#------------------------------------------------------------------------------ #$Date: 2021-08-05 04:20:23 +0300 (Thu, 05 Aug 2021) $ #$Revision: 267955 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/79/7707956.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_7707956 loop_ _publ_author_name 'Fetrow, Taylor V.' 'Daly, Scott R.' _publ_section_title ; Mechanochemical synthesis and structural analysis of trivalent lanthanide and uranium diphenylphosphinodiboranates ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT01932E _journal_year 2021 _chemical_formula_moiety 'C12 H24 B2 I2 O3 P U' _chemical_formula_sum 'C12 H24 B2 I2 O3 P U' _chemical_formula_weight 760.73 _chemical_name_common U(H-PDB) _chemical_name_systematic U(BH3Ph2BH3)I2(THF)3 _chemical_properties_physical Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive _space_group_crystal_system orthorhombic _space_group_IT_number 60 _space_group_name_Hall '-P 2n 2ab' _space_group_name_H-M_alt 'P b c n' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2020-03-06 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-06-09 deposited with the CCDC. 2021-07-16 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.5213(11) _cell_length_b 15.3494(17) _cell_length_c 15.8099(18) _cell_measurement_reflns_used 7113 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 28.14 _cell_measurement_theta_min 2.517 _cell_volume 2310.6(5) _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 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 150.15 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.966 _diffrn_measurement_device_type 'D8 Ventere Duo' _diffrn_measurement_method 'Photon 3 Phi and Omega Scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_unetI/netI 0.0276 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.966 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 24979 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.966 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.278 _diffrn_reflns_theta_min 2.517 _exptl_absorpt_coefficient_mu 9.770 _exptl_absorpt_correction_T_max 0.4920 _exptl_absorpt_correction_T_min 0.3139 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0940 before and 0.0438 after correction. The Ratio of minimum to maximum transmission is 0.6380. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'dark purple' _exptl_crystal_density_diffrn 2.187 _exptl_crystal_description 'rod like' _exptl_crystal_F_000 1372 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.085 _refine_diff_density_max 4.078 _refine_diff_density_min -3.495 _refine_diff_density_rms 0.316 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 88 _refine_ls_number_reflns 2777 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.084 _refine_ls_R_factor_all 0.0771 _refine_ls_R_factor_gt 0.0548 _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^)+(0.0882P)^2^+44.3811P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1563 _refine_ls_wR_factor_ref 0.1727 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2079 _reflns_number_total 2777 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt01932e2.cif _cod_data_source_block dal201 _cod_database_code 7707956 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.491 _shelx_estimated_absorpt_t_min 0.127 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All B(H,H,H) groups 2. Restrained distances P1-H1 1.3 with sigma of 0.02 H1-H1_$1 2.1 with sigma of 0.04 3. Uiso/Uaniso restraints and constraints Uanis(U1) = Uanis(O1) = Uanis(C11) = Uanis(C12) = Uanis(C13) = Uanis(C14) = Uanis(O1A) = Uanis(C11A) = Uanis(C12A) = Uanis(C13A) = Uanis(C14A) 4. Others Sof(C11)=Sof(C14)=Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C13A)=Sof(H13C)=Sof(H13D)= Sof(O1A)=1-FVAR(1) Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(O1)=Sof(C11A)= Sof(C14A)=FVAR(1) 5.a Secondary CH2 refined with riding coordinates: C21(H21A,H21B), C22(H22A,H22B), C12(H12A,H12B), C13(H13A,H13B), C12A(H12C, H12D), C13A(H13C,H13D) 5.b Idealised Me refined as rotating group: B1(H1A,H1B,H1C) ; _shelx_res_file ; TITL dal201_a.res in Pbcn dal201.res created by SHELXL-2018/3 at 13:17:01 on 06-Mar-2020 REM Old TITL Dal20_1 in Pbcn sample #20001 TVF_U(HPDB) REM SHELXT solution in Pbcn REM R1 0.128, Rweak 0.002, Alpha 0.025, Orientation as input REM Formula found by SHELXT: C12 O3 P I2 U CELL 0.71073 9.5213 15.3494 15.8099 90 90 90 ZERR 4 0.0011 0.0017 0.0018 0 0 0 LATT 1 SYMM 0.5-X,0.5-Y,0.5+Z SYMM -X,+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H B I O P U UNIT 48 96 8 8 12 4 4 EQIV $1 1-X,+Y,1.5-Z DFIX 1.3 P1 H1 DANG 2.1 H1 H1_$1 EADP U1 O1 C11 C12 C13 C14 O1A C11A C12A C13A C14A L.S. 10 0 0 PLAN 99 SIZE 0.085 0.1 0.36 TEMP -123 FREE U1 B1 FREE U1 B1_$1 list 4 fmap 2 53 acta OMIT 0 0 4 OMIT 2 0 0 REM REM REM WGHT 0.088200 44.381100 FVAR 0.15417 0.48466 C21 1 0.497098 0.791589 0.826120 11.00000 0.14611 0.03685 = 0.04594 -0.01732 -0.01500 -0.00454 AFIX 23 H21A 2 0.405152 0.787359 0.855070 11.00000 -1.20000 H21B 2 0.571922 0.774553 0.866332 11.00000 -1.20000 AFIX 0 C22 1 0.520649 0.880205 0.794616 11.00000 0.04924 0.04174 = 0.09055 -0.00466 -0.01290 -0.00413 AFIX 23 H22A 2 0.463270 0.922477 0.826907 11.00000 -1.20000 H22B 2 0.620831 0.896389 0.800456 11.00000 -1.20000 AFIX 0 I2 4 0.765002 0.600120 0.864864 11.00000 0.04674 0.04193 = 0.04815 -0.00297 -0.01166 0.00081 O2 5 0.500000 0.735118 0.750000 10.50000 0.04686 0.02528 = 0.03251 0.00000 -0.00914 0.00000 P1 6 0.500000 0.332313 0.750000 10.50000 0.07432 0.02069 = 0.04489 0.00000 -0.00368 0.00000 U1 7 0.500000 0.572176 0.750000 10.50000 0.03493 0.02063 = 0.02153 0.00000 -0.00283 0.00000 PART 1 C11 1 0.599538 0.612219 0.537535 -21.00000 0.03493 0.02063 = 0.02153 0.00000 -0.00283 0.00000 C12 1 0.707211 0.665789 0.492194 21.00000 0.03493 0.02063 = 0.02153 0.00000 -0.00283 0.00000 AFIX 23 H12A 2 0.697955 0.728613 0.505224 21.00000 -1.20000 H12B 2 0.703530 0.656939 0.430206 21.00000 -1.20000 AFIX 0 C13 1 0.852517 0.622628 0.534980 21.00000 0.03493 0.02063 = 0.02153 0.00000 -0.00283 0.00000 AFIX 23 H13A 2 0.940220 0.650840 0.515455 21.00000 -1.20000 H13B 2 0.858439 0.558585 0.528467 21.00000 -1.20000 AFIX 0 C14 1 0.802531 0.654277 0.632542 -21.00000 0.03493 0.02063 = 0.02153 0.00000 -0.00283 0.00000 O1 5 0.654132 0.605233 0.624939 21.00000 0.03493 0.02063 = 0.02153 0.00000 -0.00283 0.00000 PART 0 PART 2 C11A 1 0.628405 0.586291 0.539425 21.00000 0.03493 0.02063 = 0.02153 0.00000 -0.00283 0.00000 C12A 1 0.727049 0.637924 0.482541 -21.00000 0.03493 0.02063 = 0.02153 0.00000 -0.00283 0.00000 AFIX 23 H12C 2 0.766188 0.600727 0.437139 -21.00000 -1.20000 H12D 2 0.678178 0.688215 0.456640 -21.00000 -1.20000 AFIX 0 C13A 1 0.839343 0.667386 0.541763 -21.00000 0.03493 0.02063 = 0.02153 0.00000 -0.00283 0.00000 AFIX 23 H13C 2 0.834269 0.730992 0.551676 -21.00000 -1.20000 H13D 2 0.933831 0.652364 0.520076 -21.00000 -1.20000 AFIX 0 C14A 1 0.804407 0.615580 0.623346 21.00000 0.03493 0.02063 = 0.02153 0.00000 -0.00283 0.00000 O1A 5 0.645051 0.622697 0.625911 -21.00000 0.03493 0.02063 = 0.02153 0.00000 -0.00283 0.00000 PART 0 B1 3 0.593988 0.407583 0.669794 11.00000 0.05980 0.02352 = 0.04310 -0.00843 -0.00144 0.00248 AFIX 137 1.2000 H1A 2 0.508209 0.448922 0.631299 11.00000 -1.50000 H1B 2 0.661255 0.364174 0.621379 11.00000 -1.50000 H1C 2 0.670794 0.456337 0.706959 11.00000 -1.50000 AFIX 0 H1 2 0.585497 0.283147 0.792688 11.00000 0.08878 HKLF 4 REM dal201_a.res in Pbcn REM wR2 = 0.1727, GooF = S = 1.084, Restrained GooF = 1.084 for all data REM R1 = 0.0548 for 2079 Fo > 4sig(Fo) and 0.0771 for all 2777 data REM 88 parameters refined using 2 restraints END WGHT 0.0902 47.6924 REM Highest difference peak 4.078, deepest hole -3.495, 1-sigma level 0.316 Q1 1 0.5188 0.5912 0.7525 11.00000 0.05 3.66 Q2 1 0.7704 0.6024 0.6389 11.00000 0.05 1.53 Q3 1 0.8830 0.6145 0.8813 11.00000 0.05 1.34 Q4 1 0.8802 0.5872 0.8919 11.00000 0.05 1.24 Q5 1 0.7664 0.5330 0.8645 11.00000 0.05 1.22 Q6 1 0.6598 0.5822 0.6429 11.00000 0.05 1.15 Q7 1 0.7030 0.6596 0.8717 11.00000 0.05 0.95 Q8 1 0.5000 0.3110 0.7500 10.50000 0.05 0.93 Q9 1 0.7010 0.6988 0.6150 11.00000 0.05 0.90 Q10 1 0.7851 0.7155 0.6354 11.00000 0.05 0.89 Q11 1 0.6782 0.5581 0.9038 11.00000 0.05 0.88 Q12 1 0.6679 0.5998 0.6058 11.00000 0.05 0.77 Q13 1 0.5066 0.6370 0.5225 11.00000 0.05 0.75 Q14 1 0.8519 0.5758 0.6586 11.00000 0.05 0.74 Q15 1 0.8274 0.5825 0.5821 11.00000 0.05 0.72 Q16 1 0.6517 0.5951 0.9076 11.00000 0.05 0.71 Q17 1 0.6678 0.5637 0.8482 11.00000 0.05 0.71 Q18 1 0.7848 0.5271 0.3618 11.00000 0.05 0.66 Q19 1 0.6335 0.6635 0.4798 11.00000 0.05 0.66 Q20 1 0.8046 0.3766 0.6181 11.00000 0.05 0.65 Q21 1 0.7591 0.5798 0.7980 11.00000 0.05 0.65 Q22 1 0.7002 0.5606 0.8190 11.00000 0.05 0.65 Q23 1 0.5833 0.6412 0.6197 11.00000 0.05 0.64 Q24 1 0.6405 0.5918 0.8658 11.00000 0.05 0.64 Q25 1 0.7690 0.6028 0.4043 11.00000 0.05 0.63 Q26 1 0.8637 0.6160 0.6552 11.00000 0.05 0.63 Q27 1 0.5873 0.6604 0.5408 11.00000 0.05 0.63 Q28 1 0.7417 0.7278 0.8664 11.00000 0.05 0.63 Q29 1 0.5890 0.8030 0.7910 11.00000 0.05 0.62 Q30 1 0.6860 0.5410 0.3782 11.00000 0.05 0.61 Q31 1 0.4257 0.7616 0.7592 11.00000 0.05 0.60 Q32 1 0.7380 0.6210 0.7983 11.00000 0.05 0.60 Q33 1 0.7356 0.7554 0.8772 11.00000 0.05 0.59 Q34 1 0.7713 0.5980 0.4815 11.00000 0.05 0.59 Q35 1 0.6061 0.5348 0.5235 11.00000 0.05 0.59 Q36 1 0.3974 0.5654 0.6958 11.00000 0.05 0.58 Q37 1 0.7697 0.6392 0.5222 11.00000 0.05 0.58 Q38 1 0.6987 0.6376 0.8170 11.00000 0.05 0.57 Q39 1 0.7616 0.5969 0.9430 11.00000 0.05 0.57 Q40 1 0.4536 0.8757 0.7994 11.00000 0.05 0.55 Q41 1 0.6754 0.7644 0.3991 11.00000 0.05 0.52 Q42 1 0.5446 0.5897 0.6188 11.00000 0.05 0.52 Q43 1 0.6959 0.5596 0.5474 11.00000 0.05 0.52 Q44 1 0.7775 0.5187 0.4867 11.00000 0.05 0.52 Q45 1 0.5994 0.6597 0.4184 11.00000 0.05 0.51 Q46 1 0.7299 0.4382 0.6104 11.00000 0.05 0.50 Q47 1 0.7061 0.7438 0.5485 11.00000 0.05 0.50 Q48 1 0.8253 0.6375 0.5869 11.00000 0.05 0.50 Q49 1 1.0524 0.6783 0.5222 11.00000 0.05 0.49 Q50 1 0.6008 0.5975 0.5762 11.00000 0.05 0.49 Q51 1 0.8234 0.5968 0.9808 11.00000 0.05 0.49 Q52 1 0.7030 0.7046 0.5246 11.00000 0.05 0.48 Q53 1 0.5879 0.5940 0.6821 11.00000 0.05 0.48 Q54 1 0.5000 0.6756 0.7500 10.50000 0.05 0.48 Q55 1 0.7130 0.4006 0.5808 11.00000 0.05 0.48 Q56 1 0.8573 0.5225 0.6623 11.00000 0.05 0.47 Q57 1 0.5533 0.5828 0.5228 11.00000 0.05 0.47 Q58 1 0.7920 0.7061 0.5526 11.00000 0.05 0.47 Q59 1 0.3935 0.5505 0.8059 11.00000 0.05 0.46 Q60 1 0.6787 0.7956 0.7664 11.00000 0.05 0.45 Q61 1 0.7771 0.5414 0.8236 11.00000 0.05 0.45 Q62 1 0.7308 0.6791 0.7199 11.00000 0.05 0.44 Q63 1 0.5074 0.6720 0.5422 11.00000 0.05 0.43 Q64 1 0.5908 0.6166 0.8794 11.00000 0.05 0.43 Q65 1 0.5451 0.4506 0.6730 11.00000 0.05 0.43 Q66 1 0.5838 0.3539 0.7026 11.00000 0.05 0.43 Q67 1 0.5020 0.7657 0.8102 11.00000 0.05 0.42 Q68 1 0.6963 0.4013 0.6133 11.00000 0.05 0.42 Q69 1 0.6399 0.3851 0.6218 11.00000 0.05 0.42 Q70 1 0.7589 0.5125 0.7598 11.00000 0.05 0.41 Q71 1 0.9570 0.5718 0.5050 11.00000 0.05 0.41 Q72 1 0.7012 0.7191 0.8997 11.00000 0.05 0.41 Q73 1 0.3240 0.9271 0.8997 11.00000 0.05 0.40 Q74 1 0.5731 0.5897 0.8720 11.00000 0.05 0.40 Q75 1 0.6837 0.4560 0.6371 11.00000 0.05 0.40 Q76 1 0.5987 0.8339 0.8285 11.00000 0.05 0.40 Q77 1 0.5373 0.6416 0.6986 11.00000 0.05 0.40 Q78 1 0.2737 0.7861 0.8853 11.00000 0.05 0.40 Q79 1 0.6772 0.4376 0.6762 11.00000 0.05 0.40 Q80 1 0.7050 0.6231 0.5137 11.00000 0.05 0.40 Q81 1 0.6448 0.5098 0.5982 11.00000 0.05 0.39 Q82 1 0.7565 0.4595 0.6532 11.00000 0.05 0.39 Q83 1 0.8847 0.6431 0.5660 11.00000 0.05 0.39 Q84 1 0.4800 0.7871 0.7880 11.00000 0.05 0.39 Q85 1 0.6678 0.4199 0.7360 11.00000 0.05 0.39 Q86 1 0.9134 0.7199 0.5598 11.00000 0.05 0.38 Q87 1 0.6099 0.6784 0.8752 11.00000 0.05 0.38 Q88 1 0.5416 0.7509 0.8885 11.00000 0.05 0.38 Q89 1 0.7570 0.6553 0.8243 11.00000 0.05 0.38 Q90 1 0.7560 0.6191 0.7451 11.00000 0.05 0.38 Q91 1 0.5144 0.4187 0.6588 11.00000 0.05 0.38 Q92 1 1.0862 0.6738 0.5963 11.00000 0.05 0.37 Q93 1 0.7123 0.3213 0.7574 11.00000 0.05 0.37 Q94 1 0.8568 0.5961 0.4986 11.00000 0.05 0.37 Q95 1 0.8620 0.5607 0.4768 11.00000 0.05 0.37 Q96 1 0.7066 0.6198 0.3520 11.00000 0.05 0.37 Q97 1 0.8212 0.6567 0.6869 11.00000 0.05 0.36 Q98 1 0.6862 0.4838 0.8474 11.00000 0.05 0.36 Q99 1 0.7308 0.5620 0.7547 11.00000 0.05 0.36 ; _shelx_res_checksum 15235 _shelx_hkl_file ; 1 0 0 0.50 0.50 -1 0 0 0.40 0.50 -1 0 0 -0.60 0.60 -2 0 0 153.58 5.30 -2 0 0 151.58 5.70 2 0 0 151.88 5.40 -3 0 0 3.70 2.00 -3 0 0 6.90 2.70 3 0 0 3.90 1.90 -4 0 0 5894.11 145.89 4 0 0 5726.33 145.99 -4 0 0 5911.21 146.59 -5 0 0 0.00 3.00 5 0 0 4.00 3.50 -5 0 0 1.80 3.50 6 0 0 172.28 9.70 -6 0 0 192.78 9.80 -6 0 0 178.38 11.20 -7 0 0 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20.20 14.60 11 -3 4 6.60 14.00 11 3 4 26.40 13.70 -11 -3 4 14.10 16.10 11 -3 -4 -4.30 12.70 -11 3 -4 9.20 12.80 -12 3 4 23.50 16.10 12 3 4 -10.10 21.60 -12 3 -4 17.30 21.40 0 -4 -4 709.83 18.90 0 -4 -4 756.12 19.40 0 4 -4 764.92 19.60 0 -4 4 740.33 19.90 0 -4 -4 717.63 19.30 0 4 -4 721.33 19.90 0 -4 4 716.23 19.90 0 4 4 711.53 19.70 0 4 4 723.43 19.00 0 4 4 680.83 18.80 1 4 -4 98.29 3.90 -1 -4 -4 96.59 4.30 1 -4 4 88.09 4.40 -1 4 4 94.89 4.40 -1 4 4 96.69 3.60 1 4 -4 91.79 4.70 -1 -4 -4 97.59 4.70 1 -4 4 95.79 4.80 -1 4 4 100.59 4.30 1 4 4 94.19 4.10 -1 -4 4 97.19 4.70 1 -4 -4 100.49 4.00 -1 4 -4 93.69 3.50 -1 -4 4 108.89 4.80 -1 4 -4 83.49 4.40 1 4 4 92.19 4.80 1 4 4 91.59 3.10 2 -4 4 2055.19 51.89 2 4 -4 2021.60 50.59 2 4 -4 2018.30 51.89 -2 4 4 1947.61 51.09 2 -4 4 2090.89 52.09 -2 4 4 1999.20 51.89 -2 -4 -4 2025.40 52.29 -2 4 4 2044.30 50.79 2 -4 4 2008.20 50.79 -2 -4 4 2059.19 51.99 2 -4 -4 2001.00 49.80 -2 -4 4 2034.70 52.29 2 -4 -4 1955.80 49.80 -2 4 -4 1949.90 51.79 2 4 4 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37.70 8.30 -5 6 -14 56.69 10.30 6 -6 14 242.18 16.70 -6 -6 -14 220.38 18.20 6 -6 -14 230.68 16.30 6 6 14 250.27 18.30 -6 6 -14 255.57 18.30 -6 -6 14 238.68 18.70 7 6 -14 11.00 12.20 -7 -6 -14 33.40 13.80 7 -6 14 20.10 11.80 -7 6 -14 32.30 12.20 7 -6 -14 33.00 11.20 -7 -6 14 12.40 12.10 7 6 14 0.30 10.70 8 -6 14 21.20 15.50 8 6 14 31.30 17.80 -8 6 -14 35.50 14.30 0 7 -14 3.70 6.60 0 7 -14 -7.80 4.60 0 -7 -14 -0.30 6.10 0 -7 14 -0.30 6.20 1 -7 14 346.27 16.90 1 7 -14 353.56 14.70 1 7 -14 336.67 16.30 -1 -7 -14 339.77 14.40 -1 -7 -14 328.67 15.70 -1 7 -14 329.57 13.80 -1 7 -14 350.96 16.50 -1 -7 14 326.47 16.70 1 -7 -14 349.07 15.90 2 7 -14 5.30 6.20 -2 -7 -14 -6.60 5.70 2 7 -14 -3.40 4.90 2 -7 14 1.70 6.00 2 7 14 7.80 6.00 -2 7 -14 7.70 6.20 -2 7 -14 -2.90 5.20 -2 -7 14 1.40 6.10 2 -7 -14 -8.60 5.50 3 7 -14 239.28 13.00 3 7 -14 215.88 14.10 3 -7 14 200.28 14.60 -3 -7 -14 226.48 14.30 3 -7 14 218.88 14.30 -3 7 -14 196.38 13.20 3 -7 -14 207.48 13.40 3 7 14 214.58 13.80 -3 -7 14 205.78 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11.60 0 2 -18 99.39 10.60 0 2 18 140.69 13.10 1 2 -18 -4.60 6.50 1 -2 18 -5.60 8.30 1 2 -18 5.60 8.20 -1 -2 -18 -5.50 7.00 -1 2 18 7.40 7.80 -1 -2 -18 -14.50 7.90 -1 2 -18 -3.30 7.80 -1 -2 18 1.20 8.40 -1 2 -18 10.90 7.80 1 -2 -18 0.40 6.40 1 2 18 -1.20 7.50 1 -2 -18 -1.20 8.20 2 2 -18 26.70 8.00 -2 -2 -18 18.70 8.30 -2 2 18 32.80 8.90 2 -2 18 32.90 9.20 -2 -2 -18 39.00 9.60 2 2 -18 23.40 9.00 2 -2 -18 28.70 9.60 2 -2 -18 32.40 7.50 -2 2 -18 12.50 8.50 -2 2 -18 31.30 9.00 -2 -2 18 36.10 9.80 2 2 18 37.90 9.20 3 2 -18 1.40 9.10 3 -2 18 -0.70 9.30 -3 2 18 -2.20 7.80 3 2 -18 -3.10 7.10 -3 -2 -18 -3.30 8.50 -3 -2 18 16.50 9.40 -3 2 -18 -0.30 8.60 3 -2 -18 1.40 9.40 4 2 -18 88.29 12.30 -4 -2 -18 77.09 12.70 -4 2 18 62.99 11.10 4 2 -18 85.69 10.40 -4 2 -18 91.09 12.90 -4 -2 18 82.59 12.70 4 -2 -18 103.19 13.00 -5 -2 -18 1.20 11.60 5 2 -18 5.30 10.70 -5 2 18 -18.20 9.00 5 2 -18 -2.30 8.40 -5 -2 18 -12.90 9.80 -5 2 -18 -4.00 12.00 5 -2 -18 13.50 11.30 6 2 -18 -2.20 10.70 -6 2 18 23.30 17.90 0 3 -18 17.70 7.80 0 -3 -18 2.30 6.80 0 3 18 13.20 7.60 0 -3 18 15.90 8.80 0 3 -18 9.00 8.10 0 -3 -18 8.30 8.40 1 3 -18 -3.50 7.20 1 3 -18 11.90 8.50 -1 -3 -18 13.00 7.50 -1 -3 -18 7.60 8.90 -1 3 18 3.40 7.40 1 -3 18 -0.70 8.30 1 -3 -18 -1.30 8.90 -1 -3 18 7.40 8.30 1 3 18 9.60 8.00 -1 3 -18 3.10 8.00 -1 3 -18 -13.10 7.40 1 -3 -18 11.00 6.60 2 -3 18 -6.20 7.40 -2 -3 -18 6.90 8.90 -2 -3 -18 -9.20 7.70 2 3 -18 -7.80 6.90 -2 3 18 0.50 7.60 2 3 -18 4.50 8.30 2 3 18 -1.70 8.00 2 -3 -18 -5.00 8.30 -2 3 -18 7.40 8.20 -2 3 -18 -5.80 7.90 -2 -3 18 -6.30 7.60 3 3 -18 -7.00 7.20 3 -3 18 -4.50 9.50 -3 -3 -18 -10.10 8.80 -3 3 18 5.70 7.80 3 3 -18 -2.90 7.70 3 -3 -18 7.10 9.70 -3 -3 18 -1.40 8.40 -3 3 -18 8.10 9.10 4 3 -18 -3.60 8.10 4 3 -18 2.40 9.10 -4 -3 -18 -8.30 9.70 -4 3 18 -10.40 12.20 4 -3 -18 -2.60 9.80 -4 3 -18 -7.90 9.20 -4 -3 18 -6.10 8.20 -5 -3 -18 15.10 12.00 5 3 -18 -3.00 9.00 5 3 -18 2.40 10.90 -5 -3 18 0.40 10.80 5 -3 -18 7.70 13.00 0 4 -18 153.58 12.70 0 -4 -18 153.48 13.50 0 4 -18 143.59 12.40 0 -4 18 124.79 13.50 0 4 18 115.99 11.70 0 -4 -18 121.29 10.40 1 4 -18 -10.40 7.40 1 -4 18 14.70 9.50 1 4 -18 33.50 8.80 -1 -4 -18 7.60 9.40 -1 4 18 2.80 7.60 -1 -4 -18 12.40 7.70 -1 4 -18 3.00 8.00 -1 -4 18 12.30 8.90 1 -4 -18 24.00 9.50 1 4 18 15.10 8.30 -1 4 -18 3.50 8.30 2 4 -18 8.40 8.00 -2 -4 -18 4.30 9.10 -2 -4 -18 2.40 8.10 2 4 -18 14.70 8.60 2 -4 18 12.20 9.20 -2 -4 18 3.50 8.80 -2 4 -18 3.70 8.30 -2 4 -18 13.10 9.10 2 -4 -18 -7.50 7.50 3 4 -18 6.50 9.00 3 -4 18 7.60 9.70 3 4 -18 10.60 8.20 -3 -4 -18 12.40 9.60 3 -4 -18 10.10 9.50 -3 -4 18 3.50 9.30 -3 4 -18 8.20 9.00 -4 -4 -18 88.39 12.90 4 4 -18 68.99 11.20 4 4 -18 54.49 11.40 -4 4 -18 63.59 11.20 4 -4 -18 66.39 11.00 -4 -4 18 80.69 13.10 5 4 -18 -12.10 10.10 5 4 -18 12.90 10.10 -5 -4 -18 9.50 15.70 0 5 -18 6.40 8.10 0 -5 18 -8.10 8.10 0 5 -18 -1.00 7.90 0 -5 -18 6.10 9.30 -1 -5 -18 43.00 8.80 1 5 -18 64.89 10.50 1 5 -18 57.09 10.30 -1 -5 -18 54.59 10.80 1 -5 18 48.60 10.80 1 5 18 56.99 13.60 1 -5 -18 38.10 9.90 -1 5 -18 37.50 9.60 -1 5 -18 55.69 9.50 -1 -5 18 39.80 9.20 2 5 -18 -6.30 8.00 -2 -5 -18 -1.50 8.10 -2 -5 -18 -7.70 8.70 2 5 -18 0.30 8.20 2 -5 18 -3.00 8.30 -2 5 -18 5.80 8.50 -2 -5 18 9.80 9.50 2 -5 -18 -2.50 8.70 -2 5 -18 -7.50 8.20 -3 -5 -18 79.59 11.90 3 5 -18 99.99 12.30 3 5 -18 111.19 12.10 3 -5 18 101.39 14.20 -3 5 -18 106.69 12.90 3 -5 -18 83.19 12.10 -3 -5 18 101.59 13.00 4 5 -18 14.50 9.80 4 5 -18 9.30 9.80 -4 -5 -18 9.40 10.90 -4 -5 18 -9.80 10.00 -4 5 -18 8.60 10.10 4 -5 -18 -2.00 10.10 5 5 -18 10.80 10.80 0 -6 -18 315.37 17.10 0 6 -18 301.47 17.80 0 6 -18 294.17 16.50 0 -6 18 292.87 19.00 1 -6 18 4.90 9.70 -1 -6 -18 1.70 8.20 1 6 -18 8.80 8.60 1 6 -18 12.60 8.50 1 -6 -18 8.30 9.60 -1 6 -18 7.50 9.20 -1 -6 18 -0.30 8.40 -1 6 -18 19.10 9.40 -2 -6 -18 31.60 10.20 2 -6 18 21.70 10.70 2 6 -18 24.60 9.70 -2 -6 -18 38.10 9.90 2 6 -18 29.60 9.70 -2 -6 18 20.00 10.10 2 -6 -18 24.70 9.30 -2 6 -18 7.30 8.70 -3 -6 -18 14.30 10.10 3 6 -18 8.50 8.90 3 6 -18 2.50 9.30 3 -6 18 4.80 9.10 3 -6 -18 17.90 10.20 -3 6 -18 13.10 9.60 -3 -6 18 13.70 9.80 4 6 -18 206.68 15.90 -4 -6 -18 179.58 16.60 4 -6 -18 188.78 15.50 5 6 -18 5.80 13.70 0 7 -18 0.30 8.60 0 -7 18 -23.20 8.70 0 -7 -18 -0.90 9.40 -1 -7 -18 171.48 14.50 1 -7 18 186.38 16.50 1 7 -18 134.99 13.80 -1 7 -18 165.68 14.40 -1 -7 18 163.38 15.10 1 -7 -18 149.69 13.60 2 7 -18 -5.40 8.10 2 7 -18 12.20 9.70 2 -7 18 -4.50 9.80 -2 7 -18 0.80 8.70 -2 -7 18 1.90 9.80 2 -7 -18 -1.50 9.70 -3 -7 -18 161.68 14.80 3 -7 18 169.88 16.70 3 7 -18 154.78 13.50 3 7 -18 154.88 18.30 3 -7 -18 173.08 15.10 -3 -7 18 122.49 20.40 -3 7 -18 135.09 16.90 -4 -7 -18 -1.40 11.90 4 7 -18 -11.60 9.10 0 -8 -18 68.49 11.60 0 -8 18 63.09 12.40 0 8 -18 68.89 12.20 1 -8 18 -3.30 9.90 1 8 -18 -7.00 8.90 -1 -8 -18 -2.70 9.20 1 -8 -18 25.00 10.50 -1 8 -18 15.20 10.60 -1 -8 18 0.60 8.40 2 -8 18 152.28 16.20 -2 8 -18 170.08 20.90 2 -8 -18 165.58 14.80 -2 -8 18 201.98 23.60 3 -8 -18 -5.80 10.20 -4 -8 -18 37.30 13.90 0 -9 18 -1.10 12.50 0 -9 -18 -5.60 8.90 -1 -9 -18 61.99 13.50 1 -9 -18 58.69 12.10 2 -9 -18 12.40 10.70 0 0 -19 14.20 9.40 0 0 -19 0.10 7.60 0 0 19 8.70 8.10 -1 0 -19 -7.00 7.50 1 0 -19 3.20 7.40 1 0 -19 4.30 9.00 1 0 19 3.20 7.80 -1 0 -19 8.70 9.20 -1 0 19 1.90 8.70 2 0 19 4.00 8.40 -2 0 19 -3.50 8.50 2 0 -19 -3.10 8.20 2 0 -19 -2.60 7.20 -2 0 -19 -4.20 9.10 -2 0 -19 -5.50 8.30 -3 0 19 3.10 9.10 3 0 -19 -0.90 7.30 3 0 19 2.70 8.50 3 0 -19 -11.40 9.30 -3 0 -19 -5.60 9.20 4 0 -19 -2.20 7.70 4 0 -19 15.60 13.00 -4 0 19 -13.50 9.20 -5 0 19 -0.90 10.90 0 -1 -19 -8.30 7.80 0 1 19 9.40 9.00 0 -1 -19 0.80 7.60 0 1 -19 4.60 7.50 0 1 -19 3.10 8.70 0 -1 19 4.20 8.50 -1 -1 -19 15.80 8.40 1 -1 19 32.80 10.00 1 1 -19 17.70 9.20 1 1 -19 17.00 8.00 -1 1 19 10.30 9.20 -1 -1 -19 25.00 8.90 1 -1 -19 27.70 9.90 1 1 19 28.40 9.50 -1 1 -19 22.30 8.70 1 -1 -19 34.20 8.60 -1 -1 19 16.00 9.20 -1 1 -19 23.20 9.00 2 1 -19 -10.80 8.80 -2 1 19 0.80 8.60 2 -1 19 0.90 8.60 -2 -1 -19 16.00 9.40 -2 -1 -19 11.10 8.70 2 1 -19 -10.30 7.20 -2 -1 19 -2.60 8.80 2 1 19 -1.50 9.10 2 -1 -19 6.20 7.20 -2 1 -19 -2.60 8.60 -2 1 -19 -9.50 9.00 2 -1 -19 11.20 9.60 -3 1 19 34.30 10.60 3 1 -19 38.60 9.00 3 -1 19 44.30 10.80 3 1 -19 27.70 9.60 -3 -1 -19 34.10 10.90 3 -1 -19 31.10 8.20 -3 1 -19 26.30 10.60 3 -1 -19 38.30 11.20 -3 -1 19 33.40 10.50 4 1 -19 7.00 8.20 -4 1 19 -5.40 9.50 -4 -1 -19 -0.90 14.30 4 1 -19 7.00 12.90 -4 -1 19 9.20 10.80 -5 1 19 9.90 10.80 5 1 -19 -0.70 8.50 0 -2 -19 229.48 16.10 0 -2 -19 189.28 13.80 0 2 19 222.58 16.50 0 2 -19 185.58 14.70 0 -2 19 222.48 15.90 0 2 -19 216.88 15.90 -1 2 19 53.99 10.70 -1 -2 -19 52.69 10.90 1 2 -19 16.70 9.70 1 -2 19 34.60 9.80 -1 -2 -19 30.80 9.20 1 2 -19 42.80 9.00 -1 2 -19 31.80 9.70 1 -2 -19 23.70 9.30 -1 -2 19 30.50 10.20 1 2 19 26.60 9.20 1 -2 -19 48.30 8.70 -1 2 -19 39.10 9.70 2 2 -19 23.50 9.90 -2 2 19 43.70 10.10 -2 -2 -19 57.49 10.70 2 2 -19 38.70 9.10 -2 -2 -19 44.70 10.70 2 -2 19 36.80 10.00 2 -2 -19 47.60 11.10 -2 2 -19 55.29 10.80 -2 -2 19 42.30 10.90 2 2 19 35.90 10.30 -2 2 -19 44.40 10.40 3 -2 19 27.30 10.10 -3 2 19 48.70 10.80 3 2 -19 54.09 11.70 3 2 -19 46.30 9.60 -3 -2 -19 54.39 11.50 3 -2 -19 49.60 11.70 -3 -2 19 33.60 11.20 -3 2 -19 64.89 11.30 -4 2 19 94.79 13.40 -4 -2 -19 103.99 17.50 4 2 -19 80.69 16.70 4 2 -19 80.49 11.00 -4 -2 19 104.89 14.30 -5 2 19 27.60 15.30 0 3 -19 6.50 9.20 0 3 -19 2.10 8.20 0 3 19 13.50 9.00 0 -3 -19 -2.20 9.50 0 -3 -19 -0.70 7.50 0 -3 19 6.80 9.70 1 -3 19 171.98 15.70 1 3 -19 166.28 13.40 1 3 -19 172.78 14.10 -1 -3 -19 178.88 13.70 -1 3 19 185.78 15.30 -1 -3 -19 182.38 15.20 -1 3 -19 163.98 14.00 -1 3 -19 162.18 14.00 -1 -3 19 180.98 16.20 1 3 19 179.38 15.30 1 -3 -19 169.38 14.10 -2 -3 -19 1.40 8.90 2 3 -19 -13.50 7.70 -2 3 19 -8.10 8.00 -2 -3 -19 7.90 9.80 2 3 -19 8.40 9.50 2 -3 19 -0.90 9.40 -2 3 -19 -1.40 8.50 -2 -3 19 -6.50 8.80 -2 3 -19 -7.40 9.00 2 -3 -19 6.70 9.90 2 3 19 19.80 10.20 3 -3 19 194.48 17.50 -3 -3 -19 193.58 15.80 3 3 -19 167.18 14.50 3 3 -19 185.28 14.30 -3 3 19 146.39 22.20 -3 3 -19 184.88 16.10 3 -3 -19 196.08 16.40 -3 -3 19 112.29 13.50 4 3 -19 -25.70 12.30 -4 -3 -19 12.50 15.00 4 3 -19 7.20 9.40 0 -4 -19 253.57 17.40 0 4 -19 228.08 17.20 0 4 19 203.48 15.90 0 -4 19 222.48 17.60 0 4 -19 224.38 16.10 -1 -4 -19 20.50 8.70 1 4 -19 27.20 9.70 1 -4 19 21.60 10.70 1 4 -19 15.80 9.10 -1 -4 -19 35.60 10.60 1 4 19 13.40 9.50 1 -4 -19 18.80 9.20 -1 4 -19 18.40 9.10 -1 4 -19 35.50 9.80 -1 -4 19 17.10 10.20 2 -4 19 162.88 16.20 -2 -4 -19 128.49 13.20 2 4 -19 109.79 12.30 -2 -4 -19 161.98 14.80 2 4 -19 147.09 14.00 -2 -4 19 139.19 15.00 -2 4 -19 136.29 13.30 -2 4 -19 109.09 12.40 2 -4 -19 139.39 14.00 3 4 -19 28.90 10.20 -3 -4 -19 13.60 10.50 3 4 -19 27.70 9.80 -3 -4 19 21.60 11.60 3 -4 -19 4.90 14.70 0 -5 19 8.40 10.50 0 5 -19 7.60 9.20 0 5 -19 -8.90 8.40 0 -5 -19 11.40 10.10 -1 -5 -19 132.69 14.10 1 -5 19 115.99 14.20 1 5 -19 123.99 12.80 1 5 -19 119.39 12.90 -1 -5 19 114.59 14.10 -1 5 -19 127.69 12.50 1 -5 -19 130.99 14.00 -1 5 -19 100.39 12.80 -2 -5 -19 -6.90 12.40 2 5 -19 -3.40 8.90 -2 -5 -19 -9.10 8.90 2 5 -19 -7.50 9.20 2 -5 19 -5.40 9.80 -2 -5 19 1.30 10.60 -2 5 -19 -10.60 9.80 -2 5 -19 4.90 9.20 2 -5 -19 -2.90 9.10 -3 -5 -19 48.40 11.70 3 5 -19 88.09 12.20 0 -6 -19 2.80 10.30 0 6 -19 25.90 11.30 0 6 -19 24.60 10.00 0 -6 19 25.60 13.40 1 -6 19 26.10 13.40 1 6 -19 14.50 9.60 -1 -6 -19 20.40 14.10 1 -6 -19 9.30 11.10 -1 -6 19 10.50 14.80 2 6 -19 47.80 11.00 -3 -6 -19 17.70 11.20 3 6 -19 4.50 9.90 -3 -7 -19 11.70 12.60 3 7 -19 13.90 10.60 0 0 -20 50.89 10.20 0 0 20 75.09 13.20 0 0 -20 75.09 12.50 -1 0 -20 30.50 10.10 1 0 -20 18.20 8.60 1 0 20 26.80 10.70 -1 0 20 19.50 10.20 -1 0 -20 30.50 11.00 1 0 -20 33.60 11.60 -2 0 -20 306.37 24.70 2 0 20 261.67 18.50 -2 0 -20 287.17 21.20 2 0 -20 276.47 16.50 -2 0 20 276.97 19.50 -3 0 20 47.30 12.20 3 0 -20 51.89 9.80 0 1 -20 -16.20 9.20 0 -1 -20 0.80 8.70 0 1 20 -2.70 9.30 0 1 -20 1.90 8.40 0 -1 20 -16.60 9.50 0 -1 -20 -7.90 10.20 1 1 -20 128.29 14.30 -1 -1 -20 106.89 12.60 1 1 -20 116.49 12.10 -1 1 20 101.69 13.50 1 -1 20 110.39 14.10 -1 -1 -20 95.39 15.50 -1 1 -20 109.69 13.40 -1 -1 20 112.79 13.70 1 -1 -20 129.39 18.30 -1 1 -20 125.09 13.10 1 -1 -20 106.39 11.70 1 1 20 125.29 14.10 2 -1 20 -3.50 13.50 2 1 -20 19.70 8.80 -2 -1 -20 1.10 9.80 -2 1 20 3.30 9.80 2 -1 -20 3.00 7.90 -2 -1 20 8.80 10.30 -2 1 -20 18.00 10.80 2 1 20 -8.20 10.20 3 1 -20 111.69 11.90 -3 1 20 101.89 14.10 0 2 -20 34.60 10.40 0 -2 -20 33.20 15.30 0 -2 20 22.60 11.30 0 -2 -20 41.80 10.00 0 2 -20 41.50 10.00 0 2 20 35.80 10.70 1 -2 20 1.80 12.60 -1 -2 -20 6.00 9.10 -1 2 20 1.30 9.80 1 2 -20 1.60 10.10 1 2 -20 14.90 9.00 1 2 20 -3.60 8.40 -1 2 -20 -2.20 9.60 -1 -2 20 8.40 9.60 -1 2 -20 9.20 9.90 1 -2 -20 19.40 8.60 -2 2 20 62.89 12.10 2 2 -20 58.29 10.30 -2 -2 -20 59.09 11.50 2 2 -20 69.69 17.30 -2 -2 20 45.50 16.80 2 2 20 79.39 13.00 -2 2 -20 65.09 12.00 -3 2 20 17.60 10.60 0 3 -20 2.00 12.20 0 3 -20 4.60 9.10 0 3 20 2.10 8.80 0 -3 -20 -1.30 9.60 1 3 -20 0.50 11.30 -1 -3 -20 7.20 9.20 -1 3 20 -10.10 8.90 1 3 -20 -3.90 9.40 -1 3 -20 3.40 9.50 1 3 20 11.10 10.00 2 3 -20 14.90 14.70 -2 -3 -20 2.20 10.00 -2 3 -20 -3.20 9.60 0 4 -20 -3.10 9.40 1 4 -20 18.70 10.00 -1 -4 -20 11.00 11.50 -1 4 -20 9.10 10.20 1 4 20 33.30 12.40 -2 -4 -20 30.70 11.20 2 4 -20 10.20 14.70 -2 4 -20 51.19 11.40 0 5 -20 -2.30 9.60 1 5 -20 47.00 11.30 -1 5 -20 29.70 11.00 -2 -5 -20 17.40 10.90 2 5 -20 0.10 13.90 1 6 -20 14.60 10.80 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 22643 _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+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' 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 C21 C 0.497(2) 0.7916(10) 0.8261(11) 0.076(6) Uani 1 1 d . . . . . H21A H 0.405152 0.787359 0.855070 0.092 Uiso 1 1 calc R . . . . H21B H 0.571922 0.774553 0.866332 0.092 Uiso 1 1 calc R . . . . C22 C 0.5206(16) 0.8802(10) 0.7946(12) 0.061(4) Uani 1 1 d . . . . . H22A H 0.463270 0.922477 0.826907 0.073 Uiso 1 1 calc R . . . . H22B H 0.620831 0.896389 0.800456 0.073 Uiso 1 1 calc R . . . . I2 I 0.76500(9) 0.60012(6) 0.86486(5) 0.0456(3) Uani 1 1 d . . . . . O2 O 0.500000 0.7351(7) 0.750000 0.035(3) Uani 1 2 d S T P A . P1 P 0.500000 0.3323(3) 0.750000 0.0466(12) Uani 1 2 d DS T P . . U1 U 0.500000 0.57218(3) 0.750000 0.0257(2) Uani 1 2 d S T P . . C11 C 0.600(3) 0.6122(13) 0.5375(13) 0.0257(2) Uani 0.515(16) 1 d . . . A 1 C12 C 0.707(3) 0.6658(15) 0.4922(14) 0.0257(2) Uani 0.485(16) 1 d . . . A 1 H12A H 0.697955 0.728613 0.505224 0.031 Uiso 0.485(16) 1 calc R . . A 1 H12B H 0.703530 0.656939 0.430206 0.031 Uiso 0.485(16) 1 calc R . . A 1 C13 C 0.853(2) 0.6226(15) 0.5350(13) 0.0257(2) Uani 0.485(16) 1 d . . . A 1 H13A H 0.940220 0.650840 0.515455 0.031 Uiso 0.485(16) 1 calc R . . A 1 H13B H 0.858439 0.558585 0.528467 0.031 Uiso 0.485(16) 1 calc R . . A 1 C14 C 0.803(2) 0.6543(15) 0.6325(12) 0.0257(2) Uani 0.515(16) 1 d . . . A 1 O1 O 0.654(2) 0.6052(10) 0.6249(14) 0.0257(2) Uani 0.485(16) 1 d . . . A 1 C11A C 0.628(3) 0.5863(15) 0.5394(15) 0.0257(2) Uani 0.485(16) 1 d . . . A 2 C12A C 0.727(2) 0.6379(14) 0.4825(13) 0.0257(2) Uani 0.515(16) 1 d . . . A 2 H12C H 0.766188 0.600727 0.437139 0.031 Uiso 0.515(16) 1 calc R . . A 2 H12D H 0.678178 0.688215 0.456640 0.031 Uiso 0.515(16) 1 calc R . . A 2 C13A C 0.839(2) 0.6674(14) 0.5418(12) 0.0257(2) Uani 0.515(16) 1 d . . . A 2 H13C H 0.834269 0.730992 0.551676 0.031 Uiso 0.515(16) 1 calc R . . A 2 H13D H 0.933831 0.652364 0.520076 0.031 Uiso 0.515(16) 1 calc R . . A 2 C14A C 0.804(3) 0.6156(16) 0.6233(13) 0.0257(2) Uani 0.485(16) 1 d . . . A 2 O1A O 0.645(2) 0.6227(10) 0.6259(13) 0.0257(2) Uani 0.515(16) 1 d . . . A 2 B1 B 0.5940(18) 0.4076(9) 0.6698(10) 0.042(3) Uani 1 1 d . . . . . H1A H 0.508209 0.448922 0.631299 0.063 Uiso 1 1 calc GR . . . . H1B H 0.661255 0.364174 0.621379 0.063 Uiso 1 1 calc GR . . . . H1C H 0.670794 0.456337 0.706959 0.063 Uiso 1 1 calc GR . . . . H1 H 0.585(13) 0.283(3) 0.793(9) 0.09(6) Uiso 1 1 d D . . . . 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 C21 0.15(2) 0.037(7) 0.046(8) -0.017(7) -0.015(10) -0.005(9) C22 0.049(9) 0.042(8) 0.091(13) -0.005(8) -0.013(8) -0.004(6) I2 0.0467(5) 0.0419(5) 0.0481(5) -0.0030(4) -0.0117(4) 0.0008(4) O2 0.047(7) 0.025(5) 0.033(6) 0.000 -0.009(5) 0.000 P1 0.074(4) 0.0207(19) 0.045(3) 0.000 -0.004(2) 0.000 U1 0.0349(3) 0.0206(3) 0.0215(3) 0.000 -0.0028(2) 0.000 C11 0.0349(3) 0.0206(3) 0.0215(3) 0.000 -0.0028(2) 0.000 C12 0.0349(3) 0.0206(3) 0.0215(3) 0.000 -0.0028(2) 0.000 C13 0.0349(3) 0.0206(3) 0.0215(3) 0.000 -0.0028(2) 0.000 C14 0.0349(3) 0.0206(3) 0.0215(3) 0.000 -0.0028(2) 0.000 O1 0.0349(3) 0.0206(3) 0.0215(3) 0.000 -0.0028(2) 0.000 C11A 0.0349(3) 0.0206(3) 0.0215(3) 0.000 -0.0028(2) 0.000 C12A 0.0349(3) 0.0206(3) 0.0215(3) 0.000 -0.0028(2) 0.000 C13A 0.0349(3) 0.0206(3) 0.0215(3) 0.000 -0.0028(2) 0.000 C14A 0.0349(3) 0.0206(3) 0.0215(3) 0.000 -0.0028(2) 0.000 O1A 0.0349(3) 0.0206(3) 0.0215(3) 0.000 -0.0028(2) 0.000 B1 0.060(9) 0.024(6) 0.043(7) -0.008(6) -0.001(7) 0.002(6) 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' B B 0.0013 0.0007 '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' 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' 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 C22 C21 O2 105.3(14) . . ? C22 C22 C21 106.6(10) 3_656 . ? C21 O2 C21 108.5(16) . 3_656 ? C21 O2 U1 125.8(8) . . ? C21 O2 U1 125.8(8) 3_656 . ? B1 P1 B1 106.7(8) 3_656 . ? I2 U1 I2 164.29(4) . 3_656 ? O2 U1 I2 82.144(19) . . ? O2 U1 I2 82.144(19) . 3_656 ? O2 U1 O1 78.4(4) . 3_656 ? O2 U1 O1 78.4(4) . . ? O2 U1 O1A 72.1(4) . . ? O2 U1 O1A 72.1(3) . 3_656 ? O1 U1 I2 87.6(5) . . ? O1 U1 I2 87.6(5) 3_656 3_656 ? O1 U1 I2 89.2(5) . 3_656 ? O1 U1 I2 89.2(5) 3_656 . ? O1 U1 O1 156.7(7) . 3_656 ? O1 U1 O1A 150.4(4) . 3_656 ? O1 U1 O1A 6.4(6) 3_656 3_656 ? O1A U1 I2 88.2(5) . . ? O1A U1 I2 87.0(5) 3_656 . ? O1A U1 O1A 144.2(7) . 3_656 ? O1 C11 C12 104.3(18) . . ? C11 C12 C13 98.9(17) . . ? C12 C13 C14 91.3(16) . . ? O1 C14 C13 92.6(15) . . ? C11 O1 U1 122.9(16) . . ? C11 O1 C14 110.2(17) . . ? C14 O1 U1 123.3(13) . . ? O1A C11A C12A 106.4(18) . . ? C13A C12A C11A 103.3(17) . . ? C12A C13A C14A 102.3(17) . . ? O1A C14A C13A 101.5(17) . . ? C11A O1A U1 122.8(14) . . ? C11A O1A C14A 93.1(17) . . ? C14A O1A U1 123.0(13) . . ? 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 C21 C22 1.47(2) . ? C21 O2 1.483(16) . ? C22 C22 1.46(4) 3_656 ? I2 U1 3.1382(9) . ? O2 U1 2.501(11) . ? P1 B1 1.935(16) 3_656 ? P1 B1 1.935(16) . ? U1 O1 2.51(2) 3_656 ? U1 O1 2.51(2) . ? U1 O1A 2.52(2) . ? U1 O1A 2.52(2) 3_656 ? C11 C12 1.50(3) . ? C11 O1 1.48(3) . ? C12 C13 1.68(3) . ? C13 C14 1.69(3) . ? C14 O1 1.61(3) . ? C11A C12A 1.52(3) . ? C11A O1A 1.49(3) . ? C12A C13A 1.49(3) . ? C13A C14A 1.55(3) . ? C14A O1A 1.52(3) . ?