# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2005 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 loop_ _publ_author_name _publ_author_address _publ_author_footnote 'E. Constable' ; ? # Address for author 1 ; ; ? # Footnote for author 1 ; 'Bianca A. Hermann' ; ? # Address 2 ; ; ? # Footnote 2 ; 'Catherine E. Housecroft' '' '' 'Markus Neuburger' '' '' ; S.Schaffner ; '' '' 'Lukas Scherer' '' '' _publ_contact_author_name 'E. Constable' _publ_contact_author_address ; Departement Chemie University of Basel Spitalstrasse 51 Basel CH-4056 SWITZERLAND ; _publ_contact_author_email EDWIN.CONSTABLE@UNIBAS.CH _publ_section_title ; 2,2':6',2"-Terpyridine-4'(1'H)-thione: a missing link in metallosupramolecular chemistry ; _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ? _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? # PROCESSING SUMMARY (IUCr Office Use Only): _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_volume ? _journal_year ? _publ_contact_author_fax '+44 1865 285018' _publ_contact_author_phone '+44 1865 285024' # Check this file using the IUCr facility at: # http://journals.iucr.org/services/cif/checking/checkfull.html # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_contact_letter ; Please consider this CIF submission for publication as a Short Format Paper in Acta Crystallographica C. The figures have been sent by mail. ; _publ_requested_category CO # choose from: FI FM FO CI CM CO AD _publ_requested_coeditor_name 'Prof William Clegg' data_ls_a111_123k _database_code_depnum_ccdc_archive 'CCDC 269056' _audit_creation_date 05-07-27 _audit_creation_method CRYSTALS_ver_12.24 _oxford_structure_analysis_title '10061518 ls_a111_123k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 60.749(2) _cell_length_b 4.92820(10) _cell_length_c 19.1272(7) _cell_angle_alpha 90 _cell_angle_beta 95.9860(11) _cell_angle_gamma 90 _cell_volume 5695.1(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 _chemical_formula_sum 'C36 H29 N3 O2 S1' _chemical_formula_moiety 'C36 H29 N3 O2 S1' _chemical_compound_source ? _chemical_formula_weight 567.71 _cell_measurement_reflns_used 9313 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27 _cell_measurement_temperature 123 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_max 0.38 _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2384 _exptl_absorpt_coefficient_mu 0.153 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_absorpt_correction_T_min 0.99 _exptl_absorpt_correction_T_max 0.99 # Sheldrick geometric definitions 0.99 0.99 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' _computing_data_collection 'COLLECT (Nonius BV, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 123 _diffrn_reflns_number 18807 _reflns_number_total 6411 _diffrn_reflns_av_R_equivalents 0.070 # Number of reflections with Friedels Law is 6411 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 6516 _diffrn_reflns_theta_min 2.022 _diffrn_reflns_theta_max 27.461 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 22.518 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -78 _diffrn_reflns_limit_h_max 78 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -78 _reflns_limit_h_max 78 _reflns_limit_k_min 0 _reflns_limit_k_max 6 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.37 _refine_diff_density_max 0.30 _refine_ls_number_reflns 4223 _refine_ls_number_restraints 96 _refine_ls_number_parameters 415 #_refine_ls_R_factor_ref 0.0472 _refine_ls_wR_factor_ref 0.0365 _refine_ls_goodness_of_fit_ref 1.1570 #_reflns_number_all 5013 _refine_ls_R_factor_all 0.0575 _refine_ls_wR_factor_all 0.0376 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>1.80u(I) _reflns_number_gt 4223 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_gt 0.0365 _refine_ls_shift/su_max 0.002420 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.47 1.71 1.08 ; _publ_section_abstract # Text of the abstract ; ? ; _publ_section_comment # Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen ; H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, (1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens S1 S 0.644338(5) 0.50317(7) 0.208814(17) 0.0278 1.0000 Uani . . . . . . N1 N 0.663879(19) 0.1050(3) -0.04032(6) 0.0302 1.0000 Uani . . . . . . N2 N 0.695619(17) 0.6320(2) 0.05395(6) 0.0259 1.0000 Uani . . . . . . N3 N 0.713700(19) 1.1188(3) 0.18888(6) 0.0326 1.0000 Uani . . . . . . O1 O 0.584597(15) -0.1402(2) 0.35149(5) 0.0272 1.0000 Uani . . . . . . O2 O 0.547721(15) 0.5113(2) 0.20837(5) 0.0316 1.0000 Uani . . . . . . C1 C 0.66360(2) -0.0350(3) -0.10029(8) 0.0331 1.0000 Uani . . . . . . C2 C 0.67856(2) 0.0056(3) -0.14939(7) 0.0333 1.0000 Uani . . . . . . C3 C 0.69431(2) 0.2047(4) -0.13616(8) 0.0386 1.0000 Uani . . . . . . C4 C 0.69512(2) 0.3516(3) -0.07404(7) 0.0328 1.0000 Uani . . . . . . C5 C 0.67960(2) 0.2939(3) -0.02716(7) 0.0250 1.0000 Uani . . . . . . C6 C 0.67967(2) 0.4460(3) 0.04015(7) 0.0250 1.0000 Uani . . . . . . C7 C 0.66355(2) 0.3918(3) 0.08548(7) 0.0241 1.0000 Uani . . . . . . C8 C 0.66366(2) 0.5416(3) 0.14707(7) 0.0248 1.0000 Uani . . . . . . C9 C 0.67997(2) 0.7375(3) 0.16117(7) 0.0266 1.0000 Uani . . . . . . C10 C 0.69562(2) 0.7739(3) 0.11385(7) 0.0250 1.0000 Uani . . . . . . C11 C 0.71352(2) 0.9800(3) 0.12853(7) 0.0273 1.0000 Uani . . . . . . C12 C 0.72916(2) 1.0230(3) 0.08088(8) 0.0336 1.0000 Uani . . . . . . C13 C 0.74541(2) 1.2168(3) 0.09654(9) 0.0373 1.0000 Uani . . . . . . C14 C 0.74554(2) 1.3640(3) 0.15798(9) 0.0380 1.0000 Uani . . . . . . C15 C 0.72944(2) 1.3076(3) 0.20212(8) 0.0354 1.0000 Uani . . . . . . C16 C 0.62421(2) 0.2698(3) 0.16468(7) 0.0246 1.0000 Uani . . . . . . C17 C 0.60440(2) 0.2489(3) 0.20602(6) 0.0226 1.0000 Uani . . . . . . C18 C 0.60485(2) 0.0649(2) 0.26133(7) 0.0227 1.0000 Uani . . . . . . C19 C 0.58614(2) 0.0364(2) 0.29736(6) 0.0225 1.0000 Uani . . . . . . C20 C 0.56734(2) 0.1903(3) 0.27814(7) 0.0252 1.0000 Uani . . . . . . C21 C 0.56714(2) 0.3737(3) 0.22324(7) 0.0255 1.0000 Uani . . . . . . C22 C 0.58569(2) 0.4067(3) 0.18654(7) 0.0244 1.0000 Uani . . . . . . C23 C 0.60381(2) -0.2943(3) 0.37404(7) 0.0255 1.0000 Uani . . . . . . C24 C 0.59890(2) -0.4864(3) 0.43126(6) 0.0234 1.0000 Uani . . . . . . C25 C 0.61676(2) -0.6036(3) 0.47211(7) 0.0279 1.0000 Uani . . . . . . C26 C 0.61331(2) -0.7966(3) 0.52221(7) 0.0324 1.0000 Uani . . . . . . C27 C 0.59201(2) -0.8772(3) 0.53247(7) 0.0316 1.0000 Uani . . . . . . C28 C 0.57421(2) -0.7575(3) 0.49302(7) 0.0298 1.0000 Uani . . . . . . C29 C 0.57768(2) -0.5627(3) 0.44247(7) 0.0279 1.0000 Uani . . . . . . C30 C 0.54494(2) 0.6666(3) 0.14502(7) 0.0308 1.0000 Uani . . . . . . C31 C 0.52069(2) 0.7408(3) 0.13132(7) 0.0293 1.0000 Uani D U . . . . C34 C 0.47595(2) 0.8656(3) 0.10476(8) 0.0347 1.0000 Uani D U . . . . C32 C 0.51071(5) 0.7699(6) 0.06458(15) 0.0345 0.5000 Uani D U . . . . C33 C 0.48848(5) 0.8352(6) 0.05071(16) 0.0360 0.5000 Uani D U . . . . C35 C 0.48473(5) 0.8319(8) 0.17430(16) 0.0434 0.5000 Uani D U . . . . C36 C 0.50733(5) 0.7729(7) 0.18810(15) 0.0401 0.5000 Uani D U . . . . C320 C 0.50572(5) 0.5445(6) 0.1028(2) 0.0454 0.5000 Uani D U . . . . C330 C 0.48352(6) 0.6084(7) 0.0905(2) 0.0493 0.5000 Uani D U . . . . C350 C 0.49136(5) 1.0614(6) 0.12941(17) 0.0378 0.5000 Uani D U . . . . C360 C 0.51366(5) 0.9961(6) 0.14176(16) 0.0352 0.5000 Uani D U . . . . H11 H 0.6523 -0.1706 -0.1100 0.0377 1.0000 Uiso R . . . . . H21 H 0.6779 -0.1021 -0.1914 0.0414 1.0000 Uiso R . . . . . H31 H 0.7047 0.2411 -0.1695 0.0468 1.0000 Uiso R . . . . . H41 H 0.7060 0.4905 -0.0635 0.0376 1.0000 Uiso R . . . . . H71 H 0.6526 0.2533 0.0743 0.0292 1.0000 Uiso R . . . . . H91 H 0.6804 0.8456 0.2030 0.0320 1.0000 Uiso R . . . . . H121 H 0.7287 0.9203 0.0381 0.0381 1.0000 Uiso R . . . . . H131 H 0.7564 1.2483 0.0649 0.0456 1.0000 Uiso R . . . . . H141 H 0.7565 1.5016 0.1697 0.0436 1.0000 Uiso R . . . . . H151 H 0.7296 1.4101 0.2448 0.0434 1.0000 Uiso R . . . . . H161 H 0.6309 0.0940 0.1617 0.0295 1.0000 Uiso R . . . . . H162 H 0.6196 0.3354 0.1182 0.0295 1.0000 Uiso R . . . . . H181 H 0.6179 -0.0406 0.2747 0.0264 1.0000 Uiso R . . . . . H201 H 0.5545 0.1691 0.3029 0.0307 1.0000 Uiso R . . . . . H221 H 0.5856 0.5348 0.1487 0.0285 1.0000 Uiso R . . . . . H231 H 0.6156 -0.1740 0.3914 0.0299 1.0000 Uiso R . . . . . H232 H 0.6082 -0.3959 0.3350 0.0299 1.0000 Uiso R . . . . . H251 H 0.6315 -0.5483 0.4654 0.0326 1.0000 Uiso R . . . . . H261 H 0.6257 -0.8756 0.5501 0.0385 1.0000 Uiso R . . . . . H271 H 0.5896 -1.0154 0.5662 0.0380 1.0000 Uiso R . . . . . H281 H 0.5594 -0.8089 0.5009 0.0356 1.0000 Uiso R . . . . . H291 H 0.5652 -0.4815 0.4152 0.0326 1.0000 Uiso R . . . . . H301 H 0.5537 0.8285 0.1503 0.0383 1.0000 Uiso R . . . . . H302 H 0.5493 0.5612 0.1066 0.0383 1.0000 Uiso R . . . . . H341 H 0.4606 0.9136 0.0948 0.0416 1.0000 Uiso R . . . . . H321 H 0.5194 0.7456 0.0259 0.0408 0.5000 Uiso R . . . . . H331 H 0.4820 0.8576 0.0031 0.0447 0.5000 Uiso R . . . . . H351 H 0.4756 0.8468 0.2122 0.0510 0.5000 Uiso R . . . . . H361 H 0.5139 0.7533 0.2357 0.0468 0.5000 Uiso R . . . . . H3201 H 0.5110 0.3700 0.0895 0.0581 0.5000 Uiso R . . . . . H3301 H 0.4731 0.4706 0.0736 0.0581 0.5000 Uiso R . . . . . H3501 H 0.4864 1.2420 0.1384 0.0449 0.5000 Uiso R . . . . . H3601 H 0.5242 1.1360 0.1561 0.0412 0.5000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.02752(15) 0.03115(17) 0.02579(16) -0.00453(14) 0.00816(11) -0.00491(14) N1 0.0327(6) 0.0314(6) 0.0273(6) 0.0000(5) 0.0075(4) -0.0007(5) N2 0.0224(5) 0.0273(5) 0.0281(5) 0.0027(5) 0.0028(4) 0.0004(5) N3 0.0314(6) 0.0309(6) 0.0349(6) -0.0006(5) 0.0013(5) -0.0007(5) O1 0.0280(5) 0.0266(5) 0.0278(5) 0.0075(4) 0.0070(3) 0.0049(4) O2 0.0274(5) 0.0392(5) 0.0287(5) 0.0121(5) 0.0053(3) 0.0089(4) C1 0.0361(7) 0.0337(8) 0.0295(6) -0.0013(6) 0.0029(5) -0.0041(6) C2 0.0378(7) 0.0377(8) 0.0250(6) -0.0006(7) 0.0060(5) 0.0013(7) C3 0.0346(7) 0.0515(9) 0.0315(7) 0.0015(7) 0.0125(6) -0.0034(7) C4 0.0284(7) 0.0415(8) 0.0292(7) -0.0025(6) 0.0067(5) -0.0058(6) C5 0.0226(6) 0.0269(6) 0.0257(6) 0.0025(5) 0.0035(5) 0.0027(5) C6 0.0208(6) 0.0270(7) 0.0276(6) 0.0040(5) 0.0035(4) 0.0046(5) C7 0.0221(6) 0.0238(6) 0.0267(6) 0.0017(5) 0.0039(5) 0.0009(5) C8 0.0239(5) 0.0245(6) 0.0264(6) 0.0047(5) 0.0040(4) 0.0042(5) C9 0.0252(6) 0.0265(7) 0.0282(6) -0.0033(5) 0.0030(5) 0.0004(5) C10 0.0212(6) 0.0256(6) 0.0281(6) 0.0054(5) 0.0021(5) 0.0019(5) C11 0.0258(6) 0.0255(6) 0.0299(6) 0.0050(6) 0.0000(5) -0.0004(5) C12 0.0285(7) 0.0377(8) 0.0345(7) 0.0058(6) 0.0035(5) -0.0023(6) C13 0.0279(7) 0.0420(8) 0.0419(8) 0.0074(7) 0.0031(6) -0.0085(6) C14 0.0294(7) 0.0344(8) 0.0490(9) 0.0036(7) -0.0020(6) -0.0090(6) C15 0.0351(7) 0.0307(7) 0.0391(8) -0.0001(6) -0.0024(6) -0.0037(6) C16 0.0270(6) 0.0255(6) 0.0223(6) -0.0012(5) 0.0071(5) -0.0015(5) C17 0.0263(6) 0.0212(6) 0.0208(5) -0.0046(5) 0.0050(4) -0.0030(5) C18 0.0236(6) 0.0196(6) 0.0252(6) -0.0025(5) 0.0039(5) 0.0006(4) C19 0.0287(6) 0.0198(6) 0.0190(5) 0.0008(5) 0.0032(4) -0.0020(5) C20 0.0244(6) 0.0288(7) 0.0231(6) 0.0006(5) 0.0060(5) -0.0006(5) C21 0.0241(6) 0.0264(6) 0.0260(6) 0.0016(5) 0.0023(5) 0.0010(5) C22 0.0291(6) 0.0237(6) 0.0206(6) 0.0031(5) 0.0042(5) -0.0017(5) C23 0.0261(6) 0.0250(6) 0.0259(6) -0.0001(5) 0.0046(5) 0.0006(5) C24 0.0296(6) 0.0194(6) 0.0213(5) -0.0041(5) 0.0031(4) 0.0012(5) C25 0.0314(7) 0.0260(6) 0.0263(6) 0.0011(5) 0.0028(5) 0.0024(5) C26 0.0377(7) 0.0307(7) 0.0287(7) 0.0009(6) 0.0026(5) 0.0074(6) C27 0.0494(8) 0.0222(6) 0.0241(6) 0.0032(5) 0.0087(6) 0.0016(6) C28 0.0334(7) 0.0288(7) 0.0276(6) -0.0013(6) 0.0047(5) -0.0062(6) C29 0.0314(7) 0.0283(7) 0.0235(6) -0.0013(5) 0.0002(5) 0.0013(5) C30 0.0297(6) 0.0321(7) 0.0307(7) 0.0057(6) 0.0040(5) 0.0003(5) C31 0.0313(7) 0.0269(7) 0.0294(7) 0.0035(6) 0.0020(5) 0.0028(5) C34 0.0301(7) 0.0385(8) 0.0345(7) 0.0042(6) -0.0013(5) 0.0065(6) C32 0.0379(15) 0.0379(16) 0.0277(13) -0.0027(12) 0.0033(11) 0.0014(12) C33 0.0387(15) 0.0346(15) 0.0329(14) 0.0021(13) -0.0044(11) 0.0055(13) C35 0.0455(18) 0.053(2) 0.0334(14) 0.0044(14) 0.0113(13) 0.0190(15) C36 0.0455(17) 0.0527(19) 0.0218(12) 0.0033(13) 0.0021(11) 0.0167(15) C320 0.0349(16) 0.0316(16) 0.068(2) -0.0081(15) -0.0011(14) 0.0060(12) C330 0.0403(18) 0.0375(17) 0.068(2) -0.0118(17) -0.0064(15) 0.0004(15) C350 0.0393(16) 0.0274(14) 0.0470(17) 0.0068(13) 0.0057(13) 0.0112(11) C360 0.0356(14) 0.0307(14) 0.0391(15) 0.0019(13) 0.0025(11) -0.0026(13) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.11163(19) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 . C8 . 1.7598(13) yes S1 . C16 . 1.8209(13) yes N1 . C1 . 1.3373(19) yes N1 . C5 . 1.3387(18) yes N2 . C6 . 1.3400(18) yes N2 . C10 . 1.3423(18) yes N3 . C11 . 1.3408(19) yes N3 . C15 . 1.3391(19) yes O1 . C19 . 1.3631(15) yes O1 . C23 . 1.4214(15) yes O2 . C21 . 1.3648(16) yes O2 . C30 . 1.4280(16) yes C1 . C2 . 1.388(2) yes C1 . H11 . 0.960 no C2 . C3 . 1.376(2) yes C2 . H21 . 0.960 no C3 . C4 . 1.388(2) yes C3 . H31 . 0.960 no C4 . C5 . 1.3964(18) yes C4 . H41 . 0.960 no C5 . C6 . 1.4892(18) yes C6 . C7 . 1.3995(17) yes C7 . C8 . 1.3898(19) yes C7 . H71 . 0.960 no C8 . C9 . 1.3896(19) yes C9 . C10 . 1.3910(18) yes C9 . H91 . 0.960 no C10 . C11 . 1.4932(18) yes C11 . C12 . 1.3995(19) yes C12 . C13 . 1.384(2) yes C12 . H121 . 0.960 no C13 . C14 . 1.380(2) yes C13 . H131 . 0.960 no C14 . C15 . 1.385(2) yes C14 . H141 . 0.960 no C15 . H151 . 0.960 no C16 . C17 . 1.5110(17) yes C16 . H161 . 0.960 no C16 . H162 . 0.960 no C17 . C18 . 1.3916(18) yes C17 . C22 . 1.3954(18) yes C18 . C19 . 1.3967(17) yes C18 . H181 . 0.960 no C19 . C20 . 1.3882(18) yes C20 . C21 . 1.3847(19) yes C20 . H201 . 0.960 no C21 . C22 . 1.3976(18) yes C22 . H221 . 0.960 no C23 . C24 . 1.5006(18) yes C23 . H231 . 0.960 no C23 . H232 . 0.960 no C24 . C25 . 1.3944(18) yes C24 . C29 . 1.3803(19) yes C25 . C26 . 1.381(2) yes C25 . H251 . 0.960 no C26 . C27 . 1.387(2) yes C26 . H261 . 0.960 no C27 . C28 . 1.384(2) yes C27 . H271 . 0.960 no C28 . C29 . 1.394(2) yes C28 . H281 . 0.960 no C29 . H291 . 0.960 no C30 . C31 . 1.5142(19) yes C30 . H301 . 0.960 no C30 . H302 . 0.960 no C31 . C32 . 1.362(3) yes C31 . C36 . 1.431(3) yes C31 . C320 . 1.399(3) yes C31 . C360 . 1.350(3) yes C34 . C33 . 1.355(3) yes C34 . C35 . 1.390(3) yes C34 . C330 . 1.385(4) yes C34 . C350 . 1.392(3) yes C34 . H341 . 0.960 no C32 . C33 . 1.386(4) yes C32 . C320 . 1.380(5) yes C32 . C360 . 1.843(4) yes C32 . H321 . 0.960 no C33 . C330 . 1.402(5) yes C33 . H331 . 0.960 no C35 . C36 . 1.401(4) yes C35 . C350 . 1.500(5) yes C35 . H351 . 0.960 no C36 . C360 . 1.488(4) yes C36 . H361 . 0.960 no C320 . C330 . 1.381(4) yes C320 . H3201 . 0.960 no C330 . H3301 . 0.960 no C350 . C360 . 1.388(4) yes C350 . H3501 . 0.960 no C360 . H3601 . 0.960 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C8 . S1 . C16 . 102.68(6) yes C1 . N1 . C5 . 117.73(12) yes C6 . N2 . C10 . 117.40(11) yes C11 . N3 . C15 . 117.31(13) yes C19 . O1 . C23 . 116.88(10) yes C21 . O2 . C30 . 117.79(10) yes N1 . C1 . C2 . 123.74(14) yes N1 . C1 . H11 . 118.055 no C2 . C1 . H11 . 118.207 no C1 . C2 . C3 . 118.05(13) yes C1 . C2 . H21 . 120.864 no C3 . C2 . H21 . 121.081 no C2 . C3 . C4 . 119.44(13) yes C2 . C3 . H31 . 120.319 no C4 . C3 . H31 . 120.240 no C3 . C4 . C5 . 118.53(13) yes C3 . C4 . H41 . 120.951 no C5 . C4 . H41 . 120.514 no C4 . C5 . N1 . 122.47(13) yes C4 . C5 . C6 . 120.77(12) yes N1 . C5 . C6 . 116.75(11) yes C5 . C6 . N2 . 116.83(11) yes C5 . C6 . C7 . 120.03(12) yes N2 . C6 . C7 . 123.14(12) yes C6 . C7 . C8 . 118.83(12) yes C6 . C7 . H71 . 120.685 no C8 . C7 . H71 . 120.489 no S1 . C8 . C7 . 124.57(10) yes S1 . C8 . C9 . 117.15(10) yes C7 . C8 . C9 . 118.27(12) yes C8 . C9 . C10 . 119.04(12) yes C8 . C9 . H91 . 120.380 no C10 . C9 . H91 . 120.584 no C9 . C10 . N2 . 123.30(12) yes C9 . C10 . C11 . 119.96(12) yes N2 . C10 . C11 . 116.74(11) yes C10 . C11 . N3 . 116.69(12) yes C10 . C11 . C12 . 120.73(13) yes N3 . C11 . C12 . 122.58(13) yes C11 . C12 . C13 . 118.74(15) yes C11 . C12 . H121 . 120.908 no C13 . C12 . H121 . 120.353 no C12 . C13 . C14 . 119.16(14) yes C12 . C13 . H131 . 120.245 no C14 . C13 . H131 . 120.592 no C13 . C14 . C15 . 118.17(14) yes C13 . C14 . H141 . 120.802 no C15 . C14 . H141 . 121.031 no C14 . C15 . N3 . 124.03(15) yes C14 . C15 . H151 . 117.995 no N3 . C15 . H151 . 117.976 no S1 . C16 . C17 . 109.47(9) yes S1 . C16 . H161 . 109.319 no C17 . C16 . H161 . 109.439 no S1 . C16 . H162 . 109.478 no C17 . C16 . H162 . 109.650 no H161 . C16 . H162 . 109.467 no C16 . C17 . C18 . 119.22(11) yes C16 . C17 . C22 . 119.57(11) yes C18 . C17 . C22 . 121.16(12) yes C17 . C18 . C19 . 119.20(11) yes C17 . C18 . H181 . 120.366 no C19 . C18 . H181 . 120.431 no C18 . C19 . O1 . 124.26(11) yes C18 . C19 . C20 . 120.25(11) yes O1 . C19 . C20 . 115.48(11) yes C19 . C20 . C21 . 119.97(12) yes C19 . C20 . H201 . 119.917 no C21 . C20 . H201 . 120.110 no C20 . C21 . O2 . 114.93(11) yes C20 . C21 . C22 . 120.87(12) yes O2 . C21 . C22 . 124.20(12) yes C21 . C22 . C17 . 118.54(12) yes C21 . C22 . H221 . 120.752 no C17 . C22 . H221 . 120.704 no O1 . C23 . C24 . 109.80(10) yes O1 . C23 . H231 . 109.422 no C24 . C23 . H231 . 109.534 no O1 . C23 . H232 . 109.258 no C24 . C23 . H232 . 109.343 no H231 . C23 . H232 . 109.466 no C23 . C24 . C25 . 117.87(11) yes C23 . C24 . C29 . 123.03(12) yes C25 . C24 . C29 . 118.99(12) yes C24 . C25 . C26 . 120.55(13) yes C24 . C25 . H251 . 119.466 no C26 . C25 . H251 . 119.984 no C25 . C26 . C27 . 120.44(13) yes C25 . C26 . H261 . 119.783 no C27 . C26 . H261 . 119.778 no C26 . C27 . C28 . 119.21(13) yes C26 . C27 . H271 . 120.464 no C28 . C27 . H271 . 120.321 no C27 . C28 . C29 . 120.34(13) yes C27 . C28 . H281 . 119.534 no C29 . C28 . H281 . 120.124 no C28 . C29 . C24 . 120.44(13) yes C28 . C29 . H291 . 119.759 no C24 . C29 . H291 . 119.801 no O2 . C30 . C31 . 107.65(11) yes O2 . C30 . H301 . 109.975 no C31 . C30 . H301 . 109.767 no O2 . C30 . H302 . 109.966 no C31 . C30 . H302 . 109.993 no H301 . C30 . H302 . 109.466 no C30 . C31 . C32 . 121.16(17) yes C30 . C31 . C36 . 120.92(15) yes C32 . C31 . C36 . 117.88(19) yes C30 . C31 . C320 . 118.77(17) yes C32 . C31 . C320 . 60.0(2) yes C36 . C31 . C320 . 88.6(2) yes C30 . C31 . C360 . 121.09(17) yes C32 . C31 . C360 . 85.63(19) yes C36 . C31 . C360 . 64.6(2) yes C320 . C31 . C360 . 120.0(2) yes C33 . C34 . C35 . 121.8(2) yes C33 . C34 . C330 . 61.6(2) yes C35 . C34 . C330 . 88.7(2) yes C33 . C34 . C350 . 85.6(2) yes C35 . C34 . C350 . 65.2(2) yes C330 . C34 . C350 . 118.4(2) yes C33 . C34 . H341 . 119.150 no C35 . C34 . H341 . 119.063 no C330 . C34 . H341 . 121.440 no C350 . C34 . H341 . 120.011 no C31 . C32 . C33 . 122.2(3) yes C31 . C32 . C320 . 61.33(19) yes C33 . C32 . C320 . 91.4(3) yes C31 . C32 . C360 . 46.90(14) yes C33 . C32 . C360 . 91.4(2) yes C320 . C32 . C360 . 94.1(2) yes C31 . C32 . H321 . 118.830 no C33 . C32 . H321 . 118.962 no C320 . C32 . H321 . 118.395 no C360 . C32 . H321 . 132.624 no C32 . C33 . C34 . 119.6(2) yes C32 . C33 . C330 . 88.4(2) yes C34 . C33 . C330 . 60.3(2) yes C32 . C33 . H331 . 120.358 no C34 . C33 . H331 . 120.085 no C330 . C33 . H331 . 121.015 no C34 . C35 . C36 . 118.4(3) yes C34 . C35 . C350 . 57.44(19) yes C36 . C35 . C350 . 87.0(3) yes C34 . C35 . H351 . 121.289 no C36 . C35 . H351 . 120.307 no C350 . C35 . H351 . 125.811 no C31 . C36 . C35 . 120.1(2) yes C31 . C36 . C360 . 55.06(17) yes C35 . C36 . C360 . 92.5(3) yes C31 . C36 . H361 . 119.599 no C35 . C36 . H361 . 120.276 no C360 . C36 . H361 . 122.020 no C31 . C320 . C32 . 58.70(18) yes C31 . C320 . C330 . 119.5(3) yes C32 . C320 . C330 . 89.5(3) yes C31 . C320 . H3201 . 120.206 no C32 . C320 . H3201 . 118.927 no C330 . C320 . H3201 . 120.253 no C33 . C330 . C34 . 58.1(2) yes C33 . C330 . C320 . 90.7(3) yes C34 . C330 . C320 . 120.9(3) yes C33 . C330 . H3301 . 123.488 no C34 . C330 . H3301 . 119.534 no C320 . C330 . H3301 . 119.509 no C35 . C350 . C34 . 57.32(18) yes C35 . C350 . C360 . 92.5(2) yes C34 . C350 . C360 . 120.4(3) yes C35 . C350 . H3501 . 119.270 no C34 . C350 . H3501 . 119.516 no C360 . C350 . H3501 . 120.039 no C36 . C360 . C350 . 88.0(2) yes C36 . C360 . C31 . 60.30(18) yes C350 . C360 . C31 . 120.6(3) yes C36 . C360 . C32 . 91.2(2) yes C350 . C360 . C32 . 89.6(2) yes C31 . C360 . C32 . 47.47(15) yes C36 . C360 . H3601 . 124.516 no C350 . C360 . H3601 . 119.364 no C31 . C360 . H3601 . 120.011 no C32 . C360 . H3601 . 131.957 no data_ls_a94_173k _database_code_depnum_ccdc_archive 'CCDC 283215' _audit_creation_date 05-06-22 _audit_creation_method CRYSTALS_ver_12.24 _oxford_structure_analysis_title '7061710 ls_a94_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 7.8119(3) _cell_length_b 17.8280(6) _cell_length_c 11.3151(5) _cell_angle_alpha 90 _cell_angle_beta 92.703(2) _cell_angle_gamma 90 _cell_volume 1574.11(10) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C16 H13 Cl2 N3 S1' _chemical_formula_moiety 'C15 H11 N3 S, C H2 Cl2' _chemical_compound_source ? _chemical_formula_weight 350.27 _cell_measurement_reflns_used 2358 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _cell_measurement_temperature 173 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_min 0.24 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_max 0.28 _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.544 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.88 # Sheldrick geometric definitions 0.86 0.88 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' _computing_data_collection 'COLLECT (Nonius BV, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 173 _diffrn_reflns_number 4572 _reflns_number_total 2305 _diffrn_reflns_av_R_equivalents 0.031 # Number of reflections with Friedels Law is 2305 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 2314 _diffrn_reflns_theta_min 3.306 _diffrn_reflns_theta_max 30.089 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.089 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 24 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.21 _refine_diff_density_max 0.22 _refine_ls_number_reflns 1209 _refine_ls_number_restraints 6 _refine_ls_number_parameters 107 #_refine_ls_R_factor_ref 0.0351 _refine_ls_wR_factor_ref 0.0372 _refine_ls_goodness_of_fit_ref 1.1341 #_reflns_number_all 2294 _refine_ls_R_factor_all 0.0829 _refine_ls_wR_factor_all 0.0886 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>2.00u(I) _reflns_number_gt 1209 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_gt 0.0372 _refine_ls_shift/su_max 0.000348 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.220 0.149 0.639E-01 ; _publ_section_abstract # Text of the abstract ; ? ; _publ_section_comment # Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen ; H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, (1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens C1 C -0.2607(3) -0.07887(12) 0.51999(19) 0.0357 1.0000 Uani . . . . . . C2 C -0.3363(3) -0.05447(12) 0.4135(2) 0.0367 1.0000 Uani . . . . . . C3 C -0.3331(3) 0.02139(13) 0.3884(2) 0.0372 1.0000 Uani . . . . . . C4 C -0.2555(3) 0.07009(12) 0.46944(18) 0.0339 1.0000 Uani . . . . . . C5 C -0.1809(2) 0.04082(11) 0.57340(18) 0.0290 1.0000 Uani . . . . . . C6 C -0.0907(2) 0.08919(11) 0.66252(17) 0.0281 1.0000 Uani . . . . . . C7 C -0.0927(3) 0.16621(11) 0.66224(18) 0.0326 1.0000 Uani . . . . . . C8 C 0.0000 0.20808(16) 0.7500 0.0312 1.0000 Uani S T . . . . C9 C 0.000000(10) 0.19519(19) 0.250000(10) 0.0512 1.0000 Uani S T . . . . S1 S 0.0000 0.30352(4) 0.7500 0.0469 1.0000 Uani S T . . . . Cl1 Cl 0.01930(8) 0.25014(4) 0.37946(6) 0.0542 1.0000 Uani . . . . . . N1 N -0.1824(2) -0.03290(10) 0.59930(15) 0.0323 1.0000 Uani . . . . . . N2 N 0.000000(7) 0.05256(12) 0.750000(7) 0.0278 1.0000 Uani S T . . . . H2 H 0.0000 0.0005 0.7500 0.0400 1.0000 Uiso RS . . . . . H11 H -0.2592 -0.1301 0.5410 0.0401 1.0000 Uiso R . . . . . H21 H -0.3896 -0.0888 0.3610 0.0414 1.0000 Uiso R . . . . . H31 H -0.3843 0.0393 0.3173 0.0428 1.0000 Uiso R . . . . . H41 H -0.2569 0.1217 0.4527 0.0423 1.0000 Uiso R . . . . . H71 H -0.1575 0.1913 0.6025 0.0368 1.0000 Uiso R . . . . . H91 H -0.0979 0.1639 0.2499 0.0589 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0387(11) 0.0299(9) 0.0382(14) -0.0029(8) -0.0010(10) 0.0009(9) C2 0.0343(12) 0.0414(11) 0.0342(12) -0.0085(9) -0.0005(9) 0.0008(9) C3 0.0350(11) 0.0450(12) 0.0310(11) 0.0005(9) -0.0049(8) 0.0029(10) C4 0.0330(10) 0.0361(11) 0.0323(12) 0.0030(8) -0.0017(9) 0.0025(8) C5 0.0241(9) 0.0332(9) 0.0298(10) 0.0006(8) 0.0006(7) 0.0017(8) C6 0.0260(9) 0.0303(9) 0.0281(10) 0.0011(8) 0.0011(7) -0.0003(8) C7 0.0331(10) 0.0316(10) 0.0328(10) 0.0034(8) -0.0014(8) 0.0027(8) C8 0.0277(14) 0.0294(14) 0.0365(16) 0.0000 0.0027(12) 0.0000 C9 0.070(2) 0.0310(15) 0.052(2) 0.0000 -0.0057(18) 0.0000 S1 0.0554(5) 0.0246(3) 0.0598(6) 0.0000 -0.0065(4) 0.0000 Cl1 0.0553(4) 0.0459(3) 0.0608(4) -0.0110(3) -0.0024(3) 0.0029(3) N1 0.0339(9) 0.0298(8) 0.0328(9) 0.0006(7) -0.0027(7) 0.0001(7) N2 0.0282(11) 0.0251(10) 0.0298(12) 0.0000 0.0000(9) 0.0000 _refine_ls_extinction_coef 30(3) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' _oxford_refine_ls_scale 0.1570(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 . C2 . 1.387(3) yes C1 . N1 . 1.341(3) yes C1 . H11 . 0.944 no C2 . C3 . 1.382(3) yes C2 . H21 . 0.937 no C3 . C4 . 1.382(3) yes C3 . H31 . 0.937 no C4 . C5 . 1.390(3) yes C4 . H41 . 0.940 no C5 . C6 . 1.480(3) yes C5 . N1 . 1.347(3) yes C6 . C7 . 1.373(3) yes C6 . N2 . 1.357(2) yes C7 . C8 . 1.414(3) yes C7 . H71 . 0.938 no C8 . S1 . 1.702(3) yes C9 . Cl1 5_555 1.763(2) yes C9 . H91 5_555 0.946 no C9 . Cl1 . 1.763(2) yes C9 . H91 . 0.946 no N2 . H2 . 0.928 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 . C1 . N1 . 123.5(2) yes C2 . C1 . H11 . 121.487 no N1 . C1 . H11 . 115.014 no C1 . C2 . C3 . 118.3(2) yes C1 . C2 . H21 . 120.274 no C3 . C2 . H21 . 121.426 no C2 . C3 . C4 . 119.4(2) yes C2 . C3 . H31 . 119.903 no C4 . C3 . H31 . 120.736 no C3 . C4 . C5 . 118.6(2) yes C3 . C4 . H41 . 118.732 no C5 . C4 . H41 . 122.637 no C4 . C5 . C6 . 121.68(18) yes C4 . C5 . N1 . 122.90(19) yes C6 . C5 . N1 . 115.41(17) yes C5 . C6 . C7 . 125.16(18) yes C5 . C6 . N2 . 115.60(17) yes C7 . C6 . N2 . 119.24(18) yes C6 . C7 . C8 . 121.4(2) yes C6 . C7 . H71 . 118.932 no C8 . C7 . H71 . 119.690 no C7 5_556 C8 . C7 . 116.3(3) yes C7 5_556 C8 . S1 . 121.86(13) yes C7 . C8 . S1 . 121.86(13) yes Cl1 5_555 C9 . H91 5_555 111.444 no Cl1 5_555 C9 . Cl1 . 112.47(19) yes H91 5_555 C9 . Cl1 . 106.817 no Cl1 5_555 C9 . H91 . 106.817 no H91 5_555 C9 . H91 . 107.796 no Cl1 . C9 . H91 . 111.444 no C5 . N1 . C1 . 117.33(18) yes C6 . N2 . C6 5_556 122.5(2) yes C6 . N2 . H2 . 118.761 no C6 5_556 N2 . H2 . 118.761 no data_ls_a95_173k _database_code_depnum_ccdc_archive 'CCDC 283216' _audit_creation_date 04-08-24 _audit_creation_method CRYSTALS_ver_12.24 _oxford_structure_analysis_title '8241153 ls_a95_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 11.5557(4) _cell_length_b 5.5221(2) _cell_length_c 22.6510(9) _cell_angle_alpha 90 _cell_angle_beta 120.5668(15) _cell_angle_gamma 90 _cell_volume 1244.54(8) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2/c' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y,-z+1/2 x,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 _chemical_formula_sum 'C30 H20 N6 S2' _chemical_formula_moiety 'C30 H20 N6 S2' _chemical_compound_source ? _chemical_formula_weight 528.66 _cell_measurement_reflns_used 5906 _cell_measurement_theta_min 3 _cell_measurement_theta_max 29 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_max 0.24 _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 0.247 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_absorpt_correction_T_min 0.98 _exptl_absorpt_correction_T_max 0.99 # Sheldrick geometric definitions 0.98 0.99 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' _computing_data_collection 'COLLECT (Nonius BV, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 173 _diffrn_reflns_number 12042 _reflns_number_total 3333 _diffrn_reflns_av_R_equivalents 0.028 # Number of reflections with Friedels Law is 3333 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3349 _diffrn_reflns_theta_min 3.526 _diffrn_reflns_theta_max 29.127 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.544 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _reflns_limit_h_min -15 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 7 _reflns_limit_l_min 0 _reflns_limit_l_max 30 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.26 _refine_diff_density_max 0.35 _refine_ls_number_reflns 1876 _refine_ls_number_restraints 0 _refine_ls_number_parameters 172 #_refine_ls_R_factor_ref 0.0485 _refine_ls_wR_factor_ref 0.0465 _refine_ls_goodness_of_fit_ref 1.0807 #_reflns_number_all 3318 _refine_ls_R_factor_all 0.1003 _refine_ls_wR_factor_all 0.0746 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>1.00u(I) _reflns_number_gt 1876 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_gt 0.0465 _refine_ls_shift/su_max 0.000146 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.574 0.621 0.353 ; _publ_section_abstract # Text of the abstract ; ? ; _publ_section_comment # Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen ; H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, (1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens S1 S 0.47844(6) 0.41909(11) 0.20065(3) 0.0389 1.0000 Uani . . . . . . N1 N 0.6463(2) 0.2195(4) 0.02955(10) 0.0500 1.0000 Uani . . . . . . N2 N 0.75318(17) -0.1307(3) 0.18267(9) 0.0336 1.0000 Uani . . . . . . N3 N 0.8241(2) -0.2982(4) 0.35135(10) 0.0423 1.0000 Uani . . . . . . C1 C 0.6594(3) 0.2187(6) -0.02610(13) 0.0568 1.0000 Uani . . . . . . C2 C 0.7232(2) 0.0428(6) -0.04115(12) 0.0495 1.0000 Uani . . . . . . C3 C 0.7778(3) -0.1480(6) 0.00404(14) 0.0565 1.0000 Uani . . . . . . C4 C 0.7661(3) -0.1543(5) 0.06190(13) 0.0480 1.0000 Uani . . . . . . C5 C 0.6996(2) 0.0326(4) 0.07284(11) 0.0359 1.0000 Uani . . . . . . C6 C 0.6842(2) 0.0374(4) 0.13430(11) 0.0331 1.0000 Uani . . . . . . C7 C 0.6017(2) 0.2082(4) 0.13982(11) 0.0357 1.0000 Uani . . . . . . C8 C 0.58806(19) 0.2016(4) 0.19738(11) 0.0327 1.0000 Uani . . . . . . C9 C 0.65733(19) 0.0266(4) 0.24763(11) 0.0331 1.0000 Uani . . . . . . C10 C 0.7401(2) -0.1325(4) 0.23823(11) 0.0324 1.0000 Uani . . . . . . C11 C 0.82028(19) -0.3191(4) 0.29120(10) 0.0332 1.0000 Uani . . . . . . C12 C 0.8863(2) -0.5031(5) 0.27803(12) 0.0387 1.0000 Uani . . . . . . C13 C 0.9587(2) -0.6732(5) 0.32862(13) 0.0450 1.0000 Uani . . . . . . C14 C 0.9626(2) -0.6534(5) 0.39034(13) 0.0490 1.0000 Uani . . . . . . C15 C 0.8945(2) -0.4655(5) 0.39911(13) 0.0507 1.0000 Uani . . . . . . H11 H 0.6196 0.3573 -0.0588 0.0680 1.0000 Uiso R . . . . . H21 H 0.7300 0.0517 -0.0834 0.0593 1.0000 Uiso R . . . . . H31 H 0.8255 -0.2810 -0.0049 0.0724 1.0000 Uiso R . . . . . H41 H 0.8050 -0.2916 0.0952 0.0606 1.0000 Uiso R . . . . . H71 H 0.5534 0.3328 0.1033 0.0424 1.0000 Uiso R . . . . . H91 H 0.6479 0.0156 0.2891 0.0415 1.0000 Uiso R . . . . . H121 H 0.8817 -0.5124 0.2328 0.0444 1.0000 Uiso R . . . . . H131 H 1.0070 -0.8076 0.3206 0.0502 1.0000 Uiso R . . . . . H141 H 1.0140 -0.7731 0.4279 0.0532 1.0000 Uiso R . . . . . H151 H 0.8979 -0.4533 0.4440 0.0606 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0375(3) 0.0383(3) 0.0462(3) 0.0059(3) 0.0251(2) 0.0067(3) N1 0.0554(12) 0.0558(14) 0.0407(11) 0.0138(10) 0.0258(10) 0.0136(11) N2 0.0307(8) 0.0380(12) 0.0318(9) 0.0045(7) 0.0156(7) 0.0027(7) N3 0.0415(10) 0.0515(12) 0.0376(10) 0.0116(9) 0.0228(8) 0.0043(10) C1 0.0635(16) 0.0707(19) 0.0359(12) 0.0175(13) 0.0251(12) 0.0080(15) C2 0.0492(13) 0.0697(19) 0.0293(11) -0.0057(12) 0.0198(10) -0.0110(13) C3 0.0668(17) 0.064(2) 0.0496(15) -0.0065(13) 0.0379(14) 0.0029(14) C4 0.0603(15) 0.0478(15) 0.0434(13) 0.0042(11) 0.0320(12) 0.0083(12) C5 0.0324(9) 0.0432(14) 0.0298(10) 0.0029(9) 0.0143(9) -0.0025(9) C6 0.0296(9) 0.0341(12) 0.0338(10) 0.0016(9) 0.0148(8) -0.0001(8) C7 0.0320(10) 0.0386(12) 0.0354(11) 0.0058(9) 0.0165(9) 0.0030(9) C8 0.0258(9) 0.0309(11) 0.0406(12) 0.0008(9) 0.0164(9) 0.0005(8) C9 0.0325(10) 0.0360(12) 0.0351(11) 0.0030(9) 0.0203(9) -0.0005(8) C10 0.0274(9) 0.0354(13) 0.0328(10) 0.0011(8) 0.0142(8) -0.0018(8) C11 0.0263(9) 0.0372(11) 0.0336(11) 0.0052(9) 0.0133(9) -0.0020(9) C12 0.0313(10) 0.0412(12) 0.0387(12) 0.0043(9) 0.0142(10) 0.0024(9) C13 0.0348(11) 0.0400(13) 0.0506(14) 0.0065(11) 0.0148(11) 0.0041(9) C14 0.0379(12) 0.0461(15) 0.0491(14) 0.0198(11) 0.0120(11) 0.0030(10) C15 0.0448(12) 0.0655(18) 0.0415(13) 0.0183(12) 0.0216(11) 0.0027(13) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2293(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 . S1 3_655 2.0281(12) yes S1 . C8 . 1.774(2) yes N1 . C1 . 1.344(3) yes N1 . C5 . 1.339(3) yes N2 . C6 . 1.345(3) yes N2 . C10 . 1.342(3) yes N3 . C11 . 1.346(3) yes N3 . C15 . 1.338(3) yes C1 . C2 . 1.363(4) yes C1 . H11 . 1.000 no C2 . C3 . 1.378(4) yes C2 . H21 . 1.000 no C3 . C4 . 1.385(3) yes C3 . H31 . 1.000 no C4 . C5 . 1.382(3) yes C4 . H41 . 1.000 no C5 . C6 . 1.491(3) yes C6 . C7 . 1.391(3) yes C7 . C8 . 1.391(3) yes C7 . H71 . 1.000 no C8 . C9 . 1.394(3) yes C9 . C10 . 1.393(3) yes C9 . H91 . 1.000 no C10 . C11 . 1.493(3) yes C11 . C12 . 1.391(3) yes C12 . C13 . 1.386(3) yes C12 . H121 . 1.000 no C13 . C14 . 1.380(4) yes C13 . H131 . 1.000 no C14 . C15 . 1.376(4) yes C14 . H141 . 1.000 no C15 . H151 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 3_655 S1 . C8 . 105.41(8) yes C1 . N1 . C5 . 117.1(2) yes C6 . N2 . C10 . 117.81(18) yes C11 . N3 . C15 . 116.9(2) yes N1 . C1 . C2 . 124.8(3) yes N1 . C1 . H11 . 117.618 no C2 . C1 . H11 . 117.629 no C1 . C2 . C3 . 117.4(2) yes C1 . C2 . H21 . 121.294 no C3 . C2 . H21 . 121.290 no C2 . C3 . C4 . 119.6(3) yes C2 . C3 . H31 . 120.172 no C4 . C3 . H31 . 120.188 no C3 . C4 . C5 . 118.8(2) yes C3 . C4 . H41 . 120.602 no C5 . C4 . H41 . 120.632 no C4 . C5 . N1 . 122.4(2) yes C4 . C5 . C6 . 121.5(2) yes N1 . C5 . C6 . 116.2(2) yes C5 . C6 . N2 . 116.46(19) yes C5 . C6 . C7 . 120.58(19) yes N2 . C6 . C7 . 123.0(2) yes C6 . C7 . C8 . 118.4(2) yes C6 . C7 . H71 . 120.792 no C8 . C7 . H71 . 120.791 no S1 . C8 . C7 . 116.43(17) yes S1 . C8 . C9 . 124.11(16) yes C7 . C8 . C9 . 119.4(2) yes C8 . C9 . C10 . 117.8(2) yes C8 . C9 . H91 . 121.107 no C10 . C9 . H91 . 121.102 no C9 . C10 . N2 . 123.5(2) yes C9 . C10 . C11 . 120.40(19) yes N2 . C10 . C11 . 116.07(19) yes C10 . C11 . N3 . 116.2(2) yes C10 . C11 . C12 . 121.0(2) yes N3 . C11 . C12 . 122.7(2) yes C11 . C12 . C13 . 118.9(2) yes C11 . C12 . H121 . 120.550 no C13 . C12 . H121 . 120.521 no C12 . C13 . C14 . 118.7(2) yes C12 . C13 . H131 . 120.669 no C14 . C13 . H131 . 120.667 no C13 . C14 . C15 . 118.6(2) yes C13 . C14 . H141 . 120.674 no C15 . C14 . H141 . 120.704 no C14 . C15 . N3 . 124.1(2) yes C14 . C15 . H151 . 117.917 no N3 . C15 . H151 . 117.939 no data_ls_a134_153k _database_code_depnum_ccdc_archive 'CCDC 283217' _audit_creation_date 05-07-26 _audit_creation_method CRYSTALS_ver_12.24 _oxford_structure_analysis_title '7130929 ls_a134_153k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 25.4086(9) _cell_length_b 20.1144(8) _cell_length_c 34.5052(11) _cell_angle_alpha 90 _cell_angle_beta 91.118(2) _cell_angle_gamma 90 _cell_volume 17631.5(11) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C138 H123.50 B8 F32 Fe4 N29.50 O7 S8' _chemical_formula_moiety ; C120 H80 Fe4 N24 S8, 8(BF4), 5.5(C2H3N), 1.5(C4H10O), CH3O, 4.5(H2O) ; _chemical_compound_source ? _chemical_formula_weight 3481.53 _cell_measurement_reflns_used 20097 _cell_measurement_theta_min 1 _cell_measurement_theta_max 25 _cell_measurement_temperature 153 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_max 0.19 _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 7096 _exptl_absorpt_coefficient_mu 0.508 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 0.95 # Sheldrick geometric definitions 0.91 0.95 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' _computing_data_collection 'COLLECT (Nonius BV, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 153 _diffrn_reflns_number 59868 _reflns_number_total 26995 _diffrn_reflns_av_R_equivalents 0.247 # Number of reflections with Friedels Law is 26995 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 30855 _diffrn_special_details ; Datacollection of the crystals of this compound presented problems. As the scattering power of this crystal was very weak we tried several times to repeat the experiment with newly grown crystals, but we could not find a sample which produced better data. We tried to repeat datacollection with the same sample, but in the meantime the crystal unfortunately had decomposed due to solvent loss. ; _diffrn_reflns_theta_min 1.760 _diffrn_reflns_theta_max 24.948 _diffrn_measured_fraction_theta_max 0.875 _diffrn_reflns_theta_full 18.711 _diffrn_measured_fraction_theta_full 0.924 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 39 _reflns_limit_h_min -30 _reflns_limit_h_max 30 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 40 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.77 _refine_diff_density_max 1.30 _refine_ls_number_reflns 10395 _refine_ls_number_restraints 3787 _refine_ls_number_parameters 1272 #_refine_ls_R_factor_ref 0.1621 _refine_ls_wR_factor_ref 0.1601 _refine_ls_goodness_of_fit_ref 1.1801 #_reflns_number_all 26610 _refine_ls_R_factor_all 0.2783 _refine_ls_wR_factor_all 0.2587 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>1.40u(I) _reflns_number_gt 10395 _refine_ls_R_factor_gt 0.1621 _refine_ls_wR_factor_gt 0.1601 _refine_ls_shift/su_max 0.011809 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 2.61 3.12 2.31 0.855 0.527 ; _refine_special_details ; As described earlier this is the only dataset we could collect from this compound. In order to partially compensate the lack of observed reflections the following measures have been taken: - Groups with known geometries have been refined as rigid bodies. - Solvent molecules have been refined with a common isotropic U-value. - BF4 molecules have been refined with a common isotropic U-value for the fluorine atoms. - Restraints have been used to optimize the geometry of the remaining structure fragments using common mean values for series of equivalent bonds. The difference map still shows maxima in the solvent areas. Calculations with Platon show that there are still potentially solvent accessible areas in the structure (about 11% of the volume of the unit cell or roughly 500 cubic Angstrom per assymetric unit). As the electron density distribution does not any more show clearly identifiable features we have left the refinement at this stage knowing that there are with very high probability more solvent molecules present in this structure. (Please note that this result has been reached without using SQUEEZE.) ; _publ_section_abstract # Text of the abstract ; ? ; _publ_section_comment # Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen ; H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, (1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Fe1 Fe 0.18836(9) 0.20698(12) 0.48773(7) 0.0574 1.0000 Uani . U . . . . Fe2 Fe 0.53794(10) 0.21588(13) 0.30901(7) 0.0636 1.0000 Uani . U . . . . Fe3 Fe 0.30445(10) 0.27085(13) 0.08263(8) 0.0685 1.0000 Uani . U . . . . Fe4 Fe -0.04758(11) 0.21424(15) 0.25917(8) 0.0787 1.0000 Uani . U . . . . S1 S 0.4389(2) 0.2278(3) 0.50636(17) 0.1016 1.0000 Uani . U . . . . S2 S 0.4737(2) 0.1479(3) 0.48244(14) 0.0851 1.0000 Uani . U . . . . S3 S 0.58571(19) 0.3020(3) 0.13560(14) 0.0812 1.0000 Uani . U . . . . S4 S 0.5529(2) 0.2364(3) 0.09740(15) 0.0898 1.0000 Uani . U . . . . S5 S 0.05383(19) 0.2944(3) 0.06787(13) 0.0780 1.0000 Uani . U . . . . S6 S 0.02159(19) 0.2065(3) 0.08262(14) 0.0796 1.0000 Uani . U . . . . S7 S -0.0952(2) 0.2160(5) 0.43969(17) 0.1250 1.0000 Uani . U . . . . S8 S -0.0560(2) 0.1432(4) 0.46847(16) 0.1077 1.0000 Uani . U . . . . N1 N 0.1793(4) 0.1398(4) 0.5291(2) 0.0536 1.0000 Uani G U . . . . N2 N 0.1133(3) 0.1959(5) 0.4845(3) 0.0568 1.0000 Uani G U . . . . N3 N 0.1715(5) 0.2717(5) 0.4461(3) 0.0754 1.0000 Uani G U . . . . N4 N 0.1949(4) 0.2808(5) 0.5263(3) 0.0700 1.0000 Uani G U . . . . N5 N 0.2630(3) 0.2131(6) 0.4904(3) 0.0666 1.0000 Uani G U . . . . N6 N 0.2067(4) 0.1358(4) 0.4507(2) 0.0525 1.0000 Uani G U . . . . N7 N 0.4808(4) 0.2834(5) 0.3141(3) 0.0728 1.0000 Uani G U . . . . N8 N 0.5198(4) 0.1988(5) 0.3607(2) 0.0654 1.0000 Uani G U . . . . N9 N 0.5888(4) 0.1440(5) 0.3205(3) 0.0615 1.0000 Uani G U . . . . N10 N 0.4885(4) 0.1535(5) 0.2829(3) 0.0594 1.0000 Uani G U . . . . N11 N 0.5554(4) 0.2326(5) 0.2570(2) 0.0654 1.0000 Uani G U . . . . N12 N 0.5936(4) 0.2836(5) 0.3182(3) 0.0671 1.0000 Uani G U . . . . N13 N 0.3178(5) 0.2148(6) 0.0361(3) 0.0777 1.0000 Uani G U . . . . N14 N 0.3778(3) 0.2651(6) 0.0869(3) 0.0730 1.0000 Uani G U . . . . N15 N 0.3138(4) 0.3247(6) 0.1286(3) 0.0771 1.0000 Uani G U . . . . N16 N 0.2985(4) 0.3521(4) 0.0498(3) 0.0590 1.0000 Uani G U . . . . N17 N 0.2299(3) 0.2778(5) 0.0784(3) 0.0686 1.0000 Uani G U . . . . N18 N 0.2863(5) 0.1911(6) 0.1133(5) 0.0999 1.0000 Uani G U . . . . N19 N 0.0064(4) 0.2811(6) 0.2627(3) 0.0731 1.0000 Uani G U . . . . N20 N -0.0290(4) 0.2170(5) 0.2078(2) 0.0679 1.0000 Uani G U . . . . N21 N -0.1002(4) 0.1486(6) 0.2372(3) 0.0817 1.0000 Uani G U . . . . N22 N 0.0031(4) 0.1455(6) 0.2750(3) 0.0802 1.0000 Uani G U . . . . N23 N -0.0639(5) 0.2091(7) 0.3111(2) 0.0916 1.0000 Uani G U . . . . N24 N -0.1033(4) 0.2817(6) 0.2599(3) 0.0793 1.0000 Uani G U . . . . C1 C 0.2177(3) 0.1163(5) 0.5537(3) 0.0597 1.0000 Uani G U . . . . C2 C 0.2055(4) 0.0685(6) 0.5809(3) 0.0764 1.0000 Uani G U . . . . C3 C 0.1548(5) 0.0478(5) 0.5850(3) 0.0766 1.0000 Uani G U . . . . C4 C 0.1156(4) 0.0720(6) 0.5612(3) 0.0628 1.0000 Uani G U . . . . C5 C 0.1293(3) 0.1184(5) 0.5344(2) 0.0530 1.0000 Uani G U . . . . C6 C 0.0923(4) 0.1519(5) 0.5077(2) 0.0544 1.0000 Uani G U . . . . C7 C 0.0403(4) 0.1351(5) 0.5025(3) 0.0636 1.0000 Uani G U . . . . C8 C 0.0081(3) 0.1715(6) 0.4754(3) 0.0743 1.0000 Uani G U . . . . C9 C 0.0324(4) 0.2225(6) 0.4521(3) 0.0734 1.0000 Uani G U . . . . C10 C 0.0845(4) 0.2331(4) 0.4592(3) 0.0659 1.0000 Uani G U . . . . C11 C 0.1184(4) 0.2825(6) 0.4379(4) 0.0749 1.0000 Uani G U . . . . C12 C 0.0973(5) 0.3288(8) 0.4138(4) 0.1023 1.0000 Uani G U . . . . C13 C 0.1329(7) 0.3695(7) 0.3977(4) 0.1210 1.0000 Uani G U . . . . C14 C 0.1858(6) 0.3650(7) 0.4032(4) 0.1173 1.0000 Uani G U . . . . C15 C 0.2044(4) 0.3142(7) 0.4298(4) 0.0963 1.0000 Uani G U . . . . C16 C 0.1565(3) 0.3126(6) 0.5408(3) 0.0761 1.0000 Uani G U . . . . C17 C 0.1670(5) 0.3671(6) 0.5691(4) 0.0873 1.0000 Uani G U . . . . C18 C 0.2207(5) 0.3812(6) 0.5808(4) 0.1066 1.0000 Uani G U . . . . C19 C 0.2582(4) 0.3467(7) 0.5618(4) 0.0910 1.0000 Uani G U . . . . C20 C 0.2462(4) 0.2976(6) 0.5364(4) 0.0834 1.0000 Uani G U . . . . C21 C 0.2868(4) 0.2562(5) 0.5162(3) 0.0756 1.0000 Uani G U . . . . C22 C 0.3411(4) 0.2619(6) 0.5199(4) 0.0900 1.0000 Uani G U . . . . C23 C 0.3713(3) 0.2174(7) 0.4978(4) 0.0799 1.0000 Uani G U . . . . C24 C 0.3471(4) 0.1717(6) 0.4728(3) 0.0692 1.0000 Uani G U . . . . C25 C 0.2921(4) 0.1693(5) 0.4704(3) 0.0711 1.0000 Uani G U . . . . C26 C 0.2587(3) 0.1271(5) 0.4459(3) 0.0572 1.0000 Uani G U . . . . C27 C 0.2781(3) 0.0782(6) 0.4225(3) 0.0616 1.0000 Uani G U . . . . C28 C 0.2425(4) 0.0383(5) 0.4002(3) 0.0651 1.0000 Uani G U . . . . C29 C 0.1913(4) 0.0479(5) 0.4040(3) 0.0604 1.0000 Uani G U . . . . C30 C 0.1736(3) 0.0969(5) 0.4301(3) 0.0571 1.0000 Uani G U . . . . C31 C 0.4660(6) 0.3297(7) 0.2880(3) 0.0989 1.0000 Uani G U . . . . C32 C 0.4276(7) 0.3764(7) 0.2935(5) 0.1182 1.0000 Uani G U . . . . C33 C 0.4066(6) 0.3770(7) 0.3283(5) 0.1248 1.0000 Uani G U . . . . C34 C 0.4201(6) 0.3315(8) 0.3598(4) 0.1084 1.0000 Uani G U . . . . C35 C 0.4597(5) 0.2853(6) 0.3496(3) 0.0785 1.0000 Uani G U . . . . C36 C 0.4805(4) 0.2346(5) 0.3765(3) 0.0686 1.0000 Uani G U . . . . C37 C 0.4650(4) 0.2236(6) 0.4154(3) 0.0760 1.0000 Uani G U . . . . C38 C 0.4926(4) 0.1763(6) 0.4341(2) 0.0729 1.0000 Uani G U . . . . C39 C 0.5327(4) 0.1391(5) 0.4192(3) 0.0587 1.0000 Uani G U . . . . C40 C 0.5461(3) 0.1536(5) 0.3820(3) 0.0576 1.0000 Uani G U . . . . C41 C 0.5864(4) 0.1191(5) 0.3596(3) 0.0599 1.0000 Uani G U . . . . C42 C 0.6195(5) 0.0701(6) 0.3737(3) 0.0737 1.0000 Uani G U . . . . C43 C 0.6591(5) 0.0444(6) 0.3489(4) 0.0878 1.0000 Uani G U . . . . C44 C 0.6568(4) 0.0686(6) 0.3086(3) 0.0822 1.0000 Uani G U . . . . C45 C 0.6240(4) 0.1167(6) 0.2955(2) 0.0720 1.0000 Uani G U . . . . C46 C 0.4571(5) 0.1089(6) 0.2982(2) 0.0715 1.0000 Uani G U . . . . C47 C 0.4258(5) 0.0671(6) 0.2772(4) 0.0846 1.0000 Uani G U . . . . C48 C 0.4273(5) 0.0678(6) 0.2370(4) 0.0899 1.0000 Uani G U . . . . C49 C 0.4589(5) 0.1117(6) 0.2199(2) 0.0782 1.0000 Uani G U . . . . C50 C 0.4907(4) 0.1531(5) 0.2424(3) 0.0660 1.0000 Uani G U . . . . C51 C 0.5281(4) 0.2021(5) 0.2285(3) 0.0595 1.0000 Uani G U . . . . C52 C 0.5386(4) 0.2196(6) 0.1901(2) 0.0647 1.0000 Uani G U . . . . C53 C 0.5747(5) 0.2662(6) 0.1820(2) 0.0690 1.0000 Uani G U . . . . C54 C 0.6029(4) 0.2980(6) 0.2115(3) 0.0744 1.0000 Uani G U . . . . C55 C 0.5912(4) 0.2804(5) 0.2502(3) 0.0676 1.0000 Uani G U . . . . C56 C 0.6149(5) 0.3093(6) 0.2851(2) 0.0695 1.0000 Uani G U . . . . C57 C 0.6533(5) 0.3577(7) 0.2868(3) 0.0896 1.0000 Uani G U . . . . C58 C 0.6731(5) 0.3761(7) 0.3212(4) 0.1033 1.0000 Uani G U . . . . C59 C 0.6532(6) 0.3512(8) 0.3543(3) 0.1061 1.0000 Uani G U . . . . C60 C 0.6126(5) 0.3048(7) 0.3527(2) 0.0854 1.0000 Uani G U . . . . C61 C 0.2802(4) 0.1902(7) 0.0083(5) 0.1018 1.0000 Uani G U . . . . C62 C 0.2964(6) 0.1545(8) -0.0199(4) 0.1223 1.0000 Uani G U . . . . C63 C 0.3483(6) 0.1373(8) -0.0236(4) 0.1194 1.0000 Uani G U . . . . C64 C 0.3859(4) 0.1570(7) 0.0033(5) 0.1096 1.0000 Uani G U . . . . C65 C 0.3706(4) 0.1994(7) 0.0312(4) 0.0812 1.0000 Uani G U . . . . C66 C 0.4049(4) 0.2296(6) 0.0600(3) 0.0780 1.0000 Uani G U . . . . C67 C 0.4574(4) 0.2237(6) 0.0625(3) 0.0796 1.0000 Uani G U . . . . C68 C 0.4843(3) 0.2529(6) 0.0936(3) 0.0741 1.0000 Uani G U . . . . C69 C 0.4570(4) 0.2959(6) 0.1214(3) 0.0677 1.0000 Uani G U . . . . C70 C 0.4038(4) 0.2973(6) 0.1167(3) 0.0750 1.0000 Uani G U . . . . C71 C 0.3672(4) 0.3325(7) 0.1415(3) 0.0784 1.0000 Uani G U . . . . C72 C 0.3801(4) 0.3693(8) 0.1735(3) 0.0956 1.0000 Uani G U . . . . C73 C 0.3393(5) 0.4022(8) 0.1953(3) 0.1097 1.0000 Uani G U . . . . C74 C 0.2900(5) 0.3916(7) 0.1837(3) 0.0925 1.0000 Uani G U . . . . C75 C 0.2763(3) 0.3570(7) 0.1503(3) 0.0850 1.0000 Uani G U . . . . C76 C 0.3386(3) 0.3891(6) 0.0372(3) 0.0607 1.0000 Uani G U . . . . C77 C 0.3269(5) 0.4456(5) 0.0132(3) 0.0809 1.0000 Uani G U . . . . C78 C 0.2767(5) 0.4607(5) 0.0038(3) 0.0805 1.0000 Uani G U . . . . C79 C 0.2356(4) 0.4231(6) 0.0182(3) 0.0764 1.0000 Uani G U . . . . C80 C 0.2481(4) 0.3686(5) 0.0407(3) 0.0576 1.0000 Uani G U . . . . C81 C 0.2080(4) 0.3251(5) 0.0567(3) 0.0559 1.0000 Uani G U . . . . C82 C 0.1539(4) 0.3322(5) 0.0553(3) 0.0568 1.0000 Uani G U . . . . C83 C 0.1239(3) 0.2819(6) 0.0740(3) 0.0674 1.0000 Uani G U . . . . C84 C 0.1471(4) 0.2307(6) 0.0953(4) 0.0758 1.0000 Uani G U . . . . C85 C 0.2008(4) 0.2319(5) 0.0966(3) 0.0785 1.0000 Uani G U . . . . C86 C 0.2322(4) 0.1802(8) 0.1157(6) 0.1110 1.0000 Uani G U . . . . C87 C 0.2139(5) 0.1244(10) 0.1347(8) 0.1672 1.0000 Uani G U . . . . C88 C 0.2494(7) 0.0814(10) 0.1531(8) 0.1991 1.0000 Uani G U . . . . C89 C 0.3030(6) 0.0937(11) 0.1515(8) 0.2018 1.0000 Uani G U . . . . C90 C 0.3212(4) 0.1457(9) 0.1291(7) 0.1616 1.0000 Uani G U . . . . C91 C 0.0243(5) 0.3164(7) 0.2945(2) 0.0968 1.0000 Uani G U . . . . C92 C 0.0618(6) 0.3642(7) 0.2948(3) 0.0969 1.0000 Uani G U . . . . C93 C 0.0891(5) 0.3785(6) 0.2601(4) 0.0886 1.0000 Uani G U . . . . C94 C 0.0729(5) 0.3441(7) 0.2260(3) 0.0807 1.0000 Uani G U . . . . C95 C 0.0312(5) 0.2976(6) 0.2296(2) 0.0693 1.0000 Uani G U . . . . C96 C 0.0110(4) 0.2586(5) 0.1964(2) 0.0616 1.0000 Uani G U . . . . C97 C 0.0288(4) 0.2582(5) 0.1589(3) 0.0604 1.0000 Uani G U . . . . C98 C 0.0018(4) 0.2170(6) 0.1322(2) 0.0665 1.0000 Uani G U . . . . C99 C -0.0407(4) 0.1775(6) 0.1434(3) 0.0689 1.0000 Uani G U . . . . C100 C -0.0560(4) 0.1783(5) 0.1800(3) 0.0707 1.0000 Uani G U . . . . C101 C -0.0973(4) 0.1409(6) 0.1968(3) 0.0811 1.0000 Uani G U . . . . C102 C -0.1332(6) 0.1026(7) 0.1785(3) 0.0946 1.0000 Uani G U . . . . C103 C -0.1747(5) 0.0700(7) 0.1978(5) 0.1081 1.0000 Uani G U . . . . C104 C -0.1739(5) 0.0779(7) 0.2357(5) 0.1199 1.0000 Uani G U . . . . C105 C -0.1387(6) 0.1166(8) 0.2569(3) 0.1039 1.0000 Uani G U . . . . C106 C 0.0366(5) 0.1118(7) 0.2530(2) 0.0808 1.0000 Uani G U . . . . C107 C 0.0727(5) 0.0645(7) 0.2671(4) 0.0926 1.0000 Uani G U . . . . C108 C 0.0728(5) 0.0514(7) 0.3061(4) 0.1011 1.0000 Uani G U . . . . C109 C 0.0398(6) 0.0834(7) 0.3290(3) 0.0884 1.0000 Uani G U . . . . C110 C 0.0044(5) 0.1290(6) 0.3127(3) 0.0777 1.0000 Uani G U . . . . C111 C -0.0366(5) 0.1687(6) 0.3361(3) 0.0852 1.0000 Uani G U . . . . C112 C -0.0430(5) 0.1680(8) 0.3769(3) 0.0929 1.0000 Uani G U . . . . C113 C -0.0816(5) 0.2082(8) 0.3908(2) 0.1066 1.0000 Uani G U . . . . C114 C -0.1095(5) 0.2519(7) 0.3664(3) 0.0965 1.0000 Uani G U . . . . C115 C -0.0991(5) 0.2523(7) 0.3273(3) 0.0862 1.0000 Uani G U . . . . C116 C -0.1217(5) 0.2963(6) 0.2959(3) 0.0833 1.0000 Uani G U . . . . C117 C -0.1589(5) 0.3433(7) 0.3031(3) 0.0863 1.0000 Uani G U . . . . C118 C -0.1791(5) 0.3828(6) 0.2701(4) 0.0875 1.0000 Uani G U . . . . C119 C -0.1601(5) 0.3661(7) 0.2319(3) 0.0823 1.0000 Uani G U . . . . C120 C -0.1221(5) 0.3196(6) 0.2286(2) 0.0856 1.0000 Uani G U . . . . B1 B 0.3578(3) -0.0836(4) 0.3501(2) 0.127(2) 1.0000 Uiso G U . . . . B2 B 0.3729(3) 0.0075(4) 0.5277(2) 0.136(2) 1.0000 Uiso G U . . . . B3 B 0.2225(3) 0.0481(4) 0.6887(2) 0.149(2) 1.0000 Uiso G U . . . . B4 B 0.0405(3) -0.0110(4) 0.4206(2) 0.148(2) 1.0000 Uiso G U . . . . B5 B 0.2155(3) 0.5585(4) 0.6132(2) 0.148(2) 1.0000 Uiso G U . . . . F1 F 0.4115(3) -0.0773(6) 0.3529(3) 0.1269(19) 1.0000 Uiso G U . . . . F2 F 0.3345(4) -0.0611(5) 0.3837(3) 0.1210(19) 1.0000 Uiso G U . . . . F3 F 0.3469(4) -0.1510(4) 0.3445(3) 0.1161(19) 1.0000 Uiso G U . . . . F4 F 0.3399(5) -0.0468(5) 0.3191(3) 0.1471(19) 1.0000 Uiso G U . . . . F5 F 0.3606(5) 0.0267(6) 0.4907(2) 0.128(2) 1.0000 Uiso G U . . . . F6 F 0.3319(4) 0.0201(6) 0.5515(3) 0.126(2) 1.0000 Uiso G U . . . . F7 F 0.4190(4) 0.0357(6) 0.5418(4) 0.154(2) 1.0000 Uiso G U . . . . F8 F 0.3790(5) -0.0607(4) 0.5263(3) 0.137(2) 1.0000 Uiso G U . . . . F9 F 0.2392(5) 0.0377(7) 0.7262(2) 0.148(2) 1.0000 Uiso G U . . . . F10 F 0.2616(4) 0.0687(5) 0.6651(3) 0.105(2) 1.0000 Uiso G U . . . . F11 F 0.1839(4) 0.0953(6) 0.6855(4) 0.191(2) 1.0000 Uiso G U . . . . F12 F 0.2049(5) -0.0113(5) 0.6732(4) 0.152(2) 1.0000 Uiso G U . . . . F13 F 0.0759(4) -0.0378(5) 0.3953(3) 0.117(2) 1.0000 Uiso G U . . . . F14 F 0.0490(5) 0.0571(4) 0.4223(3) 0.124(2) 1.0000 Uiso G U . . . . F15 F -0.0095(3) -0.0215(6) 0.4065(4) 0.160(2) 1.0000 Uiso G U . . . . F16 F 0.0468(6) -0.0381(7) 0.4562(3) 0.192(2) 1.0000 Uiso G U . . . . F17 F 0.2078(5) 0.6263(4) 0.6147(3) 0.126(2) 1.0000 Uiso G U . . . . F18 F 0.2222(5) 0.5344(6) 0.6498(3) 0.142(2) 1.0000 Uiso G U . . . . F19 F 0.1726(4) 0.5290(6) 0.5955(3) 0.137(2) 1.0000 Uiso G U . . . . F20 F 0.2595(4) 0.5458(7) 0.5920(4) 0.186(2) 1.0000 Uiso G U . . . . N50 N 0.4122(8) 0.0802(9) 0.3910(5) 0.113(3) 1.0000 Uiso G U . . . . C501 C 0.4310(9) 0.0357(8) 0.4083(4) 0.102(3) 1.0000 Uiso G U . . . . C502 C 0.4546(9) -0.0167(9) 0.4344(6) 0.096(3) 1.0000 Uiso G U . . . . N51 N 0.0315(9) 0.3747(12) 0.5049(6) 0.125(4) 1.0000 Uiso G U . . . . C511 C 0.0509(10) 0.4169(13) 0.5026(9) 0.153(4) 1.0000 Uiso G U . . . . C512 C 0.0703(16) 0.4813(15) 0.5036(13) 0.222(4) 1.0000 Uiso G U . . . . B6 B -0.0522(6) 0.4456(7) 0.6077(4) 0.243(3) 1.0000 Uiso G U . . . . F21 F -0.0444(9) 0.3862(8) 0.6263(6) 0.242(3) 1.0000 Uiso G U . . . . F22 F -0.0946(7) 0.4407(11) 0.5831(6) 0.243(3) 1.0000 Uiso G U . . . . F23 F -0.0610(9) 0.4942(9) 0.6348(6) 0.242(3) 1.0000 Uiso G U . . . . F24 F -0.0082(7) 0.4615(11) 0.5871(6) 0.244(3) 1.0000 Uiso G U . . . . B7 B 0.3397(6) 0.3779(8) 0.4404(4) 0.255(3) 1.0000 Uiso G U . . . . F25 F 0.3268(9) 0.4152(11) 0.4084(5) 0.255(3) 1.0000 Uiso G U . . . . F26 F 0.3038(8) 0.3908(11) 0.4691(6) 0.254(3) 1.0000 Uiso G U . . . . F27 F 0.3375(9) 0.3119(8) 0.4311(7) 0.255(3) 1.0000 Uiso G U . . . . F28 F 0.3888(7) 0.3938(12) 0.4538(7) 0.256(3) 1.0000 Uiso G U . . . . B8 B 0.4049(11) 0.4376(15) 0.5573(8) 0.405(3) 1.0000 Uiso G U . . . . F29 F 0.3847(16) 0.3833(18) 0.5754(12) 0.405(3) 1.0000 Uiso G U . . . . F30 F 0.4556(12) 0.449(2) 0.5707(12) 0.405(3) 1.0000 Uiso G U . . . . F31 F 0.3747(16) 0.4922(18) 0.5641(12) 0.405(3) 1.0000 Uiso G U . . . . F32 F 0.4059(17) 0.426(2) 0.5177(8) 0.406(3) 1.0000 Uiso G U . . . . N52 N 0.4186(12) 0.5840(16) 0.3424(9) 0.194(4) 1.0000 Uiso G U . . . . C521 C 0.4174(14) 0.5540(16) 0.3710(9) 0.194(4) 1.0000 Uiso G U . . . . C522 C 0.4232(16) 0.5248(19) 0.4108(10) 0.194(4) 1.0000 Uiso G U . . . . N53 N -0.0015(9) 0.1039(12) 0.7012(6) 0.145(4) 1.0000 Uiso G U . . . . C531 C 0.0314(9) 0.0673(14) 0.6936(6) 0.145(4) 1.0000 Uiso G U . . . . C532 C 0.0670(11) 0.0169(14) 0.6756(9) 0.146(4) 1.0000 Uiso G U . . . . N54 N 0.0511(12) 0.0122(14) 0.7723(9) 0.183(4) 1.0000 Uiso G U . . . . C541 C 0.0466(15) 0.0220(12) 0.8052(9) 0.183(4) 1.0000 Uiso G U . . . . C542 C 0.0384(15) 0.0280(18) 0.8480(9) 0.182(4) 1.0000 Uiso G U . . . . N55 N 0.330(2) 0.603(3) 0.4630(13) 0.158(4) 0.5000 Uiso G U . . . . C551 C 0.294(2) 0.574(3) 0.4509(11) 0.158(4) 0.5000 Uiso G U . . . . C552 C 0.248(2) 0.537(3) 0.4332(18) 0.159(4) 0.5000 Uiso G U . . . . O60 O 0.4468(7) 0.0782(9) 0.6746(6) 0.199(3) 1.0000 Uiso G U . . . . C601 C 0.4017(14) 0.1475(17) 0.6278(8) 0.198(3) 1.0000 Uiso G U . . . . C602 C 0.4440(11) 0.0969(14) 0.6341(6) 0.198(3) 1.0000 Uiso G U . . . . C603 C 0.4771(10) 0.0339(13) 0.6994(8) 0.199(3) 1.0000 Uiso G U . . . . C604 C 0.4556(14) 0.0350(17) 0.7395(7) 0.199(3) 1.0000 Uiso G U . . . . O61 O 0.5936(14) 0.307(2) 0.4502(12) 0.166(4) 0.5000 Uiso G U . . . . O611 O 0.6765(14) 0.227(2) 0.4444(12) 0.166(4) 0.5000 Uiso G U . . . . C611 C 0.6297(14) 0.2608(18) 0.4651(7) 0.166(4) 1.0000 Uiso G U . . . . O62 O 0.1514(12) 0.2254(15) 0.3016(9) 0.159(3) 0.5000 Uiso G U . . . . C621 C 0.1107(19) 0.207(3) 0.3632(11) 0.158(3) 0.5000 Uiso G U . . . . C622 C 0.1606(16) 0.202(2) 0.3410(9) 0.158(3) 0.5000 Uiso G U . . . . C623 C 0.1943(15) 0.207(2) 0.2767(11) 0.158(3) 0.5000 Uiso G U . . . . C624 C 0.183(2) 0.231(3) 0.2361(10) 0.159(3) 0.5000 Uiso G U . . . . O501 O 0.1927(16) 0.443(2) 0.3059(12) 0.151(2) 0.5000 Uiso . U . . . . O511 O 0.2592(16) 0.437(2) 0.3295(12) 0.151(2) 0.5000 Uiso . U . . . . O502 O -0.0335(16) 0.372(2) 0.3893(12) 0.151(2) 0.5000 Uiso . . . . . . O503 O 0.3263(16) 0.189(2) 0.3458(12) 0.151(2) 0.5000 Uiso . . . . . . O513 O 0.3518(16) 0.223(2) 0.2876(12) 0.151(2) 0.5000 Uiso . . . . . . O504 O 0.2434(16) 0.278(2) 0.7656(12) 0.151(2) 0.5000 Uiso . U . . . . O514 O 0.2443(16) 0.277(2) 0.8099(12) 0.151(2) 0.5000 Uiso . U . . . . O505 O 0.5203(16) 0.387(2) 0.4515(14) 0.151(2) 0.5000 Uiso . U . . . . O515 O 0.5262(16) 0.369(2) 0.4217(13) 0.151(2) 0.5000 Uiso . U . . . . H11 H 0.2531 0.1329 0.5521 0.0715 1.0000 Uiso . . . . . . H21 H 0.2329 0.0497 0.5970 0.0916 1.0000 Uiso . . . . . . H31 H 0.1465 0.0161 0.6047 0.0919 1.0000 Uiso . . . . . . H41 H 0.0800 0.0570 0.5632 0.0754 1.0000 Uiso . . . . . . H71 H 0.0255 0.0992 0.5171 0.0766 1.0000 Uiso . . . . . . H91 H 0.0129 0.2472 0.4329 0.0883 1.0000 Uiso . . . . . . H121 H 0.0602 0.3325 0.4087 0.1229 1.0000 Uiso . . . . . . H131 H 0.1199 0.4042 0.3811 0.1452 1.0000 Uiso . . . . . . H141 H 0.2096 0.3941 0.3902 0.1411 1.0000 Uiso . . . . . . H151 H 0.2414 0.3110 0.4357 0.1162 1.0000 Uiso . . . . . . H161 H 0.1210 0.3014 0.5336 0.0920 1.0000 Uiso . . . . . . H171 H 0.1385 0.3926 0.5793 0.1051 1.0000 Uiso . . . . . . H181 H 0.2294 0.4129 0.6007 0.1284 1.0000 Uiso . . . . . . H191 H 0.2946 0.3575 0.5666 0.1097 1.0000 Uiso . . . . . . H221 H 0.3573 0.2944 0.5366 0.1085 1.0000 Uiso . . . . . . H241 H 0.3679 0.1423 0.4574 0.0833 1.0000 Uiso . . . . . . H271 H 0.3154 0.0708 0.4212 0.0742 1.0000 Uiso . . . . . . H281 H 0.2553 0.0052 0.3827 0.0783 1.0000 Uiso . . . . . . H291 H 0.1664 0.0219 0.3892 0.0725 1.0000 Uiso . . . . . . H301 H 0.1364 0.1025 0.4333 0.0687 1.0000 Uiso . . . . . . H311 H 0.4836 0.3300 0.2636 0.1182 1.0000 Uiso . . . . . . H321 H 0.4167 0.4068 0.2734 0.1411 1.0000 Uiso . . . . . . H331 H 0.3803 0.4100 0.3332 0.1493 1.0000 Uiso . . . . . . H341 H 0.4039 0.3327 0.3847 0.1302 1.0000 Uiso . . . . . . H371 H 0.4371 0.2480 0.4272 0.0914 1.0000 Uiso . . . . . . H391 H 0.5503 0.1050 0.4340 0.0705 1.0000 Uiso . . . . . . H421 H 0.6161 0.0536 0.3997 0.0888 1.0000 Uiso . . . . . . H431 H 0.6853 0.0134 0.3578 0.1056 1.0000 Uiso . . . . . . H441 H 0.6803 0.0488 0.2905 0.0988 1.0000 Uiso . . . . . . H451 H 0.6253 0.1314 0.2690 0.0866 1.0000 Uiso . . . . . . H461 H 0.4562 0.1058 0.3260 0.0861 1.0000 Uiso . . . . . . H471 H 0.4027 0.0370 0.2901 0.1016 1.0000 Uiso . . . . . . H481 H 0.4062 0.0375 0.2219 0.1077 1.0000 Uiso . . . . . . H491 H 0.4596 0.1146 0.1921 0.0936 1.0000 Uiso . . . . . . H521 H 0.5198 0.1980 0.1692 0.0776 1.0000 Uiso . . . . . . H541 H 0.6293 0.3306 0.2059 0.0894 1.0000 Uiso . . . . . . H571 H 0.6655 0.3779 0.2634 0.1072 1.0000 Uiso . . . . . . H581 H 0.7018 0.4072 0.3226 0.1237 1.0000 Uiso . . . . . . H591 H 0.6671 0.3657 0.3790 0.1269 1.0000 Uiso . . . . . . H601 H 0.5981 0.2879 0.3762 0.1021 1.0000 Uiso . . . . . . H611 H 0.2434 0.2001 0.0107 0.1221 1.0000 Uiso . . . . . . H621 H 0.2714 0.1393 -0.0392 0.1467 1.0000 Uiso . . . . . . H631 H 0.3586 0.1110 -0.0454 0.1432 1.0000 Uiso . . . . . . H641 H 0.4216 0.1413 0.0022 0.1316 1.0000 Uiso . . . . . . H671 H 0.4761 0.1997 0.0430 0.0956 1.0000 Uiso . . . . . . H691 H 0.4753 0.3209 0.1411 0.0814 1.0000 Uiso . . . . . . H721 H 0.4163 0.3733 0.1817 0.1149 1.0000 Uiso . . . . . . H731 H 0.3476 0.4304 0.2170 0.1320 1.0000 Uiso . . . . . . H741 H 0.2623 0.4088 0.1994 0.1114 1.0000 Uiso . . . . . . H751 H 0.2400 0.3554 0.1420 0.1022 1.0000 Uiso . . . . . . H761 H 0.3743 0.3780 0.0441 0.0730 1.0000 Uiso . . . . . . H771 H 0.3550 0.4727 0.0037 0.0971 1.0000 Uiso . . . . . . H781 H 0.2692 0.4977 -0.0130 0.0965 1.0000 Uiso . . . . . . H791 H 0.1996 0.4348 0.0127 0.0918 1.0000 Uiso . . . . . . H821 H 0.1373 0.3693 0.0425 0.0682 1.0000 Uiso . . . . . . H841 H 0.1269 0.1972 0.1081 0.0910 1.0000 Uiso . . . . . . H871 H 0.1768 0.1153 0.1352 0.2006 1.0000 Uiso . . . . . . H881 H 0.2368 0.0433 0.1669 0.2388 1.0000 Uiso . . . . . . H891 H 0.3274 0.0662 0.1659 0.2421 1.0000 Uiso . . . . . . H901 H 0.3582 0.1501 0.1246 0.1942 1.0000 Uiso . . . . . . H911 H 0.0085 0.3062 0.3189 0.1160 1.0000 Uiso . . . . . . H921 H 0.0700 0.3882 0.3181 0.1160 1.0000 Uiso . . . . . . H931 H 0.1174 0.4102 0.2598 0.1061 1.0000 Uiso . . . . . . H941 H 0.0893 0.3520 0.2016 0.0966 1.0000 Uiso . . . . . . H971 H 0.0583 0.2847 0.1514 0.0723 1.0000 Uiso . . . . . . H991 H -0.0587 0.1500 0.1246 0.0827 1.0000 Uiso . . . . . . H1021 H -0.1307 0.0970 0.1509 0.1136 1.0000 Uiso . . . . . . H1031 H -0.2012 0.0443 0.1844 0.1297 1.0000 Uiso . . . . . . H1041 H -0.2002 0.0547 0.2499 0.1438 1.0000 Uiso . . . . . . H1051 H -0.1413 0.1207 0.2845 0.1248 1.0000 Uiso . . . . . . H1061 H 0.0360 0.1207 0.2257 0.0971 1.0000 Uiso . . . . . . H1071 H 0.0963 0.0421 0.2501 0.1112 1.0000 Uiso . . . . . . H1081 H 0.0968 0.0192 0.3168 0.1216 1.0000 Uiso . . . . . . H1091 H 0.0404 0.0753 0.3565 0.1060 1.0000 Uiso . . . . . . H1121 H -0.0214 0.1408 0.3937 0.1118 1.0000 Uiso . . . . . . H1141 H -0.1355 0.2812 0.3768 0.1161 1.0000 Uiso . . . . . . H1171 H -0.1715 0.3504 0.3289 0.1036 1.0000 Uiso . . . . . . H1181 H -0.2038 0.4182 0.2737 0.1050 1.0000 Uiso . . . . . . H1191 H -0.1745 0.3878 0.2092 0.0989 1.0000 Uiso . . . . . . H1201 H -0.1073 0.3122 0.2036 0.1029 1.0000 Uiso . . . . . . H5021 H 0.4628 -0.0554 0.4194 0.1150 1.0000 Uiso . . . . . . H5022 H 0.4862 0.0002 0.4465 0.1150 1.0000 Uiso . . . . . . H5023 H 0.4299 -0.0284 0.4540 0.1150 1.0000 Uiso . . . . . . H5121 H 0.1024 0.4833 0.4894 0.2668 1.0000 Uiso . . . . . . H5122 H 0.0772 0.4941 0.5300 0.2668 1.0000 Uiso . . . . . . H5123 H 0.0449 0.5109 0.4921 0.2668 1.0000 Uiso . . . . . . H5221 H 0.4011 0.4862 0.4128 0.2331 1.0000 Uiso . . . . . . H5222 H 0.4128 0.5571 0.4297 0.2331 1.0000 Uiso . . . . . . H5223 H 0.4592 0.5124 0.4155 0.2331 1.0000 Uiso . . . . . . H5321 H 0.0973 0.0101 0.6922 0.1751 1.0000 Uiso . . . . . . H5322 H 0.0484 -0.0244 0.6724 0.1751 1.0000 Uiso . . . . . . H5323 H 0.0780 0.0326 0.6508 0.1751 1.0000 Uiso . . . . . . H5421 H 0.0515 0.0702 0.8569 0.2190 1.0000 Uiso . . . . . . H5422 H 0.0568 -0.0072 0.8612 0.2190 1.0000 Uiso . . . . . . H5423 H 0.0014 0.0250 0.8531 0.2190 1.0000 Uiso . . . . . . H552 H 0.2276 0.5174 0.4533 0.1903 0.5000 Uiso . . . . . . H553 H 0.2262 0.5676 0.4185 0.1903 0.5000 Uiso . . . . . . H554 H 0.2606 0.5031 0.4163 0.1903 0.5000 Uiso . . . . . . H6011 H 0.4000 0.1597 0.6009 0.2375 1.0000 Uiso . . . . . . H6012 H 0.4094 0.1862 0.6432 0.2375 1.0000 Uiso . . . . . . H6013 H 0.3685 0.1292 0.6352 0.2375 1.0000 Uiso . . . . . . H6021 H 0.4772 0.1153 0.6266 0.2376 1.0000 Uiso . . . . . . H6022 H 0.4363 0.0583 0.6186 0.2376 1.0000 Uiso . . . . . . H6031 H 0.5132 0.0482 0.7002 0.2388 1.0000 Uiso . . . . . . H6032 H 0.4751 -0.0104 0.6892 0.2388 1.0000 Uiso . . . . . . H6041 H 0.4759 0.0055 0.7558 0.2385 1.0000 Uiso . . . . . . H6042 H 0.4577 0.0793 0.7497 0.2385 1.0000 Uiso . . . . . . H6043 H 0.4196 0.0207 0.7387 0.2385 1.0000 Uiso . . . . . . H6111 H 0.6456 0.2825 0.4872 0.1994 1.0000 Uiso . . . . . . H6112 H 0.6084 0.2244 0.4737 0.1994 1.0000 Uiso . . . . . . H6211 H 0.1169 0.1917 0.3893 0.1902 0.5000 Uiso . . . . . . H6212 H 0.0991 0.2524 0.3637 0.1902 0.5000 Uiso . . . . . . H6213 H 0.0841 0.1799 0.3509 0.1902 0.5000 Uiso . . . . . . H6221 H 0.1872 0.2294 0.3534 0.1900 0.5000 Uiso . . . . . . H6222 H 0.1722 0.1569 0.3406 0.1900 0.5000 Uiso . . . . . . H6231 H 0.2263 0.2270 0.2862 0.1901 0.5000 Uiso . . . . . . H6232 H 0.1981 0.1595 0.2766 0.1901 0.5000 Uiso . . . . . . H6241 H 0.2112 0.2186 0.2197 0.1905 0.5000 Uiso . . . . . . H6242 H 0.1789 0.2783 0.2362 0.1905 0.5000 Uiso . . . . . . H6243 H 0.1507 0.2108 0.2266 0.1905 0.5000 Uiso . . . . . . H6113 H 0.6568 0.2442 0.4487 0.1994 0.5000 Uiso . . . . . . H6114 H 0.6082 0.2920 0.4510 0.1994 0.5000 Uiso . . . . . . 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 Fe1 0.0638(13) 0.0517(14) 0.0577(13) -0.0016(11) 0.0237(11) -0.0058(12) Fe2 0.0633(16) 0.0609(16) 0.0667(14) 0.0119(12) 0.0057(12) -0.0051(11) Fe3 0.0622(14) 0.0673(17) 0.0760(16) 0.0200(12) 0.0054(12) -0.0005(12) Fe4 0.0731(17) 0.095(2) 0.0686(15) 0.0283(14) 0.0085(13) 0.0083(13) S1 0.073(2) 0.133(4) 0.100(4) -0.052(3) 0.031(3) -0.042(3) S2 0.070(3) 0.120(4) 0.067(3) -0.009(3) 0.020(2) -0.018(3) S3 0.063(3) 0.112(4) 0.069(2) 0.023(2) 0.008(2) -0.012(3) S4 0.062(2) 0.134(4) 0.074(3) -0.005(3) 0.015(2) 0.006(3) S5 0.066(2) 0.108(3) 0.060(3) 0.003(3) -0.006(2) -0.001(2) S6 0.066(3) 0.108(3) 0.066(2) -0.015(3) -0.001(2) -0.011(3) S7 0.079(3) 0.224(6) 0.072(3) 0.033(4) 0.018(3) 0.039(4) S8 0.061(3) 0.192(5) 0.071(3) 0.038(3) 0.011(2) -0.002(3) N1 0.063(3) 0.052(5) 0.046(4) -0.005(3) 0.011(4) -0.005(4) N2 0.061(2) 0.057(6) 0.053(5) 0.003(3) 0.022(3) 0.006(3) N3 0.093(3) 0.058(5) 0.076(5) 0.015(4) 0.030(5) -0.005(4) N4 0.081(3) 0.055(5) 0.075(5) -0.013(4) 0.041(5) -0.016(4) N5 0.065(2) 0.078(6) 0.058(6) -0.015(4) 0.025(3) -0.014(3) N6 0.056(3) 0.055(5) 0.047(5) -0.001(3) 0.019(4) -0.006(4) N7 0.074(4) 0.049(5) 0.096(5) 0.006(4) 0.005(5) -0.004(3) N8 0.053(5) 0.076(6) 0.068(3) 0.008(3) 0.011(3) 0.002(3) N9 0.061(5) 0.062(5) 0.063(4) 0.005(4) 0.012(4) -0.002(3) N10 0.058(5) 0.047(5) 0.073(4) 0.011(4) 0.012(4) -0.001(3) N11 0.069(5) 0.060(6) 0.068(2) 0.014(3) 0.005(3) -0.012(3) N12 0.073(4) 0.062(5) 0.067(3) 0.021(5) -0.008(5) -0.010(4) N13 0.071(4) 0.058(5) 0.104(5) 0.002(4) 0.000(4) 0.005(5) N14 0.062(2) 0.091(7) 0.065(6) 0.015(4) 0.010(3) 0.002(3) N15 0.062(3) 0.114(6) 0.055(4) 0.018(4) 0.007(4) 0.009(5) N16 0.074(3) 0.054(4) 0.049(5) 0.002(3) 0.003(5) -0.009(4) N17 0.063(2) 0.072(6) 0.071(6) 0.024(4) 0.004(3) 0.001(3) N18 0.072(3) 0.092(5) 0.137(7) 0.061(4) 0.019(6) 0.012(4) N19 0.079(4) 0.093(5) 0.047(4) 0.027(4) -0.012(4) 0.008(4) N20 0.066(5) 0.072(6) 0.065(3) 0.018(3) 0.001(3) 0.004(3) N21 0.073(5) 0.074(5) 0.098(4) 0.038(5) 0.009(4) 0.009(4) N22 0.077(5) 0.092(6) 0.073(4) 0.031(5) 0.013(4) 0.010(4) N23 0.080(6) 0.121(7) 0.074(3) 0.036(3) 0.019(3) 0.022(4) N24 0.076(5) 0.090(6) 0.072(4) 0.019(5) 0.007(5) 0.008(4) C1 0.076(5) 0.054(7) 0.049(6) -0.020(4) -0.007(5) -0.009(6) C2 0.088(5) 0.082(8) 0.059(7) 0.006(5) -0.007(6) 0.007(6) C3 0.099(5) 0.079(8) 0.052(7) 0.011(6) 0.001(6) -0.007(6) C4 0.080(5) 0.073(7) 0.035(6) 0.001(4) 0.007(5) -0.020(6) C5 0.069(4) 0.063(7) 0.027(5) -0.007(4) 0.008(4) -0.016(5) C6 0.058(3) 0.061(7) 0.045(6) -0.002(4) 0.021(4) 0.000(5) C7 0.057(4) 0.080(7) 0.055(7) 0.003(5) 0.020(5) 0.000(5) C8 0.066(4) 0.105(8) 0.052(7) 0.004(5) 0.016(5) 0.008(4) C9 0.075(4) 0.082(8) 0.064(7) 0.007(5) 0.011(5) 0.019(5) C10 0.073(3) 0.064(7) 0.061(7) 0.005(5) 0.021(5) 0.016(5) C11 0.101(4) 0.059(7) 0.066(7) 0.006(5) 0.014(6) 0.001(5) C12 0.120(5) 0.090(8) 0.097(8) 0.037(6) 0.007(7) -0.001(6) C13 0.162(5) 0.114(8) 0.088(8) 0.041(6) -0.005(8) -0.039(7) C14 0.153(5) 0.108(8) 0.092(8) 0.043(6) 0.028(8) -0.042(7) C15 0.123(5) 0.087(8) 0.080(8) 0.020(5) 0.041(7) -0.024(6) C16 0.093(4) 0.059(7) 0.079(7) -0.004(5) 0.046(6) -0.004(5) C17 0.103(4) 0.071(7) 0.089(8) -0.019(5) 0.026(7) 0.025(7) C18 0.108(5) 0.079(8) 0.134(9) -0.045(6) 0.036(7) -0.003(7) C19 0.088(5) 0.069(8) 0.117(8) -0.038(5) 0.041(6) -0.026(6) C20 0.086(3) 0.076(7) 0.089(7) -0.029(5) 0.036(6) -0.023(5) C21 0.076(3) 0.071(7) 0.081(7) -0.022(5) 0.022(6) -0.017(5) C22 0.078(3) 0.090(8) 0.103(8) -0.041(6) 0.032(6) -0.036(6) C23 0.070(3) 0.092(8) 0.078(7) -0.026(6) 0.030(5) -0.032(5) C24 0.060(3) 0.079(8) 0.070(7) -0.019(5) 0.020(6) -0.014(5) C25 0.059(3) 0.092(7) 0.063(7) -0.024(5) 0.027(5) -0.017(5) C26 0.056(3) 0.078(7) 0.039(6) -0.007(4) 0.012(5) 0.000(5) C27 0.050(5) 0.077(7) 0.059(7) -0.012(5) 0.021(5) -0.006(5) C28 0.067(4) 0.079(7) 0.050(7) -0.014(5) 0.012(6) -0.003(6) C29 0.063(4) 0.069(7) 0.049(7) -0.008(5) 0.000(6) -0.005(6) C30 0.060(5) 0.068(7) 0.043(6) 0.000(4) 0.010(5) -0.006(5) C31 0.106(7) 0.086(8) 0.104(7) 0.014(6) -0.023(7) 0.016(6) C32 0.134(7) 0.088(8) 0.130(7) -0.001(7) -0.042(7) 0.034(6) C33 0.134(7) 0.093(8) 0.147(7) -0.018(7) -0.025(7) 0.046(7) C34 0.101(7) 0.094(8) 0.130(7) -0.014(6) 0.006(7) 0.033(6) C35 0.069(6) 0.063(7) 0.104(5) 0.001(5) 0.012(5) 0.002(5) C36 0.046(6) 0.077(7) 0.083(5) -0.002(5) 0.010(5) -0.003(4) C37 0.054(6) 0.095(8) 0.080(5) -0.011(5) 0.012(5) 0.005(5) C38 0.066(6) 0.080(7) 0.073(5) -0.003(4) 0.019(5) -0.006(5) C39 0.043(6) 0.074(7) 0.059(5) 0.003(5) 0.005(5) -0.012(5) C40 0.052(6) 0.060(7) 0.061(5) 0.003(5) 0.010(5) -0.008(4) C41 0.058(6) 0.053(7) 0.069(5) 0.010(5) 0.018(5) -0.005(4) C42 0.061(6) 0.075(7) 0.086(6) 0.023(6) 0.019(5) 0.005(5) C43 0.082(6) 0.089(8) 0.093(6) 0.004(6) 0.013(6) 0.027(6) C44 0.066(6) 0.101(8) 0.080(6) -0.013(6) 0.010(6) 0.016(5) C45 0.051(6) 0.099(8) 0.066(6) 0.000(6) 0.012(5) 0.000(5) C46 0.069(6) 0.060(7) 0.087(6) 0.016(6) 0.020(6) -0.008(5) C47 0.081(6) 0.064(7) 0.109(6) 0.019(6) 0.011(7) -0.020(5) C48 0.086(7) 0.077(8) 0.107(5) 0.016(7) -0.006(7) -0.025(5) C49 0.097(6) 0.050(7) 0.086(5) 0.014(6) -0.010(6) -0.015(5) C50 0.068(6) 0.059(7) 0.072(4) 0.012(5) 0.003(5) -0.009(4) C51 0.059(6) 0.052(7) 0.068(3) 0.021(5) -0.004(5) 0.000(4) C52 0.072(6) 0.056(7) 0.066(4) 0.015(5) 0.002(6) 0.002(5) C53 0.051(6) 0.086(8) 0.070(3) 0.025(5) -0.002(5) -0.001(5) C54 0.063(6) 0.090(8) 0.071(3) 0.020(6) 0.006(5) -0.015(6) C55 0.076(6) 0.057(7) 0.070(3) 0.019(5) 0.001(5) -0.014(5) C56 0.065(6) 0.071(7) 0.072(3) 0.020(6) -0.003(5) -0.013(5) C57 0.098(7) 0.092(8) 0.078(5) 0.030(6) -0.015(6) -0.039(5) C58 0.117(7) 0.110(9) 0.083(6) 0.024(7) -0.019(6) -0.052(6) C59 0.130(7) 0.110(8) 0.077(5) 0.025(7) -0.024(7) -0.055(6) C60 0.091(6) 0.094(8) 0.071(4) 0.022(6) -0.017(6) -0.026(6) C61 0.075(5) 0.086(8) 0.145(8) -0.036(6) -0.002(5) -0.003(7) C62 0.088(5) 0.105(9) 0.174(8) -0.065(7) 0.000(7) -0.007(7) C63 0.099(5) 0.085(8) 0.173(8) -0.060(7) -0.005(6) 0.015(7) C64 0.086(5) 0.077(8) 0.166(8) -0.046(6) 0.004(6) 0.005(7) C65 0.070(4) 0.060(8) 0.113(7) -0.008(5) 0.004(5) 0.001(6) C66 0.064(3) 0.085(8) 0.085(7) 0.003(5) 0.012(4) -0.002(6) C67 0.066(3) 0.077(8) 0.096(7) -0.006(6) 0.006(5) 0.005(6) C68 0.061(3) 0.088(8) 0.074(7) 0.009(5) 0.015(4) -0.004(5) C69 0.062(3) 0.087(8) 0.055(6) 0.020(5) 0.010(5) 0.003(6) C70 0.062(3) 0.099(8) 0.065(6) 0.013(5) 0.007(5) 0.007(6) C71 0.064(3) 0.123(8) 0.049(6) 0.014(5) 0.005(4) 0.011(6) C72 0.070(5) 0.163(9) 0.055(7) -0.003(6) 0.015(5) -0.009(7) C73 0.084(5) 0.177(9) 0.068(7) -0.022(6) 0.028(6) -0.017(7) C74 0.077(4) 0.138(9) 0.063(7) 0.009(5) 0.029(6) -0.001(7) C75 0.063(5) 0.122(9) 0.070(7) 0.013(5) 0.016(5) 0.004(6) C76 0.083(4) 0.050(6) 0.049(7) -0.013(5) 0.009(6) -0.017(5) C77 0.114(4) 0.052(7) 0.078(8) 0.003(5) 0.007(7) -0.029(6) C78 0.125(5) 0.054(7) 0.063(8) 0.015(6) 0.001(7) -0.014(6) C79 0.101(5) 0.058(7) 0.070(8) 0.017(5) 0.011(7) 0.007(5) C80 0.078(3) 0.060(6) 0.035(6) 0.006(4) 0.004(6) -0.001(4) C81 0.068(3) 0.051(6) 0.049(7) 0.000(4) 0.005(5) 0.005(4) C82 0.069(3) 0.061(6) 0.041(6) -0.004(5) 0.004(6) 0.010(5) C83 0.065(3) 0.074(7) 0.063(7) 0.002(5) 0.001(6) 0.000(4) C84 0.067(3) 0.076(7) 0.085(8) 0.020(6) 0.002(6) -0.010(5) C85 0.066(3) 0.089(7) 0.080(8) 0.035(6) 0.000(6) -0.007(5) C86 0.075(3) 0.104(7) 0.154(9) 0.076(6) 0.004(7) -0.006(5) C87 0.100(5) 0.152(8) 0.249(10) 0.142(7) 0.010(8) -0.012(6) C88 0.121(5) 0.168(8) 0.309(10) 0.175(7) 0.004(9) -0.006(7) C89 0.115(5) 0.173(8) 0.317(10) 0.181(7) -0.002(9) 0.007(7) C90 0.089(5) 0.144(8) 0.252(10) 0.135(7) 0.018(8) 0.023(6) C91 0.104(7) 0.133(8) 0.054(5) 0.007(6) -0.008(6) -0.001(6) C92 0.122(7) 0.109(8) 0.058(5) 0.002(7) -0.019(6) 0.002(6) C93 0.103(7) 0.092(8) 0.070(6) 0.001(6) -0.016(6) -0.004(6) C94 0.086(6) 0.099(8) 0.057(5) 0.013(6) -0.013(6) -0.014(5) C95 0.079(6) 0.071(7) 0.058(4) 0.007(5) 0.004(5) 0.003(4) C96 0.069(6) 0.062(7) 0.054(4) 0.014(5) 0.002(5) 0.006(4) C97 0.054(6) 0.079(7) 0.047(4) 0.018(5) -0.010(5) 0.003(5) C98 0.040(5) 0.099(8) 0.060(4) 0.004(5) -0.009(4) 0.006(5) C99 0.050(6) 0.077(8) 0.079(4) -0.002(6) -0.001(5) 0.007(5) C100 0.056(6) 0.081(7) 0.074(4) 0.020(5) -0.007(5) 0.003(5) C101 0.075(6) 0.069(7) 0.099(4) 0.027(6) 0.001(5) -0.001(5) C102 0.075(6) 0.078(8) 0.131(6) 0.010(7) 0.008(6) -0.007(5) C103 0.089(6) 0.087(8) 0.149(6) 0.032(8) 0.006(7) -0.015(6) C104 0.090(6) 0.129(9) 0.141(6) 0.062(8) -0.004(7) -0.020(6) C105 0.077(6) 0.118(8) 0.117(6) 0.053(7) 0.009(6) -0.004(5) C106 0.074(6) 0.092(8) 0.077(6) 0.017(6) 0.010(6) 0.003(5) C107 0.107(7) 0.081(8) 0.090(6) 0.006(7) 0.009(7) 0.020(5) C108 0.097(7) 0.105(8) 0.102(6) 0.040(7) 0.019(7) 0.024(6) C109 0.086(6) 0.101(8) 0.078(6) 0.026(6) -0.002(6) 0.014(5) C110 0.075(6) 0.089(8) 0.069(4) 0.023(5) 0.002(5) 0.005(5) C111 0.070(6) 0.113(8) 0.072(4) 0.034(6) 0.013(5) 0.009(5) C112 0.060(6) 0.146(9) 0.074(4) 0.040(6) 0.020(6) 0.007(6) C113 0.082(6) 0.166(9) 0.073(3) 0.035(6) 0.020(6) 0.026(6) C114 0.070(6) 0.145(9) 0.076(4) 0.030(6) 0.020(6) 0.014(6) C115 0.055(6) 0.130(8) 0.074(4) 0.029(5) 0.013(6) 0.012(5) C116 0.076(6) 0.099(8) 0.075(4) 0.022(5) 0.013(6) 0.009(5) C117 0.056(6) 0.123(8) 0.080(6) 0.013(6) 0.002(6) 0.012(5) C118 0.072(6) 0.102(8) 0.089(6) 0.014(6) 0.002(6) 0.010(6) C119 0.076(6) 0.083(8) 0.088(5) 0.032(6) 0.014(6) 0.005(5) C120 0.075(6) 0.102(8) 0.080(5) 0.028(6) 0.010(6) 0.014(5) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.0743(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . N1 . 1.983(7) yes Fe1 . N2 . 1.921(8) yes Fe1 . N3 . 1.979(9) yes Fe1 . N4 . 1.999(8) yes Fe1 . N5 . 1.901(8) yes Fe1 . N6 . 1.982(7) yes Fe2 . N7 . 1.999(9) yes Fe2 . N8 . 1.883(7) yes Fe2 . N9 . 1.973(8) yes Fe2 . N10 . 1.981(8) yes Fe2 . N11 . 1.886(7) yes Fe2 . N12 . 1.985(9) yes Fe3 . N13 . 1.997(10) yes Fe3 . N14 . 1.869(8) yes Fe3 . N15 . 1.932(9) yes Fe3 . N16 . 1.992(8) yes Fe3 . N17 . 1.901(8) yes Fe3 . N18 . 1.981(10) yes Fe4 . N19 . 1.923(10) yes Fe4 . N20 . 1.844(7) yes Fe4 . N21 . 2.017(11) yes Fe4 . N22 . 1.960(9) yes Fe4 . N23 . 1.850(8) yes Fe4 . N24 . 1.961(9) yes S1 . S2 . 2.019(8) yes S1 . C23 . 1.749(9) yes S2 . C38 . 1.834(9) yes S3 . S4 . 2.033(8) yes S3 . C53 . 1.783(8) yes S4 . C68 . 1.777(9) yes S5 . S6 . 2.018(8) yes S5 . C83 . 1.806(9) yes S6 . C98 . 1.806(9) yes S7 . S8 . 2.021(10) yes S7 . C113 . 1.737(10) yes S8 . C8 . 1.736(10) yes N1 . C1 . 1.364 yes N1 . C5 . 1.357 yes N2 . C6 . 1.316 yes N2 . C10 . 1.352 yes N3 . C11 . 1.391 yes N3 . C15 . 1.327 yes N4 . C16 . 1.277 yes N4 . C20 . 1.384 yes N5 . C21 . 1.373 yes N5 . C25 . 1.351 yes N6 . C26 . 1.345 yes N6 . C30 . 1.343 yes N7 . C31 . 1.345 yes N7 . C35 . 1.347 yes N8 . C36 . 1.355 yes N8 . C40 . 1.338 yes N9 . C41 . 1.440 yes N9 . C45 . 1.372 yes N10 . C46 . 1.318 yes N10 . C50 . 1.399 yes N11 . C51 . 1.341 yes N11 . C55 . 1.347 yes N12 . C56 . 1.373 yes N12 . C60 . 1.345 yes N13 . C61 . 1.429 yes N13 . C65 . 1.389 yes N14 . C66 . 1.368 yes N14 . C70 . 1.374 yes N15 . C71 . 1.429 yes N15 . C75 . 1.384 yes N16 . C76 . 1.341 yes N16 . C80 . 1.355 yes N17 . C81 . 1.327 yes N17 . C85 . 1.345 yes N18 . C86 . 1.397 yes N18 . C90 . 1.378 yes N19 . C91 . 1.377 yes N19 . C95 . 1.357 yes N20 . C96 . 1.379 yes N20 . C100 . 1.404 yes N21 . C101 . 1.404 yes N21 . C105 . 1.364 yes N22 . C106 . 1.337 yes N22 . C110 . 1.341 yes N23 . C111 . 1.365 yes N23 . C115 . 1.373 yes N24 . C116 . 1.367 yes N24 . C120 . 1.399 yes C1 . C2 . 1.385 yes C1 . H11 . 0.960 no C2 . C3 . 1.363 yes C2 . H21 . 0.960 no C3 . C4 . 1.367 yes C3 . H31 . 0.960 no C4 . C5 . 1.362 yes C4 . H41 . 0.960 no C5 . C6 . 1.467(11) yes C6 . C7 . 1.372 yes C7 . C8 . 1.433 yes C7 . H71 . 0.960 no C8 . C9 . 1.448 yes C9 . C10 . 1.359 yes C9 . H91 . 0.960 no C10 . C11 . 1.515(11) yes C11 . C12 . 1.351 yes C12 . C13 . 1.348 yes C12 . H121 . 0.960 no C13 . C14 . 1.355 yes C13 . H131 . 0.960 no C14 . C15 . 1.446 yes C14 . H141 . 0.960 no C15 . H151 . 0.960 no C16 . C17 . 1.488 yes C16 . H161 . 0.960 no C17 . C18 . 1.444 yes C17 . H171 . 0.960 no C18 . C19 . 1.357 yes C18 . H181 . 0.960 no C19 . C20 . 1.351 yes C19 . H191 . 0.960 no C20 . C21 . 1.508(11) yes C21 . C22 . 1.387 yes C22 . C23 . 1.413 yes C22 . H221 . 0.960 no C23 . C24 . 1.394 yes C24 . C25 . 1.397 yes C24 . H241 . 0.960 no C25 . C26 . 1.458(10) yes C26 . C27 . 1.371 yes C27 . C28 . 1.424 yes C27 . H271 . 0.960 no C28 . C29 . 1.325 yes C28 . H281 . 0.960 no C29 . C30 . 1.413 yes C29 . H291 . 0.960 no C30 . H301 . 0.960 no C31 . C32 . 1.371 yes C31 . H311 . 0.960 no C32 . C33 . 1.325 yes C32 . H321 . 0.960 no C33 . C34 . 1.455 yes C33 . H331 . 0.960 no C34 . C35 . 1.420 yes C34 . H341 . 0.960 no C35 . C36 . 1.470(13) yes C36 . C37 . 1.422 yes C37 . C38 . 1.341 yes C37 . H371 . 0.960 no C38 . C39 . 1.373 yes C39 . C40 . 1.367 yes C39 . H391 . 0.960 no C40 . C41 . 1.469(10) yes C41 . C42 . 1.379 yes C42 . C43 . 1.431 yes C42 . H421 . 0.960 no C43 . C44 . 1.471 yes C43 . H431 . 0.960 no C44 . C45 . 1.350 yes C44 . H441 . 0.960 no C45 . H451 . 0.960 no C46 . C47 . 1.357 yes C46 . H461 . 0.960 no C47 . C48 . 1.386 yes C47 . H471 . 0.960 no C48 . C49 . 1.340 yes C48 . H481 . 0.960 no C49 . C50 . 1.387 yes C49 . H491 . 0.960 no C50 . C51 . 1.457(10) yes C51 . C52 . 1.401 yes C52 . C53 . 1.344 yes C52 . H521 . 0.960 no C53 . C54 . 1.389 yes C54 . C55 . 1.420 yes C54 . H541 . 0.960 no C55 . C56 . 1.457(12) yes C56 . C57 . 1.377 yes C57 . C58 . 1.335 yes C57 . H571 . 0.960 no C58 . C59 . 1.355 yes C58 . H581 . 0.960 no C59 . C60 . 1.392 yes C59 . H591 . 0.960 no C60 . H601 . 0.960 no C61 . C62 . 1.286 yes C61 . H611 . 0.960 no C62 . C63 . 1.369 yes C62 . H621 . 0.960 no C63 . C64 . 1.378 yes C63 . H631 . 0.960 no C64 . C65 . 1.350 yes C64 . H641 . 0.960 no C65 . C66 . 1.443(13) yes C66 . C67 . 1.340 yes C67 . C68 . 1.392 yes C67 . H671 . 0.960 no C68 . C69 . 1.476 yes C69 . C70 . 1.359 yes C69 . H691 . 0.960 no C70 . C71 . 1.458(11) yes C71 . C72 . 1.364 yes C72 . C73 . 1.452 yes C72 . H721 . 0.960 no C73 . C74 . 1.323 yes C73 . H731 . 0.960 no C74 . C75 . 1.387 yes C74 . H741 . 0.960 no C75 . H751 . 0.960 no C76 . C77 . 1.435 yes C76 . H761 . 0.960 no C77 . C78 . 1.345 yes C77 . H771 . 0.960 no C78 . C79 . 1.389 yes C78 . H781 . 0.960 no C79 . C80 . 1.376 yes C79 . H791 . 0.960 no C80 . C81 . 1.460(10) yes C81 . C82 . 1.382 yes C82 . C83 . 1.429 yes C82 . H821 . 0.960 no C83 . C84 . 1.389 yes C84 . C85 . 1.367 yes C84 . H841 . 0.960 no C85 . C86 . 1.459(13) yes C86 . C87 . 1.387 yes C87 . C88 . 1.394 yes C87 . H871 . 0.960 no C88 . C89 . 1.387 yes C88 . H881 . 0.960 no C89 . C90 . 1.386 yes C89 . H891 . 0.960 no C90 . H901 . 0.960 no C91 . C92 . 1.354 yes C91 . H911 . 0.960 no C92 . C93 . 1.422 yes C92 . H921 . 0.960 no C93 . C94 . 1.420 yes C93 . H931 . 0.960 no C94 . C95 . 1.421 yes C94 . H941 . 0.960 no C95 . C96 . 1.473(11) yes C96 . C97 . 1.377 yes C97 . C98 . 1.406 yes C97 . H971 . 0.960 no C98 . C99 . 1.401 yes C99 . C100 . 1.331 yes C99 . H991 . 0.960 no C100 . C101 . 1.424(11) yes C101 . C102 . 1.342 yes C102 . C103 . 1.420 yes C102 . H1021 . 0.960 no C103 . C104 . 1.314 yes C103 . H1031 . 0.960 no C104 . C105 . 1.384 yes C104 . H1041 . 0.960 no C105 . H1051 . 0.960 no C106 . C107 . 1.402 yes C106 . H1061 . 0.960 no C107 . C108 . 1.369 yes C107 . H1071 . 0.960 no C108 . C109 . 1.330 yes C108 . H1081 . 0.960 no C109 . C110 . 1.397 yes C109 . H1091 . 0.960 no C110 . C111 . 1.550(13) yes C111 . C112 . 1.422 yes C112 . C113 . 1.365 yes C112 . H1121 . 0.960 no C113 . C114 . 1.401 yes C114 . C115 . 1.381 yes C114 . H1141 . 0.960 no C115 . C116 . 1.504(12) yes C116 . C117 . 1.363 yes C117 . C118 . 1.473 yes C117 . H1171 . 0.960 no C118 . C119 . 1.453 yes C118 . H1181 . 0.960 no C119 . C120 . 1.352 yes C119 . H1191 . 0.960 no C120 . H1201 . 0.960 no B1 . F1 . 1.370 yes B1 . F2 . 1.388 yes B1 . F3 . 1.39643(5) yes B1 . F4 . 1.374 yes B2 . F5 . 1.362 yes B2 . F6 . 1.364 yes B2 . F7 . 1.381 yes B2 . F8 . 1.38109(5) yes B3 . F9 . 1.370 yes B3 . F10 . 1.361 yes B3 . F11 . 1.369 yes B3 . F12 . 1.381 yes B4 . F13 . 1.375 yes B4 . F14 . 1.38821(5) yes B4 . F15 . 1.368 yes B4 . F16 . 1.350 yes B5 . F17 . 1.37802(5) yes B5 . F18 . 1.361 yes B5 . F19 . 1.374 yes B5 . F20 . 1.371 yes N50 . C501 . 1.173 yes C501 . C502 . 1.504 yes C502 . H5021 . 0.960 no C502 . H5022 . 0.960 no C502 . H5023 . 0.960 no N51 . C511 . 0.984 yes C511 . C512 . 1.38660(6) yes C512 . H5121 . 0.960 no C512 . H5122 . 0.960 no C512 . H5123 . 0.959 no B6 . F21 . 1.371 yes B6 . F22 . 1.362 yes B6 . F23 . 1.375 yes B6 . F24 . 1.373 yes B7 . F25 . 1.371 yes B7 . F26 . 1.384 yes B7 . F27 . 1.36830(5) yes B7 . F28 . 1.358 yes B8 . F29 . 1.363 yes B8 . F30 . 1.378 yes B8 . F31 . 1.364 yes B8 . F32 . 1.385 yes N52 . C521 . 1.157 yes C521 . C522 . 1.500 yes C522 . H5221 . 0.960 no C522 . H5222 . 0.960 no C522 . H5223 . 0.960 no N53 . C531 . 1.150 yes C531 . C532 . 1.499 yes C532 . H5321 . 0.960 no C532 . H5322 . 0.960 no C532 . H5323 . 0.960 no N54 . C541 . 1.160 yes C541 . C542 . 1.50024(5) yes C542 . H5421 . 0.960 no C542 . H5422 . 0.960 no C542 . H5423 . 0.960 no N55 . C551 . 1.15052(17) yes C551 . C552 . 1.5032(2) yes C552 . H552 . 0.959 no C552 . H553 . 0.960 no C552 . H554 . 0.962 no O60 . C602 . 1.450 yes O60 . C603 . 1.445 yes C601 . C602 . 1.494 yes C601 . H6011 . 0.960 no C601 . H6012 . 0.960 no C601 . H6013 . 0.960 no C602 . H6021 . 0.960 no C602 . H6022 . 0.960 no C603 . C604 . 1.499 yes C603 . H6031 . 0.960 no C603 . H6032 . 0.960 no C604 . H6041 . 0.960 no C604 . H6042 . 0.959 no C604 . H6043 . 0.960 no O61 . C611 . 1.400 yes O611 . C611 . 1.555 yes O611 . H6113 . 0.629 no C611 . H6111 . 0.960 no C611 . H6112 . 0.960 no C611 . H6113 . 0.960 no C611 . H6114 . 0.960 no O62 . C622 . 1.450 yes O62 . C623 . 1.449 yes C621 . C622 . 1.498 yes C621 . H6211 . 0.960 no C621 . H6212 . 0.960 no C621 . H6213 . 0.960 no C622 . H6221 . 0.960 no C622 . H6222 . 0.960 no C623 . C624 . 1.503 yes C623 . H6231 . 0.960 no C623 . H6232 . 0.960 no C624 . H6241 . 0.960 no C624 . H6242 . 0.960 no C624 . H6243 . 0.960 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Fe1 . N2 . 80.5(4) yes N1 . Fe1 . N3 . 160.9(5) yes N2 . Fe1 . N3 . 80.4(5) yes N1 . Fe1 . N4 . 92.0(4) yes N2 . Fe1 . N4 . 101.2(4) yes N3 . Fe1 . N4 . 90.5(5) yes N1 . Fe1 . N5 . 97.9(5) yes N2 . Fe1 . N5 . 177.0(5) yes N3 . Fe1 . N5 . 101.2(5) yes N4 . Fe1 . N5 . 81.3(4) yes N1 . Fe1 . N6 . 90.3(4) yes N2 . Fe1 . N6 . 97.2(4) yes N3 . Fe1 . N6 . 93.3(5) yes N4 . Fe1 . N6 . 161.6(4) yes N5 . Fe1 . N6 . 80.3(4) yes N7 . Fe2 . N8 . 81.3(5) yes N7 . Fe2 . N9 . 162.5(5) yes N8 . Fe2 . N9 . 81.2(4) yes N7 . Fe2 . N10 . 90.9(5) yes N8 . Fe2 . N10 . 98.7(4) yes N9 . Fe2 . N10 . 92.0(5) yes N7 . Fe2 . N11 . 98.4(5) yes N8 . Fe2 . N11 . 179.4(5) yes N9 . Fe2 . N11 . 99.1(4) yes N10 . Fe2 . N11 . 80.7(4) yes N7 . Fe2 . N12 . 92.1(5) yes N8 . Fe2 . N12 . 99.2(5) yes N9 . Fe2 . N12 . 90.5(5) yes N10 . Fe2 . N12 . 162.1(4) yes N11 . Fe2 . N12 . 81.3(4) yes N13 . Fe3 . N14 . 81.0(5) yes N13 . Fe3 . N15 . 163.1(5) yes N14 . Fe3 . N15 . 82.2(5) yes N13 . Fe3 . N16 . 91.0(5) yes N14 . Fe3 . N16 . 99.2(5) yes N15 . Fe3 . N16 . 90.8(5) yes N13 . Fe3 . N17 . 99.5(5) yes N14 . Fe3 . N17 . 179.3(5) yes N15 . Fe3 . N17 . 97.3(5) yes N16 . Fe3 . N17 . 80.3(4) yes N13 . Fe3 . N18 . 91.1(7) yes N14 . Fe3 . N18 . 98.6(5) yes N15 . Fe3 . N18 . 92.3(6) yes N16 . Fe3 . N18 . 162.2(5) yes N17 . Fe3 . N18 . 81.9(5) yes N19 . Fe4 . N20 . 81.0(5) yes N19 . Fe4 . N21 . 161.5(5) yes N20 . Fe4 . N21 . 80.7(5) yes N19 . Fe4 . N22 . 90.7(5) yes N20 . Fe4 . N22 . 96.4(5) yes N21 . Fe4 . N22 . 94.0(5) yes N19 . Fe4 . N23 . 98.7(6) yes N20 . Fe4 . N23 . 177.6(5) yes N21 . Fe4 . N23 . 99.7(6) yes N22 . Fe4 . N23 . 81.3(5) yes N19 . Fe4 . N24 . 91.7(5) yes N20 . Fe4 . N24 . 101.0(5) yes N21 . Fe4 . N24 . 89.1(5) yes N22 . Fe4 . N24 . 162.7(5) yes N23 . Fe4 . N24 . 81.4(5) yes S2 . S1 . C23 . 105.8(5) yes S1 . S2 . C38 . 104.4(5) yes S4 . S3 . C53 . 104.5(5) yes S3 . S4 . C68 . 108.4(5) yes S6 . S5 . C83 . 104.6(5) yes S5 . S6 . C98 . 104.9(5) yes S8 . S7 . C113 . 107.8(6) yes S7 . S8 . C8 . 106.3(6) yes Fe1 . N1 . C1 . 126.3(6) yes Fe1 . N1 . C5 . 115.8(6) yes C1 . N1 . C5 . 117.822 yes Fe1 . N2 . C6 . 117.2(6) yes Fe1 . N2 . C10 . 119.8(6) yes C6 . N2 . C10 . 122.978 yes Fe1 . N3 . C11 . 116.4(7) yes Fe1 . N3 . C15 . 127.0(7) yes C11 . N3 . C15 . 115.470 yes Fe1 . N4 . C16 . 125.4(6) yes Fe1 . N4 . C20 . 114.5(6) yes C16 . N4 . C20 . 120.049 yes Fe1 . N5 . C21 . 119.9(6) yes Fe1 . N5 . C25 . 119.2(6) yes C21 . N5 . C25 . 120.334 yes Fe1 . N6 . C26 . 114.7(5) yes Fe1 . N6 . C30 . 127.5(5) yes C26 . N6 . C30 . 117.840 yes Fe2 . N7 . C31 . 127.2(7) yes Fe2 . N7 . C35 . 113.7(7) yes C31 . N7 . C35 . 118.720 yes Fe2 . N8 . C36 . 118.7(6) yes Fe2 . N8 . C40 . 120.9(6) yes C36 . N8 . C40 . 120.352 yes Fe2 . N9 . C41 . 113.8(5) yes Fe2 . N9 . C45 . 126.9(5) yes C41 . N9 . C45 . 119.290 yes Fe2 . N10 . C46 . 129.2(6) yes Fe2 . N10 . C50 . 114.8(6) yes C46 . N10 . C50 . 115.754 yes Fe2 . N11 . C51 . 119.3(6) yes Fe2 . N11 . C55 . 117.7(6) yes C51 . N11 . C55 . 122.646 yes Fe2 . N12 . C56 . 114.6(6) yes Fe2 . N12 . C60 . 126.9(6) yes C56 . N12 . C60 . 118.406 yes Fe3 . N13 . C61 . 127.8(7) yes Fe3 . N13 . C65 . 113.8(7) yes C61 . N13 . C65 . 118.434 yes Fe3 . N14 . C66 . 119.5(7) yes Fe3 . N14 . C70 . 119.6(7) yes C66 . N14 . C70 . 120.881 yes Fe3 . N15 . C71 . 114.7(6) yes Fe3 . N15 . C75 . 129.2(6) yes C71 . N15 . C75 . 116.080 yes Fe3 . N16 . C76 . 126.2(6) yes Fe3 . N16 . C80 . 113.2(6) yes C76 . N16 . C80 . 120.579 yes Fe3 . N17 . C81 . 120.2(6) yes Fe3 . N17 . C85 . 118.0(6) yes C81 . N17 . C85 . 121.787 yes Fe3 . N18 . C86 . 113.4(7) yes Fe3 . N18 . C90 . 126.4(7) yes C86 . N18 . C90 . 119.956 yes Fe4 . N19 . C91 . 129.4(6) yes Fe4 . N19 . C95 . 117.4(6) yes C91 . N19 . C95 . 113.169 yes Fe4 . N20 . C96 . 119.8(6) yes Fe4 . N20 . C100 . 120.5(6) yes C96 . N20 . C100 . 119.666 yes Fe4 . N21 . C101 . 113.5(7) yes Fe4 . N21 . C105 . 126.7(7) yes C101 . N21 . C105 . 119.608 yes Fe4 . N22 . C106 . 128.4(7) yes Fe4 . N22 . C110 . 116.7(7) yes C106 . N22 . C110 . 114.943 yes Fe4 . N23 . C111 . 121.5(7) yes Fe4 . N23 . C115 . 121.3(7) yes C111 . N23 . C115 . 116.612 yes Fe4 . N24 . C116 . 114.9(6) yes Fe4 . N24 . C120 . 127.1(6) yes C116 . N24 . C120 . 117.750 yes N1 . C1 . C2 . 119.616 yes N1 . C1 . H11 . 120.191 no C2 . C1 . H11 . 120.192 no C1 . C2 . C3 . 120.467 yes C1 . C2 . H21 . 119.765 no C3 . C2 . H21 . 119.768 no C2 . C3 . C4 . 120.504 yes C2 . C3 . H31 . 119.745 no C4 . C3 . H31 . 119.752 no C3 . C4 . C5 . 117.312 yes C3 . C4 . H41 . 121.340 no C5 . C4 . H41 . 121.348 no C4 . C5 . N1 . 124.088 yes C4 . C5 . C6 . 124.8(7) yes N1 . C5 . C6 . 111.1(7) yes C5 . C6 . N2 . 115.4(7) yes C5 . C6 . C7 . 125.0(7) yes N2 . C6 . C7 . 119.143 yes C6 . C7 . C8 . 119.767 yes C6 . C7 . H71 . 120.120 no C8 . C7 . H71 . 120.113 no C7 . C8 . S8 . 116.4(7) yes C7 . C8 . C9 . 118.629 yes S8 . C8 . C9 . 124.4(7) yes C8 . C9 . C10 . 115.886 yes C8 . C9 . H91 . 122.057 no C10 . C9 . H91 . 122.057 no C9 . C10 . N2 . 122.849 yes C9 . C10 . C11 . 125.2(8) yes N2 . C10 . C11 . 111.7(8) yes C10 . C11 . N3 . 111.0(9) yes C10 . C11 . C12 . 121.9(9) yes N3 . C11 . C12 . 127.088 yes C11 . C12 . C13 . 114.279 yes C11 . C12 . H121 . 122.864 no C13 . C12 . H121 . 122.857 no C12 . C13 . C14 . 124.955 yes C12 . C13 . H131 . 117.527 no C14 . C13 . H131 . 117.518 no C13 . C14 . C15 . 116.560 yes C13 . C14 . H141 . 121.723 no C15 . C14 . H141 . 121.717 no C14 . C15 . N3 . 121.495 yes C14 . C15 . H151 . 119.253 no N3 . C15 . H151 . 119.252 no N4 . C16 . C17 . 119.880 yes N4 . C16 . H161 . 120.067 no C17 . C16 . H161 . 120.053 no C16 . C17 . C18 . 118.943 yes C16 . C17 . H171 . 120.530 no C18 . C17 . H171 . 120.527 no C17 . C18 . C19 . 115.714 yes C17 . C18 . H181 . 122.141 no C19 . C18 . H181 . 122.145 no C18 . C19 . C20 . 122.258 yes C18 . C19 . H191 . 118.870 no C20 . C19 . H191 . 118.872 no N4 . C20 . C19 . 122.843 yes N4 . C20 . C21 . 113.4(8) yes C19 . C20 . C21 . 123.7(8) yes C20 . C21 . N5 . 110.6(8) yes C20 . C21 . C22 . 126.9(8) yes N5 . C21 . C22 . 122.410 yes C21 . C22 . C23 . 116.589 yes C21 . C22 . H221 . 121.706 no C23 . C22 . H221 . 121.705 no C22 . C23 . S1 . 112.0(7) yes C22 . C23 . C24 . 120.896 yes S1 . C23 . C24 . 127.1(7) yes C23 . C24 . C25 . 119.211 yes C23 . C24 . H241 . 120.394 no C25 . C24 . H241 . 120.395 no C24 . C25 . N5 . 120.223 yes C24 . C25 . C26 . 128.7(7) yes N5 . C25 . C26 . 110.9(7) yes C25 . C26 . N6 . 114.6(7) yes C25 . C26 . C27 . 123.1(7) yes N6 . C26 . C27 . 122.052 yes C26 . C27 . C28 . 119.358 yes C26 . C27 . H271 . 120.319 no C28 . C27 . H271 . 120.323 no C27 . C28 . C29 . 118.639 yes C27 . C28 . H281 . 120.680 no C29 . C28 . H281 . 120.681 no C28 . C29 . C30 . 119.354 yes C28 . C29 . H291 . 120.325 no C30 . C29 . H291 . 120.320 no C29 . C30 . N6 . 122.595 yes C29 . C30 . H301 . 118.706 no N6 . C30 . H301 . 118.699 no N7 . C31 . C32 . 124.827 yes N7 . C31 . H311 . 117.589 no C32 . C31 . H311 . 117.584 no C31 . C32 . C33 . 115.633 yes C31 . C32 . H321 . 122.183 no C33 . C32 . H321 . 122.185 no C32 . C33 . C34 . 125.388 yes C32 . C33 . H331 . 117.304 no C34 . C33 . H331 . 117.308 no C33 . C34 . C35 . 112.552 yes C33 . C34 . H341 . 123.725 no C35 . C34 . H341 . 123.723 no C34 . C35 . N7 . 122.698 yes C34 . C35 . C36 . 123.1(9) yes N7 . C35 . C36 . 114.2(9) yes C35 . C36 . N8 . 111.9(8) yes C35 . C36 . C37 . 126.9(8) yes N8 . C36 . C37 . 121.108 yes C36 . C37 . C38 . 114.425 yes C36 . C37 . H371 . 122.790 no C38 . C37 . H371 . 122.784 no S2 . C38 . C37 . 121.1(7) yes S2 . C38 . C39 . 112.4(7) yes C37 . C38 . C39 . 126.192 yes C38 . C39 . C40 . 115.921 yes C38 . C39 . H391 . 122.040 no C40 . C39 . H391 . 122.039 no C39 . C40 . N8 . 121.903 yes C39 . C40 . C41 . 125.7(7) yes N8 . C40 . C41 . 112.2(7) yes C40 . C41 . N9 . 111.7(7) yes C40 . C41 . C42 . 125.3(7) yes N9 . C41 . C42 . 122.967 yes C41 . C42 . C43 . 118.463 yes C41 . C42 . H421 . 120.768 no C43 . C42 . H421 . 120.770 no C42 . C43 . C44 . 115.568 yes C42 . C43 . H431 . 122.217 no C44 . C43 . H431 . 122.215 no C43 . C44 . C45 . 124.532 yes C43 . C44 . H441 . 117.735 no C45 . C44 . H441 . 117.732 no N9 . C45 . C44 . 118.818 yes N9 . C45 . H451 . 120.590 no C44 . C45 . H451 . 120.592 no N10 . C46 . C47 . 123.980 yes N10 . C46 . H461 . 118.014 no C47 . C46 . H461 . 118.006 no C46 . C47 . C48 . 120.124 yes C46 . C47 . H471 . 119.945 no C48 . C47 . H471 . 119.931 no C47 . C48 . C49 . 118.373 yes C47 . C48 . H481 . 120.822 no C49 . C48 . H481 . 120.805 no C48 . C49 . C50 . 119.820 yes C48 . C49 . H491 . 120.096 no C50 . C49 . H491 . 120.083 no N10 . C50 . C49 . 121.759 yes N10 . C50 . C51 . 111.5(8) yes C49 . C50 . C51 . 126.7(8) yes C50 . C51 . N11 . 113.4(8) yes C50 . C51 . C52 . 128.2(8) yes N11 . C51 . C52 . 118.343 yes C51 . C52 . C53 . 120.877 yes C51 . C52 . H521 . 119.559 no C53 . C52 . H521 . 119.564 no S3 . C53 . C52 . 125.9(7) yes S3 . C53 . C54 . 112.6(7) yes C52 . C53 . C54 . 120.946 yes C53 . C54 . C55 . 117.397 yes C53 . C54 . H541 . 121.300 no C55 . C54 . H541 . 121.303 no C54 . C55 . N11 . 119.734 yes C54 . C55 . C56 . 126.0(8) yes N11 . C55 . C56 . 114.3(8) yes C55 . C56 . N12 . 111.9(8) yes C55 . C56 . C57 . 126.6(8) yes N12 . C56 . C57 . 121.490 yes C56 . C57 . C58 . 119.141 yes C56 . C57 . H571 . 120.425 no C58 . C57 . H571 . 120.434 no C57 . C58 . C59 . 120.495 yes C57 . C58 . H581 . 119.751 no C59 . C58 . H581 . 119.754 no C58 . C59 . C60 . 120.178 yes C58 . C59 . H591 . 119.911 no C60 . C59 . H591 . 119.911 no C59 . C60 . N12 . 120.077 yes C59 . C60 . H601 . 119.961 no N12 . C60 . H601 . 119.962 no N13 . C61 . C62 . 118.775 yes N13 . C61 . H611 . 120.618 no C62 . C61 . H611 . 120.607 no C61 . C62 . C63 . 122.280 yes C61 . C62 . H621 . 118.867 no C63 . C62 . H621 . 118.852 no C62 . C63 . C64 . 121.509 yes C62 . C63 . H631 . 119.256 no C64 . C63 . H631 . 119.236 no C63 . C64 . C65 . 117.023 yes C63 . C64 . H641 . 121.498 no C65 . C64 . H641 . 121.478 no N13 . C65 . C64 . 121.406 yes N13 . C65 . C66 . 113.2(10) yes C64 . C65 . C66 . 125.3(10) yes C65 . C66 . N14 . 112.5(9) yes C65 . C66 . C67 . 126.5(9) yes N14 . C66 . C67 . 121.053 yes C66 . C67 . C68 . 119.122 yes C66 . C67 . H671 . 120.437 no C68 . C67 . H671 . 120.442 no S4 . C68 . C67 . 116.5(7) yes S4 . C68 . C69 . 122.3(7) yes C67 . C68 . C69 . 121.178 yes C68 . C69 . C70 . 114.518 yes C68 . C69 . H691 . 122.740 no C70 . C69 . H691 . 122.742 no N14 . C70 . C69 . 122.807 yes N14 . C70 . C71 . 111.4(9) yes C69 . C70 . C71 . 125.8(9) yes C70 . C71 . N15 . 112.1(9) yes C70 . C71 . C72 . 126.3(9) yes N15 . C71 . C72 . 121.539 yes C71 . C72 . C73 . 120.249 yes C71 . C72 . H721 . 119.879 no C73 . C72 . H721 . 119.872 no C72 . C73 . C74 . 116.850 yes C72 . C73 . H731 . 121.580 no C74 . C73 . H731 . 121.570 no C73 . C74 . C75 . 123.518 yes C73 . C74 . H741 . 118.247 no C75 . C74 . H741 . 118.236 no C74 . C75 . N15 . 121.407 yes C74 . C75 . H751 . 119.301 no N15 . C75 . H751 . 119.292 no N16 . C76 . C77 . 118.585 yes N16 . C76 . H761 . 120.711 no C77 . C76 . H761 . 120.704 no C76 . C77 . C78 . 120.125 yes C76 . C77 . H771 . 119.942 no C78 . C77 . H771 . 119.933 no C77 . C78 . C79 . 120.485 yes C77 . C78 . H781 . 119.761 no C79 . C78 . H781 . 119.753 no C78 . C79 . C80 . 117.966 yes C78 . C79 . H791 . 121.020 no C80 . C79 . H791 . 121.015 no C79 . C80 . N16 . 122.193 yes C79 . C80 . C81 . 122.4(8) yes N16 . C80 . C81 . 115.4(8) yes C80 . C81 . N17 . 110.8(8) yes C80 . C81 . C82 . 128.7(8) yes N17 . C81 . C82 . 120.010 yes C81 . C82 . C83 . 116.765 yes C81 . C82 . H821 . 121.619 no C83 . C82 . H821 . 121.617 no S5 . C83 . C82 . 112.5(7) yes S5 . C83 . C84 . 124.9(7) yes C82 . C83 . C84 . 122.620 yes C83 . C84 . C85 . 114.724 yes C83 . C84 . H841 . 122.638 no C85 . C84 . H841 . 122.637 no C84 . C85 . N17 . 123.656 yes C84 . C85 . C86 . 122.7(8) yes N17 . C85 . C86 . 113.5(8) yes C85 . C86 . N18 . 113.1(9) yes C85 . C86 . C87 . 127.2(9) yes N18 . C86 . C87 . 119.697 yes C86 . C87 . C88 . 119.818 yes C86 . C87 . H871 . 120.086 no C88 . C87 . H871 . 120.096 no C87 . C88 . C89 . 119.989 yes C87 . C88 . H881 . 119.999 no C89 . C88 . H881 . 120.012 no C88 . C89 . C90 . 119.685 yes C88 . C89 . H891 . 120.155 no C90 . C89 . H891 . 120.159 no C89 . C90 . N18 . 120.159 yes C89 . C90 . H901 . 119.922 no N18 . C90 . H901 . 119.919 no N19 . C91 . C92 . 126.379 yes N19 . C91 . H911 . 116.811 no C92 . C91 . H911 . 116.810 no C91 . C92 . C93 . 119.539 yes C91 . C92 . H921 . 120.232 no C93 . C92 . H921 . 120.229 no C92 . C93 . C94 . 117.348 yes C92 . C93 . H931 . 121.328 no C94 . C93 . H931 . 121.324 no C93 . C94 . C95 . 116.996 yes C93 . C94 . H941 . 121.504 no C95 . C94 . H941 . 121.500 no C94 . C95 . N19 . 126.415 yes C94 . C95 . C96 . 122.2(8) yes N19 . C95 . C96 . 111.4(8) yes C95 . C96 . N20 . 110.4(8) yes C95 . C96 . C97 . 128.1(8) yes N20 . C96 . C97 . 121.453 yes C96 . C97 . C98 . 116.910 yes C96 . C97 . H971 . 121.545 no C98 . C97 . H971 . 121.546 no S6 . C98 . C97 . 123.3(6) yes S6 . C98 . C99 . 115.0(7) yes C97 . C98 . C99 . 121.565 yes C98 . C99 . C100 . 119.681 yes C98 . C99 . H991 . 120.161 no C100 . C99 . H991 . 120.158 no N20 . C100 . C99 . 120.435 yes N20 . C100 . C101 . 111.7(9) yes C99 . C100 . C101 . 127.8(9) yes C100 . C101 . N21 . 113.4(10) yes C100 . C101 . C102 . 127.6(10) yes N21 . C101 . C102 . 118.921 yes C101 . C102 . C103 . 123.107 yes C101 . C102 . H1021 . 118.448 no C103 . C102 . H1021 . 118.445 no C102 . C103 . C104 . 114.413 yes C102 . C103 . H1031 . 122.790 no C104 . C103 . H1031 . 122.797 no C103 . C104 . C105 . 126.316 yes C103 . C104 . H1041 . 116.836 no C105 . C104 . H1041 . 116.848 no C104 . C105 . N21 . 117.558 yes C104 . C105 . H1051 . 121.216 no N21 . C105 . H1051 . 121.226 no N22 . C106 . C107 . 124.502 yes N22 . C106 . H1061 . 117.749 no C107 . C106 . H1061 . 117.749 no C106 . C107 . C108 . 117.382 yes C106 . C107 . H1071 . 121.308 no C108 . C107 . H1071 . 121.309 no C107 . C108 . C109 . 120.179 yes C107 . C108 . H1081 . 119.909 no C109 . C108 . H1081 . 119.911 no C108 . C109 . C110 . 119.045 yes C108 . C109 . H1091 . 120.477 no C110 . C109 . H1091 . 120.478 no C109 . C110 . N22 . 123.843 yes C109 . C110 . C111 . 124.2(8) yes N22 . C110 . C111 . 111.9(8) yes C110 . C111 . N23 . 108.5(8) yes C110 . C111 . C112 . 127.0(8) yes N23 . C111 . C112 . 124.430 yes C111 . C112 . C113 . 115.938 yes C111 . C112 . H1121 . 122.035 no C113 . C112 . H1121 . 122.027 no S7 . C113 . C112 . 123.5(8) yes S7 . C113 . C114 . 114.7(8) yes C112 . C113 . C114 . 121.437 yes C113 . C114 . C115 . 119.097 yes C113 . C114 . H1141 . 120.453 no C115 . C114 . H1141 . 120.450 no C114 . C115 . N23 . 122.153 yes C114 . C115 . C116 . 129.1(9) yes N23 . C115 . C116 . 108.8(9) yes C115 . C116 . N24 . 113.2(9) yes C115 . C116 . C117 . 122.1(8) yes N24 . C116 . C117 . 124.580 yes C116 . C117 . C118 . 117.607 yes C116 . C117 . H1171 . 121.194 no C118 . C117 . H1171 . 121.199 no C117 . C118 . C119 . 117.512 yes C117 . C118 . H1181 . 121.243 no C119 . C118 . H1181 . 121.245 no C118 . C119 . C120 . 119.052 yes C118 . C119 . H1191 . 120.474 no C120 . C119 . H1191 . 120.473 no N24 . C120 . C119 . 123.173 yes N24 . C120 . H1201 . 118.413 no C119 . C120 . H1201 . 118.413 no F1 . B1 . F2 . 110.633 yes F1 . B1 . F3 . 107.180 yes F2 . B1 . F3 . 110.310 yes F1 . B1 . F4 . 108.563 yes F2 . B1 . F4 . 109.528 yes F3 . B1 . F4 . 110.589 yes F5 . B2 . F6 . 110.298 yes F5 . B2 . F7 . 113.033 yes F6 . B2 . F7 . 111.367 yes F5 . B2 . F8 . 105.876 yes F6 . B2 . F8 . 106.986 yes F7 . B2 . F8 . 108.944(3) yes F9 . B3 . F10 . 113.381 yes F9 . B3 . F11 . 112.975 yes F10 . B3 . F11 . 105.609 yes F9 . B3 . F12 . 109.032 yes F10 . B3 . F12 . 105.477 yes F11 . B3 . F12 . 110.066(3) yes F13 . B4 . F14 . 108.033(3) yes F13 . B4 . F15 . 109.265(3) yes F14 . B4 . F15 . 108.068 yes F13 . B4 . F16 . 110.520 yes F14 . B4 . F16 . 110.091 yes F15 . B4 . F16 . 110.786 yes F17 . B5 . F18 . 109.509 yes F17 . B5 . F19 . 109.451 yes F18 . B5 . F19 . 109.915 yes F17 . B5 . F20 . 108.776 yes F18 . B5 . F20 . 109.816 yes F19 . B5 . F20 . 109.353 yes N50 . C501 . C502 . 173.659(16) yes C501 . C502 . H5021 . 109.471 no C501 . C502 . H5022 . 109.451 no H5021 . C502 . H5022 . 109.456 no C501 . C502 . H5023 . 109.490 no H5021 . C502 . H5023 . 109.488 no H5022 . C502 . H5023 . 109.471 no N51 . C511 . C512 . 168.94(2) yes C511 . C512 . H5121 . 109.447 no C511 . C512 . H5122 . 109.427 no H5121 . C512 . H5122 . 109.419 no C511 . C512 . H5123 . 109.513 no H5121 . C512 . H5123 . 109.515 no H5122 . C512 . H5123 . 109.506 no F21 . B6 . F22 . 109.594 yes F21 . B6 . F23 . 108.956 yes F22 . B6 . F23 . 109.780 yes F21 . B6 . F24 . 109.512 yes F22 . B6 . F24 . 109.669(3) yes F23 . B6 . F24 . 109.314 yes F25 . B7 . F26 . 108.877 yes F25 . B7 . F27 . 109.456(3) yes F26 . B7 . F27 . 109.039 yes F25 . B7 . F28 . 110.309 yes F26 . B7 . F28 . 109.132(3) yes F27 . B7 . F28 . 110.000 yes F29 . B8 . F30 . 109.423 yes F29 . B8 . F31 . 110.317 yes F30 . B8 . F31 . 109.886 yes F29 . B8 . F32 . 109.570(3) yes F30 . B8 . F32 . 108.760(3) yes F31 . B8 . F32 . 108.859 yes N52 . C521 . C522 . 169.017(18) yes C521 . C522 . H5221 . 109.509 no C521 . C522 . H5222 . 109.491 no H5221 . C522 . H5222 . 109.475 no C521 . C522 . H5223 . 109.468 no H5221 . C522 . H5223 . 109.464 no H5222 . C522 . H5223 . 109.422 no N53 . C531 . C532 . 167.290(14) yes C531 . C532 . H5321 . 109.476 no C531 . C532 . H5322 . 109.450 no H5321 . C532 . H5322 . 109.461 no C531 . C532 . H5323 . 109.490 no H5321 . C532 . H5323 . 109.485 no H5322 . C532 . H5323 . 109.465 no N54 . C541 . C542 . 174.38(2) yes C541 . C542 . H5421 . 109.490 no C541 . C542 . H5422 . 109.494 no H5421 . C542 . H5422 . 109.496 no C541 . C542 . H5423 . 109.453 no H5421 . C542 . H5423 . 109.452 no H5422 . C542 . H5423 . 109.444 no N55 . C551 . C552 . 177.2(6) yes C551 . C552 . H552 . 109.541 no C551 . C552 . H553 . 109.577 no H552 . C552 . H553 . 109.634 no C551 . C552 . H554 . 109.322 no H552 . C552 . H554 . 109.419 no H553 . C552 . H554 . 109.334 no C602 . O60 . C603 . 138.180 yes C602 . C601 . H6011 . 109.484 no C602 . C601 . H6012 . 109.482 no H6011 . C601 . H6012 . 109.475 no C602 . C601 . H6013 . 109.458 no H6011 . C601 . H6013 . 109.467 no H6012 . C601 . H6013 . 109.462 no C601 . C602 . O60 . 109.774 yes C601 . C602 . H6021 . 109.367 no O60 . C602 . H6021 . 109.398 no C601 . C602 . H6022 . 109.399 no O60 . C602 . H6022 . 109.424 no H6021 . C602 . H6022 . 109.465 no O60 . C603 . C604 . 109.774 yes O60 . C603 . H6031 . 109.382 no C604 . C603 . H6031 . 109.404 no O60 . C603 . H6032 . 109.392 no C604 . C603 . H6032 . 109.437 no H6031 . C603 . H6032 . 109.438 no C603 . C604 . H6041 . 109.431 no C603 . C604 . H6042 . 109.472 no H6041 . C604 . H6042 . 109.507 no C603 . C604 . H6043 . 109.432 no H6041 . C604 . H6043 . 109.464 no H6042 . C604 . H6043 . 109.521 no C611 . O611 . H6113 . 14.674 no O611 . C611 . O61 . 128.573 yes O611 . C611 . H6111 . 104.505 no O61 . C611 . H6111 . 104.486 no O611 . C611 . H6112 . 104.531 no O61 . C611 . H6112 . 104.506 no H6111 . C611 . H6112 . 109.469 no O611 . C611 . H6113 . 9.560 no O61 . C611 . H6113 . 119.014 no H6111 . C611 . H6113 . 109.487 no H6112 . C611 . H6113 . 109.486 no O611 . C611 . H6114 . 119.024 no O61 . C611 . H6114 . 9.549 no H6111 . C611 . H6114 . 109.461 no H6112 . C611 . H6114 . 109.460 no H6113 . C611 . H6114 . 109.464 no C622 . O62 . C623 . 111.450 yes C622 . C621 . H6211 . 109.490 no C622 . C621 . H6212 . 109.477 no H6211 . C621 . H6212 . 109.477 no C622 . C621 . H6213 . 109.469 no H6211 . C621 . H6213 . 109.466 no H6212 . C621 . H6213 . 109.450 no C621 . C622 . O62 . 109.642(3) yes C621 . C622 . H6221 . 109.411 no O62 . C622 . H6221 . 109.441 no C621 . C622 . H6222 . 109.417 no O62 . C622 . H6222 . 109.439 no H6221 . C622 . H6222 . 109.477 no O62 . C623 . C624 . 109.646 yes O62 . C623 . H6231 . 109.415 no C624 . C623 . H6231 . 109.447 no O62 . C623 . H6232 . 109.426 no C624 . C623 . H6232 . 109.446 no H6231 . C623 . H6232 . 109.447 no C623 . C624 . H6241 . 109.440 no C623 . C624 . H6242 . 109.452 no H6241 . C624 . H6242 . 109.467 no C623 . C624 . H6243 . 109.464 no H6241 . C624 . H6243 . 109.494 no H6242 . C624 . H6243 . 109.511 no C611 . H6113 . O611 . 155.766 no