#------------------------------------------------------------------------------ #$Date: 2020-04-05 13:25:28 +0300 (Sun, 05 Apr 2020) $ #$Revision: 250213 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/73/1557331.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_1557331 loop_ _publ_author_name 'Payne, Daniel T.' 'Webre, Whitney A.' 'Gobeze, Habtom B.' 'Seetharaman, Sairaman' 'Matsushita, Yoshitaka' 'Karr, Paul A.' 'Chahal, Mandeep K.' 'Labuta, Jan' 'Jevasuwan, Wipakorn' 'Fukata, Naoki' 'Fossey, John S.' 'Ariga, Katsuhiko' 'D'Souza, Francis' 'Hill, Jonathan P.' _publ_section_title ; Nanomolecular singlet oxygen photosensitizers based on hemiquinonoid-resorcinarenes, the fuchsonarenes. ; _journal_issue 10 _journal_name_full 'Chemical science' _journal_page_first 2614 _journal_page_last 2620 _journal_paper_doi 10.1039/d0sc00651c _journal_volume 11 _journal_year 2020 _chemical_formula_sum 'C203.82 H244.63 Cl7.63 N0 O40' _chemical_formula_weight 3604.93 _chemical_name_common rctt-2 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2013 _audit_update_record ; 2019-06-18 deposited with the CCDC. 2020-02-12 downloaded from the CCDC. ; _cell_angle_alpha 84.7250(10) _cell_angle_beta 81.7580(10) _cell_angle_gamma 89.9360(10) _cell_formula_units_Z 1 _cell_length_a 11.5721(4) _cell_length_b 16.6408(5) _cell_length_c 26.1539(8) _cell_measurement_reflns_used 9986 _cell_measurement_temperature 160(2) _cell_measurement_theta_max 30.84 _cell_measurement_theta_min 2.34 _cell_volume 4962.9(3) _computing_cell_refinement 'CrystalClear (Rigaku, 1997--2002)' _computing_data_collection 'CrystalClear (Rigaku, 1997--2002)' _computing_data_reduction 'CrystalClear (Rigaku, 1997--2002)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _diffrn_ambient_temperature 160(2) _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.856 _diffrn_measurement_device ; Rigaku AFC11 Saturn724+ (4x4 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_radiation_detector CCD _diffrn_radiation_monochromator Confocal _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_unetI/netI 0.0422 _diffrn_reflns_Laue_measured_fraction_full 0.982 _diffrn_reflns_Laue_measured_fraction_max 0.856 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 47447 _diffrn_reflns_point_group_measured_fraction_full 0.982 _diffrn_reflns_point_group_measured_fraction_max 0.856 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.953 _diffrn_reflns_theta_min 0.790 _exptl_absorpt_coefficient_mu 0.181 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.6688 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrystalClear (Rigaku, 1997--2002) ; _exptl_crystal_colour 'Pale yellow' _exptl_crystal_density_diffrn 1.206 _exptl_crystal_description Chunk _exptl_crystal_F_000 1917 _exptl_crystal_size_max 0.176 _exptl_crystal_size_mid 0.171 _exptl_crystal_size_min 0.115 _refine_diff_density_max 1.478 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.082 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 1176 _refine_ls_number_reflns 26976 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.037 _refine_ls_R_factor_all 0.0916 _refine_ls_R_factor_gt 0.0698 _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^)+(0.1121P)^2^+2.5516P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1901 _refine_ls_wR_factor_ref 0.2105 _reflns_Friedel_coverage 0.000 _reflns_number_gt 19900 _reflns_number_total 26976 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc00651c2.cif _cod_data_source_block shelx _cod_depositor_comments 'Adding full bibliography for 1557331--1557337.cif.' _cod_database_code 1557331 _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_min 0.969 _shelx_estimated_absorpt_t_max 0.980 _shelxl_version_number 2013-4 _shelx_res_file ; TITL resc_ac8@160k1_0m in P-1 CELL 0.71073 11.5721 16.6408 26.1539 84.725 81.758 89.936 ZERR 1 0.0004 0.0005 0.0008 0.001 0.001 0.001 LATT 1 SFAC C H N O Cl UNIT 203.82 244.63 0 40 7.63 acta temp -113 size 0.171 0.176 0.115 omit 1 0 0 omit 0 1 1 omit 0 -1 1 omit 0 0 2 omit 1 0 1 omit 1 0 2 omit 1 1 8 omit 0 3 3 omit 1 2 6 omit 0 5 4 omit 1 2 3 omit -1 -1 7 L.S. 100 BOND FMAP 2 PLAN 5 twin rem EXTI 0.000000 WGHT 0.112100 2.551600 BASF 0.49352 FVAR 0.07021 0.88874 MOLE 1 C01 1 0.611503 0.346846 0.251785 21.00000 0.15355 0.08634 = 0.19612 0.04638 -0.11291 -0.07532 AFIX 23 H01A 2 0.628923 0.400954 0.233167 21.00000 -1.20000 H01B 2 0.662276 0.339453 0.279230 21.00000 -1.20000 AFIX 0 CL1 5 0.642006 0.283416 0.213754 21.00000 0.07693 0.15526 = 0.20727 -0.06766 -0.04033 -0.00956 CL2 5 0.447950 0.343452 0.284698 21.00000 0.18773 0.16613 = 0.07561 -0.04663 -0.02415 0.01198 MOLE 2 C02 1 0.382292 0.884323 0.213618 11.00000 0.05130 0.05092 = 0.03624 -0.00543 -0.00895 0.01089 AFIX 23 H02A 2 0.307562 0.863019 0.205798 11.00000 -1.20000 H02B 2 0.409934 0.927886 0.186236 11.00000 -1.20000 AFIX 0 CL3 5 0.484538 0.807136 0.211819 11.00000 0.10047 0.08017 = 0.07518 0.00363 -0.01470 0.05138 CL4 5 0.357498 0.924960 0.273491 11.00000 0.06541 0.10577 = 0.03748 -0.01902 -0.00612 0.00779 MOLE 3 O1 4 0.634982 0.457456 0.666827 11.00000 0.10869 0.24113 = 0.09884 0.10175 0.05844 0.09523 O2 4 0.923147 0.557102 0.717878 11.00000 0.04197 0.05327 = 0.02403 -0.01186 -0.00714 0.01845 O3 4 1.068139 0.637032 0.734643 11.00000 0.07054 0.08055 = 0.06804 -0.04627 -0.01425 0.00714 O4 4 0.972594 0.910406 0.608326 11.00000 0.05949 0.02559 = 0.08431 -0.01927 -0.01939 0.00025 H4O 2 0.925625 0.909594 0.632145 11.00000 -1.20000 O5 4 0.833079 0.936946 0.405355 11.00000 0.05949 0.01767 = 0.06433 0.00404 -0.00396 0.00263 H5O 2 0.898398 0.946521 0.409674 11.00000 -1.20000 O6 4 0.746817 0.614070 0.324448 11.00000 0.03306 0.03063 = 0.02649 0.00099 -0.01093 0.00738 O7 4 0.653621 0.512584 0.296447 11.00000 0.05167 0.04809 = 0.11512 -0.01628 -0.03709 0.00004 O8 4 0.664669 0.447748 0.455672 11.00000 0.02688 0.02673 = 0.02534 -0.00356 -0.00592 -0.00660 O9 4 0.504751 0.401696 0.510322 11.00000 0.02943 0.05707 = 0.04135 0.00442 -0.00350 -0.00970 O10 4 0.793997 0.413006 0.622868 11.00000 0.03598 0.03007 = 0.02845 0.01051 -0.00922 -0.00234 O11 4 0.279914 1.054901 0.165706 11.00000 0.03090 0.03366 = 0.02524 -0.00166 -0.00999 -0.01050 O12 4 0.178666 1.137927 0.217529 11.00000 0.06792 0.06580 = 0.11282 -0.05953 -0.00995 -0.00260 O13 4 0.184871 1.407950 0.088960 11.00000 0.04879 0.01871 = 0.05481 -0.01050 -0.00981 0.00021 O14 4 0.022507 1.444221 -0.108926 11.00000 0.03913 0.01654 = 0.06691 -0.00260 -0.01158 0.00126 O15 4 -0.092846 1.198967 -0.235624 11.00000 0.05081 0.04176 = 0.04936 0.01729 -0.01114 0.00180 H15O 2 0.123842 1.419089 0.088707 11.00000 -1.20000 O16 4 0.057388 1.117132 -0.221676 11.00000 0.03205 0.03498 = 0.02050 0.00747 -0.00455 -0.00864 H16O 2 0.075039 1.467027 -0.110689 11.00000 -1.20000 O17 4 0.215302 0.959202 -0.134172 11.00000 0.03634 0.02820 = 0.02432 -0.01032 -0.00904 0.00658 O18 4 0.396872 1.000913 -0.164641 11.00000 0.06873 0.12455 = 0.05213 -0.03286 0.02874 -0.03800 O19 4 0.329157 0.930138 0.036533 11.00000 0.02202 0.02182 = 0.02294 0.00201 -0.00254 0.00543 O20 4 0.494686 0.914210 -0.018287 11.00000 0.02521 0.05172 = 0.03347 -0.00551 -0.00057 0.00864 C1 1 0.588381 0.648755 0.281801 11.00000 0.05787 0.06472 = 0.10490 -0.01280 -0.04986 0.02334 AFIX 137 H1A 2 0.525659 0.625722 0.265995 11.00000 -1.50000 H1B 2 0.636290 0.685660 0.255885 11.00000 -1.50000 H1C 2 0.554403 0.678396 0.310913 11.00000 -1.50000 AFIX 0 C2 1 0.662725 0.582455 0.301013 11.00000 0.03240 0.04238 = 0.04987 -0.00290 -0.01429 0.00350 C3 1 0.835136 0.563729 0.339420 11.00000 0.02896 0.02384 = 0.02371 0.00158 -0.00775 0.00341 C4 1 0.908682 0.527090 0.302325 11.00000 0.03696 0.03623 = 0.01944 -0.00097 -0.00840 0.00722 AFIX 43 H4 2 0.896882 0.532765 0.266974 11.00000 -1.20000 AFIX 0 C5 1 0.850048 0.557238 0.391517 11.00000 0.02497 0.01786 = 0.02090 0.00054 -0.00418 -0.00152 C6 1 0.764402 0.597545 0.431086 11.00000 0.02181 0.01975 = 0.01986 -0.00014 -0.00457 0.00049 AFIX 13 H6 2 0.684589 0.588830 0.422005 11.00000 -1.20000 AFIX 0 C7 1 0.766255 0.554204 0.484951 11.00000 0.02046 0.01838 = 0.02087 -0.00060 -0.00341 0.00084 C8 1 0.819048 0.585086 0.523796 11.00000 0.02241 0.01732 = 0.02192 -0.00019 -0.00314 -0.00015 AFIX 43 H8 2 0.852183 0.637902 0.517588 11.00000 -1.20000 AFIX 0 C9 1 0.825001 0.541337 0.571391 11.00000 0.02266 0.02074 = 0.02105 -0.00157 -0.00409 0.00236 C10 1 0.778986 0.463081 0.578005 11.00000 0.02509 0.02173 = 0.02322 0.00410 -0.00426 -0.00029 C11 1 0.714749 0.410706 0.664104 11.00000 0.05805 0.12807 = 0.05484 0.05111 0.01319 0.03103 C12 1 0.745657 0.351009 0.706273 11.00000 0.07271 0.13212 = 0.05134 0.05497 0.00029 0.01801 AFIX 137 H12A 2 0.830758 0.348909 0.704515 11.00000 -1.50000 H12B 2 0.715329 0.297523 0.701818 11.00000 -1.50000 H12C 2 0.711113 0.367521 0.740085 11.00000 -1.50000 AFIX 0 C13 1 0.725034 0.429912 0.540967 11.00000 0.02629 0.01878 = 0.02859 0.00282 -0.00540 -0.00402 AFIX 43 H13 2 0.694294 0.376411 0.546694 11.00000 -1.20000 AFIX 0 C14 1 0.717185 0.477077 0.495265 11.00000 0.02274 0.02137 = 0.02201 -0.00205 -0.00418 -0.00145 C15 1 0.553473 0.416397 0.467102 11.00000 0.02556 0.02491 = 0.03761 -0.00334 -0.00760 -0.00233 C16 1 0.504942 0.404913 0.418203 11.00000 0.03528 0.04900 = 0.04500 -0.01292 -0.01512 -0.00638 AFIX 137 H16A 2 0.448627 0.359905 0.424548 11.00000 -1.50000 H16B 2 0.568595 0.393000 0.391093 11.00000 -1.50000 H16C 2 0.465815 0.454311 0.406940 11.00000 -1.50000 AFIX 0 C17 1 0.875842 0.574375 0.615883 11.00000 0.02718 0.02311 = 0.02129 -0.00393 -0.00640 0.00348 AFIX 13 H17 2 0.812977 0.566990 0.646482 11.00000 -1.20000 AFIX 0 C18 1 0.977687 0.524308 0.631091 11.00000 0.02733 0.02241 = 0.02133 -0.00196 -0.00613 0.00239 C19 1 1.000327 0.517938 0.682075 11.00000 0.03360 0.03324 = 0.01963 -0.00447 -0.00463 0.00679 C20 1 0.966323 0.621434 0.738689 11.00000 0.06413 0.06157 = 0.03392 -0.02296 -0.01579 0.02409 C22 1 0.905441 0.664294 0.608951 11.00000 0.03361 0.02308 = 0.02507 -0.00695 -0.00906 0.00419 C21 1 0.867669 0.666939 0.765620 11.00000 0.08706 0.09194 = 0.06025 -0.04522 -0.01720 0.04603 AFIX 137 H21A 2 0.821277 0.691804 0.739991 11.00000 -1.50000 H21B 2 0.898993 0.709068 0.783806 11.00000 -1.50000 H21C 2 0.818118 0.629752 0.790703 11.00000 -1.50000 AFIX 0 C23 1 1.016888 0.692938 0.609903 11.00000 0.03751 0.02610 = 0.04738 -0.00797 -0.01652 0.00250 AFIX 43 H23 2 1.078749 0.655424 0.610395 11.00000 -1.20000 AFIX 0 C24 1 1.042396 0.775092 0.610173 11.00000 0.04349 0.02828 = 0.06354 -0.01146 -0.02453 -0.00120 C25 1 0.949841 0.828547 0.607974 11.00000 0.05123 0.02332 = 0.05251 -0.01315 -0.01655 0.00089 C26 1 0.835053 0.802501 0.604619 11.00000 0.04204 0.02534 = 0.03587 -0.01045 -0.00770 0.00667 C27 1 0.816071 0.719850 0.606191 11.00000 0.03264 0.02569 = 0.02961 -0.00801 -0.00673 0.00486 AFIX 43 H27 2 0.739211 0.700528 0.605352 11.00000 -1.20000 AFIX 0 C28 1 1.166042 0.803225 0.616105 11.00000 0.05286 0.04024 = 0.10555 -0.01488 -0.03935 -0.00653 C29 1 1.217740 0.861362 0.569772 11.00000 0.05052 0.04624 = 0.13133 -0.01154 -0.01825 -0.01327 AFIX 137 H29A 2 1.294809 0.880241 0.575265 11.00000 -1.50000 H29B 2 1.166081 0.907640 0.566291 11.00000 -1.50000 H29C 2 1.225448 0.833447 0.538076 11.00000 -1.50000 AFIX 0 C30 1 1.163126 0.843656 0.667725 11.00000 0.09012 0.07337 = 0.12169 -0.03710 -0.05853 -0.01014 AFIX 137 H30A 2 1.242171 0.861243 0.671236 11.00000 -1.50000 H30B 2 1.133697 0.804684 0.697092 11.00000 -1.50000 H30C 2 1.111677 0.890457 0.667297 11.00000 -1.50000 AFIX 0 C31 1 1.247908 0.731566 0.620059 11.00000 0.04652 0.05368 = 0.15338 -0.01868 -0.04894 -0.00139 AFIX 137 H31A 2 1.323845 0.750333 0.627054 11.00000 -1.50000 H31B 2 1.258169 0.706354 0.587314 11.00000 -1.50000 H31C 2 1.214235 0.692035 0.648348 11.00000 -1.50000 AFIX 0 C32 1 0.785147 0.688123 0.426503 11.00000 0.02740 0.01914 = 0.01963 0.00171 -0.00208 0.00139 C33 1 0.692218 0.739566 0.420388 11.00000 0.02908 0.02535 = 0.02722 0.00129 -0.00403 0.00358 AFIX 43 H33 2 0.616529 0.716932 0.421325 11.00000 -1.20000 AFIX 0 C35 1 0.819616 0.853747 0.412904 11.00000 0.04309 0.01815 = 0.03491 0.00264 0.00025 0.00190 C34 1 0.706482 0.823209 0.412931 11.00000 0.03689 0.02331 = 0.03467 0.00109 -0.00477 0.00791 C36 1 0.915788 0.804194 0.419967 11.00000 0.03290 0.01981 = 0.03529 0.00034 0.00308 -0.00325 C38 1 1.039220 0.838130 0.420950 11.00000 0.03636 0.02457 = 0.05920 -0.00647 0.00557 -0.00821 C37 1 0.894798 0.720831 0.425735 11.00000 0.02758 0.01955 = 0.02930 0.00034 -0.00114 0.00110 AFIX 43 H37 2 0.958355 0.685552 0.429245 11.00000 -1.20000 AFIX 0 C39 1 1.125503 0.770468 0.431551 11.00000 0.03005 0.03696 = 0.10585 -0.01755 -0.00657 -0.00563 AFIX 137 H39A 2 1.201896 0.794161 0.433804 11.00000 -1.50000 H39B 2 1.133154 0.735229 0.403252 11.00000 -1.50000 H39C 2 1.096490 0.738862 0.464358 11.00000 -1.50000 AFIX 0 C40 1 1.037880 0.892387 0.465423 11.00000 0.04701 0.03483 = 0.06804 -0.01065 -0.00349 -0.01055 AFIX 137 H40A 2 1.117764 0.910003 0.467412 11.00000 -1.50000 H40B 2 1.005343 0.862109 0.498237 11.00000 -1.50000 H40C 2 0.989677 0.939689 0.459015 11.00000 -1.50000 AFIX 0 C41 1 1.086826 0.884158 0.368230 11.00000 0.05835 0.04594 = 0.06857 -0.01161 0.02405 -0.01999 AFIX 137 H41A 2 1.161582 0.910092 0.370669 11.00000 -1.50000 H41B 2 1.030872 0.925380 0.359075 11.00000 -1.50000 H41C 2 1.098262 0.846240 0.341458 11.00000 -1.50000 AFIX 0 C42 1 0.602556 0.878014 0.403395 11.00000 0.04886 0.03079 = 0.05348 -0.00053 -0.01367 0.01675 C43 1 0.578186 0.936309 0.446604 11.00000 0.05892 0.04406 = 0.07352 -0.01234 -0.00838 0.02725 AFIX 137 H43A 2 0.515286 0.972989 0.438979 11.00000 -1.50000 H43B 2 0.649071 0.967709 0.448011 11.00000 -1.50000 H43C 2 0.554808 0.905049 0.480114 11.00000 -1.50000 AFIX 0 C44 1 0.628900 0.926109 0.349800 11.00000 0.07740 0.05079 = 0.06288 0.01445 -0.02144 0.02454 AFIX 137 H44A 2 0.563139 0.961388 0.344196 11.00000 -1.50000 H44B 2 0.640558 0.888623 0.322775 11.00000 -1.50000 H44C 2 0.699772 0.958931 0.348311 11.00000 -1.50000 AFIX 0 C45 1 0.490752 0.829161 0.403986 11.00000 0.04278 0.04682 = 0.08406 -0.00434 -0.02150 0.01879 AFIX 137 H45A 2 0.426962 0.865835 0.397641 11.00000 -1.50000 H45B 2 0.470791 0.798338 0.437885 11.00000 -1.50000 H45C 2 0.502714 0.791940 0.376813 11.00000 -1.50000 AFIX 0 C46 1 0.280707 0.940077 -0.220828 11.00000 0.09892 0.08259 = 0.03091 -0.02278 -0.00872 0.01615 AFIX 137 H46A 2 0.351293 0.942875 -0.246608 11.00000 -1.50000 H46B 2 0.220137 0.973762 -0.234162 11.00000 -1.50000 H46C 2 0.252642 0.884044 -0.213928 11.00000 -1.50000 AFIX 0 C47 1 0.308263 0.969923 -0.171646 11.00000 0.05726 0.04745 = 0.02786 -0.00938 0.00253 0.00467 C48 1 0.223104 0.990322 -0.086616 11.00000 0.02211 0.02012 = 0.02047 -0.00508 -0.00338 0.00081 C49 1 0.273997 0.943641 -0.049787 11.00000 0.02252 0.01690 = 0.02519 -0.00365 -0.00277 0.00341 AFIX 43 H49 2 0.305266 0.892271 -0.056620 11.00000 -1.20000 AFIX 0 C50 1 0.278051 0.973998 -0.002608 11.00000 0.01842 0.01768 = 0.02124 0.00035 -0.00208 0.00269 C51 1 0.229749 1.048101 0.009293 11.00000 0.01675 0.01689 = 0.01954 -0.00153 -0.00139 0.00019 C52 1 0.177688 1.092395 -0.029122 11.00000 0.01879 0.01553 = 0.02144 -0.00147 -0.00200 0.00012 AFIX 43 H52 2 0.143491 1.142760 -0.021824 11.00000 -1.20000 AFIX 0 C53 1 0.174098 1.065318 -0.077860 11.00000 0.01784 0.01599 = 0.01994 0.00020 -0.00240 -0.00066 C54 1 0.443533 0.908500 0.024728 11.00000 0.02271 0.02266 = 0.03143 -0.00306 -0.00516 0.00390 C55 1 0.492550 0.879405 0.072657 11.00000 0.02898 0.03945 = 0.04189 0.00899 -0.01076 0.00325 AFIX 137 H55A 2 0.562530 0.847630 0.063395 11.00000 -1.50000 H55B 2 0.434215 0.845667 0.095880 11.00000 -1.50000 H55C 2 0.513152 0.925775 0.090225 11.00000 -1.50000 AFIX 0 C56 1 0.118997 1.110622 -0.121382 11.00000 0.02076 0.01600 = 0.01968 -0.00007 -0.00355 0.00040 AFIX 13 H56 2 0.178568 1.111121 -0.153146 11.00000 -1.20000 AFIX 0 C57 1 0.014313 1.064279 -0.133008 11.00000 0.02105 0.01617 = 0.02010 -0.00163 -0.00389 0.00133 C58 1 -0.014744 1.069276 -0.182836 11.00000 0.02767 0.02144 = 0.01866 0.00206 -0.00266 -0.00249 C59 1 0.008699 1.183416 -0.244352 11.00000 0.04796 0.03468 = 0.02881 0.00941 -0.01336 -0.01008 C60 1 0.100172 1.232498 -0.280021 11.00000 0.06378 0.06260 = 0.04910 0.03130 -0.00835 -0.02209 AFIX 137 H60A 2 0.062887 1.275734 -0.299580 11.00000 -1.50000 H60B 2 0.143552 1.197813 -0.304198 11.00000 -1.50000 H60C 2 0.154020 1.256110 -0.259660 11.00000 -1.50000 AFIX 0 C61 1 0.090846 1.199358 -0.114284 11.00000 0.02634 0.01642 = 0.02031 0.00098 -0.00356 0.00026 C62 1 -0.021441 1.228541 -0.112588 11.00000 0.02608 0.01998 = 0.03334 -0.00222 -0.00774 0.00134 AFIX 43 H62 2 -0.083961 1.191356 -0.111982 11.00000 -1.20000 AFIX 0 C63 1 -0.046536 1.310708 -0.111730 11.00000 0.02932 0.02112 = 0.03884 -0.00275 -0.01048 0.00451 C64 1 0.047268 1.363117 -0.110559 11.00000 0.03454 0.01661 = 0.03584 -0.00006 -0.00687 0.00191 C65 1 0.163435 1.336305 -0.111449 11.00000 0.03035 0.01832 = 0.03009 0.00082 -0.00373 -0.00197 C66 1 0.181925 1.253693 -0.113804 11.00000 0.02607 0.01906 = 0.02533 0.00034 -0.00379 -0.00072 AFIX 43 H66 2 0.259248 1.233936 -0.115123 11.00000 -1.20000 AFIX 0 C67 1 -0.171719 1.341316 -0.114277 11.00000 0.03443 0.02675 = 0.06053 -0.00878 -0.01744 0.01004 C68 1 -0.255173 1.271796 -0.118691 11.00000 0.03154 0.04234 = 0.10822 -0.02278 -0.02769 0.00958 AFIX 137 H68A 2 -0.333824 1.292873 -0.120253 11.00000 -1.50000 H68B 2 -0.256807 1.232343 -0.088366 11.00000 -1.50000 H68C 2 -0.228313 1.245664 -0.150280 11.00000 -1.50000 AFIX 0 C69 1 -0.172082 1.400955 -0.162967 11.00000 0.05935 0.05319 = 0.06547 -0.00405 -0.03247 0.02244 AFIX 137 H69A 2 -0.252526 1.416592 -0.166294 11.00000 -1.50000 H69B 2 -0.138136 1.375124 -0.193764 11.00000 -1.50000 H69C 2 -0.125813 1.449067 -0.159802 11.00000 -1.50000 AFIX 0 C70 1 -0.219903 1.381724 -0.065234 11.00000 0.03653 0.03876 = 0.06767 -0.01180 -0.00937 0.01168 AFIX 137 H70A 2 -0.297864 1.402753 -0.068587 11.00000 -1.50000 H70B 2 -0.167768 1.426206 -0.060928 11.00000 -1.50000 H70C 2 -0.224810 1.341983 -0.034907 11.00000 -1.50000 AFIX 0 C71 1 0.266033 1.394492 -0.109791 11.00000 0.03393 0.01941 = 0.04896 -0.00304 -0.00040 -0.00640 C72 1 0.281232 1.456508 -0.157857 11.00000 0.05871 0.03335 = 0.06693 0.01039 0.00821 -0.01167 AFIX 137 H72A 2 0.347954 1.492124 -0.156600 11.00000 -1.50000 H72B 2 0.210327 1.488694 -0.158188 11.00000 -1.50000 H72C 2 0.295079 1.428143 -0.189351 11.00000 -1.50000 AFIX 0 C73 1 0.246284 1.437454 -0.059387 11.00000 0.04238 0.03437 = 0.06720 -0.01915 -0.01089 -0.00414 AFIX 137 H73A 2 0.312226 1.474028 -0.058662 11.00000 -1.50000 H73B 2 0.240069 1.397148 -0.029318 11.00000 -1.50000 H73C 2 0.174030 1.468433 -0.058214 11.00000 -1.50000 AFIX 0 C74 1 0.381919 1.349932 -0.109284 11.00000 0.03010 0.03117 = 0.08123 -0.01428 -0.00338 -0.00605 AFIX 137 H74A 2 0.444092 1.388553 -0.106519 11.00000 -1.50000 H74B 2 0.400888 1.323766 -0.141466 11.00000 -1.50000 H74C 2 0.374870 1.308987 -0.079544 11.00000 -1.50000 AFIX 0 C75 1 0.237123 1.074462 0.062942 11.00000 0.01881 0.01633 = 0.01950 -0.00204 -0.00341 0.00058 AFIX 13 H75 2 0.318183 1.062066 0.070080 11.00000 -1.20000 AFIX 0 C76 1 0.155388 1.024221 0.104743 11.00000 0.02060 0.01530 = 0.01864 -0.00095 -0.00293 0.00203 C77 1 0.057911 0.982945 0.094643 11.00000 0.02083 0.01772 = 0.01689 -0.00122 -0.00371 0.00142 AFIX 43 H77 2 0.039884 0.987139 0.060193 11.00000 -1.20000 AFIX 0 C78 1 0.177913 1.017904 0.155821 11.00000 0.02410 0.02152 = 0.02326 -0.00214 -0.00701 -0.00219 C79 1 0.108957 0.972285 0.195134 11.00000 0.03057 0.02795 = 0.01962 0.00027 -0.00796 -0.00306 AFIX 43 H79 2 0.125594 0.969405 0.229781 11.00000 -1.20000 AFIX 0 C80 1 0.269844 1.115531 0.197786 11.00000 0.05614 0.03536 = 0.03831 -0.00831 -0.01525 -0.01346 C81 1 0.387058 1.146458 0.203654 11.00000 0.06973 0.06160 = 0.04111 -0.00315 -0.01950 -0.03691 AFIX 137 H81A 2 0.378696 1.196735 0.220559 11.00000 -1.50000 H81B 2 0.433958 1.156766 0.169369 11.00000 -1.50000 H81C 2 0.425894 1.106289 0.224907 11.00000 -1.50000 AFIX 0 C82 1 0.220896 1.164194 0.067849 11.00000 0.02323 0.01625 = 0.01975 -0.00188 -0.00223 -0.00019 C83 1 0.111059 1.198333 0.072120 11.00000 0.02309 0.01894 = 0.02389 -0.00227 -0.00208 -0.00042 AFIX 43 H83 2 0.045215 1.164884 0.070909 11.00000 -1.20000 AFIX 0 C84 1 0.093823 1.279979 0.078126 11.00000 0.02779 0.01829 = 0.02670 -0.00349 -0.00259 0.00243 C85 1 0.194059 1.326959 0.081391 11.00000 0.03564 0.01636 = 0.03054 -0.00427 -0.00342 -0.00106 C86 1 0.306889 1.295105 0.077422 11.00000 0.03015 0.02189 = 0.02869 -0.00233 -0.00452 -0.00636 C87 1 0.316881 1.213071 0.070271 11.00000 0.02265 0.02142 = 0.02514 -0.00184 -0.00189 -0.00285 AFIX 43 H87 2 0.392273 1.189791 0.066933 11.00000 -1.20000 AFIX 0 C88 1 0.415672 1.346141 0.081526 11.00000 0.03468 0.02653 = 0.04095 -0.00193 -0.00863 -0.01134 C89 1 0.527814 1.296263 0.075616 11.00000 0.02908 0.04046 = 0.06229 -0.00371 -0.00930 -0.01255 AFIX 137 H89A 2 0.595111 1.331114 0.077309 11.00000 -1.50000 H89B 2 0.537349 1.273310 0.042095 11.00000 -1.50000 H89C 2 0.522510 1.252551 0.103673 11.00000 -1.50000 AFIX 0 C90 1 0.404773 1.380596 0.134405 11.00000 0.05177 0.04233 = 0.05305 -0.01373 -0.01806 -0.01107 AFIX 137 H90A 2 0.475196 1.412123 0.136410 11.00000 -1.50000 H90B 2 0.395763 1.336211 0.162076 11.00000 -1.50000 H90C 2 0.336396 1.415465 0.138512 11.00000 -1.50000 AFIX 0 C91 1 0.433957 1.415651 0.038049 11.00000 0.04719 0.03613 = 0.05824 0.00788 -0.00991 -0.01974 AFIX 137 H91A 2 0.501939 1.448237 0.042158 11.00000 -1.50000 H91B 2 0.364436 1.449541 0.039997 11.00000 -1.50000 H91C 2 0.447147 1.393464 0.004289 11.00000 -1.50000 AFIX 0 C92 1 -0.029469 1.315691 0.080416 11.00000 0.03091 0.02225 = 0.04363 -0.00684 -0.00308 0.00765 C93 1 -0.119707 1.251538 0.073666 11.00000 0.02508 0.03380 = 0.08227 -0.01010 -0.00964 0.00718 AFIX 137 H93A 2 -0.196460 1.276480 0.073649 11.00000 -1.50000 H93B 2 -0.123685 1.208896 0.102340 11.00000 -1.50000 H93C 2 -0.096649 1.228239 0.040695 11.00000 -1.50000 AFIX 0 C94 1 -0.031690 1.382091 0.035342 11.00000 0.04418 0.03235 = 0.04740 -0.00533 -0.01144 0.01250 AFIX 137 H94A 2 -0.111232 1.402580 0.035832 11.00000 -1.50000 H94B 2 -0.006468 1.359539 0.002289 11.00000 -1.50000 H94C 2 0.021220 1.426330 0.039275 11.00000 -1.50000 AFIX 0 C95 1 -0.069319 1.348283 0.133152 11.00000 0.04705 0.03470 = 0.04883 -0.00807 0.00715 0.01171 AFIX 137 H95A 2 -0.147913 1.370456 0.133615 11.00000 -1.50000 H95B 2 -0.015087 1.390828 0.138588 11.00000 -1.50000 H95C 2 -0.070357 1.304339 0.160869 11.00000 -1.50000 AFIX 0 C96 1 0.945598 0.513477 0.404856 11.00000 0.02186 AFIX 43 H96 2 0.959006 0.509229 0.439993 11.00000 -1.20000 AFIX 0 C97 1 0.733365 0.861918 0.600424 11.00000 0.04676 0.02509 = 0.05011 -0.00794 -0.00150 0.01074 C98 1 0.621140 0.818171 0.593261 11.00000 0.03981 0.03510 = 0.08636 0.00069 -0.00463 0.01316 AFIX 137 H98A 2 0.560154 0.857842 0.588271 11.00000 -1.50000 H98B 2 0.595294 0.781179 0.624141 11.00000 -1.50000 H98C 2 0.636206 0.787518 0.562790 11.00000 -1.50000 AFIX 0 C99 1 0.708372 0.905117 0.650506 11.00000 0.08533 0.05029 = 0.06511 -0.02442 0.00861 0.02188 AFIX 137 H99A 2 0.643859 0.942729 0.647748 11.00000 -1.50000 H99B 2 0.778340 0.934995 0.655329 11.00000 -1.50000 H99C 2 0.687042 0.865067 0.680254 11.00000 -1.50000 AFIX 0 C100 1 0.762085 0.922739 0.552903 11.00000 0.05351 0.03306 = 0.07331 0.00165 -0.00661 0.01244 AFIX 137 H11V 2 0.697632 0.960705 0.551271 11.00000 -1.50000 H11W 2 0.773239 0.894140 0.521470 11.00000 -1.50000 H11X 2 0.833820 0.952415 0.555464 11.00000 -1.50000 AFIX 0 HKLF 4 REM resc_ac8@160k1_0m in P-1 REM R1 = 0.0698 for 19900 Fo > 4sig(Fo) and 0.0916 for all 26976 data REM 1176 parameters refined using 0 restraints END WGHT 0.1124 2.5145 REM Highest difference peak 1.478, deepest hole -0.858, 1-sigma level 0.082 Q1 1 0.5983 0.3808 0.6410 11.00000 0.05 1.48 Q2 1 0.5392 0.2850 0.2939 11.00000 0.05 1.20 Q3 1 0.6341 0.3312 0.2215 11.00000 0.05 1.00 Q4 1 0.5616 0.8408 0.2067 11.00000 0.05 0.83 Q5 1 0.6048 0.2545 0.2504 11.00000 0.05 0.81 ; _shelx_res_checksum 30294 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 C01 C 0.6115(6) 0.3468(3) 0.2518(3) 0.140(3) Uani 0.889(3) 1 d . . P . . H01A H 0.6289 0.4010 0.2332 0.168 Uiso 0.889(3) 1 calc R U P . . H01B H 0.6623 0.3395 0.2792 0.168 Uiso 0.889(3) 1 calc R U P . . Cl1 Cl 0.64201(13) 0.28342(12) 0.21375(9) 0.1414(8) Uani 0.889(3) 1 d . . P . . Cl2 Cl 0.44795(19) 0.34345(12) 0.28470(6) 0.1404(8) Uani 0.889(3) 1 d . . P . . C02 C 0.3823(2) 0.88432(16) 0.21362(9) 0.0458(5) Uani 1 1 d . . . . . H02A H 0.3076 0.8630 0.2058 0.055 Uiso 1 1 calc R U . . . H02B H 0.4099 0.9279 0.1862 0.055 Uiso 1 1 calc R U . . . Cl3 Cl 0.48454(9) 0.80714(6) 0.21182(4) 0.0858(3) Uani 1 1 d . . . . . Cl4 Cl 0.35750(7) 0.92496(6) 0.27349(3) 0.0689(2) Uani 1 1 d . . . . . O1 O 0.6350(3) 0.4575(3) 0.66683(13) 0.164(2) Uani 1 1 d . . . . . O2 O 0.92315(13) 0.55710(10) 0.71788(5) 0.0390(3) Uani 1 1 d . . . . . O3 O 1.0681(2) 0.63703(14) 0.73464(9) 0.0702(6) Uani 1 1 d . . . . . O4 O 0.97259(18) 0.91041(10) 0.60833(9) 0.0547(5) Uani 1 1 d . . . . . H4O H 0.926(3) 0.910(2) 0.6321(14) 0.066 Uiso 1 1 d . U . . . O5 O 0.83308(17) 0.93695(9) 0.40535(8) 0.0481(4) Uani 1 1 d . . . . . H5O H 0.898(3) 0.9465(19) 0.4097(13) 0.058 Uiso 1 1 d . U . . . O6 O 0.74682(12) 0.61407(8) 0.32445(5) 0.0296(3) Uani 1 1 d . . . . . O7 O 0.65362(17) 0.51258(12) 0.29645(10) 0.0686(6) Uani 1 1 d . . . . . O8 O 0.66467(11) 0.44775(8) 0.45567(5) 0.0260(3) Uani 1 1 d . . . . . O9 O 0.50475(13) 0.40170(11) 0.51032(6) 0.0433(4) Uani 1 1 d . . . . . O10 O 0.79400(12) 0.41301(8) 0.62287(5) 0.0319(3) Uani 1 1 d . . . . . O11 O 0.27991(11) 1.05490(8) 0.16571(5) 0.0294(3) Uani 1 1 d . . . . . O12 O 0.1787(2) 1.13793(14) 0.21753(11) 0.0793(7) Uani 1 1 d . . . . . O13 O 0.18487(15) 1.40795(8) 0.08896(7) 0.0401(4) Uani 1 1 d . . . . . O14 O 0.02251(14) 1.44422(8) -0.10893(7) 0.0406(4) Uani 1 1 d . . . . . O15 O -0.09285(15) 1.19897(10) -0.23562(7) 0.0483(4) Uani 1 1 d . . . . . H15O H 0.124(3) 1.4191(19) 0.0887(13) 0.058 Uiso 1 1 d . U . . . O16 O 0.05739(11) 1.11713(8) -0.22168(5) 0.0297(3) Uani 1 1 d . . . . . H16O H 0.075(2) 1.4670(16) -0.1107(10) 0.036 Uiso 1 1 d . U . . . O17 O 0.21530(12) 0.95920(8) -0.13417(5) 0.0287(3) Uani 1 1 d . . . . . O18 O 0.3969(2) 1.00091(18) -0.16464(8) 0.0839(8) Uani 1 1 d . . . . . O19 O 0.32916(10) 0.93014(7) 0.03653(5) 0.0226(2) Uani 1 1 d . . . . . O20 O 0.49469(12) 0.91421(10) -0.01829(6) 0.0371(3) Uani 1 1 d . . . . . C1 C 0.5884(3) 0.64875(19) 0.28180(15) 0.0718(9) Uani 1 1 d . . . . . H1A H 0.5257 0.6257 0.2660 0.108 Uiso 1 1 calc R U . . . H1B H 0.6363 0.6857 0.2559 0.108 Uiso 1 1 calc R U . . . H1C H 0.5544 0.6784 0.3109 0.108 Uiso 1 1 calc R U . . . C2 C 0.66273(19) 0.58245(14) 0.30101(10) 0.0408(5) Uani 1 1 d . . . . . C3 C 0.83514(15) 0.56373(11) 0.33942(7) 0.0254(3) Uani 1 1 d . . . . . C4 C 0.90868(17) 0.52709(12) 0.30232(7) 0.0306(4) Uani 1 1 d . . . . . H4 H 0.8969 0.5328 0.2670 0.037 Uiso 1 1 calc R U . . . C5 C 0.85005(14) 0.55724(10) 0.39152(6) 0.0213(3) Uani 1 1 d . . . . . C6 C 0.76440(14) 0.59755(10) 0.43109(6) 0.0204(3) Uani 1 1 d . . . . . H6 H 0.6846 0.5888 0.4220 0.025 Uiso 1 1 calc R U . . . C7 C 0.76626(13) 0.55420(10) 0.48495(6) 0.0199(3) Uani 1 1 d . . . . . C8 C 0.81905(14) 0.58509(10) 0.52380(6) 0.0207(3) Uani 1 1 d . . . . . H8 H 0.8522 0.6379 0.5176 0.025 Uiso 1 1 calc R U . . . C9 C 0.82500(14) 0.54134(10) 0.57139(6) 0.0214(3) Uani 1 1 d . . . . . C10 C 0.77899(15) 0.46308(10) 0.57800(7) 0.0237(3) Uani 1 1 d . . . . . C11 C 0.7147(3) 0.4107(3) 0.66410(13) 0.0862(13) Uani 1 1 d . . . . . C12 C 0.7457(3) 0.3510(3) 0.70627(13) 0.0903(14) Uani 1 1 d . . . . . H12A H 0.8308 0.3489 0.7045 0.135 Uiso 1 1 calc R U . . . H12B H 0.7153 0.2975 0.7018 0.135 Uiso 1 1 calc R U . . . H12C H 0.7111 0.3675 0.7401 0.135 Uiso 1 1 calc R U . . . C13 C 0.72503(15) 0.42991(10) 0.54097(7) 0.0247(3) Uani 1 1 d . . . . . H13 H 0.6943 0.3764 0.5467 0.030 Uiso 1 1 calc R U . . . C14 C 0.71718(14) 0.47708(10) 0.49526(6) 0.0219(3) Uani 1 1 d . . . . . C15 C 0.55347(16) 0.41640(11) 0.46710(8) 0.0290(4) Uani 1 1 d . . . . . C16 C 0.50494(19) 0.40491(15) 0.41820(9) 0.0416(5) Uani 1 1 d . . . . . H16A H 0.4486 0.3599 0.4245 0.062 Uiso 1 1 calc R U . . . H16B H 0.5686 0.3930 0.3911 0.062 Uiso 1 1 calc R U . . . H16C H 0.4658 0.4543 0.4069 0.062 Uiso 1 1 calc R U . . . C17 C 0.87584(15) 0.57438(10) 0.61588(7) 0.0235(3) Uani 1 1 d . . . . . H17 H 0.8130 0.5670 0.6465 0.028 Uiso 1 1 calc R U . . . C18 C 0.97769(15) 0.52431(10) 0.63109(7) 0.0234(3) Uani 1 1 d . . . . . C19 C 1.00033(16) 0.51794(12) 0.68208(7) 0.0286(4) Uani 1 1 d . . . . . C20 C 0.9663(3) 0.62143(17) 0.73869(9) 0.0512(6) Uani 1 1 d . . . . . C22 C 0.90544(16) 0.66429(11) 0.60895(7) 0.0265(3) Uani 1 1 d . . . . . C21 C 0.8677(3) 0.6669(2) 0.76562(13) 0.0768(10) Uani 1 1 d . . . . . H21A H 0.8213 0.6918 0.7400 0.115 Uiso 1 1 calc R U . . . H21B H 0.8990 0.7091 0.7838 0.115 Uiso 1 1 calc R U . . . H21C H 0.8181 0.6298 0.7907 0.115 Uiso 1 1 calc R U . . . C23 C 1.01689(18) 0.69294(12) 0.60990(9) 0.0357(4) Uani 1 1 d . . . . . H23 H 1.0787 0.6554 0.6104 0.043 Uiso 1 1 calc R U . . . C24 C 1.0424(2) 0.77509(13) 0.61017(10) 0.0430(5) Uani 1 1 d . . . . . C25 C 0.9498(2) 0.82855(12) 0.60797(10) 0.0409(5) Uani 1 1 d . . . . . C26 C 0.83505(19) 0.80250(12) 0.60462(8) 0.0337(4) Uani 1 1 d . . . . . C27 C 0.81607(17) 0.71985(11) 0.60619(7) 0.0288(4) Uani 1 1 d . . . . . H27 H 0.7392 0.7005 0.6054 0.035 Uiso 1 1 calc R U . . . C28 C 1.1660(2) 0.80323(16) 0.61610(14) 0.0630(8) Uani 1 1 d . . . . . C29 C 1.2177(3) 0.86136(18) 0.56977(17) 0.0753(10) Uani 1 1 d . . . . . H29A H 1.2948 0.8802 0.5753 0.113 Uiso 1 1 calc R U . . . H29B H 1.1661 0.9076 0.5663 0.113 Uiso 1 1 calc R U . . . H29C H 1.2254 0.8334 0.5381 0.113 Uiso 1 1 calc R U . . . C30 C 1.1631(4) 0.8437(2) 0.66773(17) 0.0891(12) Uani 1 1 d . . . . . H30A H 1.2422 0.8612 0.6712 0.134 Uiso 1 1 calc R U . . . H30B H 1.1337 0.8047 0.6971 0.134 Uiso 1 1 calc R U . . . H30C H 1.1117 0.8905 0.6673 0.134 Uiso 1 1 calc R U . . . C31 C 1.2479(3) 0.73157(19) 0.62006(19) 0.0806(12) Uani 1 1 d . . . . . H31A H 1.3238 0.7503 0.6271 0.121 Uiso 1 1 calc R U . . . H31B H 1.2582 0.7064 0.5873 0.121 Uiso 1 1 calc R U . . . H31C H 1.2142 0.6920 0.6483 0.121 Uiso 1 1 calc R U . . . C32 C 0.78515(15) 0.68812(10) 0.42650(6) 0.0224(3) Uani 1 1 d . . . . . C33 C 0.69222(16) 0.73957(11) 0.42039(7) 0.0275(3) Uani 1 1 d . . . . . H33 H 0.6165 0.7169 0.4213 0.033 Uiso 1 1 calc R U . . . C35 C 0.81962(18) 0.85375(11) 0.41290(8) 0.0329(4) Uani 1 1 d . . . . . C34 C 0.70648(18) 0.82321(11) 0.41293(8) 0.0319(4) Uani 1 1 d . . . . . C36 C 0.91579(17) 0.80419(11) 0.41997(8) 0.0303(4) Uani 1 1 d . . . . . C38 C 1.03922(19) 0.83813(12) 0.42095(10) 0.0411(5) Uani 1 1 d . . . . . C37 C 0.89480(15) 0.72083(10) 0.42574(7) 0.0259(3) Uani 1 1 d . . . . . H37 H 0.9584 0.6856 0.4292 0.031 Uiso 1 1 calc R U . . . C39 C 1.1255(2) 0.77047(15) 0.43155(14) 0.0572(7) Uani 1 1 d . . . . . H39A H 1.2019 0.7942 0.4338 0.086 Uiso 1 1 calc R U . . . H39B H 1.1332 0.7352 0.4033 0.086 Uiso 1 1 calc R U . . . H39C H 1.0965 0.7389 0.4644 0.086 Uiso 1 1 calc R U . . . C40 C 1.0379(2) 0.89239(15) 0.46542(11) 0.0501(6) Uani 1 1 d . . . . . H40A H 1.1178 0.9100 0.4674 0.075 Uiso 1 1 calc R U . . . H40B H 1.0053 0.8621 0.4982 0.075 Uiso 1 1 calc R U . . . H40C H 0.9897 0.9397 0.4590 0.075 Uiso 1 1 calc R U . . . C41 C 1.0868(3) 0.88416(17) 0.36823(12) 0.0605(8) Uani 1 1 d . . . . . H41A H 1.1616 0.9101 0.3707 0.091 Uiso 1 1 calc R U . . . H41B H 1.0309 0.9254 0.3591 0.091 Uiso 1 1 calc R U . . . H41C H 1.0983 0.8462 0.3415 0.091 Uiso 1 1 calc R U . . . C42 C 0.6026(2) 0.87801(13) 0.40339(10) 0.0440(5) Uani 1 1 d . . . . . C43 C 0.5782(3) 0.93631(16) 0.44660(12) 0.0585(7) Uani 1 1 d . . . . . H43A H 0.5153 0.9730 0.4390 0.088 Uiso 1 1 calc R U . . . H43B H 0.6491 0.9677 0.4480 0.088 Uiso 1 1 calc R U . . . H43C H 0.5548 0.9050 0.4801 0.088 Uiso 1 1 calc R U . . . C44 C 0.6289(3) 0.92611(18) 0.34980(12) 0.0638(8) Uani 1 1 d . . . . . H44A H 0.5631 0.9614 0.3442 0.096 Uiso 1 1 calc R U . . . H44B H 0.6406 0.8886 0.3228 0.096 Uiso 1 1 calc R U . . . H44C H 0.6998 0.9589 0.3483 0.096 Uiso 1 1 calc R U . . . C45 C 0.4908(2) 0.82916(16) 0.40399(13) 0.0568(7) Uani 1 1 d . . . . . H45A H 0.4270 0.8658 0.3976 0.085 Uiso 1 1 calc R U . . . H45B H 0.4708 0.7983 0.4379 0.085 Uiso 1 1 calc R U . . . H45C H 0.5027 0.7919 0.3768 0.085 Uiso 1 1 calc R U . . . C46 C 0.2807(3) 0.9401(2) -0.22083(10) 0.0698(9) Uani 1 1 d . . . . . H46A H 0.3513 0.9429 -0.2466 0.105 Uiso 1 1 calc R U . . . H46B H 0.2201 0.9738 -0.2342 0.105 Uiso 1 1 calc R U . . . H46C H 0.2526 0.8840 -0.2139 0.105 Uiso 1 1 calc R U . . . C47 C 0.3083(2) 0.96992(15) -0.17165(9) 0.0447(5) Uani 1 1 d . . . . . C48 C 0.22310(14) 0.99032(10) -0.08662(6) 0.0207(3) Uani 1 1 d . . . . . C49 C 0.27400(14) 0.94364(10) -0.04979(6) 0.0215(3) Uani 1 1 d . . . . . H49 H 0.3053 0.8923 -0.0566 0.026 Uiso 1 1 calc R U . . . C50 C 0.27805(13) 0.97400(9) -0.00261(6) 0.0193(3) Uani 1 1 d . . . . . C51 C 0.22975(13) 1.04810(9) 0.00929(6) 0.0179(3) Uani 1 1 d . . . . . C52 C 0.17769(13) 1.09240(9) -0.02912(6) 0.0187(3) Uani 1 1 d . . . . . H52 H 0.1435 1.1428 -0.0218 0.022 Uiso 1 1 calc R U . . . C53 C 0.17410(13) 1.06532(9) -0.07786(6) 0.0181(3) Uani 1 1 d . . . . . C54 C 0.44353(15) 0.90850(10) 0.02473(7) 0.0254(3) Uani 1 1 d . . . . . C55 C 0.49255(17) 0.87940(13) 0.07266(9) 0.0370(4) Uani 1 1 d . . . . . H55A H 0.5625 0.8476 0.0634 0.056 Uiso 1 1 calc R U . . . H55B H 0.4342 0.8457 0.0959 0.056 Uiso 1 1 calc R U . . . H55C H 0.5132 0.9258 0.0902 0.056 Uiso 1 1 calc R U . . . C56 C 0.11900(13) 1.11062(9) -0.12138(6) 0.0188(3) Uani 1 1 d . . . . . H56 H 0.1786 1.1111 -0.1531 0.023 Uiso 1 1 calc R U . . . C57 C 0.01431(13) 1.06428(9) -0.13301(6) 0.0190(3) Uani 1 1 d . . . . . C58 C -0.01474(15) 1.06928(10) -0.18284(6) 0.0229(3) Uani 1 1 d . . . . . C59 C 0.0087(2) 1.18342(13) -0.24435(8) 0.0371(4) Uani 1 1 d . . . . . C60 C 0.1002(3) 1.23250(19) -0.28002(11) 0.0607(8) Uani 1 1 d . . . . . H60A H 0.0629 1.2757 -0.2996 0.091 Uiso 1 1 calc R U . . . H60B H 0.1436 1.1978 -0.3042 0.091 Uiso 1 1 calc R U . . . H60C H 0.1540 1.2561 -0.2597 0.091 Uiso 1 1 calc R U . . . C61 C 0.09085(14) 1.19936(10) -0.11428(6) 0.0212(3) Uani 1 1 d . . . . . C62 C -0.02144(15) 1.22854(10) -0.11259(7) 0.0261(3) Uani 1 1 d . . . . . H62 H -0.0840 1.1914 -0.1120 0.031 Uiso 1 1 calc R U . . . C63 C -0.04654(16) 1.31071(11) -0.11173(8) 0.0292(4) Uani 1 1 d . . . . . C64 C 0.04727(17) 1.36312(10) -0.11056(8) 0.0290(4) Uani 1 1 d . . . . . C65 C 0.16344(16) 1.33631(10) -0.11145(7) 0.0265(3) Uani 1 1 d . . . . . C66 C 0.18193(15) 1.25369(10) -0.11380(7) 0.0236(3) Uani 1 1 d . . . . . H66 H 0.2592 1.2339 -0.1151 0.028 Uiso 1 1 calc R U . . . C67 C -0.17172(18) 1.34132(12) -0.11428(10) 0.0392(5) Uani 1 1 d . . . . . C68 C -0.2552(2) 1.27180(15) -0.11869(14) 0.0580(8) Uani 1 1 d . . . . . H68A H -0.3338 1.2929 -0.1203 0.087 Uiso 1 1 calc R U . . . H68B H -0.2568 1.2323 -0.0884 0.087 Uiso 1 1 calc R U . . . H68C H -0.2283 1.2457 -0.1503 0.087 Uiso 1 1 calc R U . . . C69 C -0.1721(3) 1.40095(17) -0.16297(12) 0.0571(7) Uani 1 1 d . . . . . H69A H -0.2525 1.4166 -0.1663 0.086 Uiso 1 1 calc R U . . . H69B H -0.1381 1.3751 -0.1938 0.086 Uiso 1 1 calc R U . . . H69C H -0.1258 1.4491 -0.1598 0.086 Uiso 1 1 calc R U . . . C70 C -0.2199(2) 1.38172(15) -0.06523(11) 0.0470(6) Uani 1 1 d . . . . . H70A H -0.2979 1.4028 -0.0686 0.071 Uiso 1 1 calc R U . . . H70B H -0.1678 1.4262 -0.0609 0.071 Uiso 1 1 calc R U . . . H70C H -0.2248 1.3420 -0.0349 0.071 Uiso 1 1 calc R U . . . C71 C 0.26603(17) 1.39449(11) -0.10979(9) 0.0346(4) Uani 1 1 d . . . . . C72 C 0.2812(3) 1.45651(15) -0.15786(12) 0.0556(7) Uani 1 1 d . . . . . H72A H 0.3480 1.4921 -0.1566 0.083 Uiso 1 1 calc R U . . . H72B H 0.2103 1.4887 -0.1582 0.083 Uiso 1 1 calc R U . . . H72C H 0.2951 1.4281 -0.1894 0.083 Uiso 1 1 calc R U . . . C73 C 0.2463(2) 1.43745(14) -0.05939(11) 0.0468(6) Uani 1 1 d . . . . . H73A H 0.3122 1.4740 -0.0587 0.070 Uiso 1 1 calc R U . . . H73B H 0.2401 1.3971 -0.0293 0.070 Uiso 1 1 calc R U . . . H73C H 0.1740 1.4684 -0.0582 0.070 Uiso 1 1 calc R U . . . C74 C 0.38192(19) 1.34993(14) -0.10928(12) 0.0474(6) Uani 1 1 d . . . . . H74A H 0.4441 1.3886 -0.1065 0.071 Uiso 1 1 calc R U . . . H74B H 0.4009 1.3238 -0.1415 0.071 Uiso 1 1 calc R U . . . H74C H 0.3749 1.3090 -0.0795 0.071 Uiso 1 1 calc R U . . . C75 C 0.23712(13) 1.07446(9) 0.06294(6) 0.0181(3) Uani 1 1 d . . . . . H75 H 0.3182 1.0621 0.0701 0.022 Uiso 1 1 calc R U . . . C76 C 0.15539(13) 1.02422(9) 0.10474(6) 0.0182(3) Uani 1 1 d . . . . . C77 C 0.05791(13) 0.98295(9) 0.09464(6) 0.0184(3) Uani 1 1 d . . . . . H77 H 0.0399 0.9871 0.0602 0.022 Uiso 1 1 calc R U . . . C78 C 0.17791(14) 1.01790(10) 0.15582(7) 0.0226(3) Uani 1 1 d . . . . . C79 C 0.10896(15) 0.97229(11) 0.19513(7) 0.0258(3) Uani 1 1 d . . . . . H79 H 0.1256 0.9694 0.2298 0.031 Uiso 1 1 calc R U . . . C80 C 0.2698(2) 1.11553(14) 0.19779(9) 0.0421(5) Uani 1 1 d . . . . . C81 C 0.3871(3) 1.14646(18) 0.20365(10) 0.0564(7) Uani 1 1 d . . . . . H81A H 0.3787 1.1967 0.2206 0.085 Uiso 1 1 calc R U . . . H81B H 0.4340 1.1568 0.1694 0.085 Uiso 1 1 calc R U . . . H81C H 0.4259 1.1063 0.2249 0.085 Uiso 1 1 calc R U . . . C82 C 0.22090(14) 1.16419(9) 0.06785(6) 0.0198(3) Uani 1 1 d . . . . . C83 C 0.11106(14) 1.19833(10) 0.07212(7) 0.0221(3) Uani 1 1 d . . . . . H83 H 0.0452 1.1649 0.0709 0.026 Uiso 1 1 calc R U . . . C84 C 0.09382(15) 1.27998(10) 0.07813(7) 0.0243(3) Uani 1 1 d . . . . . C85 C 0.19406(16) 1.32696(10) 0.08139(7) 0.0275(4) Uani 1 1 d . . . . . C86 C 0.30689(16) 1.29511(11) 0.07742(7) 0.0269(3) Uani 1 1 d . . . . . C87 C 0.31688(14) 1.21307(10) 0.07027(7) 0.0232(3) Uani 1 1 d . . . . . H87 H 0.3923 1.1898 0.0669 0.028 Uiso 1 1 calc R U . . . C88 C 0.41567(18) 1.34614(12) 0.08153(8) 0.0338(4) Uani 1 1 d . . . . . C89 C 0.52781(18) 1.29626(14) 0.07562(11) 0.0437(5) Uani 1 1 d . . . . . H89A H 0.5951 1.3311 0.0773 0.066 Uiso 1 1 calc R U . . . H89B H 0.5373 1.2733 0.0421 0.066 Uiso 1 1 calc R U . . . H89C H 0.5225 1.2526 0.1037 0.066 Uiso 1 1 calc R U . . . C90 C 0.4048(2) 1.38060(15) 0.13440(10) 0.0474(6) Uani 1 1 d . . . . . H90A H 0.4752 1.4121 0.1364 0.071 Uiso 1 1 calc R U . . . H90B H 0.3958 1.3362 0.1621 0.071 Uiso 1 1 calc R U . . . H90C H 0.3364 1.4155 0.1385 0.071 Uiso 1 1 calc R U . . . C91 C 0.4340(2) 1.41565(14) 0.03805(11) 0.0477(6) Uani 1 1 d . . . . . H91A H 0.5019 1.4482 0.0422 0.072 Uiso 1 1 calc R U . . . H91B H 0.3644 1.4495 0.0400 0.072 Uiso 1 1 calc R U . . . H91C H 0.4471 1.3935 0.0043 0.072 Uiso 1 1 calc R U . . . C92 C -0.02947(17) 1.31569(11) 0.08042(8) 0.0323(4) Uani 1 1 d . . . . . C93 C -0.11971(18) 1.25154(13) 0.07367(12) 0.0466(6) Uani 1 1 d . . . . . H93A H -0.1965 1.2765 0.0736 0.070 Uiso 1 1 calc R U . . . H93B H -0.1237 1.2089 0.1023 0.070 Uiso 1 1 calc R U . . . H93C H -0.0966 1.2282 0.0407 0.070 Uiso 1 1 calc R U . . . C94 C -0.0317(2) 1.38209(13) 0.03534(9) 0.0407(5) Uani 1 1 d . . . . . H94A H -0.1112 1.4026 0.0358 0.061 Uiso 1 1 calc R U . . . H94B H -0.0065 1.3595 0.0023 0.061 Uiso 1 1 calc R U . . . H94C H 0.0212 1.4263 0.0393 0.061 Uiso 1 1 calc R U . . . C95 C -0.0693(2) 1.34828(14) 0.13315(10) 0.0446(5) Uani 1 1 d . . . . . H95A H -0.1479 1.3705 0.1336 0.067 Uiso 1 1 calc R U . . . H95B H -0.0151 1.3908 0.1386 0.067 Uiso 1 1 calc R U . . . H95C H -0.0704 1.3043 0.1609 0.067 Uiso 1 1 calc R U . . . C96 C 0.94560(14) 0.51348(10) 0.40486(6) 0.0219(3) Uiso 1 1 d . . . . . H96 H 0.9590 0.5092 0.4400 0.026 Uiso 1 1 calc R U . . . C97 C 0.7334(2) 0.86192(12) 0.60042(10) 0.0409(5) Uani 1 1 d . . . . . C98 C 0.6211(2) 0.81817(15) 0.59326(13) 0.0546(7) Uani 1 1 d . . . . . H98A H 0.5602 0.8578 0.5883 0.082 Uiso 1 1 calc R U . . . H98B H 0.5953 0.7812 0.6241 0.082 Uiso 1 1 calc R U . . . H98C H 0.6362 0.7875 0.5628 0.082 Uiso 1 1 calc R U . . . C99 C 0.7084(3) 0.90512(18) 0.65051(12) 0.0676(8) Uani 1 1 d . . . . . H99A H 0.6439 0.9427 0.6477 0.101 Uiso 1 1 calc R U . . . H99B H 0.7783 0.9350 0.6553 0.101 Uiso 1 1 calc R U . . . H99C H 0.6870 0.8651 0.6803 0.101 Uiso 1 1 calc R U . . . C100 C 0.7621(2) 0.92274(15) 0.55290(12) 0.0540(6) Uani 1 1 d . . . . . H11V H 0.6976 0.9607 0.5513 0.081 Uiso 1 1 calc R U . . . H11W H 0.7732 0.8941 0.5215 0.081 Uiso 1 1 calc R U . . . H11X H 0.8338 0.9524 0.5555 0.081 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C01 0.154(5) 0.086(3) 0.196(7) 0.046(4) -0.113(5) -0.075(4) Cl1 0.0769(8) 0.1553(16) 0.207(2) -0.0677(14) -0.0403(10) -0.0096(9) Cl2 0.1877(19) 0.1661(17) 0.0756(9) -0.0466(9) -0.0241(10) 0.0120(13) C02 0.0513(13) 0.0509(14) 0.0362(11) -0.0054(10) -0.0090(10) 0.0109(10) Cl3 0.1005(7) 0.0802(6) 0.0752(5) 0.0036(4) -0.0147(5) 0.0514(5) Cl4 0.0654(4) 0.1058(6) 0.0375(3) -0.0190(4) -0.0061(3) 0.0078(4) O1 0.109(2) 0.241(5) 0.099(2) 0.102(3) 0.0584(19) 0.095(3) O2 0.0420(8) 0.0533(9) 0.0240(7) -0.0119(6) -0.0071(6) 0.0185(7) O3 0.0705(14) 0.0805(15) 0.0680(13) -0.0463(12) -0.0143(11) 0.0071(11) O4 0.0595(11) 0.0256(7) 0.0843(15) -0.0193(9) -0.0194(10) 0.0003(7) O5 0.0595(10) 0.0177(7) 0.0643(11) 0.0040(7) -0.0040(9) 0.0026(7) O6 0.0331(7) 0.0306(7) 0.0265(6) 0.0010(5) -0.0109(5) 0.0074(5) O7 0.0517(11) 0.0481(11) 0.1151(19) -0.0163(11) -0.0371(11) 0.0000(8) O8 0.0269(6) 0.0267(6) 0.0253(6) -0.0036(5) -0.0059(5) -0.0066(5) O9 0.0294(7) 0.0571(10) 0.0413(9) 0.0044(7) -0.0035(6) -0.0097(7) O10 0.0360(7) 0.0301(7) 0.0285(7) 0.0105(5) -0.0092(5) -0.0023(5) O11 0.0309(6) 0.0337(7) 0.0252(6) -0.0017(5) -0.0100(5) -0.0105(5) O12 0.0679(14) 0.0658(13) 0.1128(19) -0.0595(14) -0.0099(13) -0.0026(10) O13 0.0488(9) 0.0187(6) 0.0548(10) -0.0105(6) -0.0098(8) 0.0002(6) O14 0.0391(8) 0.0165(6) 0.0669(11) -0.0026(7) -0.0116(8) 0.0013(5) O15 0.0508(10) 0.0418(9) 0.0494(10) 0.0173(8) -0.0111(8) 0.0018(7) O16 0.0320(6) 0.0350(7) 0.0205(6) 0.0075(5) -0.0046(5) -0.0086(5) O17 0.0363(7) 0.0282(6) 0.0243(6) -0.0103(5) -0.0090(5) 0.0066(5) O18 0.0687(14) 0.125(2) 0.0521(12) -0.0329(13) 0.0287(10) -0.0380(14) O19 0.0220(5) 0.0218(6) 0.0229(6) 0.0020(5) -0.0025(4) 0.0054(4) O20 0.0252(6) 0.0517(9) 0.0335(7) -0.0055(6) -0.0006(5) 0.0086(6) C1 0.0579(17) 0.0647(18) 0.105(3) -0.0128(17) -0.0499(17) 0.0233(14) C2 0.0324(10) 0.0424(12) 0.0499(13) -0.0029(10) -0.0143(9) 0.0035(8) C3 0.0290(8) 0.0238(8) 0.0237(8) 0.0016(6) -0.0077(6) 0.0034(6) C4 0.0370(9) 0.0362(10) 0.0194(8) -0.0010(7) -0.0084(7) 0.0072(8) C5 0.0250(7) 0.0179(7) 0.0209(7) 0.0005(6) -0.0042(6) -0.0015(6) C6 0.0218(7) 0.0198(7) 0.0199(7) -0.0001(6) -0.0046(6) 0.0005(6) C7 0.0205(7) 0.0184(7) 0.0209(7) -0.0006(6) -0.0034(6) 0.0008(5) C8 0.0224(7) 0.0173(7) 0.0219(7) -0.0002(6) -0.0031(6) -0.0001(5) C9 0.0227(7) 0.0207(7) 0.0211(7) -0.0016(6) -0.0041(6) 0.0024(6) C10 0.0251(7) 0.0217(8) 0.0232(8) 0.0041(6) -0.0043(6) -0.0003(6) C11 0.0581(17) 0.128(3) 0.0548(18) 0.051(2) 0.0132(14) 0.0310(19) C12 0.073(2) 0.132(3) 0.0513(18) 0.055(2) 0.0003(15) 0.018(2) C13 0.0263(8) 0.0188(8) 0.0286(8) 0.0028(6) -0.0054(6) -0.0040(6) C14 0.0227(7) 0.0214(8) 0.0220(8) -0.0020(6) -0.0042(6) -0.0015(6) C15 0.0256(8) 0.0249(8) 0.0376(10) -0.0033(7) -0.0076(7) -0.0023(6) C16 0.0353(10) 0.0490(13) 0.0450(12) -0.0129(10) -0.0151(9) -0.0064(9) C17 0.0272(8) 0.0231(8) 0.0213(8) -0.0039(6) -0.0064(6) 0.0035(6) C18 0.0273(8) 0.0224(8) 0.0213(8) -0.0020(6) -0.0061(6) 0.0024(6) C19 0.0336(9) 0.0332(9) 0.0196(8) -0.0045(7) -0.0046(7) 0.0068(7) C20 0.0641(16) 0.0616(16) 0.0339(11) -0.0230(11) -0.0158(11) 0.0241(12) C22 0.0336(9) 0.0231(8) 0.0251(8) -0.0069(7) -0.0091(7) 0.0042(7) C21 0.087(2) 0.092(2) 0.0603(18) -0.0452(17) -0.0172(16) 0.0460(19) C23 0.0375(10) 0.0261(9) 0.0474(12) -0.0080(8) -0.0165(9) 0.0025(7) C24 0.0435(11) 0.0283(10) 0.0635(15) -0.0115(10) -0.0245(11) -0.0012(8) C25 0.0512(12) 0.0233(9) 0.0525(13) -0.0131(9) -0.0166(10) 0.0009(8) C26 0.0420(10) 0.0253(9) 0.0359(10) -0.0105(8) -0.0077(8) 0.0067(7) C27 0.0326(9) 0.0257(9) 0.0296(9) -0.0080(7) -0.0067(7) 0.0049(7) C28 0.0529(15) 0.0402(13) 0.106(2) -0.0149(14) -0.0393(16) -0.0065(11) C29 0.0505(16) 0.0462(15) 0.131(3) -0.0115(18) -0.0182(18) -0.0133(12) C30 0.090(3) 0.073(2) 0.122(3) -0.037(2) -0.059(2) -0.0101(19) C31 0.0465(15) 0.0537(16) 0.153(4) -0.019(2) -0.0489(19) -0.0014(12) C32 0.0274(8) 0.0191(7) 0.0196(7) 0.0017(6) -0.0021(6) 0.0014(6) C33 0.0291(8) 0.0253(8) 0.0272(9) 0.0013(7) -0.0040(7) 0.0036(6) C35 0.0431(10) 0.0181(8) 0.0349(10) 0.0026(7) 0.0002(8) 0.0019(7) C34 0.0369(10) 0.0233(9) 0.0347(10) 0.0011(7) -0.0048(8) 0.0079(7) C36 0.0329(9) 0.0198(8) 0.0353(10) 0.0003(7) 0.0031(7) -0.0033(7) C38 0.0364(10) 0.0246(9) 0.0592(14) -0.0065(9) 0.0056(9) -0.0082(8) C37 0.0276(8) 0.0196(8) 0.0293(9) 0.0003(7) -0.0011(7) 0.0011(6) C39 0.0300(10) 0.0370(12) 0.106(2) -0.0176(14) -0.0066(12) -0.0056(9) C40 0.0470(13) 0.0348(11) 0.0680(17) -0.0106(11) -0.0035(11) -0.0105(10) C41 0.0584(16) 0.0459(14) 0.0686(18) -0.0116(13) 0.0240(13) -0.0200(12) C42 0.0489(12) 0.0308(10) 0.0535(14) -0.0005(10) -0.0137(10) 0.0168(9) C43 0.0589(15) 0.0441(13) 0.0735(18) -0.0123(13) -0.0084(13) 0.0272(12) C44 0.0774(19) 0.0508(15) 0.0629(17) 0.0145(13) -0.0214(15) 0.0245(14) C45 0.0428(13) 0.0468(14) 0.084(2) -0.0043(13) -0.0215(13) 0.0188(11) C46 0.099(2) 0.083(2) 0.0309(13) -0.0228(13) -0.0087(14) 0.0161(18) C47 0.0573(14) 0.0474(13) 0.0279(10) -0.0094(9) 0.0025(9) 0.0047(11) C48 0.0221(7) 0.0201(7) 0.0205(7) -0.0051(6) -0.0034(6) 0.0008(6) C49 0.0225(7) 0.0169(7) 0.0252(8) -0.0037(6) -0.0028(6) 0.0034(5) C50 0.0184(7) 0.0177(7) 0.0212(7) 0.0004(6) -0.0021(5) 0.0027(5) C51 0.0167(6) 0.0169(7) 0.0195(7) -0.0015(6) -0.0014(5) 0.0002(5) C52 0.0188(6) 0.0155(7) 0.0214(7) -0.0015(6) -0.0020(5) 0.0001(5) C53 0.0178(6) 0.0160(7) 0.0199(7) 0.0002(6) -0.0024(5) -0.0007(5) C54 0.0227(7) 0.0227(8) 0.0314(9) -0.0031(7) -0.0052(6) 0.0039(6) C55 0.0290(9) 0.0395(11) 0.0419(11) 0.0090(9) -0.0108(8) 0.0033(8) C56 0.0208(7) 0.0160(7) 0.0197(7) -0.0001(6) -0.0036(5) 0.0004(5) C57 0.0210(7) 0.0162(7) 0.0201(7) -0.0016(6) -0.0039(5) 0.0013(5) C58 0.0277(8) 0.0214(8) 0.0187(7) 0.0021(6) -0.0027(6) -0.0025(6) C59 0.0480(12) 0.0347(10) 0.0288(10) 0.0094(8) -0.0134(8) -0.0101(9) C60 0.0638(17) 0.0626(17) 0.0491(15) 0.0313(13) -0.0084(12) -0.0221(13) C61 0.0263(7) 0.0164(7) 0.0203(7) 0.0010(6) -0.0036(6) 0.0003(6) C62 0.0261(8) 0.0200(8) 0.0333(9) -0.0022(7) -0.0077(7) 0.0013(6) C63 0.0293(8) 0.0211(8) 0.0388(10) -0.0027(7) -0.0105(7) 0.0045(6) C64 0.0345(9) 0.0166(8) 0.0358(10) -0.0001(7) -0.0069(7) 0.0019(6) C65 0.0304(8) 0.0183(8) 0.0301(9) 0.0008(7) -0.0037(7) -0.0020(6) C66 0.0261(8) 0.0191(8) 0.0253(8) 0.0003(6) -0.0038(6) -0.0007(6) C67 0.0344(10) 0.0268(9) 0.0605(14) -0.0088(9) -0.0174(9) 0.0100(8) C68 0.0315(11) 0.0423(13) 0.108(2) -0.0228(14) -0.0277(13) 0.0096(9) C69 0.0594(15) 0.0532(15) 0.0655(17) -0.0041(13) -0.0325(13) 0.0224(12) C70 0.0365(11) 0.0388(12) 0.0677(16) -0.0118(11) -0.0094(10) 0.0117(9) C71 0.0339(9) 0.0194(8) 0.0490(12) -0.0030(8) -0.0004(8) -0.0064(7) C72 0.0587(15) 0.0334(12) 0.0669(17) 0.0104(12) 0.0082(13) -0.0117(11) C73 0.0424(12) 0.0344(11) 0.0672(16) -0.0192(11) -0.0109(11) -0.0041(9) C74 0.0301(10) 0.0312(10) 0.0812(18) -0.0143(11) -0.0034(10) -0.0061(8) C75 0.0188(6) 0.0163(7) 0.0195(7) -0.0020(6) -0.0034(5) 0.0006(5) C76 0.0206(7) 0.0153(7) 0.0186(7) -0.0010(5) -0.0029(5) 0.0020(5) C77 0.0208(7) 0.0177(7) 0.0169(7) -0.0012(6) -0.0037(5) 0.0014(5) C78 0.0241(7) 0.0215(8) 0.0233(8) -0.0021(6) -0.0070(6) -0.0022(6) C79 0.0306(8) 0.0280(9) 0.0196(8) 0.0003(6) -0.0080(6) -0.0031(7) C80 0.0561(13) 0.0354(11) 0.0383(11) -0.0083(9) -0.0152(10) -0.0135(10) C81 0.0697(17) 0.0616(16) 0.0411(13) -0.0031(11) -0.0195(12) -0.0369(14) C82 0.0232(7) 0.0163(7) 0.0197(7) -0.0019(6) -0.0022(6) -0.0002(5) C83 0.0231(7) 0.0189(7) 0.0239(8) -0.0023(6) -0.0021(6) -0.0004(6) C84 0.0278(8) 0.0183(7) 0.0267(8) -0.0035(6) -0.0026(6) 0.0024(6) C85 0.0356(9) 0.0164(7) 0.0305(9) -0.0043(7) -0.0034(7) -0.0011(6) C86 0.0302(8) 0.0219(8) 0.0287(9) -0.0023(7) -0.0045(7) -0.0064(6) C87 0.0227(7) 0.0214(8) 0.0251(8) -0.0018(6) -0.0019(6) -0.0028(6) C88 0.0347(9) 0.0265(9) 0.0409(11) -0.0019(8) -0.0086(8) -0.0113(7) C89 0.0291(9) 0.0405(12) 0.0623(15) -0.0037(11) -0.0093(9) -0.0125(8) C90 0.0518(13) 0.0423(12) 0.0531(14) -0.0137(11) -0.0181(11) -0.0111(10) C91 0.0472(12) 0.0361(12) 0.0582(15) 0.0079(11) -0.0099(11) -0.0197(10) C92 0.0309(9) 0.0223(8) 0.0436(11) -0.0068(8) -0.0031(8) 0.0076(7) C93 0.0251(9) 0.0338(11) 0.0823(18) -0.0101(11) -0.0096(10) 0.0072(8) C94 0.0442(11) 0.0324(10) 0.0474(12) -0.0053(9) -0.0114(9) 0.0125(9) C95 0.0470(12) 0.0347(11) 0.0488(13) -0.0081(10) 0.0072(10) 0.0117(9) C97 0.0468(12) 0.0251(9) 0.0501(13) -0.0079(9) -0.0015(10) 0.0107(8) C98 0.0398(12) 0.0351(12) 0.086(2) 0.0007(12) -0.0046(12) 0.0132(9) C99 0.085(2) 0.0503(15) 0.0651(18) -0.0244(14) 0.0086(15) 0.0219(15) C100 0.0535(14) 0.0331(11) 0.0733(18) 0.0017(12) -0.0066(13) 0.0124(10) 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' Cl Cl 0.1484 0.1585 '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 Cl1 C01 Cl2 114.2(2) . . ? Cl3 C02 Cl4 113.18(13) . . ? C20 O2 C19 117.31(18) . . ? C2 O6 C3 118.76(15) . . ? C15 O8 C14 119.01(14) . . ? C11 O10 C10 120.13(18) . . ? C80 O11 C78 118.49(16) . . ? C59 O16 C58 117.21(15) . . ? C47 O17 C48 117.56(16) . . ? C54 O19 C50 117.36(13) . . ? O7 C2 O6 123.5(2) . . ? O7 C2 C1 127.1(2) . . ? O6 C2 C1 109.4(2) . . ? C4 C3 C5 122.52(16) . . ? C4 C3 O6 119.75(15) . . ? C5 C3 O6 117.58(15) . . ? C19 C4 C3 118.30(16) 2_766 . ? C96 C5 C3 116.83(15) . . ? C96 C5 C6 122.89(14) . . ? C3 C5 C6 120.27(14) . . ? C32 C6 C7 115.58(13) . . ? C32 C6 C5 111.13(14) . . ? C7 C6 C5 109.42(13) . . ? C14 C7 C8 117.63(15) . . ? C14 C7 C6 117.98(14) . . ? C8 C7 C6 124.31(15) . . ? C9 C8 C7 122.43(15) . . ? C8 C9 C10 116.71(15) . . ? C8 C9 C17 124.12(15) . . ? C10 C9 C17 119.16(15) . . ? C13 C10 C9 123.09(16) . . ? C13 C10 O10 117.58(15) . . ? C9 C10 O10 119.20(15) . . ? O1 C11 O10 121.2(3) . . ? O1 C11 C12 127.3(3) . . ? O10 C11 C12 111.2(3) . . ? C10 C13 C14 117.84(16) . . ? C13 C14 C7 122.17(15) . . ? C13 C14 O8 121.37(15) . . ? C7 C14 O8 116.38(15) . . ? O9 C15 O8 123.32(17) . . ? O9 C15 C16 126.47(18) . . ? O8 C15 C16 110.21(17) . . ? C18 C17 C9 111.79(13) . . ? C18 C17 C22 111.67(14) . . ? C9 C17 C22 115.73(14) . . ? C19 C18 C96 117.34(15) . 2_766 ? C19 C18 C17 120.14(15) . . ? C96 C18 C17 122.46(15) 2_766 . ? C4 C19 C18 122.14(16) 2_766 . ? C4 C19 O2 120.97(16) 2_766 . ? C18 C19 O2 116.84(15) . . ? O3 C20 O2 123.2(2) . . ? O3 C20 C21 127.0(3) . . ? O2 C20 C21 109.7(3) . . ? C23 C22 C27 118.36(17) . . ? C23 C22 C17 122.05(16) . . ? C27 C22 C17 119.33(16) . . ? C22 C23 C24 122.59(19) . . ? C25 C24 C23 117.04(19) . . ? C25 C24 C28 122.4(2) . . ? C23 C24 C28 120.5(2) . . ? O4 C25 C24 118.3(2) . . ? O4 C25 C26 119.23(19) . . ? C24 C25 C26 122.50(18) . . ? C27 C26 C25 116.96(18) . . ? C27 C26 C97 120.52(19) . . ? C25 C26 C97 122.51(18) . . ? C26 C27 C22 122.45(18) . . ? C31 C28 C29 108.1(3) . . ? C31 C28 C24 111.0(2) . . ? C29 C28 C24 111.1(2) . . ? C31 C28 C30 105.9(3) . . ? C29 C28 C30 110.6(3) . . ? C24 C28 C30 110.0(3) . . ? C37 C32 C33 119.02(16) . . ? C37 C32 C6 121.68(15) . . ? C33 C32 C6 119.22(15) . . ? C32 C33 C34 122.20(17) . . ? O5 C35 C34 116.32(18) . . ? O5 C35 C36 120.56(19) . . ? C34 C35 C36 123.12(17) . . ? C33 C34 C35 116.69(16) . . ? C33 C34 C42 120.66(19) . . ? C35 C34 C42 122.62(18) . . ? C37 C36 C35 116.62(17) . . ? C37 C36 C38 120.50(17) . . ? C35 C36 C38 122.88(17) . . ? C40 C38 C39 105.7(2) . . ? C40 C38 C36 110.27(18) . . ? C39 C38 C36 111.52(17) . . ? C40 C38 C41 111.24(19) . . ? C39 C38 C41 107.4(2) . . ? C36 C38 C41 110.6(2) . . ? C32 C37 C36 122.29(16) . . ? C45 C42 C44 107.4(2) . . ? C45 C42 C34 111.78(18) . . ? C44 C42 C34 109.9(2) . . ? C45 C42 C43 107.2(2) . . ? C44 C42 C43 110.3(2) . . ? C34 C42 C43 110.23(19) . . ? O18 C47 O17 122.2(2) . . ? O18 C47 C46 127.5(3) . . ? O17 C47 C46 110.3(2) . . ? C49 C48 C53 122.95(14) . . ? C49 C48 O17 118.47(14) . . ? C53 C48 O17 118.50(14) . . ? C48 C49 C50 117.87(14) . . ? C49 C50 C51 122.54(14) . . ? C49 C50 O19 121.02(14) . . ? C51 C50 O19 116.43(14) . . ? C50 C51 C52 117.23(14) . . ? C50 C51 C75 117.86(13) . . ? C52 C51 C75 124.91(13) . . ? C53 C52 C51 122.39(14) . . ? C48 C53 C52 116.99(14) . . ? C48 C53 C56 118.00(14) . . ? C52 C53 C56 125.00(13) . . ? O20 C54 O19 123.14(16) . . ? O20 C54 C55 126.13(17) . . ? O19 C54 C55 110.71(16) . . ? C57 C56 C53 110.81(13) . . ? C57 C56 C61 112.06(13) . . ? C53 C56 C61 115.42(13) . . ? C58 C57 C77 117.17(14) . 2_575 ? C58 C57 C56 120.56(14) . . ? C77 C57 C56 122.25(14) 2_575 . ? C79 C58 C57 122.39(16) 2_575 . ? C79 C58 O16 120.10(15) 2_575 . ? C57 C58 O16 117.48(14) . . ? O15 C59 O16 123.50(19) . . ? O15 C59 C60 126.3(2) . . ? O16 C59 C60 110.2(2) . . ? C62 C61 C66 118.63(15) . . ? C62 C61 C56 122.00(15) . . ? C66 C61 C56 119.16(14) . . ? C61 C62 C63 122.55(16) . . ? C62 C63 C64 116.96(16) . . ? C62 C63 C67 120.75(16) . . ? C64 C63 C67 122.24(16) . . ? O14 C64 C63 117.11(16) . . ? O14 C64 C65 120.15(16) . . ? C63 C64 C65 122.74(16) . . ? C66 C65 C64 116.90(16) . . ? C66 C65 C71 120.79(16) . . ? C64 C65 C71 122.32(16) . . ? C61 C66 C65 122.19(16) . . ? C68 C67 C70 107.3(2) . . ? C68 C67 C69 107.2(2) . . ? C70 C67 C69 110.39(19) . . ? C68 C67 C63 111.18(16) . . ? C70 C67 C63 111.22(18) . . ? C69 C67 C63 109.5(2) . . ? C74 C71 C72 107.2(2) . . ? C74 C71 C65 111.98(15) . . ? C72 C71 C65 110.57(19) . . ? C74 C71 C73 106.03(19) . . ? C72 C71 C73 110.73(19) . . ? C65 C71 C73 110.19(17) . . ? C82 C75 C51 115.09(13) . . ? C82 C75 C76 111.21(12) . . ? C51 C75 C76 111.36(12) . . ? C77 C76 C78 117.12(15) . . ? C77 C76 C75 123.30(14) . . ? C78 C76 C75 119.59(14) . . ? C76 C77 C57 122.63(14) . 2_575 ? C79 C78 C76 122.45(15) . . ? C79 C78 O11 119.93(14) . . ? C76 C78 O11 117.43(15) . . ? C78 C79 C58 118.19(15) . 2_575 ? O12 C80 O11 122.7(2) . . ? O12 C80 C81 126.9(2) . . ? O11 C80 C81 110.4(2) . . ? C83 C82 C87 118.72(15) . . ? C83 C82 C75 121.33(14) . . ? C87 C82 C75 119.91(14) . . ? C82 C83 C84 122.30(15) . . ? C83 C84 C85 116.86(15) . . ? C83 C84 C92 120.27(15) . . ? C85 C84 C92 122.87(15) . . ? O13 C85 C86 116.20(16) . . ? O13 C85 C84 120.90(16) . . ? C86 C85 C84 122.90(15) . . ? C87 C86 C85 116.60(15) . . ? C87 C86 C88 120.59(16) . . ? C85 C86 C88 122.80(16) . . ? C82 C87 C86 122.60(15) . . ? C90 C88 C89 107.43(18) . . ? C90 C88 C91 109.47(18) . . ? C89 C88 C91 106.07(19) . . ? C90 C88 C86 110.78(17) . . ? C89 C88 C86 111.92(16) . . ? C91 C88 C86 110.99(17) . . ? C93 C92 C95 106.76(19) . . ? C93 C92 C84 111.29(15) . . ? C95 C92 C84 111.14(17) . . ? C93 C92 C94 106.48(19) . . ? C95 C92 C94 111.29(16) . . ? C84 C92 C94 109.76(17) . . ? C18 C96 C5 122.78(15) 2_766 . ? C100 C97 C98 106.1(2) . . ? C100 C97 C99 111.0(2) . . ? C98 C97 C99 108.0(2) . . ? C100 C97 C26 110.50(19) . . ? C98 C97 C26 111.57(17) . . ? C99 C97 C26 109.6(2) . . ? 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 C01 Cl1 1.523(8) . ? C01 Cl2 1.962(8) . ? C02 Cl3 1.745(2) . ? C02 Cl4 1.748(2) . ? O1 C11 1.205(4) . ? O2 C20 1.370(3) . ? O2 C19 1.404(2) . ? O3 C20 1.194(4) . ? O4 C25 1.389(3) . ? O5 C35 1.386(2) . ? O6 C2 1.353(3) . ? O6 C3 1.397(2) . ? O7 C2 1.186(3) . ? O8 C15 1.371(2) . ? O8 C14 1.3978(19) . ? O9 C15 1.193(3) . ? O10 C11 1.309(3) . ? O10 C10 1.407(2) . ? O11 C80 1.365(3) . ? O11 C78 1.3991(19) . ? O12 C80 1.182(3) . ? O13 C85 1.382(2) . ? O14 C64 1.383(2) . ? O15 C59 1.197(3) . ? O16 C59 1.364(2) . ? O16 C58 1.404(2) . ? O17 C47 1.347(3) . ? O17 C48 1.4050(19) . ? O18 C47 1.193(3) . ? O19 C54 1.3708(19) . ? O19 C50 1.4020(19) . ? O20 C54 1.189(2) . ? C1 C2 1.493(3) . ? C3 C4 1.381(3) . ? C3 C5 1.392(2) . ? C4 C19 1.379(2) 2_766 ? C5 C96 1.392(2) . ? C5 C6 1.528(2) . ? C6 C32 1.518(2) . ? C6 C7 1.525(2) . ? C7 C14 1.392(2) . ? C7 C8 1.394(2) . ? C8 C9 1.394(2) . ? C9 C10 1.394(2) . ? C9 C17 1.522(2) . ? C10 C13 1.380(2) . ? C11 C12 1.497(4) . ? C13 C14 1.383(2) . ? C15 C16 1.496(3) . ? C17 C18 1.521(2) . ? C17 C22 1.524(2) . ? C18 C19 1.390(2) . ? C18 C96 1.391(2) 2_766 ? C19 C4 1.379(2) 2_766 ? C20 C21 1.496(4) . ? C22 C23 1.380(3) . ? C22 C27 1.392(2) . ? C23 C24 1.400(3) . ? C24 C25 1.396(3) . ? C24 C28 1.539(3) . ? C25 C26 1.415(3) . ? C26 C27 1.389(3) . ? C26 C97 1.546(3) . ? C28 C31 1.527(4) . ? C28 C29 1.530(5) . ? C28 C30 1.559(5) . ? C32 C37 1.378(2) . ? C32 C33 1.392(2) . ? C33 C34 1.394(3) . ? C35 C34 1.405(3) . ? C35 C36 1.408(3) . ? C34 C42 1.543(3) . ? C36 C37 1.399(2) . ? C36 C38 1.541(3) . ? C38 C40 1.535(3) . ? C38 C39 1.537(3) . ? C38 C41 1.543(4) . ? C42 C45 1.526(4) . ? C42 C44 1.539(4) . ? C42 C43 1.552(4) . ? C46 C47 1.496(3) . ? C48 C49 1.379(2) . ? C48 C53 1.395(2) . ? C49 C50 1.382(2) . ? C50 C51 1.396(2) . ? C51 C52 1.397(2) . ? C51 C75 1.522(2) . ? C52 C53 1.397(2) . ? C53 C56 1.523(2) . ? C54 C55 1.490(3) . ? C56 C57 1.518(2) . ? C56 C61 1.534(2) . ? C57 C58 1.387(2) . ? C57 C77 1.392(2) 2_575 ? C58 C79 1.383(2) 2_575 ? C59 C60 1.496(3) . ? C61 C62 1.383(2) . ? C61 C66 1.392(2) . ? C62 C63 1.399(2) . ? C63 C64 1.399(3) . ? C63 C67 1.543(3) . ? C64 C65 1.414(3) . ? C65 C66 1.397(2) . ? C65 C71 1.541(3) . ? C67 C68 1.531(3) . ? C67 C70 1.537(3) . ? C67 C69 1.541(4) . ? C71 C74 1.533(3) . ? C71 C72 1.541(3) . ? C71 C73 1.545(3) . ? C75 C82 1.520(2) . ? C75 C76 1.525(2) . ? C76 C77 1.391(2) . ? C76 C78 1.392(2) . ? C77 C57 1.392(2) 2_575 ? C78 C79 1.376(3) . ? C79 C58 1.383(2) 2_575 ? C80 C81 1.485(3) . ? C82 C83 1.386(2) . ? C82 C87 1.390(2) . ? C83 C84 1.393(2) . ? C84 C85 1.417(2) . ? C84 C92 1.540(2) . ? C85 C86 1.402(3) . ? C86 C87 1.397(2) . ? C86 C88 1.541(2) . ? C88 C90 1.534(3) . ? C88 C89 1.536(3) . ? C88 C91 1.538(3) . ? C92 C93 1.533(3) . ? C92 C95 1.537(3) . ? C92 C94 1.543(3) . ? C96 C18 1.391(2) 2_766 ? C97 C100 1.527(4) . ? C97 C98 1.533(4) . ? C97 C99 1.543(3) . ?