#------------------------------------------------------------------------------ #$Date: 2011-09-28 17:24:46 +0300 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/80/2018049.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2018049 loop_ _publ_author_name 'Beheshti, Azizolla' 'Clegg, William' 'Ebrahimi Filoori, Nahid' 'Russo, Luca' _publ_section_title ; Two polymorphs of tetraethylammonium [hydrogen tris(3,5-dimethylpyrazolyl)borato]di-\m~2~-sulfido-disulfido(\h^2^-tetrasulfido)ditungsten(V) with Z' = 1 and 2 ; _journal_coeditor_code BI3009 _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m149 _journal_page_last m153 _journal_volume 67 _journal_year 2011 _chemical_formula_iupac '(C8 H20 N) [W2 S4 (S)4 (C15 H22 B N6)]' _chemical_formula_moiety 'C8 H20 N +, C15 H22 B N6 S8 W2 -' _chemical_formula_sum 'C23 H42 B N7 S8 W2' _chemical_formula_weight 1051.63 _chemical_name_systematic ; tetraethylammonium [hydrogen tris(3,5-dimethylpyrazolyl)borato]di-\m~2~-sulfido-disulfido(\h^2^- tetrasulfido)ditungsten(V) ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.343(5) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 17.8602(10) _cell_length_b 18.8742(10) _cell_length_c 20.6188(10) _cell_measurement_reflns_used 6724 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 26.93 _cell_measurement_theta_min 2.96 _cell_volume 6950.4(6) _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction, 2009)' _computing_data_collection 'CrysAlisPro (Oxford Diffraction, 2009)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction, 2009)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and local programs' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 10.3968 _diffrn_measured_fraction_theta_full 0.868 _diffrn_measured_fraction_theta_max 0.735 _diffrn_measurement_device_type 'Oxford Diffraction Gemini A Ultra diffractometer' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator none _diffrn_radiation_source 'sealed tube with Enhance optics' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1194 _diffrn_reflns_av_sigmaI/netI 0.1575 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 23985 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 26.98 _diffrn_reflns_theta_min 3.14 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 7.124 _exptl_absorpt_correction_T_max 0.765 _exptl_absorpt_correction_T_min 0.120 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(CrysAlisPro; Oxford Diffraction, 2009)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 2.010 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 4080 _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.04 _refine_diff_density_max 3.815 _refine_diff_density_min -2.257 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 759 _refine_ls_number_reflns 11129 _refine_ls_number_restraints 760 _refine_ls_restrained_S_all 0.962 _refine_ls_R_factor_all 0.1375 _refine_ls_R_factor_gt 0.0662 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0768P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1475 _refine_ls_wR_factor_ref 0.1711 _reflns_number_gt 6168 _reflns_number_total 11129 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bi3009.cif _[local]_cod_data_source_block 2 _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_database_code 2018049 _iucr_refine_instruction_details ; TITL ab89 in P2(1)/n CELL 0.71073 17.8602 18.8742 20.6188 90.000 90.343 90.000 ZERR 8.00 0.0010 0.0010 0.0010 0.000 0.005 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H S W N B UNIT 184 336 64 16 56 8 TEMP -123 ACTA CONF REM EXTI 0.000210 SIZE 0.52 0.38 0.04 FREE W1 W2 FREE W3 W4 L.S. 8 BOND $H FMAP 2 PLAN 10 SIMU DELU rem ISOR 0.01 WGHT 0.076800 FVAR 0.20839 W1 4 0.668776 0.284555 0.137329 11.00000 0.01941 0.02727 = 0.02489 -0.00076 -0.00330 0.00079 W2 4 0.776771 0.321348 0.234533 11.00000 0.02035 0.03094 = 0.04039 -0.00743 -0.00854 0.00164 W3 4 0.337820 0.525814 0.326666 11.00000 0.01930 0.03503 = 0.03161 -0.00369 -0.00677 0.00051 W4 4 0.223273 0.504030 0.232269 11.00000 0.02099 0.04185 = 0.03106 -0.00318 -0.00454 -0.00268 S1 3 0.745982 0.275687 0.058490 11.00000 0.03786 0.04831 = 0.03745 0.00163 0.00845 0.00933 S2 3 0.695879 0.395867 0.178260 11.00000 0.03310 0.02395 = 0.04759 -0.00111 -0.00854 -0.00143 S3 3 0.719001 0.212157 0.217288 11.00000 0.03208 0.02927 = 0.02911 -0.00193 -0.00726 0.00871 S4 3 0.867386 0.320545 0.190657 11.00000 0.08247 0.11299 = 0.15097 -0.02431 0.02289 -0.00214 S5 3 0.795894 0.258112 0.336973 11.00000 0.06399 0.05994 = 0.05357 -0.01095 -0.03220 0.02439 S6 3 0.805818 0.326110 0.414703 11.00000 0.12647 0.07841 = 0.07892 -0.02714 -0.04254 0.02263 S7 3 0.858754 0.406554 0.374301 11.00000 0.09833 0.06681 = 0.10916 -0.02592 -0.05868 0.02497 S8 3 0.786375 0.428494 0.298817 11.00000 0.04003 0.04212 = 0.07529 -0.01468 -0.02182 -0.00316 S11 3 0.263601 0.535274 0.406329 11.00000 0.02848 0.05671 = 0.04151 -0.01151 -0.00860 0.00351 S12 3 0.299349 0.418891 0.280917 11.00000 0.03077 0.03667 = 0.03601 -0.00136 -0.00399 -0.00096 S13 3 0.293170 0.605786 0.250527 11.00000 0.03243 0.03480 = 0.04562 -0.00143 -0.01416 0.00219 S14 3 0.133165 0.515226 0.283240 11.00000 0.07163 0.13688 = 0.08430 -0.01056 0.00642 -0.00985 S15 3 0.199926 0.565262 0.131830 11.00000 0.04469 0.10795 = 0.05084 0.02167 -0.00886 0.00779 S16 3 0.168139 0.508474 0.057396 11.00000 0.13359 0.18961 = 0.08074 -0.00720 -0.02300 -0.01562 S17 3 0.122467 0.434873 0.101949 11.00000 0.26345 0.08898 = 0.05043 -0.01536 -0.02084 0.03315 S18 3 0.202183 0.402826 0.165232 11.00000 0.07039 0.08940 = 0.06228 -0.02056 -0.00652 -0.02571 N1 5 0.533273 0.185175 0.093392 11.00000 0.03087 0.03009 = 0.02519 -0.00632 -0.01407 -0.00291 N2 5 0.608152 0.184475 0.106726 11.00000 0.03714 0.02958 = 0.03805 -0.00691 -0.01780 0.00693 N3 5 0.510832 0.310916 0.065816 11.00000 0.03888 0.03203 = 0.04289 -0.00034 -0.01216 0.00595 N4 5 0.585096 0.338670 0.072432 11.00000 0.03307 0.03347 = 0.03859 0.00352 -0.00872 0.00911 N5 5 0.491802 0.268858 0.175281 11.00000 0.01666 0.03328 = 0.03627 -0.01040 -0.00311 0.00279 N6 5 0.560846 0.289456 0.200014 11.00000 0.01147 0.04476 = 0.02568 -0.00300 -0.00603 -0.00573 N11 5 0.479669 0.618679 0.369463 11.00000 0.02400 0.03058 = 0.04519 0.00105 -0.01349 0.00417 N12 5 0.403164 0.618938 0.363696 11.00000 0.02915 0.03737 = 0.04759 -0.01245 -0.01690 0.00502 N13 5 0.493333 0.487467 0.393020 11.00000 0.01970 0.02726 = 0.03445 -0.00560 -0.00312 0.01127 N14 5 0.419508 0.464693 0.383457 11.00000 0.02437 0.04496 = 0.03157 0.00003 -0.00895 0.00402 N15 5 0.513194 0.535234 0.282924 11.00000 0.01518 0.02497 = 0.04170 0.00918 -0.00062 0.00619 N16 5 0.444011 0.516075 0.258777 11.00000 0.02048 0.04885 = 0.03240 -0.00687 -0.00572 -0.00312 C1 1 0.637439 0.120502 0.092873 11.00000 0.04479 0.03211 = 0.01913 -0.00784 -0.00781 0.00468 C2 1 0.573544 0.077669 0.076412 11.00000 0.05053 0.02291 = 0.04450 0.00354 -0.01509 -0.00413 AFIX 43 H2 2 0.574422 0.028173 0.068086 11.00000 -1.20000 AFIX 0 C3 1 0.510804 0.120150 0.074683 11.00000 0.03985 0.03811 = 0.02242 -0.01543 -0.00200 -0.00523 C4 1 0.715732 0.098070 0.097472 11.00000 0.04220 0.03594 = 0.03155 -0.01182 -0.00442 0.00612 AFIX 137 H4A 2 0.748477 0.139112 0.091077 11.00000 -1.50000 H4B 2 0.725892 0.062520 0.064020 11.00000 -1.50000 H4C 2 0.725251 0.077558 0.140399 11.00000 -1.50000 AFIX 0 C5 1 0.433566 0.098737 0.061334 11.00000 0.04661 0.04772 = 0.05230 -0.02536 -0.01809 -0.00820 AFIX 137 H5A 2 0.411352 0.130927 0.029273 11.00000 -1.50000 H5B 2 0.404577 0.100659 0.101501 11.00000 -1.50000 H5C 2 0.432994 0.050273 0.044282 11.00000 -1.50000 AFIX 0 C6 1 0.591137 0.395572 0.032087 11.00000 0.03923 0.03875 = 0.04177 0.00217 -0.00117 0.01787 C7 1 0.525204 0.403540 -0.000109 11.00000 0.05555 0.03417 = 0.03874 0.00234 -0.01219 0.01734 AFIX 43 H7 2 0.515453 0.437727 -0.032903 11.00000 -1.20000 AFIX 0 C8 1 0.475128 0.354776 0.021989 11.00000 0.04538 0.03704 = 0.02623 -0.00879 -0.01225 0.01436 C9 1 0.659282 0.435229 0.023513 11.00000 0.05862 0.05032 = 0.02586 0.00825 0.01233 0.00687 AFIX 137 H9A 2 0.669379 0.463462 0.062484 11.00000 -1.50000 H9B 2 0.653894 0.466764 -0.013984 11.00000 -1.50000 H9C 2 0.700931 0.402437 0.016206 11.00000 -1.50000 AFIX 0 C10 1 0.396949 0.340087 0.003960 11.00000 0.05451 0.05782 = 0.05640 -0.00787 -0.02630 0.00849 AFIX 137 H10A 2 0.379811 0.375307 -0.027740 11.00000 -1.50000 H10B 2 0.365508 0.342526 0.042685 11.00000 -1.50000 H10C 2 0.393381 0.292630 -0.015093 11.00000 -1.50000 AFIX 0 C11 1 0.546696 0.310534 0.263379 11.00000 0.03316 0.03414 = 0.03228 -0.00211 -0.00090 -0.00096 C12 1 0.472063 0.300020 0.277466 11.00000 0.03664 0.04799 = 0.04287 -0.02012 0.01715 -0.00200 AFIX 43 H12 2 0.448657 0.310226 0.317650 11.00000 -1.20000 AFIX 0 C13 1 0.437722 0.272562 0.224041 11.00000 0.02506 0.04849 = 0.05026 -0.01248 0.01200 -0.01600 C14 1 0.602028 0.340079 0.311090 11.00000 0.04301 0.04658 = 0.03481 -0.02783 0.00965 -0.00514 AFIX 137 H14A 2 0.643230 0.306377 0.317097 11.00000 -1.50000 H14B 2 0.577236 0.348170 0.352711 11.00000 -1.50000 H14C 2 0.621819 0.385020 0.294676 11.00000 -1.50000 AFIX 0 C15 1 0.359469 0.250988 0.209544 11.00000 0.02347 0.04939 = 0.06347 -0.02211 0.01441 -0.00331 AFIX 137 H15A 2 0.332913 0.242318 0.250234 11.00000 -1.50000 H15B 2 0.359666 0.207575 0.183472 11.00000 -1.50000 H15C 2 0.334165 0.288828 0.185354 11.00000 -1.50000 AFIX 0 SAME N17 > C53 SAME N7 C18 > C23 C16 C17 SAME N7 C22 C23 C20 C21 C18 C19 C16 C17 N7 5 0.569575 0.101446 0.379128 11.00000 0.07126 0.15317 = 0.07340 0.03343 -0.01301 -0.03346 C16 1 0.519690 0.088860 0.321151 11.00000 0.13099 0.21080 = 0.07909 0.04345 -0.03454 -0.04602 AFIX 23 H16A 2 0.495418 0.042218 0.327386 11.00000 -1.20000 H16B 2 0.479476 0.124919 0.322531 11.00000 -1.20000 AFIX 0 C17 1 0.550557 0.089609 0.254805 11.00000 0.17587 0.10724 = 0.08864 -0.01829 -0.01037 0.00806 AFIX 137 H17A 2 0.552389 0.138479 0.238837 11.00000 -1.50000 H17B 2 0.518530 0.061176 0.226142 11.00000 -1.50000 H17C 2 0.601219 0.069667 0.255446 11.00000 -1.50000 AFIX 0 C18 1 0.606226 0.173301 0.376895 11.00000 0.12119 0.14328 = 0.09238 0.02149 0.01053 -0.02655 AFIX 23 H18A 2 0.639770 0.174424 0.338858 11.00000 -1.20000 H18B 2 0.566596 0.209086 0.369340 11.00000 -1.20000 AFIX 0 C19 1 0.650900 0.195853 0.435379 11.00000 0.15317 0.15087 = 0.15817 0.00831 -0.02693 -0.06283 AFIX 137 H19A 2 0.616848 0.206475 0.471182 11.00000 -1.50000 H19B 2 0.680069 0.238248 0.424826 11.00000 -1.50000 H19C 2 0.684903 0.157534 0.448252 11.00000 -1.50000 AFIX 0 C20 1 0.518099 0.098388 0.438019 11.00000 0.07749 0.13803 = 0.09433 -0.00787 0.00368 -0.02655 AFIX 23 H20A 2 0.488880 0.053866 0.435900 11.00000 -1.20000 H20B 2 0.549560 0.096379 0.477671 11.00000 -1.20000 AFIX 0 C21 1 0.464350 0.159331 0.444398 11.00000 0.10179 0.10760 = 0.21199 -0.01486 0.01204 -0.02919 AFIX 137 H21A 2 0.489097 0.198569 0.467098 11.00000 -1.50000 H21B 2 0.420493 0.144086 0.469094 11.00000 -1.50000 H21C 2 0.448448 0.175038 0.401157 11.00000 -1.50000 AFIX 0 C22 1 0.627915 0.044397 0.382027 11.00000 0.11187 0.14437 = 0.08239 -0.03966 -0.01113 -0.00525 AFIX 23 H22A 2 0.663834 0.056703 0.417005 11.00000 -1.20000 H22B 2 0.655833 0.045234 0.340699 11.00000 -1.20000 AFIX 0 C23 1 0.601640 -0.030411 0.393385 11.00000 0.10392 0.13545 = 0.21809 -0.08297 0.04578 -0.01129 AFIX 137 H23A 2 0.570531 -0.031921 0.432352 11.00000 -1.50000 H23B 2 0.645094 -0.061505 0.399281 11.00000 -1.50000 H23C 2 0.572204 -0.046466 0.355910 11.00000 -1.50000 AFIX 0 C31 1 0.380504 0.686247 0.381404 11.00000 0.03431 0.03997 = 0.05795 -0.01195 -0.00305 0.00571 C32 1 0.443529 0.724470 0.400104 11.00000 0.03573 0.03659 = 0.03752 -0.00576 -0.01803 0.00174 AFIX 43 H32 2 0.444591 0.771761 0.415859 11.00000 -1.20000 AFIX 0 C33 1 0.503067 0.681263 0.391517 11.00000 0.03604 0.03613 = 0.04916 -0.00094 -0.02000 -0.00069 C34 1 0.300517 0.707005 0.386927 11.00000 0.03170 0.04696 = 0.08761 -0.01815 -0.03015 0.01362 AFIX 137 H34A 2 0.285939 0.735279 0.349040 11.00000 -1.50000 H34B 2 0.293533 0.735077 0.426415 11.00000 -1.50000 H34C 2 0.269340 0.664346 0.388969 11.00000 -1.50000 AFIX 0 C35 1 0.584676 0.698077 0.403094 11.00000 0.02835 0.05481 = 0.04172 -0.00873 0.00611 -0.01167 AFIX 137 H35A 2 0.603783 0.669039 0.438951 11.00000 -1.50000 H35B 2 0.590051 0.748337 0.414107 11.00000 -1.50000 H35C 2 0.613183 0.687771 0.363741 11.00000 -1.50000 AFIX 0 C36 1 0.413672 0.404694 0.421936 11.00000 0.02553 0.03295 = 0.02538 -0.00951 0.00061 0.00880 C37 1 0.481044 0.392757 0.452654 11.00000 0.02439 0.02838 = 0.02887 -0.00454 -0.00083 0.01566 AFIX 43 H37 2 0.492013 0.355053 0.481719 11.00000 -1.20000 AFIX 0 C38 1 0.529136 0.444609 0.433956 11.00000 0.02446 0.01801 = 0.04180 -0.00992 -0.00681 0.01015 C39 1 0.342341 0.365168 0.429948 11.00000 0.03240 0.06190 = 0.04731 0.00225 -0.00182 -0.00506 AFIX 137 H39A 2 0.305098 0.396047 0.450234 11.00000 -1.50000 H39B 2 0.351009 0.323641 0.457518 11.00000 -1.50000 H39C 2 0.323885 0.349756 0.387373 11.00000 -1.50000 AFIX 0 C40 1 0.611349 0.454381 0.452541 11.00000 0.03197 0.05386 = 0.03686 -0.01509 -0.02404 0.01117 AFIX 137 H40A 2 0.626326 0.417164 0.483117 11.00000 -1.50000 H40B 2 0.618212 0.500869 0.472893 11.00000 -1.50000 H40C 2 0.642289 0.451382 0.413544 11.00000 -1.50000 AFIX 0 C41 1 0.453797 0.500569 0.195078 11.00000 0.02218 0.04447 = 0.03083 0.00476 -0.00343 0.00610 C42 1 0.530207 0.510371 0.178824 11.00000 0.02672 0.02864 = 0.03850 0.01180 -0.00068 -0.00644 AFIX 43 H42 2 0.553160 0.501858 0.138116 11.00000 -1.20000 AFIX 0 C43 1 0.563746 0.534727 0.234394 11.00000 0.02316 0.03531 = 0.03566 0.00532 0.00337 -0.00100 C44 1 0.394947 0.475371 0.148458 11.00000 0.02214 0.07181 = 0.01982 0.00245 0.00103 0.00444 AFIX 137 H44A 2 0.382182 0.426025 0.158212 11.00000 -1.50000 H44B 2 0.413989 0.478608 0.104080 11.00000 -1.50000 H44C 2 0.350159 0.504989 0.152576 11.00000 -1.50000 AFIX 0 C45 1 0.644626 0.556378 0.245566 11.00000 0.01356 0.02763 = 0.05421 -0.01689 0.00669 0.00437 AFIX 137 H45A 2 0.646611 0.606268 0.258634 11.00000 -1.50000 H45B 2 0.672904 0.549947 0.205409 11.00000 -1.50000 H45C 2 0.666594 0.526903 0.279870 11.00000 -1.50000 AFIX 0 N17 5 0.074970 0.296921 0.341682 11.00000 0.03791 0.06401 = 0.04273 0.00097 0.00202 -0.01617 C46 1 0.143815 0.251659 0.347915 11.00000 0.07228 0.06094 = 0.05341 -0.01659 0.00021 0.00804 AFIX 23 H46A 2 0.147016 0.221612 0.308674 11.00000 -1.20000 H46B 2 0.187948 0.283395 0.347842 11.00000 -1.20000 AFIX 0 C47 1 0.149985 0.204645 0.405563 11.00000 0.18977 0.09467 = 0.14493 0.04647 -0.05154 0.01504 AFIX 137 H47A 2 0.102901 0.205777 0.429705 11.00000 -1.50000 H47B 2 0.190938 0.221122 0.433581 11.00000 -1.50000 H47C 2 0.160181 0.156048 0.391398 11.00000 -1.50000 AFIX 0 C48 1 0.080208 0.337224 0.278640 11.00000 0.08154 0.07642 = 0.06605 0.03274 0.00763 -0.02226 AFIX 23 H48A 2 0.127770 0.364146 0.279764 11.00000 -1.20000 H48B 2 0.084740 0.301796 0.243474 11.00000 -1.20000 AFIX 0 C49 1 0.020053 0.387634 0.259155 11.00000 0.05088 0.16319 = 0.12339 0.06926 -0.04035 -0.02662 AFIX 137 H49A 2 -0.021677 0.361350 0.239609 11.00000 -1.50000 H49B 2 0.039857 0.421487 0.227564 11.00000 -1.50000 H49C 2 0.002374 0.413253 0.297464 11.00000 -1.50000 AFIX 0 C50 1 0.004852 0.251452 0.339598 11.00000 0.07109 0.06788 = 0.07081 -0.00625 0.02039 -0.03996 AFIX 23 H50A 2 0.001798 0.224562 0.380723 11.00000 -1.20000 H50B 2 -0.039242 0.283172 0.337491 11.00000 -1.20000 AFIX 0 C51 1 -0.000104 0.200053 0.284444 11.00000 0.09720 0.03587 = 0.11142 -0.01633 0.01113 -0.02636 AFIX 137 H51A 2 0.010113 0.224760 0.243641 11.00000 -1.50000 H51B 2 -0.050476 0.179519 0.282758 11.00000 -1.50000 H51C 2 0.036806 0.162233 0.290828 11.00000 -1.50000 AFIX 0 C52 1 0.067863 0.347409 0.399012 11.00000 0.05680 0.06071 = 0.07611 -0.02097 0.00819 -0.00386 AFIX 23 H52A 2 0.025472 0.379894 0.390255 11.00000 -1.20000 H52B 2 0.054945 0.319244 0.437874 11.00000 -1.20000 AFIX 0 C53 1 0.135842 0.391400 0.414795 11.00000 0.09218 0.06672 = 0.09308 0.00331 -0.02994 -0.02408 AFIX 137 H53A 2 0.175418 0.360779 0.432268 11.00000 -1.50000 H53B 2 0.122738 0.427357 0.447081 11.00000 -1.50000 H53C 2 0.153638 0.414710 0.375313 11.00000 -1.50000 AFIX 0 B1 6 0.486417 0.248956 0.104330 11.00000 0.02341 0.03495 = 0.03510 -0.00831 -0.01276 -0.00089 AFIX 13 H1 2 0.433155 0.237654 0.093250 11.00000 -1.50000 AFIX 0 B11 6 0.523049 0.551754 0.353277 11.00000 0.01611 0.03484 = 0.04366 -0.00370 -0.00505 0.00167 AFIX 13 H11 2 0.577384 0.559143 0.363118 11.00000 -1.50000 HKLF 4 1 1 0 0 0 -1 0 0 0 -1 REM ab89 in P2(1)/n REM R1 = 0.0662 for 6168 Fo > 4sig(Fo) and 0.1375 for all 11129 data REM 759 parameters refined using 760 restraints END WGHT 0.0772 0.0000 REM Highest difference peak 3.815, deepest hole -2.257, 1-sigma level 0.253 Q1 1 0.1769 0.4569 0.1019 11.00000 0.05 3.82 Q2 1 0.6332 0.2829 0.1717 11.00000 0.05 1.94 Q3 1 0.2989 0.5288 0.3639 11.00000 0.05 1.77 Q4 1 0.7048 0.2852 0.0997 11.00000 0.05 1.76 Q5 1 0.1814 0.5033 0.2664 11.00000 0.05 1.59 Q6 1 0.2167 0.4374 0.0509 11.00000 0.05 1.59 Q7 1 0.7357 0.3228 0.2672 11.00000 0.05 1.58 Q8 1 0.2680 0.4993 0.1990 11.00000 0.05 1.52 Q9 1 0.3762 0.5295 0.2956 11.00000 0.05 1.48 Q10 1 0.0982 0.4488 0.0899 11.00000 0.05 1.44 ; loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group W W1 0.66878(4) 0.28456(4) 0.13733(3) 0.0239(2) Uani d U 1 . . W W2 0.77677(4) 0.32135(4) 0.23453(4) 0.0306(2) Uani d U 1 . . W W3 0.33782(4) 0.52581(4) 0.32667(4) 0.0287(2) Uani d U 1 . . W W4 0.22327(4) 0.50403(4) 0.23227(4) 0.0313(2) Uani d U 1 . . S S1 0.7460(3) 0.2757(3) 0.0585(2) 0.0412(12) Uani d U 1 . . S S2 0.6959(3) 0.3959(2) 0.1783(2) 0.0349(11) Uani d U 1 . . S S3 0.7190(2) 0.2122(2) 0.2173(2) 0.0302(10) Uani d U 1 . . S S4 0.8674(5) 0.3205(6) 0.1907(5) 0.115(3) Uani d U 1 . . S S5 0.7959(3) 0.2581(3) 0.3370(3) 0.0593(16) Uani d U 1 . . S S6 0.8058(5) 0.3261(4) 0.4147(4) 0.095(3) Uani d U 1 . . S S7 0.8588(4) 0.4066(4) 0.3743(4) 0.092(3) Uani d U 1 . . S S8 0.7864(3) 0.4285(3) 0.2988(3) 0.0526(15) Uani d U 1 . . S S11 0.2636(3) 0.5353(3) 0.4063(2) 0.0423(12) Uani d U 1 . . S S12 0.2993(3) 0.4189(3) 0.2809(2) 0.0345(11) Uani d U 1 . . S S13 0.2932(3) 0.6058(3) 0.2505(2) 0.0377(12) Uani d U 1 . . S S14 0.1332(4) 0.5152(5) 0.2832(4) 0.098(2) Uani d U 1 . . S S15 0.1999(3) 0.5653(4) 0.1318(3) 0.0679(17) Uani d U 1 . . S S16 0.1681(6) 0.5085(7) 0.0574(5) 0.135(4) Uani d U 1 . . S S17 0.1225(8) 0.4349(5) 0.1019(4) 0.134(4) Uani d U 1 . . S S18 0.2022(4) 0.4028(4) 0.1652(3) 0.0741(19) Uani d U 1 . . N N1 0.5333(8) 0.1852(7) 0.0934(7) 0.029(3) Uani d U 1 . . N N2 0.6082(8) 0.1845(8) 0.1067(7) 0.035(3) Uani d U 1 . . N N3 0.5108(9) 0.3109(8) 0.0658(8) 0.038(3) Uani d U 1 . . N N4 0.5851(8) 0.3387(8) 0.0724(7) 0.035(3) Uani d U 1 . . N N5 0.4918(7) 0.2689(8) 0.1753(7) 0.029(3) Uani d U 1 . . N N6 0.5608(7) 0.2895(8) 0.2000(7) 0.027(3) Uani d U 1 . . N N11 0.4797(8) 0.6187(8) 0.3695(7) 0.033(3) Uani d U 1 . . N N12 0.4032(8) 0.6189(8) 0.3637(8) 0.038(3) Uani d U 1 . . N N13 0.4933(7) 0.4875(7) 0.3930(7) 0.027(3) Uani d U 1 . . N N14 0.4195(8) 0.4647(8) 0.3835(7) 0.034(3) Uani d U 1 . . N N15 0.5132(7) 0.5352(7) 0.2829(7) 0.027(3) Uani d U 1 . . N N16 0.4440(8) 0.5161(8) 0.2588(7) 0.034(3) Uani d U 1 . . C C1 0.6374(10) 0.1205(10) 0.0929(8) 0.032(4) Uani d U 1 . . C C2 0.5735(11) 0.0777(10) 0.0764(9) 0.039(4) Uani d U 1 . . H H2 0.5744 0.0282 0.0681 0.047 Uiso calc R 1 . . C C3 0.5108(10) 0.1201(10) 0.0747(8) 0.033(4) Uani d U 1 . . C C4 0.7157(10) 0.0981(10) 0.0975(9) 0.037(4) Uani d U 1 . . H H4A 0.7485 0.1391 0.0911 0.055 Uiso calc R 1 . . H H4B 0.7259 0.0625 0.0640 0.055 Uiso calc R 1 . . H H4C 0.7253 0.0776 0.1404 0.055 Uiso calc R 1 . . C C5 0.4336(11) 0.0987(11) 0.0613(10) 0.049(5) Uani d U 1 . . H H5A 0.4114 0.1309 0.0293 0.073 Uiso calc R 1 . . H H5B 0.4046 0.1007 0.1015 0.073 Uiso calc R 1 . . H H5C 0.4330 0.0503 0.0443 0.073 Uiso calc R 1 . . C C6 0.5911(11) 0.3956(10) 0.0321(9) 0.040(4) Uani d U 1 . . C C7 0.5252(11) 0.4035(10) -0.0001(9) 0.043(4) Uani d U 1 . . H H7 0.5155 0.4377 -0.0329 0.051 Uiso calc R 1 . . C C8 0.4751(11) 0.3548(10) 0.0220(9) 0.036(4) Uani d U 1 . . C C9 0.6593(11) 0.4352(11) 0.0235(9) 0.045(5) Uani d U 1 . . H H9A 0.6694 0.4635 0.0625 0.067 Uiso calc R 1 . . H H9B 0.6539 0.4668 -0.0140 0.067 Uiso calc R 1 . . H H9C 0.7009 0.4024 0.0162 0.067 Uiso calc R 1 . . C C10 0.3969(12) 0.3401(12) 0.0040(11) 0.056(6) Uani d U 1 . . H H10A 0.3798 0.3753 -0.0277 0.085 Uiso calc R 1 . . H H10B 0.3655 0.3425 0.0427 0.085 Uiso calc R 1 . . H H10C 0.3934 0.2926 -0.0151 0.085 Uiso calc R 1 . . C C11 0.5467(10) 0.3105(10) 0.2634(9) 0.033(4) Uani d U 1 . . C C12 0.4721(11) 0.3000(10) 0.2775(10) 0.042(4) Uani d U 1 . . H H12 0.4487 0.3102 0.3176 0.051 Uiso calc R 1 . . C C13 0.4377(10) 0.2726(11) 0.2240(10) 0.041(4) Uani d U 1 . . C C14 0.6020(11) 0.3401(11) 0.3111(9) 0.041(5) Uani d U 1 . . H H14A 0.6432 0.3064 0.3171 0.062 Uiso calc R 1 . . H H14B 0.5772 0.3482 0.3527 0.062 Uiso calc R 1 . . H H14C 0.6218 0.3850 0.2947 0.062 Uiso calc R 1 . . C C15 0.3595(9) 0.2510(11) 0.2095(10) 0.045(5) Uani d U 1 . . H H15A 0.3329 0.2423 0.2502 0.068 Uiso calc R 1 . . H H15B 0.3597 0.2076 0.1835 0.068 Uiso calc R 1 . . H H15C 0.3342 0.2888 0.1854 0.068 Uiso calc R 1 . . N N7 0.5696(9) 0.1014(10) 0.3791(7) 0.099(6) Uani d DU 1 . . C C16 0.5197(14) 0.0889(19) 0.3212(10) 0.140(10) Uani d DU 1 . . H H16A 0.4954 0.0422 0.3274 0.169 Uiso calc R 1 . . H H16B 0.4795 0.1249 0.3225 0.169 Uiso calc R 1 . . C C17 0.5506(19) 0.0896(19) 0.2548(11) 0.124(12) Uani d DU 1 . . H H17A 0.5524 0.1385 0.2388 0.186 Uiso calc R 1 . . H H17B 0.5185 0.0612 0.2261 0.186 Uiso calc R 1 . . H H17C 0.6012 0.0697 0.2554 0.186 Uiso calc R 1 . . C C18 0.6062(17) 0.1733(13) 0.3769(12) 0.119(9) Uani d DU 1 . . H H18A 0.6398 0.1744 0.3389 0.143 Uiso calc R 1 . . H H18B 0.5666 0.2091 0.3693 0.143 Uiso calc R 1 . . C C19 0.651(2) 0.1959(19) 0.4354(17) 0.154(16) Uani d DU 1 . . H H19A 0.6168 0.2065 0.4712 0.231 Uiso calc R 1 . . H H19B 0.6801 0.2382 0.4248 0.231 Uiso calc R 1 . . H H19C 0.6849 0.1575 0.4483 0.231 Uiso calc R 1 . . C C20 0.5181(13) 0.0984(14) 0.4380(11) 0.103(8) Uani d DU 1 . . H H20A 0.4889 0.0539 0.4359 0.124 Uiso calc R 1 . . H H20B 0.5496 0.0964 0.4777 0.124 Uiso calc R 1 . . C C21 0.4644(16) 0.1593(16) 0.4444(18) 0.140(13) Uani d DU 1 . . H H21A 0.4891 0.1986 0.4671 0.211 Uiso calc R 1 . . H H21B 0.4205 0.1441 0.4691 0.211 Uiso calc R 1 . . H H21C 0.4484 0.1750 0.4012 0.211 Uiso calc R 1 . . C C22 0.6279(13) 0.0444(13) 0.3820(13) 0.113(8) Uani d DU 1 . . H H22A 0.6638 0.0567 0.4170 0.136 Uiso calc R 1 . . H H22B 0.6558 0.0452 0.3407 0.136 Uiso calc R 1 . . C C23 0.6016(19) -0.0304(14) 0.393(2) 0.152(14) Uani d DU 1 . . H H23A 0.5705 -0.0319 0.4324 0.228 Uiso calc R 1 . . H H23B 0.6451 -0.0615 0.3993 0.228 Uiso calc R 1 . . H H23C 0.5722 -0.0465 0.3559 0.228 Uiso calc R 1 . . C C31 0.3805(11) 0.6862(11) 0.3814(10) 0.044(4) Uani d U 1 . . C C32 0.4435(10) 0.7245(10) 0.4001(9) 0.037(4) Uani d U 1 . . H H32 0.4446 0.7718 0.4159 0.044 Uiso calc R 1 . . C C33 0.5031(11) 0.6813(10) 0.3915(10) 0.041(4) Uani d U 1 . . C C34 0.3005(10) 0.7070(11) 0.3869(12) 0.056(6) Uani d U 1 . . H H34A 0.2859 0.7353 0.3490 0.083 Uiso calc R 1 . . H H34B 0.2935 0.7351 0.4264 0.083 Uiso calc R 1 . . H H34C 0.2693 0.6643 0.3890 0.083 Uiso calc R 1 . . C C35 0.5847(10) 0.6981(11) 0.4031(9) 0.042(5) Uani d U 1 . . H H35A 0.6038 0.6690 0.4390 0.062 Uiso calc R 1 . . H H35B 0.5901 0.7483 0.4141 0.062 Uiso calc R 1 . . H H35C 0.6132 0.6878 0.3637 0.062 Uiso calc R 1 . . C C36 0.4137(9) 0.4047(9) 0.4219(8) 0.028(3) Uani d U 1 . . C C37 0.4810(9) 0.3928(9) 0.4527(8) 0.027(3) Uani d U 1 . . H H37 0.4920 0.3551 0.4817 0.033 Uiso calc R 1 . . C C38 0.5291(9) 0.4446(9) 0.4340(9) 0.028(4) Uani d U 1 . . C C39 0.3423(10) 0.3652(12) 0.4299(10) 0.047(5) Uani d U 1 . . H H39A 0.3051 0.3960 0.4502 0.071 Uiso calc R 1 . . H H39B 0.3510 0.3236 0.4575 0.071 Uiso calc R 1 . . H H39C 0.3239 0.3498 0.3874 0.071 Uiso calc R 1 . . C C40 0.6113(10) 0.4544(11) 0.4525(9) 0.041(5) Uani d U 1 . . H H40A 0.6263 0.4172 0.4831 0.061 Uiso calc R 1 . . H H40B 0.6182 0.5009 0.4729 0.061 Uiso calc R 1 . . H H40C 0.6423 0.4514 0.4135 0.061 Uiso calc R 1 . . C C41 0.4538(9) 0.5006(10) 0.1951(8) 0.033(4) Uani d U 1 . . C C42 0.5302(9) 0.5104(9) 0.1788(9) 0.031(4) Uani d U 1 . . H H42 0.5532 0.5019 0.1381 0.038 Uiso calc R 1 . . C C43 0.5637(9) 0.5347(10) 0.2344(9) 0.031(4) Uani d U 1 . . C C44 0.3949(9) 0.4754(11) 0.1485(8) 0.038(5) Uani d U 1 . . H H44A 0.3822 0.4260 0.1582 0.057 Uiso calc R 1 . . H H44B 0.4140 0.4786 0.1041 0.057 Uiso calc R 1 . . H H44C 0.3502 0.5050 0.1526 0.057 Uiso calc R 1 . . C C45 0.6446(8) 0.5564(9) 0.2456(9) 0.032(4) Uani d U 1 . . H H45A 0.6466 0.6063 0.2586 0.048 Uiso calc R 1 . . H H45B 0.6729 0.5499 0.2054 0.048 Uiso calc R 1 . . H H45C 0.6666 0.5269 0.2799 0.048 Uiso calc R 1 . . N N17 0.0750(7) 0.2969(7) 0.3417(6) 0.048(4) Uani d DU 1 . . C C46 0.1438(10) 0.2517(11) 0.3479(9) 0.062(5) Uani d DU 1 . . H H46A 0.1470 0.2216 0.3087 0.075 Uiso calc R 1 . . H H46B 0.1879 0.2834 0.3478 0.075 Uiso calc R 1 . . C C47 0.150(2) 0.2046(17) 0.4056(15) 0.143(15) Uani d DU 1 . . H H47A 0.1029 0.2058 0.4297 0.215 Uiso calc R 1 . . H H47B 0.1909 0.2211 0.4336 0.215 Uiso calc R 1 . . H H47C 0.1602 0.1560 0.3914 0.215 Uiso calc R 1 . . C C48 0.0802(12) 0.3372(12) 0.2786(9) 0.075(6) Uani d DU 1 . . H H48A 0.1278 0.3641 0.2798 0.090 Uiso calc R 1 . . H H48B 0.0847 0.3018 0.2435 0.090 Uiso calc R 1 . . C C49 0.0201(13) 0.3876(15) 0.2592(14) 0.113(12) Uani d DU 1 . . H H49A -0.0217 0.3613 0.2396 0.169 Uiso calc R 1 . . H H49B 0.0399 0.4215 0.2276 0.169 Uiso calc R 1 . . H H49C 0.0024 0.4133 0.2975 0.169 Uiso calc R 1 . . C C50 0.0049(11) 0.2515(11) 0.3396(10) 0.070(6) Uani d DU 1 . . H H50A 0.0018 0.2246 0.3807 0.084 Uiso calc R 1 . . H H50B -0.0392 0.2832 0.3375 0.084 Uiso calc R 1 . . C C51 -0.0001(15) 0.2001(12) 0.2844(12) 0.081(8) Uani d DU 1 . . H H51A 0.0101 0.2248 0.2436 0.122 Uiso calc R 1 . . H H51B -0.0505 0.1795 0.2828 0.122 Uiso calc R 1 . . H H51C 0.0368 0.1622 0.2908 0.122 Uiso calc R 1 . . C C52 0.0679(10) 0.3474(11) 0.3990(10) 0.065(6) Uani d DU 1 . . H H52A 0.0255 0.3799 0.3903 0.077 Uiso calc R 1 . . H H52B 0.0549 0.3192 0.4379 0.077 Uiso calc R 1 . . C C53 0.1358(13) 0.3914(13) 0.4148(12) 0.084(9) Uani d DU 1 . . H H53A 0.1754 0.3608 0.4323 0.126 Uiso calc R 1 . . H H53B 0.1227 0.4274 0.4471 0.126 Uiso calc R 1 . . H H53C 0.1536 0.4147 0.3753 0.126 Uiso calc R 1 . . B B1 0.4864(11) 0.2490(11) 0.1043(10) 0.031(3) Uani d U 1 . . H H1 0.4332 0.2377 0.0933 0.047 Uiso calc R 1 . . B B11 0.5230(11) 0.5518(11) 0.3533(10) 0.032(3) Uani d U 1 . . H H11 0.5774 0.5591 0.3631 0.047 Uiso calc R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 W1 0.0194(4) 0.0273(4) 0.0249(4) 0.0008(3) -0.0033(3) -0.0008(3) W2 0.0204(4) 0.0309(5) 0.0404(5) 0.0016(3) -0.0085(3) -0.0074(4) W3 0.0193(4) 0.0350(5) 0.0316(4) 0.0005(3) -0.0068(3) -0.0037(3) W4 0.0210(4) 0.0419(5) 0.0311(4) -0.0027(3) -0.0045(3) -0.0032(4) S1 0.038(3) 0.048(3) 0.037(3) 0.009(2) 0.008(2) 0.002(2) S2 0.033(3) 0.024(2) 0.048(3) -0.0014(19) -0.009(2) -0.001(2) S3 0.032(2) 0.029(2) 0.029(2) 0.009(2) -0.007(2) -0.002(2) S4 0.082(5) 0.113(7) 0.151(8) -0.002(4) 0.023(5) -0.024(6) S5 0.064(4) 0.060(4) 0.054(3) 0.024(3) -0.032(3) -0.011(3) S6 0.126(7) 0.078(5) 0.079(4) 0.023(4) -0.043(5) -0.027(4) S7 0.098(6) 0.067(4) 0.109(6) 0.025(4) -0.059(5) -0.026(4) S8 0.040(3) 0.042(3) 0.075(4) -0.003(2) -0.022(3) -0.015(3) S11 0.028(2) 0.057(3) 0.042(3) 0.004(2) -0.009(2) -0.012(2) S12 0.031(2) 0.037(3) 0.036(3) -0.001(2) -0.004(2) -0.001(2) S13 0.032(3) 0.035(3) 0.046(3) 0.002(2) -0.014(2) -0.001(2) S14 0.072(4) 0.137(8) 0.084(5) -0.010(4) 0.006(4) -0.011(5) S15 0.045(3) 0.108(5) 0.051(3) 0.008(3) -0.009(3) 0.022(3) S16 0.134(8) 0.190(10) 0.081(5) -0.016(7) -0.023(6) -0.007(5) S17 0.263(13) 0.089(6) 0.050(4) 0.033(6) -0.021(6) -0.015(4) S18 0.070(4) 0.089(4) 0.062(4) -0.026(4) -0.007(3) -0.021(3) N1 0.031(6) 0.030(6) 0.025(7) -0.003(5) -0.014(6) -0.006(5) N2 0.037(6) 0.030(5) 0.038(8) 0.007(4) -0.018(6) -0.007(6) N3 0.039(7) 0.032(7) 0.043(8) 0.006(6) -0.012(6) 0.000(6) N4 0.033(6) 0.033(7) 0.039(7) 0.009(5) -0.009(5) 0.004(5) N5 0.017(5) 0.033(8) 0.036(6) 0.003(6) -0.003(5) -0.010(6) N6 0.011(5) 0.045(8) 0.026(5) -0.006(5) -0.006(4) -0.003(6) N11 0.024(6) 0.031(6) 0.045(8) 0.004(5) -0.013(7) 0.001(6) N12 0.029(6) 0.037(6) 0.048(8) 0.005(4) -0.017(6) -0.012(6) N13 0.020(6) 0.027(6) 0.034(7) 0.011(5) -0.003(5) -0.006(5) N14 0.024(6) 0.045(7) 0.032(7) 0.004(5) -0.009(5) 0.000(5) N15 0.015(5) 0.025(8) 0.042(6) 0.006(6) -0.001(5) 0.009(5) N16 0.020(5) 0.049(9) 0.032(6) -0.003(5) -0.006(4) -0.007(6) C1 0.045(7) 0.032(7) 0.019(8) 0.005(6) -0.008(8) -0.008(7) C2 0.051(8) 0.023(7) 0.044(11) -0.004(6) -0.015(9) 0.004(8) C3 0.040(7) 0.038(8) 0.022(9) -0.005(6) -0.002(8) -0.015(8) C4 0.042(8) 0.036(11) 0.032(10) 0.006(7) -0.004(9) -0.012(9) C5 0.047(8) 0.048(13) 0.052(13) -0.008(8) -0.018(11) -0.025(11) C6 0.039(8) 0.039(10) 0.042(10) 0.018(6) -0.001(8) 0.002(7) C7 0.056(9) 0.034(10) 0.039(11) 0.017(7) -0.012(8) 0.002(7) C8 0.045(8) 0.037(10) 0.026(9) 0.014(7) -0.012(7) -0.009(7) C9 0.059(10) 0.050(13) 0.026(10) 0.007(8) 0.012(9) 0.008(9) C10 0.055(10) 0.058(15) 0.056(14) 0.008(9) -0.026(10) -0.008(12) C11 0.033(7) 0.034(10) 0.032(7) -0.001(8) -0.001(5) -0.002(7) C12 0.037(7) 0.048(12) 0.043(9) -0.002(9) 0.017(6) -0.020(9) C13 0.025(7) 0.048(12) 0.050(9) -0.016(8) 0.012(6) -0.012(9) C14 0.043(10) 0.047(13) 0.035(10) -0.005(9) 0.010(8) -0.028(9) C15 0.023(7) 0.049(13) 0.063(14) -0.003(9) 0.014(8) -0.022(11) N7 0.071(13) 0.153(15) 0.073(10) -0.033(10) -0.013(8) 0.033(13) C16 0.13(2) 0.21(3) 0.079(12) -0.046(19) -0.035(13) 0.04(2) C17 0.18(3) 0.11(3) 0.089(12) 0.01(2) -0.010(18) -0.02(2) C18 0.12(2) 0.143(17) 0.092(19) -0.027(14) 0.011(15) 0.021(18) C19 0.15(3) 0.15(3) 0.16(3) -0.06(3) -0.03(3) 0.01(3) C20 0.077(17) 0.14(2) 0.094(13) -0.027(13) 0.004(12) -0.008(17) C21 0.10(3) 0.11(3) 0.21(4) -0.029(16) 0.01(2) -0.01(3) C22 0.112(19) 0.144(18) 0.082(18) -0.005(13) -0.011(14) -0.040(18) C23 0.10(3) 0.135(16) 0.22(4) -0.011(18) 0.05(3) -0.08(3) C31 0.034(7) 0.040(8) 0.058(12) 0.006(6) -0.003(9) -0.012(9) C32 0.036(7) 0.037(8) 0.038(10) 0.002(6) -0.018(9) -0.006(8) C33 0.036(7) 0.036(8) 0.049(11) -0.001(6) -0.020(9) -0.001(9) C34 0.032(7) 0.047(13) 0.088(17) 0.014(8) -0.030(11) -0.018(12) C35 0.028(7) 0.055(14) 0.042(12) -0.012(8) 0.006(9) -0.009(10) C36 0.026(7) 0.033(9) 0.025(9) 0.009(6) 0.001(7) -0.010(6) C37 0.024(7) 0.028(9) 0.029(9) 0.016(6) -0.001(7) -0.005(6) C38 0.024(7) 0.018(8) 0.042(10) 0.010(6) -0.007(7) -0.010(6) C39 0.032(9) 0.062(14) 0.047(12) -0.005(8) -0.002(9) 0.002(10) C40 0.032(8) 0.054(13) 0.037(11) 0.011(8) -0.024(8) -0.015(10) C41 0.022(7) 0.044(11) 0.031(7) 0.006(7) -0.003(5) 0.005(8) C42 0.027(7) 0.029(10) 0.038(7) -0.006(7) -0.001(5) 0.012(8) C43 0.023(6) 0.035(10) 0.036(7) -0.001(7) 0.003(6) 0.005(8) C44 0.022(8) 0.072(15) 0.020(8) 0.004(9) 0.001(7) 0.002(9) C45 0.014(6) 0.028(10) 0.054(12) 0.004(7) 0.007(7) -0.017(9) N17 0.038(8) 0.064(10) 0.043(8) -0.016(6) 0.002(7) 0.001(6) C46 0.072(11) 0.061(14) 0.053(13) 0.008(10) 0.000(11) -0.017(9) C47 0.19(4) 0.09(3) 0.14(3) 0.02(2) -0.05(3) 0.05(2) C48 0.082(15) 0.076(16) 0.066(11) -0.022(11) 0.008(12) 0.033(10) C49 0.051(16) 0.16(3) 0.12(2) -0.027(15) -0.040(16) 0.07(2) C50 0.071(11) 0.068(15) 0.071(14) -0.040(11) 0.020(12) -0.006(10) C51 0.10(2) 0.036(15) 0.11(2) -0.026(13) 0.011(16) -0.016(12) C52 0.057(13) 0.061(14) 0.076(12) -0.004(9) 0.008(12) -0.021(10) C53 0.092(18) 0.067(17) 0.09(2) -0.024(14) -0.030(16) 0.003(13) B1 0.023(8) 0.035(8) 0.035(7) -0.001(6) -0.013(7) -0.008(6) B11 0.016(8) 0.035(8) 0.044(7) 0.002(6) -0.005(7) -0.004(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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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' B B 0.0013 0.0007 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 W1 S2 . . 102.3(2) y S1 W1 S3 . . 104.20(18) y S1 W1 N2 . . 91.8(4) y S1 W1 N4 . . 90.7(4) y S1 W1 N6 . . 164.1(3) y S2 W1 S3 . . 101.34(16) y S2 W1 N2 . . 163.2(4) y S2 W1 N4 . . 86.6(4) y S2 W1 N6 . . 86.2(4) y S3 W1 N2 . . 83.6(4) y S3 W1 N4 . . 161.0(4) y S3 W1 N6 . . 86.9(4) y N2 W1 N4 . . 84.1(5) y N2 W1 N6 . . 78.0(5) y N4 W1 N6 . . 76.3(5) y S2 W2 S3 . . 100.71(15) y S2 W2 S4 . . 107.6(4) y S2 W2 S5 . . 144.1(2) y S2 W2 S8 . . 79.03(17) y S3 W2 S4 . . 107.7(3) y S3 W2 S5 . . 76.11(17) y S3 W2 S8 . . 148.3(2) y S4 W2 S5 . . 107.4(4) y S4 W2 S8 . . 102.4(3) y S5 W2 S8 . . 85.8(2) y S11 W3 S12 . . 101.65(19) y S11 W3 S13 . . 104.80(19) y S11 W3 N12 . . 89.8(4) y S11 W3 N14 . . 92.7(4) y S11 W3 N16 . . 165.5(3) y S12 W3 S13 . . 100.99(16) y S12 W3 N12 . . 165.7(4) y S12 W3 N14 . . 87.4(4) y S12 W3 N16 . . 85.9(4) y S13 W3 N12 . . 84.0(4) y S13 W3 N14 . . 158.4(4) y S13 W3 N16 . . 85.6(4) y N12 W3 N14 . . 83.5(5) y N12 W3 N16 . . 81.1(5) y N14 W3 N16 . . 75.1(5) y S12 W4 S13 . . 100.92(16) y S12 W4 S14 . . 109.0(3) y S12 W4 S15 . . 143.2(2) y S12 W4 S18 . . 77.7(2) y S13 W4 S14 . . 105.6(3) y S13 W4 S15 . . 80.3(2) y S13 W4 S18 . . 147.1(2) y S14 W4 S15 . . 105.9(3) y S14 W4 S18 . . 105.8(3) y S15 W4 S18 . . 82.0(3) y W1 S2 W2 . . 76.14(14) y W1 S3 W2 . . 75.90(14) y W2 S5 S6 . . 112.2(4) y S5 S6 S7 . . 100.9(5) y S6 S7 S8 . . 100.0(4) y W2 S8 S7 . . 106.7(3) y W3 S12 W4 . . 75.31(15) y W3 S13 W4 . . 75.71(16) y W4 S15 S16 . . 117.4(5) y S15 S16 S17 . . 98.5(6) y S16 S17 S18 . . 103.5(7) y W4 S18 S17 . . 104.1(4) y N2 N1 C3 . . 109.8(14) ? N2 N1 B1 . . 122.0(13) ? C3 N1 B1 . . 128.0(15) ? W1 N2 N1 . . 121.0(10) ? W1 N2 C1 . . 128.4(12) ? N1 N2 C1 . . 110.3(14) ? N4 N3 C8 . . 105.5(15) ? N4 N3 B1 . . 120.9(13) ? C8 N3 B1 . . 133.6(16) ? W1 N4 N3 . . 120.2(11) ? W1 N4 C6 . . 131.8(12) ? N3 N4 C6 . . 107.9(13) ? N6 N5 C13 . . 109.7(13) ? N6 N5 B1 . . 118.4(14) ? C13 N5 B1 . . 131.8(14) ? W1 N6 N5 . . 121.4(10) ? W1 N6 C11 . . 133.5(10) ? N5 N6 C11 . . 105.0(13) ? N12 N11 C33 . . 109.7(15) ? N12 N11 B11 . . 119.5(14) ? C33 N11 B11 . . 130.7(15) ? W3 N12 N11 . . 122.9(11) ? W3 N12 C31 . . 131.1(12) ? N11 N12 C31 . . 105.9(14) ? N14 N13 C38 . . 110.6(14) ? N14 N13 B11 . . 119.2(13) ? C38 N13 B11 . . 130.0(14) ? W3 N14 N13 . . 122.5(11) ? W3 N14 C36 . . 133.1(11) ? N13 N14 C36 . . 104.1(12) ? N16 N15 C43 . . 109.4(14) ? N16 N15 B11 . . 120.4(14) ? C43 N15 B11 . . 130.2(14) ? W3 N16 N15 . . 119.0(10) ? W3 N16 C41 . . 134.1(10) ? N15 N16 C41 . . 106.6(13) ? N2 C1 C2 . . 104.2(16) ? N2 C1 C4 . . 128.1(16) ? C2 C1 C4 . . 127.5(17) ? C1 C2 H2 . . 125.6 ? C1 C2 C3 . . 108.9(16) ? H2 C2 C3 . . 125.6 ? N1 C3 C2 . . 106.4(15) ? N1 C3 C5 . . 125.8(17) ? C2 C3 C5 . . 127.6(17) ? C1 C4 H4A . . 109.5 ? C1 C4 H4B . . 109.5 ? C1 C4 H4C . . 109.5 ? H4A C4 H4B . . 109.5 ? H4A C4 H4C . . 109.5 ? H4B C4 H4C . . 109.5 ? C3 C5 H5A . . 109.5 ? C3 C5 H5B . . 109.5 ? C3 C5 H5C . . 109.5 ? H5A C5 H5B . . 109.5 ? H5A C5 H5C . . 109.5 ? H5B C5 H5C . . 109.5 ? N4 C6 C7 . . 108.3(18) ? N4 C6 C9 . . 123.7(16) ? C7 C6 C9 . . 127.9(19) ? C6 C7 H7 . . 125.3 ? C6 C7 C8 . . 109.3(17) ? H7 C7 C8 . . 125.3 ? N3 C8 C7 . . 108.8(16) ? N3 C8 C10 . . 119.2(19) ? C7 C8 C10 . . 131.8(18) ? C6 C9 H9A . . 109.5 ? C6 C9 H9B . . 109.5 ? C6 C9 H9C . . 109.5 ? H9A C9 H9B . . 109.5 ? H9A C9 H9C . . 109.5 ? H9B C9 H9C . . 109.5 ? C8 C10 H10A . . 109.5 ? C8 C10 H10B . . 109.5 ? C8 C10 H10C . . 109.5 ? H10A C10 H10B . . 109.5 ? H10A C10 H10C . . 109.5 ? H10B C10 H10C . . 109.5 ? N6 C11 C12 . . 109.7(15) ? N6 C11 C14 . . 126.9(16) ? C12 C11 C14 . . 123.3(17) ? C11 C12 H12 . . 125.8 ? C11 C12 C13 . . 108.4(17) ? H12 C12 C13 . . 125.8 ? N5 C13 C12 . . 106.9(16) ? N5 C13 C15 . . 119.6(16) ? C12 C13 C15 . . 133.4(19) ? C11 C14 H14A . . 109.5 ? C11 C14 H14B . . 109.5 ? C11 C14 H14C . . 109.5 ? H14A C14 H14B . . 109.5 ? H14A C14 H14C . . 109.5 ? H14B C14 H14C . . 109.5 ? C13 C15 H15A . . 109.5 ? C13 C15 H15B . . 109.5 ? C13 C15 H15C . . 109.5 ? H15A C15 H15B . . 109.5 ? H15A C15 H15C . . 109.5 ? H15B C15 H15C . . 109.5 ? C16 N7 C18 . . 111.9(15) ? C16 N7 C20 . . 105.6(14) ? C16 N7 C22 . . 109.0(15) ? C18 N7 C20 . . 108.8(15) ? C18 N7 C22 . . 110.2(15) ? C20 N7 C22 . . 111.2(14) ? N7 C16 H16A . . 107.1 ? N7 C16 H16B . . 107.1 ? N7 C16 C17 . . 120.7(18) ? H16A C16 H16B . . 106.8 ? H16A C16 C17 . . 107.1 ? H16B C16 C17 . . 107.1 ? C16 C17 H17A . . 109.5 ? C16 C17 H17B . . 109.5 ? C16 C17 H17C . . 109.5 ? H17A C17 H17B . . 109.5 ? H17A C17 H17C . . 109.5 ? H17B C17 H17C . . 109.5 ? N7 C18 H18A . . 108.0 ? N7 C18 H18B . . 108.0 ? N7 C18 C19 . . 117.3(18) ? H18A C18 H18B . . 107.2 ? H18A C18 C19 . . 108.0 ? H18B C18 C19 . . 108.0 ? C18 C19 H19A . . 109.5 ? C18 C19 H19B . . 109.5 ? C18 C19 H19C . . 109.5 ? H19A C19 H19B . . 109.5 ? H19A C19 H19C . . 109.5 ? H19B C19 H19C . . 109.5 ? N7 C20 H20A . . 108.4 ? N7 C20 H20B . . 108.4 ? N7 C20 C21 . . 115.3(19) ? H20A C20 H20B . . 107.5 ? H20A C20 C21 . . 108.4 ? H20B C20 C21 . . 108.4 ? C20 C21 H21A . . 109.5 ? C20 C21 H21B . . 109.5 ? C20 C21 H21C . . 109.5 ? H21A C21 H21B . . 109.5 ? H21A C21 H21C . . 109.5 ? H21B C21 H21C . . 109.5 ? N7 C22 H22A . . 107.9 ? N7 C22 H22B . . 107.9 ? N7 C22 C23 . . 117.5(18) ? H22A C22 H22B . . 107.2 ? H22A C22 C23 . . 107.9 ? H22B C22 C23 . . 107.9 ? C22 C23 H23A . . 109.5 ? C22 C23 H23B . . 109.5 ? C22 C23 H23C . . 109.5 ? H23A C23 H23B . . 109.5 ? H23A C23 H23C . . 109.5 ? H23B C23 H23C . . 109.5 ? N12 C31 C32 . . 108.2(16) ? N12 C31 C34 . . 123.0(17) ? C32 C31 C34 . . 128.3(18) ? C31 C32 H32 . . 126.7 ? C31 C32 C33 . . 106.7(17) ? H32 C32 C33 . . 126.7 ? N11 C33 C32 . . 109.5(16) ? N11 C33 C35 . . 122.8(17) ? C32 C33 C35 . . 127.7(18) ? C31 C34 H34A . . 109.5 ? C31 C34 H34B . . 109.5 ? C31 C34 H34C . . 109.5 ? H34A C34 H34B . . 109.5 ? H34A C34 H34C . . 109.5 ? H34B C34 H34C . . 109.5 ? C33 C35 H35A . . 109.5 ? C33 C35 H35B . . 109.5 ? C33 C35 H35C . . 109.5 ? H35A C35 H35B . . 109.5 ? H35A C35 H35C . . 109.5 ? H35B C35 H35C . . 109.5 ? N14 C36 C37 . . 109.2(15) ? N14 C36 C39 . . 122.7(15) ? C37 C36 C39 . . 127.9(17) ? C36 C37 H37 . . 126.1 ? C36 C37 C38 . . 107.7(15) ? H37 C37 C38 . . 126.1 ? N13 C38 C37 . . 108.4(14) ? N13 C38 C40 . . 122.9(17) ? C37 C38 C40 . . 128.6(16) ? C36 C39 H39A . . 109.5 ? C36 C39 H39B . . 109.5 ? C36 C39 H39C . . 109.5 ? H39A C39 H39B . . 109.5 ? H39A C39 H39C . . 109.5 ? H39B C39 H39C . . 109.5 ? C38 C40 H40A . . 109.5 ? C38 C40 H40B . . 109.5 ? C38 C40 H40C . . 109.5 ? H40A C40 H40B . . 109.5 ? H40A C40 H40C . . 109.5 ? H40B C40 H40C . . 109.5 ? N16 C41 C42 . . 109.3(14) ? N16 C41 C44 . . 126.5(15) ? C42 C41 C44 . . 124.2(17) ? C41 C42 H42 . . 127.4 ? C41 C42 C43 . . 105.2(17) ? H42 C42 C43 . . 127.4 ? N15 C43 C42 . . 109.3(16) ? N15 C43 C45 . . 121.7(16) ? C42 C43 C45 . . 129.0(17) ? C41 C44 H44A . . 109.5 ? C41 C44 H44B . . 109.5 ? C41 C44 H44C . . 109.5 ? H44A C44 H44B . . 109.5 ? H44A C44 H44C . . 109.5 ? H44B C44 H44C . . 109.5 ? C43 C45 H45A . . 109.5 ? C43 C45 H45B . . 109.5 ? C43 C45 H45C . . 109.5 ? H45A C45 H45B . . 109.5 ? H45A C45 H45C . . 109.5 ? H45B C45 H45C . . 109.5 ? C46 N17 C48 . . 107.8(12) ? C46 N17 C50 . . 110.8(13) ? C46 N17 C52 . . 111.2(12) ? C48 N17 C50 . . 108.4(12) ? C48 N17 C52 . . 111.0(14) ? C50 N17 C52 . . 107.6(11) ? N17 C46 H46A . . 107.9 ? N17 C46 H46B . . 107.9 ? N17 C46 C47 . . 117.7(17) ? H46A C46 H46B . . 107.2 ? H46A C46 C47 . . 107.9 ? H46B C46 C47 . . 107.9 ? C46 C47 H47A . . 109.5 ? C46 C47 H47B . . 109.5 ? C46 C47 H47C . . 109.5 ? H47A C47 H47B . . 109.5 ? H47A C47 H47C . . 109.5 ? H47B C47 H47C . . 109.5 ? N17 C48 H48A . . 107.2 ? N17 C48 H48B . . 107.2 ? N17 C48 C49 . . 120.4(16) ? H48A C48 H48B . . 106.9 ? H48A C48 C49 . . 107.2 ? H48B C48 C49 . . 107.2 ? C48 C49 H49A . . 109.5 ? C48 C49 H49B . . 109.5 ? C48 C49 H49C . . 109.5 ? H49A C49 H49B . . 109.5 ? H49A C49 H49C . . 109.5 ? H49B C49 H49C . . 109.5 ? N17 C50 H50A . . 108.4 ? N17 C50 H50B . . 108.4 ? N17 C50 C51 . . 115.6(14) ? H50A C50 H50B . . 107.4 ? H50A C50 C51 . . 108.4 ? H50B C50 C51 . . 108.4 ? C50 C51 H51A . . 109.5 ? C50 C51 H51B . . 109.5 ? C50 C51 H51C . . 109.5 ? H51A C51 H51B . . 109.5 ? H51A C51 H51C . . 109.5 ? H51B C51 H51C . . 109.5 ? N17 C52 H52A . . 108.2 ? N17 C52 H52B . . 108.2 ? N17 C52 C53 . . 116.2(15) ? H52A C52 H52B . . 107.4 ? H52A C52 C53 . . 108.2 ? H52B C52 C53 . . 108.2 ? C52 C53 H53A . . 109.5 ? C52 C53 H53B . . 109.5 ? C52 C53 H53C . . 109.5 ? H53A C53 H53B . . 109.5 ? H53A C53 H53C . . 109.5 ? H53B C53 H53C . . 109.5 ? N1 B1 N3 . . 113.0(17) ? N1 B1 N5 . . 108.4(14) ? N1 B1 H1 . . 109.2 ? N3 B1 N5 . . 107.8(15) ? N3 B1 H1 . . 109.2 ? N5 B1 H1 . . 109.2 ? N11 B11 N13 . . 110.8(15) ? N11 B11 N15 . . 109.2(14) ? N11 B11 H11 . . 109.6 ? N13 B11 N15 . . 108.0(14) ? N13 B11 H11 . . 109.6 ? N15 B11 H11 . . 109.6 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag W1 S1 . 2.144(5) y W1 S2 . 2.314(5) y W1 S3 . 2.318(4) y W1 N2 . 2.265(14) y W1 N4 . 2.246(13) y W1 N6 . 2.329(14) y W2 S2 . 2.322(4) y W2 S3 . 2.331(5) y W2 S4 . 1.859(9) y W2 S5 . 2.448(6) y W2 S8 . 2.423(5) y W3 S11 . 2.124(5) y W3 S12 . 2.330(5) y W3 S13 . 2.316(5) y W3 N12 . 2.241(14) y W3 N14 . 2.193(13) y W3 N16 . 2.371(15) y W4 S12 . 2.328(5) y W4 S13 . 2.320(5) y W4 S14 . 1.939(8) y W4 S15 . 2.406(6) y W4 S18 . 2.386(7) y S5 S6 . 2.060(9) y S6 S7 . 1.975(13) y S7 S8 . 2.059(8) y S15 S16 . 1.954(12) y S16 S17 . 1.857(16) y S17 S18 . 2.018(12) y N1 N2 . 1.364(19) ? N1 C3 . 1.35(2) ? N1 B1 . 1.48(3) ? N2 C1 . 1.35(2) ? N3 N4 . 1.43(2) ? N3 C8 . 1.38(2) ? N3 B1 . 1.48(3) ? N4 C6 . 1.36(2) ? N5 N6 . 1.387(17) ? N5 C13 . 1.40(2) ? N5 B1 . 1.51(2) ? N6 C11 . 1.39(2) ? N11 N12 . 1.371(19) ? N11 C33 . 1.33(2) ? N11 B11 . 1.52(3) ? N12 C31 . 1.38(2) ? N13 N14 . 1.400(19) ? N13 C38 . 1.33(2) ? N13 B11 . 1.56(3) ? N14 C36 . 1.39(2) ? N15 N16 . 1.378(18) ? N15 C43 . 1.35(2) ? N15 B11 . 1.49(3) ? N16 C41 . 1.36(2) ? C1 C2 . 1.44(2) ? C1 C4 . 1.46(2) ? C2 H2 . 0.950 ? C2 C3 . 1.38(3) ? C3 C5 . 1.46(2) ? C4 H4A . 0.980 ? C4 H4B . 0.980 ? C4 H4C . 0.980 ? C5 H5A . 0.980 ? C5 H5B . 0.980 ? C5 H5C . 0.980 ? C6 C7 . 1.36(2) ? C6 C9 . 1.44(3) ? C7 H7 . 0.950 ? C7 C8 . 1.36(3) ? C8 C10 . 1.47(3) ? C9 H9A . 0.980 ? C9 H9B . 0.980 ? C9 H9C . 0.980 ? C10 H10A . 0.980 ? C10 H10B . 0.980 ? C10 H10C . 0.980 ? C11 C12 . 1.38(3) ? C11 C14 . 1.50(2) ? C12 H12 . 0.950 ? C12 C13 . 1.36(3) ? C13 C15 . 1.48(2) ? C14 H14A . 0.980 ? C14 H14B . 0.980 ? C14 H14C . 0.980 ? C15 H15A . 0.980 ? C15 H15B . 0.980 ? C15 H15C . 0.980 ? N7 C16 . 1.505(15) ? N7 C18 . 1.507(15) ? N7 C20 . 1.529(15) ? N7 C22 . 1.499(15) ? C16 H16A . 0.990 ? C16 H16B . 0.990 ? C16 C17 . 1.478(18) ? C17 H17A . 0.980 ? C17 H17B . 0.980 ? C17 H17C . 0.980 ? C18 H18A . 0.990 ? C18 H18B . 0.990 ? C18 C19 . 1.503(18) ? C19 H19A . 0.980 ? C19 H19B . 0.980 ? C19 H19C . 0.980 ? C20 H20A . 0.990 ? C20 H20B . 0.990 ? C20 C21 . 1.504(18) ? C21 H21A . 0.980 ? C21 H21B . 0.980 ? C21 H21C . 0.980 ? C22 H22A . 0.990 ? C22 H22B . 0.990 ? C22 C23 . 1.507(18) ? C23 H23A . 0.980 ? C23 H23B . 0.980 ? C23 H23C . 0.980 ? C31 C32 . 1.39(3) ? C31 C34 . 1.49(3) ? C32 H32 . 0.950 ? C32 C33 . 1.35(3) ? C33 C35 . 1.51(2) ? C34 H34A . 0.980 ? C34 H34B . 0.980 ? C34 H34C . 0.980 ? C35 H35A . 0.980 ? C35 H35B . 0.980 ? C35 H35C . 0.980 ? C36 C37 . 1.38(2) ? C36 C39 . 1.49(3) ? C37 H37 . 0.950 ? C37 C38 . 1.36(2) ? C38 C40 . 1.53(2) ? C39 H39A . 0.980 ? C39 H39B . 0.980 ? C39 H39C . 0.980 ? C40 H40A . 0.980 ? C40 H40B . 0.980 ? C40 H40C . 0.980 ? C41 C42 . 1.42(2) ? C41 C44 . 1.50(2) ? C42 H42 . 0.950 ? C42 C43 . 1.37(2) ? C43 C45 . 1.52(2) ? C44 H44A . 0.980 ? C44 H44B . 0.980 ? C44 H44C . 0.980 ? C45 H45A . 0.980 ? C45 H45B . 0.980 ? C45 H45C . 0.980 ? N17 C46 . 1.502(14) ? N17 C48 . 1.509(14) ? N17 C50 . 1.519(14) ? N17 C52 . 1.524(14) ? C46 H46A . 0.990 ? C46 H46B . 0.990 ? C46 C47 . 1.487(18) ? C47 H47A . 0.980 ? C47 H47B . 0.980 ? C47 H47C . 0.980 ? C48 H48A . 0.990 ? C48 H48B . 0.990 ? C48 C49 . 1.489(17) ? C49 H49A . 0.980 ? C49 H49B . 0.980 ? C49 H49C . 0.980 ? C50 H50A . 0.990 ? C50 H50B . 0.990 ? C50 C51 . 1.497(17) ? C51 H51A . 0.980 ? C51 H51B . 0.980 ? C51 H51C . 0.980 ? C52 H52A . 0.990 ? C52 H52B . 0.990 ? C52 C53 . 1.505(17) ? C53 H53A . 0.980 ? C53 H53B . 0.980 ? C53 H53C . 0.980 ? B1 H1 . 1.000 ? B11 H11 . 1.000 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag S1 W1 S2 W2 . . . . -88.89(17) ? S3 W1 S2 W2 . . . . 18.56(17) ? N2 W1 S2 W2 . . . . 124.3(13) ? N4 W1 S2 W2 . . . . -178.9(4) ? N6 W1 S2 W2 . . . . 104.7(3) ? S3 W2 S2 W1 . . . . -18.41(17) ? S4 W2 S2 W1 . . . . 94.2(3) ? S5 W2 S2 W1 . . . . -99.5(3) ? S8 W2 S2 W1 . . . . -166.1(2) ? S1 W1 S3 W2 . . . . 87.46(18) ? S2 W1 S3 W2 . . . . -18.51(17) ? N2 W1 S3 W2 . . . . 177.8(4) ? N4 W1 S3 W2 . . . . -131.9(12) ? N6 W1 S3 W2 . . . . -104.0(4) ? S2 W2 S3 W1 . . . . 18.40(17) ? S4 W2 S3 W1 . . . . -94.2(4) ? S5 W2 S3 W1 . . . . 161.72(19) ? S8 W2 S3 W1 . . . . 104.8(3) ? S2 W2 S5 S6 . . . . -63.3(5) ? S3 W2 S5 S6 . . . . -152.4(4) ? S4 W2 S5 S6 . . . . 103.1(5) ? S8 W2 S5 S6 . . . . 1.4(4) ? W2 S5 S6 S7 . . . . -34.9(5) ? S5 S6 S7 S8 . . . . 55.6(5) ? S6 S7 S8 W2 . . . . -58.5(5) ? S2 W2 S8 S7 . . . . 179.0(4) ? S3 W2 S8 S7 . . . . 86.4(4) ? S4 W2 S8 S7 . . . . -75.1(5) ? S5 W2 S8 S7 . . . . 31.7(4) ? S13 W4 S12 W3 . . . . 20.11(18) ? S14 W4 S12 W3 . . . . -90.8(3) ? S15 W4 S12 W3 . . . . 108.5(3) ? S18 W4 S12 W3 . . . . 166.5(2) ? S11 W3 S12 W4 . . . . 87.64(17) ? S13 W3 S12 W4 . . . . -20.16(18) ? N12 W3 S12 W4 . . . . -129.7(17) ? N14 W3 S12 W4 . . . . 179.9(4) ? N16 W3 S12 W4 . . . . -104.9(4) ? S11 W3 S13 W4 . . . . -85.13(18) ? S12 W3 S13 W4 . . . . 20.19(18) ? N12 W3 S13 W4 . . . . -173.4(4) ? N14 W3 S13 W4 . . . . 131.5(11) ? N16 W3 S13 W4 . . . . 105.2(4) ? S12 W4 S13 W3 . . . . -20.20(18) ? S14 W4 S13 W3 . . . . 93.3(3) ? S15 W4 S13 W3 . . . . -162.8(2) ? S18 W4 S13 W3 . . . . -104.4(4) ? S12 W4 S15 S16 . . . . 62.9(6) ? S13 W4 S15 S16 . . . . 158.2(5) ? S14 W4 S15 S16 . . . . -98.2(6) ? S18 W4 S15 S16 . . . . 6.1(5) ? W4 S15 S16 S17 . . . . 27.4(8) ? S15 S16 S17 S18 . . . . -53.0(7) ? S16 S17 S18 W4 . . . . 62.4(6) ? S12 W4 S18 S17 . . . . 175.6(5) ? S13 W4 S18 S17 . . . . -93.2(5) ? S14 W4 S18 S17 . . . . 69.1(5) ? S15 W4 S18 S17 . . . . -35.2(5) ? C3 N1 N2 W1 . . . . 178.3(12) ? C3 N1 N2 C1 . . . . 4(2) ? B1 N1 N2 W1 . . . . -6(2) ? B1 N1 N2 C1 . . . . 179.7(16) ? S1 W1 N2 N1 . . . . -122.9(12) ? S1 W1 N2 C1 . . . . 50.1(15) ? S2 W1 N2 N1 . . . . 25(2) ? S2 W1 N2 C1 . . . . -162.3(11) ? S3 W1 N2 N1 . . . . 133.0(13) ? S3 W1 N2 C1 . . . . -54.0(15) ? N4 W1 N2 N1 . . . . -32.4(13) ? N4 W1 N2 C1 . . . . 140.6(16) ? N6 W1 N2 N1 . . . . 44.8(12) ? N6 W1 N2 C1 . . . . -142.2(16) ? C8 N3 N4 W1 . . . . -178.5(11) ? C8 N3 N4 C6 . . . . -1.4(19) ? B1 N3 N4 W1 . . . . 4(2) ? B1 N3 N4 C6 . . . . -179.2(16) ? S1 W1 N4 N3 . . . . 124.7(12) ? S1 W1 N4 C6 . . . . -51.6(17) ? S2 W1 N4 N3 . . . . -133.0(12) ? S2 W1 N4 C6 . . . . 50.7(16) ? S3 W1 N4 N3 . . . . -17(2) ? S3 W1 N4 C6 . . . . 166.4(12) ? N2 W1 N4 N3 . . . . 33.0(12) ? N2 W1 N4 C6 . . . . -143.3(17) ? N6 W1 N4 N3 . . . . -46.1(12) ? N6 W1 N4 C6 . . . . 137.6(17) ? C13 N5 N6 W1 . . . . 176.1(12) ? C13 N5 N6 C11 . . . . -4.1(19) ? B1 N5 N6 W1 . . . . -5.3(19) ? B1 N5 N6 C11 . . . . 174.5(15) ? S1 W1 N6 N5 . . . . 12(2) ? S1 W1 N6 C11 . . . . -167.5(12) ? S2 W1 N6 N5 . . . . 135.5(12) ? S2 W1 N6 C11 . . . . -44.3(16) ? S3 W1 N6 N5 . . . . -123.0(12) ? S3 W1 N6 C11 . . . . 57.3(16) ? N2 W1 N6 N5 . . . . -38.8(12) ? N2 W1 N6 C11 . . . . 141.4(17) ? N4 W1 N6 N5 . . . . 48.0(12) ? N4 W1 N6 C11 . . . . -131.8(17) ? C33 N11 N12 W3 . . . . 178.9(13) ? C33 N11 N12 C31 . . . . 2(2) ? B11 N11 N12 W3 . . . . -3(2) ? B11 N11 N12 C31 . . . . -179.9(17) ? S11 W3 N12 N11 . . . . 132.0(13) ? S11 W3 N12 C31 . . . . -52.0(18) ? S12 W3 N12 N11 . . . . -12(3) ? S12 W3 N12 C31 . . . . 164.4(14) ? S13 W3 N12 N11 . . . . -123.1(13) ? S13 W3 N12 C31 . . . . 52.9(18) ? N14 W3 N12 N11 . . . . 39.2(14) ? N14 W3 N12 C31 . . . . -144.7(19) ? N16 W3 N12 N11 . . . . -36.7(13) ? N16 W3 N12 C31 . . . . 139.4(19) ? C38 N13 N14 W3 . . . . 174.1(11) ? C38 N13 N14 C36 . . . . 0.0(18) ? B11 N13 N14 W3 . . . . -10.2(19) ? B11 N13 N14 C36 . . . . 175.7(14) ? S11 W3 N14 N13 . . . . -120.8(12) ? S11 W3 N14 C36 . . . . 51.4(15) ? S12 W3 N14 N13 . . . . 137.7(12) ? S12 W3 N14 C36 . . . . -50.2(15) ? S13 W3 N14 N13 . . . . 24(2) ? S13 W3 N14 C36 . . . . -163.9(11) ? N12 W3 N14 N13 . . . . -31.3(12) ? N12 W3 N14 C36 . . . . 140.9(16) ? N16 W3 N14 N13 . . . . 51.2(12) ? N16 W3 N14 C36 . . . . -136.6(16) ? C43 N15 N16 W3 . . . . -171.9(11) ? C43 N15 N16 C41 . . . . 2.8(19) ? B11 N15 N16 W3 . . . . 8.8(19) ? B11 N15 N16 C41 . . . . -176.5(15) ? S11 W3 N16 N15 . . . . -18(3) ? S11 W3 N16 C41 . . . . 169.0(13) ? S12 W3 N16 N15 . . . . -140.2(12) ? S12 W3 N16 C41 . . . . 46.9(17) ? S13 W3 N16 N15 . . . . 118.4(12) ? S13 W3 N16 C41 . . . . -54.5(17) ? N12 W3 N16 N15 . . . . 33.8(12) ? N12 W3 N16 C41 . . . . -139.1(18) ? N14 W3 N16 N15 . . . . -51.8(12) ? N14 W3 N16 C41 . . . . 135.3(18) ? W1 N2 C1 C2 . . . . -179.9(12) ? W1 N2 C1 C4 . . . . 4(3) ? N1 N2 C1 C2 . . . . -6(2) ? N1 N2 C1 C4 . . . . 177.3(17) ? N2 C1 C2 C3 . . . . 6(2) ? C4 C1 C2 C3 . . . . -177.3(17) ? N2 N1 C3 C2 . . . . 0(2) ? N2 N1 C3 C5 . . . . 174.9(18) ? B1 N1 C3 C2 . . . . -175.2(18) ? B1 N1 C3 C5 . . . . 0(3) ? C1 C2 C3 N1 . . . . -4(2) ? C1 C2 C3 C5 . . . . -178.6(18) ? W1 N4 C6 C7 . . . . 175.3(13) ? W1 N4 C6 C9 . . . . 0(3) ? N3 N4 C6 C7 . . . . -1(2) ? N3 N4 C6 C9 . . . . -177.1(17) ? N4 C6 C7 C8 . . . . 4(2) ? C9 C6 C7 C8 . . . . 179.1(19) ? C6 C7 C8 N3 . . . . -5(2) ? C6 C7 C8 C10 . . . . -180(2) ? N4 N3 C8 C7 . . . . 4(2) ? N4 N3 C8 C10 . . . . 179.5(17) ? B1 N3 C8 C7 . . . . -179.0(19) ? B1 N3 C8 C10 . . . . -3(3) ? W1 N6 C11 C12 . . . . -177.6(13) ? W1 N6 C11 C14 . . . . 2(3) ? N5 N6 C11 C12 . . . . 3(2) ? N5 N6 C11 C14 . . . . -177.7(17) ? N6 C11 C12 C13 . . . . 0(2) ? C14 C11 C12 C13 . . . . -179.8(18) ? C11 C12 C13 N5 . . . . -2(2) ? C11 C12 C13 C15 . . . . -180(2) ? N6 N5 C13 C12 . . . . 4(2) ? N6 N5 C13 C15 . . . . -178.3(17) ? B1 N5 C13 C12 . . . . -174.2(18) ? B1 N5 C13 C15 . . . . 3(3) ? C18 N7 C16 C17 . . . . 61(3) ? C20 N7 C16 C17 . . . . 179(3) ? C22 N7 C16 C17 . . . . -62(3) ? C16 N7 C18 C19 . . . . 174(3) ? C20 N7 C18 C19 . . . . 57(3) ? C22 N7 C18 C19 . . . . -65(3) ? C16 N7 C20 C21 . . . . -70(3) ? C18 N7 C20 C21 . . . . 50(3) ? C22 N7 C20 C21 . . . . 172(2) ? C16 N7 C22 C23 . . . . -65(3) ? C18 N7 C22 C23 . . . . 172(3) ? C20 N7 C22 C23 . . . . 51(3) ? W3 N12 C31 C32 . . . . -179.0(13) ? W3 N12 C31 C34 . . . . 9(3) ? N11 N12 C31 C32 . . . . -2(2) ? N11 N12 C31 C34 . . . . -174.9(19) ? N12 C31 C32 C33 . . . . 2(2) ? C34 C31 C32 C33 . . . . 174(2) ? N12 N11 C33 C32 . . . . -1(2) ? N12 N11 C33 C35 . . . . -179.9(17) ? B11 N11 C33 C32 . . . . -178.7(18) ? B11 N11 C33 C35 . . . . 2(3) ? C31 C32 C33 N11 . . . . -1(2) ? C31 C32 C33 C35 . . . . 178(2) ? W3 N14 C36 C37 . . . . -173.2(12) ? W3 N14 C36 C39 . . . . 3(3) ? N13 N14 C36 C37 . . . . 0.0(18) ? N13 N14 C36 C39 . . . . 176.0(16) ? N14 C36 C37 C38 . . . . 0.0(19) ? C39 C36 C37 C38 . . . . -175.8(18) ? N14 N13 C38 C37 . . . . 0.0(19) ? N14 N13 C38 C40 . . . . 178.2(15) ? B11 N13 C38 C37 . . . . -175.1(16) ? B11 N13 C38 C40 . . . . 3(3) ? C36 C37 C38 N13 . . . . 0(2) ? C36 C37 C38 C40 . . . . -178.1(17) ? W3 N16 C41 C42 . . . . 173.3(12) ? W3 N16 C41 C44 . . . . -8(3) ? N15 N16 C41 C42 . . . . 0(2) ? N15 N16 C41 C44 . . . . 178.4(17) ? N16 C41 C42 C43 . . . . -2(2) ? C44 C41 C42 C43 . . . . 179.0(17) ? N16 N15 C43 C42 . . . . -4(2) ? N16 N15 C43 C45 . . . . 177.6(15) ? B11 N15 C43 C42 . . . . 174.8(16) ? B11 N15 C43 C45 . . . . -3(3) ? C41 C42 C43 N15 . . . . 4(2) ? C41 C42 C43 C45 . . . . -178.1(18) ? C48 N17 C46 C47 . . . . -178(2) ? C50 N17 C46 C47 . . . . -59(3) ? C52 N17 C46 C47 . . . . 60(3) ? C46 N17 C48 C49 . . . . -179(2) ? C50 N17 C48 C49 . . . . 61(2) ? C52 N17 C48 C49 . . . . -57(3) ? C46 N17 C50 C51 . . . . -61(2) ? C48 N17 C50 C51 . . . . 57(2) ? C52 N17 C50 C51 . . . . 178(2) ? C46 N17 C52 C53 . . . . 51(2) ? C48 N17 C52 C53 . . . . -69(2) ? C50 N17 C52 C53 . . . . 173(2) ? N4 N3 B1 N1 . . . . -59(2) ? N4 N3 B1 N5 . . . . 61(2) ? C8 N3 B1 N1 . . . . 124(2) ? C8 N3 B1 N5 . . . . -116(2) ? N2 N1 B1 N3 . . . . 61(2) ? N2 N1 B1 N5 . . . . -59(2) ? C3 N1 B1 N3 . . . . -124.8(18) ? C3 N1 B1 N5 . . . . 115.8(18) ? N6 N5 B1 N1 . . . . 64(2) ? N6 N5 B1 N3 . . . . -58.8(19) ? C13 N5 B1 N1 . . . . -118(2) ? C13 N5 B1 N3 . . . . 119(2) ? N16 N15 B11 N11 . . . . -66(2) ? N16 N15 B11 N13 . . . . 54.3(19) ? C43 N15 B11 N11 . . . . 114.5(19) ? C43 N15 B11 N13 . . . . -124.8(18) ? N12 N11 B11 N13 . . . . -55(2) ? N12 N11 B11 N15 . . . . 64(2) ? C33 N11 B11 N13 . . . . 123(2) ? C33 N11 B11 N15 . . . . -118(2) ? N14 N13 B11 N11 . . . . 63.1(19) ? N14 N13 B11 N15 . . . . -56.5(19) ? C38 N13 B11 N11 . . . . -122.2(18) ? C38 N13 B11 N15 . . . . 118.2(18) ?