Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name _publ_author_address _publ_author_footnote 'C. E. Housecroft' ; ? # Address for author 1 ; ; ? # Footnote for author 1 ; 'Hoi Shan Chow' ; ? # Address 2 ; ; ? # Footnote 2 ; 'E. Constable' '' '' 'Markus Neuburger' '' '' 'Sylvia Schaffner' '' '' _publ_contact_author_name 'C. E. Housecroft' _publ_contact_author_address ; Departement Chemie University of Basel Spitalstrasse 51 Basel CH-4056 SWITZERLAND ; _publ_contact_author_email CATHERINE.HOUSECROFT@UNIBAS.CH _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Ligands and complexes with supramolecular aromatic-aromatic interactions: iron(II) and ruthenium(II) complexes of 2,2':6',2"-terpyridines with pendant naphthalene groups ; _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. ; _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_name_full ? _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' # Attachment 'Fe(I)2.cif' data_hsc72_173k _database_code_depnum_ccdc_archive 'CCDC 288503' _audit_creation_date 05-10-26 _audit_creation_method CRYSTALS_ver_12.24 _oxford_structure_analysis_title '9041551 hsc72_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 12.640(2) _cell_length_b 13.617(3) _cell_length_c 14.744(2) _cell_angle_alpha 85.194(13) _cell_angle_beta 85.942(11) _cell_angle_gamma 76.607(13) _cell_volume 2456.6(7) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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 57.7997 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3010 0.8450 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' P 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0140 0.0100 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' _cell_formula_units_Z 2 _chemical_formula_sum 'C54 H41 F12 Fe N7 O2 P2' _chemical_formula_moiety 'C52 H38 Fe N6 O2, 2(F6 P), C2 H3 N' _chemical_compound_source ? _chemical_formula_weight 1165.74 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_max 0.41 _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1188 _exptl_absorpt_coefficient_mu 0.470 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 0.91 # Sheldrick geometric definitions 0.91 0.91 _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 126877 _reflns_number_total 17732 _diffrn_reflns_av_R_equivalents 0.079 # Number of reflections with Friedels Law is 17732 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 17783 _diffrn_reflns_theta_min 3.081 _diffrn_reflns_theta_max 32.499 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 32.499 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -18 _reflns_limit_h_max 19 _reflns_limit_k_min -20 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _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 0.44 _refine_ls_number_reflns 11383 _refine_ls_number_restraints 0 _refine_ls_number_parameters 703 #_refine_ls_R_factor_ref 0.0342 _refine_ls_wR_factor_ref 0.0373 _refine_ls_goodness_of_fit_ref 1.0914 #_reflns_number_all 17664 _refine_ls_R_factor_all 0.0652 _refine_ls_wR_factor_all 0.0547 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 11383 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_gt 0.0373 _refine_ls_shift/su_max 0.015076 # 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: 2.19 -0.274 1.57 ; 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 0.289311(15) 0.185991(15) 0.248185(12) 0.0138 1.0000 Uani . . . . . . N1 N 0.36336(9) 0.06842(9) 0.32679(8) 0.0167 1.0000 Uani . . . . . . N2 N 0.19839(9) 0.20671(9) 0.35525(7) 0.0159 1.0000 Uani . . . . . . N3 N 0.18054(9) 0.30637(9) 0.20482(7) 0.0167 1.0000 Uani . . . . . . N4 N 0.21455(9) 0.10314(9) 0.18329(7) 0.0162 1.0000 Uani . . . . . . N5 N 0.38104(9) 0.16999(8) 0.14166(7) 0.0151 1.0000 Uani . . . . . . N6 N 0.39159(9) 0.26913(9) 0.27457(7) 0.0172 1.0000 Uani . . . . . . N7 N 0.3206(3) 0.3875(2) -0.08450(16) 0.0883 1.0000 Uani . . . . . . C1 C 0.44931(11) -0.00462(11) 0.30386(10) 0.0211 1.0000 Uani . . . . . . C2 C 0.49390(12) -0.08413(11) 0.36426(11) 0.0233 1.0000 Uani . . . . . . C3 C 0.44833(12) -0.08929(11) 0.45193(10) 0.0221 1.0000 Uani . . . . . . C4 C 0.35927(11) -0.01451(11) 0.47713(9) 0.0190 1.0000 Uani . . . . . . C5 C 0.31886(10) 0.06293(10) 0.41354(9) 0.0158 1.0000 Uani . . . . . . C6 C 0.22375(10) 0.14536(10) 0.43081(8) 0.0157 1.0000 Uani . . . . . . C7 C 0.16498(11) 0.16340(11) 0.51244(9) 0.0179 1.0000 Uani . . . . . . C8 C 0.07738(11) 0.24712(11) 0.51536(9) 0.0175 1.0000 Uani . . . . . . C9 C 0.04862(11) 0.30903(11) 0.43634(9) 0.0181 1.0000 Uani . . . . . . C10 C 0.11269(10) 0.28583(10) 0.35725(8) 0.0162 1.0000 Uani . . . . . . C11 C 0.09896(11) 0.34126(10) 0.26739(9) 0.0168 1.0000 Uani . . . . . . C12 C 0.01160(12) 0.41975(12) 0.24570(10) 0.0231 1.0000 Uani . . . . . . C13 C 0.00678(13) 0.46385(12) 0.15766(11) 0.0265 1.0000 Uani . . . . . . C14 C 0.08976(13) 0.42929(12) 0.09434(10) 0.0247 1.0000 Uani . . . . . . C15 C 0.17530(12) 0.35115(11) 0.12022(9) 0.0205 1.0000 Uani . . . . . . C16 C 0.11989(11) 0.07729(11) 0.20867(10) 0.0209 1.0000 Uani . . . . . . C17 C 0.07114(12) 0.02334(13) 0.15506(11) 0.0260 1.0000 Uani . . . . . . C18 C 0.12211(13) -0.00669(13) 0.07256(11) 0.0259 1.0000 Uani . . . . . . C19 C 0.21928(12) 0.01968(11) 0.04484(10) 0.0213 1.0000 Uani . . . . . . C20 C 0.26224(11) 0.07562(10) 0.10076(9) 0.0166 1.0000 Uani . . . . . . C21 C 0.35907(10) 0.11623(10) 0.07544(8) 0.0153 1.0000 Uani . . . . . . C22 C 0.41743(11) 0.11098(10) -0.00717(9) 0.0172 1.0000 Uani . . . . . . C23 C 0.50011(11) 0.16436(10) -0.02199(9) 0.0176 1.0000 Uani . . . . . . C24 C 0.52466(11) 0.21746(11) 0.04731(9) 0.0187 1.0000 Uani . . . . . . C25 C 0.46208(10) 0.21923(10) 0.12846(8) 0.0159 1.0000 Uani . . . . . . C26 C 0.46860(11) 0.27686(10) 0.20666(9) 0.0172 1.0000 Uani . . . . . . C27 C 0.54306(13) 0.33619(13) 0.21136(10) 0.0254 1.0000 Uani . . . . . . C28 C 0.53890(14) 0.39053(13) 0.28728(11) 0.0285 1.0000 Uani . . . . . . C29 C 0.46105(13) 0.38267(13) 0.35656(11) 0.0270 1.0000 Uani . . . . . . C30 C 0.38947(12) 0.32154(11) 0.34809(9) 0.0216 1.0000 Uani . . . . . . C31 C -0.06289(11) 0.34797(11) 0.60476(9) 0.0192 1.0000 Uani . . . . . . C32 C -0.10439(11) 0.35339(11) 0.70241(9) 0.0187 1.0000 Uani . . . . . . C33 C -0.05218(12) 0.29372(11) 0.77227(9) 0.0210 1.0000 Uani . . . . . . C34 C -0.09478(13) 0.30412(11) 0.86360(10) 0.0218 1.0000 Uani . . . . . . C35 C -0.04096(15) 0.24523(14) 0.93738(11) 0.0309 1.0000 Uani . . . . . . C36 C -0.08231(18) 0.25869(16) 1.02527(12) 0.0376 1.0000 Uani . . . . . . C37 C -0.17873(17) 0.33053(16) 1.04307(11) 0.0371 1.0000 Uani . . . . . . C38 C -0.23282(15) 0.38774(14) 0.97361(11) 0.0316 1.0000 Uani . . . . . . C39 C -0.19244(13) 0.37623(12) 0.88175(10) 0.0239 1.0000 Uani . . . . . . C40 C -0.24503(13) 0.43616(13) 0.80814(11) 0.0261 1.0000 Uani . . . . . . C41 C -0.20223(12) 0.42536(12) 0.72096(10) 0.0238 1.0000 Uani . . . . . . C42 C 0.62084(13) 0.23066(12) -0.12897(10) 0.0233 1.0000 Uani . . . . . . C43 C 0.64359(12) 0.23608(11) -0.23003(9) 0.0200 1.0000 Uani . . . . . . C44 C 0.57167(12) 0.30526(12) -0.28647(11) 0.0237 1.0000 Uani . . . . . . C45 C 0.59354(12) 0.31375(12) -0.37836(10) 0.0238 1.0000 Uani . . . . . . C46 C 0.68743(11) 0.25200(11) -0.41899(9) 0.0193 1.0000 Uani . . . . . . C47 C 0.71124(14) 0.25762(13) -0.51453(10) 0.0257 1.0000 Uani . . . . . . C48 C 0.80054(15) 0.19520(14) -0.55224(11) 0.0302 1.0000 Uani . . . . . . C49 C 0.87143(14) 0.12506(13) -0.49671(11) 0.0300 1.0000 Uani . . . . . . C50 C 0.85217(13) 0.11868(12) -0.40406(11) 0.0251 1.0000 Uani . . . . . . C51 C 0.75907(11) 0.18111(10) -0.36318(9) 0.0185 1.0000 Uani . . . . . . C52 C 0.73509(11) 0.17593(11) -0.26770(9) 0.0196 1.0000 Uani . . . . . . C53 C 0.2666(3) 0.2622(2) -0.1825(2) 0.0702 1.0000 Uani . . . . . . C54 C 0.2949(2) 0.33331(18) -0.12791(15) 0.0511 1.0000 Uani . . . . . . O1 O 0.02553(8) 0.26157(8) 0.59731(6) 0.0207 1.0000 Uani . . . . . . O2 O 0.54842(9) 0.16231(8) -0.10651(7) 0.0231 1.0000 Uani . . . . . . P1 P 0.26291(3) 0.44483(3) 0.58930(3) 0.0226 1.0000 Uani . . . . . . P2 P 0.75309(3) 0.02707(3) 0.22680(3) 0.0249 1.0000 Uani . . . . . . F1 F 0.36498(9) 0.48655(9) 0.54567(8) 0.0395 1.0000 Uani . . . . . . F2 F 0.16126(9) 0.40435(9) 0.63412(9) 0.0418 1.0000 Uani . . . . . . F3 F 0.31118(11) 0.43779(10) 0.68678(8) 0.0429 1.0000 Uani . . . . . . F4 F 0.21640(12) 0.45196(11) 0.49072(8) 0.0524 1.0000 Uani . . . . . . F5 F 0.19808(9) 0.55802(8) 0.60323(9) 0.0403 1.0000 Uani . . . . . . F6 F 0.32777(10) 0.33199(8) 0.57394(9) 0.0437 1.0000 Uani . . . . . . F7 F 0.73228(11) -0.06570(11) 0.29307(8) 0.0506 1.0000 Uani . . . . . . F8 F 0.77282(15) 0.11747(12) 0.15933(12) 0.0679 1.0000 Uani . . . . . . F9 F 0.65773(8) 0.01335(10) 0.16590(7) 0.0363 1.0000 Uani . . . . . . F10 F 0.84885(10) 0.03732(14) 0.28720(10) 0.0586 1.0000 Uani . . . . . . F11 F 0.83883(9) -0.04948(10) 0.16610(8) 0.0399 1.0000 Uani . . . . . . F12 F 0.66633(11) 0.10116(12) 0.28724(10) 0.0542 1.0000 Uani . . . . . . H531 H 0.3284 0.2348 -0.2218 0.0859 1.0000 Uiso R . . . . . H532 H 0.2072 0.2967 -0.2188 0.0859 1.0000 Uiso R . . . . . H533 H 0.2454 0.2085 -0.1444 0.0859 1.0000 Uiso R . . . . . H11 H 0.4814 -0.0016 0.2430 0.0251 1.0000 Uiso R . . . . . H21 H 0.5557 -0.1353 0.3455 0.0279 1.0000 Uiso R . . . . . H31 H 0.4780 -0.1440 0.4948 0.0266 1.0000 Uiso R . . . . . H41 H 0.3261 -0.0164 0.5377 0.0232 1.0000 Uiso R . . . . . H71 H 0.1839 0.1194 0.5661 0.0211 1.0000 Uiso R . . . . . H91 H -0.0131 0.3654 0.4369 0.0213 1.0000 Uiso R . . . . . H121 H -0.0449 0.4431 0.2911 0.0261 1.0000 Uiso R . . . . . H131 H -0.0535 0.5180 0.1409 0.0301 1.0000 Uiso R . . . . . H141 H 0.0881 0.4591 0.0330 0.0290 1.0000 Uiso R . . . . . H151 H 0.2334 0.3281 0.0761 0.0243 1.0000 Uiso R . . . . . H161 H 0.0845 0.0971 0.2662 0.0249 1.0000 Uiso R . . . . . H171 H 0.0030 0.0069 0.1750 0.0315 1.0000 Uiso R . . . . . H181 H 0.0902 -0.0450 0.0349 0.0327 1.0000 Uiso R . . . . . H191 H 0.2564 -0.0007 -0.0120 0.0267 1.0000 Uiso R . . . . . H221 H 0.4018 0.0717 -0.0535 0.0208 1.0000 Uiso R . . . . . H241 H 0.5831 0.2521 0.0391 0.0228 1.0000 Uiso R . . . . . H271 H 0.5969 0.3394 0.1626 0.0322 1.0000 Uiso R . . . . . H281 H 0.5889 0.4331 0.2916 0.0362 1.0000 Uiso R . . . . . H291 H 0.4568 0.4191 0.4102 0.0330 1.0000 Uiso R . . . . . H301 H 0.3360 0.3163 0.3967 0.0260 1.0000 Uiso R . . . . . H311 H -0.0381 0.4082 0.5849 0.0225 1.0000 Uiso R . . . . . H312 H -0.1202 0.3422 0.5675 0.0225 1.0000 Uiso R . . . . . H331 H 0.0138 0.2444 0.7595 0.0253 1.0000 Uiso R . . . . . H351 H 0.0252 0.1957 0.9259 0.0377 1.0000 Uiso R . . . . . H361 H -0.0446 0.2184 1.0748 0.0454 1.0000 Uiso R . . . . . H371 H -0.2070 0.3392 1.1048 0.0467 1.0000 Uiso R . . . . . H381 H -0.2990 0.4367 0.9866 0.0388 1.0000 Uiso R . . . . . H401 H -0.3116 0.4853 0.8194 0.0310 1.0000 Uiso R . . . . . H411 H -0.2389 0.4670 0.6716 0.0283 1.0000 Uiso R . . . . . H421 H 0.6877 0.2057 -0.0988 0.0295 1.0000 Uiso R . . . . . H422 H 0.5866 0.2968 -0.1099 0.0295 1.0000 Uiso R . . . . . H441 H 0.5066 0.3465 -0.2601 0.0278 1.0000 Uiso R . . . . . H451 H 0.5449 0.3626 -0.4158 0.0283 1.0000 Uiso R . . . . . H471 H 0.6640 0.3064 -0.5530 0.0320 1.0000 Uiso R . . . . . H481 H 0.8148 0.1990 -0.6171 0.0380 1.0000 Uiso R . . . . . H491 H 0.9341 0.0810 -0.5238 0.0353 1.0000 Uiso R . . . . . H501 H 0.9023 0.0715 -0.3666 0.0296 1.0000 Uiso R . . . . . H521 H 0.7841 0.1293 -0.2289 0.0233 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 Fe1 0.01329(8) 0.01695(8) 0.01085(7) -0.00093(6) 0.00208(6) -0.00338(6) N1 0.0145(5) 0.0194(5) 0.0162(5) -0.0019(4) 0.0015(4) -0.0045(4) N2 0.0156(5) 0.0189(5) 0.0124(4) 0.0003(4) 0.0011(4) -0.0036(4) N3 0.0180(5) 0.0192(5) 0.0127(4) -0.0005(4) 0.0020(4) -0.0050(4) N4 0.0145(5) 0.0183(5) 0.0152(5) 0.0013(4) 0.0015(4) -0.0041(4) N5 0.0149(5) 0.0175(5) 0.0134(4) -0.0025(4) 0.0010(4) -0.0044(4) N6 0.0173(5) 0.0207(5) 0.0134(4) -0.0025(4) 0.0004(4) -0.0036(4) N7 0.155(3) 0.0556(14) 0.0397(12) -0.0112(11) -0.0019(15) 0.0069(17) C1 0.0166(6) 0.0223(6) 0.0234(6) -0.0037(5) 0.0039(5) -0.0033(5) C2 0.0165(6) 0.0210(6) 0.0313(7) -0.0028(5) 0.0004(5) -0.0019(5) C3 0.0201(6) 0.0186(6) 0.0275(7) 0.0019(5) -0.0058(5) -0.0040(5) C4 0.0189(6) 0.0206(6) 0.0181(6) 0.0009(5) -0.0029(4) -0.0059(5) C5 0.0150(5) 0.0178(5) 0.0143(5) -0.0006(4) -0.0002(4) -0.0037(4) C6 0.0150(5) 0.0184(5) 0.0134(5) 0.0005(4) 0.0001(4) -0.0036(4) C7 0.0186(6) 0.0218(6) 0.0122(5) 0.0002(4) 0.0019(4) -0.0036(5) C8 0.0170(5) 0.0228(6) 0.0132(5) -0.0025(4) 0.0030(4) -0.0059(5) C9 0.0165(5) 0.0218(6) 0.0144(5) -0.0013(4) 0.0033(4) -0.0021(5) C10 0.0157(5) 0.0193(6) 0.0125(5) 0.0006(4) 0.0020(4) -0.0034(4) C11 0.0168(5) 0.0190(6) 0.0138(5) 0.0000(4) 0.0012(4) -0.0037(4) C12 0.0211(6) 0.0245(7) 0.0201(6) 0.0016(5) 0.0015(5) 0.0002(5) C13 0.0252(7) 0.0256(7) 0.0239(7) 0.0048(5) -0.0033(5) 0.0021(6) C14 0.0281(7) 0.0280(7) 0.0165(6) 0.0055(5) -0.0029(5) -0.0055(6) C15 0.0232(6) 0.0235(6) 0.0140(5) 0.0012(5) 0.0014(5) -0.0055(5) C16 0.0147(5) 0.0241(6) 0.0230(6) 0.0021(5) 0.0026(5) -0.0048(5) C17 0.0179(6) 0.0307(7) 0.0314(7) 0.0031(6) -0.0025(5) -0.0112(6) C18 0.0258(7) 0.0308(7) 0.0255(7) 0.0011(6) -0.0070(5) -0.0147(6) C19 0.0238(6) 0.0247(6) 0.0179(6) -0.0012(5) -0.0023(5) -0.0106(5) C20 0.0166(5) 0.0198(6) 0.0138(5) 0.0000(4) 0.0005(4) -0.0057(4) C21 0.0158(5) 0.0167(5) 0.0133(5) -0.0004(4) 0.0013(4) -0.0043(4) C22 0.0200(6) 0.0185(6) 0.0137(5) -0.0032(4) 0.0020(4) -0.0057(5) C23 0.0188(6) 0.0198(6) 0.0139(5) -0.0022(4) 0.0045(4) -0.0046(5) C24 0.0183(6) 0.0233(6) 0.0160(5) -0.0029(5) 0.0042(4) -0.0086(5) C25 0.0154(5) 0.0191(6) 0.0136(5) -0.0015(4) 0.0011(4) -0.0052(4) C26 0.0166(5) 0.0215(6) 0.0143(5) -0.0028(4) 0.0009(4) -0.0058(5) C27 0.0244(7) 0.0338(8) 0.0223(6) -0.0060(6) 0.0025(5) -0.0151(6) C28 0.0296(8) 0.0354(8) 0.0262(7) -0.0087(6) -0.0028(6) -0.0162(6) C29 0.0289(7) 0.0323(8) 0.0224(7) -0.0098(6) -0.0030(5) -0.0087(6) C30 0.0219(6) 0.0265(7) 0.0163(6) -0.0060(5) 0.0005(5) -0.0045(5) C31 0.0174(6) 0.0242(6) 0.0146(5) -0.0022(5) 0.0035(4) -0.0029(5) C32 0.0182(6) 0.0223(6) 0.0163(5) -0.0039(5) 0.0041(4) -0.0064(5) C33 0.0211(6) 0.0238(6) 0.0178(6) -0.0041(5) 0.0033(5) -0.0048(5) C34 0.0272(7) 0.0224(6) 0.0175(6) -0.0031(5) 0.0027(5) -0.0094(5) C35 0.0390(9) 0.0312(8) 0.0220(7) -0.0002(6) -0.0001(6) -0.0077(7) C36 0.0527(11) 0.0414(10) 0.0198(7) 0.0023(6) -0.0010(7) -0.0147(9) C37 0.0498(11) 0.0470(10) 0.0193(7) -0.0075(7) 0.0092(7) -0.0223(9) C38 0.0356(8) 0.0367(9) 0.0249(7) -0.0119(6) 0.0133(6) -0.0142(7) C39 0.0270(7) 0.0267(7) 0.0205(6) -0.0076(5) 0.0076(5) -0.0117(6) C40 0.0227(7) 0.0288(7) 0.0256(7) -0.0086(6) 0.0068(5) -0.0036(6) C41 0.0218(6) 0.0267(7) 0.0220(6) -0.0041(5) 0.0035(5) -0.0041(5) C42 0.0277(7) 0.0278(7) 0.0174(6) -0.0034(5) 0.0082(5) -0.0141(6) C43 0.0218(6) 0.0230(6) 0.0166(5) -0.0018(5) 0.0041(5) -0.0098(5) C44 0.0187(6) 0.0243(7) 0.0266(7) -0.0035(5) 0.0044(5) -0.0032(5) C45 0.0210(6) 0.0246(7) 0.0247(7) 0.0019(5) -0.0024(5) -0.0036(5) C46 0.0209(6) 0.0223(6) 0.0162(5) -0.0003(5) 0.0002(4) -0.0084(5) C47 0.0319(7) 0.0300(7) 0.0171(6) 0.0018(5) -0.0022(5) -0.0118(6) C48 0.0414(9) 0.0360(8) 0.0175(6) -0.0047(6) 0.0058(6) -0.0187(7) C49 0.0322(8) 0.0301(8) 0.0275(7) -0.0080(6) 0.0124(6) -0.0088(6) C50 0.0240(7) 0.0254(7) 0.0240(7) -0.0014(5) 0.0044(5) -0.0037(5) C51 0.0195(6) 0.0200(6) 0.0166(5) -0.0008(4) 0.0028(4) -0.0068(5) C52 0.0211(6) 0.0208(6) 0.0165(5) 0.0016(5) 0.0017(5) -0.0057(5) C53 0.080(2) 0.0641(17) 0.0740(19) 0.0315(15) -0.0277(16) -0.0381(16) C54 0.0610(14) 0.0444(11) 0.0338(10) 0.0090(9) 0.0116(9) 0.0081(10) O1 0.0206(5) 0.0258(5) 0.0128(4) -0.0014(4) 0.0053(3) -0.0013(4) O2 0.0294(5) 0.0279(5) 0.0151(4) -0.0062(4) 0.0102(4) -0.0149(4) P1 0.02000(16) 0.02466(18) 0.02247(17) -0.00229(14) -0.00108(13) -0.00343(13) P2 0.02093(17) 0.0359(2) 0.01893(16) -0.00641(15) 0.00112(13) -0.00791(15) F1 0.0302(5) 0.0378(6) 0.0475(6) -0.0012(5) 0.0154(5) -0.0074(4) F2 0.0301(5) 0.0446(6) 0.0558(7) -0.0053(5) 0.0032(5) -0.0200(5) F3 0.0531(7) 0.0540(7) 0.0297(5) 0.0040(5) -0.0150(5) -0.0271(6) F4 0.0598(8) 0.0627(8) 0.0325(6) -0.0034(6) -0.0201(6) -0.0040(7) F5 0.0325(5) 0.0282(5) 0.0544(7) -0.0053(5) 0.0124(5) 0.0011(4) F6 0.0432(6) 0.0265(5) 0.0584(8) -0.0078(5) -0.0025(6) -0.0004(5) F7 0.0503(7) 0.0636(8) 0.0341(6) 0.0187(6) -0.0013(5) -0.0134(6) F8 0.0796(11) 0.0529(8) 0.0759(11) 0.0159(8) 0.0089(9) -0.0359(8) F9 0.0251(5) 0.0607(7) 0.0241(5) -0.0058(5) -0.0039(4) -0.0103(5) F10 0.0317(6) 0.1017(12) 0.0501(7) -0.0425(8) -0.0041(5) -0.0173(7) F11 0.0250(5) 0.0599(7) 0.0356(6) -0.0229(5) 0.0045(4) -0.0059(5) F12 0.0387(6) 0.0681(9) 0.0537(8) -0.0345(7) 0.0052(6) 0.0004(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.9968(8) 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 . 1.9826(12) yes Fe1 . N2 . 1.8868(11) yes Fe1 . N3 . 1.9725(12) yes Fe1 . N4 . 1.9708(12) yes Fe1 . N5 . 1.8818(11) yes Fe1 . N6 . 1.9817(12) yes N1 . C1 . 1.3370(18) yes N1 . C5 . 1.3638(16) yes N2 . C6 . 1.3462(17) yes N2 . C10 . 1.3398(17) yes N3 . C11 . 1.3609(16) yes N3 . C15 . 1.3407(17) yes N4 . C16 . 1.3436(17) yes N4 . C20 . 1.3611(16) yes N5 . C21 . 1.3485(17) yes N5 . C25 . 1.3435(16) yes N6 . C26 . 1.3613(16) yes N6 . C30 . 1.3422(17) yes N7 . C54 . 1.132(4) yes C1 . C2 . 1.382(2) yes C1 . H11 . 0.960 no C2 . C3 . 1.381(2) yes C2 . H21 . 0.960 no C3 . C4 . 1.384(2) yes C3 . H31 . 0.960 no C4 . C5 . 1.3800(19) yes C4 . H41 . 0.960 no C5 . C6 . 1.4661(18) yes C6 . C7 . 1.3782(17) yes C7 . C8 . 1.3944(19) yes C7 . H71 . 0.960 no C8 . C9 . 1.3978(19) yes C8 . O1 . 1.3402(15) yes C9 . C10 . 1.3874(17) yes C9 . H91 . 0.960 no C10 . C11 . 1.4695(18) yes C11 . C12 . 1.3821(19) yes C12 . C13 . 1.383(2) yes C12 . H121 . 0.960 no C13 . C14 . 1.378(2) yes C13 . H131 . 0.960 no C14 . C15 . 1.380(2) yes C14 . H141 . 0.960 no C15 . H151 . 0.960 no C16 . C17 . 1.386(2) yes C16 . H161 . 0.960 no C17 . C18 . 1.383(2) yes C17 . H171 . 0.960 no C18 . C19 . 1.383(2) yes C18 . H181 . 0.960 no C19 . C20 . 1.3838(19) yes C19 . H191 . 0.960 no C20 . C21 . 1.4689(18) yes C21 . C22 . 1.3768(17) yes C22 . C23 . 1.4005(19) yes C22 . H221 . 0.960 no C23 . C24 . 1.3912(19) yes C23 . O2 . 1.3479(15) yes C24 . C25 . 1.3857(17) yes C24 . H241 . 0.960 no C25 . C26 . 1.4653(18) yes C26 . C27 . 1.3835(19) yes C27 . C28 . 1.384(2) yes C27 . H271 . 0.960 no C28 . C29 . 1.382(2) yes C28 . H281 . 0.960 no C29 . C30 . 1.382(2) yes C29 . H291 . 0.960 no C30 . H301 . 0.960 no C31 . C32 . 1.4988(18) yes C31 . O1 . 1.4284(17) yes C31 . H311 . 0.960 no C31 . H312 . 0.960 no C32 . C33 . 1.365(2) yes C32 . C41 . 1.414(2) yes C33 . C34 . 1.4203(19) yes C33 . H331 . 0.960 no C34 . C35 . 1.412(2) yes C34 . C39 . 1.413(2) yes C35 . C36 . 1.373(2) yes C35 . H351 . 0.960 no C36 . C37 . 1.399(3) yes C36 . H361 . 0.960 no C37 . C38 . 1.357(3) yes C37 . H371 . 0.960 no C38 . C39 . 1.421(2) yes C38 . H381 . 0.960 no C39 . C40 . 1.410(2) yes C40 . C41 . 1.365(2) yes C40 . H401 . 0.960 no C41 . H411 . 0.960 no C42 . C43 . 1.4965(19) yes C42 . O2 . 1.4540(17) yes C42 . H421 . 0.960 no C42 . H422 . 0.960 no C43 . C44 . 1.409(2) yes C43 . C52 . 1.365(2) yes C44 . C45 . 1.364(2) yes C44 . H441 . 0.960 no C45 . C46 . 1.413(2) yes C45 . H451 . 0.960 no C46 . C47 . 1.4189(19) yes C46 . C51 . 1.413(2) yes C47 . C48 . 1.361(2) yes C47 . H471 . 0.960 no C48 . C49 . 1.401(3) yes C48 . H481 . 0.960 no C49 . C50 . 1.370(2) yes C49 . H491 . 0.960 no C50 . C51 . 1.412(2) yes C50 . H501 . 0.960 no C51 . C52 . 1.4183(18) yes C52 . H521 . 0.960 no C53 . C54 . 1.430(4) yes C53 . H531 . 0.960 no C53 . H532 . 0.960 no C53 . H533 . 0.960 no P1 . F1 . 1.6005(12) yes P1 . F2 . 1.5933(12) yes P1 . F3 . 1.5878(12) yes P1 . F4 . 1.5934(12) yes P1 . F5 . 1.5917(12) yes P1 . F6 . 1.5915(12) yes P2 . F7 . 1.5908(14) yes P2 . F8 . 1.5712(15) yes P2 . F9 . 1.6062(11) yes P2 . F10 . 1.5904(12) yes P2 . F11 . 1.5994(11) yes P2 . F12 . 1.5857(13) yes 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 . 80.53(5) yes N1 . Fe1 . N3 . 160.98(5) yes N2 . Fe1 . N3 . 80.61(5) yes N1 . Fe1 . N4 . 92.99(5) yes N2 . Fe1 . N4 . 100.91(5) yes N3 . Fe1 . N4 . 88.13(5) yes N1 . Fe1 . N5 . 100.54(5) yes N2 . Fe1 . N5 . 177.92(5) yes N3 . Fe1 . N5 . 98.38(5) yes N4 . Fe1 . N5 . 80.84(5) yes N1 . Fe1 . N6 . 92.85(5) yes N2 . Fe1 . N6 . 97.64(5) yes N3 . Fe1 . N6 . 92.11(5) yes N4 . Fe1 . N6 . 161.23(5) yes N5 . Fe1 . N6 . 80.55(5) yes Fe1 . N1 . C1 . 127.52(10) yes Fe1 . N1 . C5 . 114.65(9) yes C1 . N1 . C5 . 117.82(12) yes Fe1 . N2 . C6 . 119.71(9) yes Fe1 . N2 . C10 . 119.84(9) yes C6 . N2 . C10 . 120.34(11) yes Fe1 . N3 . C11 . 114.70(9) yes Fe1 . N3 . C15 . 126.93(10) yes C11 . N3 . C15 . 118.18(12) yes Fe1 . N4 . C16 . 127.40(10) yes Fe1 . N4 . C20 . 114.86(9) yes C16 . N4 . C20 . 117.58(12) yes Fe1 . N5 . C21 . 119.60(9) yes Fe1 . N5 . C25 . 119.92(9) yes C21 . N5 . C25 . 120.22(11) yes Fe1 . N6 . C26 . 114.50(9) yes Fe1 . N6 . C30 . 127.69(10) yes C26 . N6 . C30 . 117.71(12) yes N1 . C1 . C2 . 122.67(13) yes N1 . C1 . H11 . 118.616 no C2 . C1 . H11 . 118.716 no C1 . C2 . C3 . 119.20(13) yes C1 . C2 . H21 . 120.432 no C3 . C2 . H21 . 120.368 no C2 . C3 . C4 . 119.11(13) yes C2 . C3 . H31 . 120.434 no C4 . C3 . H31 . 120.456 no C3 . C4 . C5 . 118.77(13) yes C3 . C4 . H41 . 120.704 no C5 . C4 . H41 . 120.530 no C4 . C5 . N1 . 122.43(12) yes C4 . C5 . C6 . 124.21(12) yes N1 . C5 . C6 . 113.35(11) yes C5 . C6 . N2 . 111.57(11) yes C5 . C6 . C7 . 127.02(12) yes N2 . C6 . C7 . 121.41(12) yes C6 . C7 . C8 . 118.42(12) yes C6 . C7 . H71 . 120.827 no C8 . C7 . H71 . 120.752 no C7 . C8 . C9 . 120.29(12) yes C7 . C8 . O1 . 115.28(12) yes C9 . C8 . O1 . 124.43(12) yes C8 . C9 . C10 . 117.46(12) yes C8 . C9 . H91 . 121.185 no C10 . C9 . H91 . 121.356 no C9 . C10 . N2 . 122.03(12) yes C9 . C10 . C11 . 126.75(12) yes N2 . C10 . C11 . 111.22(11) yes C10 . C11 . N3 . 113.37(12) yes C10 . C11 . C12 . 124.65(12) yes N3 . C11 . C12 . 121.96(12) yes C11 . C12 . C13 . 118.98(13) yes C11 . C12 . H121 . 120.416 no C13 . C12 . H121 . 120.608 no C12 . C13 . C14 . 119.19(14) yes C12 . C13 . H131 . 120.437 no C14 . C13 . H131 . 120.370 no C13 . C14 . C15 . 119.19(13) yes C13 . C14 . H141 . 120.442 no C15 . C14 . H141 . 120.370 no C14 . C15 . N3 . 122.49(13) yes C14 . C15 . H151 . 118.807 no N3 . C15 . H151 . 118.704 no N4 . C16 . C17 . 122.67(13) yes N4 . C16 . H161 . 118.651 no C17 . C16 . H161 . 118.681 no C16 . C17 . C18 . 119.12(13) yes C16 . C17 . H171 . 120.439 no C18 . C17 . H171 . 120.443 no C17 . C18 . C19 . 119.16(14) yes C17 . C18 . H181 . 120.388 no C19 . C18 . H181 . 120.449 no C18 . C19 . C20 . 118.73(13) yes C18 . C19 . H191 . 120.673 no C20 . C19 . H191 . 120.601 no C19 . C20 . N4 . 122.69(12) yes C19 . C20 . C21 . 123.94(12) yes N4 . C20 . C21 . 113.27(11) yes C20 . C21 . N5 . 111.40(11) yes C20 . C21 . C22 . 126.85(12) yes N5 . C21 . C22 . 121.49(12) yes C21 . C22 . C23 . 118.42(12) yes C21 . C22 . H221 . 120.787 no C23 . C22 . H221 . 120.797 no C22 . C23 . C24 . 119.98(12) yes C22 . C23 . O2 . 115.38(12) yes C24 . C23 . O2 . 124.60(12) yes C23 . C24 . C25 . 118.08(12) yes C23 . C24 . H241 . 120.991 no C25 . C24 . H241 . 120.932 no C24 . C25 . N5 . 121.75(12) yes C24 . C25 . C26 . 126.70(12) yes N5 . C25 . C26 . 111.44(11) yes C25 . C26 . N6 . 113.48(11) yes C25 . C26 . C27 . 124.14(12) yes N6 . C26 . C27 . 122.36(12) yes C26 . C27 . C28 . 119.11(14) yes C26 . C27 . H271 . 120.323 no C28 . C27 . H271 . 120.569 no C27 . C28 . C29 . 118.74(14) yes C27 . C28 . H281 . 120.603 no C29 . C28 . H281 . 120.655 no C28 . C29 . C30 . 119.38(14) yes C28 . C29 . H291 . 120.389 no C30 . C29 . H291 . 120.231 no C29 . C30 . N6 . 122.70(13) yes C29 . C30 . H301 . 118.722 no N6 . C30 . H301 . 118.581 no C32 . C31 . O1 . 108.91(11) yes C32 . C31 . H311 . 109.485 no O1 . C31 . H311 . 109.547 no C32 . C31 . H312 . 109.724 no O1 . C31 . H312 . 109.692 no H311 . C31 . H312 . 109.467 no C31 . C32 . C33 . 123.32(13) yes C31 . C32 . C41 . 116.88(13) yes C33 . C32 . C41 . 119.80(13) yes C32 . C33 . C34 . 120.49(13) yes C32 . C33 . H331 . 119.727 no C34 . C33 . H331 . 119.788 no C33 . C34 . C35 . 121.67(14) yes C33 . C34 . C39 . 119.48(14) yes C35 . C34 . C39 . 118.85(14) yes C34 . C35 . C36 . 120.52(17) yes C34 . C35 . H351 . 119.599 no C36 . C35 . H351 . 119.878 no C35 . C36 . C37 . 120.51(18) yes C35 . C36 . H361 . 119.597 no C37 . C36 . H361 . 119.898 no C36 . C37 . C38 . 120.39(15) yes C36 . C37 . H371 . 119.790 no C38 . C37 . H371 . 119.817 no C37 . C38 . C39 . 120.76(17) yes C37 . C38 . H381 . 119.728 no C39 . C38 . H381 . 119.511 no C38 . C39 . C34 . 118.97(16) yes C38 . C39 . C40 . 122.25(15) yes C34 . C39 . C40 . 118.76(13) yes C39 . C40 . C41 . 120.77(14) yes C39 . C40 . H401 . 119.690 no C41 . C40 . H401 . 119.538 no C32 . C41 . C40 . 120.71(15) yes C32 . C41 . H411 . 119.552 no C40 . C41 . H411 . 119.740 no C43 . C42 . O2 . 108.25(12) yes C43 . C42 . H421 . 109.862 no O2 . C42 . H421 . 109.820 no C43 . C42 . H422 . 109.682 no O2 . C42 . H422 . 109.738 no H421 . C42 . H422 . 109.467 no C42 . C43 . C44 . 119.91(13) yes C42 . C43 . C52 . 120.30(14) yes C44 . C43 . C52 . 119.77(13) yes C43 . C44 . C45 . 120.54(13) yes C43 . C44 . H441 . 119.702 no C45 . C44 . H441 . 119.758 no C44 . C45 . C46 . 120.73(14) yes C44 . C45 . H451 . 119.653 no C46 . C45 . H451 . 119.617 no C45 . C46 . C47 . 122.04(14) yes C45 . C46 . C51 . 119.17(12) yes C47 . C46 . C51 . 118.78(13) yes C46 . C47 . C48 . 120.88(15) yes C46 . C47 . H471 . 119.544 no C48 . C47 . H471 . 119.572 no C47 . C48 . C49 . 120.18(14) yes C47 . C48 . H481 . 119.934 no C49 . C48 . H481 . 119.881 no C48 . C49 . C50 . 120.59(15) yes C48 . C49 . H491 . 119.715 no C50 . C49 . H491 . 119.690 no C49 . C50 . C51 . 120.47(15) yes C49 . C50 . H501 . 119.822 no C51 . C50 . H501 . 119.709 no C46 . C51 . C50 . 119.07(13) yes C46 . C51 . C52 . 118.58(13) yes C50 . C51 . C52 . 122.35(13) yes C51 . C52 . C43 . 121.18(13) yes C51 . C52 . H521 . 119.378 no C43 . C52 . H521 . 119.442 no C54 . C53 . H531 . 108.955 no C54 . C53 . H532 . 108.738 no H531 . C53 . H532 . 109.467 no C54 . C53 . H533 . 110.266 no H531 . C53 . H533 . 109.697 no H532 . C53 . H533 . 109.697 no C53 . C54 . N7 . 177.7(3) yes C31 . O1 . C8 . 117.62(11) yes C42 . O2 . C23 . 116.68(11) yes F1 . P1 . F2 . 179.07(7) yes F1 . P1 . F3 . 89.17(7) yes F2 . P1 . F3 . 90.10(7) yes F1 . P1 . F4 . 89.93(8) yes F2 . P1 . F4 . 90.80(8) yes F3 . P1 . F4 . 179.06(8) yes F1 . P1 . F5 . 89.51(6) yes F2 . P1 . F5 . 89.91(7) yes F3 . P1 . F5 . 90.16(8) yes F4 . P1 . F5 . 90.13(8) yes F1 . P1 . F6 . 90.15(7) yes F2 . P1 . F6 . 90.44(7) yes F3 . P1 . F6 . 90.52(8) yes F4 . P1 . F6 . 89.18(8) yes F5 . P1 . F6 . 179.24(7) yes F7 . P2 . F8 . 178.60(9) yes F7 . P2 . F9 . 88.81(7) yes F8 . P2 . F9 . 90.00(9) yes F7 . P2 . F10 . 90.06(9) yes F8 . P2 . F10 . 91.11(10) yes F9 . P2 . F10 . 178.39(8) yes F7 . P2 . F11 . 89.89(8) yes F8 . P2 . F11 . 89.35(9) yes F9 . P2 . F11 . 89.19(6) yes F10 . P2 . F11 . 89.65(7) yes F7 . P2 . F12 . 89.09(9) yes F8 . P2 . F12 . 91.66(10) yes F9 . P2 . F12 . 89.94(7) yes F10 . P2 . F12 . 91.20(7) yes F11 . P2 . F12 . 178.67(8) yes # Attachment 'Fe(II)2.cif' data_hsc29_173k _database_code_depnum_ccdc_archive 'CCDC 288504' _audit_creation_date 05-10-25 _audit_creation_method CRYSTALS_ver_12.24 _oxford_structure_analysis_title '12011120 hsc29_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 16.897(3) _cell_length_b 32.914(11) _cell_length_c 18.693(11) _cell_angle_alpha 90 _cell_angle_beta 94.84(2) _cell_angle_gamma 90 _cell_volume 10359(7) _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' 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' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 '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' _cell_formula_units_Z 8 _chemical_formula_sum 'C56 H46 F12 Fe N6 O4 P2' _chemical_formula_moiety 'C56 H46 Fe N6 O4, 2(F6 P)' _chemical_compound_source ? _chemical_formula_weight 1212.79 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_max 0.27 _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 4960 _exptl_absorpt_coefficient_mu 0.452 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_absorpt_correction_T_min 0.96 _exptl_absorpt_correction_T_max 0.96 # Sheldrick geometric definitions 0.91 0.96 _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 64205 _reflns_number_total 16197 _diffrn_reflns_av_R_equivalents 0.109 # Number of reflections with Friedels Law is 16197 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 16285 _diffrn_reflns_theta_min 1.237 _diffrn_reflns_theta_max 24.017 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 23.537 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -19 _reflns_limit_h_max 19 _reflns_limit_k_min -37 _reflns_limit_k_max 0 _reflns_limit_l_min -21 _reflns_limit_l_max 0 _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 -0.90 _refine_diff_density_max 1.05 _refine_ls_number_reflns 10772 _refine_ls_number_restraints 352 _refine_ls_number_parameters 1303 #_refine_ls_R_factor_ref 0.1074 _refine_ls_wR_factor_ref 0.0783 _refine_ls_goodness_of_fit_ref 0.9943 #_reflns_number_all 16197 _refine_ls_R_factor_all 0.1629 _refine_ls_wR_factor_all 0.1122 # 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 10772 _refine_ls_R_factor_gt 0.1074 _refine_ls_wR_factor_gt 0.0783 _refine_ls_shift/su_max 0.049002 # 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: 6.21 5.99 5.45 1.02 ; _refine_special_details ; The scattering power of the sample was very low and therefore datacollection could not be carried out to higher diffraction angles. As a consequence we are short of reflections for refinement. In order to improve the data to parameter ratio group refinement was used for peripherical aromatic substituents and for the PF6 molecules. Crystals uses the full variance covariance matrix in order to calculate the esd's. Checkcif does not have access to this information and calculates the standard deviations in a different way and complains about the differences. I would like to underline that the esd's calculated by CRYSTALS are the ones to trust and that the way checkcif is behaving should be questioned. ; _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 0.26216(5) -0.01348(3) -0.22966(4) 0.0276 1.0000 Uani . . . . . . Fe2 Fe 0.05648(5) 0.23447(3) -0.27555(4) 0.0270 1.0000 Uani . . . . . . O1 O 0.3593(3) 0.00106(15) 0.0826(2) 0.0471 1.0000 Uani . . . . . . O2 O 0.3549(4) -0.00123(17) 0.2375(3) 0.0828 1.0000 Uani . . . . . . O11 O 0.1838(3) -0.00716(13) -0.5456(2) 0.0402 1.0000 Uani . . . . . . O12 O 0.1595(3) -0.02218(14) -0.6943(2) 0.0461 1.0000 Uani . . . . . . O21 O 0.1532(2) 0.24910(14) 0.0363(2) 0.0382 1.0000 Uani . . . . . . O22 O 0.2369(3) 0.25020(14) 0.1870(2) 0.0450 1.0000 Uani . . . . . . O31 O -0.0202(3) 0.23167(16) -0.5917(2) 0.0522 1.0000 Uani . . . . . . O32 O -0.1076(4) 0.22603(18) -0.7432(3) 0.0820 1.0000 Uani . . . . . . N1 N 0.3438(3) -0.05638(15) -0.2196(2) 0.0318 1.0000 Uani . . . . . . N2 N 0.2863(3) -0.01088(15) -0.1293(2) 0.0310 1.0000 Uani . . . . . . N3 N 0.1878(3) 0.03022(15) -0.2055(3) 0.0322 1.0000 Uani . . . . . . N4 N 0.3426(3) 0.02538(15) -0.2574(3) 0.0309 1.0000 Uani . . . . . . N5 N 0.2391(3) -0.01378(14) -0.3297(2) 0.0288 1.0000 Uani . . . . . . N6 N 0.1725(3) -0.05223(15) -0.2361(2) 0.0314 1.0000 Uani . . . . . . N7 N 0.1426(3) 0.19385(15) -0.2694(2) 0.0301 1.0000 Uani . . . . . . N8 N 0.0835(3) 0.23606(15) -0.1760(2) 0.0283 1.0000 Uani . . . . . . N9 N -0.0223(3) 0.27469(14) -0.2481(2) 0.0278 1.0000 Uani . . . . . . N10 N 0.1274(3) 0.27832(15) -0.3054(3) 0.0314 1.0000 Uani . . . . . . N11 N 0.0299(3) 0.23341(15) -0.3754(2) 0.0287 1.0000 Uani . . . . . . N12 N -0.0213(3) 0.19024(14) -0.2791(2) 0.0286 1.0000 Uani . . . . . . C1 C 0.3700(4) -0.0799(2) -0.2703(3) 0.0374 1.0000 Uani . . . . . . C2 C 0.4292(4) -0.1077(2) -0.2576(4) 0.0439 1.0000 Uani . . . . . . C3 C 0.4647(4) -0.1116(2) -0.1885(4) 0.0501 1.0000 Uani . . . . . . C4 C 0.4377(4) -0.0888(2) -0.1353(4) 0.0407 1.0000 Uani . . . . . . C5 C 0.3781(3) -0.06144(17) -0.1506(3) 0.0284 1.0000 Uani . . . . . . C6 C 0.3450(4) -0.03413(19) -0.0981(3) 0.0325 1.0000 Uani . . . . . . C7 C 0.3693(4) -0.03017(19) -0.0274(3) 0.0337 1.0000 Uani . . . . . . C8 C 0.3319(4) -0.0019(2) 0.0133(3) 0.0410 1.0000 Uani . . . . . . C9 C 0.2694(4) 0.0216(2) -0.0177(3) 0.0418 1.0000 Uani . . . . . . C10 C 0.2497(4) 0.01614(19) -0.0909(3) 0.0328 1.0000 Uani . . . . . . C11 C 0.1898(4) 0.03961(19) -0.1356(3) 0.0348 1.0000 Uani . . . . . . C12 C 0.1401(4) 0.0683(2) -0.1102(4) 0.0460 1.0000 Uani . . . . . . C13 C 0.0864(5) 0.0878(2) -0.1567(4) 0.0555 1.0000 Uani . . . . . . C14 C 0.0868(4) 0.0792(2) -0.2294(4) 0.0402 1.0000 Uani . . . . . . C15 C 0.1365(4) 0.0506(2) -0.2517(3) 0.0357 1.0000 Uani . . . . . . C16 C 0.3948(4) 0.04619(18) -0.2125(3) 0.0340 1.0000 Uani . . . . . . C17 C 0.4476(4) 0.0736(2) -0.2362(4) 0.0431 1.0000 Uani . . . . . . C18 C 0.4470(4) 0.0806(2) -0.3095(4) 0.0502 1.0000 Uani . . . . . . C19 C 0.3938(4) 0.0600(2) -0.3559(4) 0.0401 1.0000 Uani . . . . . . C20 C 0.3427(3) 0.03279(18) -0.3282(3) 0.0322 1.0000 Uani . . . . . . C21 C 0.2825(3) 0.00935(18) -0.3710(3) 0.0310 1.0000 Uani . . . . . . C22 C 0.2654(4) 0.01117(19) -0.4448(3) 0.0320 1.0000 Uani . . . . . . C23 C 0.2004(4) -0.01121(19) -0.4748(3) 0.0321 1.0000 Uani . . . . . . C24 C 0.1569(3) -0.03474(18) -0.4318(3) 0.0305 1.0000 Uani . . . . . . C25 C 0.1778(3) -0.03563(18) -0.3587(3) 0.0309 1.0000 Uani . . . . . . C26 C 0.1382(3) -0.05765(19) -0.3046(3) 0.0320 1.0000 Uani . . . . . . C27 C 0.0703(4) -0.0805(2) -0.3169(3) 0.0433 1.0000 Uani . . . . . . C28 C 0.0387(4) -0.0988(3) -0.2604(4) 0.0532 1.0000 Uani . . . . . . C29 C 0.0745(4) -0.0945(2) -0.1923(3) 0.0478 1.0000 Uani . . . . . . C30 C 0.1408(4) -0.0718(2) -0.1819(3) 0.0349 1.0000 Uani . . . . . . C31 C 0.4575(2) 0.04995(12) 0.3895(2) 0.0771 1.0000 Uani DG U . . . . C32 C 0.3957(3) 0.02916(12) 0.3536(2) 0.0618 1.0000 Uani DG U . . . . C33 C 0.3193(3) 0.04217(13) 0.3648(2) 0.0673 1.0000 Uani DG U . . . . C34 C 0.2990(2) 0.07388(14) 0.4078(2) 0.0691 1.0000 Uani DG U . . . . C35 C 0.3461(3) 0.12623(12) 0.4930(2) 0.0673 1.0000 Uani DG U . . . . C36 C 0.4116(3) 0.14390(11) 0.52895(19) 0.0703 1.0000 Uani DG U . . . . C37 C 0.4885(3) 0.13222(14) 0.5222(2) 0.0895 1.0000 Uani DG U . . . . C38 C 0.5038(2) 0.10140(14) 0.4772(2) 0.0855 1.0000 Uani DG U . . . . C39 C 0.44219(19) 0.08194(10) 0.43924(16) 0.0494 1.0000 Uani DG U . . . . C40 C 0.3618(2) 0.09368(10) 0.44462(15) 0.0567 1.0000 Uani DG U . . . . C41 C 0.1486(2) 0.05050(9) -0.78283(15) 0.0470 1.0000 Uani DG U . . . . C42 C 0.1209(2) 0.01357(8) -0.80835(18) 0.0443 1.0000 Uani DG U . . . . C43 C 0.0799(2) 0.01074(8) -0.87599(19) 0.0505 1.0000 Uani DG U . . . . C44 C 0.0677(2) 0.04498(9) -0.91794(15) 0.0533 1.0000 Uani DG U . . . . C45 C 0.0780(2) 0.11824(10) -0.93336(18) 0.0559 1.0000 Uani DG U . . . . C46 C 0.1022(3) 0.15571(9) -0.9069(2) 0.0716 1.0000 Uani DG U . . . . C47 C 0.1431(3) 0.15801(8) -0.8390(2) 0.0693 1.0000 Uani DG U . . . . C48 C 0.1604(2) 0.12365(9) -0.79791(19) 0.0596 1.0000 Uani DG U . . . . C49 C 0.13528(16) 0.08566(8) -0.82469(13) 0.0475 1.0000 Uani DG U . . . . C50 C 0.09492(17) 0.08285(8) -0.89308(13) 0.0473 1.0000 Uani DG U . . . . C51 C 0.3260(5) 0.0306(2) 0.1261(4) 0.0535 1.0000 Uani . . . . . . C52 C 0.3736(6) 0.0325(3) 0.1967(4) 0.0638 1.0000 Uani . . . . . . C53 C 0.4019(8) -0.0048(3) 0.3002(4) 0.1017 1.0000 Uani . . . . . . C61 C 0.1130(4) -0.0260(2) -0.5787(3) 0.0401 1.0000 Uani . . . . . . C62 C 0.0973(4) -0.0100(2) -0.6530(3) 0.0446 1.0000 Uani . . . . . . C63 C 0.1369(5) -0.0250(2) -0.7686(3) 0.0494 1.0000 Uani . . . . . . C101 C 0.1667(4) 0.17050(19) -0.3225(3) 0.0345 1.0000 Uani . . . . . . C102 C 0.2267(4) 0.1432(2) -0.3121(4) 0.0449 1.0000 Uani . . . . . . C103 C 0.2659(4) 0.1385(2) -0.2450(4) 0.0493 1.0000 Uani . . . . . . C104 C 0.2400(4) 0.1615(2) -0.1893(4) 0.0441 1.0000 Uani . . . . . . C105 C 0.1790(4) 0.18852(18) -0.2022(3) 0.0326 1.0000 Uani . . . . . . C106 C 0.1459(4) 0.21382(18) -0.1482(3) 0.0319 1.0000 Uani . . . . . . C107 C 0.1707(4) 0.2164(2) -0.0757(3) 0.0352 1.0000 Uani . . . . . . C108 C 0.1317(4) 0.24282(19) -0.0325(3) 0.0320 1.0000 Uani . . . . . . C109 C 0.0645(4) 0.26461(18) -0.0615(3) 0.0310 1.0000 Uani . . . . . . C110 C 0.0442(3) 0.26082(18) -0.1340(3) 0.0294 1.0000 Uani . . . . . . C111 C -0.0190(3) 0.28280(18) -0.1768(3) 0.0286 1.0000 Uani . . . . . . C112 C -0.0693(4) 0.3100(2) -0.1487(4) 0.0407 1.0000 Uani . . . . . . C113 C -0.1262(4) 0.3299(2) -0.1933(4) 0.0402 1.0000 Uani . . . . . . C114 C -0.1289(4) 0.3215(2) -0.2665(3) 0.0386 1.0000 Uani . . . . . . C115 C -0.0768(4) 0.29395(18) -0.2913(3) 0.0306 1.0000 Uani . . . . . . C116 C 0.1810(4) 0.3002(2) -0.2638(3) 0.0370 1.0000 Uani . . . . . . C117 C 0.2266(4) 0.3295(2) -0.2913(4) 0.0425 1.0000 Uani . . . . . . C118 C 0.2195(4) 0.3379(2) -0.3635(4) 0.0429 1.0000 Uani . . . . . . C119 C 0.1651(4) 0.31614(18) -0.4065(3) 0.0370 1.0000 Uani . . . . . . C120 C 0.1213(3) 0.28640(17) -0.3769(3) 0.0279 1.0000 Uani . . . . . . C121 C 0.0635(3) 0.25981(17) -0.4173(3) 0.0265 1.0000 Uani . . . . . . C122 C 0.0464(4) 0.25967(18) -0.4909(3) 0.0308 1.0000 Uani . . . . . . C123 C -0.0081(4) 0.2308(2) -0.5202(3) 0.0342 1.0000 Uani . . . . . . C124 C -0.0431(4) 0.20385(19) -0.4756(3) 0.0341 1.0000 Uani . . . . . . C125 C -0.0219(3) 0.20544(18) -0.4030(3) 0.0283 1.0000 Uani . . . . . . C126 C -0.0505(3) 0.18002(18) -0.3470(3) 0.0302 1.0000 Uani . . . . . . C127 C -0.1028(4) 0.14757(18) -0.3603(4) 0.0366 1.0000 Uani . . . . . . C128 C -0.1273(4) 0.12624(18) -0.3029(3) 0.0331 1.0000 Uani . . . . . . C129 C -0.0986(4) 0.13673(18) -0.2344(3) 0.0328 1.0000 Uani . . . . . . C130 C -0.0458(4) 0.16830(18) -0.2249(3) 0.0303 1.0000 Uani . . . . . . C131 C 0.3043(2) 0.27434(11) 0.37306(14) 0.0499 1.0000 Uani DG U . . . . C132 C 0.2555(2) 0.25966(12) 0.31601(12) 0.0451 1.0000 Uani DG U . . . . C133 C 0.2013(2) 0.22924(13) 0.32955(15) 0.0572 1.0000 Uani DG U . . . . C134 C 0.1966(2) 0.21452(12) 0.39827(17) 0.0589 1.0000 Uani DG U . . . . C135 C 0.2414(2) 0.21646(12) 0.52661(15) 0.0567 1.0000 Uani DG U . . . . C136 C 0.2892(3) 0.23283(13) 0.58209(13) 0.0559 1.0000 Uani DG U . . . . C137 C 0.3420(3) 0.26342(13) 0.56975(14) 0.0589 1.0000 Uani DG U . . . . C138 C 0.3484(2) 0.27735(11) 0.50069(16) 0.0546 1.0000 Uani DG U . . . . C139 C 0.29985(16) 0.26109(8) 0.44352(13) 0.0438 1.0000 Uani DG U . . . . C140 C 0.24536(17) 0.23044(8) 0.45577(13) 0.0470 1.0000 Uani DG U . . . . C141 C -0.0006(3) 0.31551(17) -0.6825(3) 0.0930 1.0000 Uani DG U . . . . C142 C -0.0372(3) 0.29044(15) -0.7347(3) 0.0872 1.0000 Uani DG U . . . . C143 C -0.0036(3) 0.28791(15) -0.8013(3) 0.0972 1.0000 Uani DG U . . . . C144 C 0.0596(4) 0.31181(17) -0.8223(3) 0.1094 1.0000 Uani DG U . . . . C145 C 0.1462(3) 0.36872(16) -0.7907(4) 0.1273 1.0000 Uani DG U . . . . C146 C 0.1749(3) 0.39621(14) -0.7397(5) 0.1430 1.0000 Uani DG U . . . . C147 C 0.1519(3) 0.39489(15) -0.6709(5) 0.1364 1.0000 Uani DG U . . . . C148 C 0.0990(4) 0.36614(17) -0.6510(3) 0.1311 1.0000 Uani DG U . . . . C149 C 0.0636(3) 0.33961(12) -0.7021(3) 0.1098 1.0000 Uani DG U . . . . C150 C 0.0917(2) 0.33955(12) -0.7710(3) 0.1073 1.0000 Uani DG U . . . . C151 C 0.2346(4) 0.2397(2) 0.0604(3) 0.0437 1.0000 Uani . . . . . . C152 C 0.2613(4) 0.2651(2) 0.1219(3) 0.0434 1.0000 Uani . . . . . . C153 C 0.2646(5) 0.2772(2) 0.2442(3) 0.0446 1.0000 Uani . . . . . . C161 C -0.0627(6) 0.1971(3) -0.6280(4) 0.0803 1.0000 Uani . . . . . . C162 C -0.0520(7) 0.2029(3) -0.7093(5) 0.0884 1.0000 Uani . . . . . . C163 C -0.1139(6) 0.2642(4) -0.7158(6) 0.1064 1.0000 Uani . . . . . . P1 P 0.07542(7) 0.09679(4) -0.48444(7) 0.0410 1.0000 Uani G . . . . . P2 P 0.15296(10) -0.09511(5) 0.02948(7) 0.0613 1.0000 Uani G . . . . . P3 P 0.38597(9) 0.13633(5) -0.00665(8) 0.0538 1.0000 Uani G . . . . . P4 P 0.22808(8) 0.35737(4) -0.05644(7) 0.0444 1.0000 Uani G . . . . . F101 F 0.09546(15) 0.09386(10) -0.56576(8) 0.0900 1.0000 Uani G . . . . . F102 F 0.05496(15) 0.10012(10) -0.40404(8) 0.0800 1.0000 Uani G . . . . . F103 F 0.16575(8) 0.08798(8) -0.45957(14) 0.0668 1.0000 Uani G . . . . . F104 F 0.09407(15) 0.14358(4) -0.48416(16) 0.0686 1.0000 Uani G . . . . . F105 F -0.01489(8) 0.10571(8) -0.50891(13) 0.0586 1.0000 Uani G . . . . . F106 F 0.05614(15) 0.05019(4) -0.48610(18) 0.0987 1.0000 Uani G . . . . . F201 F 0.11588(18) -0.12385(8) -0.03214(12) 0.0795 1.0000 Uani G . . . . . F202 F 0.19142(18) -0.06592(8) 0.09011(12) 0.1004 1.0000 Uani G . . . . . F203 F 0.23075(13) -0.09289(10) -0.01034(15) 0.0870 1.0000 Uani G . . . . . F204 F 0.1219(2) -0.05631(7) -0.01656(15) 0.1033 1.0000 Uani G . . . . . F205 F 0.07418(13) -0.09285(12) 0.06873(15) 0.1272 1.0000 Uani G . . . . . F206 F 0.1858(2) -0.13232(7) 0.07443(14) 0.0965 1.0000 Uani G . . . . . F301 F 0.3894(2) 0.12350(11) -0.08694(10) 0.0995 1.0000 Uani G . . . . . F302 F 0.3806(2) 0.14704(12) 0.07357(9) 0.1468 1.0000 Uani G . . . . . F303 F 0.47703(10) 0.14738(9) 0.00175(18) 0.0868 1.0000 Uani G . . . . . F304 F 0.36301(18) 0.18021(6) -0.03180(19) 0.0970 1.0000 Uani G . . . . . F305 F 0.29461(9) 0.12534(10) -0.01398(18) 0.0945 1.0000 Uani G . . . . . F306 F 0.40861(18) 0.09158(6) 0.0161(2) 0.1094 1.0000 Uani G . . . . . F401 F 0.14782(12) 0.34481(8) -0.10042(15) 0.0793 1.0000 Uani G . . . . . F402 F 0.30997(11) 0.36982(9) -0.01663(15) 0.0974 1.0000 Uani G . . . . . F403 F 0.18877(17) 0.34920(9) 0.01523(11) 0.0969 1.0000 Uani G . . . . . F404 F 0.19922(15) 0.40272(5) -0.05800(15) 0.0567 1.0000 Uani G . . . . . F405 F 0.26663(17) 0.36479(9) -0.12999(11) 0.0778 1.0000 Uani G . . . . . F406 F 0.25792(17) 0.31135(5) -0.05606(17) 0.1040 1.0000 Uani G . . . . . H11 H 0.3445 -0.0771 -0.3203 0.0428 1.0000 Uiso R . . . . . H21 H 0.4464 -0.1249 -0.2976 0.0538 1.0000 Uiso R . . . . . H31 H 0.5103 -0.1306 -0.1780 0.0610 1.0000 Uiso R . . . . . H41 H 0.4614 -0.0919 -0.0847 0.0495 1.0000 Uiso R . . . . . H71 H 0.4132 -0.0475 -0.0049 0.0418 1.0000 Uiso R . . . . . H91 H 0.2405 0.0413 0.0115 0.0533 1.0000 Uiso R . . . . . H121 H 0.1435 0.0749 -0.0578 0.0554 1.0000 Uiso R . . . . . H131 H 0.0477 0.1079 -0.1396 0.0674 1.0000 Uiso R . . . . . H141 H 0.0502 0.0939 -0.2653 0.0477 1.0000 Uiso R . . . . . H151 H 0.1357 0.0444 -0.3041 0.0452 1.0000 Uiso R . . . . . H161 H 0.3946 0.0412 -0.1597 0.0419 1.0000 Uiso R . . . . . H171 H 0.4854 0.0883 -0.2012 0.0495 1.0000 Uiso R . . . . . H181 H 0.4847 0.1006 -0.3285 0.0584 1.0000 Uiso R . . . . . H191 H 0.3927 0.0639 -0.4091 0.0481 1.0000 Uiso R . . . . . H221 H 0.2991 0.0275 -0.4756 0.0393 1.0000 Uiso R . . . . . H241 H 0.1102 -0.0507 -0.4531 0.0378 1.0000 Uiso R . . . . . H271 H 0.0446 -0.0836 -0.3668 0.0514 1.0000 Uiso R . . . . . H281 H -0.0110 -0.1152 -0.2687 0.0651 1.0000 Uiso R . . . . . H291 H 0.0518 -0.1081 -0.1508 0.0552 1.0000 Uiso R . . . . . H301 H 0.1675 -0.0692 -0.1322 0.0438 1.0000 Uiso R . . . . . H311 H 0.5129(3) 0.04209(17) 0.3802(3) 0.1026 1.0000 Uiso G . . . . . H331 H 0.2745(3) 0.02675(17) 0.3392(3) 0.0844 1.0000 Uiso G . . . . . H341 H 0.24294(19) 0.08249(18) 0.4125(3) 0.0873 1.0000 Uiso G . . . . . H351 H 0.2913(3) 0.13576(16) 0.5010(3) 0.0790 1.0000 Uiso G . . . . . H361 H 0.4042(4) 0.16715(13) 0.5622(2) 0.0892 1.0000 Uiso G . . . . . H371 H 0.5336(4) 0.14637(18) 0.5500(3) 0.1124 1.0000 Uiso G . . . . . H381 H 0.5598(2) 0.09265(19) 0.4723(3) 0.1060 1.0000 Uiso G . . . . . H411 H 0.1780(3) 0.05202(12) -0.73419(18) 0.0566 1.0000 Uiso G . . . . . H431 H 0.0592(3) -0.01622(9) -0.8938(2) 0.0595 1.0000 Uiso G . . . . . H441 H 0.0392(3) 0.04259(12) -0.96688(18) 0.0649 1.0000 Uiso G . . . . . H451 H 0.0480(3) 0.11607(13) -0.9816(2) 0.0677 1.0000 Uiso G . . . . . H461 H 0.0904(4) 0.18071(10) -0.9363(3) 0.0862 1.0000 Uiso G . . . . . H471 H 0.1605(4) 0.18529(9) -0.8201(3) 0.0912 1.0000 Uiso G . . . . . H481 H 0.1905(3) 0.12597(12) -0.7497(2) 0.0743 1.0000 Uiso G . . . . . H511 H 0.3258 0.0577 0.1021 0.0667 1.0000 Uiso R . . . . . H512 H 0.2703 0.0226 0.1340 0.0667 1.0000 Uiso R . . . . . H521 H 0.4314 0.0322 0.1888 0.0782 1.0000 Uiso R . . . . . H522 H 0.3609 0.0579 0.2228 0.0782 1.0000 Uiso R . . . . . H531 H 0.4584 -0.0061 0.2881 0.1208 1.0000 Uiso R . . . . . H532 H 0.3876 -0.0308 0.3237 0.1208 1.0000 Uiso R . . . . . H611 H 0.1202 -0.0561 -0.5801 0.0504 1.0000 Uiso R . . . . . H612 H 0.0673 -0.0193 -0.5501 0.0504 1.0000 Uiso R . . . . . H621 H 0.0460 -0.0213 -0.6751 0.0522 1.0000 Uiso R . . . . . H622 H 0.0941 0.0204 -0.6520 0.0522 1.0000 Uiso R . . . . . H631 H 0.1801 -0.0397 -0.7913 0.0660 1.0000 Uiso R . . . . . H632 H 0.0869 -0.0414 -0.7743 0.0660 1.0000 Uiso R . . . . . H1011 H 0.1394 0.1737 -0.3717 0.0431 1.0000 Uiso R . . . . . H1021 H 0.2425 0.1265 -0.3533 0.0540 1.0000 Uiso R . . . . . H1031 H 0.3110 0.1189 -0.2366 0.0570 1.0000 Uiso R . . . . . H1041 H 0.2663 0.1584 -0.1396 0.0512 1.0000 Uiso R . . . . . H1071 H 0.2157 0.1994 -0.0545 0.0444 1.0000 Uiso R . . . . . H1091 H 0.0333 0.2823 -0.0307 0.0367 1.0000 Uiso R . . . . . H1121 H -0.0650 0.3156 -0.0959 0.0487 1.0000 Uiso R . . . . . H1131 H -0.1636 0.3498 -0.1737 0.0487 1.0000 Uiso R . . . . . H1141 H -0.1689 0.3353 -0.3008 0.0453 1.0000 Uiso R . . . . . H1151 H -0.0796 0.2880 -0.3439 0.0355 1.0000 Uiso R . . . . . H1161 H 0.1871 0.2947 -0.2110 0.0439 1.0000 Uiso R . . . . . H1171 H 0.2655 0.3451 -0.2585 0.0521 1.0000 Uiso R . . . . . H1181 H 0.2534 0.3591 -0.3841 0.0534 1.0000 Uiso R . . . . . H1191 H 0.1571 0.3217 -0.4592 0.0465 1.0000 Uiso R . . . . . H1221 H 0.0717 0.2795 -0.5224 0.0377 1.0000 Uiso R . . . . . H1241 H -0.0824 0.1834 -0.4960 0.0409 1.0000 Uiso R . . . . . H1271 H -0.1219 0.1401 -0.4107 0.0447 1.0000 Uiso R . . . . . H1281 H -0.1655 0.1032 -0.3113 0.0421 1.0000 Uiso R . . . . . H1291 H -0.1162 0.1215 -0.1923 0.0406 1.0000 Uiso R . . . . . H1301 H -0.0247 0.1754 -0.1750 0.0372 1.0000 Uiso R . . . . . H1311 H 0.3444(3) 0.29548(14) 0.36314(19) 0.0594 1.0000 Uiso G . . . . . H1331 H 0.1664(3) 0.21779(17) 0.28856(18) 0.0670 1.0000 Uiso G . . . . . H1341 H 0.1580(3) 0.19244(15) 0.4072(2) 0.0716 1.0000 Uiso G . . . . . H1351 H 0.2040(3) 0.19399(15) 0.5364(2) 0.0738 1.0000 Uiso G . . . . . H1361 H 0.2852(3) 0.22279(17) 0.63216(14) 0.0665 1.0000 Uiso G . . . . . H1371 H 0.3752(3) 0.27569(16) 0.61100(17) 0.0731 1.0000 Uiso G . . . . . H1381 H 0.3889(3) 0.29846(15) 0.4915(2) 0.0676 1.0000 Uiso G . . . . . H1411 H -0.0191(4) 0.3161(2) -0.6331(3) 0.1118 1.0000 Uiso G . . . . . H1431 H -0.0269(5) 0.26695(19) -0.8356(4) 0.1190 1.0000 Uiso G . . . . . H1441 H 0.0805(5) 0.3095(2) -0.8706(3) 0.1450 1.0000 Uiso G . . . . . H1451 H 0.1631(4) 0.3705(2) -0.8406(5) 0.1637 1.0000 Uiso G . . . . . H1461 H 0.2145(3) 0.41717(18) -0.7517(7) 0.1804 1.0000 Uiso G . . . . . H1471 H 0.1747(4) 0.41588(19) -0.6364(6) 0.1842 1.0000 Uiso G . . . . . H1481 H 0.0873(5) 0.3650(2) -0.5995(3) 0.1549 1.0000 Uiso G . . . . . H1511 H 0.2691 0.2445 0.0203 0.0548 1.0000 Uiso R . . . . . H1512 H 0.2384 0.2105 0.0753 0.0548 1.0000 Uiso R . . . . . H1521 H 0.2386 0.2929 0.1136 0.0560 1.0000 Uiso R . . . . . H1522 H 0.3207 0.2667 0.1258 0.0560 1.0000 Uiso R . . . . . H1531 H 0.3222 0.2831 0.2402 0.0548 1.0000 Uiso R . . . . . H1532 H 0.2336 0.3031 0.2389 0.0548 1.0000 Uiso R . . . . . H1611 H -0.1205 0.1977 -0.6203 0.1029 1.0000 Uiso R . . . . . H1612 H -0.0391 0.1708 -0.6099 0.1029 1.0000 Uiso R . . . . . H1621 H 0.0003 0.2167 -0.7129 0.1148 1.0000 Uiso R . . . . . H1622 H -0.0515 0.1759 -0.7338 0.1148 1.0000 Uiso R . . . . . H1631 H -0.1635 0.2773 -0.7376 0.1181 1.0000 Uiso R . . . . . H1632 H -0.1158 0.2625 -0.6626 0.1181 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 Fe1 0.0284(5) 0.0311(5) 0.0225(4) -0.0008(4) -0.0022(3) 0.0019(4) Fe2 0.0291(5) 0.0292(5) 0.0217(4) 0.0006(4) -0.0034(3) 0.0012(4) O1 0.059(3) 0.062(3) 0.018(2) -0.007(2) -0.007(2) 0.007(2) O2 0.149(6) 0.060(4) 0.036(3) -0.003(3) -0.015(3) -0.006(4) O11 0.049(3) 0.050(3) 0.020(2) 0.007(2) -0.0026(19) -0.010(2) O12 0.054(3) 0.057(3) 0.028(2) -0.002(2) 0.002(2) 0.003(2) O21 0.037(2) 0.055(3) 0.020(2) 0.0025(19) -0.0077(18) 0.002(2) O22 0.050(3) 0.056(3) 0.027(2) -0.001(2) -0.006(2) -0.012(2) O31 0.061(3) 0.074(3) 0.020(2) 0.001(2) -0.008(2) -0.023(3) O32 0.123(6) 0.055(4) 0.060(4) 0.008(3) -0.036(4) -0.019(4) N1 0.033(3) 0.033(3) 0.027(3) 0.002(2) -0.009(2) 0.003(2) N2 0.031(3) 0.036(3) 0.026(3) 0.000(2) 0.004(2) 0.002(2) N3 0.027(3) 0.035(3) 0.035(3) -0.005(2) 0.002(2) 0.007(2) N4 0.027(3) 0.032(3) 0.033(3) 0.002(2) -0.004(2) 0.003(2) N5 0.025(3) 0.027(3) 0.033(3) 0.005(2) -0.004(2) -0.005(2) N6 0.028(3) 0.038(3) 0.027(3) -0.002(2) -0.004(2) 0.006(2) N7 0.028(3) 0.034(3) 0.028(3) 0.002(2) -0.004(2) 0.005(2) N8 0.021(3) 0.035(3) 0.027(3) 0.004(2) -0.009(2) -0.003(2) N9 0.022(3) 0.034(3) 0.028(3) 0.004(2) 0.000(2) 0.001(2) N10 0.035(3) 0.032(3) 0.027(3) -0.001(2) -0.001(2) 0.005(2) N11 0.034(3) 0.027(3) 0.025(3) 0.005(2) -0.002(2) 0.003(2) N12 0.031(3) 0.032(3) 0.022(3) 0.001(2) -0.002(2) 0.002(2) C1 0.040(4) 0.042(4) 0.029(3) -0.007(3) 0.002(3) -0.002(3) C2 0.046(4) 0.035(4) 0.051(4) -0.021(3) 0.005(3) 0.014(3) C3 0.054(4) 0.033(4) 0.060(5) -0.004(4) -0.014(4) 0.015(3) C4 0.038(4) 0.045(4) 0.037(4) -0.010(3) -0.011(3) 0.005(3) C5 0.023(3) 0.028(3) 0.033(3) 0.000(3) 0.000(3) 0.004(3) C6 0.032(3) 0.034(4) 0.031(3) 0.003(3) -0.005(3) 0.002(3) C7 0.039(4) 0.040(4) 0.022(3) 0.000(3) -0.002(3) -0.003(3) C8 0.045(4) 0.049(4) 0.028(3) 0.001(3) -0.002(3) -0.006(3) C9 0.054(4) 0.040(4) 0.033(4) -0.005(3) 0.009(3) 0.005(3) C10 0.030(3) 0.036(4) 0.032(3) 0.004(3) -0.004(3) 0.001(3) C11 0.039(4) 0.037(4) 0.029(3) 0.000(3) 0.006(3) 0.001(3) C12 0.048(4) 0.046(4) 0.044(4) -0.003(3) 0.009(3) 0.013(4) C13 0.059(5) 0.041(4) 0.067(5) 0.005(4) 0.007(4) 0.023(4) C14 0.036(4) 0.042(4) 0.041(4) 0.001(3) -0.007(3) 0.007(3) C15 0.027(3) 0.044(4) 0.034(3) 0.005(3) -0.005(3) 0.005(3) C16 0.030(4) 0.032(4) 0.037(4) -0.004(3) -0.008(3) 0.003(3) C17 0.040(4) 0.035(4) 0.052(4) 0.000(3) -0.013(3) 0.000(3) C18 0.043(4) 0.051(5) 0.055(5) 0.008(4) -0.005(3) -0.019(4) C19 0.037(4) 0.044(4) 0.039(4) 0.004(3) -0.001(3) -0.008(3) C20 0.026(3) 0.032(3) 0.037(4) 0.001(3) -0.004(3) -0.003(3) C21 0.027(3) 0.032(3) 0.033(3) 0.002(3) -0.002(3) 0.005(3) C22 0.032(3) 0.038(4) 0.025(3) 0.008(3) 0.002(3) -0.002(3) C23 0.035(3) 0.036(4) 0.026(3) 0.002(3) 0.007(3) 0.002(3) C24 0.027(3) 0.035(4) 0.028(3) -0.002(3) -0.005(3) 0.001(3) C25 0.030(3) 0.031(3) 0.030(3) 0.001(3) -0.003(3) 0.001(3) C26 0.029(3) 0.044(4) 0.023(3) 0.001(3) -0.002(3) 0.002(3) C27 0.036(4) 0.061(5) 0.032(4) 0.003(3) -0.001(3) -0.016(3) C28 0.041(4) 0.076(5) 0.043(4) 0.006(4) 0.005(3) -0.017(4) C29 0.043(4) 0.071(5) 0.030(4) 0.007(3) 0.006(3) -0.016(4) C30 0.034(4) 0.056(4) 0.016(3) 0.011(3) 0.010(3) 0.006(3) C31 0.092(6) 0.095(6) 0.045(5) 0.006(4) 0.010(4) -0.006(5) C32 0.079(5) 0.068(5) 0.036(4) 0.008(4) -0.007(4) -0.008(4) C33 0.094(6) 0.070(5) 0.041(4) 0.007(4) 0.020(4) -0.003(5) C34 0.060(5) 0.083(6) 0.063(5) 0.014(4) 0.001(4) -0.014(4) C35 0.092(6) 0.065(5) 0.049(5) 0.017(4) 0.026(4) -0.005(4) C36 0.113(6) 0.056(5) 0.043(4) 0.011(4) 0.016(4) -0.012(5) C37 0.109(7) 0.096(7) 0.064(6) 0.023(5) 0.007(5) -0.012(6) C38 0.084(6) 0.099(7) 0.073(6) 0.021(5) -0.002(5) -0.024(5) C39 0.061(4) 0.057(4) 0.031(4) 0.014(3) 0.007(3) -0.003(4) C40 0.071(4) 0.068(5) 0.029(3) 0.029(3) -0.003(3) -0.018(4) C41 0.056(4) 0.049(4) 0.036(4) -0.003(3) 0.003(3) -0.001(3) C42 0.056(4) 0.044(4) 0.032(3) 0.004(3) 0.004(3) 0.004(3) C43 0.068(5) 0.048(4) 0.036(4) -0.009(3) 0.001(3) 0.009(4) C44 0.064(5) 0.062(4) 0.034(4) 0.000(3) 0.003(3) 0.002(4) C45 0.057(5) 0.062(4) 0.050(4) 0.014(4) 0.012(4) 0.001(4) C46 0.075(6) 0.064(5) 0.077(5) 0.020(4) 0.016(4) -0.013(4) C47 0.086(6) 0.051(5) 0.075(5) 0.004(4) 0.026(4) -0.029(4) C48 0.067(5) 0.052(4) 0.062(5) -0.005(4) 0.021(4) -0.014(4) C49 0.050(4) 0.046(4) 0.048(4) 0.003(3) 0.018(3) -0.007(3) C50 0.048(4) 0.054(4) 0.040(4) 0.002(3) 0.007(3) 0.005(3) C51 0.075(5) 0.053(5) 0.033(4) -0.001(3) 0.006(4) -0.016(4) C52 0.095(7) 0.061(5) 0.034(4) 0.001(4) 0.002(4) -0.005(5) C53 0.182(12) 0.085(7) 0.035(5) -0.024(5) -0.014(6) 0.053(7) C61 0.047(4) 0.045(4) 0.027(3) -0.002(3) -0.008(3) -0.013(3) C62 0.059(5) 0.045(4) 0.028(3) 0.006(3) -0.010(3) -0.004(4) C63 0.077(5) 0.043(4) 0.027(3) 0.000(3) -0.001(3) 0.008(4) C101 0.037(4) 0.038(4) 0.030(3) 0.006(3) 0.008(3) 0.005(3) C102 0.048(4) 0.049(4) 0.037(4) -0.003(3) 0.004(3) 0.011(4) C103 0.047(4) 0.049(4) 0.051(4) 0.000(4) -0.004(3) 0.009(4) C104 0.047(4) 0.043(4) 0.040(4) 0.000(3) -0.015(3) 0.013(3) C105 0.035(4) 0.032(3) 0.029(3) 0.001(3) -0.006(3) 0.005(3) C106 0.042(4) 0.028(3) 0.024(3) -0.001(3) -0.006(3) -0.003(3) C107 0.037(4) 0.047(4) 0.021(3) 0.006(3) -0.005(3) -0.011(3) C108 0.035(4) 0.039(4) 0.021(3) -0.003(3) -0.005(3) -0.006(3) C109 0.041(4) 0.033(3) 0.019(3) 0.001(3) 0.001(3) -0.004(3) C110 0.018(3) 0.032(3) 0.037(3) -0.003(3) -0.003(3) -0.001(3) C111 0.030(3) 0.029(3) 0.026(3) -0.004(3) 0.000(3) -0.003(3) C112 0.037(4) 0.044(4) 0.040(4) -0.007(3) -0.007(3) 0.002(3) C113 0.032(4) 0.037(4) 0.052(4) -0.011(3) 0.006(3) 0.005(3) C114 0.031(4) 0.044(4) 0.039(4) 0.005(3) -0.008(3) 0.002(3) C115 0.035(4) 0.032(3) 0.025(3) 0.000(3) -0.001(3) -0.005(3) C116 0.035(4) 0.043(4) 0.032(3) -0.008(3) -0.007(3) -0.003(3) C117 0.038(4) 0.043(4) 0.046(4) -0.001(3) -0.001(3) -0.015(3) C118 0.044(4) 0.041(4) 0.044(4) 0.005(3) 0.008(3) -0.013(3) C119 0.052(4) 0.029(3) 0.029(3) 0.003(3) -0.003(3) -0.006(3) C120 0.031(3) 0.029(3) 0.024(3) 0.001(3) 0.002(2) 0.002(3) C121 0.033(3) 0.028(3) 0.019(3) 0.000(3) 0.000(2) 0.004(3) C122 0.039(4) 0.030(3) 0.023(3) 0.005(3) 0.000(3) -0.002(3) C123 0.033(4) 0.046(4) 0.023(3) -0.002(3) -0.003(3) -0.001(3) C124 0.034(4) 0.037(4) 0.030(3) -0.002(3) -0.004(3) -0.002(3) C125 0.029(3) 0.032(3) 0.024(3) 0.001(3) -0.001(2) 0.001(3) C126 0.029(3) 0.032(4) 0.030(3) -0.002(3) 0.003(3) 0.005(3) C127 0.039(4) 0.029(4) 0.041(4) -0.002(3) 0.000(3) 0.003(3) C128 0.041(4) 0.024(3) 0.036(4) 0.000(3) 0.010(3) -0.004(3) C129 0.034(3) 0.031(4) 0.034(3) 0.010(3) 0.004(3) 0.004(3) C130 0.035(4) 0.030(3) 0.026(3) 0.002(3) 0.005(3) 0.006(3) C131 0.061(5) 0.043(4) 0.044(4) 0.001(3) -0.007(3) -0.003(3) C132 0.052(4) 0.043(4) 0.039(4) 0.000(3) -0.004(3) 0.005(3) C133 0.045(4) 0.082(6) 0.043(4) -0.006(4) -0.007(3) -0.019(4) C134 0.054(5) 0.077(5) 0.045(4) 0.003(4) 0.002(3) -0.021(4) C135 0.070(5) 0.061(5) 0.040(4) 0.003(3) 0.008(3) 0.008(4) C136 0.067(5) 0.062(5) 0.038(4) 0.011(4) 0.002(3) 0.005(4) C137 0.072(5) 0.056(5) 0.045(4) 0.003(4) -0.013(4) -0.001(4) C138 0.068(5) 0.057(5) 0.037(4) -0.006(3) -0.005(3) -0.008(4) C139 0.048(4) 0.047(4) 0.035(3) 0.001(3) 0.000(3) 0.000(3) C140 0.047(4) 0.050(4) 0.044(4) -0.003(3) 0.007(3) 0.000(3) C141 0.106(7) 0.078(7) 0.086(7) 0.011(5) -0.039(6) 0.005(5) C142 0.098(8) 0.087(7) 0.070(5) 0.012(5) -0.033(5) 0.008(6) C143 0.110(8) 0.085(7) 0.093(6) -0.005(6) -0.014(6) -0.020(6) C144 0.082(7) 0.087(7) 0.153(10) 0.023(6) -0.027(7) -0.003(5) C145 0.056(6) 0.056(6) 0.266(14) -0.015(7) -0.012(7) 0.011(4) C146 0.045(6) 0.075(7) 0.305(15) -0.044(9) -0.007(8) 0.002(5) C147 0.051(6) 0.075(7) 0.271(14) -0.033(9) -0.062(7) 0.018(5) C148 0.097(8) 0.073(7) 0.207(12) -0.004(7) -0.081(8) 0.005(5) C149 0.084(7) 0.061(6) 0.173(9) 0.015(6) -0.053(6) -0.007(5) C150 0.062(6) 0.049(5) 0.203(10) 0.000(6) -0.035(6) 0.005(4) C151 0.053(4) 0.055(5) 0.022(3) 0.008(3) -0.002(3) 0.000(4) C152 0.050(4) 0.054(4) 0.025(3) -0.001(3) -0.002(3) -0.011(3) C153 0.061(5) 0.035(4) 0.036(4) -0.004(3) -0.004(3) 0.001(3) C161 0.116(8) 0.082(7) 0.040(5) 0.002(4) -0.012(5) -0.037(6) C162 0.121(9) 0.072(6) 0.066(6) -0.026(5) -0.025(6) 0.015(6) C163 0.062(6) 0.160(12) 0.091(8) -0.043(8) -0.029(5) 0.032(7) P1 0.0349(10) 0.0414(10) 0.0468(10) -0.0070(8) 0.0037(8) -0.0007(8) P2 0.0676(14) 0.0884(16) 0.0278(10) 0.0039(10) 0.0028(9) 0.0054(12) P3 0.0531(13) 0.0583(13) 0.0462(11) 0.0056(9) -0.0186(9) 0.0008(10) P4 0.0450(11) 0.0447(11) 0.0427(10) 0.0133(8) -0.0004(8) -0.0002(9) F101 0.068(3) 0.146(5) 0.058(3) -0.040(3) 0.015(2) -0.012(3) F102 0.069(3) 0.126(4) 0.045(3) 0.004(3) 0.005(2) 0.016(3) F103 0.040(2) 0.070(3) 0.089(3) -0.003(3) -0.003(2) 0.005(2) F104 0.061(3) 0.051(3) 0.092(3) -0.002(2) -0.003(2) -0.009(2) F105 0.044(2) 0.066(3) 0.063(3) -0.015(2) -0.011(2) 0.003(2) F106 0.064(3) 0.042(3) 0.193(6) -0.005(3) 0.027(4) 0.003(2) F201 0.090(4) 0.088(4) 0.057(3) 0.011(3) -0.014(2) -0.026(3) F202 0.115(5) 0.126(5) 0.055(3) -0.039(3) -0.023(3) 0.045(4) F203 0.096(4) 0.102(4) 0.066(3) -0.014(3) 0.019(3) -0.028(3) F204 0.153(6) 0.100(4) 0.053(3) -0.008(3) -0.015(3) 0.027(4) F205 0.081(4) 0.235(8) 0.068(4) 0.004(4) 0.019(3) -0.014(5) F206 0.128(5) 0.086(4) 0.070(3) 0.022(3) -0.026(3) -0.014(3) F301 0.098(4) 0.130(5) 0.067(3) -0.018(3) -0.012(3) 0.032(4) F302 0.144(6) 0.245(9) 0.047(3) -0.037(4) -0.014(3) 0.005(6) F303 0.057(3) 0.067(3) 0.129(4) 0.024(3) -0.035(3) -0.004(2) F304 0.084(4) 0.056(3) 0.143(5) 0.005(3) -0.032(3) 0.017(3) F305 0.058(3) 0.126(5) 0.095(4) 0.013(3) -0.023(3) 0.003(3) F306 0.089(4) 0.069(3) 0.158(5) 0.040(4) -0.059(4) -0.018(3) F401 0.066(3) 0.065(3) 0.102(4) 0.002(3) -0.021(3) -0.022(2) F402 0.063(3) 0.126(5) 0.094(4) 0.034(3) -0.046(3) -0.014(3) F403 0.116(4) 0.113(4) 0.065(3) 0.038(3) 0.023(3) 0.015(4) F404 0.054(3) 0.045(2) 0.071(3) -0.003(2) 0.003(2) 0.002(2) F405 0.091(4) 0.084(3) 0.062(3) 0.011(3) 0.026(3) 0.010(3) F406 0.085(4) 0.053(3) 0.180(6) 0.036(3) 0.042(4) 0.020(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1935(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 Fe1 . N1 . 1.971(5) yes Fe1 . N2 . 1.888(5) yes Fe1 . N3 . 1.987(5) yes Fe1 . N4 . 1.967(5) yes Fe1 . N5 . 1.877(5) yes Fe1 . N6 . 1.976(5) yes Fe2 . N7 . 1.973(5) yes Fe2 . N8 . 1.880(5) yes Fe2 . N9 . 1.976(5) yes Fe2 . N10 . 1.985(5) yes Fe2 . N11 . 1.883(5) yes Fe2 . N12 . 1.958(5) yes O1 . C8 . 1.343(7) yes O1 . C51 . 1.414(9) yes O2 . C52 . 1.397(9) yes O2 . C53 . 1.364(10) yes O11 . C23 . 1.337(7) yes O11 . C61 . 1.440(7) yes O12 . C62 . 1.414(8) yes O12 . C63 . 1.412(7) yes O21 . C108 . 1.323(7) yes O21 . C151 . 1.444(8) yes O22 . C152 . 1.406(8) yes O22 . C153 . 1.439(7) yes O31 . C123 . 1.337(7) yes O31 . C161 . 1.478(9) yes O32 . C162 . 1.327(11) yes O32 . C163 . 1.363(12) yes N1 . C1 . 1.329(8) yes N1 . C5 . 1.379(7) yes N2 . C6 . 1.346(7) yes N2 . C10 . 1.328(8) yes N3 . C11 . 1.340(8) yes N3 . C15 . 1.348(8) yes N4 . C16 . 1.351(7) yes N4 . C20 . 1.346(8) yes N5 . C21 . 1.345(7) yes N5 . C25 . 1.338(7) yes N6 . C26 . 1.372(7) yes N6 . C30 . 1.349(7) yes N7 . C101 . 1.345(8) yes N7 . C105 . 1.362(7) yes N8 . C106 . 1.350(7) yes N8 . C110 . 1.346(8) yes N9 . C111 . 1.356(7) yes N9 . C115 . 1.334(7) yes N10 . C116 . 1.352(8) yes N10 . C120 . 1.357(7) yes N11 . C121 . 1.330(7) yes N11 . C125 . 1.343(7) yes N12 . C126 . 1.366(7) yes N12 . C130 . 1.337(7) yes C1 . C2 . 1.361(9) yes C1 . H11 . 1.000 no C2 . C3 . 1.384(9) yes C2 . H21 . 1.000 no C3 . C4 . 1.356(9) yes C3 . H31 . 1.000 no C4 . C5 . 1.363(8) yes C4 . H41 . 1.000 no C5 . C6 . 1.474(8) yes C6 . C7 . 1.358(8) yes C7 . C8 . 1.387(9) yes C7 . H71 . 1.000 no C8 . C9 . 1.395(9) yes C9 . C10 . 1.392(9) yes C9 . H91 . 1.000 no C10 . C11 . 1.476(8) yes C11 . C12 . 1.373(9) yes C12 . C13 . 1.365(10) yes C12 . H121 . 1.000 no C13 . C14 . 1.388(10) yes C13 . H131 . 1.000 no C14 . C15 . 1.351(9) yes C14 . H141 . 1.000 no C15 . H151 . 1.000 no C16 . C17 . 1.368(9) yes C16 . H161 . 1.000 no C17 . C18 . 1.389(10) yes C17 . H171 . 1.000 no C18 . C19 . 1.376(9) yes C18 . H181 . 1.000 no C19 . C20 . 1.375(9) yes C19 . H191 . 1.000 no C20 . C21 . 1.460(8) yes C21 . C22 . 1.386(8) yes C22 . C23 . 1.400(8) yes C22 . H221 . 1.000 no C23 . C24 . 1.373(8) yes C24 . C25 . 1.383(8) yes C24 . H241 . 1.000 no C25 . C26 . 1.453(8) yes C26 . C27 . 1.375(9) yes C27 . C28 . 1.363(9) yes C27 . H271 . 1.000 no C28 . C29 . 1.369(9) yes C28 . H281 . 1.000 no C29 . C30 . 1.349(9) yes C29 . H291 . 1.000 no C30 . H301 . 1.000 no C31 . C32 . 1.3749(3) yes C31 . C39 . 1.4427(5) yes C31 . H311 . 1.00001(18) no C32 . C33 . 1.3923(2) yes C32 . C53 . 1.509(9) yes C33 . C34 . 1.3782(4) yes C33 . H331 . 1.0000(2) no C34 . C40 . 1.3791(3) yes C34 . H341 . 1.00000(18) no C35 . C36 . 1.3743(3) yes C35 . C40 . 1.4418(4) yes C35 . H351 . 1.00001(18) no C36 . C37 . 1.3716(2) yes C36 . H361 . 1.0000(3) no C37 . C38 . 1.3557(4) yes C37 . H371 . 1.0000(2) no C38 . C39 . 1.3691(3) yes C38 . H381 . 1.00001(18) no C39 . C40 . 1.4235(3) yes C41 . C42 . 1.3736(4) yes C41 . C49 . 1.4044(4) yes C41 . H411 . 1.0000(5) no C42 . C43 . 1.3923(7) yes C42 . C63 . 1.484(7) yes C43 . C44 . 1.3788(4) yes C43 . H431 . 1.0000(3) no C44 . C50 . 1.3947(4) yes C44 . H441 . 1.0000(5) no C45 . C46 . 1.3780(4) yes C45 . C50 . 1.4031(4) yes C45 . H451 . 1.0000(5) no C46 . C47 . 1.3947(7) yes C46 . H461 . 1.0000(3) no C47 . C48 . 1.3844(4) yes C47 . H471 . 1.0000(3) no C48 . C49 . 1.3996(4) yes C48 . H481 . 1.0000(5) no C49 . C50 . 1.4004(7) yes C51 . C52 . 1.489(10) yes C51 . H511 . 1.000 no C51 . H512 . 1.000 no C52 . H521 . 1.000 no C52 . H522 . 1.000 no C53 . H531 . 1.000 no C53 . H532 . 1.000 no C61 . C62 . 1.489(8) yes C61 . H611 . 1.000 no C61 . H612 . 1.000 no C62 . H621 . 1.000 no C62 . H622 . 1.000 no C63 . H631 . 1.000 no C63 . H632 . 1.000 no C101 . C102 . 1.356(9) yes C101 . H1011 . 1.000 no C102 . C103 . 1.378(9) yes C102 . H1021 . 1.000 no C103 . C104 . 1.389(10) yes C103 . H1031 . 1.000 no C104 . C105 . 1.367(9) yes C104 . H1041 . 1.000 no C105 . C106 . 1.455(9) yes C106 . C107 . 1.387(8) yes C107 . C108 . 1.388(9) yes C107 . H1071 . 1.000 no C108 . C109 . 1.412(9) yes C109 . C110 . 1.374(8) yes C109 . H1091 . 1.000 no C110 . C111 . 1.469(8) yes C111 . C112 . 1.369(9) yes C112 . C113 . 1.382(9) yes C112 . H1121 . 1.000 no C113 . C114 . 1.393(9) yes C113 . H1131 . 1.000 no C114 . C115 . 1.372(9) yes C114 . H1141 . 1.000 no C115 . H1151 . 1.000 no C116 . C117 . 1.363(9) yes C116 . H1161 . 1.000 no C117 . C118 . 1.373(9) yes C117 . H1171 . 1.000 no C118 . C119 . 1.372(9) yes C118 . H1181 . 1.000 no C119 . C120 . 1.372(8) yes C119 . H1191 . 1.000 no C120 . C121 . 1.472(8) yes C121 . C122 . 1.380(8) yes C122 . C123 . 1.401(8) yes C122 . H1221 . 1.000 no C123 . C124 . 1.384(9) yes C124 . C125 . 1.374(8) yes C124 . H1241 . 1.000 no C125 . C126 . 1.454(8) yes C126 . C127 . 1.395(9) yes C127 . C128 . 1.376(9) yes C127 . H1271 . 1.000 no C128 . C129 . 1.373(8) yes C128 . H1281 . 1.000 no C129 . C130 . 1.371(8) yes C129 . H1291 . 1.000 no C130 . H1301 . 1.000 no C131 . C132 . 1.3791(5) yes C131 . C139 . 1.3954(8) yes C131 . H1311 . 1.00001(19) no C132 . C133 . 1.3945(3) yes C132 . C153 . 1.482(7) yes C133 . C134 . 1.3812(7) yes C133 . H1331 . 1.0000(4) no C134 . C140 . 1.3997(5) yes C134 . H1341 . 1.0000(2) no C135 . C136 . 1.3693(5) yes C135 . C140 . 1.4087(8) yes C135 . H1351 . 1.0000(2) no C136 . C137 . 1.3775(3) yes C136 . H1361 . 1.0000(5) no C137 . C138 . 1.3829(7) yes C137 . H1371 . 1.0000(4) no C138 . C139 . 1.3976(5) yes C138 . H1381 . 1.00000(19) no C139 . C140 . 1.3978(3) yes C141 . C142 . 1.3836(5) yes C141 . C149 . 1.4162(3) yes C141 . H1411 . 1.0000(5) no C142 . C143 . 1.4133(7) yes C142 . C163 . 1.622(13) yes C143 . C144 . 1.4078(3) yes C143 . H1431 . 1.0000(3) no C144 . C150 . 1.4005(5) yes C144 . H1441 . 1.0000(5) no C145 . C146 . 1.3721(5) yes C145 . C150 . 1.4006(3) yes C145 . H1451 . 1.0000(5) no C146 . C147 . 1.3758(8) yes C146 . H1461 . 1.0000(2) no C147 . C148 . 1.3742(3) yes C147 . H1471 . 1.0000(3) no C148 . C149 . 1.3913(4) yes C148 . H1481 . 1.0000(6) no C149 . C150 . 1.4095(8) yes C151 . C152 . 1.463(9) yes C151 . H1511 . 1.000 no C151 . H1512 . 1.000 no C152 . H1521 . 1.000 no C152 . H1522 . 1.000 no C153 . H1531 . 1.000 no C153 . H1532 . 1.000 no C161 . C162 . 1.557(12) yes C161 . H1611 . 1.000 no C161 . H1612 . 1.000 no C162 . H1621 . 1.000 no C162 . H1622 . 1.000 no C163 . H1631 . 1.000 no C163 . H1632 . 1.000 no P1 . F101 . 1.5880(9) yes P1 . F102 . 1.5742(9) yes P1 . F103 . 1.5843(3) yes P1 . F104 . 1.5721(5) yes P1 . F105 . 1.5832(3) yes P1 . F106 . 1.5677(5) yes P2 . F201 . 1.5788(6) yes P2 . F202 . 1.5830(5) yes P2 . F203 . 1.5658(4) yes P2 . F204 . 1.6031(4) yes P2 . F205 . 1.5751(4) yes P2 . F206 . 1.5607(4) yes P3 . F301 . 1.5650(9) yes P3 . F302 . 1.5505(9) yes P3 . F303 . 1.5758(3) yes P3 . F304 . 1.5577(5) yes P3 . F305 . 1.5803(3) yes P3 . F306 . 1.5716(5) yes P4 . F401 . 1.5806(4) yes P4 . F402 . 1.5692(4) yes P4 . F403 . 1.5679(8) yes P4 . F404 . 1.5699(5) yes P4 . F405 . 1.5892(8) yes P4 . F406 . 1.5964(5) yes 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 . 81.2(2) yes N1 . Fe1 . N3 . 161.3(2) yes N2 . Fe1 . N3 . 80.2(2) yes N1 . Fe1 . N4 . 89.9(2) yes N2 . Fe1 . N4 . 97.8(2) yes N3 . Fe1 . N4 . 93.1(2) yes N1 . Fe1 . N5 . 100.2(2) yes N2 . Fe1 . N5 . 177.6(2) yes N3 . Fe1 . N5 . 98.5(2) yes N4 . Fe1 . N5 . 80.3(2) yes N1 . Fe1 . N6 . 94.0(2) yes N2 . Fe1 . N6 . 101.0(2) yes N3 . Fe1 . N6 . 89.1(2) yes N4 . Fe1 . N6 . 161.2(2) yes N5 . Fe1 . N6 . 80.9(2) yes N7 . Fe2 . N8 . 81.0(2) yes N7 . Fe2 . N9 . 161.59(19) yes N8 . Fe2 . N9 . 80.6(2) yes N7 . Fe2 . N10 . 92.8(2) yes N8 . Fe2 . N10 . 99.0(2) yes N9 . Fe2 . N10 . 91.2(2) yes N7 . Fe2 . N11 . 99.2(2) yes N8 . Fe2 . N11 . 179.4(2) yes N9 . Fe2 . N11 . 99.2(2) yes N10 . Fe2 . N11 . 80.4(2) yes N7 . Fe2 . N12 . 89.3(2) yes N8 . Fe2 . N12 . 99.2(2) yes N9 . Fe2 . N12 . 92.4(2) yes N10 . Fe2 . N12 . 161.77(19) yes N11 . Fe2 . N12 . 81.3(2) yes C8 . O1 . C51 . 118.9(5) yes C52 . O2 . C53 . 113.3(8) yes C23 . O11 . C61 . 118.7(5) yes C62 . O12 . C63 . 113.8(5) yes C108 . O21 . C151 . 116.5(5) yes C152 . O22 . C153 . 109.0(5) yes C123 . O31 . C161 . 118.1(5) yes C162 . O32 . C163 . 115.0(7) yes Fe1 . N1 . C1 . 128.4(4) yes Fe1 . N1 . C5 . 114.3(4) yes C1 . N1 . C5 . 117.2(5) yes Fe1 . N2 . C6 . 119.6(4) yes Fe1 . N2 . C10 . 119.8(4) yes C6 . N2 . C10 . 120.4(5) yes Fe1 . N3 . C11 . 115.1(4) yes Fe1 . N3 . C15 . 126.7(4) yes C11 . N3 . C15 . 118.2(5) yes Fe1 . N4 . C16 . 126.5(4) yes Fe1 . N4 . C20 . 115.8(4) yes C16 . N4 . C20 . 117.6(5) yes Fe1 . N5 . C21 . 119.4(4) yes Fe1 . N5 . C25 . 119.7(4) yes C21 . N5 . C25 . 120.8(5) yes Fe1 . N6 . C26 . 113.8(4) yes Fe1 . N6 . C30 . 127.8(4) yes C26 . N6 . C30 . 118.4(5) yes Fe2 . N7 . C101 . 127.7(4) yes Fe2 . N7 . C105 . 114.5(4) yes C101 . N7 . C105 . 117.8(5) yes Fe2 . N8 . C106 . 118.8(4) yes Fe2 . N8 . C110 . 120.3(4) yes C106 . N8 . C110 . 120.8(5) yes Fe2 . N9 . C111 . 114.5(4) yes Fe2 . N9 . C115 . 127.4(4) yes C111 . N9 . C115 . 118.1(5) yes Fe2 . N10 . C116 . 128.1(4) yes Fe2 . N10 . C120 . 114.9(4) yes C116 . N10 . C120 . 117.0(5) yes Fe2 . N11 . C121 . 119.6(4) yes Fe2 . N11 . C125 . 119.2(4) yes C121 . N11 . C125 . 121.2(5) yes Fe2 . N12 . C126 . 113.8(4) yes Fe2 . N12 . C130 . 128.8(4) yes C126 . N12 . C130 . 117.4(5) yes N1 . C1 . C2 . 123.5(6) yes N1 . C1 . H11 . 118.004 no C2 . C1 . H11 . 118.481 no C1 . C2 . C3 . 118.6(6) yes C1 . C2 . H21 . 120.421 no C3 . C2 . H21 . 120.958 no C2 . C3 . C4 . 119.2(6) yes C2 . C3 . H31 . 120.500 no C4 . C3 . H31 . 120.328 no C3 . C4 . C5 . 120.0(6) yes C3 . C4 . H41 . 120.267 no C5 . C4 . H41 . 119.730 no N1 . C5 . C4 . 121.4(5) yes N1 . C5 . C6 . 113.3(5) yes C4 . C5 . C6 . 125.3(5) yes C5 . C6 . N2 . 111.4(5) yes C5 . C6 . C7 . 127.3(6) yes N2 . C6 . C7 . 121.2(6) yes C6 . C7 . C8 . 119.0(6) yes C6 . C7 . H71 . 120.411 no C8 . C7 . H71 . 120.604 no C7 . C8 . O1 . 116.2(6) yes C7 . C8 . C9 . 120.6(6) yes O1 . C8 . C9 . 123.2(6) yes C8 . C9 . C10 . 116.5(6) yes C8 . C9 . H91 . 121.370 no C10 . C9 . H91 . 122.153 no C9 . C10 . N2 . 122.3(6) yes C9 . C10 . C11 . 125.7(6) yes N2 . C10 . C11 . 111.9(5) yes C10 . C11 . N3 . 113.0(5) yes C10 . C11 . C12 . 125.0(6) yes N3 . C11 . C12 . 122.0(6) yes C11 . C12 . C13 . 119.8(7) yes C11 . C12 . H121 . 120.060 no C13 . C12 . H121 . 120.146 no C12 . C13 . C14 . 117.9(7) yes C12 . C13 . H131 . 121.663 no C14 . C13 . H131 . 120.431 no C13 . C14 . C15 . 120.0(6) yes C13 . C14 . H141 . 120.228 no C15 . C14 . H141 . 119.760 no C14 . C15 . N3 . 122.1(6) yes C14 . C15 . H151 . 119.159 no N3 . C15 . H151 . 118.775 no N4 . C16 . C17 . 122.8(6) yes N4 . C16 . H161 . 118.271 no C17 . C16 . H161 . 118.921 no C16 . C17 . C18 . 118.6(6) yes C16 . C17 . H171 . 120.312 no C18 . C17 . H171 . 121.044 no C17 . C18 . C19 . 119.3(6) yes C17 . C18 . H181 . 120.560 no C19 . C18 . H181 . 120.131 no C18 . C19 . C20 . 118.8(6) yes C18 . C19 . H191 . 121.141 no C20 . C19 . H191 . 120.083 no C19 . C20 . N4 . 122.8(5) yes C19 . C20 . C21 . 124.5(6) yes N4 . C20 . C21 . 112.6(5) yes C20 . C21 . N5 . 111.9(5) yes C20 . C21 . C22 . 126.8(6) yes N5 . C21 . C22 . 121.2(5) yes C21 . C22 . C23 . 117.8(6) yes C21 . C22 . H221 . 121.123 no C23 . C22 . H221 . 121.058 no C22 . C23 . O11 . 115.9(5) yes C22 . C23 . C24 . 120.2(5) yes O11 . C23 . C24 . 123.9(5) yes C23 . C24 . C25 . 119.0(6) yes C23 . C24 . H241 . 120.429 no C25 . C24 . H241 . 120.543 no C24 . C25 . N5 . 120.9(5) yes C24 . C25 . C26 . 127.2(5) yes N5 . C25 . C26 . 111.8(5) yes C25 . C26 . N6 . 113.7(5) yes C25 . C26 . C27 . 125.7(5) yes N6 . C26 . C27 . 120.6(5) yes C26 . C27 . C28 . 119.2(6) yes C26 . C27 . H271 . 120.117 no C28 . C27 . H271 . 120.728 no C27 . C28 . C29 . 120.3(7) yes C27 . C28 . H281 . 119.737 no C29 . C28 . H281 . 119.962 no C28 . C29 . C30 . 119.2(6) yes C28 . C29 . H291 . 120.548 no C30 . C29 . H291 . 120.233 no N6 . C30 . C29 . 122.2(6) yes N6 . C30 . H301 . 118.759 no C29 . C30 . H301 . 118.999 no C32 . C31 . C39 . 120.54(2) yes C32 . C31 . H311 . 118.04(2) no C39 . C31 . H311 . 121.422(15) no C31 . C32 . C33 . 116.66(2) yes C31 . C32 . C53 . 126.9(6) yes C33 . C32 . C53 . 116.4(6) yes C32 . C33 . C34 . 126.881(15) yes C32 . C33 . H331 . 116.538(18) no C34 . C33 . H331 . 116.579(16) no C33 . C34 . C40 . 115.486(17) yes C33 . C34 . H341 . 123.372(15) no C40 . C34 . H341 . 121.14(2) no C36 . C35 . C40 . 115.93(2) yes C36 . C35 . H351 . 120.83(2) no C40 . C35 . H351 . 123.244(15) no C35 . C36 . C37 . 124.55(2) yes C35 . C36 . H361 . 119.34(2) no C37 . C36 . H361 . 116.110(19) no C36 . C37 . C38 . 119.893(17) yes C36 . C37 . H371 . 120.522(17) no C38 . C37 . H371 . 119.584(16) no C37 . C38 . C39 . 119.686(16) yes C37 . C38 . H381 . 120.290(16) no C39 . C38 . H381 . 120.02(2) no C31 . C39 . C38 . 120.421(16) yes C31 . C39 . C40 . 117.868(18) yes C38 . C39 . C40 . 121.64(2) yes C35 . C40 . C39 . 118.278(17) yes C35 . C40 . C34 . 119.323(16) yes C39 . C40 . C34 . 122.334(17) yes C42 . C41 . C49 . 120.12(3) yes C42 . C41 . H411 . 119.26(3) no C49 . C41 . H411 . 120.62(3) no C41 . C42 . C43 . 120.23(3) yes C41 . C42 . C63 . 122.7(3) yes C43 . C42 . C63 . 116.9(3) yes C42 . C43 . C44 . 120.065(9) yes C42 . C43 . H431 . 119.608(9) no C44 . C43 . H431 . 120.33(3) no C43 . C44 . C50 . 120.77(3) yes C43 . C44 . H441 . 119.56(3) no C50 . C44 . H441 . 119.66(3) no C46 . C45 . C50 . 120.63(3) yes C46 . C45 . H451 . 120.05(3) no C50 . C45 . H451 . 119.32(3) no C45 . C46 . C47 . 118.98(3) yes C45 . C46 . H461 . 119.99(3) no C47 . C46 . H461 . 121.030(7) no C46 . C47 . C48 . 121.725(7) yes C46 . C47 . H471 . 118.577(8) no C48 . C47 . H471 . 119.70(3) no C47 . C48 . C49 . 119.19(3) yes C47 . C48 . H481 . 120.36(3) no C49 . C48 . H481 . 120.45(3) no C41 . C49 . C48 . 120.49(3) yes C41 . C49 . C50 . 119.80(3) yes C48 . C49 . C50 . 119.69(3) yes C45 . C50 . C49 . 119.76(3) yes C45 . C50 . C44 . 121.11(3) yes C49 . C50 . C44 . 118.998(9) yes O1 . C51 . C52 . 109.1(7) yes O1 . C51 . H511 . 109.978 no C52 . C51 . H511 . 110.003 no O1 . C51 . H512 . 109.219 no C52 . C51 . H512 . 109.071 no H511 . C51 . H512 . 109.468 no C51 . C52 . O2 . 108.6(7) yes C51 . C52 . H521 . 109.223 no O2 . C52 . H521 . 110.077 no C51 . C52 . H522 . 110.087 no O2 . C52 . H522 . 109.334 no H521 . C52 . H522 . 109.468 no C32 . C53 . O2 . 115.8(7) yes C32 . C53 . H531 . 107.524 no O2 . C53 . H531 . 107.938 no C32 . C53 . H532 . 108.075 no O2 . C53 . H532 . 107.891 no H531 . C53 . H532 . 109.468 no O11 . C61 . C62 . 108.9(5) yes O11 . C61 . H611 . 109.845 no C62 . C61 . H611 . 109.774 no O11 . C61 . H612 . 109.065 no C62 . C61 . H612 . 109.724 no H611 . C61 . H612 . 109.467 no C61 . C62 . O12 . 109.1(6) yes C61 . C62 . H621 . 109.468 no O12 . C62 . H621 . 109.125 no C61 . C62 . H622 . 109.925 no O12 . C62 . H622 . 109.752 no H621 . C62 . H622 . 109.467 no C42 . C63 . O12 . 117.3(5) yes C42 . C63 . H631 . 108.151 no O12 . C63 . H631 . 107.621 no C42 . C63 . H632 . 106.916 no O12 . C63 . H632 . 107.181 no H631 . C63 . H632 . 109.467 no N7 . C101 . C102 . 122.8(6) yes N7 . C101 . H1011 . 118.349 no C102 . C101 . H1011 . 118.816 no C101 . C102 . C103 . 120.1(6) yes C101 . C102 . H1021 . 119.962 no C103 . C102 . H1021 . 119.968 no C102 . C103 . C104 . 117.6(6) yes C102 . C103 . H1031 . 121.177 no C104 . C103 . H1031 . 121.223 no C103 . C104 . C105 . 120.3(6) yes C103 . C104 . H1041 . 119.746 no C105 . C104 . H1041 . 119.981 no C104 . C105 . N7 . 121.4(6) yes C104 . C105 . C106 . 125.3(5) yes N7 . C105 . C106 . 113.3(5) yes C105 . C106 . N8 . 112.1(5) yes C105 . C106 . C107 . 127.6(6) yes N8 . C106 . C107 . 120.2(6) yes C106 . C107 . C108 . 119.2(6) yes C106 . C107 . H1071 . 120.593 no C108 . C107 . H1071 . 120.219 no C107 . C108 . O21 . 123.9(5) yes C107 . C108 . C109 . 120.0(5) yes O21 . C108 . C109 . 116.1(6) yes C108 . C109 . C110 . 117.3(6) yes C108 . C109 . H1091 . 121.303 no C110 . C109 . H1091 . 121.400 no C109 . C110 . N8 . 122.3(5) yes C109 . C110 . C111 . 127.0(6) yes N8 . C110 . C111 . 110.7(5) yes C110 . C111 . N9 . 113.9(5) yes C110 . C111 . C112 . 124.0(5) yes N9 . C111 . C112 . 122.0(5) yes C111 . C112 . C113 . 120.1(6) yes C111 . C112 . H1121 . 120.129 no C113 . C112 . H1121 . 119.785 no C112 . C113 . C114 . 117.5(6) yes C112 . C113 . H1131 . 121.143 no C114 . C113 . H1131 . 121.307 no C113 . C114 . C115 . 119.5(6) yes C113 . C114 . H1141 . 120.350 no C115 . C114 . H1141 . 120.104 no C114 . C115 . N9 . 122.7(6) yes C114 . C115 . H1151 . 118.870 no N9 . C115 . H1151 . 118.398 no N10 . C116 . C117 . 122.2(6) yes N10 . C116 . H1161 . 118.618 no C117 . C116 . H1161 . 119.153 no C116 . C117 . C118 . 120.5(6) yes C116 . C117 . H1171 . 119.622 no C118 . C117 . H1171 . 119.881 no C117 . C118 . C119 . 118.1(6) yes C117 . C118 . H1181 . 120.878 no C119 . C118 . H1181 . 121.057 no C118 . C119 . C120 . 119.6(6) yes C118 . C119 . H1191 . 120.623 no C120 . C119 . H1191 . 119.781 no C119 . C120 . N10 . 122.6(5) yes C119 . C120 . C121 . 125.0(5) yes N10 . C120 . C121 . 112.4(5) yes C120 . C121 . N11 . 112.5(5) yes C120 . C121 . C122 . 126.0(5) yes N11 . C121 . C122 . 121.4(5) yes C121 . C122 . C123 . 117.8(5) yes C121 . C122 . H1221 . 121.333 no C123 . C122 . H1221 . 120.821 no C122 . C123 . O31 . 114.7(5) yes C122 . C123 . C124 . 120.0(5) yes O31 . C123 . C124 . 125.3(6) yes C123 . C124 . C125 . 118.8(6) yes C123 . C124 . H1241 . 120.430 no C125 . C124 . H1241 . 120.803 no C124 . C125 . N11 . 120.8(5) yes C124 . C125 . C126 . 127.9(6) yes N11 . C125 . C126 . 111.3(5) yes C125 . C126 . N12 . 114.3(5) yes C125 . C126 . C127 . 123.8(5) yes N12 . C126 . C127 . 121.9(5) yes C126 . C127 . C128 . 118.7(6) yes C126 . C127 . H1271 . 120.419 no C128 . C127 . H1271 . 120.928 no C127 . C128 . C129 . 119.5(6) yes C127 . C128 . H1281 . 119.771 no C129 . C128 . H1281 . 120.692 no C128 . C129 . C130 . 119.1(6) yes C128 . C129 . H1291 . 120.201 no C130 . C129 . H1291 . 120.741 no C129 . C130 . N12 . 123.5(5) yes C129 . C130 . H1301 . 118.441 no N12 . C130 . H1301 . 118.091 no C132 . C131 . C139 . 122.98(3) yes C132 . C131 . H1311 . 118.11(4) no C139 . C131 . H1311 . 118.91(3) no C131 . C132 . C133 . 118.05(4) yes C131 . C132 . C153 . 117.5(3) yes C133 . C132 . C153 . 124.4(3) yes C132 . C133 . C134 . 120.686(19) yes C132 . C133 . H1331 . 119.011(19) no C134 . C133 . H1331 . 120.29(3) no C133 . C134 . C140 . 120.47(3) yes C133 . C134 . H1341 . 119.98(3) no C140 . C134 . H1341 . 119.55(4) no C136 . C135 . C140 . 120.80(3) yes C136 . C135 . H1351 . 119.56(4) no C140 . C135 . H1351 . 119.63(3) no C135 . C136 . C137 . 120.60(3) yes C135 . C136 . H1361 . 119.84(4) no C137 . C136 . H1361 . 119.558(19) no C136 . C137 . C138 . 120.122(19) yes C136 . C137 . H1371 . 119.691(19) no C138 . C137 . H1371 . 120.18(3) no C137 . C138 . C139 . 119.97(3) yes C137 . C138 . H1381 . 120.02(3) no C139 . C138 . H1381 . 119.99(4) no C138 . C139 . C131 . 121.84(3) yes C138 . C139 . C140 . 120.22(3) yes C131 . C139 . C140 . 117.94(3) yes C135 . C140 . C134 . 121.90(3) yes C135 . C140 . C139 . 118.27(3) yes C134 . C140 . C139 . 119.83(4) yes C142 . C141 . C149 . 117.22(4) yes C142 . C141 . H1411 . 120.52(3) no C149 . C141 . H1411 . 122.26(2) no C141 . C142 . C143 . 117.91(3) yes C141 . C142 . C163 . 118.8(5) yes C143 . C142 . C163 . 123.3(5) yes C142 . C143 . C144 . 125.617(17) yes C142 . C143 . H1431 . 116.125(19) no C144 . C143 . H1431 . 118.25(3) no C143 . C144 . C150 . 115.66(3) yes C143 . C144 . H1441 . 122.84(2) no C150 . C144 . H1441 . 121.50(3) no C146 . C145 . C150 . 118.09(4) yes C146 . C145 . H1451 . 119.85(4) no C150 . C145 . H1451 . 122.04(2) no C145 . C146 . C147 . 121.14(3) yes C145 . C146 . H1461 . 120.27(3) no C147 . C146 . H1461 . 118.56(2) no C146 . C147 . C148 . 121.068(18) yes C146 . C147 . H1471 . 117.199(18) no C148 . C147 . H1471 . 121.73(3) no C147 . C148 . C149 . 119.91(2) yes C147 . C148 . H1481 . 118.21(3) no C149 . C148 . H1481 . 121.88(3) no C141 . C149 . C148 . 117.92(3) yes C141 . C149 . C150 . 124.09(2) yes C148 . C149 . C150 . 117.95(3) yes C149 . C150 . C145 . 121.291(17) yes C149 . C150 . C144 . 119.02(2) yes C145 . C150 . C144 . 119.48(2) yes O21 . C151 . C152 . 110.2(6) yes O21 . C151 . H1511 . 109.332 no C152 . C151 . H1511 . 109.708 no O21 . C151 . H1512 . 109.284 no C152 . C151 . H1512 . 108.827 no H1511 . C151 . H1512 . 109.467 no C151 . C152 . O22 . 112.7(6) yes C151 . C152 . H1521 . 108.273 no O22 . C152 . H1521 . 108.458 no C151 . C152 . H1522 . 109.179 no O22 . C152 . H1522 . 108.724 no H1521 . C152 . H1522 . 109.466 no C132 . C153 . O22 . 112.3(5) yes C132 . C153 . H1531 . 108.651 no O22 . C153 . H1531 . 108.754 no C132 . C153 . H1532 . 109.135 no O22 . C153 . H1532 . 108.497 no H1531 . C153 . H1532 . 109.466 no O31 . C161 . C162 . 105.2(7) yes O31 . C161 . H1611 . 111.160 no C162 . C161 . H1611 . 109.556 no O31 . C161 . H1612 . 110.245 no C162 . C161 . H1612 . 111.157 no H1611 . C161 . H1612 . 109.466 no C161 . C162 . O32 . 113.5(9) yes C161 . C162 . H1621 . 107.207 no O32 . C162 . H1621 . 107.595 no C161 . C162 . H1622 . 110.110 no O32 . C162 . H1622 . 108.866 no H1621 . C162 . H1622 . 109.466 no C142 . C163 . O32 . 108.7(8) yes C142 . C163 . H1631 . 109.752 no O32 . C163 . H1631 . 109.563 no C142 . C163 . H1632 . 109.977 no O32 . C163 . H1632 . 109.361 no H1631 . C163 . H1632 . 109.465 no F101 . P1 . F102 . 179.361 yes F101 . P1 . F103 . 89.53(5) yes F102 . P1 . F103 . 90.94(5) yes F101 . P1 . F104 . 90.22(4) yes F102 . P1 . F104 . 89.35(4) yes F103 . P1 . F104 . 89.442(13) yes F101 . P1 . F105 . 90.74(5) yes F102 . P1 . F105 . 88.80(5) yes F103 . P1 . F105 . 179.700 yes F104 . P1 . F105 . 90.42(3) yes F101 . P1 . F106 . 88.99(4) yes F102 . P1 . F106 . 91.44(4) yes F103 . P1 . F106 . 91.159(12) yes F104 . P1 . F106 . 179.002 yes F105 . P1 . F106 . 88.987(12) yes F201 . P2 . F202 . 178.773 yes F201 . P2 . F203 . 88.77(3) yes F202 . P2 . F203 . 90.10(3) yes F201 . P2 . F204 . 89.66(2) yes F202 . P2 . F204 . 89.81(4) yes F203 . P2 . F204 . 87.55(3) yes F201 . P2 . F205 . 93.97(3) yes F202 . P2 . F205 . 87.12(3) yes F203 . P2 . F205 . 174.583 yes F204 . P2 . F205 . 87.80(3) yes F201 . P2 . F206 . 91.37(2) yes F202 . P2 . F206 . 89.13(2) yes F203 . P2 . F206 . 91.02(3) yes F204 . P2 . F206 . 178.219 yes F205 . P2 . F206 . 93.58(3) yes F301 . P3 . F302 . 177.218 yes F301 . P3 . F303 . 92.44(4) yes F302 . P3 . F303 . 89.27(4) yes F301 . P3 . F304 . 89.391(13) yes F302 . P3 . F304 . 92.743(14) yes F303 . P3 . F304 . 91.859(11) yes F301 . P3 . F305 . 88.31(4) yes F302 . P3 . F305 . 89.98(4) yes F303 . P3 . F305 . 179.247 yes F304 . P3 . F305 . 88.24(3) yes F301 . P3 . F306 . 88.80(5) yes F302 . P3 . F306 . 89.057(16) yes F303 . P3 . F306 . 88.624(10) yes F304 . P3 . F306 . 178.142 yes F305 . P3 . F306 . 91.297(11) yes F401 . P4 . F402 . 176.933 yes F401 . P4 . F403 . 89.59(3) yes F402 . P4 . F403 . 93.43(3) yes F401 . P4 . F404 . 89.291(12) yes F402 . P4 . F404 . 91.182(10) yes F403 . P4 . F404 . 91.48(4) yes F401 . P4 . F405 . 89.23(5) yes F402 . P4 . F405 . 87.75(3) yes F403 . P4 . F405 . 178.591 yes F404 . P4 . F405 . 89.27(3) yes F401 . P4 . F406 . 90.619(12) yes F402 . P4 . F406 . 88.860(11) yes F403 . P4 . F406 . 89.41(4) yes F404 . P4 . F406 . 179.107 yes F405 . P4 . F406 . 89.84(3) yes # Attachment 'Hydroxy.cif' data_hsc2f2_173k _database_code_depnum_ccdc_archive 'CCDC 288505' _audit_creation_date 05-10-26 _audit_creation_method CRYSTALS_ver_12.24 _oxford_structure_analysis_title '10261740 hsc2f2_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 10.5509(3) _cell_length_b 22.5202(7) _cell_length_c 7.2890(2) _cell_angle_alpha 90 _cell_angle_beta 109.0636(16) _cell_angle_gamma 90 _cell_volume 1636.94(8) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z x,-y,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' _cell_formula_units_Z 4 _chemical_formula_sum 'C19 H19 N3 O3' _chemical_formula_moiety 'C19 H19 N3 O3' _chemical_compound_source ? _chemical_formula_weight 337.38 _cell_measurement_reflns_used 2890 _cell_measurement_theta_min 3 _cell_measurement_theta_max 32 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_max 0.32 _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.094 _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 1.00 # Sheldrick geometric definitions 0.98 1.00 _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 'USER DEFINED STRUCTURE SOLUTION' _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 5652 _reflns_number_total 2835 _diffrn_reflns_av_R_equivalents 0.020 # Number of reflections with Friedels Law is 2835 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 2836 _diffrn_reflns_theta_min 3.129 _diffrn_reflns_theta_max 31.976 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 31.976 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _reflns_limit_h_min -15 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 33 _reflns_limit_l_min 0 _reflns_limit_l_max 10 _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 -0.33 _refine_diff_density_max 0.66 _refine_ls_number_reflns 1970 _refine_ls_number_restraints 2 _refine_ls_number_parameters 227 #_refine_ls_R_factor_ref 0.0511 _refine_ls_wR_factor_ref 0.0627 _refine_ls_goodness_of_fit_ref 0.9494 #_reflns_number_all 2828 _refine_ls_R_factor_all 0.0810 _refine_ls_wR_factor_all 0.1411 # 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 1970 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_gt 0.0627 _refine_ls_shift/su_max 0.020162 # 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 unk _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 ; p=P(6)*max(Fo^2^,0) + (1-P(6))Fc^2^ Method = SHELXL 97 (Sheldrick, 1997) W = 1. / [Sigma^2^(F*)+(P(1)p)^2^+P(2)p+P(4)+P(5)Sin(theta) ] P(i) are: 0.00 0.575E-01 0.00 0.00 0.00 0.333 ; _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 ; User-defined structure solution reference 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. Sheldrick, G.M. (1997). SHELXL-97. Program for the refinement of crystal structures. Univ. of Gottingen, Federal Republic of Germany. 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 O1 O -0.0107(3) 0.64479(11) 0.3304(4) 0.0346 1.0000 Uani . . . . . . O2 O 0.0421(3) 0.75913(11) 0.5497(4) 0.0420 1.0000 Uani . . . . . . O3 O 0.0347(2) 0.91707(10) 0.5414(4) 0.0313 1.0000 Uani . . . . . . N1 N -0.1057(3) 1.12776(12) 0.4991(4) 0.0278 1.0000 Uani . . . . . . N2 N 0.2346(2) 1.07654(11) 0.7087(4) 0.0229 1.0000 Uani . . . . . . N3 N 0.5222(3) 0.98078(13) 0.8972(4) 0.0286 1.0000 Uani . . . . . . C1 C -0.0213(5) 0.65684(19) 0.5158(6) 0.0479 1.0000 Uani . . . . . . C2 C -0.0681(5) 0.71675(18) 0.5252(7) 0.0495 1.0000 Uani . . . . . . C3 C -0.0120(4) 0.81656(16) 0.5351(6) 0.0349 1.0000 Uani . . . . . . C4 C 0.1007(3) 0.86135(14) 0.5911(5) 0.0274 1.0000 Uani . . . . . . C5 C 0.1071(3) 0.96788(13) 0.5977(5) 0.0226 1.0000 Uani . . . . . . C6 C 0.0349(3) 1.02025(13) 0.5499(5) 0.0253 1.0000 Uani . . . . . . C7 C 0.1027(3) 1.07359(13) 0.6099(4) 0.0203 1.0000 Uani . . . . . . C8 C 0.0291(3) 1.13096(13) 0.5707(4) 0.0214 1.0000 Uani . . . . . . C9 C -0.1740(3) 1.17917(16) 0.4747(5) 0.0308 1.0000 Uani . . . . . . C10 C -0.1141(4) 1.23398(15) 0.5174(5) 0.0305 1.0000 Uani . . . . . . C11 C 0.0239(3) 1.23700(15) 0.5854(5) 0.0313 1.0000 Uani . . . . . . C12 C 0.0965(3) 1.18477(14) 0.6124(5) 0.0266 1.0000 Uani . . . . . . C13 C 0.3029(3) 1.02530(13) 0.7534(4) 0.0207 1.0000 Uani . . . . . . C14 C 0.4484(3) 1.03048(13) 0.8661(4) 0.0216 1.0000 Uani . . . . . . C15 C 0.5038(3) 1.08534(14) 0.9358(5) 0.0255 1.0000 Uani . . . . . . C16 C 0.6393(3) 1.08955(16) 1.0366(5) 0.0318 1.0000 Uani . . . . . . C17 C 0.7158(3) 1.03862(17) 1.0672(5) 0.0327 1.0000 Uani . . . . . . C18 C 0.6544(3) 0.98547(17) 0.9975(5) 0.0340 1.0000 Uani . . . . . . C19 C 0.2445(3) 0.96947(13) 0.6996(5) 0.0235 1.0000 Uani . . . . . . H1 H 0.0108 0.6041 0.3315 0.0500 1.0000 Uiso R . . . . . H11 H 0.0693 0.6527 0.6160 0.0657 1.0000 Uiso R . . . . . H12 H -0.0845 0.6278 0.5435 0.0657 1.0000 Uiso R . . . . . H21 H -0.1036 0.7205 0.6363 0.0737 1.0000 Uiso R . . . . . H22 H -0.1413 0.7258 0.4010 0.0737 1.0000 Uiso R . . . . . H31 H -0.0697 0.8237 0.3978 0.0456 1.0000 Uiso R . . . . . H32 H -0.0673 0.8206 0.6228 0.0456 1.0000 Uiso R . . . . . H41 H 0.1512 0.8589 0.7333 0.0327 1.0000 Uiso R . . . . . H42 H 0.1637 0.8543 0.5163 0.0327 1.0000 Uiso R . . . . . H61 H -0.0633 1.0195 0.4758 0.0286 1.0000 Uiso R . . . . . H91 H -0.2742 1.1772 0.4236 0.0349 1.0000 Uiso R . . . . . H101 H -0.1697 1.2708 0.4985 0.0367 1.0000 Uiso R . . . . . H111 H 0.0711 1.2761 0.6163 0.0343 1.0000 Uiso R . . . . . H121 H 0.1967 1.1857 0.6601 0.0320 1.0000 Uiso R . . . . . H151 H 0.4458 1.1215 0.9128 0.0299 1.0000 Uiso R . . . . . H161 H 0.6816 1.1287 1.0850 0.0366 1.0000 Uiso R . . . . . H171 H 0.8141 1.0400 1.1407 0.0360 1.0000 Uiso R . . . . . H181 H 0.7102 0.9486 1.0212 0.0385 1.0000 Uiso R . . . . . H191 H 0.2984 0.9321 0.7331 0.0271 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 O1 0.0454(14) 0.0248(12) 0.0360(13) -0.0053(10) 0.0166(11) -0.0065(10) O2 0.0659(18) 0.0196(12) 0.0489(15) -0.0061(11) 0.0301(14) -0.0100(12) O3 0.0253(11) 0.0190(11) 0.0441(14) -0.0059(10) 0.0038(10) -0.0041(9) N1 0.0194(13) 0.0261(14) 0.0336(15) -0.0006(11) 0.0028(11) 0.0013(10) N2 0.0220(13) 0.0191(12) 0.0263(12) -0.0002(10) 0.0062(10) 0.0005(10) N3 0.0247(13) 0.0258(14) 0.0325(14) -0.0013(11) 0.0055(11) 0.0085(11) C1 0.066(3) 0.040(2) 0.047(2) -0.0089(18) 0.030(2) -0.022(2) C2 0.063(3) 0.038(2) 0.061(3) -0.008(2) 0.038(2) -0.0130(19) C3 0.042(2) 0.0239(16) 0.0406(19) -0.0078(14) 0.0157(16) -0.0120(14) C4 0.0280(15) 0.0183(14) 0.0350(17) -0.0020(13) 0.0091(13) -0.0016(12) C5 0.0219(15) 0.0182(14) 0.0277(15) -0.0028(11) 0.0079(13) -0.0045(11) C6 0.0222(15) 0.0228(15) 0.0302(16) -0.0026(13) 0.0074(13) -0.0022(12) C7 0.0162(13) 0.0199(14) 0.0235(14) -0.0012(11) 0.0048(11) -0.0012(11) C8 0.0211(15) 0.0180(14) 0.0230(14) -0.0005(10) 0.0044(12) 0.0006(11) C9 0.0242(15) 0.0329(18) 0.0316(17) 0.0013(14) 0.0038(13) 0.0057(13) C10 0.0328(17) 0.0265(16) 0.0297(16) 0.0022(13) 0.0068(14) 0.0092(14) C11 0.0309(17) 0.0198(15) 0.0380(19) 0.0002(13) 0.0042(14) -0.0011(13) C12 0.0192(14) 0.0250(16) 0.0333(17) 0.0006(13) 0.0057(13) 0.0000(12) C13 0.0167(13) 0.0224(15) 0.0218(14) 0.0012(11) 0.0045(11) 0.0013(11) C14 0.0183(13) 0.0217(14) 0.0229(14) -0.0011(11) 0.0042(11) 0.0004(11) C15 0.0181(14) 0.0237(15) 0.0317(16) -0.0004(12) 0.0043(12) 0.0017(12) C16 0.0287(17) 0.0317(18) 0.0305(18) -0.0049(13) 0.0035(14) -0.0026(14) C17 0.0163(14) 0.046(2) 0.0309(17) -0.0061(15) 0.0005(13) 0.0019(14) C18 0.0259(16) 0.0345(19) 0.0372(19) -0.0014(15) 0.0044(14) 0.0093(14) C19 0.0217(14) 0.0198(14) 0.0262(15) -0.0002(11) 0.0040(12) 0.0007(12) _refine_ls_extinction_coef 42(9) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' _oxford_refine_ls_scale 0.2454(8) 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 O1 . C1 . 1.418(5) yes O1 . H1 . 0.943 no O2 . C2 . 1.469(5) yes O2 . C3 . 1.403(4) yes O3 . C4 . 1.423(4) yes O3 . C5 . 1.362(4) yes N1 . C8 . 1.347(4) yes N1 . C9 . 1.345(4) yes N2 . C7 . 1.343(4) yes N2 . C13 . 1.343(4) yes N3 . C14 . 1.340(4) yes N3 . C18 . 1.351(4) yes C1 . C2 . 1.446(6) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C2 . H21 . 1.000 no C2 . H22 . 1.000 no C3 . C4 . 1.511(5) yes C3 . H31 . 1.000 no C3 . H32 . 1.000 no C4 . H41 . 1.000 no C4 . H42 . 1.000 no C5 . C6 . 1.385(4) yes C5 . C19 . 1.396(4) yes C6 . C7 . 1.393(4) yes C6 . H61 . 1.000 no C7 . C8 . 1.487(4) yes C8 . C12 . 1.388(4) yes C9 . C10 . 1.375(5) yes C9 . H91 . 1.000 no C10 . C11 . 1.379(5) yes C10 . H101 . 1.000 no C11 . C12 . 1.382(5) yes C11 . H111 . 1.000 no C12 . H121 . 1.000 no C13 . C14 . 1.490(4) yes C13 . C19 . 1.399(4) yes C14 . C15 . 1.390(4) yes C15 . C16 . 1.381(4) yes C15 . H151 . 1.000 no C16 . C17 . 1.378(5) yes C16 . H161 . 1.000 no C17 . C18 . 1.377(5) yes C17 . H171 . 1.000 no C18 . H181 . 1.000 no C19 . H191 . 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 C1 . O1 . H1 . 105.757 no C2 . O2 . C3 . 107.7(3) yes C4 . O3 . C5 . 119.0(2) yes C8 . N1 . C9 . 117.2(3) yes C7 . N2 . C13 . 117.9(3) yes C14 . N3 . C18 . 117.8(3) yes O1 . C1 . C2 . 111.0(4) yes O1 . C1 . H11 . 108.915 no C2 . C1 . H11 . 108.186 no O1 . C1 . H12 . 109.423 no C2 . C1 . H12 . 109.826 no H11 . C1 . H12 . 109.467 no O2 . C2 . C1 . 110.0(4) yes O2 . C2 . H21 . 109.706 no C1 . C2 . H21 . 109.977 no O2 . C2 . H22 . 108.908 no C1 . C2 . H22 . 108.732 no H21 . C2 . H22 . 109.467 no O2 . C3 . C4 . 109.3(3) yes O2 . C3 . H31 . 108.942 no C4 . C3 . H31 . 109.319 no O2 . C3 . H32 . 110.012 no C4 . C3 . H32 . 109.801 no H31 . C3 . H32 . 109.467 no C3 . C4 . O3 . 104.1(3) yes C3 . C4 . H41 . 110.425 no O3 . C4 . H41 . 111.271 no C3 . C4 . H42 . 110.579 no O3 . C4 . H42 . 110.932 no H41 . C4 . H42 . 109.467 no O3 . C5 . C6 . 115.5(3) yes O3 . C5 . C19 . 124.3(3) yes C6 . C5 . C19 . 120.1(3) yes C5 . C6 . C7 . 118.1(3) yes C5 . C6 . H61 . 120.557 no C7 . C6 . H61 . 121.327 no C6 . C7 . N2 . 123.1(3) yes C6 . C7 . C8 . 120.4(2) yes N2 . C7 . C8 . 116.4(2) yes C7 . C8 . N1 . 116.6(3) yes C7 . C8 . C12 . 121.2(3) yes N1 . C8 . C12 . 122.2(3) yes N1 . C9 . C10 . 123.8(3) yes N1 . C9 . H91 . 117.843 no C10 . C9 . H91 . 118.391 no C9 . C10 . C11 . 118.6(3) yes C9 . C10 . H101 . 120.566 no C11 . C10 . H101 . 120.800 no C10 . C11 . C12 . 118.7(3) yes C10 . C11 . H111 . 120.906 no C12 . C11 . H111 . 120.388 no C8 . C12 . C11 . 119.4(3) yes C8 . C12 . H121 . 120.196 no C11 . C12 . H121 . 120.351 no N2 . C13 . C14 . 116.2(2) yes N2 . C13 . C19 . 123.5(3) yes C14 . C13 . C19 . 120.3(2) yes C13 . C14 . N3 . 117.7(3) yes C13 . C14 . C15 . 120.4(3) yes N3 . C14 . C15 . 121.9(3) yes C14 . C15 . C16 . 119.6(3) yes C14 . C15 . H151 . 120.124 no C16 . C15 . H151 . 120.270 no C15 . C16 . C17 . 118.6(3) yes C15 . C16 . H161 . 120.908 no C17 . C16 . H161 . 120.456 no C16 . C17 . C18 . 118.9(3) yes C16 . C17 . H171 . 120.714 no C18 . C17 . H171 . 120.361 no C17 . C18 . N3 . 123.1(3) yes C17 . C18 . H181 . 118.583 no N3 . C18 . H181 . 118.335 no C13 . C19 . C5 . 117.2(3) yes C13 . C19 . H191 . 121.602 no C5 . C19 . H191 . 121.148 no # Attachment 'Ligand_V.cif' data_hsc92_173k _database_code_depnum_ccdc_archive 'CCDC 288506' _audit_creation_date 05-10-28 _audit_creation_method CRYSTALS_ver_12.24 _oxford_structure_analysis_title '10281153 hsc92_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 41.930(7) _cell_length_b 5.1238(11) _cell_length_c 9.745(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2093.7(10) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P c a 21 ' _symmetry_space_group_name_Hall 'P 2c -2ac' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x+1/2,y,z+1/2 x+1/2,-y,z -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' 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' 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' 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' _cell_formula_units_Z 4 _chemical_formula_sum 'C25 H20 Cl1 N3 O1 S1' _chemical_formula_moiety 'C25 H18 N3 S, H2 O, Cl' _chemical_compound_source ? _chemical_formula_weight 445.97 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 173 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 0.306 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_absorpt_correction_T_min 0.97 _exptl_absorpt_correction_T_max 0.97 # Sheldrick geometric definitions 0.97 0.97 _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 42258 _reflns_number_total 7178 _diffrn_reflns_av_R_equivalents 0.111 # Number of reflections with Friedels Law is 3947 # Number of reflections without Friedels Law is 7178 # Theoretical number of reflections is about 3639 _diffrn_reflns_theta_min 3.588 _diffrn_reflns_theta_max 32.014 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 32.014 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -61 _diffrn_reflns_limit_h_max 61 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _reflns_limit_h_min 0 _reflns_limit_h_max 61 _reflns_limit_k_min 0 _reflns_limit_k_max 7 _reflns_limit_l_min -14 _reflns_limit_l_max 14 _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 -0.34 _refine_diff_density_max 0.44 _refine_ls_number_reflns 3947 _refine_ls_number_restraints 665 _refine_ls_number_parameters 353 #_refine_ls_R_factor_ref 0.0465 _refine_ls_wR_factor_ref 0.0449 _refine_ls_goodness_of_fit_ref 0.9126 #_reflns_number_all 7143 _refine_ls_R_factor_all 0.1012 _refine_ls_wR_factor_all 0.0621 # 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 3947 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_gt 0.0449 _refine_ls_shift/su_max 0.007648 _refine_ls_abs_structure_Flack -0.02(6) _refine_ls_abs_structure_details 'Flack, 3231 Friedel-pairs' # 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 ad _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 ; p=P(6)*max(Fo^2^,0) + (1-P(6))Fc^2^ Method = SHELXL 97 (Sheldrick, 1997) W = 1. / [Sigma^2^(F*)+(P(1)p)^2^+P(2)p+P(4)+P(5)Sin(theta) ] P(i) are: 0.250E-01 0.00 0.00 0.00 0.00 0.333 ; _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. Sheldrick, G.M. (1997). SHELXL-97. Program for the refinement of crystal structures. Univ. of Gottingen, Federal Republic of Germany. 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 Cl1 Cl 0.452550(17) -0.21248(13) 0.32437(10) 0.0329 1.0000 Uani . . . . . . S1 S 0.371390(19) 0.36473(19) 1.26491(11) 0.0464 1.0000 Uani . . . . . . O1 O 0.43961(5) 0.2868(4) 0.50139(19) 0.0344 1.0000 Uani D . . . . . N1 N 0.45411(5) 0.0434(5) 0.7437(2) 0.0228 1.0000 Uani D . . . . . N2 N 0.41321(4) 0.3958(4) 0.8357(2) 0.0207 1.0000 Uani . . . . . . N3 N 0.35781(5) 0.9294(4) 0.8169(2) 0.0241 1.0000 Uani . . . . . . C1 C 0.33037(7) 0.3969(6) 1.2220(3) 0.0381 1.0000 Uani D U . . . . C6 C 0.21371(8) 0.6218(7) 1.2033(4) 0.0475 1.0000 Uani D U . . . . C11 C 0.47416(7) -0.1222(6) 0.6827(3) 0.0275 1.0000 Uani . . . . . . C12 C 0.49018(6) -0.3034(6) 0.7588(3) 0.0283 1.0000 Uani . . . . . . C13 C 0.48496(6) -0.3115(6) 0.8988(3) 0.0269 1.0000 Uani . . . . . . C14 C 0.46394(6) -0.1395(6) 0.9594(3) 0.0237 1.0000 Uani . . . . . . C15 C 0.44826(6) 0.0406(5) 0.8797(3) 0.0206 1.0000 Uani . . . . . . C16 C 0.42396(6) 0.2291(5) 0.9301(3) 0.0214 1.0000 Uani . . . . . . C17 C 0.41271(6) 0.2147(6) 1.0641(3) 0.0251 1.0000 Uani . . . . . . C18 C 0.38854(7) 0.3837(6) 1.0996(3) 0.0284 1.0000 Uani . . . . . . C19 C 0.37747(6) 0.5620(6) 1.0054(3) 0.0260 1.0000 Uani . . . . . . C20 C 0.39030(6) 0.5614(5) 0.8744(3) 0.0217 1.0000 Uani . . . . . . C21 C 0.37796(5) 0.7474(5) 0.7706(3) 0.0209 1.0000 Uani . . . . . . C22 C 0.38688(7) 0.7294(6) 0.6339(3) 0.0253 1.0000 Uani . . . . . . C23 C 0.37465(7) 0.9069(6) 0.5421(3) 0.0314 1.0000 Uani . . . . . . C24 C 0.35371(7) 1.0950(6) 0.5897(3) 0.0315 1.0000 Uani . . . . . . C25 C 0.34622(6) 1.0983(6) 0.7280(3) 0.0275 1.0000 Uani . . . . . . C2 C 0.31674(14) 0.2740(12) 1.0981(6) 0.0340 0.5000 Uani D U . . . . C3 C 0.28488(14) 0.2993(12) 1.0593(6) 0.0347 0.5000 Uani D U . . . . C4 C 0.26409(17) 0.4422(15) 1.1433(6) 0.0304 0.5000 Uani D U . . . . C5 C 0.23143(16) 0.4784(13) 1.1082(7) 0.0375 0.5000 Uani D U . . . . C7 C 0.22330(14) 0.7291(13) 1.3192(7) 0.0427 0.5000 Uani D U . . . . C8 C 0.25484(12) 0.6974(12) 1.3494(5) 0.0317 0.5000 Uani D U . . . . C9 C 0.27577(15) 0.5594(14) 1.2635(8) 0.0257 0.5000 Uani D U . . . . C10 C 0.30855(14) 0.5329(12) 1.2982(7) 0.0265 0.5000 Uani D U . . . . C52 C 0.31687(16) 0.1934(13) 1.1594(7) 0.0454 0.5000 Uani D U . . . . C53 C 0.28456(15) 0.2084(13) 1.1401(7) 0.0457 0.5000 Uani D U . . . . C54 C 0.26674(17) 0.4183(15) 1.1890(7) 0.0329 0.5000 Uani D U . . . . C55 C 0.23329(16) 0.4210(13) 1.1664(8) 0.0428 0.5000 Uani D U . . . . C57 C 0.23037(14) 0.8274(14) 1.2807(7) 0.0464 0.5000 Uani D U . . . . C58 C 0.26323(14) 0.8325(13) 1.3068(6) 0.0404 0.5000 Uani D U . . . . C59 C 0.28209(17) 0.6247(14) 1.2586(9) 0.0333 0.5000 Uani D U . . . . C60 C 0.31561(15) 0.6154(13) 1.2794(7) 0.0282 0.5000 Uani D U . . . . H1 H 0.4385 0.4391 0.4575 0.0400 1.0000 Uiso DR . . . . . H2 H 0.4413 0.1600 0.4395 0.0400 1.0000 Uiso DR . . . . . H3 H 0.4440 0.1619 0.6912 0.0266 1.0000 Uiso DR . . . . . H21 H 0.3306 0.1711 1.0413 0.0394 0.5000 Uiso R . . . . . H31 H 0.2773 0.2204 0.9760 0.0399 0.5000 Uiso R . . . . . H51 H 0.2223 0.4085 1.0258 0.0409 0.5000 Uiso R . . . . . H61 H 0.1916 0.6474 1.1801 0.0572 1.0000 Uiso R . . . . . H71 H 0.2091 0.8216 1.3788 0.0520 0.5000 Uiso R . . . . . H81 H 0.2632 0.7729 1.4321 0.0375 0.5000 Uiso R . . . . . H101 H 0.3158 0.6154 1.3813 0.0329 0.5000 Uiso R . . . . . H521 H 0.3291 0.0453 1.1295 0.0536 0.5000 Uiso R . . . . . H531 H 0.2739 0.0706 1.0916 0.0534 0.5000 Uiso R . . . . . H551 H 0.2239 0.2697 1.1243 0.0514 0.5000 Uiso R . . . . . H571 H 0.2177 0.9677 1.3168 0.0549 0.5000 Uiso R . . . . . H581 H 0.2726 0.9754 1.3566 0.0494 0.5000 Uiso R . . . . . H601 H 0.3270 0.7461 1.3298 0.0333 0.5000 Uiso R . . . . . H111 H 0.4773 -0.1141 0.5852 0.0330 1.0000 Uiso R . . . . . H121 H 0.5048 -0.4230 0.7162 0.0349 1.0000 Uiso R . . . . . H131 H 0.4961 -0.4373 0.9542 0.0320 1.0000 Uiso R . . . . . H141 H 0.4603 -0.1459 1.0565 0.0290 1.0000 Uiso R . . . . . H171 H 0.4214 0.0927 1.1290 0.0298 1.0000 Uiso R . . . . . H191 H 0.3611 0.6847 1.0298 0.0315 1.0000 Uiso R . . . . . H221 H 0.4013 0.5955 0.6041 0.0300 1.0000 Uiso R . . . . . H231 H 0.3805 0.9003 0.4469 0.0370 1.0000 Uiso R . . . . . H241 H 0.3446 1.2208 0.5279 0.0376 1.0000 Uiso R . . . . . H251 H 0.3318 1.2301 0.7608 0.0329 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 Cl1 0.0436(4) 0.0301(3) 0.0248(3) 0.0031(4) 0.0028(3) 0.0079(3) S1 0.0465(4) 0.0689(6) 0.0237(3) 0.0171(4) 0.0137(4) 0.0295(4) O1 0.0483(12) 0.0321(11) 0.0228(9) 0.0046(9) 0.0068(8) 0.0096(10) N1 0.0226(10) 0.0263(13) 0.0194(12) 0.0041(10) -0.0002(9) 0.0043(10) N2 0.0173(10) 0.0236(10) 0.0213(10) 0.0013(11) -0.0002(9) -0.0014(9) N3 0.0216(10) 0.0267(11) 0.0239(10) 0.0012(12) 0.0010(9) 0.0018(10) C1 0.0382(15) 0.0385(16) 0.0375(15) 0.0157(14) 0.0169(12) 0.0132(14) C6 0.0388(17) 0.0387(18) 0.065(2) 0.0180(17) 0.0128(15) 0.0036(15) C11 0.0308(15) 0.0319(16) 0.0197(12) -0.0033(13) 0.0049(11) 0.0060(13) C12 0.0232(12) 0.0326(17) 0.0292(13) -0.0020(14) 0.0032(13) 0.0054(12) C13 0.0257(13) 0.0279(17) 0.0271(15) 0.0030(13) -0.0056(11) 0.0050(13) C14 0.0200(12) 0.0319(16) 0.0194(12) 0.0020(12) -0.0015(10) 0.0014(13) C15 0.0186(12) 0.0220(15) 0.0214(11) -0.0006(11) -0.0014(10) -0.0003(11) C16 0.0160(11) 0.0276(14) 0.0206(12) 0.0002(11) -0.0019(9) -0.0003(12) C17 0.0263(13) 0.0308(15) 0.0181(11) 0.0049(12) -0.0002(10) 0.0068(12) C18 0.0298(14) 0.0359(16) 0.0195(12) 0.0055(12) 0.0054(11) 0.0025(14) C19 0.0267(13) 0.0282(16) 0.0231(12) 0.0010(12) 0.0032(11) 0.0071(12) C20 0.0180(11) 0.0265(15) 0.0205(11) 0.0018(11) -0.0017(10) 0.0000(12) C21 0.0183(10) 0.0217(13) 0.0228(11) 0.0003(12) -0.0013(10) -0.0011(10) C22 0.0256(14) 0.0257(16) 0.0246(13) 0.0045(12) 0.0047(10) 0.0010(13) C23 0.0365(15) 0.0354(17) 0.0224(13) 0.0101(13) 0.0035(12) 0.0019(15) C24 0.0333(15) 0.0291(16) 0.0322(15) 0.0138(13) -0.0030(12) 0.0048(14) C25 0.0237(13) 0.0246(15) 0.0341(16) 0.0032(13) 0.0009(11) 0.0067(12) C2 0.040(3) 0.024(3) 0.038(3) 0.011(3) 0.014(3) 0.006(3) C3 0.045(3) 0.033(3) 0.026(3) 0.002(3) 0.004(2) 0.000(3) C4 0.038(3) 0.027(3) 0.027(3) 0.007(3) 0.005(3) 0.001(3) C5 0.040(3) 0.031(3) 0.041(3) 0.017(3) -0.007(3) -0.001(3) C7 0.038(3) 0.045(3) 0.044(3) 0.013(3) 0.009(3) 0.010(3) C8 0.035(3) 0.035(3) 0.025(3) -0.005(2) 0.002(2) -0.002(3) C9 0.023(3) 0.025(3) 0.029(3) 0.004(3) 0.009(3) 0.001(3) C10 0.029(3) 0.025(3) 0.026(3) 0.008(3) 0.009(2) -0.006(2) C52 0.047(3) 0.027(3) 0.062(4) 0.012(3) 0.017(3) 0.007(3) C53 0.045(3) 0.040(3) 0.052(3) -0.006(3) 0.008(3) -0.005(3) C54 0.032(3) 0.034(3) 0.033(3) 0.008(3) 0.012(3) 0.001(3) C55 0.039(3) 0.035(3) 0.054(4) 0.011(3) 0.005(3) -0.003(3) C57 0.037(3) 0.057(4) 0.044(3) 0.018(3) 0.020(3) 0.018(3) C58 0.040(3) 0.038(3) 0.043(3) 0.007(3) 0.006(3) 0.011(3) C59 0.037(3) 0.031(3) 0.032(3) 0.010(3) 0.014(3) 0.007(3) C60 0.031(3) 0.034(3) 0.019(3) 0.012(3) 0.011(2) 0.002(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 1.0759(16) 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 . C1 . 1.778(3) yes S1 . C18 . 1.767(3) yes O1 . H1 . 0.891 no O1 . H2 . 0.889 no N1 . C11 . 1.334(3) yes N1 . C15 . 1.348(3) yes N1 . H3 . 0.899 no N2 . C16 . 1.334(3) yes N2 . C20 . 1.336(3) yes N3 . C21 . 1.337(3) yes N3 . C25 . 1.317(3) yes C1 . C2 . 1.477(6) yes C1 . C10 . 1.369(6) yes C1 . C52 . 1.334(6) yes C1 . C60 . 1.397(6) yes C6 . C5 . 1.397(6) yes C6 . C7 . 1.319(6) yes C6 . C55 . 1.365(6) yes C6 . C57 . 1.472(7) yes C6 . H61 . 0.961 no C11 . C12 . 1.365(4) yes C11 . H111 . 0.960 no C12 . C13 . 1.383(4) yes C12 . H121 . 0.960 no C13 . C14 . 1.379(4) yes C13 . H131 . 0.961 no C14 . C15 . 1.374(4) yes C14 . H141 . 0.960 no C15 . C16 . 1.487(4) yes C16 . C17 . 1.390(3) yes C17 . C18 . 1.377(4) yes C17 . H171 . 0.961 no C18 . C19 . 1.376(4) yes C19 . C20 . 1.385(4) yes C19 . H191 . 0.960 no C20 . C21 . 1.483(4) yes C21 . C22 . 1.387(4) yes C22 . C23 . 1.375(4) yes C22 . H221 . 0.960 no C23 . C24 . 1.384(4) yes C23 . H231 . 0.960 no C24 . C25 . 1.384(4) yes C24 . H241 . 0.961 no C25 . H251 . 0.961 no C2 . C3 . 1.394(7) yes C2 . H21 . 0.960 no C3 . C4 . 1.402(7) yes C3 . H31 . 0.961 no C4 . C5 . 1.424(7) yes C4 . C9 . 1.404(7) yes C5 . H51 . 0.959 no C7 . C8 . 1.364(7) yes C7 . H71 . 0.959 no C8 . C9 . 1.404(7) yes C8 . H81 . 0.961 no C9 . C10 . 1.422(7) yes C10 . H101 . 0.962 no C52 . C53 . 1.370(7) yes C52 . H521 . 0.960 no C53 . C54 . 1.394(7) yes C53 . H531 . 0.960 no C54 . C55 . 1.420(7) yes C54 . C59 . 1.412(7) yes C55 . H551 . 0.962 no C57 . C58 . 1.401(7) yes C57 . H571 . 0.961 no C58 . C59 . 1.407(7) yes C58 . H581 . 0.962 no C59 . C60 . 1.421(7) yes C60 . H601 . 0.958 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 C1 . S1 . C18 . 100.02(13) yes H1 . O1 . H2 . 108.597 no C11 . N1 . C15 . 123.1(2) yes C11 . N1 . H3 . 118.133 no C15 . N1 . H3 . 118.772 no C16 . N2 . C20 . 117.1(2) yes C21 . N3 . C25 . 118.0(2) yes S1 . C1 . C2 . 121.8(3) yes S1 . C1 . C10 . 124.5(4) yes C2 . C1 . C10 . 113.7(4) yes S1 . C1 . C52 . 116.5(4) yes S1 . C1 . C60 . 114.1(4) yes C52 . C1 . C60 . 128.4(5) yes C5 . C6 . C7 . 128.7(5) yes C55 . C6 . C57 . 112.9(5) yes C5 . C6 . H61 . 115.311 no C7 . C6 . H61 . 115.988 no C55 . C6 . H61 . 128.318 no C57 . C6 . H61 . 118.659 no N1 . C11 . C12 . 120.0(2) yes N1 . C11 . H111 . 120.032 no C12 . C11 . H111 . 119.946 no C11 . C12 . C13 . 118.6(3) yes C11 . C12 . H121 . 120.831 no C13 . C12 . H121 . 120.546 no C12 . C13 . C14 . 120.3(3) yes C12 . C13 . H131 . 119.835 no C14 . C13 . H131 . 119.894 no C13 . C14 . C15 . 119.6(2) yes C13 . C14 . H141 . 120.200 no C15 . C14 . H141 . 120.229 no C14 . C15 . N1 . 118.4(2) yes C14 . C15 . C16 . 125.3(2) yes N1 . C15 . C16 . 116.3(2) yes C15 . C16 . N2 . 114.8(2) yes C15 . C16 . C17 . 120.5(2) yes N2 . C16 . C17 . 124.5(2) yes C16 . C17 . C18 . 116.9(3) yes C16 . C17 . H171 . 121.602 no C18 . C17 . H171 . 121.492 no S1 . C18 . C17 . 119.6(2) yes S1 . C18 . C19 . 120.5(2) yes C17 . C18 . C19 . 119.8(2) yes C18 . C19 . C20 . 118.9(2) yes C18 . C19 . H191 . 120.657 no C20 . C19 . H191 . 120.476 no C19 . C20 . N2 . 122.7(2) yes C19 . C20 . C21 . 119.5(2) yes N2 . C20 . C21 . 117.8(2) yes C20 . C21 . N3 . 116.0(2) yes C20 . C21 . C22 . 121.2(2) yes N3 . C21 . C22 . 122.7(2) yes C21 . C22 . C23 . 118.7(3) yes C21 . C22 . H221 . 120.543 no C23 . C22 . H221 . 120.750 no C22 . C23 . C24 . 118.6(3) yes C22 . C23 . H231 . 120.674 no C24 . C23 . H231 . 120.680 no C23 . C24 . C25 . 118.6(3) yes C23 . C24 . H241 . 120.627 no C25 . C24 . H241 . 120.759 no C24 . C25 . N3 . 123.3(3) yes C24 . C25 . H251 . 118.398 no N3 . C25 . H251 . 118.332 no C1 . C2 . C3 . 123.5(5) yes C1 . C2 . H21 . 118.174 no C3 . C2 . H21 . 118.277 no C2 . C3 . C4 . 119.1(6) yes C2 . C3 . H31 . 120.338 no C4 . C3 . H31 . 120.568 no C3 . C4 . C5 . 121.7(6) yes C3 . C4 . C9 . 119.6(6) yes C5 . C4 . C9 . 118.7(6) yes C4 . C5 . C6 . 114.9(6) yes C4 . C5 . H51 . 122.606 no C6 . C5 . H51 . 122.536 no C6 . C7 . C8 . 115.5(6) yes C6 . C7 . H71 . 122.338 no C8 . C7 . H71 . 122.145 no C7 . C8 . C9 . 122.5(6) yes C7 . C8 . H81 . 119.139 no C9 . C8 . H81 . 118.365 no C4 . C9 . C8 . 119.6(6) yes C4 . C9 . C10 . 119.6(6) yes C8 . C9 . C10 . 120.7(6) yes C9 . C10 . C1 . 124.4(6) yes C9 . C10 . H101 . 117.545 no C1 . C10 . H101 . 118.009 no C1 . C52 . C53 . 116.0(6) yes C1 . C52 . H521 . 122.013 no C53 . C52 . H521 . 121.955 no C52 . C53 . C54 . 121.8(7) yes C52 . C53 . H531 . 119.230 no C54 . C53 . H531 . 119.008 no C53 . C54 . C55 . 118.9(7) yes C53 . C54 . C59 . 119.9(6) yes C55 . C54 . C59 . 121.2(7) yes C54 . C55 . C6 . 124.1(7) yes C54 . C55 . H551 . 117.595 no C6 . C55 . H551 . 118.280 no C6 . C57 . C58 . 125.0(6) yes C6 . C57 . H571 . 117.461 no C58 . C57 . H571 . 117.559 no C57 . C58 . C59 . 118.5(6) yes C57 . C58 . H581 . 120.443 no C59 . C58 . H581 . 121.007 no C54 . C59 . C58 . 118.1(6) yes C54 . C59 . C60 . 119.6(6) yes C58 . C59 . C60 . 122.3(6) yes C59 . C60 . C1 . 114.1(6) yes C59 . C60 . H601 . 122.921 no C1 . C60 . H601 . 122.990 no # Attachment 'Ru(I)2.cif' data_hsc74_193k _database_code_depnum_ccdc_archive 'CCDC 288507' _audit_creation_date 05-10-26 _audit_creation_method CRYSTALS_ver_12.24 _oxford_structure_analysis_title '2161231 hsc74_193k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 12.5716(7) _cell_length_b 13.6977(16) _cell_length_c 14.845(2) _cell_angle_alpha 85.459(11) _cell_angle_beta 86.045(7) _cell_angle_gamma 76.722(7) _cell_volume 2476.8(5) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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 57.7997 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ru -1.4200 0.8360 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 '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' P 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0140 0.0100 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' _cell_formula_units_Z 2 _chemical_formula_sum 'C54 H41 F12 N7 O2 P2 Ru' _chemical_formula_moiety 'C52 H38 N6 O2 Ru, 2(F6 P), C2 H3 N' _chemical_compound_source ? _chemical_formula_weight 1210.96 _cell_measurement_reflns_used 14117 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_max 0.35 _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.479 _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 0.91 # Sheldrick geometric definitions 0.88 0.91 _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 'USER DEFINED STRUCTURE SOLUTION' _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 62842 _reflns_number_total 14311 _diffrn_reflns_av_R_equivalents 0.072 # Number of reflections with Friedels Law is 14311 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 14446 _diffrn_reflns_theta_min 3.063 _diffrn_reflns_theta_max 29.999 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 29.099 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -17 _reflns_limit_h_max 17 _reflns_limit_k_min -19 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _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 -0.48 _refine_diff_density_max 0.48 _refine_ls_number_reflns 9830 _refine_ls_number_restraints 0 _refine_ls_number_parameters 703 #_refine_ls_R_factor_ref 0.0335 _refine_ls_wR_factor_ref 0.0298 _refine_ls_goodness_of_fit_ref 1.1327 #_reflns_number_all 14250 _refine_ls_R_factor_all 0.0641 _refine_ls_wR_factor_all 0.0483 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 9830 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_gt 0.0298 _refine_ls_shift/su_max 0.001126 # 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: 1.97 -1.05 1.07 ; _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 ; User-defined structure solution reference 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 Ru1 Ru 0.291044(14) 0.184065(13) 0.247769(11) 0.0167 1.0000 Uani . . . . . . N1 N 0.36573(13) 0.06388(12) 0.33322(11) 0.0194 1.0000 Uani . . . . . . N2 N 0.19506(13) 0.20627(12) 0.35929(11) 0.0190 1.0000 Uani . . . . . . N3 N 0.17454(13) 0.30860(12) 0.20689(11) 0.0199 1.0000 Uani . . . . . . N4 N 0.21497(13) 0.09810(12) 0.17685(11) 0.0200 1.0000 Uani . . . . . . N5 N 0.38659(13) 0.16848(12) 0.13627(10) 0.0175 1.0000 Uani . . . . . . N6 N 0.40048(14) 0.27007(13) 0.27078(11) 0.0211 1.0000 Uani . . . . . . N7 N 0.3090(5) 0.3844(3) -0.0852(2) 0.1151 1.0000 Uani . . . . . . C1 C 0.45203(16) -0.01097(16) 0.31415(14) 0.0239 1.0000 Uani . . . . . . C2 C 0.49280(17) -0.08818(16) 0.37663(15) 0.0263 1.0000 Uani . . . . . . C3 C 0.44314(17) -0.09004(16) 0.46229(15) 0.0253 1.0000 Uani . . . . . . C4 C 0.35410(17) -0.01384(15) 0.48347(13) 0.0222 1.0000 Uani . . . . . . C5 C 0.31640(15) 0.06194(14) 0.41857(13) 0.0187 1.0000 Uani . . . . . . C6 C 0.22162(15) 0.14535(15) 0.43419(12) 0.0188 1.0000 Uani . . . . . . C7 C 0.16192(16) 0.16477(15) 0.51506(13) 0.0218 1.0000 Uani . . . . . . C8 C 0.07486(16) 0.24824(16) 0.51759(13) 0.0214 1.0000 Uani . . . . . . C9 C 0.04590(16) 0.30915(15) 0.43945(13) 0.0216 1.0000 Uani . . . . . . C10 C 0.10965(15) 0.28592(15) 0.36052(13) 0.0194 1.0000 Uani . . . . . . C11 C 0.09433(16) 0.34167(15) 0.27174(13) 0.0207 1.0000 Uani . . . . . . C12 C 0.00586(18) 0.41960(17) 0.25200(15) 0.0273 1.0000 Uani . . . . . . C13 C -0.00214(19) 0.46531(18) 0.16592(16) 0.0327 1.0000 Uani . . . . . . C14 C 0.07907(19) 0.43269(18) 0.10073(15) 0.0299 1.0000 Uani . . . . . . C15 C 0.16623(18) 0.35475(16) 0.12355(13) 0.0252 1.0000 Uani . . . . . . C16 C 0.12020(17) 0.07078(16) 0.19855(14) 0.0248 1.0000 Uani . . . . . . C17 C 0.07436(18) 0.01735(18) 0.14305(16) 0.0301 1.0000 Uani . . . . . . C18 C 0.12876(19) -0.01115(18) 0.06225(15) 0.0301 1.0000 Uani . . . . . . C19 C 0.22580(18) 0.01748(16) 0.03765(14) 0.0252 1.0000 Uani . . . . . . C20 C 0.26659(16) 0.07316(15) 0.09505(12) 0.0197 1.0000 Uani . . . . . . C21 C 0.36296(16) 0.11505(14) 0.07044(12) 0.0186 1.0000 Uani . . . . . . C22 C 0.42080(17) 0.11134(15) -0.01196(13) 0.0209 1.0000 Uani . . . . . . C23 C 0.50305(16) 0.16505(15) -0.02671(13) 0.0214 1.0000 Uani . . . . . . C24 C 0.52862(16) 0.21741(15) 0.04219(13) 0.0221 1.0000 Uani . . . . . . C25 C 0.46687(16) 0.21840(15) 0.12330(13) 0.0193 1.0000 Uani . . . . . . C26 C 0.47572(16) 0.27612(15) 0.20084(13) 0.0208 1.0000 Uani . . . . . . C27 C 0.55078(19) 0.33497(19) 0.20313(16) 0.0316 1.0000 Uani . . . . . . C28 C 0.5503(2) 0.3900(2) 0.27690(17) 0.0366 1.0000 Uani . . . . . . C29 C 0.4742(2) 0.38404(19) 0.34748(16) 0.0331 1.0000 Uani . . . . . . C30 C 0.40184(18) 0.32366(17) 0.34258(14) 0.0270 1.0000 Uani . . . . . . C31 C -0.06444(17) 0.35004(16) 0.60697(13) 0.0237 1.0000 Uani . . . . . . C32 C -0.10538(16) 0.35559(16) 0.70421(13) 0.0228 1.0000 Uani . . . . . . C33 C -0.05272(18) 0.29560(16) 0.77278(14) 0.0254 1.0000 Uani . . . . . . C34 C -0.09381(18) 0.30543(16) 0.86373(14) 0.0262 1.0000 Uani . . . . . . C35 C -0.0397(2) 0.24675(19) 0.93610(16) 0.0361 1.0000 Uani . . . . . . C36 C -0.0793(3) 0.2597(2) 1.02353(17) 0.0433 1.0000 Uani . . . . . . C37 C -0.1752(2) 0.3319(2) 1.04223(16) 0.0428 1.0000 Uani . . . . . . C38 C -0.2302(2) 0.3891(2) 0.97451(16) 0.0373 1.0000 Uani . . . . . . C39 C -0.19169(19) 0.37819(17) 0.88265(15) 0.0287 1.0000 Uani . . . . . . C40 C -0.24435(19) 0.43801(18) 0.81057(16) 0.0315 1.0000 Uani . . . . . . C41 C -0.20286(18) 0.42741(17) 0.72375(15) 0.0284 1.0000 Uani . . . . . . C42 C 0.62348(19) 0.23126(18) -0.13342(14) 0.0287 1.0000 Uani . . . . . . C43 C 0.64639(17) 0.23613(16) -0.23339(14) 0.0242 1.0000 Uani . . . . . . C44 C 0.57532(18) 0.30518(17) -0.28957(15) 0.0279 1.0000 Uani . . . . . . C45 C 0.59735(18) 0.31356(17) -0.38053(15) 0.0282 1.0000 Uani . . . . . . C46 C 0.69087(17) 0.25113(16) -0.42063(14) 0.0240 1.0000 Uani . . . . . . C47 C 0.7150(2) 0.25680(18) -0.51502(15) 0.0310 1.0000 Uani . . . . . . C48 C 0.8046(2) 0.1940(2) -0.55259(16) 0.0363 1.0000 Uani . . . . . . C49 C 0.8746(2) 0.12399(19) -0.49775(17) 0.0357 1.0000 Uani . . . . . . C50 C 0.85530(19) 0.11698(17) -0.40626(16) 0.0306 1.0000 Uani . . . . . . C51 C 0.76220(17) 0.17997(16) -0.36516(14) 0.0227 1.0000 Uani . . . . . . C52 C 0.73796(17) 0.17534(16) -0.27084(14) 0.0236 1.0000 Uani . . . . . . C53 C 0.2735(4) 0.2582(3) -0.1905(3) 0.0745 1.0000 Uani . . . . . . C54 C 0.2913(3) 0.3295(3) -0.1322(2) 0.0612 1.0000 Uani . . . . . . O1 O 0.02330(12) 0.26349(11) 0.59915(9) 0.0249 1.0000 Uani . . . . . . O2 O 0.55078(13) 0.16328(12) -0.11093(10) 0.0273 1.0000 Uani . . . . . . P1 P 0.26690(5) 0.44145(4) 0.58244(4) 0.0279 1.0000 Uani . . . . . . P2 P 0.75432(5) 0.02872(5) 0.22796(4) 0.0299 1.0000 Uani . . . . . . F1 F 0.36904(13) 0.48168(13) 0.53726(13) 0.0542 1.0000 Uani . . . . . . F2 F 0.16541(13) 0.40211(13) 0.62864(12) 0.0495 1.0000 Uani . . . . . . F3 F 0.31731(15) 0.43477(13) 0.67820(11) 0.0520 1.0000 Uani . . . . . . F4 F 0.21827(17) 0.44773(15) 0.48561(12) 0.0631 1.0000 Uani . . . . . . F5 F 0.20318(13) 0.55418(11) 0.59643(12) 0.0485 1.0000 Uani . . . . . . F6 F 0.33080(14) 0.32899(12) 0.56752(12) 0.0522 1.0000 Uani . . . . . . F7 F 0.73118(14) -0.06082(14) 0.29586(10) 0.0529 1.0000 Uani . . . . . . F8 F 0.77588(18) 0.11614(15) 0.15837(14) 0.0689 1.0000 Uani . . . . . . F9 F 0.65539(11) 0.01745(13) 0.16997(9) 0.0412 1.0000 Uani . . . . . . F10 F 0.85362(14) 0.03681(17) 0.28527(13) 0.0653 1.0000 Uani . . . . . . F11 F 0.83614(12) -0.05098(12) 0.16800(10) 0.0421 1.0000 Uani . . . . . . F12 F 0.67155(14) 0.10637(14) 0.28758(12) 0.0577 1.0000 Uani . . . . . . H11 H 0.4865 -0.0103 0.2544 0.0276 1.0000 Uiso R . . . . . H21 H 0.5550 -0.1401 0.3604 0.0315 1.0000 Uiso R . . . . . H31 H 0.4701 -0.1434 0.5066 0.0306 1.0000 Uiso R . . . . . H41 H 0.3185 -0.0132 0.5428 0.0265 1.0000 Uiso R . . . . . H71 H 0.1805 0.1216 0.5685 0.0257 1.0000 Uiso R . . . . . H91 H -0.0159 0.3654 0.4403 0.0249 1.0000 Uiso R . . . . . H121 H -0.0497 0.4416 0.2983 0.0303 1.0000 Uiso R . . . . . H131 H -0.0636 0.5190 0.1513 0.0374 1.0000 Uiso R . . . . . H141 H 0.0753 0.4638 0.0404 0.0337 1.0000 Uiso R . . . . . H151 H 0.2230 0.3325 0.0782 0.0291 1.0000 Uiso R . . . . . H161 H 0.0824 0.0897 0.2552 0.0289 1.0000 Uiso R . . . . . H171 H 0.0057 0.0001 0.1607 0.0353 1.0000 Uiso R . . . . . H181 H 0.0998 -0.0506 0.0236 0.0364 1.0000 Uiso R . . . . . H191 H 0.2645 -0.0007 -0.0188 0.0303 1.0000 Uiso R . . . . . H221 H 0.4051 0.0725 -0.0584 0.0237 1.0000 Uiso R . . . . . H241 H 0.5874 0.2518 0.0339 0.0259 1.0000 Uiso R . . . . . H271 H 0.6032 0.3373 0.1533 0.0381 1.0000 Uiso R . . . . . H281 H 0.6018 0.4317 0.2791 0.0456 1.0000 Uiso R . . . . . H291 H 0.4716 0.4221 0.3995 0.0399 1.0000 Uiso R . . . . . H301 H 0.3503 0.3188 0.3926 0.0316 1.0000 Uiso R . . . . . H311 H -0.0386 0.4093 0.5872 0.0281 1.0000 Uiso R . . . . . H312 H -0.1225 0.3448 0.5702 0.0281 1.0000 Uiso R . . . . . H331 H 0.0126 0.2458 0.7591 0.0306 1.0000 Uiso R . . . . . H351 H 0.0260 0.1970 0.9238 0.0423 1.0000 Uiso R . . . . . H361 H -0.0411 0.2191 1.0721 0.0511 1.0000 Uiso R . . . . . H371 H -0.2018 0.3403 1.1040 0.0527 1.0000 Uiso R . . . . . H381 H -0.2963 0.4377 0.9887 0.0470 1.0000 Uiso R . . . . . H401 H -0.3105 0.4873 0.8227 0.0364 1.0000 Uiso R . . . . . H411 H -0.2400 0.4691 0.6752 0.0324 1.0000 Uiso R . . . . . H421 H 0.6909 0.2065 -0.1038 0.0371 1.0000 Uiso R . . . . . H422 H 0.5893 0.2969 -0.1141 0.0371 1.0000 Uiso R . . . . . H441 H 0.5106 0.3471 -0.2633 0.0325 1.0000 Uiso R . . . . . H451 H 0.5490 0.3622 -0.4178 0.0328 1.0000 Uiso R . . . . . H471 H 0.6677 0.3054 -0.5531 0.0387 1.0000 Uiso R . . . . . H481 H 0.8197 0.1985 -0.6169 0.0454 1.0000 Uiso R . . . . . H491 H 0.9370 0.0798 -0.5250 0.0437 1.0000 Uiso R . . . . . H501 H 0.9047 0.0691 -0.3692 0.0364 1.0000 Uiso R . . . . . H521 H 0.7865 0.1285 -0.2322 0.0285 1.0000 Uiso R . . . . . H531 H 0.3440 0.2284 -0.2173 0.0871 1.0000 Uiso R . . . . . H532 H 0.2459 0.2080 -0.1533 0.0871 1.0000 Uiso R . . . . . H533 H 0.2237 0.2875 -0.2365 0.0871 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 Ru1 0.01654(7) 0.01953(7) 0.01337(6) -0.00132(5) 0.00298(5) -0.00395(5) N1 0.0182(7) 0.0215(8) 0.0184(7) -0.0025(6) 0.0024(6) -0.0047(6) N2 0.0189(8) 0.0209(8) 0.0165(7) -0.0005(6) 0.0015(6) -0.0043(6) N3 0.0205(8) 0.0223(8) 0.0178(7) -0.0014(6) 0.0014(6) -0.0072(6) N4 0.0186(8) 0.0208(8) 0.0192(8) 0.0007(6) 0.0012(6) -0.0031(6) N5 0.0174(8) 0.0186(8) 0.0167(7) -0.0016(6) 0.0016(6) -0.0051(6) N6 0.0225(8) 0.0223(8) 0.0173(7) -0.0032(6) -0.0005(6) -0.0021(7) N7 0.198(5) 0.070(2) 0.057(2) -0.0207(18) -0.009(3) 0.018(3) C1 0.0201(9) 0.0268(10) 0.0245(10) -0.0047(8) 0.0039(8) -0.0052(8) C2 0.0204(10) 0.0232(10) 0.0344(11) -0.0034(8) -0.0003(8) -0.0030(8) C3 0.0255(10) 0.0219(10) 0.0297(10) 0.0019(8) -0.0064(8) -0.0073(8) C4 0.0231(9) 0.0253(10) 0.0201(9) 0.0001(7) -0.0015(7) -0.0094(8) C5 0.0172(8) 0.0202(9) 0.0193(9) -0.0030(7) 0.0014(7) -0.0058(7) C6 0.0185(9) 0.0217(9) 0.0165(8) -0.0016(7) 0.0009(7) -0.0057(7) C7 0.0227(9) 0.0258(10) 0.0160(8) -0.0002(7) 0.0021(7) -0.0051(8) C8 0.0226(9) 0.0263(10) 0.0160(8) -0.0044(7) 0.0053(7) -0.0079(8) C9 0.0177(9) 0.0243(10) 0.0215(9) -0.0026(7) 0.0029(7) -0.0030(7) C10 0.0180(9) 0.0218(9) 0.0181(8) -0.0016(7) 0.0019(7) -0.0047(7) C11 0.0211(9) 0.0227(9) 0.0181(9) -0.0015(7) 0.0007(7) -0.0049(7) C12 0.0240(10) 0.0275(11) 0.0279(10) 0.0000(8) 0.0010(8) -0.0021(8) C13 0.0296(11) 0.0312(12) 0.0337(12) 0.0047(9) -0.0046(9) -0.0008(9) C14 0.0305(11) 0.0341(12) 0.0233(10) 0.0086(9) -0.0038(8) -0.0061(9) C15 0.0281(10) 0.0302(11) 0.0176(9) 0.0012(8) 0.0015(8) -0.0088(9) C16 0.0200(9) 0.0285(10) 0.0249(10) 0.0032(8) 0.0043(8) -0.0068(8) C17 0.0209(10) 0.0369(12) 0.0341(11) 0.0034(9) -0.0018(8) -0.0119(9) C18 0.0302(11) 0.0356(12) 0.0292(11) -0.0010(9) -0.0053(9) -0.0163(10) C19 0.0266(10) 0.0293(11) 0.0222(9) -0.0016(8) -0.0016(8) -0.0113(9) C20 0.0200(9) 0.0225(9) 0.0167(8) 0.0005(7) 0.0005(7) -0.0061(7) C21 0.0197(9) 0.0185(9) 0.0173(8) -0.0008(7) 0.0013(7) -0.0043(7) C22 0.0256(10) 0.0209(9) 0.0166(8) -0.0040(7) 0.0024(7) -0.0063(8) C23 0.0216(9) 0.0240(10) 0.0177(9) -0.0024(7) 0.0068(7) -0.0053(8) C24 0.0208(9) 0.0260(10) 0.0211(9) -0.0043(8) 0.0043(7) -0.0088(8) C25 0.0186(9) 0.0215(9) 0.0178(8) -0.0024(7) 0.0014(7) -0.0048(7) C26 0.0206(9) 0.0234(9) 0.0183(9) -0.0033(7) 0.0005(7) -0.0046(7) C27 0.0274(11) 0.0413(13) 0.0307(11) -0.0088(10) 0.0032(9) -0.0168(10) C28 0.0386(13) 0.0413(14) 0.0372(13) -0.0105(11) -0.0025(10) -0.0211(11) C29 0.0343(12) 0.0371(13) 0.0300(11) -0.0136(10) -0.0040(9) -0.0076(10) C30 0.0294(11) 0.0312(11) 0.0199(9) -0.0074(8) -0.0001(8) -0.0042(9) C31 0.0217(9) 0.0279(10) 0.0204(9) -0.0037(8) 0.0064(7) -0.0045(8) C32 0.0214(9) 0.0270(10) 0.0215(9) -0.0071(8) 0.0061(7) -0.0090(8) C33 0.0259(10) 0.0272(10) 0.0238(10) -0.0069(8) 0.0050(8) -0.0077(8) C34 0.0330(11) 0.0258(10) 0.0230(10) -0.0041(8) 0.0028(8) -0.0135(9) C35 0.0441(14) 0.0350(13) 0.0294(11) -0.0011(9) 0.0011(10) -0.0108(11) C36 0.0589(17) 0.0488(16) 0.0241(11) 0.0018(11) -0.0024(11) -0.0173(13) C37 0.0541(16) 0.0571(17) 0.0229(11) -0.0100(11) 0.0105(11) -0.0256(14) C38 0.0410(13) 0.0472(14) 0.0286(11) -0.0143(10) 0.0157(10) -0.0211(11) C39 0.0319(11) 0.0317(11) 0.0267(10) -0.0110(9) 0.0095(9) -0.0159(9) C40 0.0263(11) 0.0342(12) 0.0330(11) -0.0124(9) 0.0084(9) -0.0042(9) C41 0.0257(11) 0.0300(11) 0.0282(11) -0.0068(9) 0.0040(8) -0.0036(9) C42 0.0324(11) 0.0333(11) 0.0242(10) -0.0052(9) 0.0094(8) -0.0170(9) C43 0.0264(10) 0.0266(10) 0.0223(9) -0.0027(8) 0.0056(8) -0.0133(8) C44 0.0224(10) 0.0275(11) 0.0336(11) -0.0037(9) 0.0035(8) -0.0062(8) C45 0.0258(10) 0.0289(11) 0.0295(11) 0.0026(9) -0.0019(8) -0.0069(9) C46 0.0258(10) 0.0281(10) 0.0217(9) 0.0008(8) -0.0011(8) -0.0142(8) C47 0.0390(13) 0.0369(12) 0.0217(10) 0.0025(9) -0.0040(9) -0.0186(10) C48 0.0478(14) 0.0460(14) 0.0220(10) -0.0084(10) 0.0089(10) -0.0258(12) C49 0.0362(13) 0.0381(13) 0.0346(12) -0.0118(10) 0.0153(10) -0.0139(10) C50 0.0289(11) 0.0293(11) 0.0321(11) -0.0041(9) 0.0075(9) -0.0054(9) C51 0.0230(10) 0.0241(10) 0.0222(9) -0.0023(7) 0.0027(7) -0.0088(8) C52 0.0244(10) 0.0249(10) 0.0219(9) 0.0021(8) 0.0018(8) -0.0087(8) C53 0.087(3) 0.067(2) 0.075(3) 0.030(2) -0.029(2) -0.034(2) C54 0.074(2) 0.0521(19) 0.0412(16) 0.0067(14) 0.0083(15) 0.0122(17) O1 0.0251(7) 0.0296(8) 0.0165(6) -0.0031(6) 0.0081(5) -0.0015(6) O2 0.0339(8) 0.0332(8) 0.0191(7) -0.0070(6) 0.0112(6) -0.0180(7) P1 0.0240(3) 0.0292(3) 0.0296(3) -0.0027(2) 0.0006(2) -0.0043(2) P2 0.0269(3) 0.0410(3) 0.0223(3) -0.0064(2) 0.0014(2) -0.0080(2) F1 0.0395(9) 0.0469(9) 0.0702(11) 0.0019(8) 0.0238(8) -0.0074(7) F2 0.0369(8) 0.0520(10) 0.0650(11) -0.0060(8) 0.0068(7) -0.0235(7) F3 0.0644(11) 0.0584(10) 0.0421(9) 0.0031(8) -0.0195(8) -0.0294(9) F4 0.0734(13) 0.0719(13) 0.0399(9) -0.0013(9) -0.0207(9) -0.0038(10) F5 0.0389(8) 0.0323(8) 0.0674(11) -0.0039(7) 0.0165(8) 0.0006(6) F6 0.0546(10) 0.0324(8) 0.0649(11) -0.0090(7) -0.0009(8) 0.0013(7) F7 0.0563(10) 0.0639(11) 0.0330(8) 0.0134(7) 0.0036(7) -0.0097(9) F8 0.0825(14) 0.0560(11) 0.0726(13) 0.0127(10) 0.0115(11) -0.0352(10) F9 0.0300(7) 0.0663(10) 0.0279(7) -0.0059(7) -0.0031(6) -0.0110(7) F10 0.0414(9) 0.1042(16) 0.0569(11) -0.0424(11) -0.0082(8) -0.0160(10) F11 0.0312(7) 0.0584(10) 0.0364(8) -0.0188(7) 0.0063(6) -0.0066(7) F12 0.0489(10) 0.0663(12) 0.0537(10) -0.0309(9) 0.0027(8) 0.0035(8) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.9545(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 Ru1 . N1 . 2.0796(17) yes Ru1 . N2 . 1.9812(16) yes Ru1 . N3 . 2.0578(17) yes Ru1 . N4 . 2.0645(17) yes Ru1 . N5 . 1.9728(16) yes Ru1 . N6 . 2.0664(17) yes N1 . C1 . 1.342(3) yes N1 . C5 . 1.373(2) yes N2 . C6 . 1.349(2) yes N2 . C10 . 1.344(2) yes N3 . C11 . 1.369(2) yes N3 . C15 . 1.343(3) yes N4 . C16 . 1.340(3) yes N4 . C20 . 1.367(2) yes N5 . C21 . 1.354(2) yes N5 . C25 . 1.339(2) yes N6 . C26 . 1.366(2) yes N6 . C30 . 1.344(3) yes N7 . C54 . 1.132(5) yes C1 . C2 . 1.379(3) yes C1 . H11 . 0.960 no C2 . C3 . 1.378(3) yes C2 . H21 . 0.960 no C3 . C4 . 1.381(3) yes C3 . H31 . 0.960 no C4 . C5 . 1.382(3) yes C4 . H41 . 0.960 no C5 . C6 . 1.469(3) yes C6 . C7 . 1.382(3) yes C7 . C8 . 1.390(3) yes C7 . H71 . 0.960 no C8 . C9 . 1.393(3) yes C8 . O1 . 1.341(2) yes C9 . C10 . 1.389(3) yes C9 . H91 . 0.960 no C10 . C11 . 1.471(3) yes C11 . C12 . 1.383(3) yes C12 . C13 . 1.377(3) yes C12 . H121 . 0.960 no C13 . C14 . 1.379(3) yes C13 . H131 . 0.960 no C14 . C15 . 1.383(3) yes C14 . H141 . 0.960 no C15 . H151 . 0.960 no C16 . C17 . 1.379(3) yes C16 . H161 . 0.960 no C17 . C18 . 1.377(3) yes C17 . H171 . 0.960 no C18 . C19 . 1.382(3) yes C18 . H181 . 0.960 no C19 . C20 . 1.383(3) yes C19 . H191 . 0.960 no C20 . C21 . 1.468(3) yes C21 . C22 . 1.378(3) yes C22 . C23 . 1.397(3) yes C22 . H221 . 0.960 no C23 . C24 . 1.390(3) yes C23 . O2 . 1.348(2) yes C24 . C25 . 1.386(3) yes C24 . H241 . 0.960 no C25 . C26 . 1.471(3) yes C26 . C27 . 1.378(3) yes C27 . C28 . 1.377(3) yes C27 . H271 . 0.960 no C28 . C29 . 1.379(3) yes C28 . H281 . 0.960 no C29 . C30 . 1.372(3) yes C29 . H291 . 0.960 no C30 . H301 . 0.960 no C31 . C32 . 1.501(3) yes C31 . O1 . 1.428(2) yes C31 . H311 . 0.960 no C31 . H312 . 0.960 no C32 . C33 . 1.364(3) yes C32 . C41 . 1.413(3) yes C33 . C34 . 1.417(3) yes C33 . H331 . 0.960 no C34 . C35 . 1.406(3) yes C34 . C39 . 1.421(3) yes C35 . C36 . 1.367(3) yes C35 . H351 . 0.960 no C36 . C37 . 1.400(4) yes C36 . H361 . 0.960 no C37 . C38 . 1.351(4) yes C37 . H371 . 0.960 no C38 . C39 . 1.423(3) yes C38 . H381 . 0.960 no C39 . C40 . 1.402(3) yes C40 . C41 . 1.362(3) yes C40 . H401 . 0.960 no C41 . H411 . 0.960 no C42 . C43 . 1.491(3) yes C42 . O2 . 1.454(2) yes C42 . H421 . 0.960 no C42 . H422 . 0.960 no C43 . C44 . 1.406(3) yes C43 . C52 . 1.368(3) yes C44 . C45 . 1.361(3) yes C44 . H441 . 0.960 no C45 . C46 . 1.411(3) yes C45 . H451 . 0.960 no C46 . C47 . 1.413(3) yes C46 . C51 . 1.416(3) yes C47 . C48 . 1.365(4) yes C47 . H471 . 0.960 no C48 . C49 . 1.395(4) yes C48 . H481 . 0.960 no C49 . C50 . 1.363(3) yes C49 . H491 . 0.960 no C50 . C51 . 1.417(3) yes C50 . H501 . 0.960 no C51 . C52 . 1.412(3) yes C52 . H521 . 0.960 no C53 . C54 . 1.419(5) yes C53 . H531 . 0.960 no C53 . H532 . 0.960 no C53 . H533 . 0.960 no P1 . F1 . 1.5969(16) yes P1 . F2 . 1.5891(16) yes P1 . F3 . 1.5837(16) yes P1 . F4 . 1.5888(18) yes P1 . F5 . 1.5903(16) yes P1 . F6 . 1.5900(16) yes P2 . F7 . 1.5914(17) yes P2 . F8 . 1.5778(19) yes P2 . F9 . 1.6028(15) yes P2 . F10 . 1.5872(17) yes P2 . F11 . 1.5981(15) yes P2 . F12 . 1.5846(16) yes 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 . Ru1 . N2 . 78.74(7) yes N1 . Ru1 . N3 . 157.33(6) yes N2 . Ru1 . N3 . 78.70(7) yes N1 . Ru1 . N4 . 94.28(7) yes N2 . Ru1 . N4 . 102.55(7) yes N3 . Ru1 . N4 . 88.47(7) yes N1 . Ru1 . N5 . 103.08(7) yes N2 . Ru1 . N5 . 177.41(7) yes N3 . Ru1 . N5 . 99.54(7) yes N4 . Ru1 . N5 . 79.23(7) yes N1 . Ru1 . N6 . 93.53(7) yes N2 . Ru1 . N6 . 99.49(7) yes N3 . Ru1 . N6 . 92.33(7) yes N4 . Ru1 . N6 . 157.66(6) yes N5 . Ru1 . N6 . 78.62(7) yes Ru1 . N1 . C1 . 128.22(13) yes Ru1 . N1 . C5 . 113.92(13) yes C1 . N1 . C5 . 117.84(17) yes Ru1 . N2 . C6 . 119.14(13) yes Ru1 . N2 . C10 . 119.22(13) yes C6 . N2 . C10 . 121.47(16) yes Ru1 . N3 . C11 . 114.56(13) yes Ru1 . N3 . C15 . 126.92(14) yes C11 . N3 . C15 . 118.37(18) yes Ru1 . N4 . C16 . 128.22(14) yes Ru1 . N4 . C20 . 113.71(13) yes C16 . N4 . C20 . 117.91(18) yes Ru1 . N5 . C21 . 119.01(13) yes Ru1 . N5 . C25 . 119.65(13) yes C21 . N5 . C25 . 121.03(16) yes Ru1 . N6 . C26 . 114.16(13) yes Ru1 . N6 . C30 . 127.98(14) yes C26 . N6 . C30 . 117.74(18) yes N1 . C1 . C2 . 122.75(19) yes N1 . C1 . H11 . 118.231 no C2 . C1 . H11 . 119.020 no C1 . C2 . C3 . 119.34(19) yes C1 . C2 . H21 . 120.155 no C3 . C2 . H21 . 120.500 no C2 . C3 . C4 . 118.95(19) yes C2 . C3 . H31 . 120.529 no C4 . C3 . H31 . 120.523 no C3 . C4 . C5 . 119.54(19) yes C3 . C4 . H41 . 120.517 no C5 . C4 . H41 . 119.942 no C4 . C5 . N1 . 121.58(18) yes C4 . C5 . C6 . 123.58(17) yes N1 . C5 . C6 . 114.84(17) yes C5 . C6 . N2 . 113.13(16) yes C5 . C6 . C7 . 126.58(18) yes N2 . C6 . C7 . 120.29(18) yes C6 . C7 . C8 . 118.73(18) yes C6 . C7 . H71 . 120.562 no C8 . C7 . H71 . 120.702 no C7 . C8 . C9 . 120.67(17) yes C7 . C8 . O1 . 115.00(18) yes C9 . C8 . O1 . 124.33(18) yes C8 . C9 . C10 . 117.70(18) yes C8 . C9 . H91 . 121.034 no C10 . C9 . H91 . 121.263 no C9 . C10 . N2 . 121.08(18) yes C9 . C10 . C11 . 126.19(18) yes N2 . C10 . C11 . 112.73(16) yes C10 . C11 . N3 . 114.51(17) yes C10 . C11 . C12 . 124.39(18) yes N3 . C11 . C12 . 121.08(18) yes C11 . C12 . C13 . 119.8(2) yes C11 . C12 . H121 . 119.871 no C13 . C12 . H121 . 120.291 no C12 . C13 . C14 . 119.2(2) yes C12 . C13 . H131 . 120.528 no C14 . C13 . H131 . 120.316 no C13 . C14 . C15 . 119.0(2) yes C13 . C14 . H141 . 120.480 no C15 . C14 . H141 . 120.473 no C14 . C15 . N3 . 122.51(19) yes C14 . C15 . H151 . 118.900 no N3 . C15 . H151 . 118.593 no N4 . C16 . C17 . 122.96(19) yes N4 . C16 . H161 . 118.352 no C17 . C16 . H161 . 118.686 no C16 . C17 . C18 . 119.0(2) yes C16 . C17 . H171 . 120.404 no C18 . C17 . H171 . 120.602 no C17 . C18 . C19 . 119.1(2) yes C17 . C18 . H181 . 120.444 no C19 . C18 . H181 . 120.411 no C18 . C19 . C20 . 119.3(2) yes C18 . C19 . H191 . 120.562 no C20 . C19 . H191 . 120.116 no C19 . C20 . N4 . 121.59(18) yes C19 . C20 . C21 . 122.87(17) yes N4 . C20 . C21 . 115.41(17) yes C20 . C21 . N5 . 112.58(16) yes C20 . C21 . C22 . 126.59(18) yes N5 . C21 . C22 . 120.58(18) yes C21 . C22 . C23 . 118.72(18) yes C21 . C22 . H221 . 120.773 no C23 . C22 . H221 . 120.504 no C22 . C23 . C24 . 120.18(17) yes C22 . C23 . O2 . 115.19(18) yes C24 . C23 . O2 . 124.61(18) yes C23 . C24 . C25 . 118.07(18) yes C23 . C24 . H241 . 121.005 no C25 . C24 . H241 . 120.928 no C24 . C25 . N5 . 121.35(18) yes C24 . C25 . C26 . 125.84(18) yes N5 . C25 . C26 . 112.72(16) yes C25 . C26 . N6 . 114.73(17) yes C25 . C26 . C27 . 123.67(18) yes N6 . C26 . C27 . 121.57(18) yes C26 . C27 . C28 . 119.8(2) yes C26 . C27 . H271 . 119.801 no C28 . C27 . H271 . 120.354 no C27 . C28 . C29 . 118.6(2) yes C27 . C28 . H281 . 120.604 no C29 . C28 . H281 . 120.774 no C28 . C29 . C30 . 119.5(2) yes C28 . C29 . H291 . 120.358 no C30 . C29 . H291 . 120.177 no C29 . C30 . N6 . 122.8(2) yes C29 . C30 . H301 . 118.895 no N6 . C30 . H301 . 118.344 no C32 . C31 . O1 . 108.74(17) yes C32 . C31 . H311 . 109.681 no O1 . C31 . H311 . 109.543 no C32 . C31 . H312 . 109.793 no O1 . C31 . H312 . 109.604 no H311 . C31 . H312 . 109.467 no C31 . C32 . C33 . 123.08(18) yes C31 . C32 . C41 . 117.19(19) yes C33 . C32 . C41 . 119.74(19) yes C32 . C33 . C34 . 120.7(2) yes C32 . C33 . H331 . 119.534 no C34 . C33 . H331 . 119.724 no C33 . C34 . C35 . 122.1(2) yes C33 . C34 . C39 . 119.0(2) yes C35 . C34 . C39 . 118.9(2) yes C34 . C35 . C36 . 121.0(2) yes C34 . C35 . H351 . 119.306 no C36 . C35 . H351 . 119.694 no C35 . C36 . C37 . 120.1(3) yes C35 . C36 . H361 . 119.838 no C37 . C36 . H361 . 120.017 no C36 . C37 . C38 . 120.7(2) yes C36 . C37 . H371 . 119.177 no C38 . C37 . H371 . 120.151 no C37 . C38 . C39 . 121.0(2) yes C37 . C38 . H381 . 119.432 no C39 . C38 . H381 . 119.612 no C38 . C39 . C34 . 118.4(2) yes C38 . C39 . C40 . 122.8(2) yes C34 . C39 . C40 . 118.79(19) yes C39 . C40 . C41 . 121.0(2) yes C39 . C40 . H401 . 119.366 no C41 . C40 . H401 . 119.616 no C32 . C41 . C40 . 120.7(2) yes C32 . C41 . H411 . 119.457 no C40 . C41 . H411 . 119.883 no C43 . C42 . O2 . 108.42(17) yes C43 . C42 . H421 . 109.423 no O2 . C42 . H421 . 109.694 no C43 . C42 . H422 . 110.076 no O2 . C42 . H422 . 109.741 no H421 . C42 . H422 . 109.467 no C42 . C43 . C44 . 120.1(2) yes C42 . C43 . C52 . 120.3(2) yes C44 . C43 . C52 . 119.59(19) yes C43 . C44 . C45 . 120.9(2) yes C43 . C44 . H441 . 119.459 no C45 . C44 . H441 . 119.658 no C44 . C45 . C46 . 120.5(2) yes C44 . C45 . H451 . 119.863 no C46 . C45 . H451 . 119.678 no C45 . C46 . C47 . 121.8(2) yes C45 . C46 . C51 . 119.32(19) yes C47 . C46 . C51 . 118.8(2) yes C46 . C47 . C48 . 120.8(2) yes C46 . C47 . H471 . 119.429 no C48 . C47 . H471 . 119.750 no C47 . C48 . C49 . 120.2(2) yes C47 . C48 . H481 . 119.809 no C49 . C48 . H481 . 120.028 no C48 . C49 . C50 . 121.0(2) yes C48 . C49 . H491 . 119.385 no C50 . C49 . H491 . 119.663 no C49 . C50 . C51 . 120.4(2) yes C49 . C50 . H501 . 120.099 no C51 . C50 . H501 . 119.532 no C50 . C51 . C46 . 118.84(19) yes C50 . C51 . C52 . 122.7(2) yes C46 . C51 . C52 . 118.49(19) yes C51 . C52 . C43 . 121.2(2) yes C51 . C52 . H521 . 119.425 no C43 . C52 . H521 . 119.349 no C54 . C53 . H531 . 106.232 no C54 . C53 . H532 . 107.107 no H531 . C53 . H532 . 109.467 no C54 . C53 . H533 . 113.048 no H531 . C53 . H533 . 110.413 no H532 . C53 . H533 . 110.412 no C53 . C54 . N7 . 177.6(4) yes C31 . O1 . C8 . 117.76(16) yes C42 . O2 . C23 . 116.75(16) yes F1 . P1 . F2 . 179.21(10) yes F1 . P1 . F3 . 89.39(10) yes F2 . P1 . F3 . 89.92(10) yes F1 . P1 . F4 . 89.82(11) yes F2 . P1 . F4 . 90.87(11) yes F3 . P1 . F4 . 179.07(11) yes F1 . P1 . F5 . 89.55(9) yes F2 . P1 . F5 . 90.05(9) yes F3 . P1 . F5 . 90.21(10) yes F4 . P1 . F5 . 90.28(10) yes F1 . P1 . F6 . 90.14(9) yes F2 . P1 . F6 . 90.26(10) yes F3 . P1 . F6 . 90.19(10) yes F4 . P1 . F6 . 89.31(10) yes F5 . P1 . F6 . 179.49(10) yes F7 . P2 . F8 . 178.33(11) yes F7 . P2 . F9 . 88.96(9) yes F8 . P2 . F9 . 89.56(10) yes F7 . P2 . F10 . 90.11(11) yes F8 . P2 . F10 . 91.36(12) yes F9 . P2 . F10 . 178.49(11) yes F7 . P2 . F11 . 89.67(9) yes F8 . P2 . F11 . 89.53(10) yes F9 . P2 . F11 . 89.29(8) yes F10 . P2 . F11 . 89.52(9) yes F7 . P2 . F12 . 89.51(10) yes F8 . P2 . F12 . 91.27(11) yes F9 . P2 . F12 . 89.92(9) yes F10 . P2 . F12 . 91.26(10) yes F11 . P2 . F12 . 178.88(10) yes # Attachment 'Ru(II)2.cif' data_hsc27_173k _database_code_depnum_ccdc_archive 'CCDC 288508' _audit_creation_date 05-10-15 _audit_creation_method CRYSTALS_ver_12.24 _oxford_structure_analysis_title '11181158 hsc27_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 16.8109(3) _cell_length_b 33.2255(11) _cell_length_c 18.7663(5) _cell_angle_alpha 90 _cell_angle_beta 93.5640(15) _cell_angle_gamma 90 _cell_volume 10461.7(5) _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' Ru -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 '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' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 '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' _cell_formula_units_Z 8 _chemical_formula_sum 'C56 H46 F12 N6 O4 P2 Ru' _chemical_formula_moiety 'C56 H46 N6 O4 Ru, 2(F6 P)' _chemical_compound_source ? _chemical_formula_weight 1258.01 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_min 0.17 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.33 _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 5104 _exptl_absorpt_coefficient_mu 0.459 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.92 # Sheldrick geometric definitions 0.87 0.92 _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 187884 _reflns_number_total 24040 _diffrn_reflns_av_R_equivalents 0.079 # Number of reflections with Friedels Law is 24040 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 24036 _diffrn_reflns_theta_min 1.226 _diffrn_reflns_theta_max 27.502 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.502 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -21 _reflns_limit_h_max 21 _reflns_limit_k_min 0 _reflns_limit_k_max 43 _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 -0.89 _refine_diff_density_max 1.32 _refine_ls_number_reflns 14204 _refine_ls_number_restraints 104 _refine_ls_number_parameters 1495 #_refine_ls_R_factor_ref 0.0653 _refine_ls_wR_factor_ref 0.0579 _refine_ls_goodness_of_fit_ref 1.1357 #_reflns_number_all 24040 _refine_ls_R_factor_all 0.1319 _refine_ls_wR_factor_all 0.1034 # 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 14204 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_gt 0.0579 _refine_ls_shift/su_max 0.046406 # 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: 6.38 1.41 4.73 1.05 ; _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 Ru1 Ru 0.05514(2) -0.232516(11) 0.723170(19) 0.0191 1.0000 Uani . . . . . . O1 O 0.1498(2) -0.24940(12) 1.03783(17) 0.0330 1.0000 Uani . . . . . . O2 O 0.2336(2) -0.25061(12) 1.18687(17) 0.0342 1.0000 Uani . . . . . . O11 O -0.0230(2) -0.23254(13) 0.40458(18) 0.0428 1.0000 Uani . . . . . . O12 O -0.1119(3) -0.22788(15) 0.2549(2) 0.0664 1.0000 Uani . . . . . . N1 N 0.1462(2) -0.19072(12) 0.7335(2) 0.0244 1.0000 Uani . . . . . . N2 N 0.0819(2) -0.23455(12) 0.82736(19) 0.0218 1.0000 Uani . . . . . . N3 N -0.0262(2) -0.27458(11) 0.7547(2) 0.0220 1.0000 Uani . . . . . . N4 N 0.1285(2) -0.27768(12) 0.6886(2) 0.0231 1.0000 Uani . . . . . . N5 N 0.0281(2) -0.23167(12) 0.61913(19) 0.0220 1.0000 Uani . . . . . . N6 N -0.0271(2) -0.18663(11) 0.7155(2) 0.0219 1.0000 Uani . . . . . . C1 C 0.1737(3) -0.16692(16) 0.6833(3) 0.0302 1.0000 Uani . . . . . . C2 C 0.2345(3) -0.13968(17) 0.6965(3) 0.0367 1.0000 Uani . . . . . . C3 C 0.2683(4) -0.13611(19) 0.7648(3) 0.0443 1.0000 Uani . . . . . . C4 C 0.2398(3) -0.15976(18) 0.8179(3) 0.0368 1.0000 Uani . . . . . . C5 C 0.1786(3) -0.18668(15) 0.8021(2) 0.0244 1.0000 Uani . . . . . . C6 C 0.1431(3) -0.21206(14) 0.8552(2) 0.0245 1.0000 Uani . . . . . . C7 C 0.1678(3) -0.21525(15) 0.9265(2) 0.0272 1.0000 Uani . . . . . . C8 C 0.1278(3) -0.24208(15) 0.9686(2) 0.0274 1.0000 Uani . . . . . . C9 C 0.0624(3) -0.26374(16) 0.9402(2) 0.0285 1.0000 Uani . . . . . . C10 C 0.0412(3) -0.25954(14) 0.8678(2) 0.0232 1.0000 Uani . . . . . . C11 C -0.0216(3) -0.28213(14) 0.8267(2) 0.0232 1.0000 Uani . . . . . . C12 C -0.0714(3) -0.30971(16) 0.8557(3) 0.0308 1.0000 Uani . . . . . . C13 C -0.1278(3) -0.32960(17) 0.8121(3) 0.0364 1.0000 Uani . . . . . . C14 C -0.1322(3) -0.32208(17) 0.7399(3) 0.0342 1.0000 Uani . . . . . . C15 C -0.0809(3) -0.29442(14) 0.7134(3) 0.0253 1.0000 Uani . . . . . . C16 C 0.1824(3) -0.29986(16) 0.7277(3) 0.0303 1.0000 Uani . . . . . . C17 C 0.2287(3) -0.32884(17) 0.6985(3) 0.0352 1.0000 Uani . . . . . . C18 C 0.2192(3) -0.33637(17) 0.6265(3) 0.0357 1.0000 Uani . . . . . . C19 C 0.1641(3) -0.31456(16) 0.5858(3) 0.0300 1.0000 Uani . . . . . . C20 C 0.1198(3) -0.28533(14) 0.6170(2) 0.0244 1.0000 Uani . . . . . . C21 C 0.0619(3) -0.25868(14) 0.5771(2) 0.0226 1.0000 Uani . . . . . . C22 C 0.0438(3) -0.25928(15) 0.5049(2) 0.0278 1.0000 Uani . . . . . . C23 C -0.0103(3) -0.23097(16) 0.4759(2) 0.0277 1.0000 Uani . . . . . . C24 C -0.0461(3) -0.20364(16) 0.5195(2) 0.0271 1.0000 Uani . . . . . . C25 C -0.0251(3) -0.20455(15) 0.5918(3) 0.0244 1.0000 Uani . . . . . . C26 C -0.0555(3) -0.17851(14) 0.6469(2) 0.0222 1.0000 Uani . . . . . . C27 C -0.1088(3) -0.14736(15) 0.6329(3) 0.0263 1.0000 Uani . . . . . . C28 C -0.1351(3) -0.12458(15) 0.6877(3) 0.0310 1.0000 Uani . . . . . . C29 C -0.1074(3) -0.13340(15) 0.7571(3) 0.0275 1.0000 Uani . . . . . . C30 C -0.0536(3) -0.16432(14) 0.7685(2) 0.0229 1.0000 Uani . . . . . . C31 C 0.3017(3) -0.27426(17) 1.3703(3) 0.0348 1.0000 Uani . . . . . . C32 C 0.2532(3) -0.25964(17) 1.3153(3) 0.0342 1.0000 Uani . . . . . . C33 C 0.1975(4) -0.2295(2) 1.3298(3) 0.0452 1.0000 Uani . . . . . . C34 C 0.1932(4) -0.2148(2) 1.3970(3) 0.0439 1.0000 Uani . . . . . . C35 C 0.2385(4) -0.2158(2) 1.5256(3) 0.0449 1.0000 Uani . . . . . . C36 C 0.2873(4) -0.2315(2) 1.5793(3) 0.0455 1.0000 Uani . . . . . . C37 C 0.3416(4) -0.2615(2) 1.5651(3) 0.0461 1.0000 Uani . . . . . . C38 C 0.3480(4) -0.27570(18) 1.4978(3) 0.0414 1.0000 Uani . . . . . . C39 C 0.2983(3) -0.26002(17) 1.4404(3) 0.0346 1.0000 Uani . . . . . . C40 C 0.2432(3) -0.22986(18) 1.4543(3) 0.0355 1.0000 Uani . . . . . . C41 C -0.0093(5) -0.3163(2) 0.3189(4) 0.0665 1.0000 Uani . . . . . . C42 C -0.0431(5) -0.2926(2) 0.2668(4) 0.0653 1.0000 Uani . . . . . . C43 C -0.0092(6) -0.2904(3) 0.1990(5) 0.0788 1.0000 Uani . . . . . . C44 C 0.0563(6) -0.3141(3) 0.1799(6) 0.0870 1.0000 Uani . . . . . . C45 C 0.1442(5) -0.3706(3) 0.2176(8) 0.1049 1.0000 Uani . . . . . . C46 C 0.1717(5) -0.3969(3) 0.2690(9) 0.1055 1.0000 Uani . . . . . . C47 C 0.1476(6) -0.3953(3) 0.3377(9) 0.1112 1.0000 Uani . . . . . . C48 C 0.0922(6) -0.3675(3) 0.3550(6) 0.0944 1.0000 Uani . . . . . . C49 C 0.0578(6) -0.3414(2) 0.3028(5) 0.0744 1.0000 Uani . . . . . . C50 C 0.0873(5) -0.3419(2) 0.2325(7) 0.0869 1.0000 Uani . . . . . . C51 C 0.2314(3) -0.23961(18) 1.0607(3) 0.0337 1.0000 Uani . . . . . . C52 C 0.2581(3) -0.26574(18) 1.1215(3) 0.0336 1.0000 Uani . . . . . . C53 C 0.2605(4) -0.27731(17) 1.2427(3) 0.0382 1.0000 Uani . . . . . . C61 C -0.0641(5) -0.1987(2) 0.3684(3) 0.0660 1.0000 Uani . . . . . . C62 C -0.0547(6) -0.2051(2) 0.2878(4) 0.0694 1.0000 Uani . . . . . . C63 C -0.1178(4) -0.2669(3) 0.2817(5) 0.0727 1.0000 Uani . . . . . . Ru2 Ru 0.26138(2) 0.015832(12) 0.770484(19) 0.0214 1.0000 Uani . . . . . . O21 O 0.3589(3) -0.00321(14) 1.08390(19) 0.0447 1.0000 Uani . . . . . . O22 O 0.3562(4) -0.00220(17) 1.2365(2) 0.0852 1.0000 Uani . . . . . . O31 O 0.1819(2) 0.00670(11) 0.45238(17) 0.0333 1.0000 Uani . . . . . . O32 O 0.1590(2) 0.02104(12) 0.30623(18) 0.0379 1.0000 Uani . . . . . . N7 N 0.3467(2) 0.06023(12) 0.7859(2) 0.0230 1.0000 Uani . . . . . . N8 N 0.2857(2) 0.01203(12) 0.8748(2) 0.0244 1.0000 Uani . . . . . . N9 N 0.1853(2) -0.02966(13) 0.7969(2) 0.0269 1.0000 Uani . . . . . . N10 N 0.1672(2) 0.05547(13) 0.7610(2) 0.0252 1.0000 Uani . . . . . . N11 N 0.2378(2) 0.01621(12) 0.66634(19) 0.0219 1.0000 Uani . . . . . . N12 N 0.3451(2) -0.02398(12) 0.7384(2) 0.0251 1.0000 Uani . . . . . . C101 C 0.3753(3) 0.08476(16) 0.7374(3) 0.0282 1.0000 Uani . . . . . . C102 C 0.4350(3) 0.11235(18) 0.7538(3) 0.0380 1.0000 Uani . . . . . . C103 C 0.4662(4) 0.11535(17) 0.8225(3) 0.0399 1.0000 Uani . . . . . . C104 C 0.4372(3) 0.09035(17) 0.8740(3) 0.0340 1.0000 Uani . . . . . . C105 C 0.3778(3) 0.06307(15) 0.8547(2) 0.0263 1.0000 Uani . . . . . . C106 C 0.3449(3) 0.03476(15) 0.9052(2) 0.0251 1.0000 Uani . . . . . . C107 C 0.3691(3) 0.02965(16) 0.9758(3) 0.0307 1.0000 Uani . . . . . . C108 C 0.3312(3) 0.00074(18) 1.0157(3) 0.0337 1.0000 Uani . . . . . . C109 C 0.2697(3) -0.02203(17) 0.9839(3) 0.0335 1.0000 Uani . . . . . . C110 C 0.2493(3) -0.01593(16) 0.9122(3) 0.0276 1.0000 Uani . . . . . . C111 C 0.1898(3) -0.03919(15) 0.8679(3) 0.0288 1.0000 Uani . . . . . . C112 C 0.1401(4) -0.06797(18) 0.8943(3) 0.0389 1.0000 Uani . . . . . . C113 C 0.0863(4) -0.08783(19) 0.8487(3) 0.0448 1.0000 Uani . . . . . . C114 C 0.0833(3) -0.07870(18) 0.7774(3) 0.0387 1.0000 Uani . . . . . . C115 C 0.1333(3) -0.04996(17) 0.7531(3) 0.0317 1.0000 Uani . . . . . . C116 C 0.1330(3) 0.07589(17) 0.8125(3) 0.0307 1.0000 Uani . . . . . . C117 C 0.0676(4) 0.0993(2) 0.8005(3) 0.0448 1.0000 Uani . . . . . . C118 C 0.0332(4) 0.1023(2) 0.7311(3) 0.0520 1.0000 Uani . . . . . . C119 C 0.0685(3) 0.0827(2) 0.6770(3) 0.0391 1.0000 Uani . . . . . . C120 C 0.1347(3) 0.05993(15) 0.6923(2) 0.0258 1.0000 Uani . . . . . . C121 C 0.1756(3) 0.03731(14) 0.6379(2) 0.0228 1.0000 Uani . . . . . . C122 C 0.1536(3) 0.03574(15) 0.5659(3) 0.0267 1.0000 Uani . . . . . . C123 C 0.1978(3) 0.01167(16) 0.5232(2) 0.0270 1.0000 Uani . . . . . . C124 C 0.2633(3) -0.00949(15) 0.5523(3) 0.0276 1.0000 Uani . . . . . . C125 C 0.2819(3) -0.00733(14) 0.6245(3) 0.0240 1.0000 Uani . . . . . . C126 C 0.3438(3) -0.03019(15) 0.6661(3) 0.0283 1.0000 Uani . . . . . . C127 C 0.3954(3) -0.05662(17) 0.6363(3) 0.0342 1.0000 Uani . . . . . . C128 C 0.4496(4) -0.07790(18) 0.6803(3) 0.0440 1.0000 Uani . . . . . . C129 C 0.4518(3) -0.07155(18) 0.7532(3) 0.0403 1.0000 Uani . . . . . . C130 C 0.3992(3) -0.04445(16) 0.7799(3) 0.0315 1.0000 Uani . . . . . . C131 C 0.4567(6) -0.0520(3) 1.3849(4) 0.0833 1.0000 Uani . . . . . . C132 C 0.3935(5) -0.0324(2) 1.3508(3) 0.0547 1.0000 Uani . . . . . . C133 C 0.3176(5) -0.0452(2) 1.3664(3) 0.0618 1.0000 Uani . . . . . . C134 C 0.2992(5) -0.0752(2) 1.4106(4) 0.0607 1.0000 Uani . . . . . . C135 C 0.3465(5) -0.1275(2) 1.4978(4) 0.0555 1.0000 Uani . . . . . . C136 C 0.4118(6) -0.1441(2) 1.5311(4) 0.0604 1.0000 Uani . . . . . . C137 C 0.4876(7) -0.1334(3) 1.5194(5) 0.0867 1.0000 Uani . . . . . . C138 C 0.5025(6) -0.1051(3) 1.4747(5) 0.0784 1.0000 Uani . . . . . . C139 C 0.4433(4) -0.0847(2) 1.4380(3) 0.0436 1.0000 Uani . . . . . . C140 C 0.3624(4) -0.0942(2) 1.4452(3) 0.0534 1.0000 Uani . . . . . . C141 C 0.1478(3) -0.05045(18) 0.2180(3) 0.0348 1.0000 Uani . . . . . . C142 C 0.1210(3) -0.01408(18) 0.1926(3) 0.0353 1.0000 Uani . . . . . . C143 C 0.0808(4) -0.01175(18) 0.1249(3) 0.0400 1.0000 Uani . . . . . . C144 C 0.0693(4) -0.04510(18) 0.0838(3) 0.0405 1.0000 Uani . . . . . . C145 C 0.0798(4) -0.11857(19) 0.0687(3) 0.0426 1.0000 Uani . . . . . . C146 C 0.1032(4) -0.1548(2) 0.0957(4) 0.0525 1.0000 Uani . . . . . . C147 C 0.1444(5) -0.1578(2) 0.1628(4) 0.0562 1.0000 Uani . . . . . . C148 C 0.1607(4) -0.12402(19) 0.2022(3) 0.0445 1.0000 Uani . . . . . . C149 C 0.1361(3) -0.08606(17) 0.1770(3) 0.0341 1.0000 Uani . . . . . . C150 C 0.0952(3) -0.08289(18) 0.1080(3) 0.0366 1.0000 Uani . . . . . . C151 C 0.3243(5) -0.0330(2) 1.1272(3) 0.0532 1.0000 Uani . . . . . . C152 C 0.3718(6) -0.0356(2) 1.1955(3) 0.0656 1.0000 Uani . . . . . . C153 C 0.4019(7) 0.0011(3) 1.2987(4) 0.0960 1.0000 Uani . . . . . . C161 C 0.1098(3) 0.02450(17) 0.4220(3) 0.0344 1.0000 Uani . . . . . . C162 C 0.0960(3) 0.00871(17) 0.3476(3) 0.0352 1.0000 Uani . . . . . . C163 C 0.1371(4) 0.02460(17) 0.2324(3) 0.0414 1.0000 Uani . . . . . . P1 P 0.38210(10) -0.13817(6) 0.99597(9) 0.0499 1.0000 Uani . . . . . . P2 P 0.07650(9) -0.09658(5) 0.52211(8) 0.0368 1.0000 Uani . . . . . . P3 P -0.27394(9) -0.14470(5) 0.43447(8) 0.0380 1.0000 Uani . . . . . . P4 P 0.14854(10) 0.09831(6) 1.02979(8) 0.0509 1.0000 Uani D U . . . . F101 F 0.3740(4) -0.1522(2) 1.0749(2) 0.1172 1.0000 Uani . . . . . . F102 F 0.4738(2) -0.14959(13) 1.0027(3) 0.0724 1.0000 Uani . . . . . . F103 F 0.3883(3) -0.12309(16) 0.9170(2) 0.0816 1.0000 Uani . . . . . . F104 F 0.3598(3) -0.18147(13) 0.9663(3) 0.0786 1.0000 Uani . . . . . . F105 F 0.2900(3) -0.12681(16) 0.9895(2) 0.0807 1.0000 Uani . . . . . . F106 F 0.4043(3) -0.09447(15) 1.0239(3) 0.0994 1.0000 Uani . . . . . . F201 F 0.1669(2) -0.08884(13) 0.5475(2) 0.0622 1.0000 Uani . . . . . . F202 F 0.0539(3) -0.09921(17) 0.6019(2) 0.0793 1.0000 Uani . . . . . . F203 F -0.01449(19) -0.10473(12) 0.49756(19) 0.0504 1.0000 Uani . . . . . . F204 F 0.0984(3) -0.09464(19) 0.4416(2) 0.0915 1.0000 Uani . . . . . . F205 F 0.0939(2) -0.14336(12) 0.5229(3) 0.0682 1.0000 Uani . . . . . . F206 F 0.0590(3) -0.05040(13) 0.5204(4) 0.1083 1.0000 Uani . . . . . . F301 F -0.3113(3) -0.15064(16) 0.5087(2) 0.0865 1.0000 Uani . . . . . . F302 F -0.2472(3) -0.19067(13) 0.4357(3) 0.0890 1.0000 Uani . . . . . . F303 F -0.3565(2) -0.15651(13) 0.3942(2) 0.0674 1.0000 Uani . . . . . . F304 F -0.2366(3) -0.13896(13) 0.3594(2) 0.0620 1.0000 Uani . . . . . . F305 F -0.3001(2) -0.09899(10) 0.4320(2) 0.0494 1.0000 Uani . . . . . . F306 F -0.1897(2) -0.13294(15) 0.4711(2) 0.0716 1.0000 Uani . . . . . . F401 F 0.1143(2) 0.12416(12) 0.96384(18) 0.0580 1.0000 Uani D U . . . . F402 F 0.1828(3) 0.07255(16) 1.0955(2) 0.0986 1.0000 Uani D U . . . . F403 F 0.1682(8) 0.1346(3) 1.0776(5) 0.0909 0.5000 Uani D U . . . . F404 F 0.2338(5) 0.0986(4) 0.9981(6) 0.0762 0.5000 Uani D U . . . . F405 F 0.1350(7) 0.0567(2) 0.9843(4) 0.0740 0.5000 Uani D U . . . . F406 F 0.0666(4) 0.0887(3) 1.0621(5) 0.0699 0.5000 Uani D U . . . . F413 F 0.2100(6) 0.1338(3) 1.0473(6) 0.0811 0.5000 Uani D U . . . . F414 F 0.2100(7) 0.0790(4) 0.9834(5) 0.0943 0.5000 Uani D U . . . . F415 F 0.0820(8) 0.0678(3) 1.0102(8) 0.1318 0.5000 Uani D U . . . . F416 F 0.0855(6) 0.1256(4) 1.0727(4) 0.0921 0.5000 Uani D U . . . . H11 H 0.1491 -0.1690 0.6335 0.0335 1.0000 Uiso R . . . . . H21 H 0.2537 -0.1227 0.6570 0.0429 1.0000 Uiso R . . . . . H31 H 0.3132 -0.1169 0.7755 0.0505 1.0000 Uiso R . . . . . H41 H 0.2632 -0.1571 0.8680 0.0441 1.0000 Uiso R . . . . . H71 H 0.2129 -0.1985 0.9474 0.0322 1.0000 Uiso R . . . . . H91 H 0.0321 -0.2820 0.9711 0.0285 1.0000 Uiso R . . . . . H121 H -0.0673 -0.3153 0.9081 0.0340 1.0000 Uiso R . . . . . H131 H -0.1651 -0.3492 0.8329 0.0405 1.0000 Uiso R . . . . . H141 H -0.1715 -0.3368 0.7073 0.0365 1.0000 Uiso R . . . . . H151 H -0.0847 -0.2889 0.6609 0.0276 1.0000 Uiso R . . . . . H161 H 0.1888 -0.2950 0.7803 0.0348 1.0000 Uiso R . . . . . H171 H 0.2683 -0.3445 0.7292 0.0389 1.0000 Uiso R . . . . . H181 H 0.2514 -0.3577 0.6042 0.0403 1.0000 Uiso R . . . . . H191 H 0.1572 -0.3195 0.5332 0.0355 1.0000 Uiso R . . . . . H221 H 0.0685 -0.2794 0.4733 0.0335 1.0000 Uiso R . . . . . H241 H -0.0860 -0.1838 0.4989 0.0300 1.0000 Uiso R . . . . . H271 H -0.1286 -0.1415 0.5826 0.0306 1.0000 Uiso R . . . . . H281 H -0.1735 -0.1020 0.6780 0.0333 1.0000 Uiso R . . . . . H291 H -0.1259 -0.1177 0.7984 0.0322 1.0000 Uiso R . . . . . H301 H -0.0331 -0.1702 0.8186 0.0242 1.0000 Uiso R . . . . . H311 H 0.3408 -0.2959 1.3603 0.0412 1.0000 Uiso R . . . . . H331 H 0.1618 -0.2181 1.2902 0.0522 1.0000 Uiso R . . . . . H341 H 0.1539 -0.1931 1.4062 0.0507 1.0000 Uiso R . . . . . H351 H 0.1993 -0.1943 1.5362 0.0535 1.0000 Uiso R . . . . . H361 H 0.2839 -0.2211 1.6291 0.0524 1.0000 Uiso R . . . . . H371 H 0.3762 -0.2730 1.6054 0.0533 1.0000 Uiso R . . . . . H381 H 0.3884 -0.2969 1.4887 0.0457 1.0000 Uiso R . . . . . H411 H -0.0293 -0.3168 0.3680 0.0957 1.0000 Uiso R . . . . . H431 H -0.0312 -0.2702 0.1635 0.1091 1.0000 Uiso R . . . . . H441 H 0.0793 -0.3117 0.1322 0.1095 1.0000 Uiso R . . . . . H451 H 0.1653 -0.3725 0.1691 0.1230 1.0000 Uiso R . . . . . H461 H 0.2118 -0.4176 0.2570 0.1266 1.0000 Uiso R . . . . . H471 H 0.1694 -0.4147 0.3747 0.1224 1.0000 Uiso R . . . . . H481 H 0.0751 -0.3653 0.4049 0.1071 1.0000 Uiso R . . . . . H511 H 0.2350 -0.2107 1.0754 0.0367 1.0000 Uiso R . . . . . H512 H 0.2661 -0.2443 1.0201 0.0367 1.0000 Uiso R . . . . . H521 H 0.3176 -0.2674 1.1240 0.0366 1.0000 Uiso R . . . . . H522 H 0.2351 -0.2933 1.1135 0.0366 1.0000 Uiso R . . . . . H531 H 0.2277 -0.3024 1.2384 0.0443 1.0000 Uiso R . . . . . H532 H 0.3178 -0.2841 1.2371 0.0443 1.0000 Uiso R . . . . . H611 H -0.1218 -0.1996 0.3782 0.0877 1.0000 Uiso R . . . . . H612 H -0.0408 -0.1725 0.3855 0.0877 1.0000 Uiso R . . . . . H621 H -0.0018 -0.2180 0.2816 0.0867 1.0000 Uiso R . . . . . H622 H -0.0563 -0.1781 0.2645 0.0867 1.0000 Uiso R . . . . . H631 H -0.1224 -0.2653 0.3345 0.0940 1.0000 Uiso R . . . . . H632 H -0.1666 -0.2800 0.2590 0.0940 1.0000 Uiso R . . . . . H1011 H 0.3524 0.0832 0.6870 0.0314 1.0000 Uiso R . . . . . H1021 H 0.4549 0.1302 0.7158 0.0440 1.0000 Uiso R . . . . . H1031 H 0.5101 0.1349 0.8352 0.0456 1.0000 Uiso R . . . . . H1041 H 0.4590 0.0924 0.9247 0.0381 1.0000 Uiso R . . . . . H1071 H 0.4133 0.0462 0.9986 0.0320 1.0000 Uiso R . . . . . H1091 H 0.2413 -0.0424 1.0123 0.0391 1.0000 Uiso R . . . . . H1121 H 0.1430 -0.0744 0.9464 0.0453 1.0000 Uiso R . . . . . H1131 H 0.0504 -0.1089 0.8671 0.0524 1.0000 Uiso R . . . . . H1141 H 0.0446 -0.0929 0.7435 0.0460 1.0000 Uiso R . . . . . H1151 H 0.1313 -0.0442 0.7007 0.0373 1.0000 Uiso R . . . . . H1161 H 0.1571 0.0740 0.8625 0.0363 1.0000 Uiso R . . . . . H1171 H 0.0437 0.1140 0.8404 0.0497 1.0000 Uiso R . . . . . H1181 H -0.0161 0.1187 0.7209 0.0603 1.0000 Uiso R . . . . . H1191 H 0.0451 0.0848 0.6268 0.0426 1.0000 Uiso R . . . . . H1221 H 0.1067 0.0513 0.5453 0.0304 1.0000 Uiso R . . . . . H1241 H 0.2959 -0.0262 0.5208 0.0308 1.0000 Uiso R . . . . . H1271 H 0.3942 -0.0605 0.5834 0.0379 1.0000 Uiso R . . . . . H1281 H 0.4859 -0.0980 0.6596 0.0488 1.0000 Uiso R . . . . . H1291 H 0.4912 -0.0864 0.7856 0.0440 1.0000 Uiso R . . . . . H1301 H 0.4017 -0.0398 0.8327 0.0361 1.0000 Uiso R . . . . . H1311 H 0.5125 -0.0448 1.3743 0.0991 1.0000 Uiso R . . . . . H1331 H 0.2720 -0.0300 1.3427 0.0815 1.0000 Uiso R . . . . . H1341 H 0.2427 -0.0832 1.4170 0.0864 1.0000 Uiso R . . . . . H1351 H 0.2908 -0.1359 1.5063 0.0666 1.0000 Uiso R . . . . . H1361 H 0.4038 -0.1662 1.5661 0.0738 1.0000 Uiso R . . . . . H1371 H 0.5328 -0.1476 1.5459 0.1103 1.0000 Uiso R . . . . . H1381 H 0.5593 -0.0977 1.4684 0.1012 1.0000 Uiso R . . . . . H1411 H 0.1764 -0.0520 0.2663 0.0427 1.0000 Uiso R . . . . . H1431 H 0.0590 0.0146 0.1069 0.0474 1.0000 Uiso R . . . . . H1441 H 0.0428 -0.0426 0.0349 0.0475 1.0000 Uiso R . . . . . H1451 H 0.0517 -0.1171 0.0202 0.0493 1.0000 Uiso R . . . . . H1461 H 0.0917 -0.1797 0.0668 0.0566 1.0000 Uiso R . . . . . H1471 H 0.1617 -0.1847 0.1818 0.0674 1.0000 Uiso R . . . . . H1481 H 0.1899 -0.1265 0.2501 0.0529 1.0000 Uiso R . . . . . H1511 H 0.2688 -0.0249 1.1374 0.0649 1.0000 Uiso R . . . . . H1512 H 0.3230 -0.0594 1.1018 0.0649 1.0000 Uiso R . . . . . H1521 H 0.3591 -0.0608 1.2215 0.0844 1.0000 Uiso R . . . . . H1522 H 0.4295 -0.0356 1.1853 0.0844 1.0000 Uiso R . . . . . H1531 H 0.3881 0.0268 1.3227 0.1107 1.0000 Uiso R . . . . . H1532 H 0.4590 0.0019 1.2866 0.1107 1.0000 Uiso R . . . . . H1611 H 0.0644 0.0171 0.4514 0.0391 1.0000 Uiso R . . . . . H1612 H 0.1154 0.0544 0.4208 0.0391 1.0000 Uiso R . . . . . H1621 H 0.0929 -0.0213 0.3488 0.0407 1.0000 Uiso R . . . . . H1622 H 0.0448 0.0198 0.3260 0.0407 1.0000 Uiso R . . . . . H1631 H 0.1806 0.0391 0.2089 0.0491 1.0000 Uiso R . . . . . H1632 H 0.0872 0.0410 0.2281 0.0491 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 Ru1 0.02150(18) 0.02171(18) 0.01379(16) -0.00062(15) -0.00163(13) -0.00051(16) O1 0.036(2) 0.046(2) 0.0157(16) -0.0009(15) -0.0068(14) 0.0043(17) O2 0.041(2) 0.043(2) 0.0180(16) -0.0009(15) -0.0039(15) 0.0140(18) O11 0.053(2) 0.056(3) 0.0182(17) -0.0057(17) -0.0064(16) 0.021(2) O12 0.096(4) 0.050(3) 0.048(3) -0.008(2) -0.029(3) 0.015(3) N1 0.026(2) 0.027(2) 0.0202(19) 0.0008(16) 0.0000(16) -0.0002(17) N2 0.022(2) 0.025(2) 0.0179(18) -0.0046(16) -0.0021(15) 0.0061(17) N3 0.024(2) 0.022(2) 0.0198(18) 0.0010(15) 0.0015(15) 0.0047(16) N4 0.024(2) 0.025(2) 0.0211(19) 0.0000(15) -0.0003(16) -0.0004(16) N5 0.025(2) 0.0209(19) 0.0196(18) -0.0008(16) -0.0005(15) -0.0026(17) N6 0.024(2) 0.020(2) 0.0215(19) -0.0003(15) -0.0008(16) -0.0034(16) C1 0.033(3) 0.033(3) 0.025(2) -0.001(2) 0.000(2) 0.000(2) C2 0.038(3) 0.036(3) 0.036(3) 0.008(2) 0.008(2) -0.012(3) C3 0.042(3) 0.044(3) 0.046(3) 0.002(3) -0.006(3) -0.020(3) C4 0.036(3) 0.042(3) 0.031(3) -0.002(2) -0.005(2) -0.009(3) C5 0.026(2) 0.027(3) 0.019(2) -0.0029(19) -0.0047(18) -0.002(2) C6 0.027(3) 0.024(3) 0.022(2) -0.0046(19) -0.0021(19) -0.002(2) C7 0.032(3) 0.029(3) 0.019(2) -0.0034(19) -0.007(2) -0.001(2) C8 0.035(3) 0.028(3) 0.018(2) -0.0013(19) -0.006(2) 0.008(2) C9 0.031(3) 0.034(3) 0.020(2) 0.002(2) 0.0005(19) 0.006(2) C10 0.026(2) 0.023(2) 0.021(2) -0.0005(18) 0.0028(19) 0.0052(19) C11 0.027(3) 0.022(2) 0.020(2) 0.0012(18) 0.0016(19) 0.005(2) C12 0.033(3) 0.031(3) 0.029(3) 0.008(2) 0.001(2) 0.000(2) C13 0.033(3) 0.037(3) 0.039(3) 0.006(2) 0.005(2) -0.008(2) C14 0.031(3) 0.033(3) 0.038(3) -0.004(2) -0.005(2) -0.006(2) C15 0.029(3) 0.024(2) 0.021(2) -0.0036(19) -0.007(2) 0.000(2) C16 0.026(3) 0.039(3) 0.025(2) 0.002(2) -0.002(2) 0.000(2) C17 0.039(3) 0.032(3) 0.034(3) 0.003(2) -0.002(2) 0.013(2) C18 0.036(3) 0.033(3) 0.039(3) -0.001(2) 0.011(2) 0.012(2) C19 0.035(3) 0.032(3) 0.022(2) -0.002(2) 0.002(2) 0.005(2) C20 0.029(3) 0.022(2) 0.022(2) -0.0008(19) 0.0018(19) 0.000(2) C21 0.029(3) 0.023(2) 0.016(2) -0.0013(18) -0.0001(18) -0.0009(19) C22 0.034(3) 0.029(3) 0.020(2) -0.0018(19) 0.001(2) -0.002(2) C23 0.036(3) 0.032(3) 0.014(2) -0.0036(19) -0.0024(19) -0.002(2) C24 0.031(3) 0.034(3) 0.016(2) 0.0026(19) -0.0050(19) 0.003(2) C25 0.022(2) 0.025(2) 0.026(2) 0.0019(19) -0.0005(19) -0.0031(19) C26 0.023(2) 0.028(2) 0.016(2) 0.0005(18) 0.0044(18) -0.006(2) C27 0.028(3) 0.026(3) 0.025(2) 0.0035(19) -0.001(2) 0.000(2) C28 0.032(3) 0.024(3) 0.038(3) 0.004(2) 0.006(2) 0.005(2) C29 0.029(3) 0.024(3) 0.030(3) -0.007(2) 0.007(2) -0.002(2) C30 0.027(2) 0.023(2) 0.018(2) -0.0058(18) 0.0015(18) -0.005(2) C31 0.034(3) 0.040(3) 0.029(3) 0.001(2) -0.001(2) 0.001(2) C32 0.032(3) 0.043(3) 0.027(3) 0.002(2) -0.003(2) -0.003(2) C33 0.042(3) 0.061(4) 0.032(3) 0.006(3) -0.003(2) 0.011(3) C34 0.044(3) 0.051(4) 0.037(3) 0.003(3) 0.006(3) 0.020(3) C35 0.053(4) 0.049(4) 0.033(3) -0.005(3) 0.011(3) 0.001(3) C36 0.058(4) 0.052(4) 0.027(3) -0.008(3) 0.005(3) -0.006(3) C37 0.057(4) 0.055(4) 0.024(3) -0.001(3) -0.010(3) -0.005(3) C38 0.046(3) 0.044(4) 0.033(3) 0.007(2) -0.004(3) 0.005(3) C39 0.036(3) 0.041(3) 0.027(3) -0.001(2) 0.002(2) -0.005(2) C40 0.038(3) 0.042(3) 0.027(3) -0.002(2) 0.007(2) -0.002(3) C41 0.073(5) 0.053(4) 0.071(5) -0.005(4) -0.019(4) -0.006(4) C42 0.071(5) 0.066(5) 0.056(4) 0.000(4) -0.016(4) -0.004(4) C43 0.088(6) 0.081(6) 0.066(5) 0.010(4) -0.004(5) 0.017(5) C44 0.081(6) 0.064(6) 0.111(8) -0.017(5) -0.030(6) 0.003(5) C45 0.044(5) 0.072(6) 0.198(13) 0.016(7) -0.001(6) -0.013(5) C46 0.034(4) 0.054(5) 0.228(15) 0.043(8) 0.003(7) 0.000(4) C47 0.042(5) 0.082(7) 0.203(14) 0.047(8) -0.043(7) -0.016(5) C48 0.067(6) 0.079(6) 0.130(9) 0.003(6) -0.055(6) -0.004(5) C49 0.075(6) 0.054(5) 0.089(6) -0.008(4) -0.037(5) 0.000(4) C50 0.052(5) 0.046(5) 0.157(10) 0.006(5) -0.034(6) -0.006(4) C51 0.028(3) 0.048(3) 0.025(2) -0.006(2) -0.005(2) 0.007(2) C52 0.036(3) 0.041(3) 0.023(2) -0.004(2) -0.004(2) 0.010(3) C53 0.052(4) 0.030(3) 0.032(3) 0.000(2) -0.006(2) 0.003(2) C61 0.090(6) 0.074(5) 0.033(3) 0.001(3) -0.014(3) 0.033(4) C62 0.109(7) 0.059(5) 0.037(4) 0.008(3) -0.018(4) -0.002(5) C63 0.046(4) 0.098(7) 0.072(5) 0.015(5) -0.011(4) -0.008(4) Ru2 0.02170(19) 0.0255(2) 0.01667(17) 0.00045(16) -0.00088(13) -0.00303(16) O21 0.050(3) 0.064(3) 0.0192(18) 0.0086(18) -0.0035(17) -0.005(2) O22 0.162(6) 0.062(3) 0.029(2) 0.010(2) -0.021(3) -0.001(4) O31 0.037(2) 0.046(2) 0.0173(16) -0.0039(15) -0.0028(14) 0.0118(17) O32 0.048(2) 0.044(2) 0.0215(17) -0.0051(16) 0.0009(16) -0.0052(19) N7 0.024(2) 0.026(2) 0.0187(19) 0.0009(16) -0.0007(15) -0.0007(17) N8 0.026(2) 0.026(2) 0.0212(19) 0.0007(16) 0.0018(16) -0.0026(17) N9 0.028(2) 0.027(2) 0.026(2) -0.0007(17) 0.0009(17) 0.0003(17) N10 0.023(2) 0.036(2) 0.0170(18) 0.0000(17) 0.0000(15) -0.0019(18) N11 0.0220(19) 0.026(2) 0.0173(18) -0.0019(16) 0.0002(15) -0.0040(17) N12 0.024(2) 0.026(2) 0.025(2) 0.0007(16) -0.0016(16) -0.0034(17) C101 0.029(3) 0.032(3) 0.024(2) 0.001(2) 0.001(2) -0.002(2) C102 0.035(3) 0.039(3) 0.040(3) 0.011(2) -0.001(2) -0.009(3) C103 0.037(3) 0.034(3) 0.046(3) 0.004(3) -0.011(3) -0.014(3) C104 0.033(3) 0.040(3) 0.028(3) 0.001(2) -0.005(2) -0.008(2) C105 0.025(2) 0.030(3) 0.023(2) 0.000(2) -0.0033(19) -0.001(2) C106 0.027(3) 0.029(3) 0.019(2) -0.0018(19) -0.0026(19) -0.001(2) C107 0.032(3) 0.034(3) 0.026(2) -0.001(2) -0.003(2) -0.005(2) C108 0.036(3) 0.044(3) 0.021(2) 0.003(2) 0.002(2) 0.005(3) C109 0.038(3) 0.038(3) 0.025(2) 0.011(2) 0.007(2) -0.006(2) C110 0.030(3) 0.028(3) 0.025(2) 0.000(2) 0.006(2) -0.003(2) C111 0.031(3) 0.029(3) 0.027(2) 0.003(2) 0.008(2) 0.000(2) C112 0.043(3) 0.040(3) 0.035(3) 0.001(2) 0.013(2) -0.011(3) C113 0.044(4) 0.044(4) 0.047(3) 0.000(3) 0.012(3) -0.018(3) C114 0.031(3) 0.040(3) 0.045(3) -0.005(3) 0.000(2) -0.013(2) C115 0.027(3) 0.038(3) 0.030(3) -0.008(2) -0.001(2) -0.007(2) C116 0.027(3) 0.050(3) 0.016(2) -0.004(2) 0.0047(19) -0.003(2) C117 0.039(3) 0.070(4) 0.028(3) -0.012(3) 0.013(2) 0.016(3) C118 0.045(4) 0.074(5) 0.038(3) -0.004(3) 0.005(3) 0.031(3) C119 0.028(3) 0.067(4) 0.023(3) -0.003(3) 0.001(2) 0.014(3) C120 0.025(3) 0.035(3) 0.018(2) 0.001(2) 0.0009(18) 0.004(2) C121 0.023(2) 0.025(2) 0.021(2) 0.0003(18) 0.0023(18) -0.0042(19) C122 0.026(3) 0.030(3) 0.024(2) 0.001(2) -0.002(2) 0.001(2) C123 0.031(3) 0.035(3) 0.015(2) -0.003(2) -0.0012(19) -0.003(2) C124 0.031(3) 0.030(3) 0.021(2) -0.009(2) 0.003(2) 0.002(2) C125 0.020(2) 0.025(3) 0.027(2) -0.0049(19) 0.0026(19) -0.0009(19) C126 0.028(3) 0.026(2) 0.030(3) 0.001(2) -0.008(2) -0.003(2) C127 0.031(3) 0.037(3) 0.034(3) -0.011(2) -0.004(2) 0.008(2) C128 0.039(3) 0.041(3) 0.050(4) -0.013(3) -0.009(3) 0.012(3) C129 0.034(3) 0.040(3) 0.046(3) 0.002(3) -0.012(3) 0.003(3) C130 0.032(3) 0.028(3) 0.034(3) 0.005(2) -0.004(2) 0.000(2) C131 0.078(6) 0.127(8) 0.045(4) -0.022(5) 0.004(4) 0.003(6) C132 0.065(5) 0.074(5) 0.023(3) 0.005(3) -0.011(3) -0.006(4) C133 0.096(6) 0.060(4) 0.031(3) -0.001(3) 0.016(4) -0.004(4) C134 0.057(4) 0.072(5) 0.053(4) -0.025(4) 0.003(3) -0.004(4) C135 0.075(5) 0.048(4) 0.044(4) -0.017(3) 0.009(3) -0.003(4) C136 0.092(6) 0.052(4) 0.038(4) -0.006(3) 0.008(4) 0.009(4) C137 0.102(8) 0.100(8) 0.058(5) -0.018(5) 0.007(5) 0.019(6) C138 0.069(5) 0.108(7) 0.055(5) -0.019(5) -0.015(4) 0.024(5) C139 0.038(3) 0.062(4) 0.032(3) -0.003(3) 0.009(2) -0.006(3) C140 0.056(4) 0.068(5) 0.035(3) -0.026(3) -0.008(3) 0.022(4) C141 0.039(3) 0.043(3) 0.022(2) 0.001(2) 0.000(2) 0.002(3) C142 0.047(3) 0.039(3) 0.020(2) 0.000(2) 0.005(2) -0.009(3) C143 0.060(4) 0.032(3) 0.027(3) 0.001(2) -0.003(3) 0.003(3) C144 0.053(4) 0.042(3) 0.026(3) 0.002(2) -0.002(2) -0.003(3) C145 0.042(3) 0.049(4) 0.038(3) -0.009(3) 0.011(3) -0.001(3) C146 0.057(4) 0.043(4) 0.059(4) -0.015(3) 0.015(3) 0.007(3) C147 0.071(5) 0.040(4) 0.060(4) 0.002(3) 0.019(4) 0.018(3) C148 0.045(4) 0.043(4) 0.047(3) 0.004(3) 0.010(3) 0.017(3) C149 0.029(3) 0.039(3) 0.034(3) 0.003(2) 0.007(2) 0.004(2) C150 0.039(3) 0.040(3) 0.031(3) -0.007(2) 0.011(2) -0.005(3) C151 0.074(5) 0.062(4) 0.024(3) 0.012(3) 0.008(3) 0.001(4) C152 0.105(6) 0.063(5) 0.030(3) 0.014(3) 0.004(4) 0.011(4) C153 0.162(10) 0.083(6) 0.041(4) 0.015(4) -0.012(5) -0.056(7) C161 0.040(3) 0.038(3) 0.024(2) -0.001(2) -0.004(2) 0.006(2) C162 0.042(3) 0.042(3) 0.021(2) -0.003(2) -0.006(2) 0.004(3) C163 0.072(4) 0.033(3) 0.019(2) 0.000(2) -0.002(3) -0.005(3) P1 0.0431(9) 0.0572(11) 0.0463(9) -0.0086(8) -0.0217(7) -0.0007(8) P2 0.0278(7) 0.0394(8) 0.0434(8) 0.0085(7) 0.0049(6) 0.0006(6) P3 0.0357(8) 0.0392(8) 0.0386(8) 0.0127(6) -0.0012(6) 0.0014(7) P4 0.0511(10) 0.0793(13) 0.0223(7) 0.0037(7) 0.0021(7) -0.0127(9) F101 0.100(4) 0.202(7) 0.047(3) 0.024(3) -0.023(3) -0.007(4) F102 0.050(2) 0.066(3) 0.097(3) -0.020(2) -0.028(2) 0.009(2) F103 0.075(3) 0.106(4) 0.062(3) 0.019(3) -0.016(2) -0.023(3) F104 0.077(3) 0.057(3) 0.098(3) -0.005(2) -0.026(3) -0.015(2) F105 0.048(2) 0.115(4) 0.076(3) -0.019(3) -0.018(2) 0.006(3) F106 0.073(3) 0.073(3) 0.143(5) -0.047(3) -0.059(3) 0.019(3) F201 0.0298(19) 0.069(3) 0.087(3) 0.001(2) -0.0009(19) -0.0103(18) F202 0.052(2) 0.141(5) 0.045(2) -0.014(3) 0.0105(19) -0.017(3) F203 0.0292(18) 0.065(2) 0.056(2) 0.0163(18) -0.0064(15) -0.0008(17) F204 0.055(3) 0.168(5) 0.053(3) 0.041(3) 0.013(2) 0.004(3) F205 0.050(2) 0.050(2) 0.102(3) 0.001(2) -0.012(2) 0.0069(19) F206 0.055(3) 0.035(2) 0.237(7) 0.020(3) 0.030(4) 0.002(2) F301 0.093(4) 0.113(4) 0.056(3) 0.040(3) 0.028(2) 0.012(3) F302 0.072(3) 0.042(2) 0.156(5) 0.029(3) 0.035(3) 0.018(2) F303 0.054(2) 0.057(3) 0.090(3) 0.002(2) -0.010(2) -0.021(2) F304 0.066(3) 0.077(3) 0.044(2) 0.0057(19) 0.0137(19) -0.002(2) F305 0.049(2) 0.040(2) 0.059(2) -0.0002(16) -0.0035(17) 0.0000(16) F306 0.049(2) 0.094(3) 0.067(3) 0.019(2) -0.028(2) 0.000(2) F401 0.063(2) 0.071(3) 0.039(2) 0.0005(18) -0.0049(17) 0.016(2) F402 0.094(4) 0.149(5) 0.049(2) 0.056(3) -0.029(2) -0.054(3) F403 0.156(13) 0.072(6) 0.043(5) -0.014(4) -0.001(6) -0.017(8) F404 0.069(6) 0.094(9) 0.069(8) 0.031(6) 0.028(6) 0.012(6) F405 0.115(9) 0.078(6) 0.030(4) -0.003(4) 0.005(5) 0.016(7) F406 0.052(5) 0.069(7) 0.091(7) 0.027(5) 0.027(5) 0.001(5) F413 0.072(7) 0.067(6) 0.097(8) 0.011(6) -0.050(6) -0.005(5) F414 0.131(12) 0.111(11) 0.039(5) -0.017(6) -0.009(6) 0.087(9) F415 0.119(11) 0.103(11) 0.161(14) 0.058(9) -0.088(10) -0.071(9) F416 0.074(7) 0.165(11) 0.040(5) 0.017(6) 0.024(4) 0.039(7) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.4989(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 Ru1 . N1 . 2.067(4) yes Ru1 . N2 . 1.980(4) yes Ru1 . N3 . 2.067(4) yes Ru1 . N4 . 2.072(4) yes Ru1 . N5 . 1.977(4) yes Ru1 . N6 . 2.058(4) yes O1 . C8 . 1.350(5) yes O1 . C51 . 1.449(6) yes O2 . C52 . 1.410(6) yes O2 . C53 . 1.425(6) yes O11 . C23 . 1.343(5) yes O11 . C61 . 1.464(8) yes O12 . C62 . 1.342(9) yes O12 . C63 . 1.396(10) yes N1 . C1 . 1.335(6) yes N1 . C5 . 1.373(6) yes N2 . C6 . 1.349(6) yes N2 . C10 . 1.342(6) yes N3 . C11 . 1.373(6) yes N3 . C15 . 1.338(6) yes N4 . C16 . 1.348(6) yes N4 . C20 . 1.368(6) yes N5 . C21 . 1.344(6) yes N5 . C25 . 1.348(6) yes N6 . C26 . 1.371(6) yes N6 . C30 . 1.339(6) yes C1 . C2 . 1.376(7) yes C1 . H11 . 1.000 no C2 . C3 . 1.375(8) yes C2 . H21 . 1.000 no C3 . C4 . 1.378(8) yes C3 . H31 . 1.000 no C4 . C5 . 1.382(7) yes C4 . H41 . 1.000 no C5 . C6 . 1.460(7) yes C6 . C7 . 1.380(6) yes C7 . C8 . 1.392(7) yes C7 . H71 . 1.000 no C8 . C9 . 1.393(7) yes C9 . C10 . 1.389(6) yes C9 . H91 . 1.000 no C10 . C11 . 1.473(7) yes C11 . C12 . 1.376(7) yes C12 . C13 . 1.381(8) yes C12 . H121 . 1.000 no C13 . C14 . 1.376(8) yes C13 . H131 . 1.000 no C14 . C15 . 1.374(7) yes C14 . H141 . 1.000 no C15 . H151 . 1.000 no C16 . C17 . 1.374(7) yes C16 . H161 . 1.000 no C17 . C18 . 1.375(8) yes C17 . H171 . 1.000 no C18 . C19 . 1.370(7) yes C18 . H181 . 1.000 no C19 . C20 . 1.377(7) yes C19 . H191 . 1.000 no C20 . C21 . 1.483(7) yes C21 . C22 . 1.371(6) yes C22 . C23 . 1.395(7) yes C22 . H221 . 1.000 no C23 . C24 . 1.385(7) yes C24 . C25 . 1.381(6) yes C24 . H241 . 1.000 no C25 . C26 . 1.464(7) yes C26 . C27 . 1.383(7) yes C27 . C28 . 1.371(7) yes C27 . H271 . 1.000 no C28 . C29 . 1.387(7) yes C28 . H281 . 1.000 no C29 . C30 . 1.376(7) yes C29 . H291 . 1.000 no C30 . H301 . 1.000 no C31 . C32 . 1.364(7) yes C31 . C39 . 1.402(7) yes C31 . H311 . 1.000 no C32 . C33 . 1.409(8) yes C32 . C53 . 1.496(7) yes C33 . C34 . 1.358(8) yes C33 . H331 . 1.000 no C34 . C40 . 1.414(8) yes C34 . H341 . 1.000 no C35 . C36 . 1.363(9) yes C35 . C40 . 1.425(7) yes C35 . H351 . 1.000 no C36 . C37 . 1.389(9) yes C36 . H361 . 1.000 no C37 . C38 . 1.359(8) yes C37 . H371 . 1.000 no C38 . C39 . 1.421(7) yes C38 . H381 . 1.000 no C39 . C40 . 1.400(8) yes C41 . C42 . 1.353(10) yes C41 . C49 . 1.451(12) yes C41 . H411 . 1.000 no C42 . C43 . 1.429(12) yes C42 . C63 . 1.558(12) yes C43 . C44 . 1.418(13) yes C43 . H431 . 1.000 no C44 . C50 . 1.426(13) yes C44 . H441 . 1.000 no C45 . C46 . 1.361(15) yes C45 . C50 . 1.391(13) yes C45 . H451 . 1.000 no C46 . C47 . 1.375(17) yes C46 . H461 . 1.000 no C47 . C48 . 1.364(15) yes C47 . H471 . 1.000 no C48 . C49 . 1.404(12) yes C48 . H481 . 1.000 no C49 . C50 . 1.438(14) yes C51 . C52 . 1.481(7) yes C51 . H511 . 1.000 no C51 . H512 . 1.000 no C52 . H521 . 1.000 no C52 . H522 . 1.000 no C53 . H531 . 1.000 no C53 . H532 . 1.000 no C61 . C62 . 1.547(9) yes C61 . H611 . 1.000 no C61 . H612 . 1.000 no C62 . H621 . 1.000 no C62 . H622 . 1.000 no C63 . H631 . 1.000 no C63 . H632 . 1.000 no Ru2 . N7 . 2.065(4) yes Ru2 . N8 . 1.979(4) yes Ru2 . N9 . 2.060(4) yes Ru2 . N10 . 2.059(4) yes Ru2 . N11 . 1.970(4) yes Ru2 . N12 . 2.049(4) yes O21 . C108 . 1.342(6) yes O21 . C151 . 1.426(7) yes O22 . C152 . 1.384(9) yes O22 . C153 . 1.362(9) yes O31 . C123 . 1.348(5) yes O31 . C161 . 1.434(6) yes O32 . C162 . 1.412(7) yes O32 . C163 . 1.416(6) yes N7 . C101 . 1.332(6) yes N7 . C105 . 1.367(6) yes N8 . C106 . 1.346(6) yes N8 . C110 . 1.336(6) yes N9 . C111 . 1.366(6) yes N9 . C115 . 1.344(6) yes N10 . C116 . 1.340(6) yes N10 . C120 . 1.376(6) yes N11 . C121 . 1.342(6) yes N11 . C125 . 1.360(6) yes N12 . C126 . 1.373(6) yes N12 . C130 . 1.344(6) yes C101 . C102 . 1.380(7) yes C101 . H1011 . 1.000 no C102 . C103 . 1.366(8) yes C102 . H1021 . 1.000 no C103 . C104 . 1.385(8) yes C103 . H1031 . 1.000 no C104 . C105 . 1.380(7) yes C104 . H1041 . 1.000 no C105 . C106 . 1.467(7) yes C106 . C107 . 1.373(7) yes C107 . C108 . 1.395(8) yes C107 . H1071 . 1.000 no C108 . C109 . 1.386(8) yes C109 . C110 . 1.382(7) yes C109 . H1091 . 1.000 no C110 . C111 . 1.478(7) yes C111 . C112 . 1.381(7) yes C112 . C113 . 1.374(8) yes C112 . H1121 . 1.000 no C113 . C114 . 1.370(8) yes C113 . H1131 . 1.000 no C114 . C115 . 1.369(8) yes C114 . H1141 . 1.000 no C115 . H1151 . 1.000 no C116 . C117 . 1.354(8) yes C116 . H1161 . 1.000 no C117 . C118 . 1.394(8) yes C117 . H1171 . 1.000 no C118 . C119 . 1.372(8) yes C118 . H1181 . 1.000 no C119 . C120 . 1.362(7) yes C119 . H1191 . 1.000 no C120 . C121 . 1.473(7) yes C121 . C122 . 1.380(6) yes C122 . C123 . 1.381(7) yes C122 . H1221 . 1.000 no C123 . C124 . 1.391(7) yes C124 . C125 . 1.374(7) yes C124 . H1241 . 1.000 no C125 . C126 . 1.472(7) yes C126 . C127 . 1.378(7) yes C127 . C128 . 1.384(8) yes C127 . H1271 . 1.000 no C128 . C129 . 1.383(8) yes C128 . H1281 . 1.000 no C129 . C130 . 1.378(8) yes C129 . H1291 . 1.000 no C130 . H1301 . 1.000 no C131 . C132 . 1.371(11) yes C131 . C139 . 1.499(12) yes C131 . H1311 . 1.000 no C132 . C133 . 1.393(11) yes C132 . C153 . 1.493(10) yes C133 . C134 . 1.346(10) yes C133 . H1331 . 1.000 no C134 . C140 . 1.364(10) yes C134 . H1341 . 1.000 no C135 . C136 . 1.347(11) yes C135 . C140 . 1.519(10) yes C135 . H1351 . 1.000 no C136 . C137 . 1.354(13) yes C136 . H1361 . 1.000 no C137 . C138 . 1.293(13) yes C137 . H1371 . 1.000 no C138 . C139 . 1.357(10) yes C138 . H1381 . 1.000 no C139 . C140 . 1.412(9) yes C141 . C142 . 1.365(8) yes C141 . C149 . 1.419(8) yes C141 . H1411 . 1.000 no C142 . C143 . 1.404(7) yes C142 . C163 . 1.502(8) yes C143 . C144 . 1.357(8) yes C143 . H1431 . 1.000 no C144 . C150 . 1.396(8) yes C144 . H1441 . 1.000 no C145 . C146 . 1.356(9) yes C145 . C150 . 1.412(8) yes C145 . H1451 . 1.000 no C146 . C147 . 1.402(10) yes C146 . H1461 . 1.000 no C147 . C148 . 1.363(9) yes C147 . H1471 . 1.000 no C148 . C149 . 1.401(8) yes C148 . H1481 . 1.000 no C149 . C150 . 1.431(8) yes C151 . C152 . 1.471(9) yes C151 . H1511 . 1.000 no C151 . H1512 . 1.000 no C152 . H1521 . 1.000 no C152 . H1522 . 1.000 no C153 . H1531 . 1.000 no C153 . H1532 . 1.000 no C161 . C162 . 1.496(7) yes C161 . H1611 . 1.000 no C161 . H1612 . 1.000 no C162 . H1621 . 1.000 no C162 . H1622 . 1.000 no C163 . H1631 . 1.000 no C163 . H1632 . 1.000 no P1 . F101 . 1.566(5) yes P1 . F102 . 1.585(4) yes P1 . F103 . 1.575(5) yes P1 . F104 . 1.579(5) yes P1 . F105 . 1.592(5) yes P1 . F106 . 1.580(5) yes P2 . F201 . 1.586(4) yes P2 . F202 . 1.570(4) yes P2 . F203 . 1.593(3) yes P2 . F204 . 1.579(4) yes P2 . F205 . 1.581(4) yes P2 . F206 . 1.562(5) yes P3 . F301 . 1.576(4) yes P3 . F302 . 1.592(4) yes P3 . F303 . 1.588(4) yes P3 . F304 . 1.589(4) yes P3 . F305 . 1.581(4) yes P3 . F306 . 1.585(4) yes P4 . F401 . 1.585(4) yes P4 . F402 . 1.580(4) yes P4 . F403 . 1.527(7) yes P4 . F404 . 1.586(8) yes P4 . F405 . 1.633(7) yes P4 . F406 . 1.572(7) yes P4 . F413 . 1.589(7) yes P4 . F414 . 1.533(8) yes P4 . F415 . 1.537(7) yes P4 . F416 . 1.642(7) yes 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 . Ru1 . N2 . 78.96(16) yes N1 . Ru1 . N3 . 157.91(15) yes N2 . Ru1 . N3 . 78.96(16) yes N1 . Ru1 . N4 . 93.70(16) yes N2 . Ru1 . N4 . 100.42(15) yes N3 . Ru1 . N4 . 90.97(15) yes N1 . Ru1 . N5 . 101.94(16) yes N2 . Ru1 . N5 . 178.85(16) yes N3 . Ru1 . N5 . 100.15(15) yes N4 . Ru1 . N5 . 78.84(16) yes N1 . Ru1 . N6 . 89.97(15) yes N2 . Ru1 . N6 . 101.84(15) yes N3 . Ru1 . N6 . 93.85(15) yes N4 . Ru1 . N6 . 157.73(15) yes N5 . Ru1 . N6 . 78.91(16) yes C8 . O1 . C51 . 116.2(4) yes C52 . O2 . C53 . 108.8(4) yes C23 . O11 . C61 . 118.2(4) yes C62 . O12 . C63 . 115.0(5) yes Ru1 . N1 . C1 . 128.3(3) yes Ru1 . N1 . C5 . 113.7(3) yes C1 . N1 . C5 . 118.0(4) yes Ru1 . N2 . C6 . 119.0(3) yes Ru1 . N2 . C10 . 119.2(3) yes C6 . N2 . C10 . 121.8(4) yes Ru1 . N3 . C11 . 114.0(3) yes Ru1 . N3 . C15 . 127.6(3) yes C11 . N3 . C15 . 118.4(4) yes Ru1 . N4 . C16 . 128.2(3) yes Ru1 . N4 . C20 . 114.4(3) yes C16 . N4 . C20 . 117.4(4) yes Ru1 . N5 . C21 . 119.3(3) yes Ru1 . N5 . C25 . 119.5(3) yes C21 . N5 . C25 . 121.2(4) yes Ru1 . N6 . C26 . 113.9(3) yes Ru1 . N6 . C30 . 127.7(3) yes C26 . N6 . C30 . 118.4(4) yes N1 . C1 . C2 . 123.3(5) yes N1 . C1 . H11 . 118.555 no C2 . C1 . H11 . 118.146 no C1 . C2 . C3 . 118.9(5) yes C1 . C2 . H21 . 120.439 no C3 . C2 . H21 . 120.632 no C2 . C3 . C4 . 118.9(5) yes C2 . C3 . H31 . 120.305 no C4 . C3 . H31 . 120.832 no C3 . C4 . C5 . 120.1(5) yes C3 . C4 . H41 . 119.626 no C5 . C4 . H41 . 120.235 no C4 . C5 . N1 . 120.8(5) yes C4 . C5 . C6 . 123.9(4) yes N1 . C5 . C6 . 115.3(4) yes C5 . C6 . N2 . 112.9(4) yes C5 . C6 . C7 . 126.4(4) yes N2 . C6 . C7 . 120.6(5) yes C6 . C7 . C8 . 118.2(4) yes C6 . C7 . H71 . 120.961 no C8 . C7 . H71 . 120.821 no C7 . C8 . O1 . 123.3(4) yes C7 . C8 . C9 . 120.7(4) yes O1 . C8 . C9 . 115.9(5) yes C8 . C9 . C10 . 118.1(5) yes C8 . C9 . H91 . 120.676 no C10 . C9 . H91 . 121.222 no C9 . C10 . N2 . 120.4(4) yes C9 . C10 . C11 . 126.3(4) yes N2 . C10 . C11 . 113.1(4) yes C10 . C11 . N3 . 114.7(4) yes C10 . C11 . C12 . 124.5(4) yes N3 . C11 . C12 . 120.8(4) yes C11 . C12 . C13 . 119.8(5) yes C11 . C12 . H121 . 120.346 no C13 . C12 . H121 . 119.804 no C12 . C13 . C14 . 119.3(5) yes C12 . C13 . H131 . 120.380 no C14 . C13 . H131 . 120.356 no C13 . C14 . C15 . 118.8(5) yes C13 . C14 . H141 . 120.450 no C15 . C14 . H141 . 120.761 no C14 . C15 . N3 . 122.9(4) yes C14 . C15 . H151 . 118.405 no N3 . C15 . H151 . 118.648 no N4 . C16 . C17 . 123.0(5) yes N4 . C16 . H161 . 118.430 no C17 . C16 . H161 . 118.583 no C16 . C17 . C18 . 119.1(5) yes C16 . C17 . H171 . 120.629 no C18 . C17 . H171 . 120.310 no C17 . C18 . C19 . 119.0(5) yes C17 . C18 . H181 . 120.507 no C19 . C18 . H181 . 120.448 no C18 . C19 . C20 . 120.0(5) yes C18 . C19 . H191 . 119.752 no C20 . C19 . H191 . 120.189 no C19 . C20 . N4 . 121.4(4) yes C19 . C20 . C21 . 124.2(4) yes N4 . C20 . C21 . 114.3(4) yes C20 . C21 . N5 . 113.1(4) yes C20 . C21 . C22 . 126.1(4) yes N5 . C21 . C22 . 120.9(4) yes C21 . C22 . C23 . 118.4(5) yes C21 . C22 . H221 . 121.326 no C23 . C22 . H221 . 120.245 no C22 . C23 . O11 . 115.0(4) yes C22 . C23 . C24 . 120.5(4) yes O11 . C23 . C24 . 124.5(5) yes C23 . C24 . C25 . 118.2(5) yes C23 . C24 . H241 . 120.594 no C25 . C24 . H241 . 121.207 no C24 . C25 . N5 . 120.7(4) yes C24 . C25 . C26 . 127.0(4) yes N5 . C25 . C26 . 112.2(4) yes C25 . C26 . N6 . 115.5(4) yes C25 . C26 . C27 . 123.9(4) yes N6 . C26 . C27 . 120.6(4) yes C26 . C27 . C28 . 120.3(4) yes C26 . C27 . H271 . 119.856 no C28 . C27 . H271 . 119.793 no C27 . C28 . C29 . 118.9(5) yes C27 . C28 . H281 . 120.878 no C29 . C28 . H281 . 120.254 no C28 . C29 . C30 . 118.8(4) yes C28 . C29 . H291 . 120.979 no C30 . C29 . H291 . 120.182 no C29 . C30 . N6 . 122.9(4) yes C29 . C30 . H301 . 118.490 no N6 . C30 . H301 . 118.619 no C32 . C31 . C39 . 122.1(5) yes C32 . C31 . H311 . 118.889 no C39 . C31 . H311 . 118.961 no C31 . C32 . C33 . 118.7(5) yes C31 . C32 . C53 . 118.0(5) yes C33 . C32 . C53 . 123.3(5) yes C32 . C33 . C34 . 120.6(5) yes C32 . C33 . H331 . 120.035 no C34 . C33 . H331 . 119.330 no C33 . C34 . C40 . 121.0(5) yes C33 . C34 . H341 . 119.494 no C40 . C34 . H341 . 119.538 no C36 . C35 . C40 . 120.2(6) yes C36 . C35 . H351 . 120.035 no C40 . C35 . H351 . 119.749 no C35 . C36 . C37 . 120.4(5) yes C35 . C36 . H361 . 119.470 no C37 . C36 . H361 . 120.169 no C36 . C37 . C38 . 121.2(6) yes C36 . C37 . H371 . 119.222 no C38 . C37 . H371 . 119.552 no C37 . C38 . C39 . 120.1(6) yes C37 . C38 . H381 . 119.807 no C39 . C38 . H381 . 120.106 no C38 . C39 . C31 . 122.1(5) yes C38 . C39 . C40 . 119.1(5) yes C31 . C39 . C40 . 118.8(5) yes C35 . C40 . C34 . 122.2(5) yes C35 . C40 . C39 . 119.1(5) yes C34 . C40 . C39 . 118.8(5) yes C42 . C41 . C49 . 118.8(9) yes C42 . C41 . H411 . 121.623 no C49 . C41 . H411 . 119.548 no C41 . C42 . C43 . 120.1(8) yes C41 . C42 . C63 . 119.8(8) yes C43 . C42 . C63 . 120.1(7) yes C42 . C43 . C44 . 123.7(9) yes C42 . C43 . H431 . 118.488 no C44 . C43 . H431 . 117.717 no C43 . C44 . C50 . 116.2(10) yes C43 . C44 . H441 . 122.142 no C50 . C44 . H441 . 121.694 no C46 . C45 . C50 . 120.3(13) yes C46 . C45 . H451 . 118.796 no C50 . C45 . H451 . 120.915 no C45 . C46 . C47 . 122.2(11) yes C45 . C46 . H461 . 119.138 no C47 . C46 . H461 . 118.655 no C46 . C47 . C48 . 119.6(11) yes C46 . C47 . H471 . 120.602 no C48 . C47 . H471 . 119.761 no C47 . C48 . C49 . 120.6(12) yes C47 . C48 . H481 . 120.897 no C49 . C48 . H481 . 118.525 no C41 . C49 . C48 . 120.1(10) yes C41 . C49 . C50 . 120.9(8) yes C48 . C49 . C50 . 118.9(10) yes C49 . C50 . C44 . 119.8(9) yes C49 . C50 . C45 . 118.2(10) yes C44 . C50 . C45 . 122.0(12) yes O1 . C51 . C52 . 109.4(5) yes O1 . C51 . H511 . 109.721 no C52 . C51 . H511 . 109.796 no O1 . C51 . H512 . 109.083 no C52 . C51 . H512 . 109.369 no H511 . C51 . H512 . 109.468 no C51 . C52 . O2 . 111.8(4) yes C51 . C52 . H521 . 108.805 no O2 . C52 . H521 . 108.820 no C51 . C52 . H522 . 108.946 no O2 . C52 . H522 . 108.996 no H521 . C52 . H522 . 109.467 no C32 . C53 . O2 . 112.6(5) yes C32 . C53 . H531 . 108.903 no O2 . C53 . H531 . 108.155 no C32 . C53 . H532 . 108.647 no O2 . C53 . H532 . 108.984 no H531 . C53 . H532 . 109.466 no O11 . C61 . C62 . 105.9(6) yes O11 . C61 . H611 . 109.134 no C62 . C61 . H611 . 109.508 no O11 . C61 . H612 . 110.862 no C62 . C61 . H612 . 111.903 no H611 . C61 . H612 . 109.468 no C61 . C62 . O12 . 114.4(7) yes C61 . C62 . H621 . 108.568 no O12 . C62 . H621 . 108.856 no C61 . C62 . H622 . 107.564 no O12 . C62 . H622 . 107.860 no H621 . C62 . H622 . 109.468 no C42 . C63 . O12 . 111.6(7) yes C42 . C63 . H631 . 108.711 no O12 . C63 . H631 . 108.563 no C42 . C63 . H632 . 109.481 no O12 . C63 . H632 . 108.952 no H631 . C63 . H632 . 109.467 no N7 . Ru2 . N8 . 78.93(16) yes N7 . Ru2 . N9 . 157.88(15) yes N8 . Ru2 . N9 . 78.95(16) yes N7 . Ru2 . N10 . 94.54(16) yes N8 . Ru2 . N10 . 103.73(16) yes N9 . Ru2 . N10 . 90.26(16) yes N7 . Ru2 . N11 . 103.27(15) yes N8 . Ru2 . N11 . 176.69(17) yes N9 . Ru2 . N11 . 98.85(16) yes N10 . Ru2 . N11 . 78.67(16) yes N7 . Ru2 . N12 . 91.04(16) yes N8 . Ru2 . N12 . 98.36(16) yes N9 . Ru2 . N12 . 92.59(16) yes N10 . Ru2 . N12 . 157.86(16) yes N11 . Ru2 . N12 . 79.20(16) yes C108 . O21 . C151 . 118.8(5) yes C152 . O22 . C153 . 115.1(7) yes C123 . O31 . C161 . 116.8(4) yes C162 . O32 . C163 . 113.8(4) yes Ru2 . N7 . C101 . 128.2(3) yes Ru2 . N7 . C105 . 113.8(3) yes C101 . N7 . C105 . 118.0(4) yes Ru2 . N8 . C106 . 119.0(3) yes Ru2 . N8 . C110 . 119.4(3) yes C106 . N8 . C110 . 121.2(4) yes Ru2 . N9 . C111 . 114.0(3) yes Ru2 . N9 . C115 . 127.7(4) yes C111 . N9 . C115 . 118.3(4) yes Ru2 . N10 . C116 . 128.5(3) yes Ru2 . N10 . C120 . 114.1(3) yes C116 . N10 . C120 . 117.3(4) yes Ru2 . N11 . C121 . 120.1(3) yes Ru2 . N11 . C125 . 119.1(3) yes C121 . N11 . C125 . 120.7(4) yes Ru2 . N12 . C126 . 114.7(3) yes Ru2 . N12 . C130 . 127.5(4) yes C126 . N12 . C130 . 117.8(4) yes N7 . C101 . C102 . 122.9(5) yes N7 . C101 . H1011 . 118.711 no C102 . C101 . H1011 . 118.423 no C101 . C102 . C103 . 119.3(5) yes C101 . C102 . H1021 . 120.345 no C103 . C102 . H1021 . 120.322 no C102 . C103 . C104 . 118.9(5) yes C102 . C103 . H1031 . 120.368 no C104 . C103 . H1031 . 120.669 no C103 . C104 . C105 . 119.4(5) yes C103 . C104 . H1041 . 119.969 no C105 . C104 . H1041 . 120.615 no C104 . C105 . N7 . 121.4(5) yes C104 . C105 . C106 . 123.3(4) yes N7 . C105 . C106 . 115.3(4) yes C105 . C106 . N8 . 112.7(4) yes C105 . C106 . C107 . 126.9(5) yes N8 . C106 . C107 . 120.4(5) yes C106 . C107 . C108 . 119.0(5) yes C106 . C107 . H1071 . 120.798 no C108 . C107 . H1071 . 120.184 no C107 . C108 . O21 . 115.9(5) yes C107 . C108 . C109 . 119.9(5) yes O21 . C108 . C109 . 124.2(5) yes C108 . C109 . C110 . 118.2(5) yes C108 . C109 . H1091 . 120.507 no C110 . C109 . H1091 . 121.324 no C109 . C110 . N8 . 121.3(5) yes C109 . C110 . C111 . 126.1(5) yes N8 . C110 . C111 . 112.6(4) yes C110 . C111 . N9 . 114.9(4) yes C110 . C111 . C112 . 124.3(5) yes N9 . C111 . C112 . 120.8(5) yes C111 . C112 . C113 . 119.9(5) yes C111 . C112 . H1121 . 120.289 no C113 . C112 . H1121 . 119.784 no C112 . C113 . C114 . 119.0(5) yes C112 . C113 . H1131 . 120.657 no C114 . C113 . H1131 . 120.376 no C113 . C114 . C115 . 119.6(5) yes C113 . C114 . H1141 . 119.978 no C115 . C114 . H1141 . 120.458 no C114 . C115 . N9 . 122.4(5) yes C114 . C115 . H1151 . 118.471 no N9 . C115 . H1151 . 119.098 no N10 . C116 . C117 . 123.4(5) yes N10 . C116 . H1161 . 118.562 no C117 . C116 . H1161 . 118.058 no C116 . C117 . C118 . 118.8(5) yes C116 . C117 . H1171 . 121.048 no C118 . C117 . H1171 . 120.108 no C117 . C118 . C119 . 119.0(5) yes C117 . C118 . H1181 . 120.602 no C119 . C118 . H1181 . 120.435 no C118 . C119 . C120 . 119.5(5) yes C118 . C119 . H1191 . 120.150 no C120 . C119 . H1191 . 120.387 no N10 . C120 . C119 . 122.0(4) yes N10 . C120 . C121 . 114.8(4) yes C119 . C120 . C121 . 123.2(4) yes C120 . C121 . N11 . 112.1(4) yes C120 . C121 . C122 . 126.2(4) yes N11 . C121 . C122 . 121.7(4) yes C121 . C122 . C123 . 118.0(4) yes C121 . C122 . H1221 . 121.093 no C123 . C122 . H1221 . 120.907 no C122 . C123 . O31 . 124.2(4) yes C122 . C123 . C124 . 120.4(4) yes O31 . C123 . C124 . 115.4(4) yes C123 . C124 . C125 . 119.1(4) yes C123 . C124 . H1241 . 119.941 no C125 . C124 . H1241 . 120.911 no C124 . C125 . N11 . 120.1(4) yes C124 . C125 . C126 . 127.2(4) yes N11 . C125 . C126 . 112.6(4) yes C125 . C126 . N12 . 114.5(4) yes C125 . C126 . C127 . 123.8(5) yes N12 . C126 . C127 . 121.7(5) yes C126 . C127 . C128 . 119.5(5) yes C126 . C127 . H1271 . 120.621 no C128 . C127 . H1271 . 119.926 no C127 . C128 . C129 . 119.2(5) yes C127 . C128 . H1281 . 120.278 no C129 . C128 . H1281 . 120.485 no C128 . C129 . C130 . 118.8(5) yes C128 . C129 . H1291 . 120.082 no C130 . C129 . H1291 . 121.145 no C129 . C130 . N12 . 123.1(5) yes C129 . C130 . H1301 . 118.180 no N12 . C130 . H1301 . 118.746 no C132 . C131 . C139 . 120.7(8) yes C132 . C131 . H1311 . 120.053 no C139 . C131 . H1311 . 119.216 no C131 . C132 . C133 . 116.7(7) yes C131 . C132 . C153 . 123.9(8) yes C133 . C132 . C153 . 119.4(8) yes C132 . C133 . C134 . 127.3(8) yes C132 . C133 . H1331 . 116.100 no C134 . C133 . H1331 . 116.624 no C133 . C134 . C140 . 115.6(8) yes C133 . C134 . H1341 . 121.808 no C140 . C134 . H1341 . 122.553 no C136 . C135 . C140 . 115.4(7) yes C136 . C135 . H1351 . 123.808 no C140 . C135 . H1351 . 120.756 no C135 . C136 . C137 . 124.4(8) yes C135 . C136 . H1361 . 117.769 no C137 . C136 . H1361 . 117.833 no C136 . C137 . C138 . 121.2(10) yes C136 . C137 . H1371 . 119.235 no C138 . C137 . H1371 . 119.525 no C137 . C138 . C139 . 121.8(10) yes C137 . C138 . H1381 . 118.835 no C139 . C138 . H1381 . 119.330 no C131 . C139 . C138 . 124.4(8) yes C131 . C139 . C140 . 114.2(6) yes C138 . C139 . C140 . 121.4(7) yes C135 . C140 . C139 . 115.7(6) yes C135 . C140 . C134 . 118.9(7) yes C139 . C140 . C134 . 125.4(7) yes C142 . C141 . C149 . 121.1(5) yes C142 . C141 . H1411 . 119.433 no C149 . C141 . H1411 . 119.433 no C141 . C142 . C143 . 119.6(5) yes C141 . C142 . C163 . 122.6(5) yes C143 . C142 . C163 . 117.7(5) yes C142 . C143 . C144 . 120.8(5) yes C142 . C143 . H1431 . 119.948 no C144 . C143 . H1431 . 119.183 no C143 . C144 . C150 . 121.3(5) yes C143 . C144 . H1441 . 119.520 no C150 . C144 . H1441 . 119.173 no C146 . C145 . C150 . 120.8(6) yes C146 . C145 . H1451 . 119.492 no C150 . C145 . H1451 . 119.747 no C145 . C146 . C147 . 120.9(6) yes C145 . C146 . H1461 . 119.270 no C147 . C146 . H1461 . 119.807 no C146 . C147 . C148 . 120.1(6) yes C146 . C147 . H1471 . 119.953 no C148 . C147 . H1471 . 119.968 no C147 . C148 . C149 . 120.8(6) yes C147 . C148 . H1481 . 119.505 no C149 . C148 . H1481 . 119.654 no C141 . C149 . C148 . 122.6(5) yes C141 . C149 . C150 . 118.2(5) yes C148 . C149 . C150 . 119.2(5) yes C149 . C150 . C145 . 118.2(5) yes C149 . C150 . C144 . 118.9(5) yes C145 . C150 . C144 . 122.8(5) yes O21 . C151 . C152 . 108.6(6) yes O21 . C151 . H1511 . 109.983 no C152 . C151 . H1511 . 108.165 no O21 . C151 . H1512 . 109.626 no C152 . C151 . H1512 . 110.998 no H1511 . C151 . H1512 . 109.467 no C151 . C152 . O22 . 109.0(6) yes C151 . C152 . H1521 . 110.731 no O22 . C152 . H1521 . 110.268 no C151 . C152 . H1522 . 108.333 no O22 . C152 . H1522 . 109.014 no H1521 . C152 . H1522 . 109.466 no C132 . C153 . O22 . 115.5(7) yes C132 . C153 . H1531 . 107.961 no O22 . C153 . H1531 . 108.658 no C132 . C153 . H1532 . 107.417 no O22 . C153 . H1532 . 107.733 no H1531 . C153 . H1532 . 109.468 no O31 . C161 . C162 . 107.7(4) yes O31 . C161 . H1611 . 109.667 no C162 . C161 . H1611 . 110.372 no O31 . C161 . H1612 . 109.967 no C162 . C161 . H1612 . 109.631 no H1611 . C161 . H1612 . 109.468 no C161 . C162 . O32 . 109.5(4) yes C161 . C162 . H1621 . 109.507 no O32 . C162 . H1621 . 110.114 no C161 . C162 . H1622 . 109.234 no O32 . C162 . H1622 . 109.012 no H1621 . C162 . H1622 . 109.466 no C142 . C163 . O32 . 116.3(4) yes C142 . C163 . H1631 . 107.890 no O32 . C163 . H1631 . 108.559 no C142 . C163 . H1632 . 107.643 no O32 . C163 . H1632 . 106.887 no H1631 . C163 . H1632 . 109.467 no F101 . P1 . F102 . 89.7(3) yes F101 . P1 . F103 . 178.3(4) yes F102 . P1 . F103 . 91.7(3) yes F101 . P1 . F104 . 91.7(3) yes F102 . P1 . F104 . 91.0(2) yes F103 . P1 . F104 . 89.2(3) yes F101 . P1 . F105 . 90.1(3) yes F102 . P1 . F105 . 179.8(3) yes F103 . P1 . F105 . 88.5(3) yes F104 . P1 . F105 . 88.9(3) yes F101 . P1 . F106 . 89.6(4) yes F102 . P1 . F106 . 89.2(2) yes F103 . P1 . F106 . 89.5(3) yes F104 . P1 . F106 . 178.7(3) yes F105 . P1 . F106 . 90.9(3) yes F201 . P2 . F202 . 90.4(2) yes F201 . P2 . F203 . 179.2(2) yes F202 . P2 . F203 . 89.0(2) yes F201 . P2 . F204 . 90.3(2) yes F202 . P2 . F204 . 179.0(3) yes F203 . P2 . F204 . 90.4(2) yes F201 . P2 . F205 . 89.0(2) yes F202 . P2 . F205 . 89.5(3) yes F203 . P2 . F205 . 90.5(2) yes F204 . P2 . F205 . 89.7(3) yes F201 . P2 . F206 . 91.3(3) yes F202 . P2 . F206 . 91.0(3) yes F203 . P2 . F206 . 89.1(2) yes F204 . P2 . F206 . 89.7(4) yes F205 . P2 . F206 . 179.3(3) yes F301 . P3 . F302 . 89.7(3) yes F301 . P3 . F303 . 90.3(3) yes F302 . P3 . F303 . 90.5(3) yes F301 . P3 . F304 . 179.6(3) yes F302 . P3 . F304 . 90.1(3) yes F303 . P3 . F304 . 89.4(2) yes F301 . P3 . F305 . 91.2(3) yes F302 . P3 . F305 . 179.1(3) yes F303 . P3 . F305 . 89.4(2) yes F304 . P3 . F305 . 89.0(2) yes F301 . P3 . F306 . 92.4(3) yes F302 . P3 . F306 . 89.2(3) yes F303 . P3 . F306 . 177.3(3) yes F304 . P3 . F306 . 87.9(2) yes F305 . P3 . F306 . 90.9(2) yes F401 . P4 . F402 . 180.0(3) yes F401 . P4 . F403 . 94.9(4) yes F402 . P4 . F403 . 85.1(4) yes F401 . P4 . F404 . 89.8(4) yes F402 . P4 . F404 . 90.2(4) yes F403 . P4 . F404 . 92.7(6) yes F401 . P4 . F405 . 91.0(3) yes F402 . P4 . F405 . 89.0(4) yes F403 . P4 . F405 . 173.6(6) yes F404 . P4 . F405 . 84.8(5) yes F401 . P4 . F406 . 97.3(4) yes F402 . P4 . F406 . 82.7(4) yes F403 . P4 . F406 . 95.6(5) yes F404 . P4 . F406 . 168.6(5) yes F405 . P4 . F406 . 86.1(5) yes F401 . P4 . F413 . 87.7(4) yes F402 . P4 . F413 . 92.3(4) yes F401 . P4 . F414 . 90.5(4) yes F402 . P4 . F414 . 89.5(4) yes F401 . P4 . F415 . 86.9(4) yes F402 . P4 . F415 . 93.1(4) yes F401 . P4 . F416 . 82.5(3) yes F402 . P4 . F416 . 97.5(4) yes F413 . P4 . F414 . 88.6(6) yes F413 . P4 . F415 . 173.3(6) yes F414 . P4 . F415 . 95.4(7) yes F413 . P4 . F416 . 85.4(5) yes F414 . P4 . F416 . 170.9(6) yes F415 . P4 . F416 . 89.9(7) yes