0.14585(11) 0.5324(2) 0.0530(6) Uani 1 1 d . . H00G H 0.6043 0.1564 0.4590 0.064 Uiso 1 1 calc R U C00H C 0.7421(2) 0.30509(10) 0.7301(2) 0.0454(5) Uani 1 1 d . . H00A H 0.7105 0.2894 0.7946 0.054 Uiso 1 1 calc R U H00B H 0.8478 0.3016 0.7577 0.054 Uiso 1 1 calc R U C00I C 1.1437(3) 0.43071(13) 1.0283(2) 0.0577(6) Uani 1 1 d . . H00I H 1.1284 0.4404 1.1009 0.069 Uiso 1 1 calc R U C00J C 0.6002(3) 0.55115(11) 0.6398(2) 0.0532(6) Uani 1 1 d . . H00J H 0.6696 0.5770 0.6298 0.064 Uiso 1 1 calc R U C00K C 0.3926(3) 0.47393(14) 0.6683(2) 0.0571(6) Uani 1 1 d . . H00K H 0.3222 0.4485 0.6778 0.069 Uiso 1 1 calc R U C00L C 1.2842(3) 0.42963(14) 1.0253(2) 0.0618(7) Uani 1 1 d . . H00L H 1.3650 0.4383 1.0954 0.074 Uiso 1 1 calc R U C00M C 0.8424(3) 0.07277(11) 0.6561(2) 0.0524(6) Uani 1 1 d . . H00M H 0.8786 0.0342 0.6667 0.063 Uiso 1 1 calc R U C00N C 0.8448(3) 0.17147(11) 0.7327(2) 0.0579(6) Uani 1 1 d . . H00N H 0.8821 0.1989 0.7962 0.069 Uiso 1 1 calc R U C00O C 1.2999(3) 0.41551(14) 0.9169(3) 0.0610(7) Uani 1 1 d . . H00O H 1.3943 0.4149 0.9150 0.073 Uiso 1 1 calc R U C00P C 0.7306(3) 0.08851(12) 0.5485(3) 0.0584(6) Uani 1 1 d . . H00P H 0.6906 0.0604 0.4869 0.070 Uiso 1 1 calc R U C00Q C 0.3610(3) 0.53299(15) 0.6439(2) 0.0644(7) Uani 1 1 d . . H00Q H 0.2689 0.5472 0.6365 0.077 Uiso 1 1 calc R U C00R C 0.8999(3) 0.11406(12) 0.7471(3) 0.0593(6) Uani 1 1 d . . H00R H 0.9763 0.1036 0.8190 0.071 Uiso 1 1 calc R U C00S C 0.4650(3) 0.57216(13) 0.6298(2) 0.0633(7) Uani 1 1 d . . H00S H 0.4425 0.6122 0.6137 0.076 Uiso 1 1 calc R U C00T C 0.9693(3) 0.38421(14) 0.5904(2) 0.0603(7) Uani 1 1 d . . H00C H 0.8883 0.3649 0.5289 0.090 Uiso 1 1 calc R U H00F H 1.0573 0.3620 0.6026 0.090 Uiso 1 1 calc R U H00H H 0.9802 0.4236 0.5632 0.090 Uiso 1 1 calc R U C00U C 0.4213(3) 0.22471(19) 0.6504(3) 0.0822(10) Uani 1 1 d . . H00U H 0.4894 0.2084 0.7214 0.099 Uiso 1 1 calc R U C00V C 0.1726(3) 0.24248(19) 0.5285(4) 0.0878(11) Uani 1 1 d . . H00V H 0.0734 0.2393 0.5156 0.105 Uiso 1 1 calc R U C00W C 0.2735(4) 0.2190(2) 0.6295(4) 0.0932(12) Uani 1 1 d . . H00W H 0.2436 0.1985 0.6863 0.112 Uiso 1 1 calc R U C00X C 0.3662(4) 0.2768(3) 0.4653(4) 0.1068(16) Uani 1 1 d . . H00X H 0.3957 0.2965 0.4074 0.128 Uiso 1 1 calc R U C00Y C 0.2188(4) 0.2709(3) 0.4458(5) 0.141(2) Uani 1 1 d . . H00Y H 0.1501 0.2868 0.3746 0.170 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 P01 0.0439(3) 0.0307(3) 0.0434(3) 0.00150(19) 0.0038(2) 0.0003(2) O002 0.0470(9) 0.0434(9) 0.0762(11) 0.0018(8) 0.0134(8) -0.0131(7) O003 0.0682(11) 0.0459(9) 0.0516(9) 0.0073(7) 0.0129(8) 0.0018(8) N004 0.0312(8) 0.0355(9) 0.0471(9) -0.0040(7) 0.0082(7) -0.0007(7) N005 0.0339(8) 0.0465(10) 0.0491(10) -0.0070(8) 0.0103(7) 0.0011(7) N006 0.0374(9) 0.0633(13) 0.0532(11) 0.0050(9) 0.0142(8) 0.0042(8) C007 0.0350(10) 0.0353(10) 0.0488(11) 0.0022(8) 0.0111(9) 0.0010(8) C008 0.0443(11) 0.0397(11) 0.0350(10) -0.0058(8) 0.0060(8) 0.0019(9) C009 0.0413(10) 0.0347(10) 0.0432(10) -0.0048(8) 0.0057(8) -0.0054(8) C00A 0.0378(10) 0.0342(10) 0.0478(11) 0.0020(8) 0.0106(9) -0.0004(8) C00B 0.0431(11) 0.0483(12) 0.0321(9) -0.0018(8) 0.0091(8) 0.0060(9) C00C 0.0394(10) 0.0345(10) 0.0387(10) -0.0024(8) 0.0080(8) -0.0042(8) C00D 0.0394(10) 0.0453(12) 0.0428(11) 0.0004(8) 0.0117(9) -0.0057(9) C00E 0.0408(11) 0.0537(13) 0.0510(12) -0.0014(10) 0.0156(9) 0.0010(10) C00F 0.0441(11) 0.0378(11) 0.0534(13) -0.0020(9) 0.0025(10) 0.0019(9) C00G 0.0496(12) 0.0467(13) 0.0533(13) -0.0014(10) 0.0064(10) 0.0052(10) C00H 0.0457(11) 0.0358(11) 0.0458(11) 0.0010(8) 0.0053(9) -0.0030(9) C00I 0.0587(14) 0.0646(16) 0.0464(12) 0.0014(11) 0.0145(11) 0.0020(12) C00J 0.0667(14) 0.0401(12) 0.0438(11) -0.0024(9) 0.0086(11) 0.0072(11) C00K 0.0505(13) 0.0777(18) 0.0467(12) 0.0057(11) 0.0216(10) 0.0143(12) C00L 0.0453(12) 0.0737(18) 0.0506(13) 0.0080(12) -0.0026(11) -0.0030(12) C00M 0.0511(12) 0.0400(12) 0.0691(15) 0.0046(10) 0.0249(11) 0.0103(10) C00N 0.0576(13) 0.0406(12) 0.0582(14) -0.0027(10) -0.0007(11) 0.0036(11) C00O 0.0353(11) 0.0775(19) 0.0630(15) 0.0085(13) 0.0086(10) 0.0016(11) C00P 0.0586(14) 0.0417(13) 0.0686(15) -0.0098(11) 0.0147(12) 0.0035(11) C00Q 0.0624(15) 0.0796(19) 0.0520(13) 0.0057(12) 0.0214(12) 0.0329(14) C00R 0.0532(13) 0.0513(14) 0.0604(14) 0.0087(11) 0.0041(11) 0.0121(11) C00S 0.0818(18) 0.0545(15) 0.0474(13) 0.0001(11) 0.0153(13) 0.0299(14) C00T 0.0521(13) 0.0760(18) 0.0522(13) -0.0141(12) 0.0176(11) -0.0003(13) C00U 0.0509(15) 0.105(3) 0.079(2) 0.0267(19) 0.0082(14) -0.0041(16) C00V 0.0443(14) 0.098(3) 0.109(3) -0.009(2) 0.0126(17) 0.0016(15) C00W 0.0639(19) 0.122(3) 0.094(3) 0.009(2) 0.0278(18) -0.013(2) C00X 0.0525(17) 0.159(4) 0.090(3) 0.053(3) 0.0025(17) 0.013(2) C00Y 0.0496(18) 0.221(7) 0.123(4) 0.069(4) -0.007(2) 0.018(3) 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' P P 0.2955 0.4335 '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 O003 P01 C00A 112.86(11) O003 P01 C00F 111.93(11) C00A P01 C00F 104.95(10) O003 P01 C00H 114.26(11) C00A P01 C00H 105.93(10) C00F P01 C00H 106.21(11) C009 N004 N005 116.91(17) C009 N004 C00C 124.40(18) N005 N004 C00C 118.64(17) N004 N005 C007 115.15(17) N004 N005 C00T 114.24(18) C007 N005 C00T 120.00(18) C007 N006 C00O 117.1(2) N006 C007 C00E 122.6(2) N006 C007 N005 116.0(2) C00E C007 N005 121.28(19) C00B C008 C00J 120.4(2) C00B C008 C009 120.5(2) C00J C008 C009 119.1(2) O002 C009 N004 120.1(2) O002 C009 C008 124.6(2) N004 C009 C008 115.34(19) C00N C00A C00G 118.7(2) C00N C00A P01 125.33(18) C00G C00A P01 115.94(16) C008 C00B C00K 118.5(2) C008 C00B C00D 119.48(19) C00K C00B C00D 122.0(2) C00D C00C N004 118.65(19) C00D C00C C00H 123.6(2) N004 C00C C00H 117.73(18) C00C C00D C00B 121.7(2) C00C C00D H00D 119.2 C00B C00D H00D 119.2 C00I C00E C007 118.3(2) C00I C00E H00E 120.8 C007 C00E H00E 120.8 C00U C00F C00X 118.2(3) C00U C00F P01 123.1(2) C00X C00F P01 118.7(3) C00P C00G C00A 120.7(2) C00P C00G H00G 119.6 C00A C00G H00G 119.6 C00C C00H P01 111.18(15) C00C C00H H00A 109.4 P01 C00H H00A 109.4 C00C C00H H00B 109.4 P01 C00H H00B 109.4 H00A C00H H00B 108.0 C00E C00I C00L 119.5(2) C00E C00I H00I 120.2 C00L C00I H00I 120.2 C00S C00J C008 120.4(3) C00S C00J H00J 119.8 C008 C00J H00J 119.8 C00Q C00K C00B 120.1(3) C00Q C00K H00K 120.0 C00B C00K H00K 120.0 C00O C00L C00I 117.7(2) C00O C00L H00L 121.2 C00I C00L H00L 121.2 C00R C00M C00P 119.8(2) C00R C00M H00M 120.1 C00P C00M H00M 120.1 C00A C00N C00R 120.3(2) C00A C00N H00N 119.8 C00R C00N H00N 119.8 N006 C00O C00L 124.7(2) N006 C00O H00O 117.6 C00L C00O H00O 117.6 C00G C00P C00M 120.0(2) C00G C00P H00P 120.0 C00M C00P H00P 120.0 C00K C00Q C00S 121.1(2) C00K C00Q H00Q 119.4 C00S C00Q H00Q 119.4 C00M C00R C00N 120.4(2) C00M C00R H00R 119.8 C00N C00R H00R 119.8 C00J C00S C00Q 119.4(2) C00J C00S H00S 120.3 C00Q C00S H00S 120.3 N005 C00T H00C 109.5 N005 C00T H00F 109.5 H00C C00T H00F 109.5 N005 C00T H00H 109.5 H00C C00T H00H 109.5 H00F C00T H00H 109.5 C00F C00U C00W 120.9(3) C00F C00U H00U 119.5 C00W C00U H00U 119.5 C00W C00V C00Y 118.5(3) C00W C00V H00V 120.8 C00Y C00V H00V 120.8 C00V C00W C00U 120.9(4) C00V C00W H00W 119.5 C00U C00W H00W 119.5 C00F C00X C00Y 120.3(4) C00F C00X H00X 119.9 C00Y C00X H00X 119.9 C00V C00Y C00X 121.2(4) C00V C00Y H00Y 119.4 C00X C00Y H00Y 119.4 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance P01 O003 1.4808(18) P01 C00A 1.800(2) P01 C00F 1.805(3) P01 C00H 1.825(2) O002 C009 1.219(3) N004 C009 1.397(3) N004 N005 1.401(2) N004 C00C 1.403(3) N005 C007 1.401(3) N005 C00T 1.464(3) N006 C007 1.324(3) N006 C00O 1.339(3) C007 C00E 1.399(3) C008 C00B 1.396(3) C008 C00J 1.399(3) C008 C009 1.462(3) C00A C00N 1.382(3) C00A C00G 1.388(3) C00B C00K 1.409(3) C00B C00D 1.426(3) C00C C00D 1.348(3) C00C C00H 1.498(3) C00D H00D 0.9300 C00E C00I 1.369(4) C00E H00E 0.9300 C00F C00U 1.356(4) C00F C00X 1.360(4) C00G C00P 1.376(4) C00G H00G 0.9300 C00H H00A 0.9700 C00H H00B 0.9700 C00I C00L 1.385(4) C00I H00I 0.9300 C00J C00S 1.368(4) C00J H00J 0.9300 C00K C00Q 1.371(4) C00K H00K 0.9300 C00L C00O 1.355(4) C00L H00L 0.9300 C00M C00R 1.367(4) C00M C00P 1.381(4) C00M H00M 0.9300 C00N C00R 1.387(4) C00N H00N 0.9300 C00O H00O 0.9300 C00P H00P 0.9300 C00Q C00S 1.397(5) C00Q H00Q 0.9300 C00R H00R 0.9300 C00S H00S 0.9300 C00T H00C 0.9600 C00T H00F 0.9600 C00T H00H 0.9600 C00U C00W 1.382(5) C00U H00U 0.9300 C00V C00W 1.342(6) C00V C00Y 1.354(7) C00V H00V 0.9300 C00W H00W 0.9300 C00X C00Y 1.383(6) C00X H00X 0.9300 C00Y H00Y 0.9300