# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H48 Cl4 Li2 N6 O4 P2 U' _chemical_formula_weight 1228.57 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' Cl Cl 0.1484 0.1585 '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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5374(19) _cell_length_b 12.329(3) _cell_length_c 13.578(3) _cell_angle_alpha 114.91(3) _cell_angle_beta 93.92(3) _cell_angle_gamma 108.10(3) _cell_volume 1339.2(5) _cell_formula_units_Z 1 _cell_measurement_temperature 108(2) _cell_measurement_reflns_used 4118 _cell_measurement_theta_min 3.1415 _cell_measurement_theta_max 31.2338 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 606 _exptl_absorpt_coefficient_mu 3.335 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.1900 _exptl_absorpt_correction_T_max 0.6610 _exptl_absorpt_process_details 'face indexed' _exptl_special_details ; ? ; _diffrn_ambient_temperature 108(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_details ; AFC12 (Right): Kappa 3 circle ; _diffrn_measurement_device ; Saturn724 (2x2 bin mode) ; _diffrn_measurement_details ; scan: Number of images: 250 Slice: -55.0000 - 70.0000 Image width: 0.5000 Exp time: 12.0000 Rotation axis: Omega Omega: 0.0000 Kappa: 50.0000 Phi: 0.0000 XTD: 45.1786 2theta: -20.0542 scan: Number of images: 218 Slice: -55.0000 - 54.0000 Image width: 0.5000 Exp time: 12.0000 Rotation axis: Omega Omega: 0.0000 Kappa: 50.0000 Phi: 90.0000 XTD: 45.1786 2theta: -20.0542 scan: Number of images: 180 Slice: -110.0000 - -20.0000 Image width: 0.5000 Exp time: 12.0000 Rotation axis: Omega Omega: 0.0000 Kappa: 0.0000 Phi: 0.0000 XTD: 45.1786 2theta: -20.0542 scan: Number of images: 150 Slice: -91.2500 - -16.2500 Image width: 0.5000 Exp time: 12.0000 Rotation axis: Omega Omega: 0.0000 Kappa: 0.0000 Phi: 90.0000 XTD: 45.1786 2theta: -20.0542 ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12900 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 31.18 _diffrn_reflns_reduction_process 'Lp corrections applied' _reflns_number_total 6805 _reflns_number_gt 6804 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SHELXL-97 (Sheldrick, 2008)' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury 2.3' _computing_publication_material 'Mercury 2.3' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+0.7418P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6805 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0193 _refine_ls_R_factor_gt 0.0193 _refine_ls_wR_factor_ref 0.0560 _refine_ls_wR_factor_gt 0.0560 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL eh in P-1 CELL 0.71073 9.5374 12.3291 13.5777 114.909 93.920 108.096 ZERR 1.00 0.0019 0.0025 0.0027 0.030 0.030 0.030 LATT 1 SFAC C H N O P CL U LI UNIT 48 48 6 4 2 4 1 2 MERG 2 FMAP 2 PLAN -5 SIZE 0.40 0.45 0.50 ACTA 50.00 WGHT 0.03590 0.74180 L.S. 44 TEMP -165.00 FVAR 8.08912 U1 7 0.000000 0.500000 0.500000 10.50000 0.01492 0.01473 = 0.01314 0.00605 0.00220 0.00593 CL1 6 -0.041092 0.251706 0.380615 11.00000 0.02432 0.01635 = 0.03319 0.00365 0.00294 0.00872 CL2 6 -0.294381 0.447690 0.432648 11.00000 0.01575 0.02754 = 0.02375 0.00629 0.00101 0.00877 P1 5 1.056739 0.241643 -0.008937 11.00000 0.01591 0.01278 = 0.01353 0.00698 0.00262 0.00620 O1 4 0.036496 0.526172 0.383907 11.00000 0.02463 0.02624 = 0.01824 0.01318 0.00474 0.00729 O2 4 1.038573 0.120591 0.000722 11.00000 0.01855 0.01440 = 0.01856 0.00972 0.00354 0.00697 N1 3 0.709475 0.007306 0.046477 11.00000 0.02179 0.02667 = 0.02994 0.01383 0.00914 0.01083 N2 3 0.773461 -0.107640 -0.212803 11.00000 0.02287 0.02750 = 0.02450 0.01132 0.00324 0.01149 C6 1 0.304101 0.791402 0.434595 11.00000 0.03106 0.04221 = 0.06626 0.03550 0.00843 0.00756 AFIX 137 H6A 2 0.382117 0.810633 0.496874 11.00000 -1.50000 H6B 2 0.278012 0.702674 0.376220 11.00000 -1.50000 H6C 2 0.213545 0.801049 0.461157 11.00000 -1.50000 AFIX 0 LI1 8 0.857425 -0.033737 -0.047935 11.00000 0.01701 0.01959 = 0.02074 0.00962 0.00447 0.00865 C1 1 0.654909 0.054645 0.116394 11.00000 0.01512 0.02382 = 0.02604 0.01273 0.00369 0.00546 C2 1 0.583546 0.114591 0.204668 11.00000 0.02410 0.02964 = 0.02538 0.00838 0.00956 0.00925 AFIX 137 H2A 2 0.501517 0.131381 0.173722 11.00000 -1.50000 H2B 2 0.659084 0.196115 0.263258 11.00000 -1.50000 H2C 2 0.542050 0.056587 0.236385 11.00000 -1.50000 AFIX 0 C3 1 0.729000 -0.161668 -0.307278 11.00000 0.01692 0.02464 = 0.02232 0.01083 0.00460 0.00943 C4 1 0.669340 -0.233765 -0.428059 11.00000 0.02780 0.03594 = 0.02140 0.01019 0.00432 0.01333 AFIX 137 H4A 2 0.729710 -0.284972 -0.462145 11.00000 -1.50000 H4B 2 0.674698 -0.173392 -0.458221 11.00000 -1.50000 H4C 2 0.563585 -0.291304 -0.444846 11.00000 -1.50000 AFIX 0 C5 1 0.360840 0.879314 0.389844 11.00000 0.05078 0.03547 = 0.02947 0.01434 -0.00845 -0.00353 N3 3 0.404314 0.949610 0.355571 11.00000 0.10705 0.05574 = 0.03683 0.02800 -0.01807 -0.02006 C11 1 0.891021 0.280358 0.011642 11.00000 0.01753 0.01425 = 0.01851 0.00893 0.00340 0.00700 C12 1 0.877632 0.354643 0.118727 11.00000 0.02108 0.01807 = 0.01859 0.00704 0.00281 0.00800 AFIX 43 H12 2 0.962525 0.396722 0.180151 11.00000 -1.20000 AFIX 0 C13 1 0.740221 0.367148 0.135639 11.00000 0.02663 0.02050 = 0.02371 0.00834 0.01031 0.01274 AFIX 43 H13 2 0.731519 0.417987 0.208643 11.00000 -1.20000 AFIX 0 C14 1 0.615496 0.305610 0.046225 11.00000 0.02214 0.02455 = 0.03516 0.01554 0.00974 0.01328 AFIX 43 H14 2 0.521422 0.313581 0.058229 11.00000 -1.20000 AFIX 0 C15 1 0.628518 0.232523 -0.060587 11.00000 0.01985 0.02223 = 0.02878 0.01074 -0.00012 0.00843 AFIX 43 H15 2 0.543637 0.191866 -0.121808 11.00000 -1.20000 AFIX 0 C16 1 0.764889 0.218387 -0.078627 11.00000 0.02046 0.02034 = 0.01738 0.00789 0.00043 0.00851 AFIX 43 H16 2 0.772767 0.167001 -0.151741 11.00000 -1.20000 AFIX 0 C21 1 1.219819 0.373511 0.094078 11.00000 0.01643 0.01555 = 0.01592 0.00666 0.00257 0.00680 C22 1 1.248068 0.378922 0.198940 11.00000 0.02184 0.01989 = 0.01921 0.00928 0.00144 0.00582 AFIX 43 H22 2 1.177842 0.318269 0.215062 11.00000 -1.20000 AFIX 0 C23 1 1.378190 0.472470 0.279542 11.00000 0.02708 0.02582 = 0.01944 0.00714 -0.00126 0.00769 AFIX 43 H23 2 1.397284 0.475431 0.350403 11.00000 -1.20000 AFIX 0 C24 1 1.480593 0.561936 0.256076 11.00000 0.02081 0.02551 = 0.02593 0.00629 -0.00115 0.00385 AFIX 43 H24 2 1.570711 0.624847 0.310489 11.00000 -1.20000 AFIX 0 C25 1 1.451377 0.559400 0.153710 11.00000 0.02154 0.01775 = 0.02789 0.00692 0.00380 0.00125 AFIX 43 H25 2 1.520282 0.622051 0.138901 11.00000 -1.20000 AFIX 0 C26 1 1.321221 0.465300 0.072079 11.00000 0.02195 0.01909 = 0.02123 0.01009 0.00380 0.00433 AFIX 43 H26 2 1.301730 0.463731 0.001837 11.00000 -1.20000 AFIX 0 C31 1 1.079408 0.219421 -0.145863 11.00000 0.01869 0.01935 = 0.01372 0.00910 0.00301 0.00683 C32 1 1.064488 0.305478 -0.184037 11.00000 0.02632 0.02107 = 0.02134 0.01268 0.00406 0.00877 AFIX 43 H32 2 1.045980 0.379605 -0.136419 11.00000 -1.20000 AFIX 0 C33 1 1.076874 0.281902 -0.291688 11.00000 0.02911 0.03123 = 0.02448 0.02036 0.00144 0.00481 AFIX 43 H33 2 1.067311 0.340334 -0.317684 11.00000 -1.20000 AFIX 0 C34 1 1.102928 0.174386 -0.361029 11.00000 0.03558 0.03434 = 0.01736 0.01311 0.00733 0.00479 AFIX 43 H34 2 1.109930 0.158456 -0.434983 11.00000 -1.20000 AFIX 0 C35 1 1.119083 0.088926 -0.323845 11.00000 0.04787 0.02644 = 0.01777 0.00579 0.01488 0.01559 AFIX 43 H35 2 1.138138 0.015348 -0.372003 11.00000 -1.20000 AFIX 0 C36 1 1.107311 0.111188 -0.215666 11.00000 0.03083 0.02215 = 0.01892 0.01014 0.00854 0.01165 AFIX 43 H36 2 1.118245 0.052971 -0.189843 11.00000 -1.20000 AFIX 0 HKLF 4 1.0 1.00 0.00 0.00 0.00 -1.00 0.00 0.00 1.00 -1.00 END ; 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.0000 0.5000 0.5000 0.01439(4) Uani 1 2 d S . . Cl1 Cl -0.04109(6) 0.25171(5) 0.38062(5) 0.02753(11) Uani 1 1 d . . . Cl2 Cl -0.29438(5) 0.44769(6) 0.43265(5) 0.02452(10) Uani 1 1 d . . . P1 P 1.05674(5) 0.24164(5) -0.00894(4) 0.01358(9) Uani 1 1 d . . . O1 O 0.03649(17) 0.52617(16) 0.38391(13) 0.0226(3) Uani 1 1 d . . . O2 O 1.03857(15) 0.12059(14) 0.00072(12) 0.0162(3) Uani 1 1 d . . . N1 N 0.7095(2) 0.0073(2) 0.04648(18) 0.0253(4) Uani 1 1 d . . . N2 N 0.7735(2) -0.1076(2) -0.21280(17) 0.0248(4) Uani 1 1 d . . . C6 C 0.3041(3) 0.7914(3) 0.4346(3) 0.0445(7) Uani 1 1 d . . . H6A H 0.3821 0.8107 0.4969 0.067 Uiso 1 1 calc R . . H6B H 0.2780 0.7027 0.3762 0.067 Uiso 1 1 calc R . . H6C H 0.2135 0.8010 0.4611 0.067 Uiso 1 1 calc R . . Li1 Li 0.8574(4) -0.0337(4) -0.0479(3) 0.0185(7) Uani 1 1 d . . . C1 C 0.6549(2) 0.0546(2) 0.11639(19) 0.0218(4) Uani 1 1 d . . . C2 C 0.5835(3) 0.1146(3) 0.2047(2) 0.0281(5) Uani 1 1 d . . . H2A H 0.5015 0.1313 0.1737 0.042 Uiso 1 1 calc R . . H2B H 0.6591 0.1961 0.2632 0.042 Uiso 1 1 calc R . . H2C H 0.5421 0.0566 0.2364 0.042 Uiso 1 1 calc R . . C3 C 0.7290(2) -0.1617(2) -0.30728(18) 0.0209(4) Uani 1 1 d . . . C4 C 0.6693(3) -0.2338(3) -0.4281(2) 0.0293(5) Uani 1 1 d . . . H4A H 0.7297 -0.2850 -0.4621 0.044 Uiso 1 1 calc R . . H4B H 0.6747 -0.1734 -0.4582 0.044 Uiso 1 1 calc R . . H4C H 0.5636 -0.2913 -0.4448 0.044 Uiso 1 1 calc R . . C5 C 0.3608(4) 0.8793(3) 0.3898(2) 0.0451(7) Uani 1 1 d . . . N3 N 0.4043(5) 0.9496(4) 0.3556(3) 0.0796(13) Uani 1 1 d . . . C11 C 0.8910(2) 0.2804(2) 0.01164(17) 0.0160(3) Uani 1 1 d . . . C12 C 0.8776(2) 0.3546(2) 0.11873(18) 0.0197(4) Uani 1 1 d . . . H12 H 0.9625 0.3967 0.1801 0.024 Uiso 1 1 calc R . . C13 C 0.7402(2) 0.3671(2) 0.1356(2) 0.0231(4) Uani 1 1 d . . . H13 H 0.7315 0.4180 0.2086 0.028 Uiso 1 1 calc R . . C14 C 0.6155(2) 0.3056(2) 0.0462(2) 0.0253(4) Uani 1 1 d . . . H14 H 0.5214 0.3136 0.0582 0.030 Uiso 1 1 calc R . . C15 C 0.6285(2) 0.2325(2) -0.0606(2) 0.0242(4) Uani 1 1 d . . . H15 H 0.5436 0.1919 -0.1218 0.029 Uiso 1 1 calc R . . C16 C 0.7649(2) 0.2184(2) -0.07863(18) 0.0197(4) Uani 1 1 d . . . H16 H 0.7728 0.1670 -0.1517 0.024 Uiso 1 1 calc R . . C21 C 1.2198(2) 0.3735(2) 0.09408(16) 0.0161(3) Uani 1 1 d . . . C22 C 1.2481(2) 0.3789(2) 0.19894(18) 0.0210(4) Uani 1 1 d . . . H22 H 1.1778 0.3183 0.2151 0.025 Uiso 1 1 calc R . . C23 C 1.3782(3) 0.4725(2) 0.27954(19) 0.0264(4) Uani 1 1 d . . . H23 H 1.3973 0.4754 0.3504 0.032 Uiso 1 1 calc R . . C24 C 1.4806(3) 0.5619(3) 0.2561(2) 0.0279(5) Uani 1 1 d . . . H24 H 1.5707 0.6248 0.3105 0.033 Uiso 1 1 calc R . . C25 C 1.4514(2) 0.5594(2) 0.1537(2) 0.0255(4) Uani 1 1 d . . . H25 H 1.5203 0.6221 0.1389 0.031 Uiso 1 1 calc R . . C26 C 1.3212(2) 0.4653(2) 0.07208(18) 0.0215(4) Uani 1 1 d . . . H26 H 1.3017 0.4637 0.0018 0.026 Uiso 1 1 calc R . . C31 C 1.0794(2) 0.2194(2) -0.14586(16) 0.0169(4) Uani 1 1 d . . . C32 C 1.0645(2) 0.3055(2) -0.18404(19) 0.0220(4) Uani 1 1 d . . . H32 H 1.0460 0.3796 -0.1364 0.026 Uiso 1 1 calc R . . C33 C 1.0769(3) 0.2819(2) -0.2917(2) 0.0275(5) Uani 1 1 d . . . H33 H 1.0673 0.3403 -0.3177 0.033 Uiso 1 1 calc R . . C34 C 1.1029(3) 0.1744(3) -0.36103(19) 0.0308(5) Uani 1 1 d . . . H34 H 1.1099 0.1585 -0.4350 0.037 Uiso 1 1 calc R . . C35 C 1.1191(3) 0.0889(3) -0.3238(2) 0.0316(5) Uani 1 1 d . . . H35 H 1.1381 0.0153 -0.3720 0.038 Uiso 1 1 calc R . . C36 C 1.1073(3) 0.1112(2) -0.21567(18) 0.0231(4) Uani 1 1 d . . . H36 H 1.1182 0.0530 -0.1898 0.028 Uiso 1 1 calc R . . 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 0.01492(5) 0.01473(6) 0.01314(5) 0.00605(5) 0.00220(3) 0.00593(4) Cl1 0.0243(2) 0.0163(3) 0.0332(3) 0.0036(3) 0.0029(2) 0.00872(19) Cl2 0.01574(19) 0.0275(3) 0.0237(2) 0.0063(2) 0.00101(17) 0.00877(18) P1 0.01591(19) 0.0128(2) 0.0135(2) 0.0070(2) 0.00262(16) 0.00620(17) O1 0.0246(7) 0.0262(9) 0.0182(7) 0.0132(7) 0.0047(5) 0.0073(6) O2 0.0185(6) 0.0144(7) 0.0186(7) 0.0097(6) 0.0035(5) 0.0070(5) N1 0.0218(8) 0.0267(11) 0.0299(10) 0.0138(9) 0.0091(7) 0.0108(7) N2 0.0229(8) 0.0275(11) 0.0245(9) 0.0113(9) 0.0032(7) 0.0115(7) C6 0.0311(12) 0.0422(18) 0.066(2) 0.0355(17) 0.0084(13) 0.0076(11) Li1 0.0170(15) 0.0196(19) 0.0207(17) 0.0096(16) 0.0045(12) 0.0086(13) C1 0.0151(8) 0.0238(12) 0.0260(10) 0.0127(10) 0.0037(7) 0.0055(7) C2 0.0241(10) 0.0296(14) 0.0254(11) 0.0084(11) 0.0096(8) 0.0093(9) C3 0.0169(8) 0.0246(12) 0.0223(10) 0.0108(10) 0.0046(7) 0.0094(8) C4 0.0278(10) 0.0359(15) 0.0214(11) 0.0102(11) 0.0043(8) 0.0133(10) C5 0.0508(16) 0.0355(17) 0.0295(13) 0.0143(14) -0.0084(12) -0.0035(12) N3 0.107(3) 0.056(2) 0.0368(15) 0.0280(16) -0.0181(17) -0.0201(19) C11 0.0175(8) 0.0142(10) 0.0185(9) 0.0089(9) 0.0034(7) 0.0070(7) C12 0.0211(9) 0.0181(11) 0.0186(9) 0.0070(9) 0.0028(7) 0.0080(7) C13 0.0266(10) 0.0205(12) 0.0237(10) 0.0083(10) 0.0103(8) 0.0127(8) C14 0.0221(9) 0.0246(12) 0.0352(12) 0.0155(11) 0.0097(8) 0.0133(8) C15 0.0199(9) 0.0222(12) 0.0288(11) 0.0107(10) -0.0001(8) 0.0084(8) C16 0.0205(8) 0.0203(11) 0.0174(9) 0.0079(9) 0.0004(7) 0.0085(7) C21 0.0164(8) 0.0155(10) 0.0159(9) 0.0067(8) 0.0026(6) 0.0068(7) C22 0.0218(9) 0.0199(11) 0.0192(9) 0.0093(9) 0.0014(7) 0.0058(7) C23 0.0271(10) 0.0258(13) 0.0194(10) 0.0071(10) -0.0013(8) 0.0077(9) C24 0.0208(9) 0.0255(13) 0.0259(11) 0.0063(11) -0.0011(8) 0.0039(8) C25 0.0215(9) 0.0177(12) 0.0279(11) 0.0069(10) 0.0038(8) 0.0012(8) C26 0.0219(9) 0.0191(11) 0.0212(10) 0.0101(9) 0.0038(7) 0.0043(7) C31 0.0187(8) 0.0193(10) 0.0137(8) 0.0091(9) 0.0030(6) 0.0068(7) C32 0.0263(9) 0.0211(11) 0.0213(10) 0.0127(10) 0.0041(7) 0.0088(8) C33 0.0291(10) 0.0312(13) 0.0245(11) 0.0204(11) 0.0014(8) 0.0048(9) C34 0.0356(12) 0.0343(15) 0.0174(10) 0.0131(11) 0.0073(8) 0.0048(10) C35 0.0479(14) 0.0264(14) 0.0178(10) 0.0058(11) 0.0149(10) 0.0156(11) C36 0.0308(10) 0.0222(12) 0.0189(10) 0.0101(10) 0.0085(8) 0.0116(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 U1 O1 1.7730(14) . ? U1 O1 1.7730(14) 2_566 ? U1 Cl1 2.6721(12) 2_566 ? U1 Cl1 2.6721(12) . ? U1 Cl2 2.6762(9) 2_566 ? U1 Cl2 2.6762(9) . ? P1 O2 1.5106(14) . ? P1 C11 1.795(2) . ? P1 C21 1.799(2) . ? P1 C31 1.8002(19) . ? O2 Li1 1.922(4) 2_755 ? O2 Li1 1.945(4) . ? N1 C1 1.141(3) . ? N1 Li1 2.009(4) . ? N2 C3 1.140(3) . ? N2 Li1 2.016(4) . ? C6 C5 1.439(4) . ? Li1 O2 1.922(4) 2_755 ? Li1 Li1 2.642(7) 2_755 ? C1 C2 1.457(3) . ? C3 C4 1.461(3) . ? C5 N3 1.132(4) . ? C11 C12 1.395(3) . ? C11 C16 1.404(3) . ? C12 C13 1.390(3) . ? C13 C14 1.389(3) . ? C14 C15 1.387(4) . ? C15 C16 1.389(3) . ? C21 C26 1.396(3) . ? C21 C22 1.400(3) . ? C22 C23 1.389(3) . ? C23 C24 1.393(3) . ? C24 C25 1.384(3) . ? C25 C26 1.396(3) . ? C31 C36 1.393(3) . ? C31 C32 1.401(3) . ? C32 C33 1.386(3) . ? C33 C34 1.375(4) . ? C34 C35 1.388(4) . ? C35 C36 1.396(3) . ? 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 O1 U1 O1 180.000(1) . 2_566 ? O1 U1 Cl1 89.82(6) . 2_566 ? O1 U1 Cl1 90.18(6) 2_566 2_566 ? O1 U1 Cl1 90.18(6) . . ? O1 U1 Cl1 89.82(6) 2_566 . ? Cl1 U1 Cl1 180.0 2_566 . ? O1 U1 Cl2 90.27(6) . 2_566 ? O1 U1 Cl2 89.73(6) 2_566 2_566 ? Cl1 U1 Cl2 91.17(5) 2_566 2_566 ? Cl1 U1 Cl2 88.83(5) . 2_566 ? O1 U1 Cl2 89.73(6) . . ? O1 U1 Cl2 90.27(6) 2_566 . ? Cl1 U1 Cl2 88.83(5) 2_566 . ? Cl1 U1 Cl2 91.17(5) . . ? Cl2 U1 Cl2 180.0 2_566 . ? O2 P1 C11 110.34(8) . . ? O2 P1 C21 109.61(9) . . ? C11 P1 C21 109.45(10) . . ? O2 P1 C31 110.77(10) . . ? C11 P1 C31 107.24(9) . . ? C21 P1 C31 109.39(9) . . ? P1 O2 Li1 144.84(14) . 2_755 ? P1 O2 Li1 128.93(13) . . ? Li1 O2 Li1 86.19(15) 2_755 . ? C1 N1 Li1 164.0(2) . . ? C3 N2 Li1 172.1(2) . . ? O2 Li1 O2 93.81(15) 2_755 . ? O2 Li1 N1 110.13(17) 2_755 . ? O2 Li1 N1 109.8(2) . . ? O2 Li1 N2 117.9(2) 2_755 . ? O2 Li1 N2 109.13(18) . . ? N1 Li1 N2 114.05(17) . . ? O2 Li1 Li1 47.28(11) 2_755 2_755 ? O2 Li1 Li1 46.53(12) . 2_755 ? N1 Li1 Li1 120.0(2) . 2_755 ? N2 Li1 Li1 125.6(2) . 2_755 ? N1 C1 C2 179.3(2) . . ? N2 C3 C4 178.5(3) . . ? N3 C5 C6 178.9(5) . . ? C12 C11 C16 119.58(18) . . ? C12 C11 P1 120.58(15) . . ? C16 C11 P1 119.07(16) . . ? C13 C12 C11 120.1(2) . . ? C14 C13 C12 120.3(2) . . ? C15 C14 C13 119.9(2) . . ? C14 C15 C16 120.4(2) . . ? C15 C16 C11 119.7(2) . . ? C26 C21 C22 119.50(19) . . ? C26 C21 P1 123.02(15) . . ? C22 C21 P1 117.41(15) . . ? C23 C22 C21 120.38(19) . . ? C22 C23 C24 119.8(2) . . ? C25 C24 C23 120.2(2) . . ? C24 C25 C26 120.4(2) . . ? C25 C26 C21 119.75(19) . . ? C36 C31 C32 120.05(18) . . ? C36 C31 P1 118.36(14) . . ? C32 C31 P1 121.55(17) . . ? C33 C32 C31 119.6(2) . . ? C34 C33 C32 120.3(2) . . ? C33 C34 C35 120.5(2) . . ? C34 C35 C36 119.9(2) . . ? C31 C36 C35 119.5(2) . . ? _diffrn_measured_fraction_theta_max 0.786 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.909 _refine_diff_density_max 0.682 _refine_diff_density_min -1.651 _refine_diff_density_rms 0.085 _database_code_depnum_ccdc_archive 'CCDC 959953' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H30 Br2 O4 P2 U' _chemical_formula_weight 986.39 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' Br Br -0.2901 2.4595 '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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.2695(19) _cell_length_b 10.430(2) _cell_length_c 18.221(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.91(3) _cell_angle_gamma 90.00 _cell_volume 1744.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.877 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 7.070 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2255 _exptl_absorpt_correction_T_max 0.3321 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'AFC12 (Right): Kappa 3 circle' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17097 _diffrn_reflns_av_R_equivalents 0.1519 _diffrn_reflns_av_sigmaI/netI 0.0743 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3022 _reflns_number_gt 2831 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SHELXL-97 (Sheldrick, 2008)' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP _computing_publication_material ORTEP _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1479P)^2^+91.3955P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3022 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1176 _refine_ls_R_factor_gt 0.1019 _refine_ls_wR_factor_ref 0.2991 _refine_ls_wR_factor_gt 0.2766 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_restrained_S_all 1.149 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.721(2) 0.3533(19) 0.0596(10) 0.030(4) Uani 1 1 d . . . C2 C 0.666(2) 0.323(2) 0.1251(11) 0.038(5) Uani 1 1 d . . . H2 H 0.6645 0.2368 0.1416 0.045 Uiso 1 1 calc R . . C3 C 0.613(2) 0.419(3) 0.1653(13) 0.047(6) Uani 1 1 d . . . H3 H 0.5827 0.4001 0.2117 0.057 Uiso 1 1 calc R . . C4 C 0.604(4) 0.544(3) 0.1390(14) 0.063(8) Uani 1 1 d . . . H4 H 0.5642 0.6081 0.1670 0.075 Uiso 1 1 calc R . . C5 C 0.651(2) 0.576(2) 0.0735(14) 0.046(6) Uani 1 1 d . . . H5 H 0.6453 0.6619 0.0566 0.055 Uiso 1 1 calc R . . C6 C 0.710(3) 0.479(2) 0.0307(14) 0.045(5) Uani 1 1 d . . . H6 H 0.7403 0.4988 -0.0157 0.053 Uiso 1 1 calc R . . C7 C 0.861(2) 0.2761(18) -0.0683(11) 0.033(4) Uani 1 1 d . . . C8 C 0.740(2) 0.312(2) -0.1219(11) 0.040(5) Uani 1 1 d . . . H8 H 0.6439 0.3138 -0.1099 0.048 Uiso 1 1 calc R . . C9 C 0.770(3) 0.344(2) -0.1933(11) 0.050(6) Uani 1 1 d . . . H9 H 0.6913 0.3655 -0.2303 0.060 Uiso 1 1 calc R . . C10 C 0.910(3) 0.345(3) -0.2118(13) 0.069(9) Uani 1 1 d . . . H10 H 0.9288 0.3722 -0.2593 0.083 Uiso 1 1 calc R . . C11 C 1.025(3) 0.304(4) -0.1579(12) 0.068(9) Uani 1 1 d . . . H11 H 1.1205 0.2968 -0.1704 0.081 Uiso 1 1 calc R . . C12 C 0.998(2) 0.273(3) -0.0861(11) 0.042(5) Uani 1 1 d . . . H12 H 1.0771 0.2507 -0.0495 0.050 Uiso 1 1 calc R . . C13 C 0.978(2) 0.199(2) 0.0806(10) 0.029(4) Uani 1 1 d . . . C14 C 1.064(3) 0.303(2) 0.1116(14) 0.046(5) Uani 1 1 d . . . H14 H 1.0323 0.3882 0.1005 0.055 Uiso 1 1 calc R . . C15 C 1.190(3) 0.282(3) 0.1564(15) 0.057(7) Uani 1 1 d . . . H15 H 1.2436 0.3540 0.1779 0.069 Uiso 1 1 calc R . . C16 C 1.244(3) 0.162(3) 0.1717(11) 0.050(6) Uani 1 1 d . . . H16 H 1.3349 0.1490 0.2015 0.060 Uiso 1 1 calc R . . C17 C 1.157(3) 0.058(3) 0.1412(13) 0.050(6) Uani 1 1 d . . . H17 H 1.1892 -0.0274 0.1524 0.060 Uiso 1 1 calc R . . C18 C 1.030(3) 0.076(2) 0.0970(12) 0.040(5) Uani 1 1 d . . . H18 H 0.9750 0.0036 0.0769 0.048 Uiso 1 1 calc R . . Br1 Br 0.5747(3) -0.0716(2) 0.15066(11) 0.0426(6) Uani 1 1 d . . . O1 O 0.7202(16) 0.1059(13) 0.0092(7) 0.035(3) Uani 1 1 d . . . O2 O 0.4192(14) 0.1415(12) 0.0262(8) 0.034(3) Uani 1 1 d . . . P1 P 0.8134(5) 0.2265(4) 0.0188(2) 0.0240(10) Uani 1 1 d . . . U1 U 0.5000 0.0000 0.0000 0.0265(4) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.032(10) 0.030(10) 0.026(9) -0.002(7) -0.001(7) -0.001(8) C2 0.038(12) 0.041(12) 0.035(10) -0.001(9) 0.007(8) 0.008(9) C3 0.030(12) 0.069(17) 0.044(12) -0.006(11) 0.013(9) 0.009(11) C4 0.08(2) 0.063(17) 0.038(13) -0.014(12) 0.002(12) 0.029(16) C5 0.021(10) 0.035(12) 0.078(16) -0.001(11) -0.008(10) 0.013(9) C6 0.060(15) 0.024(11) 0.052(14) -0.004(9) 0.019(11) -0.006(10) C7 0.041(12) 0.021(9) 0.041(11) 0.002(8) 0.019(9) -0.013(9) C8 0.033(11) 0.052(14) 0.033(10) 0.004(9) -0.001(8) 0.008(10) C9 0.075(18) 0.049(14) 0.025(10) 0.007(9) 0.004(10) 0.001(13) C10 0.09(2) 0.10(2) 0.024(11) 0.001(12) 0.008(12) -0.043(19) C11 0.049(15) 0.13(3) 0.027(11) -0.004(13) 0.004(10) -0.021(17) C12 0.017(9) 0.073(16) 0.034(10) 0.004(10) -0.001(7) -0.006(10) C13 0.021(9) 0.042(11) 0.025(9) -0.001(8) 0.003(7) -0.011(8) C14 0.039(13) 0.031(12) 0.069(15) 0.002(10) 0.008(11) -0.008(10) C15 0.029(12) 0.068(18) 0.072(17) 0.000(14) -0.006(11) 0.001(12) C16 0.040(13) 0.076(18) 0.030(10) -0.008(11) -0.010(9) 0.016(12) C17 0.047(14) 0.051(15) 0.049(13) 0.002(11) -0.004(10) 0.022(12) C18 0.046(13) 0.031(11) 0.042(11) -0.004(8) 0.004(9) 0.003(10) Br1 0.0560(14) 0.0422(12) 0.0289(10) 0.0043(8) 0.0031(9) -0.0024(10) O1 0.049(9) 0.023(7) 0.032(7) 0.002(5) 0.006(6) -0.003(6) O2 0.025(7) 0.016(6) 0.063(9) -0.001(6) 0.015(6) 0.005(5) P1 0.022(2) 0.023(2) 0.028(2) 0.0011(17) 0.0067(17) -0.0016(18) U1 0.0328(6) 0.0217(6) 0.0259(6) 0.0004(3) 0.0070(4) -0.0026(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 C1 C2 1.40(3) . ? C1 C6 1.41(3) . ? C1 P1 1.79(2) . ? C2 C3 1.37(3) . ? C2 H2 0.9500 . ? C3 C4 1.38(4) . ? C3 H3 0.9500 . ? C4 C5 1.37(4) . ? C4 H4 0.9500 . ? C5 C6 1.43(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.36(3) . ? C7 C8 1.43(3) . ? C7 P1 1.782(19) . ? C8 C9 1.41(3) . ? C8 H8 0.9500 . ? C9 C10 1.39(4) . ? C9 H9 0.9500 . ? C10 C11 1.41(4) . ? C10 H10 0.9500 . ? C11 C12 1.40(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.39(3) . ? C13 C14 1.42(3) . ? C13 P1 1.787(19) . ? C14 C15 1.35(3) . ? C14 H14 0.9500 . ? C15 C16 1.36(4) . ? C15 H15 0.9500 . ? C16 C17 1.42(4) . ? C16 H16 0.9500 . ? C17 C18 1.34(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? Br1 U1 2.837(2) . ? O1 P1 1.523(14) . ? O1 U1 2.306(15) . ? O2 U1 1.751(12) . ? U1 O2 1.751(12) 3_655 ? U1 O1 2.306(15) 3_655 ? U1 Br1 2.837(2) 3_655 ? 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 C2 C1 C6 120.7(19) . . ? C2 C1 P1 116.1(15) . . ? C6 C1 P1 123.1(16) . . ? C3 C2 C1 119(2) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 121(2) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 121(2) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C4 C5 C6 120(2) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C1 C6 C5 118(2) . . ? C1 C6 H6 121.1 . . ? C5 C6 H6 121.1 . . ? C12 C7 C8 120.9(18) . . ? C12 C7 P1 124.2(17) . . ? C8 C7 P1 114.8(15) . . ? C9 C8 C7 117(2) . . ? C9 C8 H8 121.3 . . ? C7 C8 H8 121.3 . . ? C10 C9 C8 122(2) . . ? C10 C9 H9 118.8 . . ? C8 C9 H9 118.8 . . ? C9 C10 C11 118(2) . . ? C9 C10 H10 121.0 . . ? C11 C10 H10 121.0 . . ? C12 C11 C10 121(2) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C7 C12 C11 121(2) . . ? C7 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C18 C13 C14 117.5(19) . . ? C18 C13 P1 121.7(15) . . ? C14 C13 P1 120.7(17) . . ? C15 C14 C13 121(2) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 122(3) . . ? C14 C15 H15 119.0 . . ? C16 C15 H15 119.0 . . ? C15 C16 C17 117(2) . . ? C15 C16 H16 121.5 . . ? C17 C16 H16 121.5 . . ? C18 C17 C16 122(2) . . ? C18 C17 H17 119.0 . . ? C16 C17 H17 119.0 . . ? C17 C18 C13 120(2) . . ? C17 C18 H18 119.8 . . ? C13 C18 H18 119.8 . . ? P1 O1 U1 152.5(9) . . ? O1 P1 C7 110.0(8) . . ? O1 P1 C13 111.0(9) . . ? C7 P1 C13 108.4(9) . . ? O1 P1 C1 111.2(9) . . ? C7 P1 C1 110.2(9) . . ? C13 P1 C1 105.8(9) . . ? O2 U1 O2 180.0(11) . 3_655 ? O2 U1 O1 90.9(6) . 3_655 ? O2 U1 O1 89.1(6) 3_655 3_655 ? O2 U1 O1 89.1(6) . . ? O2 U1 O1 90.9(6) 3_655 . ? O1 U1 O1 180.0(7) 3_655 . ? O2 U1 Br1 90.8(5) . . ? O2 U1 Br1 89.2(5) 3_655 . ? O1 U1 Br1 92.3(3) 3_655 . ? O1 U1 Br1 87.7(3) . . ? O2 U1 Br1 89.2(5) . 3_655 ? O2 U1 Br1 90.8(5) 3_655 3_655 ? O1 U1 Br1 87.7(3) 3_655 3_655 ? O1 U1 Br1 92.3(3) . 3_655 ? Br1 U1 Br1 180.00(9) . 3_655 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 4.587 _refine_diff_density_min -2.643 _refine_diff_density_rms 0.574 _iucr_refine_instructions_details ; TITL eha173 in P21/c CELL 0.71073 9.2695 10.4300 18.2210 90.000 97.910 90.000 ZERR 2.00 0.0019 0.0020 0.0040 0.000 0.030 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H BR O P U UNIT 72 60 4 8 4 2 MERG 2 OMIT -2.00 50.00 FMAP 2 PLAN 5 SIZE 0.20 0.20 0.30 ACTA BOND $H L.S. 5 TEMP -103.00 WGHT 0.147900 91.395500 FVAR 0.23266 C1 1 0.721142 0.353273 0.059580 11.00000 0.03244 0.03047 = 0.02622 -0.00211 -0.00051 -0.00067 C2 1 0.665694 0.323111 0.125130 11.00000 0.03799 0.04142 = 0.03475 -0.00057 0.00729 0.00778 AFIX 43 H2 2 0.664480 0.236759 0.141620 11.00000 -1.20000 AFIX 0 C3 1 0.613227 0.419215 0.165255 11.00000 0.03019 0.06910 = 0.04448 -0.00637 0.01256 0.00922 AFIX 43 H3 2 0.582724 0.400127 0.211727 11.00000 -1.20000 AFIX 0 C4 1 0.604095 0.543506 0.139029 11.00000 0.08493 0.06263 = 0.03840 -0.01427 0.00247 0.02919 AFIX 43 H4 2 0.564188 0.608086 0.167016 11.00000 -1.20000 AFIX 0 C5 1 0.651407 0.575604 0.073472 11.00000 0.02055 0.03477 = 0.07792 -0.00118 -0.00830 0.01313 AFIX 43 H5 2 0.645257 0.661861 0.056583 11.00000 -1.20000 AFIX 0 C6 1 0.709911 0.479106 0.030676 11.00000 0.06020 0.02413 = 0.05233 -0.00355 0.01884 -0.00556 AFIX 43 H6 2 0.740339 0.498755 -0.015740 11.00000 -1.20000 AFIX 0 C7 1 0.860819 0.276067 -0.068346 11.00000 0.04093 0.02074 = 0.04118 0.00173 0.01899 -0.01320 C8 1 0.740310 0.311769 -0.121941 11.00000 0.03343 0.05214 = 0.03275 0.00354 -0.00149 0.00832 AFIX 43 H8 2 0.643860 0.313831 -0.109852 11.00000 -1.20000 AFIX 0 C9 1 0.770100 0.343760 -0.193341 11.00000 0.07461 0.04927 = 0.02487 0.00662 0.00366 0.00114 AFIX 43 H9 2 0.691278 0.365470 -0.230267 11.00000 -1.20000 AFIX 0 C10 1 0.910418 0.344759 -0.211795 11.00000 0.08689 0.09704 = 0.02413 0.00135 0.00799 -0.04293 AFIX 43 H10 2 0.928831 0.372216 -0.259345 11.00000 -1.20000 AFIX 0 C11 1 1.024579 0.303865 -0.157934 11.00000 0.04910 0.12650 = 0.02666 -0.00435 0.00396 -0.02093 AFIX 43 H11 2 1.120474 0.296827 -0.170384 11.00000 -1.20000 AFIX 0 C12 1 0.998122 0.273445 -0.086138 11.00000 0.01676 0.07297 = 0.03386 0.00416 -0.00077 -0.00619 AFIX 43 H12 2 1.077110 0.250749 -0.049536 11.00000 -1.20000 AFIX 0 C13 1 0.977517 0.198579 0.080630 11.00000 0.02068 0.04154 = 0.02525 -0.00072 0.00336 -0.01091 C14 1 1.063899 0.302816 0.111564 11.00000 0.03856 0.03129 = 0.06855 0.00244 0.00754 -0.00810 AFIX 43 H14 2 1.032273 0.388166 0.100548 11.00000 -1.20000 AFIX 0 C15 1 1.190275 0.282378 0.156388 11.00000 0.02892 0.06750 = 0.07201 -0.00017 -0.00567 0.00130 AFIX 43 H15 2 1.243629 0.353982 0.177890 11.00000 -1.20000 AFIX 0 C16 1 1.243608 0.162376 0.171728 11.00000 0.03967 0.07614 = 0.02976 -0.00789 -0.01020 0.01571 AFIX 43 H16 2 1.334854 0.149012 0.201480 11.00000 -1.20000 AFIX 0 C17 1 1.156582 0.057626 0.141204 11.00000 0.04657 0.05094 = 0.04902 0.00196 -0.00409 0.02240 AFIX 43 H17 2 1.189250 -0.027391 0.152382 11.00000 -1.20000 AFIX 0 C18 1 1.029546 0.075593 0.097031 11.00000 0.04591 0.03101 = 0.04152 -0.00430 0.00399 0.00331 AFIX 43 H18 2 0.975019 0.003615 0.076907 11.00000 -1.20000 AFIX 0 BR1 3 0.574679 -0.071617 0.150664 11.00000 0.05604 0.04223 = 0.02886 0.00435 0.00311 -0.00237 O1 4 0.720157 0.105896 0.009172 11.00000 0.04899 0.02304 = 0.03228 0.00163 0.00596 -0.00339 O2 4 0.419187 0.141515 0.026210 11.00000 0.02548 0.01641 = 0.06294 -0.00062 0.01475 0.00513 P1 5 0.813442 0.226457 0.018841 11.00000 0.02151 0.02325 = 0.02822 0.00109 0.00675 -0.00160 U1 6 0.500000 0.000000 0.000000 10.50000 0.03278 0.02165 = 0.02588 0.00039 0.00701 -0.00256 HKLF 4 1.0 1.00 0.00 0.00 0.00 -1.00 0.00 0.00 0.00 -1.00 REM eha173 in P21/c REM R1 = 0.1019 for 2831 Fo > 4sig(Fo) and 0.1176 for all 3022 data REM 205 parameters refined using 0 restraints END WGHT 0.1479 91.3797 REM Highest difference peak 4.587, deepest hole -2.643, 1-sigma level 0.574 Q1 1 0.5219 0.0007 0.0544 11.00000 0.05 4.59 Q2 1 0.3412 0.0743 -0.0024 11.00000 0.05 2.48 Q3 1 0.5682 -0.0673 0.1008 11.00000 0.05 2.26 Q4 1 0.6044 0.0603 0.0030 11.00000 0.05 2.07 Q5 1 0.6017 -0.0739 0.2059 11.00000 0.05 1.89 ; _database_code_depnum_ccdc_archive 'CCDC 959954' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound_5 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H60 I3 Li O4 P4' _chemical_formula_weight 1500.72 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' Li Li -0.0003 0.0001 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _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. ; 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' _cell_length_a 16.4991(9) _cell_length_b 23.6236(12) _cell_length_c 23.0801(9) _cell_angle_alpha 90 _cell_angle_beta 132.690(2) _cell_angle_gamma 90 _cell_volume 6612.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_F_000 2984 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_absorpt_coefficient_mu 1.562 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.4819 _exptl_absorpt_correction_T_max 0.4904 _exptl_absorpt_process_details ; Interpolation using Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3 for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959) p.302; Table 5.3.6 B for muR in the range 2.6-10.0. The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975) A31,146-148) is used with some modification. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'AFC12 (Right): Kappa 3 circle' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 103271 _diffrn_reflns_av_unetI/netI 0.0391 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.478 _diffrn_reflns_theta_max 27.920 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 15824 _reflns_number_gt 11085 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'SHELXL-97 (Sheldrick, 2008)' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Mercury 2.3' _computing_publication_material 'Mercury 2.3' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+12.2628P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 15824 _refine_ls_number_parameters 767 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.0967 _refine_ls_wR_factor_gt 0.0832 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 C1 C 0.7061(3) 0.62731(16) 0.1722(2) 0.0311(8) Uani 1 1 d . . . . . C2 C 0.6292(7) 0.5824(4) 0.1509(6) 0.039(2) Uani 0.565(10) 1 d . . P A 1 H2 H 0.5651 0.5755 0.0972 0.046 Uiso 0.565(10) 1 calc R U P A 1 C2A C 0.6212(10) 0.6080(6) 0.1622(8) 0.039(2) Uani 0.435(10) 1 d . . P A 2 H2A H 0.5481 0.6184 0.1164 0.046 Uiso 0.435(10) 1 calc R U P A 2 C3 C 0.6517(10) 0.5500(5) 0.2108(8) 0.046(3) Uani 0.565(10) 1 d . . P A 1 H3 H 0.6018 0.5213 0.1984 0.055 Uiso 0.565(10) 1 calc R U P A 1 C3A C 0.6389(15) 0.5736(6) 0.2174(12) 0.046(3) Uani 0.435(10) 1 d . . P A 2 H3A H 0.5775 0.5586 0.2081 0.055 Uiso 0.435(10) 1 calc R U P A 2 C4 C 0.7468(3) 0.55978(18) 0.2882(2) 0.0411(9) Uani 1 1 d . . . . . H4 H 0.7559 0.5429 0.3297 0.049 Uiso 1 1 calc R U . A 1 C5 C 0.8273(3) 0.59348(19) 0.3051(2) 0.0490(11) Uani 1 1 d . . . . . H5 H 0.8980 0.5939 0.3570 0.059 Uiso 1 1 calc R U . . . C6 C 0.8074(3) 0.62705(18) 0.2477(2) 0.0439(10) Uani 1 1 d . . . . . H6 H 0.8648 0.6503 0.2606 0.053 Uiso 1 1 calc R U . . . C7 C 0.7916(3) 0.71368(15) 0.13685(19) 0.0272(7) Uani 1 1 d . . . . . C8 C 0.7858(3) 0.77022(18) 0.1506(3) 0.0498(11) Uani 1 1 d . . . . . H8 H 0.7201 0.7844 0.1358 0.060 Uiso 1 1 calc R U . . . C9 C 0.8746(4) 0.80582(19) 0.1854(3) 0.0635(14) Uani 1 1 d . . . . . H9 H 0.8700 0.8442 0.1951 0.076 Uiso 1 1 calc R U . . . C10 C 0.9701(3) 0.78593(17) 0.2064(3) 0.0475(10) Uani 1 1 d . . . . . H10 H 1.0309 0.8106 0.2300 0.057 Uiso 1 1 calc R U . . . C11 C 0.9768(3) 0.72999(17) 0.1928(2) 0.0374(9) Uani 1 1 d . . . . . H11 H 1.0424 0.7161 0.2071 0.045 Uiso 1 1 calc R U . . . C12 C 0.8886(3) 0.69423(15) 0.1586(2) 0.0302(8) Uani 1 1 d . . . . . H12 H 0.8941 0.6557 0.1497 0.036 Uiso 1 1 calc R U . . . C13 C 0.6481(3) 0.62209(15) 0.02367(19) 0.0280(7) Uani 1 1 d . . . . . C14 C 0.7170(3) 0.57691(16) 0.0441(2) 0.0352(8) Uani 1 1 d . . . . . H14 H 0.7811 0.5706 0.0980 0.042 Uiso 1 1 calc R U . . . C15 C 0.6933(3) 0.54101(16) -0.0130(2) 0.0410(9) Uani 1 1 d . . . . . H15 H 0.7417 0.5106 0.0015 0.049 Uiso 1 1 calc R U . . . C16 C 0.5992(3) 0.54937(18) -0.0910(2) 0.0436(10) Uani 1 1 d . . . . . H16 H 0.5826 0.5245 -0.1302 0.052 Uiso 1 1 calc R U . . . C17 C 0.5293(3) 0.59371(19) -0.1125(2) 0.0438(10) Uani 1 1 d . . . . . H17 H 0.4642 0.5989 -0.1663 0.053 Uiso 1 1 calc R U . . . C18 C 0.5537(3) 0.63087(18) -0.0557(2) 0.0364(9) Uani 1 1 d . . . . . H18 H 0.5065 0.6620 -0.0707 0.044 Uiso 1 1 calc R U . . . C19 C 0.4843(3) 0.85161(15) 0.19278(19) 0.0274(7) Uani 1 1 d . . . . . C20 C 0.3841(3) 0.82300(18) 0.1474(2) 0.0381(9) Uani 1 1 d . . . . . H20 H 0.3798 0.7841 0.1350 0.046 Uiso 1 1 calc R U . . . C21 C 0.2905(3) 0.8518(2) 0.1203(2) 0.0465(11) Uani 1 1 d . . . . . H21 H 0.2219 0.8325 0.0891 0.056 Uiso 1 1 calc R U . . . C22 C 0.2965(3) 0.9086(2) 0.1383(2) 0.0460(11) Uani 1 1 d . . . . . H22 H 0.2326 0.9280 0.1205 0.055 Uiso 1 1 calc R U . . . C23 C 0.3958(3) 0.93683(19) 0.1821(2) 0.0425(10) Uani 1 1 d . . . . . H23 H 0.3998 0.9758 0.1939 0.051 Uiso 1 1 calc R U . . . C24 C 0.4891(3) 0.90892(16) 0.2090(2) 0.0327(8) Uani 1 1 d . . . . . H24 H 0.5569 0.9288 0.2386 0.039 Uiso 1 1 calc R U . . . C25 C 0.6760(3) 0.78542(14) 0.32256(19) 0.0251(7) Uani 1 1 d . . . . . C26 C 0.7045(3) 0.81873(16) 0.38354(19) 0.0307(8) Uani 1 1 d . . . . . H26 H 0.6852 0.8577 0.3748 0.037 Uiso 1 1 calc R U . . . C27 C 0.7611(3) 0.79510(17) 0.4570(2) 0.0351(8) Uani 1 1 d . . . . . H27 H 0.7816 0.8180 0.4990 0.042 Uiso 1 1 calc R U . . . C28 C 0.7880(3) 0.73792(17) 0.4696(2) 0.0371(9) Uani 1 1 d . . . . . H28 H 0.8266 0.7217 0.5200 0.045 Uiso 1 1 calc R U . . . C29 C 0.7587(3) 0.70461(16) 0.4087(2) 0.0353(8) Uani 1 1 d . . . . . H29 H 0.7769 0.6655 0.4173 0.042 Uiso 1 1 calc R U . . . C30 C 0.7028(3) 0.72803(15) 0.3347(2) 0.0276(7) Uani 1 1 d . . . . . H30 H 0.6832 0.7052 0.2929 0.033 Uiso 1 1 calc R U . . . C31 C 0.6861(2) 0.86511(13) 0.22937(19) 0.0241(7) Uani 1 1 d . . . . . C32 C 0.7829(3) 0.88840(16) 0.2984(2) 0.0336(8) Uani 1 1 d . . . . . H32 H 0.8125 0.8752 0.3484 0.040 Uiso 1 1 calc R U . . . C33 C 0.8355(3) 0.93115(17) 0.2933(2) 0.0399(9) Uani 1 1 d . . . . . H33 H 0.9005 0.9479 0.3401 0.048 Uiso 1 1 calc R U . . . C34 C 0.7940(3) 0.94961(16) 0.2206(2) 0.0365(8) Uani 1 1 d . . . . . H34 H 0.8306 0.9789 0.2177 0.044 Uiso 1 1 calc R U . . . C35 C 0.6998(3) 0.92561(14) 0.1526(2) 0.0319(8) Uani 1 1 d . . . . . H35 H 0.6721 0.9379 0.1028 0.038 Uiso 1 1 calc R U . . . C36 C 0.6456(3) 0.88385(14) 0.15646(19) 0.0268(7) Uani 1 1 d . . . . . H36 H 0.5803 0.8676 0.1093 0.032 Uiso 1 1 calc R U . . . C37 C 0.2335(3) 0.61335(14) -0.06412(19) 0.0271(7) Uani 1 1 d . . . . . C38 C 0.3120(3) 0.59314(17) -0.0645(2) 0.0378(9) Uani 1 1 d . . . . . H38 H 0.3869 0.6041 -0.0237 0.045 Uiso 1 1 calc R U . . . C39 C 0.2831(3) 0.55755(18) -0.1230(2) 0.0431(10) Uani 1 1 d . . . . . H39 H 0.3380 0.5439 -0.1223 0.052 Uiso 1 1 calc R U . . . C40 C 0.1747(3) 0.54158(17) -0.1828(2) 0.0439(10) Uani 1 1 d . . . . . H40 H 0.1546 0.5169 -0.2233 0.053 Uiso 1 1 calc R U . . . C41 C 0.0963(3) 0.56141(19) -0.1835(3) 0.0505(11) Uani 1 1 d . . . . . H41 H 0.0216 0.5504 -0.2247 0.061 Uiso 1 1 calc R U . . . C42 C 0.1245(3) 0.59740(16) -0.1247(2) 0.0416(10) Uani 1 1 d . . . . . H42 H 0.0692 0.6111 -0.1259 0.050 Uiso 1 1 calc R U . . . C43 C 0.1623(3) 0.70450(14) -0.02257(19) 0.0275(7) Uani 1 1 d . . . . . C44 C 0.1456(3) 0.75461(17) -0.0609(3) 0.0437(10) Uani 1 1 d . . . . . H44 H 0.1944 0.7650 -0.0677 0.052 Uiso 1 1 calc R U . . . C45 C 0.0583(3) 0.78926(18) -0.0892(3) 0.0555(13) Uani 1 1 d . . . . . H45 H 0.0464 0.8231 -0.1162 0.067 Uiso 1 1 calc R U . . . C46 C -0.0116(3) 0.77529(18) -0.0786(3) 0.0538(12) Uani 1 1 d . . . . . H46 H -0.0715 0.7995 -0.0982 0.065 Uiso 1 1 calc R U . . . C47 C 0.0050(3) 0.72580(19) -0.0393(3) 0.0487(11) Uani 1 1 d . . . . . H47 H -0.0429 0.7162 -0.0315 0.058 Uiso 1 1 calc R U . . . C48 C 0.0919(3) 0.69052(16) -0.0117(2) 0.0371(9) Uani 1 1 d . . . . . H48 H 0.1032 0.6565 0.0150 0.045 Uiso 1 1 calc R U . . . C49 C 0.3262(3) 0.62385(14) 0.09746(19) 0.0259(7) Uani 1 1 d . . . . . C50 C 0.2698(3) 0.57811(15) 0.0934(2) 0.0314(8) Uani 1 1 d . . . . . H50 H 0.2044 0.5648 0.0436 0.038 Uiso 1 1 calc R U . . . C51 C 0.3081(3) 0.55184(17) 0.1616(2) 0.0397(9) Uani 1 1 d . . . . . H51 H 0.2687 0.5209 0.1587 0.048 Uiso 1 1 calc R U . . . C52 C 0.4040(3) 0.5707(2) 0.2340(2) 0.0462(11) Uani 1 1 d . . . . . H52 H 0.4307 0.5526 0.2809 0.055 Uiso 1 1 calc R U . . . C53 C 0.4607(4) 0.6155(2) 0.2383(2) 0.0531(12) Uani 1 1 d . . . . . H53 H 0.5268 0.6280 0.2884 0.064 Uiso 1 1 calc R U . . . C54 C 0.4233(3) 0.64263(18) 0.1713(2) 0.0400(9) Uani 1 1 d . . . . . H54 H 0.4629 0.6738 0.1749 0.048 Uiso 1 1 calc R U . . . C55 C 0.2566(3) 0.88292(13) -0.10625(19) 0.0237(7) Uani 1 1 d . . . . . C56 C 0.2592(3) 0.90102(15) -0.0476(2) 0.0296(7) Uani 1 1 d . . . . . H56 H 0.3198 0.8911 0.0058 0.036 Uiso 1 1 calc R U . . . C57 C 0.1738(3) 0.93346(16) -0.0668(2) 0.0355(8) Uani 1 1 d . . . . . H57 H 0.1762 0.9459 -0.0265 0.043 Uiso 1 1 calc R U . . . C58 C 0.0851(3) 0.94772(16) -0.1443(2) 0.0363(9) Uani 1 1 d . . . . . H58 H 0.0267 0.9699 -0.1573 0.044 Uiso 1 1 calc R U . . . C59 C 0.0812(3) 0.92975(15) -0.2030(2) 0.0349(8) Uani 1 1 d . . . . . H59 H 0.0201 0.9397 -0.2562 0.042 Uiso 1 1 calc R U . . . C60 C 0.1658(3) 0.89728(14) -0.1847(2) 0.0307(8) Uani 1 1 d . . . . . H60 H 0.1622 0.8847 -0.2255 0.037 Uiso 1 1 calc R U . . . C61 C 0.4658(3) 0.88498(14) -0.06777(19) 0.0267(7) Uani 1 1 d . . . . . C62 C 0.4548(3) 0.94298(14) -0.0777(2) 0.0283(7) Uani 1 1 d . . . . . H62 H 0.3912 0.9611 -0.0933 0.034 Uiso 1 1 calc R U . . . C63 C 0.5359(3) 0.97499(16) -0.0653(2) 0.0344(8) Uani 1 1 d . . . . . H63 H 0.5274 1.0148 -0.0726 0.041 Uiso 1 1 calc R U . . . C64 C 0.6284(3) 0.94938(17) -0.0424(2) 0.0379(9) Uani 1 1 d . . . . . H64 H 0.6835 0.9715 -0.0342 0.046 Uiso 1 1 calc R U . . . C65 C 0.6415(3) 0.89166(18) -0.0313(2) 0.0432(10) Uani 1 1 d . . . . . H65 H 0.7062 0.8742 -0.0148 0.052 Uiso 1 1 calc R U . . . C66 C 0.5607(3) 0.85902(16) -0.0442(2) 0.0378(9) Uani 1 1 d . . . . . H66 H 0.5696 0.8192 -0.0372 0.045 Uiso 1 1 calc R U . . . C67 C 0.3154(3) 0.79247(14) -0.15680(19) 0.0265(7) Uani 1 1 d . . . . . C68 C 0.2887(3) 0.81049(16) -0.2255(2) 0.0365(8) Uani 1 1 d . . . . . H68 H 0.3033 0.8484 -0.2297 0.044 Uiso 1 1 calc R U . . . C69 C 0.2411(4) 0.77346(19) -0.2874(2) 0.0446(10) Uani 1 1 d . . . . . H69 H 0.2222 0.7860 -0.3344 0.054 Uiso 1 1 calc R U . . . C70 C 0.2208(3) 0.71788(18) -0.2809(2) 0.0430(10) Uani 1 1 d . . . . . H70 H 0.1874 0.6925 -0.3238 0.052 Uiso 1 1 calc R U . . . C71 C 0.2487(3) 0.69922(16) -0.2127(2) 0.0367(9) Uani 1 1 d . . . . . H71 H 0.2356 0.6610 -0.2084 0.044 Uiso 1 1 calc R U . . . C72 C 0.2956(3) 0.73620(14) -0.1507(2) 0.0285(7) Uani 1 1 d . . . . . H72 H 0.3145 0.7234 -0.1038 0.034 Uiso 1 1 calc R U . . . Li1 Li 0.4832(4) 0.7453(2) 0.0635(3) 0.0203(10) Uani 1 1 d . . . . . O1 O 0.57197(19) 0.70580(12) 0.05414(14) 0.0397(7) Uani 1 1 d . . . . . O2 O 0.5712(2) 0.76491(10) 0.17067(13) 0.0314(5) Uani 1 1 d . . . . . O3 O 0.36881(19) 0.69886(11) 0.03216(15) 0.0366(6) Uani 1 1 d . . . . . O4 O 0.42256(19) 0.81052(10) -0.00162(13) 0.0323(6) Uani 1 1 d . . . . . P1 P 0.67220(7) 0.67074(4) 0.09395(5) 0.02795(19) Uani 1 1 d . . . . . P2 P 0.60322(7) 0.81245(4) 0.22514(5) 0.02360(17) Uani 1 1 d . . . . . P3 P 0.27909(6) 0.66281(4) 0.01247(5) 0.02467(18) Uani 1 1 d . . . . . P4 P 0.36930(7) 0.83992(3) -0.07706(5) 0.02397(18) Uani 1 1 d . . . . . I1 I 0.98331(2) 0.58936(2) 0.57897(2) 0.06029(10) Uani 1 1 d . . . . . I2 I 1.0000 0.5000 0.5000 0.04490(11) Uani 1 2 d S . P . . I3 I 0.00803(2) 0.90961(2) 0.58948(2) 0.04332(7) Uani 1 1 d . . . . . I4 I 0.0000 1.0000 0.5000 0.03039(8) Uani 1 2 d S . P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0253(16) 0.046(2) 0.0243(16) 0.0036(16) 0.0177(14) 0.0048(15) C2 0.025(2) 0.050(6) 0.027(3) -0.003(4) 0.012(2) -0.013(4) C2A 0.025(2) 0.050(6) 0.027(3) -0.003(4) 0.012(2) -0.013(4) C3 0.032(4) 0.054(8) 0.044(3) 0.011(6) 0.022(2) -0.009(5) C3A 0.032(4) 0.054(8) 0.044(3) 0.011(6) 0.022(2) -0.009(5) C4 0.038(2) 0.049(2) 0.034(2) 0.0065(19) 0.0235(17) -0.0033(17) C5 0.034(2) 0.064(3) 0.0245(18) 0.012(2) 0.0099(16) -0.0079(19) C6 0.0327(19) 0.053(2) 0.0274(18) 0.0070(18) 0.0129(16) -0.0117(17) C7 0.0264(16) 0.0314(18) 0.0232(16) 0.0021(15) 0.0166(14) 0.0083(13) C8 0.041(2) 0.039(2) 0.065(3) -0.011(2) 0.034(2) 0.0064(18) C9 0.058(3) 0.034(2) 0.095(4) -0.017(3) 0.051(3) 0.002(2) C10 0.045(2) 0.032(2) 0.058(3) -0.005(2) 0.032(2) -0.0026(17) C11 0.0303(18) 0.039(2) 0.042(2) 0.0014(18) 0.0237(17) 0.0038(15) C12 0.0297(17) 0.0269(17) 0.0322(18) 0.0019(15) 0.0203(15) 0.0090(14) C13 0.0275(16) 0.0362(19) 0.0268(17) -0.0041(15) 0.0210(15) -0.0045(14) C14 0.0370(19) 0.0321(19) 0.0338(19) 0.0018(16) 0.0229(17) 0.0017(15) C15 0.052(2) 0.0287(19) 0.049(2) -0.0096(18) 0.036(2) -0.0055(17) C16 0.051(2) 0.041(2) 0.045(2) -0.016(2) 0.036(2) -0.0190(19) C17 0.036(2) 0.060(3) 0.0302(19) -0.012(2) 0.0202(17) -0.0128(19) C18 0.0264(17) 0.052(2) 0.0307(18) -0.0011(18) 0.0192(16) -0.0024(16) C19 0.0255(16) 0.0311(18) 0.0215(16) 0.0052(14) 0.0142(14) 0.0044(13) C20 0.0304(18) 0.046(2) 0.0337(19) 0.0049(18) 0.0203(16) -0.0021(16) C21 0.0257(18) 0.072(3) 0.037(2) 0.011(2) 0.0193(17) -0.0010(19) C22 0.035(2) 0.072(3) 0.039(2) 0.025(2) 0.0284(18) 0.023(2) C23 0.046(2) 0.045(2) 0.041(2) 0.0123(19) 0.032(2) 0.0174(18) C24 0.0303(17) 0.035(2) 0.0297(18) 0.0032(16) 0.0192(15) 0.0056(15) C25 0.0236(15) 0.0246(16) 0.0241(16) 0.0020(14) 0.0150(13) 0.0001(12) C26 0.0358(18) 0.0315(19) 0.0262(17) -0.0006(15) 0.0216(15) 0.0045(15) C27 0.0382(19) 0.046(2) 0.0261(17) -0.0036(17) 0.0238(16) -0.0007(17) C28 0.0356(19) 0.047(2) 0.0241(17) 0.0077(17) 0.0183(16) 0.0020(16) C29 0.0359(19) 0.0294(19) 0.0324(19) 0.0051(16) 0.0199(16) -0.0003(15) C30 0.0267(16) 0.0259(16) 0.0266(17) -0.0021(15) 0.0166(14) -0.0034(13) C31 0.0239(15) 0.0216(16) 0.0245(16) -0.0027(14) 0.0155(13) 0.0005(12) C32 0.0301(17) 0.043(2) 0.0231(16) -0.0064(16) 0.0162(15) -0.0048(15) C33 0.0345(19) 0.041(2) 0.041(2) -0.0182(19) 0.0242(18) -0.0154(16) C34 0.043(2) 0.0277(19) 0.050(2) -0.0021(18) 0.0357(19) -0.0044(15) C35 0.0366(18) 0.0247(17) 0.0337(19) 0.0029(15) 0.0235(16) 0.0023(14) C36 0.0280(16) 0.0242(17) 0.0239(16) -0.0028(14) 0.0159(14) -0.0004(13) C37 0.0255(16) 0.0239(16) 0.0271(17) 0.0036(14) 0.0160(14) -0.0012(13) C38 0.0272(17) 0.051(2) 0.0311(18) -0.0027(18) 0.0182(16) -0.0014(16) C39 0.048(2) 0.048(2) 0.042(2) 0.002(2) 0.034(2) 0.0048(19) C40 0.055(2) 0.034(2) 0.036(2) -0.0068(18) 0.028(2) -0.0018(18) C41 0.032(2) 0.049(2) 0.047(2) -0.024(2) 0.0169(19) -0.0120(18) C42 0.0251(17) 0.039(2) 0.048(2) -0.0123(19) 0.0199(17) -0.0047(15) C43 0.0208(15) 0.0267(17) 0.0280(17) -0.0005(14) 0.0138(14) -0.0022(12) C44 0.0338(19) 0.037(2) 0.055(2) 0.016(2) 0.0281(19) 0.0032(16) C45 0.039(2) 0.038(2) 0.073(3) 0.024(2) 0.031(2) 0.0071(18) C46 0.036(2) 0.036(2) 0.077(3) 0.009(2) 0.033(2) 0.0097(17) C47 0.037(2) 0.049(2) 0.067(3) 0.005(2) 0.038(2) 0.0018(18) C48 0.0355(19) 0.0300(19) 0.049(2) 0.0059(18) 0.0300(18) 0.0020(15) C49 0.0239(15) 0.0302(18) 0.0251(16) -0.0002(14) 0.0171(14) 0.0018(13) C50 0.0290(17) 0.0324(19) 0.0305(18) 0.0052(16) 0.0192(15) 0.0012(14) C51 0.043(2) 0.039(2) 0.048(2) 0.0155(19) 0.035(2) 0.0124(17) C52 0.053(2) 0.059(3) 0.035(2) 0.018(2) 0.033(2) 0.024(2) C53 0.048(2) 0.066(3) 0.026(2) -0.003(2) 0.0173(19) 0.000(2) C54 0.0314(19) 0.048(2) 0.0290(19) -0.0043(18) 0.0159(16) -0.0045(17) C55 0.0278(16) 0.0163(15) 0.0267(16) 0.0021(13) 0.0184(14) -0.0007(12) C56 0.0295(17) 0.0301(18) 0.0265(17) 0.0007(15) 0.0179(15) -0.0011(14) C57 0.040(2) 0.0327(19) 0.042(2) -0.0042(17) 0.0308(18) 0.0006(15) C58 0.0297(18) 0.0308(19) 0.047(2) 0.0017(18) 0.0252(17) 0.0024(14) C59 0.0299(17) 0.0284(18) 0.0320(18) 0.0032(16) 0.0153(15) 0.0009(14) C60 0.0360(18) 0.0239(17) 0.0273(17) 0.0020(14) 0.0195(15) 0.0017(14) C61 0.0281(16) 0.0254(17) 0.0250(16) -0.0026(14) 0.0174(14) -0.0013(13) C62 0.0316(17) 0.0239(17) 0.0304(17) 0.0010(15) 0.0213(15) 0.0002(13) C63 0.043(2) 0.0275(18) 0.0331(19) -0.0020(16) 0.0256(17) -0.0075(15) C64 0.041(2) 0.045(2) 0.038(2) -0.0122(19) 0.0309(18) -0.0143(17) C65 0.035(2) 0.050(2) 0.051(2) -0.014(2) 0.0313(19) -0.0022(17) C66 0.0342(19) 0.0298(19) 0.045(2) -0.0090(17) 0.0250(18) 0.0018(15) C67 0.0283(16) 0.0226(16) 0.0279(17) -0.0016(14) 0.0188(15) 0.0001(13) C68 0.046(2) 0.032(2) 0.0337(19) -0.0034(17) 0.0279(18) -0.0047(16) C69 0.060(3) 0.050(2) 0.037(2) -0.009(2) 0.038(2) -0.006(2) C70 0.049(2) 0.041(2) 0.045(2) -0.017(2) 0.034(2) -0.0096(18) C71 0.040(2) 0.0256(18) 0.045(2) -0.0077(17) 0.0286(18) -0.0068(15) C72 0.0285(17) 0.0245(17) 0.0288(17) -0.0031(14) 0.0179(15) -0.0028(13) Li1 0.018(2) 0.020(2) 0.019(2) 0.000(2) 0.010(2) -0.0007(19) O1 0.0278(12) 0.0621(18) 0.0283(13) 0.0052(13) 0.0188(11) 0.0184(12) O2 0.0371(13) 0.0242(12) 0.0222(11) -0.0043(10) 0.0158(11) -0.0023(10) O3 0.0250(12) 0.0418(15) 0.0360(13) -0.0031(12) 0.0179(11) -0.0132(10) O4 0.0387(13) 0.0237(12) 0.0239(12) 0.0030(10) 0.0171(11) 0.0021(10) P1 0.0218(4) 0.0390(5) 0.0227(4) 0.0035(4) 0.0149(3) 0.0086(4) P2 0.0239(4) 0.0224(4) 0.0186(4) -0.0014(3) 0.0121(3) -0.0001(3) P3 0.0181(4) 0.0260(4) 0.0250(4) -0.0007(4) 0.0126(3) -0.0053(3) P4 0.0282(4) 0.0166(4) 0.0228(4) 0.0012(3) 0.0156(4) 0.0012(3) I1 0.04855(17) 0.05386(19) 0.05983(19) 0.01140(16) 0.02932(15) -0.00026(13) I2 0.02208(15) 0.0490(2) 0.03322(17) 0.01896(17) 0.00665(13) -0.00717(14) I3 0.04414(14) 0.04826(16) 0.04126(14) 0.00750(13) 0.03043(12) 0.00078(12) I4 0.02773(15) 0.03800(18) 0.02211(14) -0.00099(14) 0.01557(12) 0.00552(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C1 C2A 1.337(13) . ? C1 C6 1.371(5) . ? C1 C2 1.460(10) . ? C1 P1 1.804(4) . ? C2 C3 1.393(17) . ? C2A C3A 1.37(2) . ? C3 C4 1.380(14) . ? C3A C4 1.414(18) . ? C4 C5 1.359(5) . ? C5 C6 1.379(5) . ? C7 C8 1.391(5) . ? C7 C12 1.392(4) . ? C7 P1 1.801(4) . ? C8 C9 1.380(6) . ? C9 C10 1.381(6) . ? C10 C11 1.379(6) . ? C11 C12 1.377(5) . ? C13 C14 1.387(5) . ? C13 C18 1.398(5) . ? C13 P1 1.799(4) . ? C14 C15 1.382(5) . ? C15 C16 1.379(6) . ? C16 C17 1.378(6) . ? C17 C18 1.392(5) . ? C19 C24 1.392(5) . ? C19 C20 1.393(5) . ? C19 P2 1.809(3) . ? C20 C21 1.389(5) . ? C21 C22 1.388(6) . ? C22 C23 1.379(6) . ? C23 C24 1.377(5) . ? C25 C26 1.387(5) . ? C25 C30 1.395(5) . ? C25 P2 1.801(3) . ? C26 C27 1.383(5) . ? C27 C28 1.390(5) . ? C28 C29 1.381(5) . ? C29 C30 1.392(5) . ? C31 C32 1.393(4) . ? C31 C36 1.396(5) . ? C31 P2 1.802(3) . ? C32 C33 1.389(5) . ? C33 C34 1.385(6) . ? C34 C35 1.376(5) . ? C35 C36 1.374(5) . ? C37 C42 1.386(5) . ? C37 C38 1.387(5) . ? C37 P3 1.804(4) . ? C38 C39 1.372(5) . ? C39 C40 1.378(6) . ? C40 C41 1.366(6) . ? C41 C42 1.387(6) . ? C43 C48 1.386(5) . ? C43 C44 1.389(5) . ? C43 P3 1.795(3) . ? C44 C45 1.377(6) . ? C45 C46 1.371(6) . ? C46 C47 1.388(6) . ? C47 C48 1.384(5) . ? C49 C50 1.388(5) . ? C49 C54 1.401(5) . ? C49 P3 1.798(3) . ? C50 C51 1.382(5) . ? C51 C52 1.382(6) . ? C52 C53 1.370(6) . ? C53 C54 1.376(6) . ? C55 C56 1.392(5) . ? C55 C60 1.400(4) . ? C55 P4 1.802(3) . ? C56 C57 1.387(5) . ? C57 C58 1.381(5) . ? C58 C59 1.378(5) . ? C59 C60 1.384(5) . ? C61 C62 1.381(5) . ? C61 C66 1.404(5) . ? C61 P4 1.803(3) . ? C62 C63 1.387(5) . ? C63 C64 1.372(5) . ? C64 C65 1.377(6) . ? C65 C66 1.386(5) . ? C67 C68 1.394(5) . ? C67 C72 1.398(5) . ? C67 P4 1.793(3) . ? C68 C69 1.379(5) . ? C69 C70 1.388(6) . ? C70 C71 1.379(6) . ? C71 C72 1.381(5) . ? Li1 O3 1.854(5) . ? Li1 O1 1.868(6) . ? Li1 O2 1.889(5) . ? Li1 O4 1.896(6) . ? O1 P1 1.485(2) . ? O2 P2 1.490(2) . ? O3 P3 1.487(2) . ? O4 P4 1.487(2) . ? I1 I2 2.9215(4) . ? I2 I1 2.9214(4) 3_766 ? I3 I4 2.9105(3) . ? I4 I3 2.9104(3) 3_576 ? 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 C2A C1 C6 116.7(6) . . ? C6 C1 C2 117.2(5) . . ? C2A C1 P1 116.3(6) . . ? C6 C1 P1 123.9(3) . . ? C2 C1 P1 117.8(4) . . ? C3 C2 C1 118.6(8) . . ? C1 C2A C3A 120.4(12) . . ? C4 C3 C2 119.8(10) . . ? C2A C3A C4 121.4(14) . . ? C5 C4 C3 120.0(7) . . ? C5 C4 C3A 114.5(8) . . ? C4 C5 C6 120.8(4) . . ? C1 C6 C5 120.9(4) . . ? C8 C7 C12 118.4(3) . . ? C8 C7 P1 116.6(3) . . ? C12 C7 P1 125.0(3) . . ? C9 C8 C7 120.5(4) . . ? C8 C9 C10 120.4(4) . . ? C11 C10 C9 119.6(4) . . ? C12 C11 C10 120.2(4) . . ? C11 C12 C7 120.9(3) . . ? C14 C13 C18 119.2(3) . . ? C14 C13 P1 123.7(3) . . ? C18 C13 P1 117.1(3) . . ? C15 C14 C13 120.7(4) . . ? C16 C15 C14 119.9(4) . . ? C17 C16 C15 120.3(4) . . ? C16 C17 C18 120.3(4) . . ? C17 C18 C13 119.6(4) . . ? C24 C19 C20 119.7(3) . . ? C24 C19 P2 122.6(3) . . ? C20 C19 P2 117.7(3) . . ? C21 C20 C19 119.4(4) . . ? C22 C21 C20 120.5(4) . . ? C23 C22 C21 119.6(4) . . ? C24 C23 C22 120.6(4) . . ? C23 C24 C19 120.1(4) . . ? C26 C25 C30 120.4(3) . . ? C26 C25 P2 123.1(3) . . ? C30 C25 P2 116.5(3) . . ? C27 C26 C25 119.9(3) . . ? C26 C27 C28 120.2(3) . . ? C29 C28 C27 120.0(3) . . ? C28 C29 C30 120.4(3) . . ? C29 C30 C25 119.2(3) . . ? C32 C31 C36 119.6(3) . . ? C32 C31 P2 125.0(3) . . ? C36 C31 P2 115.4(2) . . ? C33 C32 C31 119.2(3) . . ? C34 C33 C32 120.6(3) . . ? C35 C34 C33 120.0(3) . . ? C36 C35 C34 120.2(3) . . ? C35 C36 C31 120.4(3) . . ? C42 C37 C38 118.6(3) . . ? C42 C37 P3 123.9(3) . . ? C38 C37 P3 117.3(3) . . ? C39 C38 C37 121.0(3) . . ? C38 C39 C40 120.1(4) . . ? C41 C40 C39 119.6(4) . . ? C40 C41 C42 120.8(4) . . ? C37 C42 C41 119.9(4) . . ? C48 C43 C44 119.3(3) . . ? C48 C43 P3 124.3(3) . . ? C44 C43 P3 116.4(3) . . ? C45 C44 C43 120.1(4) . . ? C46 C45 C44 120.6(4) . . ? C45 C46 C47 120.1(4) . . ? C48 C47 C46 119.6(4) . . ? C47 C48 C43 120.4(4) . . ? C50 C49 C54 119.3(3) . . ? C50 C49 P3 123.5(3) . . ? C54 C49 P3 117.2(3) . . ? C51 C50 C49 120.3(3) . . ? C52 C51 C50 119.8(4) . . ? C53 C52 C51 120.2(4) . . ? C52 C53 C54 121.0(4) . . ? C53 C54 C49 119.4(4) . . ? C56 C55 C60 119.0(3) . . ? C56 C55 P4 117.8(2) . . ? C60 C55 P4 123.2(3) . . ? C57 C56 C55 120.3(3) . . ? C58 C57 C56 120.2(4) . . ? C59 C58 C57 120.0(3) . . ? C58 C59 C60 120.4(3) . . ? C59 C60 C55 120.1(3) . . ? C62 C61 C66 119.0(3) . . ? C62 C61 P4 124.0(3) . . ? C66 C61 P4 116.9(3) . . ? C61 C62 C63 120.4(3) . . ? C64 C63 C62 120.3(4) . . ? C63 C64 C65 120.1(4) . . ? C64 C65 C66 120.2(4) . . ? C65 C66 C61 119.9(4) . . ? C68 C67 C72 119.3(3) . . ? C68 C67 P4 122.1(3) . . ? C72 C67 P4 118.6(3) . . ? C69 C68 C67 120.2(4) . . ? C68 C69 C70 119.9(4) . . ? C71 C70 C69 120.5(4) . . ? C70 C71 C72 119.9(4) . . ? C71 C72 C67 120.2(3) . . ? O3 Li1 O1 109.3(3) . . ? O3 Li1 O2 109.4(3) . . ? O1 Li1 O2 107.9(3) . . ? O3 Li1 O4 108.7(3) . . ? O1 Li1 O4 110.3(3) . . ? O2 Li1 O4 111.2(3) . . ? P1 O1 Li1 147.0(2) . . ? P2 O2 Li1 143.9(2) . . ? P3 O3 Li1 175.8(2) . . ? P4 O4 Li1 152.0(2) . . ? O1 P1 C13 109.02(15) . . ? O1 P1 C7 111.71(16) . . ? C13 P1 C7 110.25(15) . . ? O1 P1 C1 113.35(16) . . ? C13 P1 C1 105.55(17) . . ? C7 P1 C1 106.77(16) . . ? O2 P2 C25 109.95(15) . . ? O2 P2 C31 112.83(15) . . ? C25 P2 C31 109.77(15) . . ? O2 P2 C19 111.85(15) . . ? C25 P2 C19 108.35(16) . . ? C31 P2 C19 103.87(15) . . ? O3 P3 C43 111.42(16) . . ? O3 P3 C49 110.82(15) . . ? C43 P3 C49 108.09(16) . . ? O3 P3 C37 109.75(16) . . ? C43 P3 C37 107.87(15) . . ? C49 P3 C37 108.80(16) . . ? O4 P4 C67 113.45(15) . . ? O4 P4 C55 109.98(15) . . ? C67 P4 C55 107.51(15) . . ? O4 P4 C61 111.31(15) . . ? C67 P4 C61 105.93(16) . . ? C55 P4 C61 108.44(15) . . ? I1 I2 I1 180.0 3_766 . ? I3 I4 I3 180.0 3_576 . ? _refine_diff_density_max 1.673 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.090 _iucr_refine_instructions_details ; TITL mo_eha110713_0m CELL 0.71073 16.4991 23.6236 23.0801 90.000 132.690 90.000 ZERR 4.00 0.0009 0.0012 0.0009 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H LI O P I UNIT 288 240 4 16 16 12 MERG 2 FMAP 2 PLAN -5 ACTA L.S. 24 TEMP -170.00 WGHT 0.030800 12.262800 FVAR 0.03369 0.56496 0.02498 0.05036 0.02736 -0.00301 0.01241 FVAR -0.01295 0.03229 0.05365 0.04374 0.01076 0.02245 -0.00867 C1 1 0.706132 0.627314 0.172168 11.00000 0.02525 0.04602 = 0.02425 0.00360 0.01770 0.00479 PART 1 C2 1 0.629222 0.582429 0.150868 21.00000 31.00000 41.00000 = 51.00000 61.00000 71.00000 81.00000 AFIX 43 H2 2 0.565119 0.575467 0.097238 21.00000 -1.20000 AFIX 0 PART 2 C2A 1 0.621190 0.608042 0.162186 -21.00000 31.00000 41.00000 = 51.00000 61.00000 71.00000 81.00000 AFIX 43 H2A 2 0.548063 0.618359 0.116433 -21.00000 -1.20000 AFIX 0 PART 1 C3 1 0.651733 0.550019 0.210771 21.00000 91.00000 101.00000 = 111.00000 121.00000 131.00000 141.00000 AFIX 43 H3 2 0.601803 0.521260 0.198379 21.00000 -1.20000 AFIX 0 PART 2 C3A 1 0.638946 0.573580 0.217427 -21.00000 91.00000 101.00000 = 111.00000 121.00000 131.00000 141.00000 AFIX 43 H3A 2 0.577523 0.558577 0.208070 -21.00000 -1.20000 AFIX 0 PART 0 C4 1 0.746777 0.559780 0.288203 11.00000 0.03760 0.04946 = 0.03418 0.00655 0.02352 -0.00331 AFIX 43 H4 2 0.755936 0.542943 0.329711 11.00000 -1.20000 AFIX 0 C5 1 0.827261 0.593480 0.305066 11.00000 0.03380 0.06366 = 0.02455 0.01232 0.00988 -0.00786 AFIX 43 H5 2 0.898029 0.593920 0.357011 11.00000 -1.20000 AFIX 0 C6 1 0.807436 0.627046 0.247675 11.00000 0.03268 0.05291 = 0.02738 0.00704 0.01288 -0.01167 AFIX 43 H6 2 0.864769 0.650308 0.260638 11.00000 -1.20000 AFIX 0 C7 1 0.791583 0.713684 0.136847 11.00000 0.02639 0.03143 = 0.02321 0.00206 0.01661 0.00826 C8 1 0.785760 0.770216 0.150578 11.00000 0.04101 0.03868 = 0.06496 -0.01089 0.03400 0.00644 AFIX 43 H8 2 0.720087 0.784429 0.135828 11.00000 -1.20000 AFIX 0 C9 1 0.874583 0.805820 0.185446 11.00000 0.05802 0.03389 = 0.09520 -0.01657 0.05062 0.00235 AFIX 43 H9 2 0.869976 0.844247 0.195102 11.00000 -1.20000 AFIX 0 C10 1 0.970126 0.785929 0.206387 11.00000 0.04523 0.03237 = 0.05760 -0.00451 0.03193 -0.00263 AFIX 43 H10 2 1.030934 0.810624 0.229993 11.00000 -1.20000 AFIX 0 C11 1 0.976775 0.729989 0.192832 11.00000 0.03030 0.03873 = 0.04150 0.00138 0.02372 0.00382 AFIX 43 H11 2 1.042350 0.716108 0.207148 11.00000 -1.20000 AFIX 0 C12 1 0.888630 0.694228 0.158614 11.00000 0.02974 0.02688 = 0.03224 0.00192 0.02032 0.00899 AFIX 43 H12 2 0.894125 0.655731 0.149734 11.00000 -1.20000 AFIX 0 C13 1 0.648117 0.622088 0.023669 11.00000 0.02754 0.03621 = 0.02683 -0.00407 0.02100 -0.00451 C14 1 0.716962 0.576910 0.044128 11.00000 0.03695 0.03213 = 0.03385 0.00184 0.02291 0.00168 AFIX 43 H14 2 0.781063 0.570584 0.097954 11.00000 -1.20000 AFIX 0 C15 1 0.693269 0.541009 -0.012980 11.00000 0.05154 0.02868 = 0.04889 -0.00957 0.03644 -0.00548 AFIX 43 H15 2 0.741675 0.510626 0.001525 11.00000 -1.20000 AFIX 0 C16 1 0.599248 0.549372 -0.091038 11.00000 0.05139 0.04133 = 0.04547 -0.01641 0.03575 -0.01898 AFIX 43 H16 2 0.582614 0.524456 -0.130205 11.00000 -1.20000 AFIX 0 C17 1 0.529311 0.593705 -0.112492 11.00000 0.03618 0.05954 = 0.03015 -0.01173 0.02024 -0.01283 AFIX 43 H17 2 0.464166 0.598924 -0.166294 11.00000 -1.20000 AFIX 0 C18 1 0.553720 0.630865 -0.055667 11.00000 0.02641 0.05170 = 0.03071 -0.00109 0.01917 -0.00239 AFIX 43 H18 2 0.506499 0.662022 -0.070705 11.00000 -1.20000 AFIX 0 C19 1 0.484350 0.851609 0.192783 11.00000 0.02547 0.03110 = 0.02146 0.00521 0.01420 0.00436 C20 1 0.384105 0.822998 0.147367 11.00000 0.03044 0.04645 = 0.03371 0.00489 0.02029 -0.00214 AFIX 43 H20 2 0.379773 0.784108 0.135045 11.00000 -1.20000 AFIX 0 C21 1 0.290529 0.851840 0.120256 11.00000 0.02570 0.07192 = 0.03695 0.01105 0.01933 -0.00098 AFIX 43 H21 2 0.221917 0.832549 0.089148 11.00000 -1.20000 AFIX 0 C22 1 0.296488 0.908642 0.138265 11.00000 0.03510 0.07152 = 0.03938 0.02456 0.02841 0.02350 AFIX 43 H22 2 0.232573 0.927980 0.120497 11.00000 -1.20000 AFIX 0 C23 1 0.395755 0.936826 0.182106 11.00000 0.04577 0.04549 = 0.04127 0.01228 0.03153 0.01743 AFIX 43 H23 2 0.399758 0.975824 0.193868 11.00000 -1.20000 AFIX 0 C24 1 0.489136 0.908917 0.208980 11.00000 0.03035 0.03493 = 0.02971 0.00318 0.01916 0.00558 AFIX 43 H24 2 0.556942 0.928808 0.238627 11.00000 -1.20000 AFIX 0 C25 1 0.675964 0.785420 0.322563 11.00000 0.02355 0.02461 = 0.02407 0.00205 0.01495 0.00014 C26 1 0.704504 0.818733 0.383538 11.00000 0.03584 0.03151 = 0.02618 -0.00062 0.02156 0.00451 AFIX 43 H26 2 0.685228 0.857705 0.374849 11.00000 -1.20000 AFIX 0 C27 1 0.761092 0.795103 0.457032 11.00000 0.03817 0.04598 = 0.02607 -0.00363 0.02375 -0.00067 AFIX 43 H27 2 0.781602 0.818016 0.499037 11.00000 -1.20000 AFIX 0 C28 1 0.788025 0.737918 0.469583 11.00000 0.03556 0.04703 = 0.02407 0.00769 0.01833 0.00196 AFIX 43 H28 2 0.826563 0.721741 0.520044 11.00000 -1.20000 AFIX 0 C29 1 0.758736 0.704610 0.408659 11.00000 0.03592 0.02939 = 0.03244 0.00507 0.01993 -0.00028 AFIX 43 H29 2 0.776851 0.665486 0.417318 11.00000 -1.20000 AFIX 0 C30 1 0.702847 0.728026 0.334666 11.00000 0.02667 0.02588 = 0.02663 -0.00212 0.01661 -0.00340 AFIX 43 H30 2 0.683241 0.705180 0.292894 11.00000 -1.20000 AFIX 0 C31 1 0.686101 0.865109 0.229373 11.00000 0.02385 0.02161 = 0.02453 -0.00274 0.01548 0.00046 C32 1 0.782859 0.888397 0.298436 11.00000 0.03013 0.04281 = 0.02309 -0.00636 0.01615 -0.00481 AFIX 43 H32 2 0.812453 0.875193 0.348414 11.00000 -1.20000 AFIX 0 C33 1 0.835484 0.931153 0.293282 11.00000 0.03453 0.04141 = 0.04067 -0.01815 0.02420 -0.01538 AFIX 43 H33 2 0.900531 0.947889 0.340061 11.00000 -1.20000 AFIX 0 C34 1 0.794003 0.949609 0.220579 11.00000 0.04293 0.02768 = 0.04969 -0.00212 0.03565 -0.00437 AFIX 43 H34 2 0.830620 0.978862 0.217650 11.00000 -1.20000 AFIX 0 C35 1 0.699779 0.925609 0.152567 11.00000 0.03656 0.02473 = 0.03370 0.00292 0.02352 0.00229 AFIX 43 H35 2 0.672072 0.937944 0.102767 11.00000 -1.20000 AFIX 0 C36 1 0.645632 0.883851 0.156461 11.00000 0.02804 0.02418 = 0.02393 -0.00284 0.01594 -0.00038 AFIX 43 H36 2 0.580301 0.867640 0.109287 11.00000 -1.20000 AFIX 0 C37 1 0.233494 0.613346 -0.064124 11.00000 0.02550 0.02390 = 0.02715 0.00357 0.01600 -0.00116 C38 1 0.312020 0.593136 -0.064527 11.00000 0.02716 0.05115 = 0.03113 -0.00275 0.01821 -0.00141 AFIX 43 H38 2 0.386907 0.604085 -0.023728 11.00000 -1.20000 AFIX 0 C39 1 0.283114 0.557551 -0.123006 11.00000 0.04791 0.04816 = 0.04248 0.00209 0.03429 0.00484 AFIX 43 H39 2 0.337965 0.543896 -0.122270 11.00000 -1.20000 AFIX 0 C40 1 0.174677 0.541575 -0.182812 11.00000 0.05515 0.03386 = 0.03569 -0.00676 0.02797 -0.00183 AFIX 43 H40 2 0.154581 0.516930 -0.223316 11.00000 -1.20000 AFIX 0 C41 1 0.096308 0.561408 -0.183463 11.00000 0.03156 0.04904 = 0.04664 -0.02440 0.01689 -0.01200 AFIX 43 H41 2 0.021554 0.550420 -0.224687 11.00000 -1.20000 AFIX 0 C42 1 0.124517 0.597395 -0.124672 11.00000 0.02515 0.03891 = 0.04832 -0.01232 0.01990 -0.00470 AFIX 43 H42 2 0.069215 0.611087 -0.125914 11.00000 -1.20000 AFIX 0 C43 1 0.162346 0.704504 -0.022565 11.00000 0.02079 0.02666 = 0.02805 -0.00048 0.01381 -0.00219 C44 1 0.145563 0.754608 -0.060916 11.00000 0.03384 0.03663 = 0.05531 0.01620 0.02807 0.00316 AFIX 43 H44 2 0.194353 0.764985 -0.067669 11.00000 -1.20000 AFIX 0 C45 1 0.058256 0.789264 -0.089167 11.00000 0.03867 0.03794 = 0.07317 0.02406 0.03120 0.00714 AFIX 43 H45 2 0.046363 0.823143 -0.116208 11.00000 -1.20000 AFIX 0 C46 1 -0.011644 0.775290 -0.078603 11.00000 0.03552 0.03602 = 0.07703 0.00873 0.03301 0.00967 AFIX 43 H46 2 -0.071534 0.799509 -0.098176 11.00000 -1.20000 AFIX 0 C47 1 0.005016 0.725795 -0.039342 11.00000 0.03703 0.04920 = 0.06731 0.00462 0.03833 0.00183 AFIX 43 H47 2 -0.042893 0.716199 -0.031515 11.00000 -1.20000 AFIX 0 C48 1 0.091851 0.690518 -0.011674 11.00000 0.03554 0.03003 = 0.04909 0.00589 0.02998 0.00200 AFIX 43 H48 2 0.103235 0.656495 0.014957 11.00000 -1.20000 AFIX 0 C49 1 0.326209 0.623849 0.097463 11.00000 0.02386 0.03016 = 0.02505 -0.00020 0.01712 0.00184 C50 1 0.269763 0.578109 0.093445 11.00000 0.02901 0.03239 = 0.03046 0.00523 0.01924 0.00123 AFIX 43 H50 2 0.204442 0.564794 0.043606 11.00000 -1.20000 AFIX 0 C51 1 0.308138 0.551836 0.161615 11.00000 0.04317 0.03926 = 0.04772 0.01550 0.03526 0.01239 AFIX 43 H51 2 0.268717 0.520889 0.158690 11.00000 -1.20000 AFIX 0 C52 1 0.404013 0.570721 0.234032 11.00000 0.05273 0.05900 = 0.03468 0.01756 0.03271 0.02407 AFIX 43 H52 2 0.430681 0.552616 0.280935 11.00000 -1.20000 AFIX 0 C53 1 0.460692 0.615483 0.238346 11.00000 0.04796 0.06640 = 0.02578 -0.00297 0.01733 0.00005 AFIX 43 H53 2 0.526795 0.627975 0.288395 11.00000 -1.20000 AFIX 0 C54 1 0.423301 0.642631 0.171255 11.00000 0.03136 0.04847 = 0.02897 -0.00430 0.01594 -0.00445 AFIX 43 H54 2 0.462947 0.673817 0.174934 11.00000 -1.20000 AFIX 0 C55 1 0.256553 0.882918 -0.106250 11.00000 0.02780 0.01632 = 0.02667 0.00210 0.01839 -0.00069 C56 1 0.259206 0.901018 -0.047576 11.00000 0.02948 0.03010 = 0.02650 0.00074 0.01789 -0.00106 AFIX 43 H56 2 0.319786 0.891112 0.005832 11.00000 -1.20000 AFIX 0 C57 1 0.173752 0.933456 -0.066785 11.00000 0.03950 0.03266 = 0.04215 -0.00419 0.03081 0.00065 AFIX 43 H57 2 0.176241 0.945898 -0.026460 11.00000 -1.20000 AFIX 0 C58 1 0.085071 0.947722 -0.144343 11.00000 0.02972 0.03085 = 0.04665 0.00172 0.02523 0.00245 AFIX 43 H58 2 0.026691 0.969943 -0.157281 11.00000 -1.20000 AFIX 0 C59 1 0.081199 0.929753 -0.202967 11.00000 0.02986 0.02836 = 0.03201 0.00316 0.01526 0.00089 AFIX 43 H59 2 0.020118 0.939706 -0.256245 11.00000 -1.20000 AFIX 0 C60 1 0.165784 0.897281 -0.184697 11.00000 0.03603 0.02393 = 0.02725 0.00198 0.01949 0.00169 AFIX 43 H60 2 0.162224 0.884718 -0.225479 11.00000 -1.20000 AFIX 0 C61 1 0.465812 0.884978 -0.067773 11.00000 0.02813 0.02543 = 0.02499 -0.00259 0.01744 -0.00131 C62 1 0.454760 0.942976 -0.077747 11.00000 0.03156 0.02385 = 0.03041 0.00102 0.02135 0.00018 AFIX 43 H62 2 0.391160 0.961073 -0.093266 11.00000 -1.20000 AFIX 0 C63 1 0.535892 0.974987 -0.065259 11.00000 0.04253 0.02748 = 0.03309 -0.00203 0.02556 -0.00748 AFIX 43 H63 2 0.527355 1.014841 -0.072581 11.00000 -1.20000 AFIX 0 C64 1 0.628386 0.949383 -0.042389 11.00000 0.04080 0.04510 = 0.03816 -0.01216 0.03087 -0.01428 AFIX 43 H64 2 0.683516 0.971514 -0.034161 11.00000 -1.20000 AFIX 0 C65 1 0.641514 0.891663 -0.031329 11.00000 0.03486 0.05004 = 0.05059 -0.01359 0.03126 -0.00218 AFIX 43 H65 2 0.706167 0.874154 -0.014790 11.00000 -1.20000 AFIX 0 C66 1 0.560739 0.859024 -0.044240 11.00000 0.03425 0.02982 = 0.04488 -0.00899 0.02502 0.00176 AFIX 43 H66 2 0.569601 0.819160 -0.037177 11.00000 -1.20000 AFIX 0 C67 1 0.315400 0.792467 -0.156803 11.00000 0.02835 0.02258 = 0.02793 -0.00164 0.01881 0.00014 C68 1 0.288686 0.810488 -0.225513 11.00000 0.04615 0.03185 = 0.03366 -0.00342 0.02790 -0.00471 AFIX 43 H68 2 0.303339 0.848416 -0.229720 11.00000 -1.20000 AFIX 0 C69 1 0.241065 0.773455 -0.287399 11.00000 0.05958 0.04987 = 0.03673 -0.00893 0.03760 -0.00584 AFIX 43 H69 2 0.222187 0.785960 -0.334391 11.00000 -1.20000 AFIX 0 C70 1 0.220751 0.717876 -0.280929 11.00000 0.04923 0.04119 = 0.04479 -0.01718 0.03439 -0.00962 AFIX 43 H70 2 0.187396 0.692504 -0.323792 11.00000 -1.20000 AFIX 0 C71 1 0.248653 0.699219 -0.212700 11.00000 0.03956 0.02560 = 0.04486 -0.00768 0.02859 -0.00683 AFIX 43 H71 2 0.235583 0.660967 -0.208352 11.00000 -1.20000 AFIX 0 C72 1 0.295596 0.736200 -0.150737 11.00000 0.02847 0.02452 = 0.02879 -0.00308 0.01794 -0.00280 AFIX 43 H72 2 0.314494 0.723381 -0.103848 11.00000 -1.20000 AFIX 0 LI1 3 0.483224 0.745289 0.063520 11.00000 0.01781 0.01974 = 0.01869 0.00002 0.01046 -0.00066 O1 4 0.571972 0.705799 0.054136 11.00000 0.02785 0.06212 = 0.02834 0.00522 0.01875 0.01838 O2 4 0.571201 0.764914 0.170672 11.00000 0.03708 0.02423 = 0.02215 -0.00435 0.01584 -0.00227 O3 4 0.368810 0.698855 0.032160 11.00000 0.02501 0.04179 = 0.03596 -0.00312 0.01787 -0.01317 O4 4 0.422562 0.810521 -0.001615 11.00000 0.03872 0.02371 = 0.02387 0.00295 0.01705 0.00213 P1 5 0.672202 0.670735 0.093952 11.00000 0.02180 0.03898 = 0.02269 0.00352 0.01493 0.00861 P2 5 0.603219 0.812446 0.225144 11.00000 0.02390 0.02239 = 0.01861 -0.00143 0.01206 -0.00011 P3 5 0.279090 0.662807 0.012469 11.00000 0.01808 0.02596 = 0.02495 -0.00066 0.01259 -0.00531 P4 5 0.369303 0.839922 -0.077059 11.00000 0.02819 0.01656 = 0.02284 0.00118 0.01558 0.00125 I1 6 0.983309 0.589363 0.578968 11.00000 0.04855 0.05386 = 0.05983 0.01140 0.02932 -0.00026 I2 6 1.000000 0.500000 0.500000 10.50000 0.02208 0.04904 = 0.03322 0.01896 0.00665 -0.00717 I3 6 0.008032 0.909614 0.589480 11.00000 0.04414 0.04826 = 0.04126 0.00750 0.03043 0.00078 I4 6 0.000000 1.000000 0.500000 10.50000 0.02773 0.03800 = 0.02211 -0.00099 0.01557 0.00552 HKLF 4 REM mo_eha110713_0m REM R1 = 0.0422 for 11085 Fo > 4sig(Fo) and 0.0765 for all 15824 data REM 767 parameters refined using 0 restraints END WGHT 0.0309 12.2475 REM Highest difference peak 1.673, deepest hole -1.015, 1-sigma level 0.090 Q1 1 0.9516 0.5961 0.5906 11.00000 0.05 1.67 Q2 1 0.9465 0.5743 0.5417 11.00000 0.05 1.45 Q3 1 -0.0438 0.9146 0.5397 11.00000 0.05 1.41 Q4 1 -0.0301 0.9338 0.5885 11.00000 0.05 1.12 Q5 1 -0.0410 0.8833 0.5589 11.00000 0.05 0.70 ; _database_code_depnum_ccdc_archive 'CCDC 959955'