#------------------------------------------------------------------------------ #$Date: 2020-08-29 04:40:53 +0300 (Sat, 29 Aug 2020) $ #$Revision: 255724 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705296.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_7705296 loop_ _publ_author_name 'Exp\'osito, J. Emilio' 'Aull\'on, Gabriel' 'Bardaji, Manuel' 'Miguel, Jesus Angel' 'Espinet, Pablo' _publ_section_title ; Fluorescent perylenylpyridine complexes: an experimental and theoretical study ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02494E _journal_year 2020 _chemical_formula_moiety 'C44 H32 Ag Cl N O4 P' _chemical_formula_sum 'C44 H32 Ag Cl N O4 P' _chemical_formula_weight 812.99 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_date 2020-08-06 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-08-08 deposited with the CCDC. 2020-08-28 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 109.521(14) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 18.675(2) _cell_length_b 10.7526(12) _cell_length_c 19.190(3) _cell_measurement_reflns_used 4776 _cell_measurement_temperature 293 _cell_measurement_theta_max 28.8249 _cell_measurement_theta_min 2.1564 _cell_volume 3631.9(9) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve (Bourhis et al., 2015)' _diffrn_ambient_temperature 293 _diffrn_detector_area_resol_mean 10.4757 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.836 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -29.00 42.00 1.0000 94.2400 omega____ theta____ kappa____ phi______ frames - -10.5095 77.0000 30.0000 71 #__ type_ start__ end____ width___ exp.time_ 2 omega -43.00 59.00 1.0000 94.2400 omega____ theta____ kappa____ phi______ frames - -10.5095 77.0000 150.0000 102 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0309924000 _diffrn_orient_matrix_UB_12 -0.0358899000 _diffrn_orient_matrix_UB_13 0.0021658000 _diffrn_orient_matrix_UB_21 0.0229694000 _diffrn_orient_matrix_UB_22 -0.0230772000 _diffrn_orient_matrix_UB_23 0.0350130000 _diffrn_orient_matrix_UB_31 -0.0116488000 _diffrn_orient_matrix_UB_32 0.0500764000 _diffrn_orient_matrix_UB_33 0.0177739000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_unetI/netI 0.0548 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.836 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 15923 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.836 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.889 _diffrn_reflns_theta_min 2.203 _diffrn_source 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.718 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_correction_T_min 0.947 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.487 _exptl_crystal_description prism _exptl_crystal_F_000 1656 _exptl_crystal_preparation 293 _exptl_crystal_recrystallization_method 293 _exptl_crystal_size_max 0.2692 _exptl_crystal_size_mid 0.1184 _exptl_crystal_size_min 0.0667 _refine_diff_density_max 0.475 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.054 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 498 _refine_ls_number_reflns 7991 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.018 _refine_ls_R_factor_all 0.0960 _refine_ls_R_factor_gt 0.0488 _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^)+(0.0423P)^2^+0.8824P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0961 _refine_ls_wR_factor_ref 0.1146 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4797 _reflns_number_total 7991 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02494e2.cif _cod_data_source_block 2 _cod_original_cell_volume 3632.0(8) _cod_database_code 7705296 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C43 H32 N Ag P' _chemical_oxdiff_usercomment 'yellow prism' _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. ; _reflns_odcompleteness_completeness 99.67 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 25.63 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Others Sof(O1A)=Sof(O2A)=Sof(O4A)=1-FVAR(1) Sof(O1)=Sof(O2)=Sof(O4)=FVAR(1) 3.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C7(H7), C8(H8), C9(H9), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C22(H22), C24(H24), C25(H25), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44) 3.b Idealised Me refined as rotating group: C26(H26A,H26B,H26C) ; _shelx_res_file ; TITL je272_a.res in P2(1)/n je272.res created by SHELXL-2018/3 at 12:51:19 on 06-Aug-2020 REM Old TITL JE272 in P21/n #14 REM SHELXT solution in P2(1)/n REM R1 0.267, Rweak 0.031, Alpha 0.042, Orientation as input REM Formula found by SHELXT: C43 N5 P2 Ag CELL 0.71073 18.675 10.7526 19.1904 90 109.521 90 ZERR 4 0.0024 0.0012 0.0025 0 0.014 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Ag Cl N O P UNIT 176 128 4 4 4 16 4 L.S. 40 PLAN 10 TEMP 19.85 BIND O1 Ag1 BOND $H LIST 6 fmap 2 53 acta REM REM REM WGHT 0.042300 0.882400 FVAR 0.31297 0.60634 AG1 3 0.377422 0.607412 0.516780 11.00000 0.04915 0.05783 = 0.08410 -0.02091 -0.00846 -0.00162 CL1 4 0.519035 0.388410 0.643078 11.00000 0.06956 0.05618 = 0.05731 -0.00105 0.00826 0.01670 P1 7 0.258064 0.511019 0.458624 11.00000 0.04420 0.04219 = 0.04769 -0.00445 -0.00356 0.00426 PART 1 O1 6 0.498166 0.474585 0.583549 21.00000 0.09113 0.07426 = 0.07180 0.02000 -0.00071 0.00265 O2 6 0.458838 0.307153 0.633555 21.00000 0.13666 0.16109 = 0.12320 0.01793 0.02857 -0.06140 PART 0 O3 6 0.542779 0.460247 0.707820 11.00000 0.11737 0.13636 = 0.07564 -0.04379 0.00443 0.02948 PART 1 O4 6 0.580204 0.325511 0.635841 21.00000 0.13801 0.12926 = 0.16555 -0.03260 -0.00918 0.10193 PART 0 N1 5 0.463629 0.756815 0.556980 11.00000 0.04826 0.04883 = 0.05326 -0.01079 0.00240 0.00057 C1 1 0.374054 0.868595 0.603709 11.00000 0.06635 0.04772 = 0.05156 -0.01239 0.01437 -0.00685 C2 1 0.327674 0.970904 0.576221 11.00000 0.05645 0.04677 = 0.07823 -0.00518 0.02056 0.00771 AFIX 43 H2 2 0.344534 1.035802 0.553648 11.00000 -1.20000 AFIX 0 C3 1 0.254690 0.975200 0.582951 11.00000 0.06825 0.05847 = 0.08142 -0.00504 0.01661 0.01833 AFIX 43 H3 2 0.224289 1.044434 0.564935 11.00000 -1.20000 AFIX 0 C4 1 0.226928 0.881536 0.614927 11.00000 0.06821 0.05325 = 0.04618 -0.01600 0.01740 -0.01492 C5 1 0.274599 0.777292 0.646575 11.00000 0.04211 0.06202 = 0.04232 -0.02180 0.00215 0.00573 C6 1 0.350634 0.773499 0.641194 11.00000 0.06359 0.04729 = 0.04594 -0.01188 -0.00170 0.00751 C7 1 0.397873 0.674838 0.675250 11.00000 0.04767 0.05192 = 0.05084 -0.00399 0.00281 0.00563 AFIX 43 H7 2 0.446856 0.671012 0.673137 11.00000 -1.20000 AFIX 0 C8 1 0.373500 0.583543 0.711720 11.00000 0.07045 0.06798 = 0.06312 0.00446 0.00672 0.01144 AFIX 43 H8 2 0.406178 0.519360 0.734873 11.00000 -1.20000 AFIX 0 C9 1 0.299173 0.586653 0.714232 11.00000 0.07961 0.06308 = 0.06060 0.00154 0.01076 0.00278 AFIX 43 H9 2 0.283005 0.522839 0.738132 11.00000 -1.20000 AFIX 0 C10 1 0.249655 0.681606 0.682269 11.00000 0.06480 0.05701 = 0.03986 -0.00681 0.00602 0.00221 C11 1 0.173261 0.683557 0.685066 11.00000 0.06810 0.06975 = 0.03992 -0.01342 0.01519 -0.00189 C12 1 0.124501 0.783233 0.653458 11.00000 0.05195 0.07014 = 0.04352 -0.01571 0.01332 -0.00266 C13 1 0.147512 0.883356 0.618021 11.00000 0.05851 0.05779 = 0.04550 -0.01337 0.00649 0.01289 C14 1 0.098978 0.979197 0.589106 11.00000 0.07101 0.08340 = 0.07413 -0.00477 0.02035 0.02251 AFIX 43 H14 2 0.115082 1.044702 0.566357 11.00000 -1.20000 AFIX 0 C15 1 0.026811 0.981281 0.592788 11.00000 0.07193 0.11386 = 0.09460 -0.00665 0.02859 0.02403 AFIX 43 H15 2 -0.004638 1.048355 0.572360 11.00000 -1.20000 AFIX 0 C16 1 0.000136 0.889688 0.624906 11.00000 0.04975 0.12044 = 0.08321 -0.02071 0.02235 0.01088 AFIX 43 H16 2 -0.048952 0.893528 0.626742 11.00000 -1.20000 AFIX 0 C17 1 0.047980 0.786584 0.656124 11.00000 0.07797 0.09913 = 0.05877 -0.02088 0.03120 -0.01687 C18 1 0.023868 0.692343 0.690245 11.00000 0.08564 0.13559 = 0.08653 -0.01545 0.03551 -0.00897 AFIX 43 H18 2 -0.024995 0.694450 0.692757 11.00000 -1.20000 AFIX 0 C19 1 0.069806 0.596565 0.720252 11.00000 0.08505 0.11490 = 0.09022 0.00284 0.04180 -0.02007 AFIX 43 H19 2 0.051449 0.533386 0.742777 11.00000 -1.20000 AFIX 0 C20 1 0.143815 0.587600 0.719149 11.00000 0.09311 0.08630 = 0.06228 -0.00415 0.01770 -0.00240 AFIX 43 H20 2 0.173845 0.519503 0.740493 11.00000 -1.20000 AFIX 0 C21 1 0.449845 0.859938 0.591105 11.00000 0.04793 0.05293 = 0.04618 -0.00769 0.00942 -0.00110 C22 1 0.501871 0.955556 0.611495 11.00000 0.05456 0.04657 = 0.05479 -0.00807 0.01284 -0.00218 AFIX 43 H22 2 0.490765 1.026095 0.634010 11.00000 -1.20000 AFIX 0 C23 1 0.570646 0.947671 0.598778 11.00000 0.04831 0.04575 = 0.05847 0.00285 0.00797 0.00032 C24 1 0.583835 0.840723 0.564557 11.00000 0.04627 0.05679 = 0.06389 0.00178 0.01462 0.00744 AFIX 43 H24 2 0.629194 0.830962 0.555063 11.00000 -1.20000 AFIX 0 C25 1 0.529960 0.750293 0.545003 11.00000 0.05100 0.05110 = 0.05717 -0.01155 0.00780 0.00890 AFIX 43 H25 2 0.539893 0.679562 0.521872 11.00000 -1.20000 AFIX 0 C26 1 0.629277 1.048455 0.622154 11.00000 0.06466 0.05837 = 0.11424 -0.00390 0.02668 -0.00915 AFIX 137 H26A 2 0.604506 1.127750 0.617600 11.00000 -1.50000 H26B 2 0.660365 1.046748 0.591172 11.00000 -1.50000 H26C 2 0.660514 1.035421 0.672664 11.00000 -1.50000 AFIX 0 C27 1 0.254480 0.393345 0.389993 11.00000 0.04132 0.04534 = 0.05085 -0.00577 -0.00301 0.00857 C28 1 0.296942 0.412137 0.344030 11.00000 0.06470 0.06195 = 0.06369 0.00407 0.01290 0.01156 AFIX 43 H28 2 0.328927 0.480753 0.351303 11.00000 -1.20000 AFIX 0 C29 1 0.292126 0.328906 0.286860 11.00000 0.08968 0.09934 = 0.06604 0.00277 0.02824 0.02741 AFIX 43 H29 2 0.320489 0.342050 0.255866 11.00000 -1.20000 AFIX 0 C30 1 0.245718 0.228693 0.276907 11.00000 0.08611 0.08611 = 0.07012 -0.02372 0.00207 0.02504 AFIX 43 H30 2 0.242289 0.173392 0.238664 11.00000 -1.20000 AFIX 0 C31 1 0.204306 0.207782 0.321681 11.00000 0.05999 0.07112 = 0.09749 -0.03390 0.00298 -0.00223 AFIX 43 H31 2 0.172961 0.138312 0.314103 11.00000 -1.20000 AFIX 0 C32 1 0.208379 0.289382 0.378764 11.00000 0.05325 0.06031 = 0.07358 -0.02098 0.01045 -0.00066 AFIX 43 H32 2 0.180066 0.274224 0.409583 11.00000 -1.20000 AFIX 0 C33 1 0.188440 0.624512 0.407799 11.00000 0.04447 0.04470 = 0.04246 0.00087 0.00776 0.00379 C34 1 0.128951 0.597584 0.344160 11.00000 0.05924 0.05195 = 0.06495 -0.00986 -0.00914 0.00759 AFIX 43 H34 2 0.124196 0.517818 0.324394 11.00000 -1.20000 AFIX 0 C35 1 0.076497 0.687326 0.309511 11.00000 0.06943 0.07042 = 0.06099 0.00364 -0.01573 0.01320 AFIX 43 H35 2 0.035823 0.667025 0.267520 11.00000 -1.20000 AFIX 0 C36 1 0.083832 0.805396 0.336331 11.00000 0.07063 0.07044 = 0.06096 0.00874 0.00537 0.02773 AFIX 43 H36 2 0.048494 0.865906 0.312655 11.00000 -1.20000 AFIX 0 C37 1 0.143243 0.834513 0.398078 11.00000 0.09158 0.05768 = 0.08162 -0.01341 0.00282 0.02890 AFIX 43 H37 2 0.148663 0.915243 0.416505 11.00000 -1.20000 AFIX 0 C38 1 0.195368 0.744567 0.433325 11.00000 0.06740 0.05894 = 0.06010 -0.01275 -0.00791 0.01741 AFIX 43 H38 2 0.235977 0.765691 0.475185 11.00000 -1.20000 AFIX 0 C39 1 0.215551 0.437084 0.520385 11.00000 0.09081 0.04321 = 0.04152 -0.00144 0.00689 0.00233 C40 1 0.261535 0.364691 0.577558 11.00000 0.14397 0.06092 = 0.05518 0.00422 -0.00177 0.00453 AFIX 43 H40 2 0.313130 0.357298 0.584749 11.00000 -1.20000 AFIX 0 C41 1 0.229703 0.302361 0.624724 11.00000 0.22701 0.06637 = 0.05461 0.01362 0.01665 -0.00341 AFIX 43 H41 2 0.260043 0.252190 0.662588 11.00000 -1.20000 AFIX 0 C42 1 0.156573 0.315244 0.615120 11.00000 0.28265 0.08566 = 0.09987 -0.00027 0.09928 -0.03144 AFIX 43 H42 2 0.136492 0.275160 0.647383 11.00000 -1.20000 AFIX 0 C43 1 0.110431 0.384693 0.560001 11.00000 0.16797 0.12615 = 0.13427 0.02316 0.08838 -0.01378 AFIX 43 H43 2 0.058993 0.390974 0.553774 11.00000 -1.20000 AFIX 0 C44 1 0.140173 0.446796 0.512577 11.00000 0.11134 0.10124 = 0.08792 0.02487 0.04992 0.00303 AFIX 43 H44 2 0.108460 0.495786 0.474897 11.00000 -1.20000 AFIX 0 PART 2 O1A 6 0.451665 0.427543 0.591674 -21.00000 0.11171 0.11492 = 0.10984 -0.03218 -0.03980 0.07680 O2A 6 0.509458 0.271145 0.669217 -21.00000 0.19525 0.07734 = 0.14149 0.02713 0.07309 -0.02224 O4A 6 0.578884 0.365766 0.614315 -21.00000 0.10310 0.18242 = 0.14730 -0.10355 0.10610 -0.08683 HKLF 4 REM je272_a.res in P2(1)/n REM wR2 = 0.1146, GooF = S = 1.018, Restrained GooF = 1.018 for all data REM R1 = 0.0488 for 4797 Fo > 4sig(Fo) and 0.0960 for all 7991 data REM 498 parameters refined using 0 restraints END WGHT 0.0423 0.8970 REM Highest difference peak 0.475, deepest hole -0.330, 1-sigma level 0.054 Q1 1 0.2573 1.0627 0.5399 11.00000 0.05 0.47 Q2 1 0.2020 1.0331 0.5572 11.00000 0.05 0.45 Q3 1 0.3333 0.6666 0.6823 11.00000 0.05 0.41 Q4 1 0.2042 0.5767 0.7194 11.00000 0.05 0.40 Q5 1 0.3206 0.8846 0.5989 11.00000 0.05 0.35 Q6 1 0.4044 0.7830 0.6226 11.00000 0.05 0.30 Q7 1 0.3973 0.6421 0.4865 11.00000 0.05 0.26 Q8 1 0.6188 1.0848 0.6652 11.00000 0.05 0.26 Q9 1 0.1860 0.9397 0.6079 11.00000 0.05 0.24 Q10 1 0.2890 0.2842 0.6213 11.00000 0.05 0.23 ; _shelx_res_checksum 69254 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 Ag1 Ag 0.37742(2) 0.60741(3) 0.51678(2) 0.07140(14) Uani 1 1 d . . . . . Cl1 Cl 0.51903(6) 0.38841(8) 0.64308(5) 0.0643(3) Uani 1 1 d . . . . . P1 P 0.25806(5) 0.51102(8) 0.45862(5) 0.0494(2) Uani 1 1 d . . . . . O1 O 0.4982(7) 0.4746(6) 0.5835(4) 0.086(3) Uani 0.61(2) 1 d . . P A 1 O2 O 0.4588(8) 0.3072(14) 0.6336(6) 0.144(5) Uani 0.61(2) 1 d . . P A 1 O3 O 0.5428(2) 0.4602(3) 0.70782(17) 0.1168(13) Uani 1 1 d . . . . . O4 O 0.5802(7) 0.3255(12) 0.6358(8) 0.159(7) Uani 0.61(2) 1 d . . P A 1 N1 N 0.46363(15) 0.7568(2) 0.55698(15) 0.0538(8) Uani 1 1 d . . . . . C1 C 0.3741(2) 0.8686(3) 0.60371(19) 0.0565(10) Uani 1 1 d . . . . . C2 C 0.3277(2) 0.9709(3) 0.5762(2) 0.0610(10) Uani 1 1 d . . . . . H2 H 0.344534 1.035802 0.553648 0.073 Uiso 1 1 calc R . . . . C3 C 0.2547(2) 0.9752(4) 0.5830(2) 0.0715(12) Uani 1 1 d . . . . . H3 H 0.224289 1.044434 0.564935 0.086 Uiso 1 1 calc R . . . . C4 C 0.2269(2) 0.8815(3) 0.61493(19) 0.0563(9) Uani 1 1 d . . . . . C5 C 0.27460(17) 0.7773(3) 0.64658(18) 0.0518(9) Uani 1 1 d . . . . . C6 C 0.3506(2) 0.7735(3) 0.64119(18) 0.0573(10) Uani 1 1 d . . . . . C7 C 0.39787(19) 0.6748(3) 0.67525(18) 0.0536(9) Uani 1 1 d . . . . . H7 H 0.446856 0.671012 0.673137 0.064 Uiso 1 1 calc R . . . . C8 C 0.3735(2) 0.5835(4) 0.7117(2) 0.0711(12) Uani 1 1 d . . . . . H8 H 0.406178 0.519360 0.734873 0.085 Uiso 1 1 calc R . . . . C9 C 0.2992(2) 0.5867(4) 0.7142(2) 0.0709(11) Uani 1 1 d . . . . . H9 H 0.283005 0.522839 0.738132 0.085 Uiso 1 1 calc R . . . . C10 C 0.2497(2) 0.6816(3) 0.68227(18) 0.0568(10) Uani 1 1 d . . . . . C11 C 0.1733(2) 0.6836(4) 0.68507(19) 0.0600(10) Uani 1 1 d . . . . . C12 C 0.12450(19) 0.7832(4) 0.65346(19) 0.0559(9) Uani 1 1 d . . . . . C13 C 0.1475(2) 0.8834(3) 0.61802(19) 0.0567(10) Uani 1 1 d . . . . . C14 C 0.0990(2) 0.9792(4) 0.5891(2) 0.0772(12) Uani 1 1 d . . . . . H14 H 0.115082 1.044702 0.566357 0.093 Uiso 1 1 calc R . . . . C15 C 0.0268(3) 0.9813(5) 0.5928(3) 0.0933(15) Uani 1 1 d . . . . . H15 H -0.004638 1.048355 0.572360 0.112 Uiso 1 1 calc R . . . . C16 C 0.0001(2) 0.8897(5) 0.6249(3) 0.0844(14) Uani 1 1 d . . . . . H16 H -0.048952 0.893528 0.626742 0.101 Uiso 1 1 calc R . . . . C17 C 0.0480(2) 0.7866(5) 0.6561(2) 0.0765(12) Uani 1 1 d . . . . . C18 C 0.0239(3) 0.6923(6) 0.6902(3) 0.1009(16) Uani 1 1 d . . . . . H18 H -0.024995 0.694450 0.692757 0.121 Uiso 1 1 calc R . . . . C19 C 0.0698(3) 0.5966(5) 0.7203(3) 0.0936(15) Uani 1 1 d . . . . . H19 H 0.051449 0.533386 0.742777 0.112 Uiso 1 1 calc R . . . . C20 C 0.1438(3) 0.5876(4) 0.7191(2) 0.0826(13) Uani 1 1 d . . . . . H20 H 0.173845 0.519503 0.740493 0.099 Uiso 1 1 calc R . . . . C21 C 0.44985(18) 0.8599(3) 0.59111(18) 0.0506(9) Uani 1 1 d . . . . . C22 C 0.50187(19) 0.9556(3) 0.61149(18) 0.0533(9) Uani 1 1 d . . . . . H22 H 0.490765 1.026095 0.634010 0.064 Uiso 1 1 calc R . . . . C23 C 0.57065(19) 0.9477(3) 0.59878(19) 0.0533(9) Uani 1 1 d . . . . . C24 C 0.58383(19) 0.8407(3) 0.56456(19) 0.0566(9) Uani 1 1 d . . . . . H24 H 0.629194 0.830962 0.555063 0.068 Uiso 1 1 calc R . . . . C25 C 0.52996(19) 0.7503(3) 0.54500(19) 0.0557(9) Uani 1 1 d . . . . . H25 H 0.539893 0.679562 0.521872 0.067 Uiso 1 1 calc R . . . . C26 C 0.6293(2) 1.0485(4) 0.6222(3) 0.0799(13) Uani 1 1 d . . . . . H26A H 0.604506 1.127750 0.617600 0.120 Uiso 1 1 calc GR . . . . H26B H 0.660365 1.046748 0.591172 0.120 Uiso 1 1 calc GR . . . . H26C H 0.660514 1.035421 0.672664 0.120 Uiso 1 1 calc GR . . . . C27 C 0.25448(18) 0.3933(3) 0.38999(19) 0.0505(9) Uani 1 1 d . . . . . C28 C 0.2969(2) 0.4121(3) 0.3440(2) 0.0656(11) Uani 1 1 d . . . . . H28 H 0.328927 0.480753 0.351303 0.079 Uiso 1 1 calc R . . . . C29 C 0.2921(3) 0.3289(5) 0.2869(2) 0.0845(13) Uani 1 1 d . . . . . H29 H 0.320489 0.342050 0.255866 0.101 Uiso 1 1 calc R . . . . C30 C 0.2457(3) 0.2287(5) 0.2769(3) 0.0868(15) Uani 1 1 d . . . . . H30 H 0.242289 0.173392 0.238664 0.104 Uiso 1 1 calc R . . . . C31 C 0.2043(2) 0.2078(4) 0.3217(3) 0.0821(14) Uani 1 1 d . . . . . H31 H 0.172961 0.138312 0.314103 0.098 Uiso 1 1 calc R . . . . C32 C 0.20838(19) 0.2894(3) 0.3788(2) 0.0651(11) Uani 1 1 d . . . . . H32 H 0.180066 0.274224 0.409583 0.078 Uiso 1 1 calc R . . . . C33 C 0.18844(17) 0.6245(3) 0.40780(17) 0.0456(8) Uani 1 1 d . . . . . C34 C 0.1290(2) 0.5976(3) 0.3442(2) 0.0662(11) Uani 1 1 d . . . . . H34 H 0.124196 0.517818 0.324394 0.079 Uiso 1 1 calc R . . . . C35 C 0.0765(2) 0.6873(4) 0.3095(2) 0.0764(13) Uani 1 1 d . . . . . H35 H 0.035823 0.667025 0.267520 0.092 Uiso 1 1 calc R . . . . C36 C 0.0838(2) 0.8054(4) 0.3363(2) 0.0715(12) Uani 1 1 d . . . . . H36 H 0.048494 0.865906 0.312655 0.086 Uiso 1 1 calc R . . . . C37 C 0.1432(2) 0.8345(4) 0.3981(2) 0.0835(14) Uani 1 1 d . . . . . H37 H 0.148663 0.915243 0.416505 0.100 Uiso 1 1 calc R . . . . C38 C 0.1954(2) 0.7446(3) 0.4333(2) 0.0695(12) Uani 1 1 d . . . . . H38 H 0.235977 0.765691 0.475185 0.083 Uiso 1 1 calc R . . . . C39 C 0.2156(2) 0.4371(3) 0.52038(19) 0.0623(11) Uani 1 1 d . . . . . C40 C 0.2615(3) 0.3647(4) 0.5776(2) 0.0955(17) Uani 1 1 d . . . . . H40 H 0.313130 0.357298 0.584749 0.115 Uiso 1 1 calc R . . . . C41 C 0.2297(5) 0.3024(6) 0.6247(3) 0.124(3) Uani 1 1 d . . . . . H41 H 0.260043 0.252190 0.662588 0.148 Uiso 1 1 calc R . . . . C42 C 0.1566(6) 0.3152(7) 0.6151(4) 0.147(3) Uani 1 1 d . . . . . H42 H 0.136492 0.275160 0.647383 0.177 Uiso 1 1 calc R . . . . C43 C 0.1104(4) 0.3847(6) 0.5600(4) 0.133(2) Uani 1 1 d . . . . . H43 H 0.058993 0.390974 0.553774 0.160 Uiso 1 1 calc R . . . . C44 C 0.1402(3) 0.4468(5) 0.5126(3) 0.0960(15) Uani 1 1 d . . . . . H44 H 0.108460 0.495786 0.474897 0.115 Uiso 1 1 calc R . . . . O1A O 0.4517(13) 0.428(2) 0.5917(8) 0.131(10) Uani 0.39(2) 1 d . . P A 2 O2A O 0.5095(17) 0.2711(11) 0.6692(12) 0.134(7) Uani 0.39(2) 1 d . . P A 2 O4A O 0.5789(8) 0.3658(19) 0.6143(11) 0.128(8) Uani 0.39(2) 1 d . . P A 2 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 Ag1 0.04915(18) 0.05783(19) 0.0841(2) -0.02091(15) -0.00846(15) -0.00162(13) Cl1 0.0696(6) 0.0562(5) 0.0573(6) -0.0010(5) 0.0083(5) 0.0167(5) P1 0.0442(5) 0.0422(5) 0.0477(5) -0.0045(4) -0.0036(4) 0.0043(4) O1 0.091(6) 0.074(4) 0.072(3) 0.020(3) -0.001(4) 0.003(4) O2 0.137(9) 0.161(10) 0.123(7) 0.018(7) 0.029(6) -0.061(8) O3 0.117(3) 0.136(3) 0.076(2) -0.044(2) 0.0044(19) 0.029(2) O4 0.138(9) 0.129(7) 0.166(10) -0.033(6) -0.009(7) 0.102(8) N1 0.0483(16) 0.0488(16) 0.0533(17) -0.0108(14) 0.0024(14) 0.0006(13) C1 0.066(2) 0.048(2) 0.052(2) -0.0124(17) 0.0144(18) -0.0069(18) C2 0.056(2) 0.047(2) 0.078(3) -0.0052(19) 0.021(2) 0.0077(17) C3 0.068(3) 0.058(2) 0.081(3) -0.005(2) 0.017(2) 0.018(2) C4 0.068(2) 0.053(2) 0.046(2) -0.0160(17) 0.0174(18) -0.0149(19) C5 0.0421(18) 0.062(2) 0.0423(19) -0.0218(17) 0.0022(15) 0.0057(17) C6 0.064(2) 0.047(2) 0.046(2) -0.0119(17) -0.0017(17) 0.0075(18) C7 0.0477(19) 0.052(2) 0.051(2) -0.0040(17) 0.0028(16) 0.0056(17) C8 0.070(3) 0.068(3) 0.063(3) 0.004(2) 0.007(2) 0.011(2) C9 0.080(3) 0.063(2) 0.061(2) 0.0015(19) 0.011(2) 0.003(2) C10 0.065(2) 0.057(2) 0.0399(19) -0.0068(17) 0.0060(17) 0.002(2) C11 0.068(2) 0.070(2) 0.040(2) -0.0134(19) 0.0152(18) -0.002(2) C12 0.052(2) 0.070(2) 0.044(2) -0.0157(19) 0.0133(17) -0.0027(19) C13 0.059(2) 0.058(2) 0.045(2) -0.0134(18) 0.0065(17) 0.0129(18) C14 0.071(3) 0.083(3) 0.074(3) -0.005(2) 0.020(2) 0.023(2) C15 0.072(3) 0.114(4) 0.095(4) -0.007(3) 0.029(3) 0.024(3) C16 0.050(2) 0.120(4) 0.083(3) -0.021(3) 0.022(2) 0.011(3) C17 0.078(3) 0.099(3) 0.059(3) -0.021(2) 0.031(2) -0.017(3) C18 0.086(3) 0.136(5) 0.087(4) -0.015(3) 0.036(3) -0.009(4) C19 0.085(3) 0.115(4) 0.090(4) 0.003(3) 0.042(3) -0.020(3) C20 0.093(3) 0.086(3) 0.062(3) -0.004(2) 0.018(2) -0.002(3) C21 0.0479(19) 0.053(2) 0.046(2) -0.0077(17) 0.0094(16) -0.0011(16) C22 0.055(2) 0.0466(19) 0.055(2) -0.0081(17) 0.0128(17) -0.0022(17) C23 0.048(2) 0.0458(19) 0.058(2) 0.0028(17) 0.0080(17) 0.0003(16) C24 0.0463(19) 0.057(2) 0.064(2) 0.0018(19) 0.0146(18) 0.0074(17) C25 0.051(2) 0.051(2) 0.057(2) -0.0116(17) 0.0078(17) 0.0089(17) C26 0.065(2) 0.058(2) 0.114(4) -0.004(2) 0.027(2) -0.009(2) C27 0.0413(17) 0.0453(18) 0.051(2) -0.0058(16) -0.0030(16) 0.0086(16) C28 0.065(2) 0.062(2) 0.064(3) 0.004(2) 0.013(2) 0.0116(19) C29 0.090(3) 0.099(4) 0.066(3) 0.003(3) 0.028(2) 0.027(3) C30 0.086(3) 0.086(3) 0.070(3) -0.024(3) 0.002(3) 0.025(3) C31 0.060(2) 0.071(3) 0.097(4) -0.034(3) 0.003(2) -0.002(2) C32 0.053(2) 0.060(2) 0.074(3) -0.021(2) 0.0104(19) -0.0007(19) C33 0.0445(17) 0.0447(18) 0.0425(18) 0.0009(15) 0.0078(15) 0.0038(15) C34 0.059(2) 0.052(2) 0.065(2) -0.0099(18) -0.0091(19) 0.0076(18) C35 0.069(2) 0.070(3) 0.061(2) 0.004(2) -0.016(2) 0.013(2) C36 0.071(2) 0.070(3) 0.061(2) 0.009(2) 0.005(2) 0.028(2) C37 0.092(3) 0.058(2) 0.082(3) -0.013(2) 0.003(3) 0.029(2) C38 0.067(2) 0.059(2) 0.060(2) -0.0128(19) -0.0079(19) 0.017(2) C39 0.091(3) 0.0432(18) 0.042(2) -0.0014(16) 0.007(2) 0.002(2) C40 0.144(4) 0.061(3) 0.055(3) 0.004(2) -0.002(3) 0.005(3) C41 0.227(8) 0.066(3) 0.055(3) 0.014(3) 0.017(5) -0.003(5) C42 0.283(11) 0.086(4) 0.100(6) 0.000(4) 0.099(7) -0.031(7) C43 0.168(6) 0.126(5) 0.134(6) 0.023(4) 0.088(5) -0.014(5) C44 0.111(4) 0.101(4) 0.088(3) 0.025(3) 0.050(3) 0.003(3) O1A 0.112(13) 0.115(13) 0.110(9) -0.032(9) -0.040(9) 0.077(12) O2A 0.195(19) 0.077(7) 0.141(13) 0.027(7) 0.073(13) -0.022(9) O4A 0.103(11) 0.182(14) 0.147(13) -0.104(11) 0.106(10) -0.087(11) 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 17 0 14 0.0606 17.0000 0.0000 14.0000 -0.4972 0.8802 0.0516 -21 0 22 0.0509 -21.0000 0.0000 22.0000 0.7011 0.2876 0.6344 2 15 -1 0.1086 2.0000 15.0000 -1.0000 -0.6029 -0.3371 0.7108 -22 0 21 0.0523 -22.0000 0.0000 21.0000 0.7300 0.2296 0.6283 -3 -15 -3 0.1452 -3.0000 -15.0000 -3.0000 0.6251 0.1742 -0.7703 21 0 -22 0.0157 21.0000 -0.0000 -22.0000 -0.7011 -0.2876 -0.6344 -14 1 -16 0.0428 -14.0000 1.0000 -16.0000 0.3637 -0.9045 -0.0718 -17 11 9 0.0758 -17.0000 11.0000 9.0000 0.1532 -0.3307 0.9084 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 _geom_angle_publ_flag P1 Ag1 O1 120.9(2) . . ? P1 Ag1 O1A 100.6(6) . . ? N1 Ag1 P1 159.59(7) . . ? N1 Ag1 O1 79.6(2) . . ? N1 Ag1 O1A 99.2(6) . . ? O2 Cl1 O1 108.2(4) . . ? O2 Cl1 O3 117.8(5) . . ? O3 Cl1 O1 105.9(3) . . ? O3 Cl1 O4A 112.4(6) . . ? O4 Cl1 O1 104.7(6) . . ? O4 Cl1 O2 110.0(7) . . ? O4 Cl1 O3 109.5(5) . . ? O1A Cl1 O3 114.1(5) . . ? O1A Cl1 O2A 109.8(9) . . ? O1A Cl1 O4A 114.9(10) . . ? O2A Cl1 O3 102.7(8) . . ? O2A Cl1 O4A 101.4(9) . . ? C27 P1 Ag1 116.61(12) . . ? C27 P1 C33 103.50(14) . . ? C27 P1 C39 104.53(17) . . ? C33 P1 Ag1 110.58(10) . . ? C33 P1 C39 104.75(17) . . ? C39 P1 Ag1 115.56(12) . . ? Cl1 O1 Ag1 135.3(7) . . ? C21 N1 Ag1 121.8(2) . . ? C25 N1 Ag1 120.6(2) . . ? C25 N1 C21 117.6(3) . . ? C2 C1 C6 120.7(4) . . ? C2 C1 C21 119.0(3) . . ? C6 C1 C21 120.3(3) . . ? C1 C2 H2 120.4 . . ? C1 C2 C3 119.3(4) . . ? C3 C2 H2 120.4 . . ? C2 C3 H3 118.7 . . ? C4 C3 C2 122.6(4) . . ? C4 C3 H3 118.7 . . ? C3 C4 C5 119.4(4) . . ? C3 C4 C13 122.3(4) . . ? C5 C4 C13 118.3(3) . . ? C4 C5 C6 118.2(3) . . ? C10 C5 C4 121.4(3) . . ? C10 C5 C6 120.4(3) . . ? C1 C6 C5 119.6(3) . . ? C7 C6 C1 122.6(4) . . ? C7 C6 C5 117.8(4) . . ? C6 C7 H7 119.4 . . ? C8 C7 C6 121.2(4) . . ? C8 C7 H7 119.4 . . ? C7 C8 H8 120.0 . . ? C7 C8 C9 120.1(4) . . ? C9 C8 H8 120.0 . . ? C8 C9 H9 119.1 . . ? C10 C9 C8 121.8(4) . . ? C10 C9 H9 119.1 . . ? C5 C10 C11 120.1(3) . . ? C9 C10 C5 118.7(4) . . ? C9 C10 C11 121.2(4) . . ? C12 C11 C10 120.0(4) . . ? C12 C11 C20 117.1(4) . . ? C20 C11 C10 122.9(4) . . ? C11 C12 C13 122.0(3) . . ? C11 C12 C17 120.6(4) . . ? C13 C12 C17 117.4(4) . . ? C12 C13 C4 118.1(3) . . ? C14 C13 C4 121.6(4) . . ? C14 C13 C12 120.3(4) . . ? C13 C14 H14 119.3 . . ? C13 C14 C15 121.5(5) . . ? C15 C14 H14 119.3 . . ? C14 C15 H15 118.9 . . ? C16 C15 C14 122.2(5) . . ? C16 C15 H15 118.9 . . ? C15 C16 H16 120.4 . . ? C15 C16 C17 119.2(4) . . ? C17 C16 H16 120.4 . . ? C16 C17 C12 119.5(4) . . ? C18 C17 C12 119.2(5) . . ? C18 C17 C16 121.3(5) . . ? C17 C18 H18 119.6 . . ? C19 C18 C17 120.7(5) . . ? C19 C18 H18 119.6 . . ? C18 C19 H19 118.6 . . ? C18 C19 C20 122.8(5) . . ? C20 C19 H19 118.6 . . ? C11 C20 H20 120.2 . . ? C19 C20 C11 119.6(4) . . ? C19 C20 H20 120.2 . . ? N1 C21 C1 117.7(3) . . ? N1 C21 C22 121.2(3) . . ? C22 C21 C1 121.1(3) . . ? C21 C22 H22 119.7 . . ? C21 C22 C23 120.7(3) . . ? C23 C22 H22 119.7 . . ? C22 C23 C26 122.0(3) . . ? C24 C23 C22 117.1(3) . . ? C24 C23 C26 120.9(3) . . ? C23 C24 H24 120.3 . . ? C25 C24 C23 119.5(3) . . ? C25 C24 H24 120.3 . . ? N1 C25 C24 124.0(3) . . ? N1 C25 H25 118.0 . . ? C24 C25 H25 118.0 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 P1 118.1(3) . . ? C32 C27 P1 123.2(3) . . ? C32 C27 C28 118.6(3) . . ? C27 C28 H28 119.8 . . ? C27 C28 C29 120.5(4) . . ? C29 C28 H28 119.8 . . ? C28 C29 H29 120.3 . . ? C30 C29 C28 119.4(5) . . ? C30 C29 H29 120.3 . . ? C29 C30 H30 119.4 . . ? C31 C30 C29 121.1(4) . . ? C31 C30 H30 119.4 . . ? C30 C31 H31 119.8 . . ? C30 C31 C32 120.3(4) . . ? C32 C31 H31 119.8 . . ? C27 C32 C31 120.1(4) . . ? C27 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C34 C33 P1 123.8(2) . . ? C38 C33 P1 118.5(2) . . ? C38 C33 C34 117.8(3) . . ? C33 C34 H34 119.6 . . ? C35 C34 C33 120.8(3) . . ? C35 C34 H34 119.6 . . ? C34 C35 H35 119.8 . . ? C36 C35 C34 120.4(3) . . ? C36 C35 H35 119.8 . . ? C35 C36 H36 120.2 . . ? C35 C36 C37 119.6(3) . . ? C37 C36 H36 120.2 . . ? C36 C37 H37 119.9 . . ? C36 C37 C38 120.1(4) . . ? C38 C37 H37 119.9 . . ? C33 C38 C37 121.2(3) . . ? C33 C38 H38 119.4 . . ? C37 C38 H38 119.4 . . ? C40 C39 P1 118.2(4) . . ? C44 C39 P1 123.6(3) . . ? C44 C39 C40 118.2(5) . . ? C39 C40 H40 120.2 . . ? C39 C40 C41 119.6(6) . . ? C41 C40 H40 120.2 . . ? C40 C41 H41 120.0 . . ? C42 C41 C40 119.9(7) . . ? C42 C41 H41 120.0 . . ? C41 C42 H42 119.1 . . ? C41 C42 C43 121.9(8) . . ? C43 C42 H42 119.1 . . ? C42 C43 H43 120.3 . . ? C42 C43 C44 119.5(7) . . ? C44 C43 H43 120.3 . . ? C39 C44 C43 121.0(5) . . ? C39 C44 H44 119.5 . . ? C43 C44 H44 119.5 . . ? Cl1 O1A Ag1 146.6(18) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P1 2.3719(9) . ? Ag1 O1 2.614(9) . ? Ag1 N1 2.222(3) . ? Ag1 O1A 2.529(14) . ? Cl1 O1 1.421(6) . ? Cl1 O2 1.387(8) . ? Cl1 O3 1.403(3) . ? Cl1 O4 1.374(10) . ? Cl1 O1A 1.380(9) . ? Cl1 O2A 1.390(11) . ? Cl1 O4A 1.423(12) . ? P1 C27 1.811(3) . ? P1 C33 1.812(3) . ? P1 C39 1.815(4) . ? N1 C21 1.355(4) . ? N1 C25 1.335(4) . ? C1 C2 1.390(5) . ? C1 C6 1.402(5) . ? C1 C21 1.516(5) . ? C2 H2 0.9300 . ? C2 C3 1.412(5) . ? C3 H3 0.9300 . ? C3 C4 1.368(5) . ? C4 C5 1.434(5) . ? C4 C13 1.504(5) . ? C5 C6 1.458(5) . ? C5 C10 1.399(5) . ? C6 C7 1.395(4) . ? C7 H7 0.9300 . ? C7 C8 1.369(5) . ? C8 H8 0.9300 . ? C8 C9 1.405(6) . ? C9 H9 0.9300 . ? C9 C10 1.377(5) . ? C10 C11 1.446(5) . ? C11 C12 1.406(5) . ? C11 C20 1.427(6) . ? C12 C13 1.415(5) . ? C12 C17 1.447(5) . ? C13 C14 1.362(5) . ? C14 H14 0.9300 . ? C14 C15 1.373(6) . ? C15 H15 0.9300 . ? C15 C16 1.343(6) . ? C16 H16 0.9300 . ? C16 C17 1.424(6) . ? C17 C18 1.362(7) . ? C18 H18 0.9300 . ? C18 C19 1.341(7) . ? C19 H19 0.9300 . ? C19 C20 1.393(6) . ? C20 H20 0.9300 . ? C21 C22 1.378(4) . ? C22 H22 0.9300 . ? C22 C23 1.388(5) . ? C23 C24 1.387(5) . ? C23 C26 1.499(5) . ? C24 H24 0.9300 . ? C24 C25 1.359(5) . ? C25 H25 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.384(5) . ? C27 C32 1.383(5) . ? C28 H28 0.9300 . ? C28 C29 1.395(6) . ? C29 H29 0.9300 . ? C29 C30 1.356(6) . ? C30 H30 0.9300 . ? C30 C31 1.353(6) . ? C31 H31 0.9300 . ? C31 C32 1.386(5) . ? C32 H32 0.9300 . ? C33 C34 1.379(4) . ? C33 C38 1.371(4) . ? C34 H34 0.9300 . ? C34 C35 1.378(5) . ? C35 H35 0.9300 . ? C35 C36 1.360(5) . ? C36 H36 0.9300 . ? C36 C37 1.362(5) . ? C37 H37 0.9300 . ? C37 C38 1.379(5) . ? C38 H38 0.9300 . ? C39 C40 1.385(5) . ? C39 C44 1.369(6) . ? C40 H40 0.9300 . ? C40 C41 1.408(8) . ? C41 H41 0.9300 . ? C41 C42 1.323(9) . ? C42 H42 0.9300 . ? C42 C43 1.345(9) . ? C43 H43 0.9300 . ? C43 C44 1.386(7) . ? C44 H44 0.9300 . ?