#------------------------------------------------------------------------------ #$Date: 2016-04-04 13:48:36 +0300 (Mon, 04 Apr 2016) $ #$Revision: 181379 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/08/64/4086451.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_4086451 loop_ _publ_author_name 'Magnuson, Kevin W.' 'Oshiro, Shelly M.' 'Gurr, Joshua R.' 'Yoshida, Wesley Y.' 'Gembicky, Milan' 'Rheingold, Arnold L.' 'Hughes, Russell P.' 'Cain, Matthew F.' _publ_contact_author_name ; ; _publ_section_title ; Streamlined Preparation and Coordination Chemistry of Hybrid Phosphine--Phosphaalkene Ligands ; _journal_issue 6 _journal_name_full Organometallics _journal_page_first 855 _journal_page_last 859 _journal_paper_doi 10.1021/acs.organomet.6b00101 _journal_volume 35 _journal_year 2016 _chemical_formula_moiety 'C32 H54 P2' _chemical_formula_sum 'C32 H54 P2' _chemical_formula_weight 500.69 _chemical_name_common SO7 _chemical_name_systematic ; ? ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_date 2016-02-05 _audit_creation_method ; Olex2 1.2 (compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103) ; _cell_angle_alpha 101.584(4) _cell_angle_beta 109.156(4) _cell_angle_gamma 99.100(5) _cell_formula_units_Z 2 _cell_length_a 9.8594(12) _cell_length_b 11.7510(16) _cell_length_c 14.647(2) _cell_measurement_reflns_used 4945 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.28 _cell_measurement_theta_min 2.20 _cell_volume 1523.6(4) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XM (Sheldrick, 2008)' _diffrn_ambient_temperature 100.0 _diffrn_detector 'Bruker APEX-II CCD' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD Area Detector' _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device 'Kappa Four-Circle Diffractometer' _diffrn_measurement_device_type 'Bruker APEX II Ultra' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'Double Bounce Multilayer Mirrors' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_unetI/netI 0.0449 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 7168 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.985 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 28.325 _diffrn_reflns_theta_min 1.529 _diffrn_source 'Micro Focus Rotating Anode' _diffrn_source_type 'Bruker TXS' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.160 _exptl_absorpt_correction_T_max 0.0962 _exptl_absorpt_correction_T_min 0.0627 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0619 before and 0.0436 after correction. The Ratio of minimum to maximum transmission is 0.6518. The \l/2 correction factor is 0.00150. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.091 _exptl_crystal_description block _exptl_crystal_F_000 552 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.22 _refine_diff_density_max 0.403 _refine_diff_density_min -0.234 _refine_diff_density_rms 0.055 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 336 _refine_ls_number_reflns 7168 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.047 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0410 _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^)+(0.0469P)^2^+0.5630P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1008 _refine_ls_wR_factor_ref 0.1078 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6211 _reflns_number_total 7168 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file om6b00101_si_006.cif _cod_data_source_block cain02 _cod_depositor_comments ; The following automatic conversions were performed: '_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according to the built-in table from CIF Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 4609 2016-04-01 06:22:49Z antanas ; _cod_database_code 4086451 _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. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.7815(9) 0.2185(9) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 3. Others Sof(C26')=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27')=Sof(H27D)=Sof(H27E)= Sof(H27F)=Sof(C28')=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(1) Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)= Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(1) 4.a Ternary CH refined with riding coordinates: C3(H3), C9(H9) 4.b Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B) 4.c Me refined with riding coordinates: C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B, H26C), C26'(H26D,H26E,H26F), C27(H27A,H27B,H27C), C27'(H27D,H27E,H27F), C28(H28A,H28B,H28C), C28'(H28D,H28E,H28F), C30(H30A,H30B,H30C), C31(H31A,H31B, H31C), C32(H32A,H32B,H32C) 4.d Aromatic/amide H refined with riding coordinates: C2(H2), C17(H17), C19(H19) ; _shelx_res_file ; cain02.res created by SHELXL-2014/7 TITL cain02 in P-1 CELL 0.71073 9.8594 11.751 14.6467 101.584 109.156 99.1 ZERR 2 0.0012 0.0016 0.002 0.004 0.004 0.005 LATT 1 SFAC C H P UNIT 64 108 4 L.S. 4 PLAN 10 0 0 TEMP -173.15 BOND fmap 2 acta 50 OMIT -9 5 8 OMIT 0 -1 1 REM REM REM WGHT 0.046900 0.563000 BASF 0.21849 FVAR 0.79588 0.86270 P1 3 0.032349 0.293420 0.541677 11.00000 0.01540 0.01686 = 0.01654 0.00384 0.00695 0.00316 P2 3 0.003175 0.093156 0.746822 11.00000 0.01873 0.01560 = 0.01610 0.00228 0.00655 0.00323 C1 1 -0.079317 0.177044 0.575820 11.00000 0.01589 0.02065 = 0.01870 0.00591 0.00773 0.00333 AFIX 23 H1A 2 -0.185192 0.177125 0.546594 11.00000 -1.20000 H1B 2 -0.067936 0.097232 0.546462 11.00000 -1.20000 AFIX 0 C2 1 -0.033266 0.198098 0.687459 11.00000 0.01645 0.01887 = 0.01860 0.00423 0.00923 0.00347 AFIX 43 H2 2 -0.024409 0.275897 0.726506 11.00000 -1.20000 AFIX 0 C3 1 0.158391 0.212580 0.499404 11.00000 0.01724 0.01892 = 0.01869 0.00411 0.00805 0.00500 AFIX 13 H3 2 0.097622 0.144283 0.439043 11.00000 -1.20000 AFIX 0 C4 1 0.258972 0.299831 0.469942 11.00000 0.03067 0.03186 = 0.04422 0.02148 0.02571 0.01578 AFIX 23 H4A 2 0.197222 0.325490 0.413142 11.00000 -1.20000 H4B 2 0.310988 0.371888 0.527309 11.00000 -1.20000 AFIX 0 C5 1 0.373486 0.244113 0.439735 11.00000 0.02937 0.03923 = 0.04111 0.01971 0.02424 0.01590 AFIX 23 H5A 2 0.322033 0.178012 0.377443 11.00000 -1.20000 H5B 2 0.439378 0.305220 0.425652 11.00000 -1.20000 AFIX 0 C6 1 0.465908 0.196165 0.521762 11.00000 0.01679 0.02953 = 0.03502 0.00616 0.01141 0.00521 AFIX 23 H6A 2 0.526284 0.263393 0.581778 11.00000 -1.20000 H6B 2 0.533979 0.155961 0.498159 11.00000 -1.20000 AFIX 0 C7 1 0.366260 0.107563 0.549540 11.00000 0.02154 0.02918 = 0.03210 0.01253 0.01120 0.01154 AFIX 23 H7A 2 0.427733 0.080551 0.605545 11.00000 -1.20000 H7B 2 0.313687 0.036531 0.491297 11.00000 -1.20000 AFIX 0 C8 1 0.253041 0.163968 0.580742 11.00000 0.02065 0.02888 = 0.02327 0.00942 0.00981 0.00932 AFIX 23 H8A 2 0.187857 0.103149 0.595598 11.00000 -1.20000 H8B 2 0.305712 0.230022 0.642939 11.00000 -1.20000 AFIX 0 C9 1 -0.105298 0.297032 0.420053 11.00000 0.01602 0.01967 = 0.01741 0.00476 0.00690 0.00384 AFIX 13 H9 2 -0.048892 0.342933 0.387945 11.00000 -1.20000 AFIX 0 C10 1 -0.213284 0.369607 0.441268 11.00000 0.01934 0.01850 = 0.02210 0.00348 0.00667 0.00501 AFIX 23 H10A 2 -0.268010 0.329349 0.476451 11.00000 -1.20000 H10B 2 -0.156628 0.450073 0.486097 11.00000 -1.20000 AFIX 0 C11 1 -0.323930 0.382836 0.344598 11.00000 0.02099 0.02085 = 0.02719 0.00755 0.00316 0.00583 AFIX 23 H11A 2 -0.395586 0.425317 0.360937 11.00000 -1.20000 H11B 2 -0.270515 0.431395 0.313366 11.00000 -1.20000 AFIX 0 C12 1 -0.407030 0.260689 0.270446 11.00000 0.02002 0.02540 = 0.02129 0.00615 0.00381 0.00349 AFIX 23 H12A 2 -0.467423 0.214803 0.299351 11.00000 -1.20000 H12B 2 -0.474764 0.271711 0.207682 11.00000 -1.20000 AFIX 0 C13 1 -0.300107 0.190695 0.246742 11.00000 0.02264 0.02918 = 0.01881 0.00253 0.00624 0.00489 AFIX 23 H13A 2 -0.245648 0.233246 0.212599 11.00000 -1.20000 H13B 2 -0.356270 0.110783 0.200613 11.00000 -1.20000 AFIX 0 C14 1 -0.189637 0.175947 0.342913 11.00000 0.02325 0.02269 = 0.02073 0.00165 0.00632 0.00786 AFIX 23 H14A 2 -0.118023 0.134021 0.325851 11.00000 -1.20000 H14B 2 -0.243472 0.125836 0.372933 11.00000 -1.20000 AFIX 0 C15 1 0.051904 0.177370 0.879480 11.00000 0.01823 0.01306 = 0.01677 0.00428 0.00688 0.00502 C16 1 -0.055179 0.167258 0.924746 11.00000 0.01596 0.01630 = 0.01886 0.00917 0.00619 0.00670 C17 1 -0.027081 0.251025 1.015675 11.00000 0.02075 0.01848 = 0.01899 0.00923 0.01055 0.00920 AFIX 43 H17 2 -0.099852 0.246293 1.045047 11.00000 -1.20000 AFIX 0 C18 1 0.102816 0.340745 1.064683 11.00000 0.02362 0.01486 = 0.01652 0.00683 0.00840 0.00717 C19 1 0.210466 0.340586 1.023611 11.00000 0.02086 0.01495 = 0.01897 0.00287 0.00671 0.00124 AFIX 43 H19 2 0.301963 0.398613 1.058352 11.00000 -1.20000 AFIX 0 C20 1 0.192369 0.260022 0.934009 11.00000 0.01834 0.01643 = 0.01819 0.00492 0.00684 0.00337 C21 1 -0.199888 0.066426 0.880810 11.00000 0.01496 0.02120 = 0.01967 0.00870 0.00542 0.00418 C22 1 -0.313667 0.084716 0.787050 11.00000 0.01611 0.02846 = 0.02375 0.01090 0.00698 0.00664 AFIX 33 H22A 2 -0.334041 0.163625 0.803840 11.00000 -1.50000 H22B 2 -0.273787 0.079712 0.733652 11.00000 -1.50000 H22C 2 -0.405536 0.022444 0.764025 11.00000 -1.50000 AFIX 0 C23 1 -0.166236 -0.057277 0.856021 11.00000 0.01903 0.01776 = 0.02772 0.00791 0.00474 0.00183 AFIX 33 H23A 2 -0.093822 -0.067730 0.916222 11.00000 -1.50000 H23B 2 -0.257618 -0.120019 0.833225 11.00000 -1.50000 H23C 2 -0.125868 -0.062751 0.802852 11.00000 -1.50000 AFIX 0 C24 1 -0.275589 0.061487 0.957390 11.00000 0.02064 0.03257 = 0.02506 0.01062 0.01002 0.00192 AFIX 33 H24A 2 -0.206625 0.049878 1.018470 11.00000 -1.50000 H24B 2 -0.304416 0.136732 0.974033 11.00000 -1.50000 H24C 2 -0.363810 -0.005285 0.928312 11.00000 -1.50000 AFIX 0 C25 1 0.132810 0.434846 1.163219 11.00000 0.03490 0.01723 = 0.01869 0.00446 0.01309 0.00822 PART 1 C26 1 0.009260 0.419696 1.201318 21.00000 0.03750 0.02967 = 0.02943 -0.00094 0.02135 0.00248 AFIX 33 H26A 2 0.035119 0.482069 1.263915 21.00000 -1.50000 H26B 2 -0.081436 0.426354 1.151095 21.00000 -1.50000 H26C 2 -0.006724 0.340754 1.213868 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C26' 1 -0.050306 0.460871 1.147532 -21.00000 0.03614 0.02388 = 0.03178 -0.01216 0.01614 0.01029 AFIX 33 H26D 2 -0.118649 0.385704 1.138801 -21.00000 -1.50000 H26E 2 -0.043900 0.520397 1.207155 -21.00000 -1.50000 H26F 2 -0.086614 0.490474 1.088225 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 C27 1 0.276201 0.425182 1.245660 21.00000 0.03911 0.03042 = 0.01752 0.00452 0.00440 0.01518 AFIX 33 H27A 2 0.358587 0.434865 1.222202 21.00000 -1.50000 H27B 2 0.300158 0.488067 1.307629 21.00000 -1.50000 H27C 2 0.259542 0.346569 1.258710 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C27' 1 0.148158 0.374817 1.242026 -21.00000 0.10576 0.05832 = 0.02634 0.01702 0.02399 0.05797 AFIX 33 H27D 2 0.080980 0.294825 1.214255 -21.00000 -1.50000 H27E 2 0.250395 0.367661 1.269924 -21.00000 -1.50000 H27F 2 0.123479 0.421359 1.295205 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 C28 1 0.164986 0.561414 1.148442 21.00000 0.04296 0.01410 = 0.02548 0.00610 0.01556 0.00924 AFIX 33 H28A 2 0.245891 0.570406 1.123531 21.00000 -1.50000 H28B 2 0.076048 0.572704 1.099684 21.00000 -1.50000 H28C 2 0.193440 0.621453 1.212734 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C28' 1 0.204954 0.542001 1.173379 -21.00000 0.07828 0.02455 = 0.03723 0.00707 0.04273 0.01955 AFIX 33 H28D 2 0.173613 0.560792 1.108500 -21.00000 -1.50000 H28E 2 0.184394 0.599896 1.222294 -21.00000 -1.50000 H28F 2 0.311310 0.546198 1.197012 -21.00000 -1.50000 AFIX 0 PART 0 C29 1 0.328117 0.268529 0.902147 11.00000 0.01707 0.02146 = 0.02095 -0.00012 0.00827 0.00012 C30 1 0.473564 0.314079 0.994705 11.00000 0.01902 0.04664 = 0.02725 -0.00421 0.00781 0.00184 AFIX 33 H30A 2 0.478395 0.258947 1.037143 11.00000 -1.50000 H30B 2 0.557679 0.318414 0.972841 11.00000 -1.50000 H30C 2 0.477193 0.393866 1.033041 11.00000 -1.50000 AFIX 0 C31 1 0.325419 0.357641 0.837916 11.00000 0.02673 0.02503 = 0.03155 0.00466 0.01666 -0.00136 AFIX 33 H31A 2 0.233781 0.330881 0.778255 11.00000 -1.50000 H31B 2 0.330136 0.437109 0.877404 11.00000 -1.50000 H31C 2 0.410621 0.361657 0.817204 11.00000 -1.50000 AFIX 0 C32 1 0.339988 0.146587 0.846833 11.00000 0.01903 0.02634 = 0.02575 0.00314 0.00961 0.00671 AFIX 33 H32A 2 0.341546 0.091193 0.888844 11.00000 -1.50000 H32B 2 0.254655 0.113921 0.783376 11.00000 -1.50000 H32C 2 0.431317 0.157062 0.833084 11.00000 -1.50000 AFIX 0 HKLF 5 REM cain02 in P-1 REM R1 = 0.0410 for 6211 Fo > 4sig(Fo) and 0.0508 for all 7168 data REM 336 parameters refined using 0 restraints END WGHT 0.0469 0.5630 REM Highest difference peak 0.403, deepest hole -0.234, 1-sigma level 0.055 Q1 1 -0.1518 0.2382 0.3809 11.00000 0.05 0.40 Q2 1 -0.1617 0.3371 0.4250 11.00000 0.05 0.32 Q3 1 0.0188 0.1541 0.7206 11.00000 0.05 0.32 Q4 1 -0.2466 0.1877 0.2982 11.00000 0.05 0.31 Q5 1 0.2567 0.2611 0.9154 11.00000 0.05 0.30 Q6 1 -0.2785 0.3625 0.3880 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2.78318 1 0 -9 17 0.24956 4.29708 -2 -5 -9 17 0.24956 4.29708 1 -1 -9 17 1.85462 4.21098 -2 -4 -9 17 1.85462 4.21098 1 -2 -9 17 15.9856 4.94496 -2 -3 -9 17 15.9856 4.94496 1 -3 -9 17 2.31438 3.91972 -2 -2 -9 17 2.31438 3.91972 1 -4 -9 17 1.40351 3.92336 -2 -1 -9 17 1.40351 3.92336 1 -7 -8 17 42.8016 5.66475 1 -6 -8 17 7.43392 3.34973 1 -5 -8 17 3.02527 2.55131 1 -4 -8 17 77.0512 6.69617 1 -3 -8 17 32.3065 4.73880 1 -2 -8 17 4.74552 2.58025 1 -1 -8 17 80.7551 6.61807 1 0 -8 17 1.21190 1.49811 1 1 -8 17 37.5047 3.79801 1 1 -7 17 219.592 13.3403 -2 -7 -7 17 219.592 13.3403 1 0 -7 17 30.5453 5.95089 -2 -6 -7 17 30.5453 5.95089 1 -1 -7 17 95.4529 8.05035 -2 -5 -7 17 95.4529 8.05035 1 -2 -7 17 60.6086 6.34008 -2 -4 -7 17 60.6086 6.34008 1 -3 -7 17 -2.1010 3.95820 -2 -3 -7 17 -2.1010 3.95820 1 -4 -7 17 21.0216 4.57604 -2 -2 -7 17 21.0216 4.57604 1 -5 -7 17 63.6667 4.56555 -2 -1 -7 17 63.6667 4.56555 1 -6 -7 17 31.6871 3.51058 -2 0 -7 17 31.6871 3.51058 1 -7 -7 17 75.9493 7.48006 -2 1 -7 17 75.9493 7.48006 1 -8 -6 17 152.525 10.2339 1 -7 -6 17 230.533 13.2819 1 0 -6 17 23.2282 5.41005 -2 -6 -6 17 23.2282 5.41005 1 -1 -6 17 12.6913 4.93725 -2 -5 -6 17 12.6913 4.93725 1 -2 -6 17 6.90307 4.03478 -2 -4 -6 17 6.90307 4.03478 1 -3 -6 17 0.32838 4.06461 -2 -3 -6 17 0.32838 4.06461 1 -4 -6 17 55.8139 5.72904 -2 -2 -6 17 55.8139 5.72904 1 -5 -6 17 9.99747 5.25590 -2 -1 -6 17 9.99747 5.25590 1 -6 -6 17 12.3603 5.24255 -2 0 -6 17 12.3603 5.24255 1 -7 -6 17 100.749 9.10782 -2 1 -6 17 100.749 9.10782 1 -8 -6 17 110.690 9.68356 -2 2 -6 17 110.690 9.68356 1 -8 -5 17 64.7889 6.72248 1 -7 -5 17 11.0946 3.28119 1 -6 -5 17 11.4790 3.18486 1 -5 -5 17 13.9316 3.16681 1 -4 -5 17 28.8310 4.11647 1 -3 -5 17 79.1701 6.00295 1 -2 -5 17 27.1255 2.91583 1 -1 -5 17 -2.0171 1.25343 1 0 -5 17 11.2814 2.42648 1 1 -5 17 6.27996 2.00462 1 2 -5 17 9.38882 2.36123 1 2 -4 17 2.35718 2.55749 -2 -9 -4 17 2.35718 2.55749 1 1 -4 17 35.4478 4.53418 -2 -8 -4 17 35.4478 4.53418 1 0 -4 17 70.8953 5.95465 -2 -7 -4 17 70.8953 5.95465 1 -1 -4 17 10.2222 3.15768 -2 -6 -4 17 10.2222 3.15768 1 -2 -4 17 4.39289 3.02558 -2 -5 -4 17 4.39289 3.02558 1 -3 -4 17 -1.3474 2.22147 -2 -4 -4 17 -1.3474 2.22147 1 -4 -4 17 -2.5695 1.70692 -2 -3 -4 17 -2.5695 1.70692 1 -5 -4 17 15.7589 2.48713 -2 -2 -4 17 15.7589 2.48713 1 -6 -4 17 46.2915 5.53177 -2 -1 -4 17 46.2915 5.53177 1 -7 -4 17 109.023 8.45885 -2 0 -4 17 109.023 8.45885 1 -8 -4 17 99.9917 8.33098 -2 1 -4 17 99.9917 8.33098 1 -9 -4 17 -5.4279 3.69339 -2 2 -4 17 -5.4279 3.69339 1 -9 -3 17 4.21879 2.89064 1 -8 -3 17 -1.5135 2.00719 1 -7 -3 17 5.75319 2.42108 1 -6 -3 17 -0.8539 1.75788 1 -5 -3 17 10.2978 2.68293 1 -4 -3 17 77.5242 4.37931 1 -3 -3 17 49.8471 3.70920 1 -2 -3 17 83.0512 4.50311 1 -1 -3 17 55.5573 6.33655 1 0 -3 17 7.07207 3.42321 1 1 -3 17 93.1702 7.98373 1 2 -3 17 17.9278 4.34451 1 1 -2 17 96.4492 7.63472 -2 -9 -2 17 96.4492 7.63472 1 0 -2 17 92.4632 7.61163 -2 -8 -2 17 92.4632 7.61163 1 -1 -2 17 113.509 7.77705 -2 -7 -2 17 113.509 7.77705 1 -2 -2 17 74.7893 5.95391 -2 -6 -2 17 74.7893 5.95391 1 -3 -2 17 137.394 6.35667 -2 -5 -2 17 137.394 6.35667 1 -4 -2 17 620.076 20.4971 -2 -4 -2 17 620.076 20.4971 1 -5 -2 17 134.253 6.08999 -2 -3 -2 17 134.253 6.08999 1 -6 -2 17 131.434 9.67826 -2 -2 -2 17 131.434 9.67826 1 -7 -2 17 253.303 14.8282 -2 -1 -2 17 253.303 14.8282 1 -8 -2 17 199.092 12.6601 -2 0 -2 17 199.092 12.6601 1 -9 -2 17 247.639 14.9026 -2 1 -2 17 247.639 14.9026 1 2 -2 17 120.083 9.44086 1 1 -1 17 5.82688 4.32735 -2 -9 -1 17 5.82688 4.32735 1 0 -1 17 89.2290 7.24760 -2 -8 -1 17 89.2290 7.24760 1 -1 -1 17 25.3303 4.77393 -2 -7 -1 17 25.3303 4.77393 1 -2 -1 17 2.97847 2.80059 -2 -6 -1 17 2.97847 2.80059 1 -3 -1 17 172.127 7.22333 -2 -5 -1 17 172.127 7.22333 1 -4 -1 17 40.6815 3.47178 -2 -4 -1 17 40.6815 3.47178 1 -5 -1 17 62.1860 6.87593 -2 -3 -1 17 62.1860 6.87593 1 -6 -1 17 -1.3387 4.42665 -2 -2 -1 17 -1.3387 4.42665 1 -7 -1 17 18.3874 5.77402 -2 -1 -1 17 18.3874 5.77402 1 -8 -1 17 14.5252 5.47676 -2 0 -1 17 14.5252 5.47676 1 -9 -1 17 6.71644 5.45596 -2 1 -1 17 6.71644 5.45596 1 -9 0 17 0.12851 1.35433 1 -8 0 17 4.43647 1.64601 1 -7 0 17 14.7287 2.17732 1 -6 0 17 9.42956 1.81737 1 -5 0 17 33.3139 2.84911 1 -4 0 17 84.2201 4.33531 1 -3 0 17 4.73977 2.87240 1 -2 0 17 -2.7302 2.37227 1 -1 0 17 7.22092 3.21037 1 0 0 17 -3.2696 2.41270 1 1 0 17 5.01488 2.65141 1 0 1 17 1.47543 2.53281 -2 -9 1 17 1.47543 2.53281 1 -1 1 17 2.84347 1.86760 -2 -8 1 17 2.84347 1.86760 1 -2 1 17 35.3931 2.82029 -2 -7 1 17 35.3931 2.82029 1 -3 1 17 12.2357 1.97909 -2 -6 1 17 12.2357 1.97909 1 -4 1 17 151.525 6.32442 -2 -5 1 17 151.525 6.32442 1 -5 1 17 39.3042 4.71955 -2 -4 1 17 39.3042 4.71955 1 -6 1 17 24.1890 4.34374 -2 -3 1 17 24.1890 4.34374 1 -7 1 17 32.1665 5.03225 -2 -2 1 17 32.1665 5.03225 1 -8 1 17 6.50049 4.07932 -2 -1 1 17 6.50049 4.07932 1 -9 1 17 1.75018 3.94787 -2 0 1 17 1.75018 3.94787 1 -9 2 17 -1.6626 1.71130 1 -8 2 17 5.41085 1.66488 1 -7 2 17 16.5469 2.08231 1 -6 2 17 12.6954 1.93190 1 -5 2 17 108.228 7.75864 1 -4 2 17 6.75745 2.90085 1 -3 2 17 0.56092 2.42684 1 -2 2 17 6.89586 3.28707 1 -1 2 17 5.35872 3.22168 1 -2 3 17 120.113 8.06074 -2 -8 3 17 120.113 8.06074 1 -3 3 17 75.6816 4.31629 -2 -7 3 17 75.6816 4.31629 1 -4 3 17 24.7094 5.47425 -2 -6 3 17 24.7094 5.47425 1 -5 3 17 5.36169 4.46807 -2 -5 3 17 5.36169 4.46807 1 -6 3 17 28.7920 6.05981 -2 -4 3 17 28.7920 6.05981 1 -7 3 17 49.6622 7.07584 -2 -3 3 17 49.6622 7.07584 1 -8 3 17 141.035 10.8873 -2 -2 3 17 141.035 10.8873 1 -1 3 17 134.364 9.78245 1 -4 4 17 39.7341 5.28090 -2 -6 4 17 39.7341 5.28090 1 -5 4 17 64.2327 6.85303 -2 -5 4 17 64.2327 6.85303 1 -6 4 17 72.4182 7.11602 -2 -4 4 17 72.4182 7.11602 1 -7 4 17 16.0048 5.69303 -2 -3 4 17 16.0048 5.69303 1 -1 -8 18 8.15521 4.23835 -2 -5 -8 18 8.15521 4.23835 1 -2 -8 18 28.1805 4.79488 -2 -4 -8 18 28.1805 4.79488 1 -3 -8 18 4.66408 3.29663 -2 -3 -8 18 4.66408 3.29663 1 -4 -8 18 76.7827 6.36072 -2 -2 -8 18 76.7827 6.36072 1 -5 -8 18 27.5166 3.24174 -2 -1 -8 18 27.5166 3.24174 1 -6 -7 18 21.0900 4.15442 1 -5 -7 18 2.88915 2.62643 1 -4 -7 18 10.8775 3.35053 1 -3 -7 18 156.447 9.68840 1 -2 -7 18 67.4131 5.84145 1 -1 -7 18 4.56361 1.76326 1 0 -7 18 10.8897 3.47191 1 0 -6 18 54.1056 7.30057 -2 -7 -6 18 54.1056 7.30057 1 -1 -6 18 78.8696 7.82292 -2 -6 -6 18 78.8696 7.82292 1 -2 -6 18 40.5007 5.87418 -2 -5 -6 18 40.5007 5.87418 1 -3 -6 18 49.5176 5.90766 -2 -4 -6 18 49.5176 5.90766 1 -4 -6 18 77.9122 7.10395 -2 -3 -6 18 77.9122 7.10395 1 -5 -6 18 202.657 8.71288 -2 -2 -6 18 202.657 8.71288 1 -6 -6 18 117.821 9.52879 -2 -1 -6 18 117.821 9.52879 1 -7 -6 18 37.9166 6.53336 -2 0 -6 18 37.9166 6.53336 1 0 -5 18 170.931 10.8462 -2 -7 -5 18 170.931 10.8462 1 -1 -5 18 21.8798 5.06261 -2 -6 -5 18 21.8798 5.06261 1 -2 -5 18 66.8111 6.12576 -2 -5 -5 18 66.8111 6.12576 1 -3 -5 18 140.818 8.95047 -2 -4 -5 18 140.818 8.95047 1 -4 -5 18 99.8584 5.50202 -2 -3 -5 18 99.8584 5.50202 1 -5 -5 18 19.3642 3.07190 -2 -2 -5 18 19.3642 3.07190 1 -6 -5 18 27.8275 5.74816 -2 -1 -5 18 27.8275 5.74816 1 -7 -5 18 52.0834 6.70996 -2 0 -5 18 52.0834 6.70996 1 -8 -4 18 80.1779 6.77894 1 -7 -4 18 40.8972 5.07720 1 -6 -4 18 10.5688 3.02851 1 -5 -4 18 5.74524 2.36822 1 -4 -4 18 4.30053 1.82396 1 -3 -4 18 14.3002 2.13397 1 -2 -4 18 -1.4869 2.66411 1 -1 -4 18 10.7196 3.62508 1 0 -4 18 0.54449 2.08673 1 0 -3 18 49.5790 5.39542 -2 -8 -3 18 49.5790 5.39542 1 -1 -3 18 19.8160 3.97062 -2 -7 -3 18 19.8160 3.97062 1 -2 -3 18 20.9680 3.83032 -2 -6 -3 18 20.9680 3.83032 1 -3 -3 18 26.9214 3.14385 -2 -5 -3 18 26.9214 3.14385 1 -4 -3 18 34.5491 3.23743 -2 -4 -3 18 34.5491 3.23743 1 -5 -3 18 45.6806 5.87430 -2 -3 -3 18 45.6806 5.87430 1 -6 -3 18 72.4367 7.19264 -2 -2 -3 18 72.4367 7.19264 1 -7 -3 18 57.8613 6.54657 -2 -1 -3 18 57.8613 6.54657 1 -8 -3 18 79.6129 7.52369 -2 0 -3 18 79.6129 7.52369 1 -8 -2 18 24.8627 4.05542 1 -7 -2 18 73.8894 6.04784 1 -6 -2 18 11.6929 2.05899 1 -5 -2 18 -0.4449 1.35482 1 -4 -2 18 44.2790 3.46603 1 -3 -2 18 64.5346 6.68327 1 -2 -2 18 61.2206 6.74971 1 -1 -2 18 4.99004 2.54096 1 0 -2 18 18.5306 4.30711 1 -1 -1 18 49.0187 6.76044 -2 -8 -1 18 49.0187 6.76044 1 -7 -1 18 3.67120 1.64211 1 -3 -1 18 21.4895 4.16864 -2 -6 -1 18 21.4895 4.16864 1 -4 -1 18 66.1053 5.76722 -2 -5 -1 18 66.1053 5.76722 1 -4 -1 18 140.525 9.61920 1 -3 -1 18 50.8069 5.92080 1 -2 -1 18 148.358 10.1185 1 -8 -1 18 97.2603 9.01976 -2 -1 -1 18 97.2603 9.01976 1 0 -1 18 14.2170 3.91792 1 -1 0 18 300.853 11.1140 -2 -8 0 18 300.853 11.1140 1 -2 0 18 291.481 10.8172 -2 -7 0 18 291.481 10.8172 1 -3 0 18 75.8683 4.28024 -2 -6 0 18 75.8683 4.28024 1 -4 0 18 121.219 8.69855 -2 -5 0 18 121.219 8.69855 1 -5 0 18 268.312 15.2827 -2 -4 0 18 268.312 15.2827 1 -6 0 18 129.245 9.44025 -2 -3 0 18 129.245 9.44025 1 -7 0 18 164.842 11.2089 -2 -2 0 18 164.842 11.2089 1 -8 0 18 160.776 11.3562 -2 -1 0 18 160.776 11.3562 1 -8 1 18 4.05502 1.56127 1 -7 1 18 -1.1836 1.24808 1 -6 1 18 23.1049 2.55110 1 -5 1 18 2.08782 2.35181 1 -4 1 18 6.21150 3.09110 1 -3 1 18 17.6088 4.02993 1 -2 1 18 14.6071 3.86719 1 -3 2 18 4.86170 2.38024 -2 -7 2 18 4.86170 2.38024 1 -4 2 18 38.5104 5.08040 -2 -6 2 18 38.5104 5.08040 1 -5 2 18 -2.6969 4.09584 -2 -5 2 18 -2.6969 4.09584 1 -6 2 18 6.71877 4.83890 -2 -4 2 18 6.71877 4.83890 1 -7 2 18 2.10747 4.40824 -2 -3 2 18 2.10747 4.40824 1 -6 3 18 23.5377 4.11057 1 -5 3 18 79.6904 8.16606 -2 -5 3 18 79.6904 8.16606 1 -5 -6 19 17.8315 3.65552 1 -3 -6 19 12.9824 5.02930 -2 -4 -6 19 12.9824 5.02930 1 -4 -6 19 39.2889 4.26274 -2 -3 -6 19 39.2889 4.26274 1 -5 -6 19 12.1376 6.07931 -2 -2 -6 19 12.1376 6.07931 1 -6 -5 19 71.4492 6.22414 1 -5 -5 19 16.4803 3.39490 1 -4 -5 19 3.41285 1.70361 1 -3 -5 19 4.39259 1.75982 1 -2 -5 19 15.6878 4.10604 1 -2 -4 19 14.7581 3.42227 -2 -6 -4 19 14.7581 3.42227 1 -3 -4 19 15.8600 2.63688 -2 -5 -4 19 15.8600 2.63688 1 -4 -4 19 106.111 5.44589 -2 -4 -4 19 106.111 5.44589 1 -5 -4 19 48.2112 5.78797 -2 -3 -4 19 48.2112 5.78797 1 -6 -4 19 39.3919 5.31590 -2 -2 -4 19 39.3919 5.31590 1 -7 -3 19 49.7707 5.46008 1 -6 -3 19 13.0737 2.41443 1 -5 -3 19 0.92473 1.63375 1 -4 -3 19 1.52567 2.34983 1 -3 -3 19 12.5909 3.61058 1 -2 -3 19 2.71755 3.03484 1 -2 -2 19 61.5311 4.51057 -2 -7 -2 19 61.5311 4.51057 1 -3 -2 19 51.9028 4.02397 -2 -6 -2 19 51.9028 4.02397 1 -4 -2 19 12.6328 4.69284 -2 -5 -2 19 12.6328 4.69284 1 -5 -2 19 2.75455 4.36492 -2 -4 -2 19 2.75455 4.36492 1 -6 -2 19 41.9697 6.59270 -2 -3 -2 19 41.9697 6.59270 1 -7 -2 19 17.8834 5.15855 -2 -2 -2 19 17.8834 5.15855 1 -3 -1 19 104.122 5.52393 -2 -6 -1 19 104.122 5.52393 1 -4 -1 19 46.5758 6.50648 -2 -5 -1 19 46.5758 6.50648 1 -5 -1 19 31.4006 6.06815 -2 -4 -1 19 31.4006 6.06815 1 -6 -1 19 159.877 11.4583 -2 -3 -1 19 159.877 11.4583 1 -6 0 19 3.63991 2.52451 1 -5 0 19 43.0428 5.39717 1 -4 0 19 42.3583 5.48672 1 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 22795 _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 P1 P 0.03235(4) 0.29342(4) 0.54168(3) 0.01620(9) Uani 1 1 d . . . . . P2 P 0.00318(4) 0.09316(4) 0.74682(3) 0.01722(10) Uani 1 1 d . . . . . C1 C -0.07932(17) 0.17704(14) 0.57582(11) 0.0181(3) Uani 1 1 d . . . . . H1A H -0.1852 0.1771 0.5466 0.022 Uiso 1 1 calc R . . . . H1B H -0.0679 0.0972 0.5465 0.022 Uiso 1 1 calc R . . . . C2 C -0.03327(16) 0.19810(14) 0.68746(11) 0.0175(3) Uani 1 1 d . . . . . H2 H -0.0244 0.2759 0.7265 0.021 Uiso 1 1 calc R . . . . C3 C 0.15839(17) 0.21258(14) 0.49940(12) 0.0180(3) Uani 1 1 d . . . . . H3 H 0.0976 0.1443 0.4390 0.022 Uiso 1 1 calc R . . . . C4 C 0.2590(2) 0.29983(17) 0.46994(15) 0.0298(4) Uani 1 1 d . . . . . H4A H 0.1972 0.3255 0.4131 0.036 Uiso 1 1 calc R . . . . H4B H 0.3110 0.3719 0.5273 0.036 Uiso 1 1 calc R . . . . C5 C 0.3735(2) 0.24411(18) 0.43974(15) 0.0314(4) Uani 1 1 d . . . . . H5A H 0.3220 0.1780 0.3774 0.038 Uiso 1 1 calc R . . . . H5B H 0.4394 0.3052 0.4257 0.038 Uiso 1 1 calc R . . . . C6 C 0.46591(18) 0.19616(17) 0.52176(14) 0.0271(4) Uani 1 1 d . . . . . H6A H 0.5263 0.2634 0.5818 0.033 Uiso 1 1 calc R . . . . H6B H 0.5340 0.1560 0.4982 0.033 Uiso 1 1 calc R . . . . C7 C 0.36626(19) 0.10756(17) 0.54954(14) 0.0260(4) Uani 1 1 d . . . . . H7A H 0.4277 0.0806 0.6055 0.031 Uiso 1 1 calc R . . . . H7B H 0.3137 0.0365 0.4913 0.031 Uiso 1 1 calc R . . . . C8 C 0.25304(18) 0.16397(16) 0.58074(12) 0.0231(3) Uani 1 1 d . . . . . H8A H 0.1879 0.1031 0.5956 0.028 Uiso 1 1 calc R . . . . H8B H 0.3057 0.2300 0.6429 0.028 Uiso 1 1 calc R . . . . C9 C -0.10530(17) 0.29703(14) 0.42005(11) 0.0176(3) Uani 1 1 d . . . . . H9 H -0.0489 0.3429 0.3879 0.021 Uiso 1 1 calc R . . . . C10 C -0.21328(17) 0.36961(14) 0.44127(12) 0.0205(3) Uani 1 1 d . . . . . H10A H -0.2680 0.3293 0.4765 0.025 Uiso 1 1 calc R . . . . H10B H -0.1566 0.4501 0.4861 0.025 Uiso 1 1 calc R . . . . C11 C -0.32393(18) 0.38284(15) 0.34460(13) 0.0243(3) Uani 1 1 d . . . . . H11A H -0.3956 0.4253 0.3609 0.029 Uiso 1 1 calc R . . . . H11B H -0.2705 0.4314 0.3134 0.029 Uiso 1 1 calc R . . . . C12 C -0.40703(18) 0.26069(15) 0.27045(12) 0.0235(3) Uani 1 1 d . . . . . H12A H -0.4674 0.2148 0.2994 0.028 Uiso 1 1 calc R . . . . H12B H -0.4748 0.2717 0.2077 0.028 Uiso 1 1 calc R . . . . C13 C -0.30011(19) 0.19070(16) 0.24674(12) 0.0247(4) Uani 1 1 d . . . . . H13A H -0.2456 0.2332 0.2126 0.030 Uiso 1 1 calc R . . . . H13B H -0.3563 0.1108 0.2006 0.030 Uiso 1 1 calc R . . . . C14 C -0.18964(19) 0.17595(15) 0.34291(12) 0.0231(3) Uani 1 1 d . . . . . H14A H -0.1180 0.1340 0.3259 0.028 Uiso 1 1 calc R . . . . H14B H -0.2435 0.1258 0.3729 0.028 Uiso 1 1 calc R . . . . C15 C 0.05190(16) 0.17737(13) 0.87948(11) 0.0157(3) Uani 1 1 d . . . . . C16 C -0.05518(16) 0.16726(14) 0.92475(11) 0.0161(3) Uani 1 1 d . . . . . C17 C -0.02708(17) 0.25103(14) 1.01567(11) 0.0174(3) Uani 1 1 d . . . . . H17 H -0.0999 0.2463 1.0450 0.021 Uiso 1 1 calc R . . . . C18 C 0.10282(18) 0.34074(14) 1.06468(11) 0.0174(3) Uani 1 1 d . . . . . C19 C 0.21047(17) 0.34059(14) 1.02361(12) 0.0191(3) Uani 1 1 d . . . . . H19 H 0.3020 0.3986 1.0584 0.023 Uiso 1 1 calc R . . . . C20 C 0.19237(17) 0.26002(14) 0.93401(11) 0.0177(3) Uani 1 1 d . . . . . C21 C -0.19989(16) 0.06643(14) 0.88081(12) 0.0184(3) Uani 1 1 d . . . . . C22 C -0.31367(17) 0.08472(16) 0.78705(12) 0.0221(3) Uani 1 1 d . . . . . H22A H -0.3340 0.1636 0.8038 0.033 Uiso 1 1 calc R . . . . H22B H -0.2738 0.0797 0.7337 0.033 Uiso 1 1 calc R . . . . H22C H -0.4055 0.0224 0.7640 0.033 Uiso 1 1 calc R . . . . C23 C -0.16624(18) -0.05728(14) 0.85602(13) 0.0226(3) Uani 1 1 d . . . . . H23A H -0.0938 -0.0677 0.9162 0.034 Uiso 1 1 calc R . . . . H23B H -0.2576 -0.1200 0.8332 0.034 Uiso 1 1 calc R . . . . H23C H -0.1259 -0.0628 0.8029 0.034 Uiso 1 1 calc R . . . . C24 C -0.27559(19) 0.06149(17) 0.95739(13) 0.0258(4) Uani 1 1 d . . . . . H24A H -0.2066 0.0499 1.0185 0.039 Uiso 1 1 calc R . . . . H24B H -0.3044 0.1367 0.9740 0.039 Uiso 1 1 calc R . . . . H24C H -0.3638 -0.0053 0.9283 0.039 Uiso 1 1 calc R . . . . C25 C 0.1328(2) 0.43485(15) 1.16322(12) 0.0226(3) Uani 1 1 d . . . . . C26 C 0.0093(3) 0.4197(2) 1.20132(17) 0.0319(6) Uani 0.863(5) 1 d . . P A 1 H26A H 0.0351 0.4821 1.2639 0.048 Uiso 0.863(5) 1 calc R . P A 1 H26B H -0.0814 0.4264 1.1511 0.048 Uiso 0.863(5) 1 calc R . P A 1 H26C H -0.0067 0.3408 1.2139 0.048 Uiso 0.863(5) 1 calc R . P A 1 C26' C -0.0503(16) 0.4609(13) 1.1475(11) 0.032(4) Uani 0.137(5) 1 d . . P A 2 H26D H -0.1186 0.3857 1.1388 0.049 Uiso 0.137(5) 1 calc R . P A 2 H26E H -0.0439 0.5204 1.2072 0.049 Uiso 0.137(5) 1 calc R . P A 2 H26F H -0.0866 0.4905 1.0882 0.049 Uiso 0.137(5) 1 calc R . P A 2 C27 C 0.2762(3) 0.4252(2) 1.24566(15) 0.0301(6) Uani 0.863(5) 1 d . . P A 1 H27A H 0.3586 0.4349 1.2222 0.045 Uiso 0.863(5) 1 calc R . P A 1 H27B H 0.3002 0.4881 1.3076 0.045 Uiso 0.863(5) 1 calc R . P A 1 H27C H 0.2595 0.3466 1.2587 0.045 Uiso 0.863(5) 1 calc R . P A 1 C27' C 0.148(3) 0.3748(18) 1.2420(12) 0.058(7) Uani 0.137(5) 1 d . . P A 2 H27D H 0.0810 0.2948 1.2143 0.087 Uiso 0.137(5) 1 calc R . P A 2 H27E H 0.2504 0.3677 1.2699 0.087 Uiso 0.137(5) 1 calc R . P A 2 H27F H 0.1235 0.4214 1.2952 0.087 Uiso 0.137(5) 1 calc R . P A 2 C28 C 0.1650(4) 0.5614(4) 1.1484(3) 0.0264(7) Uani 0.863(5) 1 d . . P A 1 H28A H 0.2459 0.5704 1.1235 0.040 Uiso 0.863(5) 1 calc R . P A 1 H28B H 0.0760 0.5727 1.0997 0.040 Uiso 0.863(5) 1 calc R . P A 1 H28C H 0.1934 0.6215 1.2127 0.040 Uiso 0.863(5) 1 calc R . P A 1 C28' C 0.205(4) 0.542(2) 1.173(2) 0.040(6) Uani 0.137(5) 1 d . . P A 2 H28D H 0.1736 0.5608 1.1085 0.061 Uiso 0.137(5) 1 calc R . P A 2 H28E H 0.1844 0.5999 1.2223 0.061 Uiso 0.137(5) 1 calc R . P A 2 H28F H 0.3113 0.5462 1.1970 0.061 Uiso 0.137(5) 1 calc R . P A 2 C29 C 0.32812(17) 0.26853(15) 0.90215(12) 0.0210(3) Uani 1 1 d . . . . . C30 C 0.47356(19) 0.31408(19) 0.99470(14) 0.0341(5) Uani 1 1 d . . . . . H30A H 0.4784 0.2589 1.0371 0.051 Uiso 1 1 calc R . . . . H30B H 0.5577 0.3184 0.9728 0.051 Uiso 1 1 calc R . . . . H30C H 0.4772 0.3939 1.0330 0.051 Uiso 1 1 calc R . . . . C31 C 0.3254(2) 0.35764(16) 0.83792(14) 0.0276(4) Uani 1 1 d . . . . . H31A H 0.2338 0.3309 0.7783 0.041 Uiso 1 1 calc R . . . . H31B H 0.3301 0.4371 0.8774 0.041 Uiso 1 1 calc R . . . . H31C H 0.4106 0.3617 0.8172 0.041 Uiso 1 1 calc R . . . . C32 C 0.33999(18) 0.14659(16) 0.84683(13) 0.0238(3) Uani 1 1 d . . . . . H32A H 0.3415 0.0912 0.8888 0.036 Uiso 1 1 calc R . . . . H32B H 0.2547 0.1139 0.7834 0.036 Uiso 1 1 calc R . . . . H32C H 0.4313 0.1571 0.8331 0.036 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 P1 0.01540(18) 0.01686(19) 0.01654(18) 0.00384(15) 0.00695(15) 0.00316(14) P2 0.01873(19) 0.01560(19) 0.01610(18) 0.00228(14) 0.00655(15) 0.00323(15) C1 0.0159(7) 0.0207(8) 0.0187(7) 0.0059(6) 0.0077(6) 0.0033(6) C2 0.0165(7) 0.0189(7) 0.0186(7) 0.0042(6) 0.0092(6) 0.0035(6) C3 0.0172(7) 0.0189(7) 0.0187(7) 0.0041(6) 0.0081(6) 0.0050(6) C4 0.0307(9) 0.0319(10) 0.0442(11) 0.0215(8) 0.0257(8) 0.0158(8) C5 0.0294(9) 0.0392(11) 0.0411(10) 0.0197(9) 0.0242(8) 0.0159(8) C6 0.0168(8) 0.0295(9) 0.0350(9) 0.0062(8) 0.0114(7) 0.0052(7) C7 0.0215(8) 0.0292(9) 0.0321(9) 0.0125(7) 0.0112(7) 0.0115(7) C8 0.0207(8) 0.0289(9) 0.0233(8) 0.0094(7) 0.0098(6) 0.0093(7) C9 0.0160(7) 0.0197(8) 0.0174(7) 0.0048(6) 0.0069(6) 0.0038(6) C10 0.0193(7) 0.0185(8) 0.0221(8) 0.0035(6) 0.0067(6) 0.0050(6) C11 0.0210(8) 0.0209(8) 0.0272(8) 0.0075(7) 0.0032(7) 0.0058(6) C12 0.0200(8) 0.0254(9) 0.0213(8) 0.0061(7) 0.0038(6) 0.0035(6) C13 0.0226(8) 0.0292(9) 0.0188(8) 0.0025(7) 0.0062(6) 0.0049(7) C14 0.0233(8) 0.0227(8) 0.0207(8) 0.0016(6) 0.0063(6) 0.0079(6) C15 0.0182(7) 0.0131(7) 0.0168(7) 0.0043(6) 0.0069(6) 0.0050(6) C16 0.0160(7) 0.0163(7) 0.0189(7) 0.0092(6) 0.0062(6) 0.0067(5) C17 0.0207(7) 0.0185(7) 0.0190(7) 0.0092(6) 0.0105(6) 0.0092(6) C18 0.0236(8) 0.0149(7) 0.0165(7) 0.0068(6) 0.0084(6) 0.0072(6) C19 0.0209(7) 0.0150(7) 0.0190(7) 0.0029(6) 0.0067(6) 0.0012(6) C20 0.0183(7) 0.0164(7) 0.0182(7) 0.0049(6) 0.0068(6) 0.0034(6) C21 0.0150(7) 0.0212(8) 0.0197(7) 0.0087(6) 0.0054(6) 0.0042(6) C22 0.0161(7) 0.0285(9) 0.0237(8) 0.0109(7) 0.0070(6) 0.0066(6) C23 0.0190(7) 0.0178(8) 0.0277(8) 0.0079(7) 0.0047(6) 0.0018(6) C24 0.0206(8) 0.0326(10) 0.0251(8) 0.0106(7) 0.0100(7) 0.0019(7) C25 0.0349(9) 0.0172(8) 0.0187(8) 0.0045(6) 0.0131(7) 0.0082(7) C26 0.0375(13) 0.0297(12) 0.0294(11) -0.0009(9) 0.0214(10) 0.0025(10) C26' 0.036(7) 0.024(7) 0.032(8) -0.012(6) 0.016(6) 0.010(6) C27 0.0391(13) 0.0304(12) 0.0175(9) 0.0045(8) 0.0044(9) 0.0152(10) C27' 0.106(19) 0.058(12) 0.026(8) 0.017(8) 0.024(9) 0.058(13) C28 0.0430(17) 0.0141(14) 0.0255(15) 0.0061(10) 0.0156(12) 0.0092(11) C28' 0.078(19) 0.025(11) 0.037(14) 0.007(9) 0.043(13) 0.020(10) C29 0.0171(7) 0.0215(8) 0.0210(7) -0.0001(6) 0.0083(6) 0.0001(6) C30 0.0190(8) 0.0466(12) 0.0272(9) -0.0042(8) 0.0078(7) 0.0018(8) C31 0.0267(8) 0.0250(9) 0.0315(9) 0.0047(7) 0.0167(7) -0.0014(7) C32 0.0190(7) 0.0263(9) 0.0258(8) 0.0031(7) 0.0096(7) 0.0067(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' P P 0.1023 0.0942 '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 C3 P1 C1 102.90(7) . . C3 P1 C9 101.96(7) . . C9 P1 C1 100.83(7) . . C2 P2 C15 101.59(7) . . C2 C1 P1 112.22(11) . . C1 C2 P2 123.87(12) . . C4 C3 P1 108.24(11) . . C8 C3 P1 112.26(11) . . C8 C3 C4 109.61(13) . . C5 C4 C3 112.43(15) . . C6 C5 C4 111.60(16) . . C5 C6 C7 110.36(14) . . C6 C7 C8 111.36(15) . . C3 C8 C7 112.25(14) . . C10 C9 P1 109.09(10) . . C10 C9 C14 110.74(13) . . C14 C9 P1 116.83(12) . . C11 C10 C9 111.89(13) . . C12 C11 C10 110.98(14) . . C13 C12 C11 110.97(14) . . C12 C13 C14 110.86(14) . . C13 C14 C9 111.88(14) . . C16 C15 P2 120.03(11) . . C16 C15 C20 119.37(13) . . C20 C15 P2 120.40(11) . . C15 C16 C21 123.75(13) . . C17 C16 C15 118.32(14) . . C17 C16 C21 117.91(13) . . C18 C17 C16 122.75(14) . . C17 C18 C25 123.03(14) . . C19 C18 C17 117.26(14) . . C19 C18 C25 119.67(14) . . C18 C19 C20 123.67(14) . . C15 C20 C29 125.55(13) . . C19 C20 C15 117.83(14) . . C19 C20 C29 116.62(13) . . C22 C21 C16 111.82(13) . . C22 C21 C23 110.32(13) . . C22 C21 C24 106.83(13) . . C23 C21 C16 110.62(12) . . C23 C21 C24 105.29(14) . . C24 C21 C16 111.70(13) . . C18 C25 C26' 102.6(4) . . C18 C25 C27 108.65(14) . . C18 C25 C28 109.38(19) . . C26 C25 C18 113.52(15) . . C26 C25 C27 108.13(17) . . C26 C25 C28 110.1(2) . . C27' C25 C18 108.3(7) . . C27' C25 C26' 98.1(10) . . C28 C25 C27 106.80(19) . . C28' C25 C18 116.3(11) . . C28' C25 C26' 100.1(13) . . C28' C25 C27' 126.1(15) . . C30 C29 C20 110.89(13) . . C30 C29 C32 104.06(14) . . C31 C29 C20 109.91(14) . . C31 C29 C30 107.62(15) . . C31 C29 C32 110.70(14) . . C32 C29 C20 113.40(13) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 P1 C1 1.8687(16) . P1 C3 1.8634(16) . P1 C9 1.8652(16) . P2 C2 1.6648(17) . P2 C15 1.8575(15) . C1 C2 1.502(2) . C3 C4 1.535(2) . C3 C8 1.526(2) . C4 C5 1.531(2) . C5 C6 1.519(3) . C6 C7 1.524(2) . C7 C8 1.530(2) . C9 C10 1.535(2) . C9 C14 1.535(2) . C10 C11 1.532(2) . C11 C12 1.526(2) . C12 C13 1.519(2) . C13 C14 1.533(2) . C15 C16 1.421(2) . C15 C20 1.427(2) . C16 C17 1.402(2) . C16 C21 1.552(2) . C17 C18 1.390(2) . C18 C19 1.381(2) . C18 C25 1.539(2) . C19 C20 1.394(2) . C20 C29 1.551(2) . C21 C22 1.541(2) . C21 C23 1.541(2) . C21 C24 1.543(2) . C25 C26 1.498(3) . C25 C26' 1.827(14) . C25 C27 1.567(3) . C25 C27' 1.449(17) . C25 C28 1.544(4) . C25 C28' 1.30(3) . C29 C30 1.540(2) . C29 C31 1.540(3) . C29 C32 1.540(2) . loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.7815(9) 2 0.2185(9)