Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Catherine E Housecroft' ; ? # Address for author 1 ; ; ? # Footnote for author 1 ; 'Jonathon E Beves' ; ? # Address 2 ; ; ? # Footnote 2 ; 'Edwin C. Constable' '' '' 'Cameron Kepert' '' '' 'Markus Neuburger' '' '' 'David J Price' '' '' 'Silvia Schaffner' '' '' 'Jennifer A Zampese' '' '' _publ_contact_author_name 'Catherine E Housecroft' _publ_contact_author_email CATHERINE.HOUSECROFT@UNIBAS.CH _publ_section_title ; Curly-curly, loop-loop: homoleptic metal(II) complexes of pyridinecarbaldehyde 4'-(2,2':6',2"-terpyridyl)hydrazones and their coordination polymers ; _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_address ; Chemical Crystallography Laboratory, Department of Chemistry, University of Nowhere, Nowhere, NO1 4T, UK. ; _publ_contact_author_fax '+44 1865 000000' _publ_contact_author_phone '+44 1865 000000' # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # 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 E. The figures will be sent by e-mail. ; _publ_requested_category EO # choose from: FI FM FO CI CM CO AD _publ_requested_coeditor_name 'Prof William Clegg' _publ_requested_journal 'Section E' # Attachment 'Fe_1_2_MN.cif' data_jb451 _database_code_depnum_ccdc_archive 'CCDC 692938' _audit_creation_date 06-12-08 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '12080929 jb451_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 10.2902(2) _cell_length_b 13.5226(3) _cell_length_c 20.1859(4) _cell_angle_alpha 89.1662(9) _cell_angle_beta 79.5970(12) _cell_angle_gamma 67.9900(11) _cell_volume 2557.00(9) _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 57.7998 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' 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 1 # Given Formula = C84 H64 F24 Fe2 N24 P4 # Dc = 1.36 Fooo = 1174.00 Mu = 4.43 M = 1050.57 # Found Formula = C94 H79 F24 Fe2 N29 P4 # Dc = 1.50 FOOO = 1174.00 Mu = 4.52 M = 1153.20 _chemical_formula_sum 'C94 H79 F24 Fe2 N29 P4' _chemical_formula_moiety '2(C42 H32 Fe N12), 4(F6 P), 5(C2 H3 N)' _chemical_compound_source ? _chemical_formula_weight 2306.40 _cell_measurement_reflns_used 11694 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_max 0.22 _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1174 _exptl_absorpt_coefficient_mu 0.452 # Sheldrick geometric approximatio 0.92 0.97 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.97 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _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 23137 _reflns_number_total 11743 _diffrn_reflns_av_R_equivalents 0.032 # Number of reflections with Friedels Law is 11743 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 11728 _diffrn_reflns_theta_min 1.873 _diffrn_reflns_theta_max 27.485 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.485 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min -17 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _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 0.53 _refine_ls_number_reflns 7102 _refine_ls_number_restraints 168 _refine_ls_number_parameters 703 #_refine_ls_R_factor_ref 0.0459 _refine_ls_wR_factor_ref 0.0534 _refine_ls_goodness_of_fit_ref 1.1656 #_reflns_number_all 11627 _refine_ls_R_factor_all 0.0831 _refine_ls_wR_factor_all 0.0743 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>2.3\s(I) _reflns_number_gt 7102 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_gt 0.0534 _refine_ls_shift/su_max 0.001298 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.896 0.851 0.579 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # 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). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: 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 atomsattached 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 0.26667(4) 0.23084(3) 0.757531(17) 0.0285 1.0000 Uani . . . . . . N1 N 0.1100(2) 0.31934(18) 0.71271(11) 0.0325 1.0000 Uani . . . . . . N2 N 0.1336(2) 0.30729(17) 0.83403(10) 0.0295 1.0000 Uani . . . . . . N3 N 0.3810(2) 0.17033(17) 0.82798(10) 0.0292 1.0000 Uani . . . . . . N4 N 0.3636(2) 0.33044(17) 0.73166(10) 0.0316 1.0000 Uani . . . . . . N5 N 0.3996(2) 0.15278(17) 0.68169(10) 0.0306 1.0000 Uani . . . . . . N6 N 0.2129(2) 0.10487(17) 0.75739(10) 0.0306 1.0000 Uani . . . . . . N7 N -0.1627(2) 0.4571(2) 1.00401(12) 0.0410 1.0000 Uani . . . . . . N8 N -0.2963(2) 0.52765(18) 1.00149(12) 0.0381 1.0000 Uani . . . . . . N9 N -0.8081(3) 0.7857(2) 1.07544(15) 0.0505 1.0000 Uani . . . . . . N10 N 0.6959(3) -0.0285(2) 0.51979(12) 0.0426 1.0000 Uani . . . . . . N11 N 0.7942(2) 0.0034(2) 0.48143(11) 0.0393 1.0000 Uani . . . . . . N12 N 1.2044(3) -0.0007(2) 0.29815(12) 0.0465 1.0000 Uani . . . . . . N13 N 0.8428(4) 0.2896(3) 0.5157(2) 0.0789 1.0000 Uani D U . . . . N14 N 0.4544(5) 0.3624(4) 0.1760(3) 0.0987 1.0000 Uani D U . . . . N15 N 0.3136(10) -0.0468(7) 0.9108(5) 0.0895 0.5000 Uani D U . . . . C1 C 0.1133(3) 0.3252(2) 0.64616(14) 0.0396 1.0000 Uani . . . . . . C2 C 0.0011(4) 0.3955(3) 0.61949(16) 0.0500 1.0000 Uani . . . . . . C3 C -0.1189(4) 0.4621(3) 0.66263(17) 0.0545 1.0000 Uani . . . . . . C4 C -0.1245(3) 0.4568(3) 0.73150(16) 0.0463 1.0000 Uani . . . . . . C5 C -0.0082(3) 0.3859(2) 0.75547(13) 0.0336 1.0000 Uani . . . . . . C6 C 0.0036(3) 0.3776(2) 0.82712(13) 0.0303 1.0000 Uani . . . . . . C7 C -0.0992(3) 0.4314(2) 0.88205(13) 0.0331 1.0000 Uani . . . . . . C8 C -0.0655(3) 0.4117(2) 0.94633(13) 0.0327 1.0000 Uani . . . . . . C9 C 0.0708(3) 0.3401(2) 0.95302(13) 0.0336 1.0000 Uani . . . . . . C10 C 0.1673(3) 0.2895(2) 0.89585(12) 0.0308 1.0000 Uani . . . . . . C11 C 0.3141(3) 0.2101(2) 0.89208(12) 0.0313 1.0000 Uani . . . . . . C12 C 0.3791(3) 0.1769(2) 0.94696(14) 0.0374 1.0000 Uani . . . . . . C13 C 0.5168(3) 0.1007(2) 0.93724(15) 0.0414 1.0000 Uani . . . . . . C14 C 0.5846(3) 0.0589(2) 0.87248(15) 0.0406 1.0000 Uani . . . . . . C15 C 0.5140(3) 0.0952(2) 0.81961(13) 0.0343 1.0000 Uani . . . . . . C16 C 0.3292(3) 0.4278(2) 0.76085(14) 0.0383 1.0000 Uani . . . . . . C17 C 0.4041(3) 0.4921(2) 0.73940(16) 0.0456 1.0000 Uani . . . . . . C18 C 0.5172(3) 0.4559(3) 0.68576(16) 0.0471 1.0000 Uani . . . . . . C19 C 0.5518(3) 0.3572(2) 0.65378(15) 0.0420 1.0000 Uani . . . . . . C20 C 0.4731(3) 0.2959(2) 0.67718(13) 0.0329 1.0000 Uani . . . . . . C21 C 0.4942(3) 0.1912(2) 0.64707(12) 0.0315 1.0000 Uani . . . . . . C22 C 0.5948(3) 0.1352(2) 0.59168(12) 0.0336 1.0000 Uani . . . . . . C23 C 0.5979(3) 0.0356(2) 0.57206(12) 0.0330 1.0000 Uani . . . . . . C24 C 0.4985(3) -0.0038(2) 0.60796(13) 0.0354 1.0000 Uani . . . . . . C25 C 0.4013(3) 0.0572(2) 0.66228(13) 0.0325 1.0000 Uani . . . . . . C26 C 0.2914(3) 0.0293(2) 0.70671(12) 0.0319 1.0000 Uani . . . . . . C27 C 0.2689(3) -0.0651(2) 0.69981(14) 0.0379 1.0000 Uani . . . . . . C28 C 0.1646(3) -0.0833(2) 0.74599(15) 0.0438 1.0000 Uani . . . . . . C29 C 0.0850(3) -0.0069(2) 0.79757(15) 0.0420 1.0000 Uani . . . . . . C30 C 0.1122(3) 0.0853(2) 0.80176(13) 0.0346 1.0000 Uani . . . . . . C31 C -0.3822(3) 0.5566(2) 1.05832(14) 0.0411 1.0000 Uani . . . . . . C32 C -0.5286(3) 0.6338(2) 1.06239(15) 0.0401 1.0000 Uani . . . . . . C33 C -0.6149(3) 0.6715(2) 1.12538(16) 0.0436 1.0000 Uani . . . . . . C34 C -0.7507(3) 0.7467(3) 1.12890(17) 0.0490 1.0000 Uani . . . . . . C35 C -0.7251(3) 0.7473(3) 1.01464(17) 0.0490 1.0000 Uani . . . . . . C36 C -0.5863(3) 0.6733(2) 1.00586(16) 0.0448 1.0000 Uani . . . . . . C37 C 0.8877(3) -0.0672(2) 0.43837(13) 0.0403 1.0000 Uani . . . . . . C38 C 0.9969(3) -0.0429(2) 0.39166(13) 0.0375 1.0000 Uani . . . . . . C39 C 1.0101(3) 0.0548(2) 0.39309(15) 0.0442 1.0000 Uani . . . . . . C40 C 1.1137(3) 0.0722(3) 0.34586(16) 0.0473 1.0000 Uani . . . . . . C41 C 1.1902(3) -0.0948(3) 0.29764(14) 0.0442 1.0000 Uani . . . . . . C42 C 1.0907(3) -0.1205(3) 0.34239(14) 0.0406 1.0000 Uani . . . . . . C43 C 0.8186(5) 0.3347(3) 0.4695(2) 0.0736 1.0000 Uani D U . . . . C44 C 0.7852(9) 0.3912(5) 0.4087(3) 0.1206 1.0000 Uani D U . . . . C45 C 0.4382(5) 0.2873(4) 0.1956(3) 0.0847 1.0000 Uani D U . . . . C46 C 0.4091(7) 0.1962(4) 0.2240(4) 0.1126 1.0000 Uani D U . . . . C47 C 0.2145(12) -0.0070(6) 0.9507(4) 0.0824 0.5000 Uani D U . . . . C48 C 0.0756(15) 0.0287(11) 0.9966(6) 0.1734 0.5000 Uani D U . . . . P1 P -0.01955(9) 0.71290(6) 0.84092(4) 0.0448 1.0000 Uani D U . . . . P2 P 0.36912(11) 0.32296(7) 0.46115(4) 0.0572 1.0000 Uani D U . . . . F1 F 0.0601(2) 0.59714(16) 0.86927(10) 0.0629 1.0000 Uani D U . . . . F2 F -0.0949(2) 0.82686(17) 0.81415(12) 0.0746 1.0000 Uani D U . . . . F3 F 0.0350(3) 0.7624(2) 0.89571(18) 0.1050 1.0000 Uani D U . . . . F4 F -0.0714(4) 0.6582(2) 0.78844(13) 0.0953 1.0000 Uani D U . . . . F5 F -0.1598(2) 0.7270(2) 0.89409(12) 0.0831 1.0000 Uani D U . . . . F6 F 0.1209(3) 0.6954(2) 0.78785(16) 0.1049 1.0000 Uani D U . . . . F11 F 0.2106(3) 0.4103(2) 0.47412(14) 0.0992 1.0000 Uani D U . . . . F12 F 0.5238(3) 0.2314(2) 0.44792(13) 0.0817 1.0000 Uani D U . . . . F13 F 0.3107(3) 0.2376(2) 0.49759(16) 0.1000 1.0000 Uani D U . . . . F14 F 0.4227(5) 0.4073(3) 0.4278(2) 0.1503 1.0000 Uani D U . . . . F15 F 0.3867(3) 0.35512(19) 0.53266(12) 0.0840 1.0000 Uani D U . . . . F16 F 0.3481(4) 0.2865(3) 0.39128(15) 0.1536 1.0000 Uani D U . . . . H7 H -0.1381 0.4409 1.0434 0.0367 1.0000 Uiso R . . . . . H10 H 0.6969 -0.0924 0.5117 0.0426 1.0000 Uiso R . . . . . H11 H 0.1954 0.2794 0.6165 0.0419 1.0000 Uiso R . . . . . H21 H 0.0073 0.3969 0.5724 0.0552 1.0000 Uiso R . . . . . H31 H -0.1966 0.5108 0.6460 0.0563 1.0000 Uiso R . . . . . H41 H -0.2057 0.5019 0.7617 0.0465 1.0000 Uiso R . . . . . H71 H -0.1889 0.4800 0.8770 0.0325 1.0000 Uiso R . . . . . H91 H 0.0957 0.3275 0.9953 0.0327 1.0000 Uiso R . . . . . H121 H 0.3304 0.2056 0.9910 0.0360 1.0000 Uiso R . . . . . H131 H 0.5631 0.0774 0.9738 0.0411 1.0000 Uiso R . . . . . H141 H 0.6776 0.0074 0.8643 0.0381 1.0000 Uiso R . . . . . H151 H 0.5595 0.0666 0.7754 0.0320 1.0000 Uiso R . . . . . H161 H 0.2508 0.4526 0.7974 0.0391 1.0000 Uiso R . . . . . H171 H 0.3777 0.5598 0.7611 0.0482 1.0000 Uiso R . . . . . H181 H 0.5708 0.4983 0.6708 0.0513 1.0000 Uiso R . . . . . H191 H 0.6271 0.3321 0.6166 0.0454 1.0000 Uiso R . . . . . H221 H 0.6583 0.1638 0.5681 0.0306 1.0000 Uiso R . . . . . H241 H 0.4978 -0.0702 0.5950 0.0343 1.0000 Uiso R . . . . . H271 H 0.3236 -0.1154 0.6640 0.0382 1.0000 Uiso R . . . . . H281 H 0.1473 -0.1466 0.7425 0.0440 1.0000 Uiso R . . . . . H291 H 0.0129 -0.0179 0.8293 0.0411 1.0000 Uiso R . . . . . H301 H 0.0579 0.1382 0.8371 0.0343 1.0000 Uiso R . . . . . H311 H -0.3518 0.5288 1.0991 0.0397 1.0000 Uiso R . . . . . H331 H -0.5809 0.6459 1.1652 0.0433 1.0000 Uiso R . . . . . H341 H -0.8096 0.7730 1.1716 0.0472 1.0000 Uiso R . . . . . H351 H -0.7637 0.7727 0.9754 0.0512 1.0000 Uiso R . . . . . H361 H -0.5313 0.6498 0.9623 0.0430 1.0000 Uiso R . . . . . H371 H 0.8875 -0.1373 0.4363 0.0393 1.0000 Uiso R . . . . . H391 H 0.9498 0.1080 0.4256 0.0444 1.0000 Uiso R . . . . . H401 H 1.1214 0.1395 0.3474 0.0484 1.0000 Uiso R . . . . . H411 H 1.2539 -0.1471 0.2644 0.0423 1.0000 Uiso R . . . . . H421 H 1.0855 -0.1892 0.3399 0.0418 1.0000 Uiso R . . . . . H441 H 0.8206 0.4483 0.4067 0.1573 1.0000 Uiso R . . . . . H442 H 0.6829 0.4193 0.4134 0.1572 1.0000 Uiso R . . . . . H443 H 0.8298 0.3422 0.3698 0.1572 1.0000 Uiso R . . . . . H461 H 0.4816 0.1336 0.1983 0.1570 1.0000 Uiso R . . . . . H462 H 0.4169 0.1922 0.2715 0.1571 1.0000 Uiso R . . . . . H463 H 0.3150 0.2014 0.2185 0.1572 1.0000 Uiso R . . . . . H481 H 0.0657 0.0840 1.0294 0.1900 0.5000 Uiso R . . . . . H482 H 0.0658 -0.0321 1.0198 0.1900 0.5000 Uiso R . . . . . H483 H 0.0021 0.0565 0.9695 0.1900 0.5000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02597(17) 0.03208(19) 0.02457(17) 0.00138(13) -0.00016(12) -0.00975(13) N1 0.0312(11) 0.0364(11) 0.0314(11) 0.0047(9) -0.0053(8) -0.0148(9) N2 0.0253(10) 0.0313(11) 0.0289(10) 0.0026(8) -0.0017(8) -0.0089(8) N3 0.0235(9) 0.0327(11) 0.0298(10) 0.0023(8) -0.0010(8) -0.0105(8) N4 0.0294(10) 0.0350(11) 0.0284(10) 0.0056(8) -0.0051(8) -0.0102(9) N5 0.0283(10) 0.0334(11) 0.0281(10) 0.0036(8) -0.0021(8) -0.0109(9) N6 0.0253(10) 0.0353(11) 0.0290(10) 0.0036(8) -0.0029(8) -0.0101(8) N7 0.0280(11) 0.0487(14) 0.0345(12) -0.0071(10) -0.0019(9) -0.0027(10) N8 0.0298(11) 0.0361(12) 0.0420(12) -0.0055(10) -0.0014(9) -0.0076(9) N9 0.0331(12) 0.0461(14) 0.0647(17) -0.0066(13) -0.0053(12) -0.0079(11) N10 0.0394(12) 0.0495(14) 0.0351(12) -0.0085(10) 0.0091(10) -0.0196(11) N11 0.0367(12) 0.0482(14) 0.0276(11) -0.0008(9) 0.0020(9) -0.0136(10) N12 0.0373(13) 0.0557(16) 0.0376(13) 0.0055(11) 0.0011(10) -0.0115(11) N13 0.092(3) 0.069(2) 0.072(2) -0.0009(18) -0.014(2) -0.027(2) N14 0.099(3) 0.094(3) 0.099(3) -0.019(3) -0.019(2) -0.030(3) N15 0.114(6) 0.083(5) 0.104(6) 0.038(4) -0.055(5) -0.059(5) C1 0.0404(14) 0.0487(16) 0.0325(13) 0.0071(12) -0.0078(11) -0.0198(13) C2 0.0534(18) 0.067(2) 0.0355(15) 0.0138(14) -0.0166(13) -0.0256(16) C3 0.0424(17) 0.070(2) 0.0493(17) 0.0208(16) -0.0193(14) -0.0148(15) C4 0.0325(14) 0.0527(18) 0.0468(16) 0.0113(13) -0.0092(12) -0.0079(12) C5 0.0322(12) 0.0355(13) 0.0335(13) 0.0056(10) -0.0048(10) -0.0139(11) C6 0.0297(12) 0.0303(12) 0.0321(12) 0.0029(10) -0.0056(10) -0.0128(10) C7 0.0248(11) 0.0327(13) 0.0378(13) -0.0008(10) -0.0028(10) -0.0076(10) C8 0.0319(12) 0.0311(13) 0.0325(13) -0.0049(10) 0.0007(10) -0.0116(10) C9 0.0294(12) 0.0389(14) 0.0291(12) -0.0006(10) -0.0032(10) -0.0099(10) C10 0.0263(11) 0.0321(12) 0.0305(12) 0.0005(10) -0.0011(9) -0.0090(10) C11 0.0269(11) 0.0342(13) 0.0292(12) 0.0024(10) -0.0005(9) -0.0097(10) C12 0.0368(13) 0.0421(15) 0.0302(13) 0.0043(11) -0.0059(10) -0.0118(11) C13 0.0338(13) 0.0467(16) 0.0413(15) 0.0094(12) -0.0135(11) -0.0099(12) C14 0.0267(12) 0.0391(15) 0.0488(16) 0.0036(12) -0.0055(11) -0.0052(11) C15 0.0291(12) 0.0340(13) 0.0332(13) -0.0004(10) 0.0024(10) -0.0084(10) C16 0.0385(14) 0.0396(15) 0.0361(13) 0.0010(11) -0.0061(11) -0.0144(12) C17 0.0501(17) 0.0375(15) 0.0508(17) 0.0020(12) -0.0096(13) -0.0185(13) C18 0.0516(17) 0.0454(16) 0.0511(17) 0.0125(13) -0.0097(14) -0.0264(14) C19 0.0392(14) 0.0510(17) 0.0384(14) 0.0084(12) -0.0018(11) -0.0225(13) C20 0.0306(12) 0.0376(13) 0.0294(12) 0.0065(10) -0.0057(10) -0.0118(10) C21 0.0294(12) 0.0381(13) 0.0267(12) 0.0041(10) -0.0034(9) -0.0133(10) C22 0.0287(12) 0.0442(15) 0.0261(11) 0.0038(10) -0.0007(9) -0.0139(11) C23 0.0268(11) 0.0423(14) 0.0236(11) -0.0002(10) -0.0009(9) -0.0076(10) C24 0.0356(13) 0.0396(14) 0.0285(12) -0.0004(10) -0.0008(10) -0.0138(11) C25 0.0280(12) 0.0388(14) 0.0288(12) 0.0004(10) -0.0013(9) -0.0122(10) C26 0.0307(12) 0.0347(13) 0.0277(12) 0.0022(10) -0.0029(10) -0.0107(10) C27 0.0400(14) 0.0394(14) 0.0340(13) -0.0011(11) -0.0023(11) -0.0165(12) C28 0.0452(15) 0.0418(15) 0.0479(16) 0.0069(12) -0.0057(13) -0.0220(13) C29 0.0367(14) 0.0499(17) 0.0412(15) 0.0101(12) 0.0004(11) -0.0222(12) C30 0.0266(12) 0.0391(14) 0.0334(13) 0.0018(10) -0.0001(10) -0.0097(10) C31 0.0314(13) 0.0458(16) 0.0373(14) -0.0083(12) 0.0002(11) -0.0075(12) C32 0.0291(13) 0.0382(15) 0.0479(16) -0.0057(12) -0.0005(11) -0.0098(11) C33 0.0312(13) 0.0493(17) 0.0442(16) -0.0075(13) -0.0003(11) -0.0111(12) C34 0.0318(14) 0.0529(18) 0.0539(18) -0.0105(14) 0.0036(13) -0.0113(13) C35 0.0459(16) 0.0458(17) 0.0546(18) 0.0007(14) -0.0127(14) -0.0150(14) C36 0.0384(15) 0.0459(16) 0.0452(16) -0.0071(13) -0.0010(12) -0.0132(13) C37 0.0379(14) 0.0480(16) 0.0308(13) -0.0031(11) -0.0004(11) -0.0143(12) C38 0.0295(12) 0.0478(16) 0.0288(12) -0.0020(11) 0.0006(10) -0.0100(11) C39 0.0381(14) 0.0447(16) 0.0394(15) -0.0043(12) 0.0032(11) -0.0085(12) C40 0.0413(15) 0.0478(17) 0.0481(17) 0.0002(13) 0.0021(13) -0.0163(13) C41 0.0335(14) 0.0558(18) 0.0317(13) -0.0054(12) 0.0031(11) -0.0076(12) C42 0.0332(13) 0.0499(16) 0.0317(13) -0.0032(11) 0.0013(11) -0.0111(12) C43 0.097(3) 0.049(2) 0.067(2) -0.0076(18) -0.013(2) -0.019(2) C44 0.184(6) 0.077(3) 0.081(3) 0.010(3) -0.029(4) -0.026(4) C45 0.076(3) 0.068(3) 0.105(4) -0.014(2) -0.040(3) -0.010(2) C46 0.114(4) 0.079(3) 0.155(5) 0.020(3) -0.074(4) -0.026(3) C47 0.135(7) 0.041(4) 0.061(5) 0.012(3) -0.059(4) -0.005(4) C48 0.194(12) 0.117(10) 0.077(7) 0.024(7) -0.010(8) 0.082(9) P1 0.0474(4) 0.0410(4) 0.0430(4) 0.0061(3) -0.0041(3) -0.0155(3) P2 0.0726(6) 0.0494(5) 0.0348(4) 0.0085(3) -0.0054(4) -0.0088(4) F1 0.0754(14) 0.0527(11) 0.0573(12) 0.0166(9) -0.0142(10) -0.0202(10) F2 0.0688(14) 0.0511(12) 0.0834(16) 0.0209(11) -0.0010(11) -0.0064(10) F3 0.116(2) 0.0727(16) 0.140(3) -0.0144(16) -0.065(2) -0.0311(16) F4 0.139(2) 0.0848(17) 0.0735(16) 0.0013(13) -0.0512(17) -0.0404(17) F5 0.0577(13) 0.1103(19) 0.0645(14) 0.0241(13) 0.0063(10) -0.0216(13) F6 0.0726(16) 0.0768(16) 0.122(2) 0.0378(16) 0.0352(15) -0.0051(13) F11 0.0893(18) 0.0899(18) 0.0753(17) -0.0047(14) -0.0167(14) 0.0155(15) F12 0.0714(15) 0.0781(16) 0.0719(15) 0.0011(12) -0.0056(12) -0.0051(12) F13 0.119(2) 0.0662(15) 0.112(2) -0.0187(14) 0.0170(18) -0.0490(16) F14 0.170(3) 0.094(2) 0.142(3) 0.055(2) 0.048(3) -0.037(2) F15 0.117(2) 0.0647(14) 0.0648(14) -0.0059(11) -0.0315(14) -0.0211(14) F16 0.157(3) 0.163(3) 0.0591(16) -0.0406(18) -0.0497(19) 0.046(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2640(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 . 1.975(2) yes Fe1 . N2 . 1.884(2) yes Fe1 . N3 . 1.981(2) yes Fe1 . N4 . 1.970(2) yes Fe1 . N5 . 1.881(2) yes Fe1 . N6 . 1.979(2) yes N1 . C1 . 1.340(3) yes N1 . C5 . 1.363(3) yes N2 . C6 . 1.350(3) yes N2 . C10 . 1.349(3) yes N3 . C11 . 1.363(3) yes N3 . C15 . 1.346(3) yes N4 . C16 . 1.343(4) yes N4 . C20 . 1.368(3) yes N5 . C21 . 1.353(3) yes N5 . C25 . 1.348(3) yes N6 . C26 . 1.363(3) yes N6 . C30 . 1.345(3) yes N7 . N8 . 1.358(3) yes N7 . C8 . 1.369(3) yes N7 . H7 . 0.878 no N8 . C31 . 1.280(4) yes N9 . C34 . 1.331(4) yes N9 . C35 . 1.346(4) yes N10 . N11 . 1.358(3) yes N10 . C23 . 1.367(3) yes N10 . H10 . 0.878 no N11 . C37 . 1.275(4) yes N12 . C40 . 1.336(4) yes N12 . C41 . 1.335(4) yes N13 . C43 . 1.121(5) yes N14 . C45 . 1.143(6) yes N15 . C47 . 1.132(11) yes C1 . C2 . 1.383(4) yes C1 . H11 . 0.945 no C2 . C3 . 1.377(5) yes C2 . H21 . 0.943 no C3 . C4 . 1.383(5) yes C3 . H31 . 0.939 no C4 . C5 . 1.386(4) yes C4 . H41 . 0.942 no C5 . C6 . 1.473(4) yes C6 . C7 . 1.379(3) yes C7 . C8 . 1.400(4) yes C7 . H71 . 0.933 no C8 . C9 . 1.403(4) yes C9 . C10 . 1.373(3) yes C9 . H91 . 0.931 no C10 . C11 . 1.478(3) yes C11 . C12 . 1.380(4) yes C12 . C13 . 1.385(4) yes C12 . H121 . 0.946 no C13 . C14 . 1.383(4) yes C13 . H131 . 0.937 no C14 . C15 . 1.380(4) yes C14 . H141 . 0.935 no C15 . H151 . 0.942 no C16 . C17 . 1.382(4) yes C16 . H161 . 0.947 no C17 . C18 . 1.379(5) yes C17 . H171 . 0.942 no C18 . C19 . 1.383(5) yes C18 . H181 . 0.947 no C19 . C20 . 1.385(4) yes C19 . H191 . 0.938 no C20 . C21 . 1.473(4) yes C21 . C22 . 1.384(3) yes C22 . C23 . 1.396(4) yes C22 . H221 . 0.935 no C23 . C24 . 1.409(4) yes C24 . C25 . 1.377(4) yes C24 . H241 . 0.943 no C25 . C26 . 1.473(3) yes C26 . C27 . 1.393(4) yes C27 . C28 . 1.382(4) yes C27 . H271 . 0.940 no C28 . C29 . 1.383(4) yes C28 . H281 . 0.943 no C29 . C30 . 1.382(4) yes C29 . H291 . 0.945 no C30 . H301 . 0.952 no C31 . C32 . 1.464(4) yes C31 . H311 . 0.956 no C32 . C33 . 1.392(4) yes C32 . C36 . 1.389(4) yes C33 . C34 . 1.376(4) yes C33 . H331 . 0.945 no C34 . H341 . 0.946 no C35 . C36 . 1.384(4) yes C35 . H351 . 0.953 no C36 . H361 . 0.943 no C37 . C38 . 1.465(4) yes C37 . H371 . 0.951 no C38 . C39 . 1.379(4) yes C38 . C42 . 1.396(4) yes C39 . C40 . 1.384(4) yes C39 . H391 . 0.930 no C40 . H401 . 0.944 no C41 . C42 . 1.381(4) yes C41 . H411 . 0.942 no C42 . H421 . 0.953 no C43 . C44 . 1.462(7) yes C44 . H441 . 0.967 no C44 . H442 . 0.962 no C44 . H443 . 0.961 no C45 . C46 . 1.459(8) yes C46 . H461 . 0.971 no C46 . H462 . 0.977 no C46 . H463 . 0.971 no C47 . C48 . 1.466(13) yes C48 . H481 . 0.970 no C48 . H482 . 0.970 no C48 . H483 . 0.971 no P1 . F1 . 1.622(2) yes P1 . F2 . 1.581(2) yes P1 . F3 . 1.585(3) yes P1 . F4 . 1.574(3) yes P1 . F5 . 1.585(2) yes P1 . F6 . 1.576(2) yes P2 . F11 . 1.592(3) yes P2 . F12 . 1.586(2) yes P2 . F13 . 1.603(3) yes P2 . F14 . 1.541(3) yes P2 . F15 . 1.574(2) yes P2 . F16 . 1.578(3) 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 . 80.78(9) yes N1 . Fe1 . N3 . 161.57(9) yes N2 . Fe1 . N3 . 80.83(9) yes N1 . Fe1 . N4 . 88.93(9) yes N2 . Fe1 . N4 . 100.15(9) yes N3 . Fe1 . N4 . 93.00(8) yes N1 . Fe1 . N5 . 99.65(9) yes N2 . Fe1 . N5 . 179.23(9) yes N3 . Fe1 . N5 . 98.75(9) yes N4 . Fe1 . N5 . 80.51(9) yes N1 . Fe1 . N6 . 93.65(9) yes N2 . Fe1 . N6 . 98.33(9) yes N3 . Fe1 . N6 . 90.31(9) yes N4 . Fe1 . N6 . 161.52(9) yes N5 . Fe1 . N6 . 81.01(9) yes Fe1 . N1 . C1 . 126.80(19) yes Fe1 . N1 . C5 . 114.56(17) yes C1 . N1 . C5 . 118.4(2) yes Fe1 . N2 . C6 . 120.04(17) yes Fe1 . N2 . C10 . 119.80(16) yes C6 . N2 . C10 . 120.1(2) yes Fe1 . N3 . C11 . 114.77(16) yes Fe1 . N3 . C15 . 127.66(17) yes C11 . N3 . C15 . 117.6(2) yes Fe1 . N4 . C16 . 126.32(18) yes Fe1 . N4 . C20 . 115.09(17) yes C16 . N4 . C20 . 118.6(2) yes Fe1 . N5 . C21 . 120.51(18) yes Fe1 . N5 . C25 . 119.59(16) yes C21 . N5 . C25 . 119.9(2) yes Fe1 . N6 . C26 . 114.53(16) yes Fe1 . N6 . C30 . 127.70(18) yes C26 . N6 . C30 . 117.8(2) yes N8 . N7 . C8 . 121.3(2) yes N8 . N7 . H7 . 119.3 no C8 . N7 . H7 . 119.5 no N7 . N8 . C31 . 115.6(2) yes C34 . N9 . C35 . 116.3(3) yes N11 . N10 . C23 . 121.4(2) yes N11 . N10 . H10 . 119.4 no C23 . N10 . H10 . 119.2 no N10 . N11 . C37 . 115.3(3) yes C40 . N12 . C41 . 115.9(2) yes N1 . C1 . C2 . 122.5(3) yes N1 . C1 . H11 . 118.5 no C2 . C1 . H11 . 119.0 no C1 . C2 . C3 . 119.1(3) yes C1 . C2 . H21 . 119.9 no C3 . C2 . H21 . 120.9 no C2 . C3 . C4 . 119.2(3) yes C2 . C3 . H31 . 121.1 no C4 . C3 . H31 . 119.7 no C3 . C4 . C5 . 119.2(3) yes C3 . C4 . H41 . 120.3 no C5 . C4 . H41 . 120.4 no C4 . C5 . N1 . 121.5(2) yes C4 . C5 . C6 . 124.7(3) yes N1 . C5 . C6 . 113.8(2) yes C5 . C6 . N2 . 110.7(2) yes C5 . C6 . C7 . 127.4(2) yes N2 . C6 . C7 . 121.9(2) yes C6 . C7 . C8 . 118.1(2) yes C6 . C7 . H71 . 121.6 no C8 . C7 . H71 . 120.3 no C7 . C8 . N7 . 122.4(2) yes C7 . C8 . C9 . 119.7(2) yes N7 . C8 . C9 . 117.9(2) yes C8 . C9 . C10 . 118.7(2) yes C8 . C9 . H91 . 120.7 no C10 . C9 . H91 . 120.6 no C9 . C10 . N2 . 121.5(2) yes C9 . C10 . C11 . 127.1(2) yes N2 . C10 . C11 . 111.4(2) yes C10 . C11 . N3 . 113.2(2) yes C10 . C11 . C12 . 124.7(2) yes N3 . C11 . C12 . 122.1(2) yes C11 . C12 . C13 . 119.5(3) yes C11 . C12 . H121 . 120.5 no C13 . C12 . H121 . 120.0 no C12 . C13 . C14 . 118.7(3) yes C12 . C13 . H131 . 120.9 no C14 . C13 . H131 . 120.4 no C13 . C14 . C15 . 119.1(2) yes C13 . C14 . H141 . 120.7 no C15 . C14 . H141 . 120.1 no C14 . C15 . N3 . 123.0(2) yes C14 . C15 . H151 . 119.5 no N3 . C15 . H151 . 117.6 no N4 . C16 . C17 . 122.3(3) yes N4 . C16 . H161 . 118.4 no C17 . C16 . H161 . 119.4 no C16 . C17 . C18 . 119.1(3) yes C16 . C17 . H171 . 120.3 no C18 . C17 . H171 . 120.6 no C17 . C18 . C19 . 119.5(3) yes C17 . C18 . H181 . 120.3 no C19 . C18 . H181 . 120.2 no C18 . C19 . C20 . 119.1(3) yes C18 . C19 . H191 . 120.5 no C20 . C19 . H191 . 120.4 no C19 . C20 . N4 . 121.4(3) yes C19 . C20 . C21 . 125.3(2) yes N4 . C20 . C21 . 113.3(2) yes C20 . C21 . N5 . 110.5(2) yes C20 . C21 . C22 . 127.4(2) yes N5 . C21 . C22 . 122.0(2) yes C21 . C22 . C23 . 118.1(2) yes C21 . C22 . H221 . 120.6 no C23 . C22 . H221 . 121.3 no C22 . C23 . N10 . 123.2(2) yes C22 . C23 . C24 . 119.7(2) yes N10 . C23 . C24 . 117.1(2) yes C23 . C24 . C25 . 118.6(3) yes C23 . C24 . H241 . 120.9 no C25 . C24 . H241 . 120.5 no C24 . C25 . N5 . 121.7(2) yes C24 . C25 . C26 . 126.7(2) yes N5 . C25 . C26 . 111.6(2) yes C25 . C26 . N6 . 113.3(2) yes C25 . C26 . C27 . 124.7(2) yes N6 . C26 . C27 . 122.0(2) yes C26 . C27 . C28 . 119.2(3) yes C26 . C27 . H271 . 120.2 no C28 . C27 . H271 . 120.6 no C27 . C28 . C29 . 119.0(3) yes C27 . C28 . H281 . 120.9 no C29 . C28 . H281 . 120.1 no C28 . C29 . C30 . 119.2(2) yes C28 . C29 . H291 . 119.9 no C30 . C29 . H291 . 120.9 no C29 . C30 . N6 . 122.9(2) yes C29 . C30 . H301 . 119.7 no N6 . C30 . H301 . 117.4 no N8 . C31 . C32 . 120.8(3) yes N8 . C31 . H311 . 120.6 no C32 . C31 . H311 . 118.5 no C31 . C32 . C33 . 119.4(3) yes C31 . C32 . C36 . 123.0(3) yes C33 . C32 . C36 . 117.6(3) yes C32 . C33 . C34 . 119.1(3) yes C32 . C33 . H331 . 120.6 no C34 . C33 . H331 . 120.3 no C33 . C34 . N9 . 124.3(3) yes C33 . C34 . H341 . 119.4 no N9 . C34 . H341 . 116.2 no N9 . C35 . C36 . 123.7(3) yes N9 . C35 . H351 . 118.3 no C36 . C35 . H351 . 118.0 no C32 . C36 . C35 . 119.0(3) yes C32 . C36 . H361 . 120.2 no C35 . C36 . H361 . 120.8 no N11 . C37 . C38 . 121.3(3) yes N11 . C37 . H371 . 119.9 no C38 . C37 . H371 . 118.7 no C37 . C38 . C39 . 122.9(2) yes C37 . C38 . C42 . 119.2(3) yes C39 . C38 . C42 . 117.8(3) yes C38 . C39 . C40 . 119.3(3) yes C38 . C39 . H391 . 119.9 no C40 . C39 . H391 . 120.8 no C39 . C40 . N12 . 124.0(3) yes C39 . C40 . H401 . 118.3 no N12 . C40 . H401 . 117.7 no N12 . C41 . C42 . 124.8(3) yes N12 . C41 . H411 . 116.8 no C42 . C41 . H411 . 118.5 no C38 . C42 . C41 . 118.2(3) yes C38 . C42 . H421 . 120.4 no C41 . C42 . H421 . 121.3 no N13 . C43 . C44 . 178.3(5) yes C43 . C44 . H441 . 107.5 no C43 . C44 . H442 . 106.7 no H441 . C44 . H442 . 110.9 no C43 . C44 . H443 . 109.4 no H441 . C44 . H443 . 111.1 no H442 . C44 . H443 . 111.0 no N14 . C45 . C46 . 176.0(6) yes C45 . C46 . H461 . 105.7 no C45 . C46 . H462 . 110.6 no H461 . C46 . H462 . 109.9 no C45 . C46 . H463 . 110.2 no H461 . C46 . H463 . 109.8 no H462 . C46 . H463 . 110.6 no N15 . C47 . C48 . 168.0(12) yes C47 . C48 . H481 . 111.8 no C47 . C48 . H482 . 108.8 no H481 . C48 . H482 . 109.5 no C47 . C48 . H483 . 107.7 no H481 . C48 . H483 . 109.4 no H482 . C48 . H483 . 109.5 no F1 . P1 . F2 . 178.57(14) yes F1 . P1 . F3 . 87.23(14) yes F2 . P1 . F3 . 91.42(15) yes F1 . P1 . F4 . 89.85(13) yes F2 . P1 . F4 . 91.50(15) yes F3 . P1 . F4 . 177.02(16) yes F1 . P1 . F5 . 89.46(13) yes F2 . P1 . F5 . 90.99(13) yes F3 . P1 . F5 . 89.62(18) yes F4 . P1 . F5 . 89.73(16) yes F1 . P1 . F6 . 89.21(12) yes F2 . P1 . F6 . 90.36(13) yes F3 . P1 . F6 . 91.22(19) yes F4 . P1 . F6 . 89.37(19) yes F5 . P1 . F6 . 178.40(16) yes F11 . P2 . F12 . 177.04(18) yes F11 . P2 . F13 . 89.69(18) yes F12 . P2 . F13 . 87.78(15) yes F11 . P2 . F14 . 89.2(2) yes F12 . P2 . F14 . 93.35(18) yes F13 . P2 . F14 . 178.38(19) yes F11 . P2 . F15 . 89.55(15) yes F12 . P2 . F15 . 91.88(14) yes F13 . P2 . F15 . 87.21(16) yes F14 . P2 . F15 . 91.6(2) yes F11 . P2 . F16 . 90.30(16) yes F12 . P2 . F16 . 88.14(16) yes F13 . P2 . F16 . 89.8(2) yes F14 . P2 . F16 . 91.4(3) yes F15 . P2 . F16 . 177.0(2) yes # Attachment 'Fe_H2__2__JZ.CIF' data_jb1167 _database_code_depnum_ccdc_archive 'CCDC 692939' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H33 Fe N12, 3(F6 P), 3.5(C2 H3 N), 2.5(H2 O)' _chemical_formula_sum 'C49 H48.50 F18 Fe N15.50 O2.50 P3' _chemical_formula_weight 1385.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8794(18) _cell_length_b 16.055(3) _cell_length_c 23.710(5) _cell_angle_alpha 105.43(3) _cell_angle_beta 91.68(3) _cell_angle_gamma 97.54(3) _cell_volume 3222.7(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1398 _exptl_absorpt_coefficient_mu 0.411 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28413 _diffrn_reflns_av_R_equivalents 0.0753 _diffrn_reflns_av_sigmaI/netI 0.0632 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.05 _reflns_number_total 11375 _reflns_number_gt 8715 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1403P)^2^+7.9641P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11375 _refine_ls_number_parameters 983 _refine_ls_number_restraints 67 _refine_ls_R_factor_all 0.1226 _refine_ls_R_factor_gt 0.0952 _refine_ls_wR_factor_ref 0.2723 _refine_ls_wR_factor_gt 0.2477 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.91430(7) 0.73245(4) 0.87157(3) 0.0284(2) Uani 1 1 d . . . N1 N 0.6954(4) 0.6861(3) 0.85978(17) 0.0293(8) Uani 1 1 d . . . C1 C 0.6024(5) 0.6722(3) 0.9005(2) 0.0338(11) Uani 1 1 d . . . H1A H 0.6448 0.6800 0.9391 0.041 Uiso 1 1 calc R . . N2 N 0.8846(5) 0.7250(3) 0.79113(18) 0.0336(9) Uani 1 1 d . . . C2 C 0.4473(6) 0.6472(4) 0.8891(2) 0.0400(12) Uani 1 1 d . . . H2A H 0.3837 0.6395 0.9194 0.048 Uiso 1 1 calc R . . N3 N 1.1211(4) 0.7820(3) 0.85701(18) 0.0336(9) Uani 1 1 d . . . C3 C 0.3869(6) 0.6336(4) 0.8324(3) 0.0429(13) Uani 1 1 d . . . H3A H 0.2809 0.6150 0.8231 0.052 Uiso 1 1 calc R . . C4 C 0.4803(6) 0.6469(4) 0.7897(2) 0.0371(11) Uani 1 1 d . . . H4A H 0.4397 0.6383 0.7507 0.045 Uiso 1 1 calc R . . N4 N 0.8288(7) 0.6934(5) 0.6132(2) 0.080(2) Uani 1 1 d . . . H4B H 0.9084 0.7067 0.5944 0.096 Uiso 1 1 calc R . . C5 C 0.6350(5) 0.6733(3) 0.8041(2) 0.0313(10) Uani 1 1 d . . . N5 N 0.6902(7) 0.6631(5) 0.5836(2) 0.0711(18) Uani 1 1 d . . . C6 C 0.7463(6) 0.6920(3) 0.7627(2) 0.0339(11) Uani 1 1 d . . . N6 N 0.3829(12) 0.6088(5) 0.4086(3) 0.093(3) Uani 1 1 d . . . H6 H 0.389(14) 0.610(8) 0.369(6) 0.140 Uiso 1 1 d . . . N7 N 0.9771(4) 0.6158(3) 0.86395(18) 0.0317(9) Uani 1 1 d . . . C7 C 0.7219(6) 0.6799(4) 0.7034(2) 0.0450(13) Uani 1 1 d . . . H7A H 0.6242 0.6563 0.6842 0.054 Uiso 1 1 calc R . . C8 C 0.8437(7) 0.7030(5) 0.6717(3) 0.0545(16) Uani 1 1 d . . . N8 N 0.9509(4) 0.7401(3) 0.95173(17) 0.0300(8) Uani 1 1 d . . . N9 N 0.8584(5) 0.8495(3) 0.90644(18) 0.0327(9) Uani 1 1 d . . . C9 C 0.9856(7) 0.7385(5) 0.7020(3) 0.0539(16) Uani 1 1 d . . . H9A H 1.0693 0.7562 0.6817 0.065 Uiso 1 1 calc R . . C10 C 1.0029(6) 0.7475(4) 0.7609(2) 0.0410(12) Uani 1 1 d . . . N10 N 1.0875(6) 0.7756(3) 1.1254(2) 0.0502(12) Uani 1 1 d . . . H10D H 1.0669 0.8220 1.1518 0.060 Uiso 1 1 calc R . . N11 N 1.1664(5) 0.7179(3) 1.14177(19) 0.0414(11) Uani 1 1 d . . . C11 C 1.1410(6) 0.7843(4) 0.8010(2) 0.0382(12) Uani 1 1 d . . . N12 N 1.3632(8) 0.6200(4) 1.2968(2) 0.0675(17) Uani 1 1 d . . . C12 C 1.2770(6) 0.8197(4) 0.7846(3) 0.0486(14) Uani 1 1 d . . . H12A H 1.2883 0.8197 0.7449 0.058 Uiso 1 1 calc R . . C13 C 1.3979(7) 0.8556(4) 0.8266(3) 0.0528(15) Uani 1 1 d . . . H13A H 1.4922 0.8807 0.8160 0.063 Uiso 1 1 calc R . . C14 C 1.3774(6) 0.8538(4) 0.8837(3) 0.0474(14) Uani 1 1 d . . . H14A H 1.4575 0.8782 0.9133 0.057 Uiso 1 1 calc R . . C15 C 1.2395(6) 0.8161(4) 0.8975(2) 0.0400(12) Uani 1 1 d . . . H15A H 1.2272 0.8140 0.9367 0.048 Uiso 1 1 calc R . . C16 C 0.6830(10) 0.6578(7) 0.5287(3) 0.086(3) Uani 1 1 d . . . H16A H 0.7712 0.6724 0.5097 0.103 Uiso 1 1 calc R . . C17 C 0.5331(10) 0.6282(6) 0.4960(3) 0.079(2) Uani 1 1 d . . . C18 C 0.5182(12) 0.6343(6) 0.4390(3) 0.084(3) Uani 1 1 d . . . H18A H 0.6037 0.6566 0.4215 0.101 Uiso 1 1 calc R . . C19 C 0.2621(15) 0.5756(8) 0.4305(4) 0.110(4) Uani 1 1 d . . . H19A H 0.1687 0.5569 0.4072 0.132 Uiso 1 1 calc R . . C20 C 0.2703(13) 0.5680(8) 0.4859(4) 0.119(4) Uani 1 1 d . . . H20A H 0.1828 0.5447 0.5018 0.143 Uiso 1 1 calc R . . C21 C 0.4072(12) 0.5943(8) 0.5192(4) 0.110(4) Uani 1 1 d . . . H21A H 0.4141 0.5889 0.5581 0.132 Uiso 1 1 calc R . . C22 C 0.9826(5) 0.5513(3) 0.8149(2) 0.0373(11) Uani 1 1 d . . . H22A H 0.9466 0.5588 0.7787 0.045 Uiso 1 1 calc R . . C23 C 1.0381(6) 0.4742(4) 0.8142(3) 0.0454(13) Uani 1 1 d . . . H23A H 1.0400 0.4303 0.7784 0.054 Uiso 1 1 calc R . . C24 C 1.0905(6) 0.4626(4) 0.8666(3) 0.0461(13) Uani 1 1 d . . . H24A H 1.1294 0.4105 0.8673 0.055 Uiso 1 1 calc R . . C25 C 1.0857(6) 0.5274(3) 0.9177(2) 0.0400(12) Uani 1 1 d . . . H25A H 1.1218 0.5204 0.9540 0.048 Uiso 1 1 calc R . . C26 C 1.0278(5) 0.6033(3) 0.9159(2) 0.0329(10) Uani 1 1 d . . . C27 C 1.0158(5) 0.6766(3) 0.9673(2) 0.0303(10) Uani 1 1 d . . . C28 C 1.0628(6) 0.6856(4) 1.0249(2) 0.0382(11) Uani 1 1 d . . . H28A H 1.1097 0.6415 1.0353 0.046 Uiso 1 1 calc R . . C29 C 1.0399(6) 0.7611(4) 1.0674(2) 0.0366(11) Uani 1 1 d . . . C30 C 0.9673(6) 0.8251(4) 1.0511(2) 0.0378(11) Uani 1 1 d . . . H30A H 0.9466 0.8756 1.0796 0.045 Uiso 1 1 calc R . . C31 C 0.9274(5) 0.8122(3) 0.9926(2) 0.0315(10) Uani 1 1 d . . . C32 C 0.8625(5) 0.8746(3) 0.9659(2) 0.0326(10) Uani 1 1 d . . . C33 C 0.8104(6) 0.9498(4) 0.9973(2) 0.0402(12) Uani 1 1 d . . . H33A H 0.8134 0.9647 1.0390 0.048 Uiso 1 1 calc R . . C34 C 0.7538(6) 1.0031(4) 0.9669(3) 0.0450(13) Uani 1 1 d . . . H34A H 0.7145 1.0543 0.9871 0.054 Uiso 1 1 calc R . . C35 C 0.7559(6) 0.9801(3) 0.9060(3) 0.0432(13) Uani 1 1 d . . . H35A H 0.7219 1.0168 0.8843 0.052 Uiso 1 1 calc R . . C36 C 0.8079(6) 0.9035(3) 0.8775(2) 0.0371(11) Uani 1 1 d . . . H36A H 0.8082 0.8883 0.8360 0.045 Uiso 1 1 calc R . . C37 C 1.1920(6) 0.7297(4) 1.1966(2) 0.0439(13) Uani 1 1 d . . . H37A H 1.1543 0.7758 1.2240 0.053 Uiso 1 1 calc R . . C38 C 1.2808(6) 0.6707(4) 1.2169(2) 0.0419(13) Uani 1 1 d . . . C39 C 1.2860(8) 0.6730(5) 1.2761(3) 0.0576(17) Uani 1 1 d . . . H39A H 1.2335 0.7131 1.3024 0.069 Uiso 1 1 calc R . . C40 C 1.4354(10) 0.5637(5) 1.2602(3) 0.071(2) Uani 1 1 d . . . H40A H 1.4901 0.5264 1.2752 0.085 Uiso 1 1 calc R . . C41 C 1.4342(9) 0.5572(5) 1.2012(3) 0.0626(18) Uani 1 1 d . . . H41A H 1.4869 0.5158 1.1760 0.075 Uiso 1 1 calc R . . C42 C 1.3560(7) 0.6112(4) 1.1789(3) 0.0479(14) Uani 1 1 d . . . H42A H 1.3536 0.6077 1.1382 0.057 Uiso 1 1 calc R . . P1 P 1.3488(4) 0.9875(2) 1.26261(13) 0.1138(11) Uani 1 1 d . . . F11 F 1.4120(16) 0.9551(8) 1.2009(4) 0.217(6) Uani 1 1 d . . . F12 F 1.5093(11) 1.0414(9) 1.2868(5) 0.215(5) Uani 1 1 d . . . F13 F 1.3959(13) 0.9033(8) 1.2753(5) 0.213(5) Uani 1 1 d . . . F14 F 1.2956(13) 1.0226(10) 1.3233(4) 0.219(6) Uani 1 1 d . . . F15 F 1.3068(8) 1.0684(4) 1.2447(3) 0.120(2) Uani 1 1 d . . . F16 F 1.1903(10) 0.9369(5) 1.2356(6) 0.201(5) Uani 1 1 d . . . P2 P 0.8320(5) 0.5161(9) 0.3460(2) 0.068(2) Uani 0.555(18) 1 d P A 1 P2' P 0.8202(8) 0.4663(8) 0.3486(3) 0.056(3) Uani 0.445(18) 1 d P A 2 F21 F 0.839(3) 0.5983(16) 0.3934(9) 0.178(10) Uani 0.555(18) 1 d P A 1 F21' F 0.8373(18) 0.5414(17) 0.4101(6) 0.113(8) Uani 0.445(18) 1 d P A 2 F22' F 0.762(2) 0.5364(17) 0.3013(11) 0.116(9) Uani 0.445(18) 1 d P A 2 F22 F 0.775(3) 0.557(3) 0.3091(15) 0.216(17) Uani 0.555(18) 1 d P A 1 F23 F 0.9966(9) 0.5488(12) 0.3309(4) 0.092(5) Uani 0.555(18) 1 d P A 1 F23' F 0.9926(13) 0.4774(16) 0.3395(8) 0.119(9) Uani 0.445(18) 1 d P A 2 F24 F 0.824(2) 0.4299(18) 0.2917(9) 0.139(10) Uani 0.555(18) 1 d P A 1 F24' F 0.8022(17) 0.3922(17) 0.2916(9) 0.099(8) Uani 0.445(18) 1 d P A 2 F25 F 0.6547(6) 0.4689(5) 0.3585(2) 0.110(2) Uani 0.555(18) 1 d P A 1 F25' F 0.6547(6) 0.4689(5) 0.3585(2) 0.110(2) Uani 0.445(18) 1 d P A 2 F26 F 0.9078(15) 0.4674(18) 0.3887(7) 0.138(8) Uani 0.555(18) 1 d P A 1 F26' F 0.846(3) 0.3995(19) 0.3831(8) 0.144(10) Uani 0.445(18) 1 d P A 2 P3 P 0.5000 0.5000 1.0000 0.0483(5) Uani 1 2 d S . . F31 F 0.6526(6) 0.5485(4) 0.9851(3) 0.108(2) Uani 1 1 d . . . F32 F 0.4238(6) 0.5866(3) 1.01016(19) 0.0863(15) Uani 1 1 d . . . F33 F 0.4414(6) 0.4742(3) 0.93291(17) 0.0810(14) Uani 1 1 d . . . N100 N 0.8666(11) 0.9823(6) 1.1582(4) 0.102(3) Uani 1 1 d . . . C100 C 0.8709(18) 1.0072(9) 1.2698(5) 0.140(5) Uani 1 1 d . . . H10A H 0.9303 0.9665 1.2815 0.210 Uiso 1 1 calc R . . H10B H 0.7664 0.9977 1.2814 0.210 Uiso 1 1 calc R . . H10C H 0.9173 1.0673 1.2891 0.210 Uiso 1 1 calc R . . C101 C 0.8688(13) 0.9924(6) 1.2067(5) 0.095(3) Uani 1 1 d . . . P4 P 0.5876(12) 0.8799(5) 0.4398(4) 0.175(5) Uani 0.50 1 d PD . . F41 F 0.717(3) 0.8267(10) 0.4529(12) 0.271(15) Uani 0.50 1 d PD . . F42 F 0.4639(19) 0.9394(14) 0.4365(8) 0.217(11) Uani 0.50 1 d PD . . F43 F 0.525(3) 0.8524(15) 0.4948(8) 0.256(12) Uiso 0.50 1 d PD . . F44 F 0.490(3) 0.7993(10) 0.3965(7) 0.270(17) Uani 0.50 1 d PD . . F45 F 0.676(4) 0.959(2) 0.4908(10) 0.335(18) Uiso 0.50 1 d PD . . F46 F 0.677(3) 0.9122(17) 0.3909(10) 0.267(13) Uani 0.50 1 d PDU . . N300 N 0.4399(10) 0.8270(5) 1.0235(3) 0.091(2) Uani 1 1 d . . . C300 C 0.5629(9) 0.7822(6) 1.1086(4) 0.074(2) Uani 1 1 d . . . H30B H 0.5592 0.7186 1.0981 0.111 Uiso 1 1 calc R . . H30C H 0.5080 0.8010 1.1440 0.111 Uiso 1 1 calc R . . H30D H 0.6692 0.8101 1.1160 0.111 Uiso 1 1 calc R . . C301 C 0.4926(8) 0.8070(5) 1.0610(3) 0.0609(17) Uani 1 1 d . . . C201 C 0.7744(10) 0.7639(6) 0.2598(7) 0.115(5) Uani 1 1 d . . . N200 N 0.8296(13) 0.7599(11) 0.2125(6) 0.172(6) Uani 1 1 d . . . C200 C 0.678(2) 0.7716(17) 0.2994(10) 0.271(15) Uani 1 1 d . . . H20B H 0.7249 0.7650 0.3355 0.406 Uiso 1 1 calc R . . H20C H 0.5892 0.7262 0.2858 0.406 Uiso 1 1 calc R . . H20D H 0.6448 0.8293 0.3070 0.406 Uiso 1 1 calc R . . O1 O 1.0185(14) 0.8016(8) 0.4145(6) 0.092(4) Uani 0.50 1 d P B 3 C500 C 0.955(6) 0.990(4) 0.5812(17) 0.14(3) Uani 0.25 1 d P C 1 C501 C 0.867(5) 0.929(3) 0.5632(16) 0.111(15) Uani 0.25 1 d PD C 1 H50A H 0.7660 0.9470 0.5603 0.167 Uiso 0.25 1 calc PR C 1 H50B H 0.8653 0.8914 0.5897 0.167 Uiso 0.25 1 calc PR C 1 H50C H 0.8924 0.8970 0.5243 0.167 Uiso 0.25 1 calc PR C 1 N500 N 1.058(7) 1.023(4) 0.5943(14) 0.20(3) Uani 0.25 1 d PD C 1 N400 N 1.115(5) 0.766(3) 0.5718(18) 0.090(11) Uani 0.25 1 d PU D 1 C401 C 1.235(3) 0.823(2) 0.5773(11) 0.062(9) Uani 0.25 1 d P D 1 C400 C 1.396(4) 0.857(2) 0.5687(12) 0.076(10) Uani 0.25 1 d P D 1 H40B H 1.4184 0.9188 0.5894 0.113 Uiso 0.25 1 calc PR D 1 H40C H 1.4085 0.8485 0.5268 0.113 Uiso 0.25 1 calc PR D 1 H40D H 1.4656 0.8244 0.5843 0.113 Uiso 0.25 1 calc PR D 1 O1' O 1.149(4) 0.770(2) 0.4187(13) 0.118(11) Uani 0.25 1 d P E 4 O2 O 1.043(3) 0.718(2) 0.5209(13) 0.103(9) Uani 0.25 1 d P F 3 O3 O 1.453(6) 0.789(2) 0.6182(15) 0.18(2) Uani 0.25 1 d P G 3 O2" O 1.084(3) 0.8789(19) 0.4617(13) 0.105(9) Uani 0.25 1 d P H 5 O2' O 1.031(4) 0.750(2) 0.4712(15) 0.127(10) Uani 0.25 1 d PU I 6 O1" O 1.058(4) 0.847(2) 0.3630(17) 0.127(12) Uani 0.25 1 d P J 5 O3' O 1.130(6) 0.810(3) 0.586(2) 0.119(13) Uani 0.25 1 d PU K 4 O3" O 1.347(5) 0.820(2) 0.6146(16) 0.130(11) Uani 0.25 1 d PU L 5 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 0.0266(4) 0.0323(4) 0.0253(4) 0.0097(3) -0.0073(2) -0.0009(3) N1 0.029(2) 0.029(2) 0.029(2) 0.0084(16) -0.0070(16) 0.0018(15) C1 0.032(2) 0.037(3) 0.034(3) 0.015(2) -0.004(2) 0.003(2) N2 0.031(2) 0.039(2) 0.030(2) 0.0140(18) -0.0083(16) -0.0032(17) C2 0.032(3) 0.049(3) 0.045(3) 0.022(3) 0.003(2) 0.009(2) N3 0.029(2) 0.039(2) 0.031(2) 0.0105(18) -0.0066(16) -0.0025(17) C3 0.026(2) 0.051(3) 0.053(3) 0.020(3) -0.008(2) 0.004(2) C4 0.031(3) 0.044(3) 0.035(3) 0.011(2) -0.011(2) 0.001(2) N4 0.053(3) 0.150(7) 0.041(3) 0.045(4) -0.010(2) -0.011(4) C5 0.030(2) 0.032(2) 0.032(2) 0.012(2) -0.0087(19) 0.0026(19) N5 0.066(4) 0.115(5) 0.034(3) 0.037(3) -0.018(2) -0.011(3) C6 0.034(3) 0.040(3) 0.029(2) 0.015(2) -0.0084(19) -0.001(2) N6 0.154(8) 0.079(5) 0.043(4) 0.020(3) -0.055(5) 0.012(5) N7 0.0254(19) 0.035(2) 0.030(2) 0.0045(17) -0.0064(15) 0.0000(16) C7 0.035(3) 0.063(4) 0.036(3) 0.019(3) -0.013(2) -0.006(2) C8 0.048(3) 0.083(5) 0.033(3) 0.025(3) -0.009(2) -0.003(3) N8 0.029(2) 0.033(2) 0.027(2) 0.0094(17) -0.0063(15) 0.0020(16) N9 0.032(2) 0.031(2) 0.035(2) 0.0131(17) -0.0104(17) -0.0025(16) C9 0.041(3) 0.080(5) 0.042(3) 0.027(3) -0.005(2) -0.005(3) C10 0.032(3) 0.054(3) 0.037(3) 0.019(2) -0.008(2) -0.005(2) N10 0.069(3) 0.058(3) 0.027(2) 0.012(2) -0.002(2) 0.024(3) N11 0.049(3) 0.050(3) 0.029(2) 0.018(2) -0.0065(19) 0.007(2) C11 0.032(3) 0.045(3) 0.035(3) 0.012(2) -0.008(2) -0.002(2) N12 0.100(5) 0.064(4) 0.036(3) 0.017(3) -0.037(3) 0.001(3) C12 0.036(3) 0.067(4) 0.044(3) 0.026(3) -0.001(2) -0.007(3) C13 0.034(3) 0.063(4) 0.061(4) 0.025(3) -0.004(3) -0.010(3) C14 0.032(3) 0.047(3) 0.057(4) 0.011(3) -0.012(2) -0.006(2) C15 0.033(3) 0.046(3) 0.036(3) 0.009(2) -0.010(2) -0.004(2) C16 0.079(5) 0.141(8) 0.042(4) 0.048(5) -0.018(4) -0.013(5) C17 0.091(6) 0.113(7) 0.034(3) 0.035(4) -0.027(4) -0.003(5) C18 0.124(7) 0.093(6) 0.033(4) 0.024(4) -0.030(4) 0.002(5) C19 0.125(9) 0.124(9) 0.075(6) 0.040(6) -0.065(6) -0.017(7) C20 0.104(7) 0.164(11) 0.084(7) 0.061(7) -0.057(6) -0.044(7) C21 0.096(7) 0.175(11) 0.059(5) 0.061(6) -0.044(5) -0.035(7) C22 0.030(2) 0.040(3) 0.037(3) 0.007(2) -0.009(2) -0.002(2) C23 0.039(3) 0.040(3) 0.045(3) -0.005(2) -0.007(2) 0.002(2) C24 0.042(3) 0.037(3) 0.057(4) 0.010(3) -0.008(3) 0.007(2) C25 0.038(3) 0.036(3) 0.046(3) 0.013(2) -0.009(2) 0.005(2) C26 0.029(2) 0.035(3) 0.034(3) 0.010(2) -0.0069(19) -0.0010(19) C27 0.031(2) 0.030(2) 0.032(2) 0.013(2) -0.0056(19) 0.0024(18) C28 0.037(3) 0.045(3) 0.035(3) 0.017(2) -0.005(2) 0.004(2) C29 0.038(3) 0.045(3) 0.028(2) 0.014(2) -0.008(2) 0.004(2) C30 0.044(3) 0.040(3) 0.027(2) 0.007(2) -0.004(2) 0.007(2) C31 0.031(2) 0.032(3) 0.031(2) 0.011(2) -0.0052(19) 0.0015(19) C32 0.031(2) 0.032(3) 0.034(3) 0.011(2) -0.0076(19) 0.0024(19) C33 0.042(3) 0.039(3) 0.036(3) 0.007(2) -0.011(2) 0.005(2) C34 0.044(3) 0.036(3) 0.052(3) 0.010(2) -0.014(2) 0.005(2) C35 0.044(3) 0.033(3) 0.053(3) 0.016(2) -0.017(2) 0.001(2) C36 0.032(2) 0.043(3) 0.039(3) 0.020(2) -0.007(2) -0.002(2) C37 0.048(3) 0.060(4) 0.026(3) 0.014(2) -0.003(2) 0.011(3) C38 0.051(3) 0.047(3) 0.025(2) 0.011(2) -0.014(2) -0.001(2) C39 0.077(4) 0.063(4) 0.030(3) 0.011(3) -0.014(3) 0.009(3) C40 0.102(6) 0.052(4) 0.054(4) 0.010(3) -0.038(4) 0.011(4) C41 0.079(5) 0.054(4) 0.054(4) 0.012(3) -0.019(3) 0.017(3) C42 0.058(4) 0.049(3) 0.035(3) 0.014(3) -0.012(3) 0.001(3) P1 0.128(2) 0.142(3) 0.0857(19) 0.0720(19) -0.0252(17) -0.007(2) F11 0.360(16) 0.235(11) 0.107(6) 0.059(6) 0.026(7) 0.194(11) F12 0.120(7) 0.302(14) 0.195(10) 0.052(9) -0.038(6) -0.031(8) F13 0.222(10) 0.218(10) 0.257(12) 0.178(10) -0.055(9) 0.023(8) F14 0.212(10) 0.365(17) 0.123(7) 0.133(9) 0.069(7) 0.040(10) F15 0.150(6) 0.105(4) 0.116(5) 0.049(4) 0.008(4) 0.017(4) F16 0.132(7) 0.103(5) 0.352(15) 0.052(7) -0.066(8) 0.002(5) P2 0.045(2) 0.106(6) 0.049(2) 0.026(3) -0.0129(15) -0.009(3) P2' 0.044(2) 0.080(6) 0.034(2) -0.003(3) -0.0169(17) 0.014(3) F21 0.171(16) 0.168(18) 0.144(16) -0.010(13) 0.070(12) -0.062(14) F21' 0.079(9) 0.168(19) 0.055(8) -0.034(9) -0.021(6) 0.025(11) F22' 0.056(9) 0.130(14) 0.122(16) -0.029(13) -0.017(9) 0.011(8) F22 0.123(17) 0.34(4) 0.24(3) 0.21(3) 0.037(18) -0.01(2) F23 0.044(4) 0.165(13) 0.057(5) 0.039(6) -0.025(3) -0.029(6) F23' 0.046(6) 0.163(18) 0.104(12) -0.035(12) -0.016(7) 0.005(8) F24 0.114(11) 0.22(2) 0.063(9) 0.030(12) 0.011(7) -0.044(12) F24' 0.046(7) 0.153(17) 0.077(10) -0.023(10) -0.029(7) 0.051(10) F25 0.067(3) 0.196(7) 0.077(3) 0.049(4) 0.008(2) 0.023(3) F25' 0.067(3) 0.196(7) 0.077(3) 0.049(4) 0.008(2) 0.023(3) F26 0.080(8) 0.25(2) 0.109(10) 0.120(14) -0.033(7) -0.017(11) F26' 0.16(2) 0.21(2) 0.100(12) 0.083(15) 0.023(12) 0.102(18) P3 0.0629(14) 0.0558(13) 0.0353(11) 0.0221(10) -0.0014(9) 0.0217(11) F31 0.078(3) 0.147(5) 0.125(5) 0.091(4) 0.001(3) -0.002(3) F32 0.133(4) 0.076(3) 0.063(3) 0.024(2) -0.008(3) 0.057(3) F33 0.120(4) 0.088(3) 0.042(2) 0.022(2) -0.019(2) 0.039(3) N100 0.118(7) 0.090(6) 0.084(6) -0.004(4) 0.030(5) 0.021(5) C100 0.204(15) 0.134(11) 0.085(8) 0.012(7) 0.019(8) 0.071(10) C101 0.123(8) 0.073(6) 0.076(6) -0.002(5) 0.012(6) 0.014(5) P4 0.251(12) 0.102(5) 0.158(8) 0.009(5) 0.097(8) 0.009(7) F41 0.40(4) 0.069(10) 0.35(4) 0.061(15) -0.02(3) 0.066(16) F42 0.165(16) 0.33(3) 0.22(2) 0.16(2) 0.001(14) 0.124(19) F44 0.45(4) 0.140(15) 0.186(18) 0.079(14) -0.19(2) -0.10(2) F46 0.284(15) 0.267(15) 0.260(15) 0.096(10) 0.015(10) 0.021(10) N300 0.132(7) 0.078(5) 0.068(4) 0.020(4) -0.021(4) 0.039(5) C300 0.063(4) 0.089(6) 0.074(5) 0.034(4) -0.008(4) 0.007(4) C301 0.062(4) 0.062(4) 0.060(4) 0.015(3) 0.000(3) 0.015(3) C201 0.053(5) 0.059(5) 0.204(13) -0.004(6) 0.031(7) -0.012(4) N200 0.103(8) 0.280(18) 0.169(12) 0.082(12) 0.033(8) 0.108(10) C200 0.144(15) 0.29(3) 0.27(3) -0.09(2) 0.107(17) -0.049(16) O1 0.085(8) 0.083(8) 0.093(9) -0.003(7) 0.021(7) 0.011(7) C500 0.16(4) 0.14(4) 0.05(2) -0.04(2) 0.05(2) -0.09(3) C501 0.12(3) 0.12(3) 0.06(2) -0.03(2) 0.02(2) 0.01(3) N500 0.33(8) 0.19(5) 0.040(19) 0.04(3) 0.02(3) -0.09(5) N400 0.095(17) 0.096(18) 0.085(17) 0.047(15) 0.030(14) -0.014(14) C401 0.017(10) 0.13(3) 0.049(14) 0.048(16) 0.010(9) -0.007(12) C400 0.074(19) 0.09(2) 0.044(14) 0.010(14) 0.018(13) -0.040(17) O1' 0.16(3) 0.12(2) 0.097(19) 0.041(17) -0.011(18) 0.09(2) O2 0.070(15) 0.16(3) 0.095(19) 0.07(2) 0.006(13) 0.023(16) O3 0.27(5) 0.13(3) 0.11(2) -0.06(2) -0.03(3) 0.15(3) O2" 0.11(2) 0.096(19) 0.11(2) 0.025(16) -0.019(16) 0.017(16) O2' 0.143(18) 0.117(17) 0.110(16) 0.021(13) 0.056(14) -0.017(14) O1" 0.11(2) 0.12(2) 0.19(3) 0.11(3) 0.05(2) 0.050(19) O3' 0.14(2) 0.105(19) 0.13(2) 0.050(16) 0.038(16) 0.039(16) O3" 0.139(19) 0.112(17) 0.125(18) 0.024(15) -0.011(15) -0.015(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.887(4) . ? Fe1 N8 1.887(4) . ? Fe1 N1 1.971(4) . ? Fe1 N9 1.976(4) . ? Fe1 N3 1.981(4) . ? Fe1 N7 1.988(4) . ? N1 C1 1.333(6) . ? N1 C5 1.364(6) . ? C1 C2 1.381(7) . ? C1 H1A 0.9500 . ? N2 C10 1.353(7) . ? N2 C6 1.354(6) . ? C2 C3 1.383(8) . ? C2 H2A 0.9500 . ? N3 C15 1.355(6) . ? N3 C11 1.355(7) . ? C3 C4 1.371(8) . ? C3 H3A 0.9500 . ? C4 C5 1.387(7) . ? C4 H4A 0.9500 . ? N4 C8 1.354(8) . ? N4 N5 1.362(8) . ? N4 H4B 0.8800 . ? C5 C6 1.471(7) . ? N5 C16 1.281(8) . ? C6 C7 1.374(7) . ? N6 C19 1.316(14) . ? N6 C18 1.339(12) . ? N6 H6 0.95(13) . ? N7 C22 1.343(7) . ? N7 C26 1.372(6) . ? C7 C8 1.401(8) . ? C7 H7A 0.9500 . ? C8 C9 1.403(8) . ? N8 C31 1.342(7) . ? N8 C27 1.361(6) . ? N9 C36 1.351(6) . ? N9 C32 1.356(6) . ? C9 C10 1.368(8) . ? C9 H9A 0.9500 . ? C10 C11 1.482(7) . ? N10 N11 1.358(6) . ? N10 C29 1.376(7) . ? N10 H10D 0.8800 . ? N11 C37 1.273(7) . ? C11 C12 1.377(8) . ? N12 C40 1.322(10) . ? N12 C39 1.337(9) . ? C12 C13 1.394(8) . ? C12 H12A 0.9500 . ? C13 C14 1.381(9) . ? C13 H13A 0.9500 . ? C14 C15 1.380(8) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.475(11) . ? C16 H16A 0.9500 . ? C17 C21 1.372(13) . ? C17 C18 1.386(9) . ? C18 H18A 0.9500 . ? C19 C20 1.352(14) . ? C19 H19A 0.9500 . ? C20 C21 1.381(11) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.386(8) . ? C22 H22A 0.9500 . ? C23 C24 1.380(8) . ? C23 H23A 0.9500 . ? C24 C25 1.377(8) . ? C24 H24A 0.9500 . ? C25 C26 1.394(7) . ? C25 H25A 0.9500 . ? C26 C27 1.470(7) . ? C27 C28 1.379(7) . ? C28 C29 1.398(8) . ? C28 H28A 0.9500 . ? C29 C30 1.412(7) . ? C30 C31 1.375(7) . ? C30 H30A 0.9500 . ? C31 C32 1.485(7) . ? C32 C33 1.385(8) . ? C33 C34 1.388(8) . ? C33 H33A 0.9500 . ? C34 C35 1.392(8) . ? C34 H34A 0.9500 . ? C35 C36 1.380(8) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C38 1.471(8) . ? C37 H37A 0.9500 . ? C38 C42 1.384(9) . ? C38 C39 1.396(8) . ? C39 H39A 0.9500 . ? C40 C41 1.375(10) . ? C40 H40A 0.9500 . ? C41 C42 1.377(9) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? P1 F14 1.514(10) . ? P1 F15 1.554(7) . ? P1 F16 1.556(9) . ? P1 F11 1.565(10) . ? P1 F13 1.566(9) . ? P1 F12 1.572(10) . ? P2 F22 1.35(3) . ? P2 F21 1.48(2) . ? P2 F23 1.571(9) . ? P2 F24 1.61(2) . ? P2 F26 1.614(15) . ? P2 F25 1.724(8) . ? P2' F24' 1.53(2) . ? P2' F23' 1.546(14) . ? P2' F26' 1.546(19) . ? P2' F21' 1.615(15) . ? P2' F22' 1.89(3) . ? P3 F31 1.570(5) . ? P3 F31 1.570(5) 2_667 ? P3 F33 1.587(4) . ? P3 F33 1.587(4) 2_667 ? P3 F32 1.590(4) 2_667 ? P3 F32 1.590(4) . ? N100 C101 1.116(12) . ? C100 C101 1.451(15) . ? C100 H10A 0.9800 . ? C100 H10B 0.9800 . ? C100 H10C 0.9800 . ? P4 F44 1.557(13) . ? P4 F42 1.561(13) . ? P4 F43 1.578(16) . ? P4 F46 1.586(16) . ? P4 F41 1.592(15) . ? P4 F45 1.600(17) . ? N300 C301 1.131(9) . ? C300 C301 1.445(10) . ? C300 H30B 0.9800 . ? C300 H30C 0.9800 . ? C300 H30D 0.9800 . ? C201 N200 1.226(17) . ? C201 C200 1.28(2) . ? C200 H20B 0.9800 . ? C200 H20C 0.9800 . ? C200 H20D 0.9800 . ? C500 N500 0.99(5) . ? C500 C501 1.14(4) . ? C501 H50A 0.9800 . ? C501 H50B 0.9800 . ? C501 H50C 0.9800 . ? N400 C401 1.29(5) . ? C401 C400 1.50(3) . ? C400 H40B 0.9800 . ? C400 H40C 0.9800 . ? C400 H40D 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N8 178.15(18) . . ? N2 Fe1 N1 81.00(17) . . ? N8 Fe1 N1 100.76(17) . . ? N2 Fe1 N9 100.13(18) . . ? N8 Fe1 N9 80.56(17) . . ? N1 Fe1 N9 88.37(17) . . ? N2 Fe1 N3 80.35(17) . . ? N8 Fe1 N3 97.92(17) . . ? N1 Fe1 N3 161.16(16) . . ? N9 Fe1 N3 92.26(18) . . ? N2 Fe1 N7 98.59(18) . . ? N8 Fe1 N7 80.77(17) . . ? N1 Fe1 N7 93.54(16) . . ? N9 Fe1 N7 161.25(17) . . ? N3 Fe1 N7 91.88(17) . . ? C1 N1 C5 118.5(4) . . ? C1 N1 Fe1 127.1(3) . . ? C5 N1 Fe1 114.2(3) . . ? N1 C1 C2 122.9(5) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C10 N2 C6 119.7(4) . . ? C10 N2 Fe1 120.3(3) . . ? C6 N2 Fe1 119.9(3) . . ? C1 C2 C3 118.3(5) . . ? C1 C2 H2A 120.9 . . ? C3 C2 H2A 120.9 . . ? C15 N3 C11 118.2(4) . . ? C15 N3 Fe1 126.6(4) . . ? C11 N3 Fe1 115.2(3) . . ? C4 C3 C2 119.8(5) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C3 C4 C5 119.2(5) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? C8 N4 N5 119.9(6) . . ? C8 N4 H4B 120.1 . . ? N5 N4 H4B 120.1 . . ? N1 C5 C4 121.2(5) . . ? N1 C5 C6 114.3(4) . . ? C4 C5 C6 124.4(4) . . ? C16 N5 N4 116.7(6) . . ? N2 C6 C7 121.9(5) . . ? N2 C6 C5 110.4(4) . . ? C7 C6 C5 127.7(4) . . ? C19 N6 C18 122.3(7) . . ? C19 N6 H6 125(7) . . ? C18 N6 H6 112(8) . . ? C22 N7 C26 117.5(4) . . ? C22 N7 Fe1 128.3(3) . . ? C26 N7 Fe1 114.1(3) . . ? C6 C7 C8 118.8(5) . . ? C6 C7 H7A 120.6 . . ? C8 C7 H7A 120.6 . . ? N4 C8 C7 122.4(5) . . ? N4 C8 C9 119.0(6) . . ? C7 C8 C9 118.6(5) . . ? C31 N8 C27 120.3(4) . . ? C31 N8 Fe1 119.7(3) . . ? C27 N8 Fe1 119.6(3) . . ? C36 N9 C32 117.5(5) . . ? C36 N9 Fe1 127.0(4) . . ? C32 N9 Fe1 115.3(3) . . ? C10 C9 C8 119.7(5) . . ? C10 C9 H9A 120.2 . . ? C8 C9 H9A 120.2 . . ? N2 C10 C9 121.3(5) . . ? N2 C10 C11 110.4(4) . . ? C9 C10 C11 128.2(5) . . ? N11 N10 C29 119.7(5) . . ? N11 N10 H10D 120.1 . . ? C29 N10 H10D 120.1 . . ? C37 N11 N10 116.5(5) . . ? N3 C11 C12 121.9(5) . . ? N3 C11 C10 113.5(4) . . ? C12 C11 C10 124.7(5) . . ? C40 N12 C39 119.3(6) . . ? C11 C12 C13 119.7(5) . . ? C11 C12 H12A 120.1 . . ? C13 C12 H12A 120.1 . . ? C14 C13 C12 118.4(5) . . ? C14 C13 H13A 120.8 . . ? C12 C13 H13A 120.8 . . ? C15 C14 C13 119.3(5) . . ? C15 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? N3 C15 C14 122.5(5) . . ? N3 C15 H15A 118.8 . . ? C14 C15 H15A 118.8 . . ? N5 C16 C17 117.8(7) . . ? N5 C16 H16A 121.1 . . ? C17 C16 H16A 121.1 . . ? C21 C17 C18 118.1(8) . . ? C21 C17 C16 123.2(6) . . ? C18 C17 C16 118.7(8) . . ? N6 C18 C17 119.8(9) . . ? N6 C18 H18A 120.1 . . ? C17 C18 H18A 120.1 . . ? N6 C19 C20 120.4(9) . . ? N6 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C19 C20 C21 119.4(11) . . ? C19 C20 H20A 120.3 . . ? C21 C20 H20A 120.3 . . ? C17 C21 C20 120.0(8) . . ? C17 C21 H21A 120.0 . . ? C20 C21 H21A 120.0 . . ? N7 C22 C23 123.6(5) . . ? N7 C22 H22A 118.2 . . ? C23 C22 H22A 118.2 . . ? C24 C23 C22 118.6(5) . . ? C24 C23 H23A 120.7 . . ? C22 C23 H23A 120.7 . . ? C25 C24 C23 119.2(5) . . ? C25 C24 H24A 120.4 . . ? C23 C24 H24A 120.4 . . ? C24 C25 C26 119.8(5) . . ? C24 C25 H25A 120.1 . . ? C26 C25 H25A 120.1 . . ? N7 C26 C25 121.4(5) . . ? N7 C26 C27 113.8(4) . . ? C25 C26 C27 124.9(4) . . ? N8 C27 C28 121.2(5) . . ? N8 C27 C26 111.0(4) . . ? C28 C27 C26 127.8(5) . . ? C27 C28 C29 118.5(5) . . ? C27 C28 H28A 120.7 . . ? C29 C28 H28A 120.7 . . ? N10 C29 C28 121.7(5) . . ? N10 C29 C30 118.4(5) . . ? C28 C29 C30 119.9(4) . . ? C31 C30 C29 117.9(5) . . ? C31 C30 H30A 121.0 . . ? C29 C30 H30A 121.0 . . ? N8 C31 C30 122.1(5) . . ? N8 C31 C32 111.5(4) . . ? C30 C31 C32 126.4(5) . . ? N9 C32 C33 123.1(4) . . ? N9 C32 C31 112.4(4) . . ? C33 C32 C31 124.5(5) . . ? C32 C33 C34 118.6(5) . . ? C32 C33 H33A 120.7 . . ? C34 C33 H33A 120.7 . . ? C33 C34 C35 118.7(5) . . ? C33 C34 H34A 120.7 . . ? C35 C34 H34A 120.7 . . ? C36 C35 C34 119.4(5) . . ? C36 C35 H35A 120.3 . . ? C34 C35 H35A 120.3 . . ? N9 C36 C35 122.5(5) . . ? N9 C36 H36A 118.7 . . ? C35 C36 H36A 118.7 . . ? N11 C37 C38 118.8(5) . . ? N11 C37 H37A 120.6 . . ? C38 C37 H37A 120.6 . . ? C42 C38 C39 118.7(6) . . ? C42 C38 C37 122.3(5) . . ? C39 C38 C37 119.0(6) . . ? N12 C39 C38 121.6(7) . . ? N12 C39 H39A 119.2 . . ? C38 C39 H39A 119.2 . . ? N12 C40 C41 122.5(6) . . ? N12 C40 H40A 118.8 . . ? C41 C40 H40A 118.8 . . ? C40 C41 C42 119.3(7) . . ? C40 C41 H41A 120.3 . . ? C42 C41 H41A 120.3 . . ? C41 C42 C38 118.7(6) . . ? C41 C42 H42A 120.7 . . ? C38 C42 H42A 120.7 . . ? F14 P1 F15 90.5(6) . . ? F14 P1 F16 94.9(7) . . ? F15 P1 F16 88.9(5) . . ? F14 P1 F11 176.8(8) . . ? F15 P1 F11 88.7(4) . . ? F16 P1 F11 88.1(7) . . ? F14 P1 F13 94.4(7) . . ? F15 P1 F13 175.1(6) . . ? F16 P1 F13 90.7(5) . . ? F11 P1 F13 86.4(6) . . ? F14 P1 F12 87.2(7) . . ? F15 P1 F12 88.3(6) . . ? F16 P1 F12 176.6(7) . . ? F11 P1 F12 89.8(7) . . ? F13 P1 F12 91.8(7) . . ? F22 P2 F21 88(2) . . ? F22 P2 F23 88.6(12) . . ? F21 P2 F23 89.1(8) . . ? F22 P2 F24 88.9(18) . . ? F21 P2 F24 176.7(14) . . ? F23 P2 F24 89.9(8) . . ? F22 P2 F26 177.1(13) . . ? F21 P2 F26 92.7(13) . . ? F23 P2 F26 88.6(6) . . ? F24 P2 F26 90.4(13) . . ? F22 P2 F25 93.6(12) . . ? F21 P2 F25 96.9(7) . . ? F23 P2 F25 173.7(8) . . ? F24 P2 F25 84.2(8) . . ? F26 P2 F25 89.1(6) . . ? F24' P2' F23' 86.8(8) . . ? F24' P2' F26' 89.2(13) . . ? F23' P2' F26' 88.8(12) . . ? F24' P2' F21' 177.6(14) . . ? F23' P2' F21' 94.0(8) . . ? F26' P2' F21' 88.6(12) . . ? F24' P2' F22' 85.5(10) . . ? F23' P2' F22' 97.8(12) . . ? F26' P2' F22' 171.4(13) . . ? F21' P2' F22' 96.5(11) . . ? F31 P3 F31 180.000(2) . 2_667 ? F31 P3 F33 89.8(3) . . ? F31 P3 F33 90.2(3) 2_667 . ? F31 P3 F33 90.2(3) . 2_667 ? F31 P3 F33 89.8(3) 2_667 2_667 ? F33 P3 F33 180.000(3) . 2_667 ? F31 P3 F32 89.2(3) . 2_667 ? F31 P3 F32 90.8(3) 2_667 2_667 ? F33 P3 F32 90.9(2) . 2_667 ? F33 P3 F32 89.1(2) 2_667 2_667 ? F31 P3 F32 90.8(3) . . ? F31 P3 F32 89.2(3) 2_667 . ? F33 P3 F32 89.1(2) . . ? F33 P3 F32 90.9(2) 2_667 . ? F32 P3 F32 180.000(5) 2_667 . ? C101 C100 H10A 109.5 . . ? C101 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? C101 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? N100 C101 C100 179.0(12) . . ? F44 P4 F42 92.0(9) . . ? F44 P4 F43 91.9(9) . . ? F42 P4 F43 94.7(9) . . ? F44 P4 F46 95.5(14) . . ? F42 P4 F46 91.1(8) . . ? F43 P4 F46 170.4(14) . . ? F44 P4 F41 94.5(8) . . ? F42 P4 F41 171.8(14) . . ? F43 P4 F41 80.0(15) . . ? F46 P4 F41 93.3(9) . . ? F44 P4 F45 172.7(15) . . ? F42 P4 F45 87.6(17) . . ? F43 P4 F45 80.8(16) . . ? F46 P4 F45 91.8(10) . . ? F41 P4 F45 85.4(18) . . ? C301 C300 H30B 109.5 . . ? C301 C300 H30C 109.5 . . ? H30B C300 H30C 109.5 . . ? C301 C300 H30D 109.5 . . ? H30B C300 H30D 109.5 . . ? H30C C300 H30D 109.5 . . ? N300 C301 C300 178.9(9) . . ? N200 C201 C200 160.6(19) . . ? C201 C200 H20B 109.5 . . ? C201 C200 H20C 109.5 . . ? H20B C200 H20C 109.5 . . ? C201 C200 H20D 109.5 . . ? H20B C200 H20D 109.5 . . ? H20C C200 H20D 109.5 . . ? N500 C500 C501 157(10) . . ? C500 C501 H50A 109.5 . . ? C500 C501 H50B 109.5 . . ? H50A C501 H50B 109.5 . . ? C500 C501 H50C 109.5 . . ? H50A C501 H50C 109.5 . . ? H50B C501 H50C 109.5 . . ? N400 C401 C400 156(4) . . ? C401 C400 H40B 109.5 . . ? C401 C400 H40C 109.5 . . ? H40B C400 H40C 109.5 . . ? C401 C400 H40D 109.5 . . ? H40B C400 H40D 109.5 . . ? H40C C400 H40D 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.809 _refine_diff_density_min -1.039 _refine_diff_density_rms 0.103 # start Validation Reply Form _vrf_PLAT242_jb1167 ; PROBLEM: Check Low Ueq as Compared to Neighbors for P4 RESPONSE: PF6 anion disordered ; _vrf_PLAT430_jb1167 ; PROBLEM: Short Inter D...A Contact O1" .. N500 .. 2.44 Ang. RESPONSE: Refers to atoms of partial occupancy ; _vrf_PLAT432_jb1167 ; PROBLEM: Short Inter X...Y Contact F45 .. C501 .. 2.56 Ang. RESPONSE: Refers to atoms of partial occupancy ; _vrf_PLAT780_jb1167 ; PROBLEM: Coordinates do not Form a Properly Connected Set ? RESPONSE: There are two complexes and two sets of disordered solvent molecules ; # end Validation Reply Form # Attachment 'Ligand_1_JZ.CIF' data_jb999 _database_code_depnum_ccdc_archive 'CCDC 692940' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H16 N6, C H Cl3, H2 O' _chemical_formula_sum 'C22 H19 Cl3 N6 O' _chemical_formula_weight 489.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.957(2) _cell_length_b 10.336(2) _cell_length_c 12.413(3) _cell_angle_alpha 71.39(3) _cell_angle_beta 71.60(3) _cell_angle_gamma 88.82(3) _cell_volume 1144.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 0.428 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20589 _diffrn_reflns_av_R_equivalents 0.1144 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3989 _reflns_number_gt 3666 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+1.8426P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3989 _refine_ls_number_parameters 295 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1401 _refine_ls_wR_factor_gt 0.1367 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.4652(2) 1.1666(2) 0.7729(2) 0.0271(5) Uani 1 1 d . . . C1 C 0.1575(3) 0.5074(3) 0.6598(3) 0.0306(6) Uani 1 1 d . . . H1 H 0.0778 0.4598 0.6583 0.037 Uiso 1 1 calc R . . N2 N 0.3468(2) 0.8987(2) 0.69256(19) 0.0220(5) Uani 1 1 d . . . C2 C 0.2866(3) 0.4520(3) 0.6345(3) 0.0319(6) Uani 1 1 d . . . H2 H 0.2952 0.3683 0.6175 0.038 Uiso 1 1 calc R . . N3 N 0.1373(2) 0.6235(2) 0.6862(2) 0.0270(5) Uani 1 1 d . . . C3 C 0.4033(3) 0.5229(3) 0.6347(3) 0.0306(6) Uani 1 1 d . . . H3A H 0.4940 0.4883 0.6178 0.037 Uiso 1 1 calc R . . N4 N -0.0562(2) 0.9939(2) 0.8661(2) 0.0255(5) Uani 1 1 d . . . H4B H -0.1298 0.9345 0.8879 0.031 Uiso 1 1 calc R . . C4 C 0.3863(3) 0.6438(3) 0.6596(2) 0.0262(6) Uani 1 1 d . . . H4A H 0.4654 0.6945 0.6586 0.031 Uiso 1 1 calc R . . N5 N -0.0735(2) 1.1143(2) 0.8888(2) 0.0229(5) Uani 1 1 d . . . C5 C 0.2516(3) 0.6911(3) 0.6864(2) 0.0221(5) Uani 1 1 d . . . C6 C 0.2286(3) 0.8185(3) 0.7187(2) 0.0208(5) Uani 1 1 d . . . N6 N -0.2862(3) 1.5071(2) 1.0226(2) 0.0307(5) Uani 1 1 d . . . C7 C 0.0938(3) 0.8477(3) 0.7758(2) 0.0220(5) Uani 1 1 d . . . H7A H 0.0131 0.7880 0.7925 0.026 Uiso 1 1 calc R . . C8 C 0.0778(3) 0.9659(3) 0.8087(2) 0.0218(5) Uani 1 1 d . . . C9 C 0.2004(3) 1.0498(3) 0.7825(2) 0.0219(5) Uani 1 1 d . . . H9A H 0.1944 1.1315 0.8028 0.026 Uiso 1 1 calc R . . C10 C 0.3304(3) 1.0106(3) 0.7265(2) 0.0203(5) Uani 1 1 d . . . C11 C 0.4673(3) 1.0896(3) 0.7032(2) 0.0215(5) Uani 1 1 d . . . C12 C 0.5901(3) 1.0766(3) 0.6170(2) 0.0274(6) Uani 1 1 d . . . H12A H 0.5873 1.0233 0.5678 0.033 Uiso 1 1 calc R . . C13 C 0.7174(3) 1.1429(3) 0.6034(3) 0.0307(6) Uani 1 1 d . . . H13A H 0.8032 1.1351 0.5452 0.037 Uiso 1 1 calc R . . C14 C 0.7170(3) 1.2201(3) 0.6760(3) 0.0318(6) Uani 1 1 d . . . H14A H 0.8026 1.2652 0.6697 0.038 Uiso 1 1 calc R . . C15 C 0.5898(3) 1.2304(3) 0.7575(3) 0.0326(6) Uani 1 1 d . . . H15A H 0.5899 1.2856 0.8057 0.039 Uiso 1 1 calc R . . C16 C -0.1999(3) 1.1319(3) 0.9487(2) 0.0236(5) Uani 1 1 d . . . H16A H -0.2750 1.0620 0.9758 0.028 Uiso 1 1 calc R . . C17 C -0.2272(3) 1.2594(3) 0.9748(2) 0.0219(5) Uani 1 1 d . . . C18 C -0.3641(3) 1.2821(3) 1.0366(2) 0.0262(6) Uani 1 1 d . . . H18A H -0.4407 1.2138 1.0632 0.031 Uiso 1 1 calc R . . C19 C -0.3874(3) 1.4050(3) 1.0588(3) 0.0295(6) Uani 1 1 d . . . H19A H -0.4811 1.4175 1.1025 0.035 Uiso 1 1 calc R . . C20 C -0.1546(3) 1.4840(3) 0.9638(3) 0.0305(6) Uani 1 1 d . . . H20A H -0.0806 1.5547 0.9374 0.037 Uiso 1 1 calc R . . C21 C -0.1200(3) 1.3643(3) 0.9393(3) 0.0270(6) Uani 1 1 d . . . H21A H -0.0244 1.3531 0.8987 0.032 Uiso 1 1 calc R . . Cl1 Cl -0.13027(12) 0.83353(13) 0.48550(8) 0.0669(3) Uani 1 1 d . . . O1 O -0.2884(3) 0.7884(2) 1.0087(2) 0.0413(6) Uani 1 1 d . . . Cl2 Cl -0.22524(12) 0.55745(10) 0.65021(12) 0.0638(3) Uani 1 1 d . . . Cl3 Cl -0.25525(9) 0.78390(9) 0.74076(8) 0.0440(2) Uani 1 1 d . . . C22 C -0.1499(3) 0.7199(3) 0.6304(3) 0.0344(7) Uani 1 1 d . . . H22A H -0.0537 0.7092 0.6396 0.041 Uiso 1 1 calc R . . H1B H -0.284(4) 0.706(5) 1.024(4) 0.052 Uiso 1 1 d . . . H2B H -0.329(4) 0.795(4) 1.081(4) 0.052 Uiso 1 1 d . . . 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 N1 0.0248(12) 0.0286(12) 0.0291(12) -0.0120(10) -0.0076(10) -0.0007(9) C1 0.0298(15) 0.0296(14) 0.0338(16) -0.0155(12) -0.0069(12) -0.0021(11) N2 0.0219(11) 0.0232(11) 0.0200(11) -0.0066(9) -0.0062(9) 0.0005(9) C2 0.0383(16) 0.0280(14) 0.0322(15) -0.0164(12) -0.0090(13) 0.0053(12) N3 0.0251(12) 0.0272(12) 0.0306(12) -0.0134(10) -0.0075(10) 0.0005(9) C3 0.0289(14) 0.0346(15) 0.0322(15) -0.0166(13) -0.0103(12) 0.0105(12) N4 0.0191(11) 0.0245(11) 0.0333(13) -0.0148(10) -0.0036(9) 0.0006(9) C4 0.0242(13) 0.0306(14) 0.0269(14) -0.0135(12) -0.0085(11) 0.0032(11) N5 0.0237(11) 0.0227(11) 0.0235(11) -0.0092(9) -0.0078(9) 0.0031(9) C5 0.0248(13) 0.0234(13) 0.0178(12) -0.0064(10) -0.0066(10) 0.0008(10) C6 0.0219(12) 0.0224(12) 0.0178(12) -0.0060(10) -0.0067(10) 0.0013(10) N6 0.0389(14) 0.0259(12) 0.0278(12) -0.0093(10) -0.0111(11) 0.0079(10) C7 0.0219(12) 0.0216(12) 0.0225(13) -0.0070(10) -0.0073(10) -0.0010(10) C8 0.0221(13) 0.0236(13) 0.0179(12) -0.0056(10) -0.0057(10) 0.0030(10) C9 0.0248(13) 0.0200(12) 0.0206(13) -0.0067(10) -0.0068(10) 0.0013(10) C10 0.0218(12) 0.0205(12) 0.0168(12) -0.0040(10) -0.0059(10) -0.0008(10) C11 0.0226(13) 0.0196(12) 0.0198(12) -0.0030(10) -0.0070(10) 0.0007(10) C12 0.0267(14) 0.0285(14) 0.0256(14) -0.0099(11) -0.0053(11) -0.0008(11) C13 0.0226(13) 0.0337(15) 0.0288(15) -0.0069(12) -0.0019(11) -0.0019(11) C14 0.0253(14) 0.0305(15) 0.0379(16) -0.0078(13) -0.0109(12) -0.0055(11) C15 0.0315(15) 0.0331(15) 0.0383(16) -0.0181(13) -0.0117(13) -0.0007(12) C16 0.0222(13) 0.0245(13) 0.0235(13) -0.0072(11) -0.0071(11) 0.0010(10) C17 0.0229(13) 0.0244(13) 0.0187(12) -0.0070(10) -0.0076(10) 0.0046(10) C18 0.0228(13) 0.0280(14) 0.0254(14) -0.0068(11) -0.0066(11) 0.0021(11) C19 0.0284(14) 0.0327(15) 0.0270(14) -0.0115(12) -0.0073(12) 0.0100(12) C20 0.0338(15) 0.0249(14) 0.0320(15) -0.0084(12) -0.0108(12) -0.0005(11) C21 0.0233(13) 0.0251(13) 0.0296(15) -0.0080(11) -0.0056(11) 0.0026(11) Cl1 0.0674(7) 0.0859(8) 0.0321(5) -0.0026(5) -0.0131(4) 0.0103(5) O1 0.0447(13) 0.0298(11) 0.0388(13) -0.0185(10) 0.0086(10) -0.0093(10) Cl2 0.0668(6) 0.0471(5) 0.1007(9) -0.0336(5) -0.0493(6) 0.0058(4) Cl3 0.0389(4) 0.0509(5) 0.0410(5) -0.0173(4) -0.0097(3) 0.0087(3) C22 0.0308(15) 0.0423(17) 0.0344(16) -0.0132(14) -0.0158(13) 0.0050(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C11 1.345(3) . ? N1 C15 1.347(4) . ? C1 N3 1.338(4) . ? C1 C2 1.381(4) . ? C1 H1 0.9500 . ? N2 C10 1.342(3) . ? N2 C6 1.344(3) . ? C2 C3 1.388(4) . ? C2 H2 0.9500 . ? N3 C5 1.348(3) . ? C3 C4 1.375(4) . ? C3 H3A 0.9500 . ? N4 N5 1.357(3) . ? N4 C8 1.374(3) . ? N4 H4B 0.8800 . ? C4 C5 1.394(4) . ? C4 H4A 0.9500 . ? N5 C16 1.288(4) . ? C5 C6 1.489(4) . ? C6 C7 1.383(4) . ? N6 C19 1.337(4) . ? N6 C20 1.342(4) . ? C7 C8 1.398(4) . ? C7 H7A 0.9500 . ? C8 C9 1.400(4) . ? C9 C10 1.383(4) . ? C9 H9A 0.9500 . ? C10 C11 1.501(3) . ? C11 C12 1.384(4) . ? C12 C13 1.390(4) . ? C12 H12A 0.9500 . ? C13 C14 1.381(4) . ? C13 H13A 0.9500 . ? C14 C15 1.376(4) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.455(4) . ? C16 H16A 0.9500 . ? C17 C18 1.394(4) . ? C17 C21 1.398(4) . ? C18 C19 1.383(4) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C21 1.378(4) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? Cl1 C22 1.758(3) . ? O1 H1B 0.81(4) . ? O1 H2B 0.89(4) . ? Cl2 C22 1.765(3) . ? Cl3 C22 1.748(3) . ? C22 H22A 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 N1 C15 117.2(2) . . ? N3 C1 C2 124.3(3) . . ? N3 C1 H1 117.9 . . ? C2 C1 H1 117.9 . . ? C10 N2 C6 117.0(2) . . ? C1 C2 C3 117.7(3) . . ? C1 C2 H2 121.1 . . ? C3 C2 H2 121.1 . . ? C1 N3 C5 117.3(2) . . ? C4 C3 C2 119.3(3) . . ? C4 C3 H3A 120.4 . . ? C2 C3 H3A 120.4 . . ? N5 N4 C8 119.1(2) . . ? N5 N4 H4B 120.5 . . ? C8 N4 H4B 120.5 . . ? C3 C4 C5 119.3(3) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? C16 N5 N4 116.5(2) . . ? N3 C5 C4 122.1(2) . . ? N3 C5 C6 117.3(2) . . ? C4 C5 C6 120.5(2) . . ? N2 C6 C7 123.2(2) . . ? N2 C6 C5 115.5(2) . . ? C7 C6 C5 121.2(2) . . ? C19 N6 C20 116.1(2) . . ? C6 C7 C8 119.2(2) . . ? C6 C7 H7A 120.4 . . ? C8 C7 H7A 120.4 . . ? N4 C8 C7 118.9(2) . . ? N4 C8 C9 123.0(2) . . ? C7 C8 C9 118.1(2) . . ? C10 C9 C8 118.2(2) . . ? C10 C9 H9A 120.9 . . ? C8 C9 H9A 120.9 . . ? N2 C10 C9 124.2(2) . . ? N2 C10 C11 114.3(2) . . ? C9 C10 C11 121.5(2) . . ? N1 C11 C12 122.7(2) . . ? N1 C11 C10 117.1(2) . . ? C12 C11 C10 120.2(2) . . ? C11 C12 C13 119.0(3) . . ? C11 C12 H12A 120.5 . . ? C13 C12 H12A 120.5 . . ? C14 C13 C12 118.8(3) . . ? C14 C13 H13A 120.6 . . ? C12 C13 H13A 120.6 . . ? C15 C14 C13 118.6(3) . . ? C15 C14 H14A 120.7 . . ? C13 C14 H14A 120.7 . . ? N1 C15 C14 123.7(3) . . ? N1 C15 H15A 118.1 . . ? C14 C15 H15A 118.1 . . ? N5 C16 C17 119.7(2) . . ? N5 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C18 C17 C21 117.0(2) . . ? C18 C17 C16 120.5(2) . . ? C21 C17 C16 122.4(2) . . ? C19 C18 C17 119.3(3) . . ? C19 C18 H18A 120.3 . . ? C17 C18 H18A 120.3 . . ? N6 C19 C18 124.1(3) . . ? N6 C19 H19A 117.9 . . ? C18 C19 H19A 117.9 . . ? N6 C20 C21 124.3(3) . . ? N6 C20 H20A 117.9 . . ? C21 C20 H20A 117.9 . . ? C20 C21 C17 119.2(3) . . ? C20 C21 H21A 120.4 . . ? C17 C21 H21A 120.4 . . ? H1B O1 H2B 102(4) . . ? Cl3 C22 Cl1 110.99(17) . . ? Cl3 C22 Cl2 109.86(18) . . ? Cl1 C22 Cl2 110.52(17) . . ? Cl3 C22 H22A 108.5 . . ? Cl1 C22 H22A 108.5 . . ? Cl2 C22 H22A 108.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.510 _refine_diff_density_min -0.759 _refine_diff_density_rms 0.061 # Attachment 'Polymer.CIF' data_jb21ap-1 _database_code_depnum_ccdc_archive 'CCDC 692941' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[{Ru(tpyNHNCHpy)2}2Fe(NCS)2]An(NCS)2' _chemical_melting_point ? _chemical_formula_moiety 'Fe (N C S)2 Ru2 C84 H64 N24,Fe2 O4 C8 H22 (N C S)6,(NCS)2,C8 H26 O5' _chemical_formula_sum 'C116 H132 Fe3 N34 O13 Ru2 S10' _chemical_formula_weight 2900.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.812(8) _cell_length_b 15.073(8) _cell_length_c 18.604(10) _cell_angle_alpha 67.221(8) _cell_angle_beta 70.821(8) _cell_angle_gamma 73.834(8) _cell_volume 3322(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 986 _cell_measurement_theta_min 2.567 _cell_measurement_theta_max 20.1165 _exptl_crystal_description plate _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.770 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.905 _exptl_absorpt_correction_T_max 0.977 _exptl_absorpt_process_details 'SADABS, Bruker 1995' _exptl_special_details ; In a thin film of perfluoropolyether oil on a mohair fibre ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 48 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 28554 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.2446 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 26.37 _reflns_number_total 13366 _reflns_number_gt 5422 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1109P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13366 _refine_ls_number_parameters 750 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.2173 _refine_ls_R_factor_gt 0.0822 _refine_ls_wR_factor_ref 0.2416 _refine_ls_wR_factor_gt 0.1821 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.34446(6) 0.23985(5) 1.13850(4) 0.0288(2) Uani 1 1 d . . . Fe1 Fe 0.0000 0.5000 0.5000 0.0280(4) Uani 1 2 d S . . Fe2 Fe 0.04463(13) -0.03744(13) 1.07580(10) 0.0631(5) Uani 1 1 d . . . S1 S 0.3207(3) 0.6156(4) 0.4475(3) 0.1300(18) Uani 1 1 d . . . S2 S 0.3816(2) 0.0412(2) 0.9531(2) 0.0726(10) Uani 1 1 d . . . S3 S 0.0218(3) 0.0886(3) 1.2797(3) 0.1176(17) Uani 1 1 d . . . S4 S 0.2134(3) -0.2910(2) 1.25693(19) 0.0686(9) Uani 1 1 d . . . S5 S -0.2541(2) 0.4530(2) 1.22207(17) 0.0604(8) Uani 1 1 d . . . O1 O 0.0415(5) -0.0752(5) 0.9857(4) 0.059(2) Uani 1 1 d . . . O2 O -0.1016(6) -0.0901(6) 1.1360(5) 0.084(3) Uani 1 1 d . . . O70 O 0.8041(10) 0.2215(10) 1.4772(8) 0.155(5) Uiso 1 1 d . . . H70 H 0.8429 0.2196 1.4321 0.186 Uiso 1 1 calc R . . O76 O 0.508(2) 0.351(2) 0.4244(17) 0.357(10) Uiso 1 1 d D . . H76 H 0.5537 0.3025 0.4180 0.429 Uiso 1 1 calc . . . O77 O 0.4519(13) 0.2375(13) 0.5951(10) 0.213(7) Uiso 1 1 d D . . H77 H 0.5006 0.2527 0.5538 0.256 Uiso 1 1 calc R . . O80 O 0.669(3) -0.043(3) 1.556(3) 0.293(15) Uiso 0.50 1 d PD . . O730 O 0.788(3) 0.2198(17) 1.317(2) 0.085(11) Uiso 0.40(4) 1 d P . . O731 O 0.7340(16) 0.2322(10) 1.3518(11) 0.061(6) Uiso 0.60(4) 1 d P . . N1 N 0.3427(5) 0.0921(5) 1.1798(4) 0.0332(18) Uani 1 1 d . . . N2 N 0.4582(5) 0.1886(5) 1.1935(4) 0.0303(17) Uani 1 1 d . . . N3 N 0.3931(5) 0.3657(5) 1.1177(4) 0.0250(16) Uani 1 1 d . . . N4 N 0.6929(6) 0.0832(5) 1.3092(4) 0.043(2) Uani 1 1 d . . . H4 H 0.7245 0.1249 1.3114 0.052 Uiso 1 1 calc R . . N5 N 0.7232(6) -0.0139(5) 1.3419(4) 0.0365(18) Uani 1 1 d . . . N6 N 0.9297(6) -0.3409(5) 1.4607(4) 0.0312(17) Uani 1 1 d . . . N7 N 0.4191(5) 0.2409(5) 1.0229(4) 0.0281(16) Uani 1 1 d . . . N8 N 0.2285(5) 0.2920(5) 1.0867(4) 0.0270(16) Uani 1 1 d . . . N9 N 0.2223(5) 0.2575(5) 1.2342(4) 0.0281(17) Uani 1 1 d . . . N10 N -0.0171(5) 0.3966(5) 0.9807(4) 0.0326(18) Uani 1 1 d . . . H10 H -0.0807 0.4095 1.0098 0.039 Uiso 1 1 calc R . . N11 N -0.0001(6) 0.4110(5) 0.9025(4) 0.0318(17) Uani 1 1 d . . . N12 N -0.0273(5) 0.4948(5) 0.6232(4) 0.0297(17) Uani 1 1 d . . . N13 N 0.1485(6) 0.5355(5) 0.4740(4) 0.0338(18) Uani 1 1 d . . . N14 N 0.1798(8) 0.0138(8) 1.0153(6) 0.072(3) Uani 1 1 d . . . N15 N 0.0190(8) 0.0185(8) 1.1647(7) 0.075(3) Uani 1 1 d . . . N16 N 0.1165(8) -0.1675(8) 1.1365(7) 0.076(3) Uani 1 1 d . . . N17 N -0.2288(6) 0.4367(6) 1.0727(5) 0.052(2) Uani 1 1 d . . . C1 C 0.2804(7) 0.0467(7) 1.1703(5) 0.041(2) Uani 1 1 d . . . H1 H 0.2338 0.0841 1.1370 0.049 Uiso 1 1 calc R . . C2 C 0.2803(8) -0.0498(7) 1.2056(6) 0.045(3) Uani 1 1 d . . . H2 H 0.2332 -0.0787 1.1978 0.053 Uiso 1 1 calc R . . C3 C 0.3473(8) -0.1065(7) 1.2525(6) 0.050(3) Uani 1 1 d . . . H3 H 0.3473 -0.1746 1.2785 0.059 Uiso 1 1 calc R . . C4 C 0.4146(7) -0.0610(6) 1.2605(5) 0.035(2) Uani 1 1 d . . . H4A H 0.4638 -0.0984 1.2915 0.042 Uiso 1 1 calc R . . C5 C 0.4120(7) 0.0362(6) 1.2250(5) 0.030(2) Uani 1 1 d . . . C6 C 0.4797(6) 0.0921(6) 1.2309(5) 0.028(2) Uani 1 1 d . . . C7 C 0.5587(7) 0.0523(6) 1.2701(5) 0.036(2) Uani 1 1 d . . . H7 H 0.5756 -0.0163 1.2947 0.043 Uiso 1 1 calc R . . C8 C 0.6127(7) 0.1160(7) 1.2726(5) 0.034(2) Uani 1 1 d . . . C9 C 0.8070(7) -0.0406(7) 1.3662(5) 0.042(2) Uani 1 1 d . . . H9 H 0.8429 0.0074 1.3616 0.050 Uiso 1 1 calc R . . C10 C 0.8474(7) -0.1435(6) 1.4005(5) 0.031(2) Uani 1 1 d . . . C11 C 0.7849(7) -0.2145(7) 1.4305(5) 0.038(2) Uani 1 1 d . . . H11A H 0.7135 -0.1970 1.4297 0.046 Uiso 1 1 calc R . . C12 C 0.8288(7) -0.3105(7) 1.4612(5) 0.038(2) Uani 1 1 d . . . H12 H 0.7849 -0.3582 1.4843 0.046 Uiso 1 1 calc R . . C13 C 0.9868(8) -0.2721(7) 1.4320(5) 0.040(2) Uani 1 1 d . . . H13 H 1.0585 -0.2916 1.4315 0.048 Uiso 1 1 calc R . . C14 C 0.9497(7) -0.1745(7) 1.4029(6) 0.043(3) Uani 1 1 d . . . H14 H 0.9947 -0.1283 1.3844 0.051 Uiso 1 1 calc R . . C15 C 0.5879(6) 0.2169(6) 1.2358(5) 0.032(2) Uani 1 1 d . . . H15 H 0.6241 0.2608 1.2375 0.039 Uiso 1 1 calc R . . C16 C 0.5092(6) 0.2503(6) 1.1969(5) 0.0252(19) Uani 1 1 d . . . C17 C 0.4701(6) 0.3517(6) 1.1550(5) 0.028(2) Uani 1 1 d . . . C18 C 0.5051(7) 0.4315(6) 1.1506(5) 0.036(2) Uani 1 1 d . . . H18 H 0.5564 0.4215 1.1780 0.043 Uiso 1 1 calc R . . C19 C 0.4677(7) 0.5239(6) 1.1081(6) 0.040(2) Uani 1 1 d . . . H19 H 0.4922 0.5784 1.1054 0.048 Uiso 1 1 calc R . . C20 C 0.3924(7) 0.5367(7) 1.0686(5) 0.039(2) Uani 1 1 d . . . H20 H 0.3649 0.6002 1.0380 0.046 Uiso 1 1 calc R . . C21 C 0.3587(6) 0.4564(6) 1.0746(5) 0.031(2) Uani 1 1 d . . . H21 H 0.3082 0.4657 1.0467 0.037 Uiso 1 1 calc R . . C22 C 0.5200(7) 0.2112(6) 0.9943(5) 0.035(2) Uani 1 1 d . . . H22 H 0.5638 0.1828 1.0305 0.042 Uiso 1 1 calc R . . C23 C 0.5635(8) 0.2203(7) 0.9139(6) 0.042(2) Uani 1 1 d . . . H23 H 0.6356 0.1976 0.8954 0.050 Uiso 1 1 calc R . . C24 C 0.5010(7) 0.2625(7) 0.8616(6) 0.040(2) Uani 1 1 d . . . H24 H 0.5294 0.2716 0.8058 0.048 Uiso 1 1 calc R . . C25 C 0.3970(7) 0.2915(6) 0.8904(5) 0.031(2) Uani 1 1 d . . . H25 H 0.3528 0.3204 0.8546 0.037 Uiso 1 1 calc R . . C26 C 0.3561(6) 0.2788(6) 0.9713(5) 0.0260(19) Uani 1 1 d . . . C27 C 0.2466(7) 0.3058(6) 1.0078(5) 0.028(2) Uani 1 1 d . . . C28 C 0.1665(7) 0.3386(6) 0.9716(5) 0.031(2) Uani 1 1 d . . . H28 H 0.1796 0.3459 0.9164 0.038 Uiso 1 1 calc R . . C29 C 0.0656(6) 0.3614(6) 1.0154(5) 0.0263(19) Uani 1 1 d . . . C30 C -0.0764(7) 0.4400(6) 0.8719(5) 0.034(2) Uani 1 1 d . . . H30 H -0.1450 0.4484 0.9050 0.041 Uiso 1 1 calc R . . C31 C -0.0611(7) 0.4608(6) 0.7865(5) 0.031(2) Uani 1 1 d . . . C32 C 0.0389(7) 0.4502(7) 0.7379(5) 0.037(2) Uani 1 1 d . . . H32 H 0.0975 0.4311 0.7599 0.044 Uiso 1 1 calc R . . C33 C 0.0521(7) 0.4674(7) 0.6579(5) 0.036(2) Uani 1 1 d . . . H33 H 0.1210 0.4595 0.6252 0.044 Uiso 1 1 calc R . . C34 C -0.1226(7) 0.5071(6) 0.6706(5) 0.031(2) Uani 1 1 d . . . H34 H -0.1800 0.5289 0.6470 0.037 Uiso 1 1 calc R . . C35 C -0.1427(7) 0.4902(6) 0.7514(5) 0.033(2) Uani 1 1 d . . . H35 H -0.2124 0.4986 0.7827 0.039 Uiso 1 1 calc R . . C36 C 0.0478(6) 0.3486(6) 1.0965(5) 0.029(2) Uani 1 1 d . . . H36 H -0.0205 0.3644 1.1274 0.035 Uiso 1 1 calc R . . C37 C 0.1308(6) 0.3126(6) 1.1315(5) 0.0262(19) Uani 1 1 d . . . C38 C 0.1289(6) 0.2927(6) 1.2162(5) 0.0252(19) Uani 1 1 d . . . C39 C 0.0379(7) 0.3065(7) 1.2745(5) 0.034(2) Uani 1 1 d . . . H39 H -0.0271 0.3324 1.2607 0.041 Uiso 1 1 calc R . . C40 C 0.0432(8) 0.2823(7) 1.3518(5) 0.039(2) Uani 1 1 d . . . H40 H -0.0180 0.2908 1.3926 0.047 Uiso 1 1 calc R . . C41 C 0.1373(8) 0.2458(6) 1.3696(5) 0.038(2) Uani 1 1 d . . . H41 H 0.1419 0.2281 1.4234 0.045 Uiso 1 1 calc R . . C42 C 0.2244(7) 0.2346(6) 1.3112(5) 0.035(2) Uani 1 1 d . . . H42 H 0.2894 0.2096 1.3249 0.042 Uiso 1 1 calc R . . C50 C 0.2185(9) 0.5681(8) 0.4639(7) 0.055(3) Uani 1 1 d . . . C60 C 0.2637(9) 0.0249(7) 0.9899(6) 0.048(3) Uani 1 1 d . . . C61 C 0.0158(10) 0.0514(10) 1.2110(8) 0.078(4) Uani 1 1 d . . . C62 C 0.1560(9) -0.2201(9) 1.1880(7) 0.057(3) Uani 1 1 d . . . C63 C 0.0799(10) -0.1696(9) 0.9776(8) 0.078(4) Uani 1 1 d . . . H63A H 0.0356 -0.1828 0.9518 0.094 Uiso 1 1 calc R . . H63B H 0.0762 -0.2194 1.0316 0.094 Uiso 1 1 calc R . . C64 C 0.1919(11) -0.1777(11) 0.9272(9) 0.108(5) Uani 1 1 d . . . H64A H 0.2164 -0.2436 0.9231 0.162 Uiso 1 1 calc R . . H64B H 0.2361 -0.1651 0.9528 0.162 Uiso 1 1 calc R . . H64C H 0.1955 -0.1296 0.8732 0.162 Uiso 1 1 calc R . . C65 C -0.1256(12) -0.1703(14) 1.1938(9) 0.124(5) Uani 1 1 d . . . H65A H -0.1086 -0.1699 1.2413 0.149 Uiso 1 1 calc R . . H65B H -0.0761 -0.2248 1.1773 0.149 Uiso 1 1 calc R . . C66 C -0.2238(12) -0.1972(13) 1.2216(9) 0.124(5) Uani 1 1 d . . . H66A H -0.2218 -0.2610 1.2640 0.186 Uiso 1 1 calc R . . H66B H -0.2435 -0.2011 1.1770 0.186 Uiso 1 1 calc R . . H66C H -0.2751 -0.1482 1.2433 0.186 Uiso 1 1 calc R . . C71 C 0.8215(19) 0.1211(18) 1.5409(13) 0.155(8) Uiso 1 1 d . . . C74 C 0.384(3) 0.297(3) 0.380(2) 0.357(10) Uiso 1 1 d D . . H74A H 0.3371 0.3231 0.3440 0.536 Uiso 1 1 calc R . . H74B H 0.3450 0.2704 0.4354 0.536 Uiso 1 1 calc R . . H74C H 0.4381 0.2448 0.3640 0.536 Uiso 1 1 calc R . . C75 C 0.434(3) 0.375(2) 0.373(2) 0.357(10) Uiso 1 1 d D . . H75A H 0.3778 0.4285 0.3854 0.429 Uiso 1 1 calc R . . H75B H 0.4718 0.4014 0.3159 0.429 Uiso 1 1 calc R . . C78 C 0.431(2) 0.3031(19) 0.6398(15) 0.230(12) Uiso 1 1 d D . . H78A H 0.3802 0.2766 0.6911 0.276 Uiso 1 1 calc R . . H78B H 0.4963 0.2958 0.6541 0.276 Uiso 1 1 calc R . . C79 C 0.395(3) 0.403(2) 0.612(2) 0.313(18) Uiso 1 1 d D . . H79A H 0.3791 0.4297 0.6560 0.469 Uiso 1 1 calc R . . H79B H 0.3311 0.4143 0.5951 0.469 Uiso 1 1 calc R . . H79C H 0.4478 0.4345 0.5670 0.469 Uiso 1 1 calc R . . C81 C 0.580(3) -0.071(3) 1.544(4) 0.293(15) Uiso 0.50 1 d PD . . H81A H 0.5399 -0.1051 1.5986 0.352 Uiso 0.50 1 calc PR . . H81B H 0.6113 -0.1212 1.5168 0.352 Uiso 0.50 1 calc PR . . C82 C 0.5000 0.0000 1.5000 0.293(15) Uiso 1 2 d SD . . H82A H 0.4525 -0.0358 1.4975 0.440 Uiso 0.50 1 calc PR . . H82B H 0.5356 0.0354 1.4452 0.440 Uiso 0.50 1 calc PR . . H82C H 0.4604 0.0465 1.5287 0.440 Uiso 0.50 1 calc PR . . C90 C -0.2408(6) 0.4430(7) 1.1352(7) 0.044(3) Uani 1 1 d . . . C720 C 0.773(3) 0.053(2) 1.5380(19) 0.153(17) Uiso 0.60(3) 1 d P . . H72A H 0.6977 0.0699 1.5569 0.229 Uiso 0.60(3) 1 calc PR . . H72B H 0.7976 -0.0125 1.5726 0.229 Uiso 0.60(3) 1 calc PR . . H72C H 0.7909 0.0527 1.4825 0.229 Uiso 0.60(3) 1 calc PR . . C721 C 0.891(4) 0.054(3) 1.514(2) 0.118(19) Uiso 0.40(3) 1 d P . . H72D H 0.9604 0.0690 1.5014 0.177 Uiso 0.40(3) 1 calc PR . . H72E H 0.8774 0.0538 1.4660 0.177 Uiso 0.40(3) 1 calc PR . . H72F H 0.8858 -0.0098 1.5560 0.177 Uiso 0.40(3) 1 calc PR . . 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 0.0335(5) 0.0286(4) 0.0307(4) -0.0141(3) -0.0120(3) -0.0039(3) Fe1 0.0310(10) 0.0336(11) 0.0264(10) -0.0158(8) -0.0129(8) -0.0004(8) Fe2 0.0579(11) 0.0692(12) 0.0751(12) -0.0340(10) -0.0087(9) -0.0251(9) S1 0.089(3) 0.128(4) 0.210(5) -0.049(4) -0.071(3) -0.044(3) S2 0.0520(19) 0.0516(19) 0.112(3) -0.0283(19) -0.0149(19) -0.0105(15) S3 0.130(4) 0.118(3) 0.128(3) -0.089(3) 0.049(3) -0.081(3) S4 0.087(2) 0.058(2) 0.063(2) -0.0176(16) -0.0056(18) -0.0356(18) S5 0.077(2) 0.0612(19) 0.0478(18) -0.0194(15) -0.0191(15) -0.0134(16) O1 0.060(5) 0.052(5) 0.075(5) -0.031(4) 0.000(4) -0.030(4) O2 0.080(6) 0.081(6) 0.088(6) 0.000(5) -0.025(5) -0.043(5) N1 0.036(4) 0.035(4) 0.037(4) -0.020(4) -0.007(4) -0.012(4) N2 0.034(4) 0.031(4) 0.024(4) -0.008(3) -0.011(3) 0.001(3) N3 0.022(4) 0.028(4) 0.027(4) -0.012(3) -0.009(3) 0.001(3) N4 0.047(5) 0.035(5) 0.054(5) -0.011(4) -0.024(4) -0.007(4) N5 0.038(5) 0.023(4) 0.044(5) -0.005(4) -0.020(4) 0.005(4) N6 0.035(5) 0.038(5) 0.026(4) -0.017(3) -0.009(3) -0.003(4) N7 0.023(4) 0.029(4) 0.031(4) -0.013(3) -0.004(3) -0.001(3) N8 0.037(5) 0.022(4) 0.024(4) -0.010(3) -0.005(3) -0.008(3) N9 0.034(4) 0.032(4) 0.025(4) -0.011(3) -0.013(3) -0.007(3) N10 0.024(4) 0.055(5) 0.023(4) -0.024(4) -0.001(3) -0.003(4) N11 0.043(5) 0.032(4) 0.029(4) -0.018(3) -0.012(4) -0.002(4) N12 0.033(4) 0.032(4) 0.029(4) -0.015(3) -0.013(4) 0.000(3) N13 0.035(5) 0.039(5) 0.039(5) -0.022(4) -0.021(4) 0.002(4) N14 0.060(7) 0.088(8) 0.086(8) -0.046(6) 0.001(6) -0.035(6) N15 0.063(7) 0.085(8) 0.091(8) -0.051(7) -0.012(6) -0.011(6) N16 0.063(7) 0.087(8) 0.098(9) -0.037(7) -0.024(6) -0.030(6) N17 0.045(5) 0.065(6) 0.037(5) -0.021(5) -0.008(4) 0.005(4) C1 0.052(6) 0.040(6) 0.040(6) -0.017(5) -0.013(5) -0.014(5) C2 0.054(7) 0.046(7) 0.051(7) -0.031(5) -0.014(5) -0.013(5) C3 0.065(7) 0.036(6) 0.057(7) -0.027(5) -0.008(6) -0.015(6) C4 0.041(6) 0.032(6) 0.030(5) -0.012(4) -0.005(4) -0.004(4) C5 0.034(5) 0.025(5) 0.032(5) -0.008(4) -0.017(4) 0.004(4) C6 0.023(5) 0.028(5) 0.034(5) -0.013(4) -0.007(4) -0.003(4) C7 0.046(6) 0.021(5) 0.044(6) -0.008(4) -0.021(5) 0.001(4) C8 0.027(5) 0.036(6) 0.040(6) -0.015(4) -0.017(4) 0.006(4) C9 0.043(6) 0.034(6) 0.045(6) -0.007(5) -0.018(5) -0.002(5) C10 0.030(5) 0.035(5) 0.031(5) -0.011(4) -0.017(4) 0.001(4) C11 0.031(5) 0.042(6) 0.049(6) -0.019(5) -0.022(5) 0.003(5) C12 0.037(6) 0.044(6) 0.041(6) -0.014(5) -0.017(5) -0.008(5) C13 0.040(6) 0.043(6) 0.037(6) -0.009(5) -0.013(5) -0.008(5) C14 0.025(5) 0.043(6) 0.050(6) -0.003(5) -0.010(5) -0.007(5) C15 0.033(5) 0.031(5) 0.037(5) -0.010(4) -0.011(4) -0.008(4) C16 0.026(5) 0.027(5) 0.028(5) -0.013(4) -0.009(4) -0.005(4) C17 0.025(5) 0.034(5) 0.025(5) -0.013(4) -0.004(4) -0.001(4) C18 0.039(6) 0.030(5) 0.043(6) -0.009(4) -0.018(5) -0.008(4) C19 0.046(6) 0.025(5) 0.057(6) -0.013(5) -0.020(5) -0.012(5) C20 0.036(6) 0.032(6) 0.043(6) -0.007(5) -0.015(5) 0.002(4) C21 0.029(5) 0.027(5) 0.035(5) -0.009(4) -0.014(4) 0.003(4) C22 0.036(6) 0.029(5) 0.036(6) -0.005(4) -0.010(5) -0.009(4) C23 0.041(6) 0.036(6) 0.042(6) -0.016(5) -0.002(5) -0.001(5) C24 0.047(6) 0.047(6) 0.033(6) -0.027(5) 0.000(5) -0.009(5) C25 0.035(5) 0.031(5) 0.029(5) -0.019(4) -0.001(4) -0.005(4) C26 0.023(5) 0.033(5) 0.027(5) -0.019(4) -0.001(4) -0.008(4) C27 0.035(5) 0.032(5) 0.024(5) -0.011(4) -0.009(4) -0.015(4) C28 0.034(5) 0.033(5) 0.028(5) -0.013(4) -0.002(4) -0.008(4) C29 0.027(5) 0.032(5) 0.025(5) -0.015(4) -0.008(4) -0.002(4) C30 0.033(5) 0.048(6) 0.024(5) -0.014(4) -0.015(4) 0.002(4) C31 0.046(6) 0.029(5) 0.026(5) -0.010(4) -0.014(5) -0.010(4) C32 0.028(5) 0.047(6) 0.041(6) -0.021(5) -0.021(5) 0.008(4) C33 0.028(5) 0.059(6) 0.029(5) -0.024(5) -0.010(4) -0.002(5) C34 0.031(5) 0.038(5) 0.028(5) -0.018(4) -0.010(4) 0.000(4) C35 0.032(5) 0.032(5) 0.037(6) -0.013(4) -0.013(4) -0.002(4) C36 0.027(5) 0.042(6) 0.026(5) -0.018(4) -0.009(4) -0.003(4) C37 0.028(5) 0.031(5) 0.029(5) -0.013(4) -0.008(4) -0.012(4) C38 0.028(5) 0.024(5) 0.029(5) -0.013(4) -0.009(4) -0.004(4) C39 0.027(5) 0.047(6) 0.041(6) -0.028(5) -0.006(4) -0.007(4) C40 0.047(6) 0.047(6) 0.030(6) -0.019(5) -0.008(5) -0.013(5) C41 0.061(7) 0.043(6) 0.011(5) -0.009(4) -0.007(5) -0.014(5) C42 0.043(6) 0.040(6) 0.031(5) -0.012(4) -0.020(5) -0.010(5) C50 0.057(7) 0.048(7) 0.071(8) -0.027(6) -0.027(6) -0.004(6) C60 0.051(7) 0.046(7) 0.058(7) -0.023(5) -0.012(6) -0.016(6) C61 0.069(9) 0.089(10) 0.081(10) -0.046(8) 0.035(7) -0.058(8) C62 0.064(8) 0.060(8) 0.060(8) -0.025(6) -0.002(6) -0.039(7) C63 0.092(10) 0.064(9) 0.098(10) -0.040(8) -0.017(8) -0.030(8) C64 0.091(11) 0.097(12) 0.127(13) -0.071(10) 0.020(10) -0.010(9) C65 0.115(10) 0.157(12) 0.095(9) 0.003(8) -0.036(8) -0.068(9) C66 0.115(10) 0.157(12) 0.095(9) 0.003(8) -0.036(8) -0.068(9) C90 0.014(5) 0.053(7) 0.059(7) -0.018(6) -0.009(5) 0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N8 1.958(7) . ? Ru1 N2 1.970(7) . ? Ru1 N3 2.043(7) . ? Ru1 N7 2.053(7) . ? Ru1 N9 2.056(7) . ? Ru1 N1 2.059(7) . ? Fe1 N13 2.117(8) 2_566 ? Fe1 N13 2.117(8) . ? Fe1 N12 2.171(7) . ? Fe1 N12 2.171(7) 2_566 ? Fe1 N6 2.245(7) 1_464 ? Fe1 N6 2.245(7) 2_657 ? Fe2 O1 1.968(8) 2_557 ? Fe2 O1 1.984(7) . ? Fe2 N16 2.010(12) . ? Fe2 N14 2.024(10) . ? Fe2 N15 2.026(11) . ? Fe2 O2 2.163(8) . ? S1 C50 1.646(12) . ? S2 C60 1.594(11) . ? S3 C61 1.615(14) . ? S4 C62 1.597(14) . ? S5 C90 1.626(12) . ? O1 C63 1.422(13) . ? O1 Fe2 1.968(8) 2_557 ? O2 C65 1.308(15) . ? O70 C71 1.53(2) . ? O70 H70 0.8400 . ? O76 C75 1.512(18) . ? O76 H76 0.8400 . ? O77 C78 1.441(17) . ? O77 H77 0.8400 . ? O80 C81 1.51(2) . ? O730 O731 0.83(3) . ? N1 C1 1.329(10) . ? N1 C5 1.366(10) . ? N2 C6 1.342(10) . ? N2 C16 1.343(10) . ? N3 C21 1.333(10) . ? N3 C17 1.379(10) . ? N4 N5 1.351(10) . ? N4 C8 1.364(10) . ? N4 H4 0.8800 . ? N5 C9 1.284(11) . ? N6 C13 1.317(11) . ? N6 C12 1.338(10) . ? N6 Fe1 2.245(7) 1_646 ? N7 C22 1.332(10) . ? N7 C26 1.361(10) . ? N8 C27 1.347(10) . ? N8 C37 1.356(10) . ? N9 C42 1.345(10) . ? N9 C38 1.351(10) . ? N10 N11 1.334(9) . ? N10 C29 1.372(10) . ? N10 H10 0.8800 . ? N11 C30 1.254(10) . ? N12 C34 1.332(10) . ? N12 C33 1.340(10) . ? N13 C50 1.134(11) . ? N14 C60 1.133(12) . ? N15 C61 1.132(14) . ? N16 C62 1.166(14) . ? N17 C90 1.156(12) . ? C1 C2 1.345(13) . ? C1 H1 0.9500 . ? C2 C3 1.365(13) . ? C2 H2 0.9500 . ? C3 C4 1.373(12) . ? C3 H3 0.9500 . ? C4 C5 1.348(11) . ? C4 H4A 0.9500 . ? C5 C6 1.474(11) . ? C6 C7 1.380(11) . ? C7 C8 1.393(12) . ? C7 H7 0.9500 . ? C8 C15 1.399(12) . ? C9 C10 1.452(12) . ? C9 H9 0.9500 . ? C10 C14 1.369(11) . ? C10 C11 1.392(12) . ? C11 C12 1.374(12) . ? C11 H11A 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.366(13) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.374(11) . ? C15 H15 0.9500 . ? C16 C17 1.458(11) . ? C17 C18 1.382(11) . ? C18 C19 1.360(12) . ? C18 H18 0.9500 . ? C19 C20 1.392(12) . ? C19 H19 0.9500 . ? C20 C21 1.366(12) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.383(12) . ? C22 H22 0.9500 . ? C23 C24 1.365(12) . ? C23 H23 0.9500 . ? C24 C25 1.366(12) . ? C24 H24 0.9500 . ? C25 C26 1.378(11) . ? C25 H25 0.9500 . ? C26 C27 1.453(11) . ? C27 C28 1.359(11) . ? C28 C29 1.389(11) . ? C28 H28 0.9500 . ? C29 C36 1.390(11) . ? C30 C31 1.448(11) . ? C30 H30 0.9500 . ? C31 C35 1.370(11) . ? C31 C32 1.385(12) . ? C32 C33 1.365(11) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.366(11) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.379(11) . ? C36 H36 0.9500 . ? C37 C38 1.478(11) . ? C38 C39 1.390(11) . ? C39 C40 1.361(12) . ? C39 H39 0.9500 . ? C40 C41 1.358(12) . ? C40 H40 0.9500 . ? C41 C42 1.353(12) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C63 C64 1.522(16) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C66 1.398(17) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C71 C721 1.31(4) . ? C71 C720 1.40(3) . ? C74 C75 1.467(19) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C78 C79 1.385(18) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C81 C82 1.51(2) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C720 H72A 0.9800 . ? C720 H72B 0.9800 . ? C720 H72C 0.9800 . ? C721 H72D 0.9800 . ? C721 H72E 0.9800 . ? C721 H72F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 Ru1 N2 178.2(3) . . ? N8 Ru1 N3 100.7(3) . . ? N2 Ru1 N3 78.9(3) . . ? N8 Ru1 N7 78.6(3) . . ? N2 Ru1 N7 103.2(3) . . ? N3 Ru1 N7 91.2(3) . . ? N8 Ru1 N9 79.3(3) . . ? N2 Ru1 N9 98.9(3) . . ? N3 Ru1 N9 93.9(3) . . ? N7 Ru1 N9 157.9(3) . . ? N8 Ru1 N1 101.4(3) . . ? N2 Ru1 N1 79.0(3) . . ? N3 Ru1 N1 157.9(3) . . ? N7 Ru1 N1 92.9(3) . . ? N9 Ru1 N1 90.5(3) . . ? N13 Fe1 N13 180.00(11) 2_566 . ? N13 Fe1 N12 90.9(3) 2_566 . ? N13 Fe1 N12 89.1(3) . . ? N13 Fe1 N12 89.1(3) 2_566 2_566 ? N13 Fe1 N12 90.9(3) . 2_566 ? N12 Fe1 N12 180.000(1) . 2_566 ? N13 Fe1 N6 89.1(3) 2_566 1_464 ? N13 Fe1 N6 90.9(3) . 1_464 ? N12 Fe1 N6 92.6(2) . 1_464 ? N12 Fe1 N6 87.4(2) 2_566 1_464 ? N13 Fe1 N6 90.9(3) 2_566 2_657 ? N13 Fe1 N6 89.1(3) . 2_657 ? N12 Fe1 N6 87.4(2) . 2_657 ? N12 Fe1 N6 92.6(2) 2_566 2_657 ? N6 Fe1 N6 180.000(1) 1_464 2_657 ? O1 Fe2 O1 75.3(3) 2_557 . ? O1 Fe2 N16 169.2(3) 2_557 . ? O1 Fe2 N16 97.1(4) . . ? O1 Fe2 N14 94.9(4) 2_557 . ? O1 Fe2 N14 92.9(3) . . ? N16 Fe2 N14 93.1(4) . . ? O1 Fe2 N15 94.1(4) 2_557 . ? O1 Fe2 N15 168.1(4) . . ? N16 Fe2 N15 92.7(4) . . ? N14 Fe2 N15 93.3(4) . . ? O1 Fe2 O2 83.4(3) 2_557 . ? O1 Fe2 O2 85.2(3) . . ? N16 Fe2 O2 88.5(4) . . ? N14 Fe2 O2 177.7(4) . . ? N15 Fe2 O2 88.3(4) . . ? C63 O1 Fe2 129.0(7) . 2_557 ? C63 O1 Fe2 125.6(7) . . ? Fe2 O1 Fe2 104.7(3) 2_557 . ? C65 O2 Fe2 132.1(9) . . ? C71 O70 H70 109.5 . . ? C75 O76 H76 109.5 . . ? C78 O77 H77 109.5 . . ? C1 N1 C5 117.4(8) . . ? C1 N1 Ru1 127.9(6) . . ? C5 N1 Ru1 114.7(5) . . ? C6 N2 C16 121.0(7) . . ? C6 N2 Ru1 118.8(6) . . ? C16 N2 Ru1 120.1(6) . . ? C21 N3 C17 118.4(7) . . ? C21 N3 Ru1 128.1(6) . . ? C17 N3 Ru1 113.5(5) . . ? N5 N4 C8 119.4(7) . . ? N5 N4 H4 120.3 . . ? C8 N4 H4 120.3 . . ? C9 N5 N4 116.5(8) . . ? C13 N6 C12 116.0(8) . . ? C13 N6 Fe1 121.6(6) . 1_646 ? C12 N6 Fe1 122.3(6) . 1_646 ? C22 N7 C26 118.5(7) . . ? C22 N7 Ru1 127.3(6) . . ? C26 N7 Ru1 114.1(5) . . ? C27 N8 C37 121.0(7) . . ? C27 N8 Ru1 119.7(6) . . ? C37 N8 Ru1 119.2(5) . . ? C42 N9 C38 117.6(7) . . ? C42 N9 Ru1 128.1(6) . . ? C38 N9 Ru1 114.2(5) . . ? N11 N10 C29 119.2(7) . . ? N11 N10 H10 120.4 . . ? C29 N10 H10 120.4 . . ? C30 N11 N10 118.8(7) . . ? C34 N12 C33 116.6(7) . . ? C34 N12 Fe1 122.4(5) . . ? C33 N12 Fe1 120.5(6) . . ? C50 N13 Fe1 168.2(8) . . ? C60 N14 Fe2 166.5(11) . . ? C61 N15 Fe2 172.4(10) . . ? C62 N16 Fe2 153.8(10) . . ? N1 C1 C2 122.9(9) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C1 C2 C3 120.5(9) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C2 C3 C4 117.1(9) . . ? C2 C3 H3 121.4 . . ? C4 C3 H3 121.4 . . ? C5 C4 C3 120.9(9) . . ? C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C4 C5 N1 121.1(8) . . ? C4 C5 C6 125.1(8) . . ? N1 C5 C6 113.8(7) . . ? N2 C6 C7 121.3(8) . . ? N2 C6 C5 113.6(7) . . ? C7 C6 C5 125.1(8) . . ? C6 C7 C8 117.8(8) . . ? C6 C7 H7 121.1 . . ? C8 C7 H7 121.1 . . ? N4 C8 C7 121.9(8) . . ? N4 C8 C15 117.4(8) . . ? C7 C8 C15 120.7(8) . . ? N5 C9 C10 120.6(9) . . ? N5 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C14 C10 C11 117.4(8) . . ? C14 C10 C9 120.9(9) . . ? C11 C10 C9 121.7(8) . . ? C12 C11 C10 118.4(8) . . ? C12 C11 H11A 120.8 . . ? C10 C11 H11A 120.8 . . ? N6 C12 C11 124.1(9) . . ? N6 C12 H12 118.0 . . ? C11 C12 H12 118.0 . . ? N6 C13 C14 124.4(9) . . ? N6 C13 H13 117.8 . . ? C14 C13 H13 117.8 . . ? C13 C14 C10 119.7(9) . . ? C13 C14 H14 120.2 . . ? C10 C14 H14 120.2 . . ? C16 C15 C8 117.7(8) . . ? C16 C15 H15 121.1 . . ? C8 C15 H15 121.1 . . ? N2 C16 C15 121.4(8) . . ? N2 C16 C17 111.5(7) . . ? C15 C16 C17 127.1(8) . . ? N3 C17 C18 119.6(8) . . ? N3 C17 C16 115.8(7) . . ? C18 C17 C16 124.6(8) . . ? C19 C18 C17 121.4(8) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C18 C19 C20 118.2(8) . . ? C18 C19 H19 120.9 . . ? C20 C19 H19 120.9 . . ? C21 C20 C19 119.0(8) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? N3 C21 C20 123.3(8) . . ? N3 C21 H21 118.4 . . ? C20 C21 H21 118.4 . . ? N7 C22 C23 122.6(8) . . ? N7 C22 H22 118.7 . . ? C23 C22 H22 118.7 . . ? C24 C23 C22 118.8(9) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C23 C24 C25 119.2(9) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C24 C25 C26 120.3(8) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? N7 C26 C25 120.5(7) . . ? N7 C26 C27 115.2(7) . . ? C25 C26 C27 124.3(8) . . ? N8 C27 C28 120.5(8) . . ? N8 C27 C26 112.2(7) . . ? C28 C27 C26 127.3(8) . . ? C27 C28 C29 120.1(8) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? N10 C29 C28 121.9(7) . . ? N10 C29 C36 119.0(7) . . ? C28 C29 C36 119.0(8) . . ? N11 C30 C31 120.6(8) . . ? N11 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C35 C31 C32 118.1(8) . . ? C35 C31 C30 122.2(8) . . ? C32 C31 C30 119.8(8) . . ? C33 C32 C31 119.1(8) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? N12 C33 C32 123.3(8) . . ? N12 C33 H33 118.4 . . ? C32 C33 H33 118.4 . . ? N12 C34 C35 123.9(8) . . ? N12 C34 H34 118.1 . . ? C35 C34 H34 118.1 . . ? C34 C35 C31 119.1(8) . . ? C34 C35 H35 120.5 . . ? C31 C35 H35 120.5 . . ? C37 C36 C29 119.1(8) . . ? C37 C36 H36 120.5 . . ? C29 C36 H36 120.5 . . ? N8 C37 C36 120.3(7) . . ? N8 C37 C38 112.0(7) . . ? C36 C37 C38 127.7(8) . . ? N9 C38 C39 121.5(7) . . ? N9 C38 C37 115.2(7) . . ? C39 C38 C37 123.2(7) . . ? C40 C39 C38 119.1(8) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? C41 C40 C39 119.1(9) . . ? C41 C40 H40 120.4 . . ? C39 C40 H40 120.4 . . ? C42 C41 C40 120.2(8) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? N9 C42 C41 122.4(8) . . ? N9 C42 H42 118.8 . . ? C41 C42 H42 118.8 . . ? N13 C50 S1 179.0(10) . . ? N14 C60 S2 179.3(10) . . ? N15 C61 S3 173.6(15) . . ? N16 C62 S4 178.2(11) . . ? O1 C63 C64 111.4(10) . . ? O1 C63 H63A 109.4 . . ? C64 C63 H63A 109.4 . . ? O1 C63 H63B 109.4 . . ? C64 C63 H63B 109.4 . . ? H63A C63 H63B 108.0 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? O2 C65 C66 124.8(15) . . ? O2 C65 H65A 106.1 . . ? C66 C65 H65A 106.1 . . ? O2 C65 H65B 106.1 . . ? C66 C65 H65B 106.1 . . ? H65A C65 H65B 106.3 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C721 C71 C720 69(2) . . ? C721 C71 O70 115(3) . . ? C720 C71 O70 113(2) . . ? C75 C74 H74A 109.5 . . ? C75 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C75 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C74 C75 O76 118(3) . . ? C74 C75 H75A 107.7 . . ? O76 C75 H75A 107.7 . . ? C74 C75 H75B 107.7 . . ? O76 C75 H75B 107.7 . . ? H75A C75 H75B 107.1 . . ? C79 C78 O77 125(2) . . ? C79 C78 H78A 106.0 . . ? O77 C78 H78A 106.0 . . ? C79 C78 H78B 106.0 . . ? O77 C78 H78B 106.0 . . ? H78A C78 H78B 106.3 . . ? C78 C79 H79A 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C78 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? O80 C81 C82 125(3) . . ? O80 C81 H81A 106.2 . . ? C82 C81 H81A 106.2 . . ? O80 C81 H81B 106.2 . . ? C82 C81 H81B 106.2 . . ? H81A C81 H81B 106.4 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N17 C90 S5 178.2(9) . . ? C71 C720 H72A 109.5 . . ? C71 C720 H72B 109.5 . . ? H72A C720 H72B 109.5 . . ? C71 C720 H72C 109.5 . . ? H72A C720 H72C 109.5 . . ? H72B C720 H72C 109.5 . . ? C71 C721 H72D 109.5 . . ? C71 C721 H72E 109.5 . . ? H72D C721 H72E 109.5 . . ? C71 C721 H72F 109.5 . . ? H72D C721 H72F 109.5 . . ? H72E C721 H72F 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4 O730 0.88 1.92 2.80(2) 177.4 . N4 H4 O731 0.88 2.08 2.894(16) 154.0 . N10 H10 N17 0.88 2.01 2.893(11) 177.0 . O77 H77 O76 0.84 2.27 2.92(3) 134.3 . O76 H76 O731 0.84 2.52 3.28(4) 150.0 1_554 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.999 _refine_diff_density_min -0.905 _refine_diff_density_rms 0.140 # Attachment 'Ru[H2_1_]2_MN.cif' data_jb984 _database_code_depnum_ccdc_archive 'CCDC 692942' _audit_creation_date 07-11-14 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '11131708 jb984_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 11.0743(1) _cell_length_b 14.7284(1) _cell_length_c 15.5483(2) _cell_angle_alpha 77.6715(5) _cell_angle_beta 88.2000(5) _cell_angle_gamma 68.6393(5) _cell_volume 2304.36(4) _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 57.7998 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' 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' _cell_formula_units_Z 2 # Given Formula = C88 H88 N30 O30 Ru2 # Dc = 3.24 Fooo = 1136.00 Mu = 8.60 M = 2247.99 # Found Formula = C42 H40 N16 O15 Ru1 # Dc = 1.60 FOOO = 1136.00 Mu = 4.30 M = 1109.95 _chemical_formula_sum 'C42 H40 N16 O15 Ru1' _chemical_formula_moiety 'C42 H34 N12 Ru, 4(N O3), 3(H2 O)' _chemical_compound_source ? _chemical_formula_weight 1109.95 _cell_measurement_reflns_used 10973 _cell_measurement_theta_min 1 _cell_measurement_theta_max 28 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_min 0.09 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_max 0.36 _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.430 # Sheldrick geometric approximatio 0.89 0.96 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.96 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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 21783 _reflns_number_total 10975 _diffrn_reflns_av_R_equivalents 0.023 # Number of reflections with Friedels Law is 10975 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 10972 _diffrn_reflns_theta_min 1.342 _diffrn_reflns_theta_max 27.857 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.857 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _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 -14 _reflns_limit_h_max 14 _reflns_limit_k_min -18 _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 -0.64 _refine_diff_density_max 0.66 _refine_ls_number_reflns 9207 _refine_ls_number_restraints 0 _refine_ls_number_parameters 667 #_refine_ls_R_factor_ref 0.0309 _refine_ls_wR_factor_ref 0.0356 _refine_ls_goodness_of_fit_ref 1.0958 #_reflns_number_all 10901 _refine_ls_R_factor_all 0.0375 _refine_ls_wR_factor_all 0.0420 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 9207 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_gt 0.0356 _refine_ls_shift/su_max 0.001980 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.428 0.218 0.170 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: 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 atomsattached 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 0.494871(13) 0.250876(10) 0.243638(8) 0.0196 1.0000 Uani . . . . . . N1 N 0.42372(13) 0.19760(10) 0.36046(9) 0.0209 1.0000 Uani . . . . . . N2 N 0.54143(13) 0.32317(10) 0.32306(9) 0.0204 1.0000 Uani . . . . . . N3 N 0.58275(14) 0.33432(11) 0.15794(9) 0.0232 1.0000 Uani . . . . . . N4 N 0.65837(14) 0.12285(11) 0.27025(9) 0.0213 1.0000 Uani . . . . . . N5 N 0.45172(13) 0.17003(10) 0.17180(9) 0.0193 1.0000 Uani . . . . . . N6 N 0.31468(14) 0.34730(11) 0.18938(9) 0.0222 1.0000 Uani . . . . . . N7 N 0.67209(15) 0.44589(12) 0.49739(10) 0.0268 1.0000 Uani . . . . . . N8 N 0.74075(15) 0.50407(11) 0.46927(10) 0.0254 1.0000 Uani . . . . . . N9 N 1.01450(17) 0.70746(12) 0.44977(11) 0.0323 1.0000 Uani . . . . . . N10 N 0.34946(14) -0.01465(11) 0.04817(10) 0.0245 1.0000 Uani . . . . . . N11 N 0.23762(14) 0.01953(12) -0.00110(9) 0.0242 1.0000 Uani . . . . . . N12 N -0.13289(16) 0.04554(14) -0.18985(11) 0.0348 1.0000 Uani . . . . . . N13 N 0.81913(16) 0.14802(12) 0.54477(11) 0.0302 1.0000 Uani . . . . . . N14 N 0.9805(2) 0.27910(17) 0.24723(13) 0.0457 1.0000 Uani . . . . . . N15 N 0.3437(2) 0.63932(14) 0.27169(13) 0.0484 1.0000 Uani . . . . . . N16 N 0.8211(2) 0.71116(13) 0.12766(13) 0.0411 1.0000 Uani . . . . . . C1 C 0.36115(18) 0.13297(14) 0.37440(12) 0.0270 1.0000 Uani . . . . . . C2 C 0.3272(2) 0.09680(15) 0.45780(14) 0.0327 1.0000 Uani . . . . . . C3 C 0.3581(2) 0.12809(15) 0.52867(13) 0.0323 1.0000 Uani . . . . . . C4 C 0.42024(18) 0.19597(14) 0.51525(12) 0.0269 1.0000 Uani . . . . . . C5 C 0.45213(16) 0.22988(12) 0.43057(11) 0.0212 1.0000 Uani . . . . . . C6 C 0.51983(16) 0.30118(12) 0.40950(11) 0.0203 1.0000 Uani . . . . . . C7 C 0.56194(16) 0.34253(13) 0.46883(11) 0.0227 1.0000 Uani . . . . . . C8 C 0.62954(16) 0.40550(13) 0.43725(11) 0.0231 1.0000 Uani . . . . . . C9 C 0.65397(17) 0.42575(13) 0.34764(12) 0.0246 1.0000 Uani . . . . . . C10 C 0.60715(16) 0.38368(12) 0.29168(11) 0.0221 1.0000 Uani . . . . . . C11 C 0.62344(17) 0.39471(13) 0.19578(11) 0.0238 1.0000 Uani . . . . . . C12 C 0.6754(2) 0.46080(15) 0.14625(13) 0.0317 1.0000 Uani . . . . . . C13 C 0.6897(2) 0.46397(17) 0.05714(13) 0.0380 1.0000 Uani . . . . . . C14 C 0.6518(2) 0.40105(17) 0.01915(13) 0.0373 1.0000 Uani . . . . . . C15 C 0.59788(19) 0.33804(15) 0.07120(12) 0.0303 1.0000 Uani . . . . . . C16 C 0.76223(17) 0.10472(14) 0.32309(12) 0.0274 1.0000 Uani . . . . . . C17 C 0.86354(18) 0.01302(15) 0.34136(12) 0.0306 1.0000 Uani . . . . . . C18 C 0.85831(18) -0.06201(14) 0.30361(12) 0.0291 1.0000 Uani . . . . . . C19 C 0.75177(17) -0.04493(13) 0.24897(11) 0.0252 1.0000 Uani . . . . . . C20 C 0.65246(16) 0.04794(12) 0.23303(10) 0.0205 1.0000 Uani . . . . . . C21 C 0.53366(16) 0.07480(12) 0.17685(10) 0.0201 1.0000 Uani . . . . . . C22 C 0.50149(17) 0.01234(13) 0.13471(11) 0.0223 1.0000 Uani . . . . . . C23 C 0.38132(17) 0.04966(13) 0.08765(10) 0.0216 1.0000 Uani . . . . . . C24 C 0.29633(16) 0.14806(13) 0.08373(11) 0.0223 1.0000 Uani . . . . . . C25 C 0.33466(16) 0.20663(12) 0.12777(10) 0.0204 1.0000 Uani . . . . . . C26 C 0.25670(16) 0.30993(13) 0.13630(11) 0.0219 1.0000 Uani . . . . . . C27 C 0.13424(18) 0.36547(14) 0.09639(12) 0.0274 1.0000 Uani . . . . . . C28 C 0.06895(19) 0.46086(15) 0.11103(13) 0.0336 1.0000 Uani . . . . . . C29 C 0.1294(2) 0.49913(15) 0.16282(13) 0.0343 1.0000 Uani . . . . . . C30 C 0.25160(19) 0.44075(13) 0.20061(12) 0.0278 1.0000 Uani . . . . . . C31 C 0.77943(17) 0.53985(13) 0.52713(12) 0.0260 1.0000 Uani . . . . . . C32 C 0.85829(17) 0.59980(13) 0.49911(12) 0.0258 1.0000 Uani . . . . . . C33 C 0.90597(19) 0.63685(15) 0.56044(13) 0.0303 1.0000 Uani . . . . . . C34 C 0.9839(2) 0.69100(15) 0.53362(13) 0.0328 1.0000 Uani . . . . . . C35 C 0.9704(2) 0.67320(15) 0.38849(13) 0.0332 1.0000 Uani . . . . . . C36 C 0.89128(19) 0.62016(14) 0.41148(13) 0.0302 1.0000 Uani . . . . . . C37 C 0.20972(17) -0.04466(14) -0.03302(12) 0.0256 1.0000 Uani . . . . . . C38 C 0.09004(18) -0.01201(14) -0.08716(11) 0.0266 1.0000 Uani . . . . . . C39 C 0.00753(19) 0.08843(15) -0.10925(13) 0.0308 1.0000 Uani . . . . . . C40 C -0.1037(2) 0.11504(17) -0.16061(13) 0.0359 1.0000 Uani . . . . . . C41 C -0.05626(19) -0.05080(17) -0.17071(13) 0.0331 1.0000 Uani . . . . . . C42 C 0.05654(19) -0.08210(15) -0.11894(12) 0.0291 1.0000 Uani . . . . . . O1 O 0.82800(15) 0.18669(12) 0.60817(9) 0.0375 1.0000 Uani . . . . . . O2 O 0.74437(16) 0.10144(12) 0.54821(10) 0.0417 1.0000 Uani . . . . . . O3 O 0.88316(19) 0.15795(16) 0.48001(11) 0.0538 1.0000 Uani . . . . . . O4 O 0.9355(2) 0.36069(16) 0.27147(12) 0.0591 1.0000 Uani . . . . . . O5 O 1.0860(2) 0.21563(17) 0.27834(14) 0.0668 1.0000 Uani . . . . . . O6 O 0.9245(3) 0.26572(19) 0.1867(2) 0.0964 1.0000 Uani . . . . . . O7 O 0.35020(19) 0.67245(15) 0.19226(11) 0.0526 1.0000 Uani . . . . . . O8 O 0.4322(2) 0.62600(18) 0.32571(13) 0.0786 1.0000 Uani . . . . . . O9 O 0.2452(3) 0.62119(19) 0.29743(16) 0.0872 1.0000 Uani . . . . . . O10 O 0.7930(4) 0.7469(2) 0.19310(18) 0.1053 1.0000 Uani . . . . . . O11 O 0.91870(17) 0.71491(13) 0.08704(13) 0.0508 1.0000 Uani . . . . . . O12 O 0.75380(18) 0.67023(14) 0.10044(13) 0.0510 1.0000 Uani . . . . . . O13 O 0.48410(15) 0.77570(11) 0.07589(10) 0.0364 1.0000 Uani . . . . . . O14 O 0.34814(15) 0.92351(14) 0.28469(10) 0.0447 1.0000 Uani . . . . . . O15 O 0.5704(2) 0.7555(2) 0.28783(14) 0.0788 1.0000 Uani . . . . . . H1 H 0.6566 0.4323 0.5527 0.0372 1.0000 Uiso R . . . . . H2 H 1.0649 0.7399 0.4340 0.0410 1.0000 Uiso R . . . . . H3 H 0.4002 -0.0769 0.0564 0.0319 1.0000 Uiso R . . . . . H4 H -0.2047 0.0643 -0.2221 0.0427 1.0000 Uiso R . . . . . H5 H 0.4531 0.7443 0.1139 0.0545 1.0000 Uiso R . . . . . H6 H 0.5619 0.7500 0.0860 0.0546 1.0000 Uiso R . . . . . H7 H 0.4089 0.8731 0.2795 0.0674 1.0000 Uiso R . . . . . H8 H 0.3265 0.9129 0.3364 0.0669 1.0000 Uiso R . . . . . H9 H 0.6318 0.7496 0.2569 0.1087 1.0000 Uiso R . . . . . H10 H 0.5519 0.7065 0.2890 0.1089 1.0000 Uiso R . . . . . H11 H 0.3433 0.1117 0.3256 0.0348 1.0000 Uiso R . . . . . H21 H 0.2848 0.0521 0.4647 0.0411 1.0000 Uiso R . . . . . H31 H 0.3363 0.1051 0.5847 0.0401 1.0000 Uiso R . . . . . H41 H 0.4398 0.2187 0.5621 0.0329 1.0000 Uiso R . . . . . H71 H 0.5450 0.3298 0.5285 0.0285 1.0000 Uiso R . . . . . H91 H 0.7000 0.4666 0.3262 0.0303 1.0000 Uiso R . . . . . H121 H 0.7016 0.5027 0.1736 0.0387 1.0000 Uiso R . . . . . H131 H 0.7253 0.5086 0.0234 0.0458 1.0000 Uiso R . . . . . H141 H 0.6614 0.4002 -0.0411 0.0447 1.0000 Uiso R . . . . . H151 H 0.5696 0.2961 0.0470 0.0355 1.0000 Uiso R . . . . . H161 H 0.7623 0.1580 0.3487 0.0329 1.0000 Uiso R . . . . . H171 H 0.9322 0.0030 0.3797 0.0335 1.0000 Uiso R . . . . . H181 H 0.9259 -0.1246 0.3147 0.0331 1.0000 Uiso R . . . . . H191 H 0.7469 -0.0949 0.2236 0.0294 1.0000 Uiso R . . . . . H221 H 0.5580 -0.0529 0.1380 0.0279 1.0000 Uiso R . . . . . H241 H 0.2159 0.1733 0.0516 0.0283 1.0000 Uiso R . . . . . H271 H 0.0963 0.3388 0.0610 0.0326 1.0000 Uiso R . . . . . H281 H -0.0150 0.4989 0.0863 0.0375 1.0000 Uiso R . . . . . H291 H 0.0894 0.5647 0.1718 0.0392 1.0000 Uiso R . . . . . H301 H 0.2946 0.4655 0.2370 0.0312 1.0000 Uiso R . . . . . H311 H 0.7600 0.5255 0.5869 0.0329 1.0000 Uiso R . . . . . H331 H 0.8846 0.6261 0.6195 0.0386 1.0000 Uiso R . . . . . H341 H 1.0154 0.7162 0.5740 0.0411 1.0000 Uiso R . . . . . H351 H 0.9976 0.6855 0.3308 0.0404 1.0000 Uiso R . . . . . H361 H 0.8607 0.5967 0.3692 0.0371 1.0000 Uiso R . . . . . H371 H 0.2642 -0.1129 -0.0220 0.0325 1.0000 Uiso R . . . . . H391 H 0.0278 0.1374 -0.0898 0.0374 1.0000 Uiso R . . . . . H401 H -0.1601 0.1819 -0.1758 0.0425 1.0000 Uiso R . . . . . H411 H -0.0779 -0.0972 -0.1934 0.0420 1.0000 Uiso R . . . . . H421 H 0.1115 -0.1515 -0.1057 0.0378 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 0.02140(7) 0.01937(7) 0.02103(7) -0.00605(5) -0.00125(4) -0.00973(5) N1 0.0209(6) 0.0206(7) 0.0236(7) -0.0053(5) -0.0008(5) -0.0101(5) N2 0.0208(6) 0.0205(7) 0.0225(6) -0.0056(5) -0.0001(5) -0.0101(5) N3 0.0242(7) 0.0240(7) 0.0227(7) -0.0045(5) -0.0010(5) -0.0103(6) N4 0.0210(6) 0.0223(7) 0.0210(6) -0.0047(5) -0.0018(5) -0.0082(5) N5 0.0206(6) 0.0192(6) 0.0201(6) -0.0048(5) -0.0007(5) -0.0091(5) N6 0.0247(7) 0.0203(7) 0.0228(6) -0.0053(5) -0.0011(5) -0.0092(6) N7 0.0333(8) 0.0315(8) 0.0264(7) -0.0101(6) 0.0022(6) -0.0223(7) N8 0.0246(7) 0.0249(7) 0.0320(7) -0.0089(6) -0.0008(6) -0.0135(6) N9 0.0346(8) 0.0287(8) 0.0386(9) -0.0004(7) -0.0075(7) -0.0205(7) N10 0.0247(7) 0.0252(7) 0.0277(7) -0.0103(6) -0.0014(6) -0.0112(6) N11 0.0248(7) 0.0301(8) 0.0223(7) -0.0085(6) 0.0011(5) -0.0137(6) N12 0.0276(8) 0.0517(11) 0.0270(8) -0.0053(7) -0.0023(6) -0.0182(8) N13 0.0309(8) 0.0298(8) 0.0340(8) -0.0043(6) -0.0045(6) -0.0170(7) N14 0.0412(10) 0.0562(12) 0.0411(10) -0.0106(9) -0.0023(8) -0.0189(9) N15 0.0782(15) 0.0289(9) 0.0364(10) -0.0105(7) 0.0169(10) -0.0171(10) N16 0.0461(11) 0.0279(9) 0.0466(10) -0.0081(7) -0.0046(8) -0.0099(8) C1 0.0308(9) 0.0270(9) 0.0310(9) -0.0096(7) 0.0010(7) -0.0176(7) C2 0.0373(10) 0.0301(9) 0.0393(10) -0.0063(8) 0.0036(8) -0.0230(8) C3 0.0369(10) 0.0367(10) 0.0286(9) -0.0036(7) 0.0055(7) -0.0217(9) C4 0.0299(9) 0.0303(9) 0.0255(8) -0.0072(7) 0.0008(7) -0.0162(7) C5 0.0205(7) 0.0210(8) 0.0247(8) -0.0068(6) -0.0007(6) -0.0093(6) C6 0.0199(7) 0.0210(8) 0.0224(7) -0.0066(6) 0.0007(6) -0.0092(6) C7 0.0236(8) 0.0247(8) 0.0229(7) -0.0066(6) 0.0005(6) -0.0117(7) C8 0.0213(8) 0.0248(8) 0.0276(8) -0.0108(6) -0.0015(6) -0.0103(7) C9 0.0254(8) 0.0241(8) 0.0292(8) -0.0072(7) 0.0013(6) -0.0141(7) C10 0.0228(8) 0.0211(8) 0.0246(8) -0.0040(6) 0.0002(6) -0.0110(6) C11 0.0245(8) 0.0240(8) 0.0250(8) -0.0049(6) -0.0018(6) -0.0111(7) C12 0.0368(10) 0.0352(10) 0.0284(9) -0.0027(7) -0.0001(7) -0.0216(8) C13 0.0437(11) 0.0450(12) 0.0291(9) 0.0010(8) 0.0023(8) -0.0256(10) C14 0.0454(12) 0.0464(12) 0.0221(8) -0.0035(8) 0.0032(8) -0.0215(10) C15 0.0355(10) 0.0331(10) 0.0239(8) -0.0069(7) 0.0000(7) -0.0138(8) C16 0.0240(8) 0.0319(9) 0.0272(8) -0.0069(7) -0.0045(7) -0.0104(7) C17 0.0244(8) 0.0376(10) 0.0271(8) -0.0031(7) -0.0058(7) -0.0099(8) C18 0.0250(8) 0.0295(9) 0.0273(8) -0.0007(7) -0.0003(7) -0.0065(7) C19 0.0268(8) 0.0238(8) 0.0248(8) -0.0043(6) 0.0026(6) -0.0098(7) C20 0.0219(7) 0.0226(8) 0.0186(7) -0.0038(6) 0.0011(6) -0.0104(6) C21 0.0228(7) 0.0224(8) 0.0177(7) -0.0048(6) 0.0022(6) -0.0111(6) C22 0.0248(8) 0.0210(8) 0.0237(8) -0.0071(6) 0.0029(6) -0.0103(6) C23 0.0256(8) 0.0264(8) 0.0188(7) -0.0080(6) 0.0033(6) -0.0148(7) C24 0.0232(8) 0.0252(8) 0.0215(7) -0.0060(6) -0.0003(6) -0.0116(7) C25 0.0216(7) 0.0223(8) 0.0191(7) -0.0045(6) -0.0003(6) -0.0101(6) C26 0.0239(8) 0.0234(8) 0.0198(7) -0.0047(6) -0.0006(6) -0.0103(7) C27 0.0263(8) 0.0291(9) 0.0250(8) -0.0047(7) -0.0045(7) -0.0082(7) C28 0.0286(9) 0.0323(10) 0.0316(9) -0.0078(8) -0.0060(7) -0.0006(8) C29 0.0372(10) 0.0238(9) 0.0356(10) -0.0092(7) -0.0034(8) -0.0021(8) C30 0.0323(9) 0.0226(8) 0.0288(8) -0.0088(7) -0.0021(7) -0.0082(7) C31 0.0275(8) 0.0262(9) 0.0296(8) -0.0097(7) -0.0003(7) -0.0138(7) C32 0.0248(8) 0.0220(8) 0.0328(9) -0.0068(7) -0.0034(7) -0.0103(7) C33 0.0354(10) 0.0316(9) 0.0304(9) -0.0070(7) -0.0039(7) -0.0191(8) C34 0.0386(10) 0.0311(10) 0.0350(10) -0.0043(8) -0.0089(8) -0.0207(8) C35 0.0402(11) 0.0316(10) 0.0317(9) -0.0039(7) -0.0019(8) -0.0191(8) C36 0.0349(10) 0.0283(9) 0.0324(9) -0.0065(7) -0.0045(7) -0.0170(8) C37 0.0263(8) 0.0295(9) 0.0262(8) -0.0097(7) 0.0018(7) -0.0141(7) C38 0.0270(8) 0.0356(10) 0.0227(8) -0.0082(7) 0.0030(6) -0.0170(8) C39 0.0310(9) 0.0352(10) 0.0302(9) -0.0091(7) 0.0031(7) -0.0159(8) C40 0.0322(10) 0.0415(11) 0.0308(9) -0.0045(8) 0.0016(8) -0.0117(9) C41 0.0315(10) 0.0484(12) 0.0281(9) -0.0095(8) 0.0012(7) -0.0242(9) C42 0.0299(9) 0.0364(10) 0.0271(8) -0.0088(7) 0.0005(7) -0.0180(8) O1 0.0480(9) 0.0466(9) 0.0333(7) -0.0136(6) 0.0022(6) -0.0326(7) O2 0.0521(9) 0.0477(9) 0.0440(8) -0.0125(7) 0.0029(7) -0.0388(8) O3 0.0691(12) 0.0807(13) 0.0442(9) -0.0281(9) 0.0186(8) -0.0583(11) O4 0.0630(12) 0.0691(13) 0.0464(10) -0.0246(9) -0.0014(8) -0.0183(10) O5 0.0497(11) 0.0728(14) 0.0637(12) -0.0095(10) -0.0179(9) -0.0072(10) O6 0.0825(16) 0.0678(15) 0.134(2) -0.0484(15) -0.0602(16) -0.0017(12) O7 0.0615(11) 0.0637(11) 0.0323(8) -0.0023(7) 0.0074(7) -0.0273(9) O8 0.0798(15) 0.0742(15) 0.0411(10) -0.0093(10) -0.0101(10) 0.0184(12) O9 0.151(2) 0.0894(17) 0.0737(14) -0.0471(13) 0.0649(16) -0.0932(18) O10 0.185(3) 0.098(2) 0.0787(17) -0.0623(16) 0.0505(19) -0.084(2) O11 0.0417(9) 0.0414(9) 0.0656(11) -0.0086(8) -0.0091(8) -0.0117(7) O12 0.0482(10) 0.0505(10) 0.0616(11) -0.0215(8) 0.0021(8) -0.0212(8) O13 0.0371(8) 0.0337(7) 0.0373(7) -0.0058(6) -0.0023(6) -0.0124(6) O14 0.0364(8) 0.0631(11) 0.0336(8) 0.0031(7) -0.0045(6) -0.0241(8) O15 0.0699(14) 0.1030(18) 0.0516(11) -0.0400(12) -0.0061(10) -0.0042(13) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3472(3) 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 . 2.0707(14) yes Ru1 . N2 . 1.9815(13) yes Ru1 . N3 . 2.0792(15) yes Ru1 . N4 . 2.0572(14) yes Ru1 . N5 . 1.9773(13) yes Ru1 . N6 . 2.0592(14) yes N1 . C1 . 1.348(2) yes N1 . C5 . 1.366(2) yes N2 . C6 . 1.349(2) yes N2 . C10 . 1.351(2) yes N3 . C11 . 1.368(2) yes N3 . C15 . 1.346(2) yes N4 . C16 . 1.346(2) yes N4 . C20 . 1.373(2) yes N5 . C21 . 1.352(2) yes N5 . C25 . 1.352(2) yes N6 . C26 . 1.371(2) yes N6 . C30 . 1.344(2) yes N7 . N8 . 1.341(2) yes N7 . C8 . 1.385(2) yes N7 . H1 . 0.866 no N8 . C31 . 1.289(2) yes N9 . C34 . 1.331(3) yes N9 . C35 . 1.348(2) yes N9 . H2 . 0.857 no N10 . N11 . 1.347(2) yes N10 . C23 . 1.380(2) yes N10 . H3 . 0.868 no N11 . C37 . 1.288(2) yes N12 . C40 . 1.344(3) yes N12 . C41 . 1.334(3) yes N12 . H4 . 0.875 no N13 . O1 . 1.262(2) yes N13 . O2 . 1.247(2) yes N13 . O3 . 1.227(2) yes N14 . O4 . 1.257(3) yes N14 . O5 . 1.232(3) yes N14 . O6 . 1.231(3) yes N15 . O7 . 1.237(2) yes N15 . O8 . 1.243(3) yes N15 . O9 . 1.250(3) yes N16 . O10 . 1.224(3) yes N16 . O11 . 1.247(3) yes N16 . O12 . 1.247(3) yes C1 . C2 . 1.388(3) yes C1 . H11 . 0.932 no C2 . C3 . 1.378(3) yes C2 . H21 . 0.926 no C3 . C4 . 1.385(3) yes C3 . H31 . 0.924 no C4 . C5 . 1.388(2) yes C4 . H41 . 0.926 no C5 . C6 . 1.478(2) yes C6 . C7 . 1.383(2) yes C7 . C8 . 1.396(2) yes C7 . H71 . 0.934 no C8 . C9 . 1.400(2) yes C9 . C10 . 1.379(2) yes C9 . H91 . 0.928 no C10 . C11 . 1.478(2) yes C11 . C12 . 1.390(3) yes C12 . C13 . 1.382(3) yes C12 . H121 . 0.946 no C13 . C14 . 1.385(3) yes C13 . H131 . 0.944 no C14 . C15 . 1.387(3) yes C14 . H141 . 0.942 no C15 . H151 . 0.932 no C16 . C17 . 1.384(3) yes C16 . H161 . 0.953 no C17 . C18 . 1.376(3) yes C17 . H171 . 0.930 no C18 . C19 . 1.390(2) yes C18 . H181 . 0.937 no C19 . C20 . 1.385(2) yes C19 . H191 . 0.925 no C20 . C21 . 1.482(2) yes C21 . C22 . 1.383(2) yes C22 . C23 . 1.402(2) yes C22 . H221 . 0.927 no C23 . C24 . 1.401(2) yes C24 . C25 . 1.389(2) yes C24 . H241 . 0.943 no C25 . C26 . 1.483(2) yes C26 . C27 . 1.386(2) yes C27 . C28 . 1.391(3) yes C27 . H271 . 0.928 no C28 . C29 . 1.384(3) yes C28 . H281 . 0.937 no C29 . C30 . 1.380(3) yes C29 . H291 . 0.944 no C30 . H301 . 0.955 no C31 . C32 . 1.451(2) yes C31 . H311 . 0.944 no C32 . C33 . 1.396(2) yes C32 . C36 . 1.398(3) yes C33 . C34 . 1.375(3) yes C33 . H331 . 0.936 no C34 . H341 . 0.929 no C35 . C36 . 1.365(3) yes C35 . H351 . 0.939 no C36 . H361 . 0.928 no C37 . C38 . 1.459(2) yes C37 . H371 . 0.946 no C38 . C39 . 1.400(3) yes C38 . C42 . 1.398(2) yes C39 . C40 . 1.373(3) yes C39 . H391 . 0.936 no C40 . H401 . 0.937 no C41 . C42 . 1.381(3) yes C41 . H411 . 0.937 no C42 . H421 . 0.960 no O13 . H5 . 0.818 no O13 . H6 . 0.810 no O14 . H7 . 0.818 no O14 . H8 . 0.830 no O15 . H9 . 0.809 no O15 . H10 . 0.816 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Ru1 . N2 . 79.42(6) yes N1 . Ru1 . N3 . 158.07(5) yes N2 . Ru1 . N3 . 78.65(6) yes N1 . Ru1 . N4 . 88.38(6) yes N2 . Ru1 . N4 . 97.63(6) yes N3 . Ru1 . N4 . 95.13(6) yes N1 . Ru1 . N5 . 97.21(5) yes N2 . Ru1 . N5 . 175.74(6) yes N3 . Ru1 . N5 . 104.72(6) yes N4 . Ru1 . N5 . 79.58(6) yes N1 . Ru1 . N6 . 94.20(6) yes N2 . Ru1 . N6 . 103.81(6) yes N3 . Ru1 . N6 . 90.40(6) yes N4 . Ru1 . N6 . 158.51(6) yes N5 . Ru1 . N6 . 78.93(6) yes Ru1 . N1 . C1 . 127.73(12) yes Ru1 . N1 . C5 . 113.45(11) yes C1 . N1 . C5 . 118.72(15) yes Ru1 . N2 . C6 . 118.39(11) yes Ru1 . N2 . C10 . 119.43(11) yes C6 . N2 . C10 . 121.72(14) yes Ru1 . N3 . C11 . 114.18(11) yes Ru1 . N3 . C15 . 127.52(12) yes C11 . N3 . C15 . 118.23(16) yes Ru1 . N4 . C16 . 127.02(12) yes Ru1 . N4 . C20 . 113.85(11) yes C16 . N4 . C20 . 118.99(15) yes Ru1 . N5 . C21 . 118.64(11) yes Ru1 . N5 . C25 . 119.39(11) yes C21 . N5 . C25 . 121.47(14) yes Ru1 . N6 . C26 . 114.73(11) yes Ru1 . N6 . C30 . 126.64(12) yes C26 . N6 . C30 . 118.63(15) yes N8 . N7 . C8 . 119.07(15) yes N8 . N7 . H1 . 120.4 no C8 . N7 . H1 . 120.5 no N7 . N8 . C31 . 117.37(16) yes C34 . N9 . C35 . 121.98(17) yes C34 . N9 . H2 . 119.5 no C35 . N9 . H2 . 118.6 no N11 . N10 . C23 . 119.46(15) yes N11 . N10 . H3 . 120.6 no C23 . N10 . H3 . 120.0 no N10 . N11 . C37 . 116.90(16) yes C40 . N12 . C41 . 122.02(17) yes C40 . N12 . H4 . 118.8 no C41 . N12 . H4 . 119.2 no O1 . N13 . O2 . 119.68(17) yes O1 . N13 . O3 . 119.40(16) yes O2 . N13 . O3 . 120.92(17) yes O4 . N14 . O5 . 120.5(2) yes O4 . N14 . O6 . 119.8(2) yes O5 . N14 . O6 . 119.4(2) yes O7 . N15 . O8 . 121.0(2) yes O7 . N15 . O9 . 118.9(3) yes O8 . N15 . O9 . 120.1(2) yes O10 . N16 . O11 . 120.2(2) yes O10 . N16 . O12 . 121.1(2) yes O11 . N16 . O12 . 118.7(2) yes N1 . C1 . C2 . 122.12(16) yes N1 . C1 . H11 . 117.2 no C2 . C1 . H11 . 120.7 no C1 . C2 . C3 . 119.02(17) yes C1 . C2 . H21 . 119.5 no C3 . C2 . H21 . 121.5 no C2 . C3 . C4 . 119.60(18) yes C2 . C3 . H31 . 120.5 no C4 . C3 . H31 . 119.9 no C3 . C4 . C5 . 119.15(16) yes C3 . C4 . H41 . 120.4 no C5 . C4 . H41 . 120.4 no C4 . C5 . N1 . 121.37(15) yes C4 . C5 . C6 . 123.34(15) yes N1 . C5 . C6 . 115.28(14) yes C5 . C6 . N2 . 113.09(14) yes C5 . C6 . C7 . 126.40(15) yes N2 . C6 . C7 . 120.49(15) yes C6 . C7 . C8 . 118.38(16) yes C6 . C7 . H71 . 121.4 no C8 . C7 . H71 . 120.2 no C7 . C8 . N7 . 117.86(16) yes C7 . C8 . C9 . 120.48(15) yes N7 . C8 . C9 . 121.65(16) yes C8 . C9 . C10 . 118.24(15) yes C8 . C9 . H91 . 121.1 no C10 . C9 . H91 . 120.7 no C9 . C10 . N2 . 120.66(16) yes C9 . C10 . C11 . 126.71(15) yes N2 . C10 . C11 . 112.61(14) yes C10 . C11 . N3 . 114.76(15) yes C10 . C11 . C12 . 123.72(16) yes N3 . C11 . C12 . 121.52(16) yes C11 . C12 . C13 . 119.44(18) yes C11 . C12 . H121 . 120.1 no C13 . C12 . H121 . 120.4 no C12 . C13 . C14 . 119.14(19) yes C12 . C13 . H131 . 119.6 no C14 . C13 . H131 . 121.3 no C13 . C14 . C15 . 119.07(18) yes C13 . C14 . H141 . 121.6 no C15 . C14 . H141 . 119.3 no C14 . C15 . N3 . 122.56(18) yes C14 . C15 . H151 . 120.8 no N3 . C15 . H151 . 116.7 no N4 . C16 . C17 . 122.31(17) yes N4 . C16 . H161 . 116.7 no C17 . C16 . H161 . 121.0 no C16 . C17 . C18 . 118.82(17) yes C16 . C17 . H171 . 119.6 no C18 . C17 . H171 . 121.6 no C17 . C18 . C19 . 119.80(17) yes C17 . C18 . H181 . 120.4 no C19 . C18 . H181 . 119.8 no C18 . C19 . C20 . 119.25(17) yes C18 . C19 . H191 . 120.6 no C20 . C19 . H191 . 120.2 no C19 . C20 . N4 . 120.83(15) yes C19 . C20 . C21 . 124.24(15) yes N4 . C20 . C21 . 114.92(14) yes C20 . C21 . N5 . 112.74(14) yes C20 . C21 . C22 . 126.52(15) yes N5 . C21 . C22 . 120.71(15) yes C21 . C22 . C23 . 118.49(15) yes C21 . C22 . H221 . 120.6 no C23 . C22 . H221 . 120.9 no C22 . C23 . N10 . 117.60(15) yes C22 . C23 . C24 . 120.40(15) yes N10 . C23 . C24 . 121.97(15) yes C23 . C24 . C25 . 118.10(15) yes C23 . C24 . H241 . 120.4 no C25 . C24 . H241 . 121.5 no C24 . C25 . N5 . 120.81(15) yes C24 . C25 . C26 . 126.68(15) yes N5 . C25 . C26 . 112.46(14) yes C25 . C26 . N6 . 114.37(14) yes C25 . C26 . C27 . 124.24(15) yes N6 . C26 . C27 . 121.37(16) yes C26 . C27 . C28 . 119.08(17) yes C26 . C27 . H271 . 120.2 no C28 . C27 . H271 . 120.8 no C27 . C28 . C29 . 119.25(17) yes C27 . C28 . H281 . 120.5 no C29 . C28 . H281 . 120.2 no C28 . C29 . C30 . 119.21(18) yes C28 . C29 . H291 . 121.4 no C30 . C29 . H291 . 119.4 no C29 . C30 . N6 . 122.40(17) yes C29 . C30 . H301 . 120.5 no N6 . C30 . H301 . 117.1 no N8 . C31 . C32 . 118.49(17) yes N8 . C31 . H311 . 121.1 no C32 . C31 . H311 . 120.4 no C31 . C32 . C33 . 120.19(17) yes C31 . C32 . C36 . 121.61(16) yes C33 . C32 . C36 . 118.19(17) yes C32 . C33 . C34 . 119.68(18) yes C32 . C33 . H331 . 120.8 no C34 . C33 . H331 . 119.5 no C33 . C34 . N9 . 120.22(17) yes C33 . C34 . H341 . 120.1 no N9 . C34 . H341 . 119.7 no N9 . C35 . C36 . 120.10(19) yes N9 . C35 . H351 . 117.9 no C36 . C35 . H351 . 121.9 no C32 . C36 . C35 . 119.82(17) yes C32 . C36 . H361 . 120.1 no C35 . C36 . H361 . 120.1 no N11 . C37 . C38 . 119.41(17) yes N11 . C37 . H371 . 122.0 no C38 . C37 . H371 . 118.6 no C37 . C38 . C39 . 121.74(17) yes C37 . C38 . C42 . 119.66(17) yes C39 . C38 . C42 . 118.60(17) yes C38 . C39 . C40 . 119.30(19) yes C38 . C39 . H391 . 120.8 no C40 . C39 . H391 . 119.9 no C39 . C40 . N12 . 120.4(2) yes C39 . C40 . H401 . 120.3 no N12 . C40 . H401 . 119.2 no N12 . C41 . C42 . 120.16(18) yes N12 . C41 . H411 . 120.1 no C42 . C41 . H411 . 119.8 no C38 . C42 . C41 . 119.48(19) yes C38 . C42 . H421 . 120.8 no C41 . C42 . H421 . 119.8 no H5 . O13 . H6 . 105.3 no H7 . O14 . H8 . 106.3 no H9 . O15 . H10 . 105.8 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag N9 . H2 . O1 2_766 176 0.86 1.89 2.751(2) yes N10 . H3 . O13 1_545 169 0.87 1.98 2.839(2) yes N12 . H4 . O14 2_565 168 0.88 1.82 2.685(2) yes O13 . H5 . O7 . 170 0.82 2.03 2.843(2) yes O13 . H6 . O12 . 171 0.81 2.01 2.814(2) yes O14 . H7 . O15 . 168 0.82 1.97 2.775(2) yes O14 . H8 . O2 2_666 173 0.83 1.94 2.763(2) yes O15 . H9 . O10 . 171 0.81 2.01 2.808(2) yes O15 . H10 . O8 . 151 0.82 2.07 2.815(2) yes # Attachment 'Ru_1_2_NO3_JZ.CIF' data_jb1220 _database_code_depnum_ccdc_archive 'CCDC 692943' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H32 N12 Ru, 2(N O3), 4.25(H2 O)' _chemical_formula_sum 'C42 H40.5 N14 O10.25 Ru' _chemical_formula_weight 1005.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.840(2) _cell_length_b 14.336(3) _cell_length_c 15.614(3) _cell_angle_alpha 105.45(3) _cell_angle_beta 92.24(3) _cell_angle_gamma 107.05(3) _cell_volume 2217.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 0.429 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32184 _diffrn_reflns_av_R_equivalents 0.0965 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.05 _reflns_number_total 7769 _reflns_number_gt 7180 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+6.1660P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7769 _refine_ls_number_parameters 629 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1502 _refine_ls_wR_factor_gt 0.1469 _refine_ls_goodness_of_fit_ref 1.186 _refine_ls_restrained_S_all 1.193 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.49965(3) 0.25230(2) 0.24603(2) 0.02581(13) Uani 1 1 d . . . N1 N 0.4313(3) 0.3108(3) 0.3641(2) 0.0301(8) Uani 1 1 d . . . N2 N 0.5441(3) 0.1730(3) 0.3211(2) 0.0287(7) Uani 1 1 d . . . N3 N 0.5844(3) 0.1609(3) 0.1577(2) 0.0285(7) Uani 1 1 d . . . N4 N 0.6711(4) 0.0334(3) 0.4904(3) 0.0386(9) Uani 1 1 d . . . H4B H 0.6476 0.0419 0.5445 0.046 Uiso 1 1 calc R . . N5 N 0.7501(4) -0.0245(3) 0.4626(3) 0.0383(9) Uani 1 1 d . . . N6 N 1.0635(5) -0.2245(4) 0.4615(4) 0.0634(15) Uani 1 1 d . . . N7 N 0.3135(3) 0.1652(3) 0.1865(2) 0.0305(8) Uani 1 1 d . . . N8 N 0.4596(3) 0.3374(3) 0.1752(2) 0.0270(7) Uani 1 1 d . . . N9 N 0.6678(3) 0.3751(3) 0.2811(2) 0.0283(7) Uani 1 1 d . . . N10 N 0.3643(4) 0.5305(3) 0.0499(3) 0.0370(8) Uani 1 1 d . . . H10A H 0.4190 0.5921 0.0580 0.044 Uiso 1 1 calc R . . N11 N 0.2479(4) 0.4993(3) -0.0018(3) 0.0380(9) Uani 1 1 d . . . N12 N -0.1384(4) 0.4846(4) -0.2007(3) 0.0524(12) Uani 1 1 d . . . C1 C 0.3723(4) 0.3834(3) 0.3805(3) 0.0368(10) Uani 1 1 d . . . H1A H 0.3596 0.4130 0.3345 0.044 Uiso 1 1 calc R . . C2 C 0.3295(5) 0.4163(4) 0.4624(3) 0.0440(12) Uani 1 1 d . . . H2A H 0.2878 0.4673 0.4723 0.053 Uiso 1 1 calc R . . C3 C 0.3485(5) 0.3740(4) 0.5288(3) 0.0440(12) Uani 1 1 d . . . H3A H 0.3195 0.3954 0.5852 0.053 Uiso 1 1 calc R . . C4 C 0.4098(4) 0.3000(4) 0.5137(3) 0.0368(10) Uani 1 1 d . . . H4A H 0.4232 0.2700 0.5592 0.044 Uiso 1 1 calc R . . C5 C 0.4515(4) 0.2704(3) 0.4306(3) 0.0301(9) Uani 1 1 d . . . C6 C 0.5202(4) 0.1928(3) 0.4080(3) 0.0290(9) Uani 1 1 d . . . C7 C 0.5606(4) 0.1465(3) 0.4649(3) 0.0329(9) Uani 1 1 d . . . H7A H 0.5425 0.1609 0.5252 0.040 Uiso 1 1 calc R . . C8 C 0.6293(4) 0.0776(3) 0.4331(3) 0.0335(9) Uani 1 1 d . . . C9 C 0.6528(4) 0.0571(3) 0.3427(3) 0.0331(9) Uani 1 1 d . . . H9A H 0.6979 0.0101 0.3193 0.040 Uiso 1 1 calc R . . C10 C 0.6096(4) 0.1058(3) 0.2889(3) 0.0296(9) Uani 1 1 d . . . C11 C 0.6276(4) 0.0974(3) 0.1935(3) 0.0309(9) Uani 1 1 d . . . C12 C 0.6828(4) 0.0289(4) 0.1423(3) 0.0374(10) Uani 1 1 d . . . H12A H 0.7116 -0.0156 0.1676 0.045 Uiso 1 1 calc R . . C13 C 0.6955(5) 0.0261(4) 0.0532(3) 0.0435(12) Uani 1 1 d . . . H13A H 0.7333 -0.0203 0.0174 0.052 Uiso 1 1 calc R . . C14 C 0.6528(5) 0.0912(4) 0.0172(3) 0.0418(11) Uani 1 1 d . . . H14A H 0.6618 0.0908 -0.0431 0.050 Uiso 1 1 calc R . . C15 C 0.5971(4) 0.1567(3) 0.0709(3) 0.0340(9) Uani 1 1 d . . . H15A H 0.5663 0.2006 0.0459 0.041 Uiso 1 1 calc R . . C16 C 0.7963(4) -0.0563(4) 0.5216(3) 0.0400(10) Uani 1 1 d . . . H16A H 0.7726 -0.0414 0.5805 0.048 Uiso 1 1 calc R . . C17 C 0.8856(5) -0.1156(4) 0.4989(4) 0.0424(11) Uani 1 1 d . . . C18 C 0.9261(5) -0.1382(4) 0.4141(4) 0.0496(13) Uani 1 1 d . . . H18A H 0.8936 -0.1174 0.3674 0.060 Uiso 1 1 calc R . . C19 C 1.0144(6) -0.1914(4) 0.3998(5) 0.0615(16) Uani 1 1 d . . . H19A H 1.0424 -0.2054 0.3422 0.074 Uiso 1 1 calc R . . C20 C 1.0237(6) -0.2028(4) 0.5424(5) 0.0622(17) Uani 1 1 d . . . H20A H 1.0566 -0.2260 0.5873 0.075 Uiso 1 1 calc R . . C21 C 0.9368(5) -0.1480(4) 0.5644(4) 0.0526(13) Uani 1 1 d . . . H21A H 0.9129 -0.1330 0.6232 0.063 Uiso 1 1 calc R . . C22 C 0.2441(5) 0.0753(3) 0.1976(3) 0.0395(11) Uani 1 1 d . . . H22A H 0.2847 0.0447 0.2324 0.047 Uiso 1 1 calc R . . C23 C 0.1163(5) 0.0261(4) 0.1601(4) 0.0485(13) Uani 1 1 d . . . H23A H 0.0691 -0.0368 0.1695 0.058 Uiso 1 1 calc R . . C24 C 0.0585(5) 0.0703(4) 0.1089(4) 0.0489(13) Uani 1 1 d . . . H24A H -0.0299 0.0383 0.0834 0.059 Uiso 1 1 calc R . . C25 C 0.1288(4) 0.1615(4) 0.0941(3) 0.0399(11) Uani 1 1 d . . . H25A H 0.0901 0.1915 0.0576 0.048 Uiso 1 1 calc R . . C26 C 0.2574(4) 0.2079(3) 0.1340(3) 0.0308(9) Uani 1 1 d . . . C27 C 0.3406(4) 0.3071(3) 0.1270(3) 0.0282(8) Uani 1 1 d . . . C28 C 0.3068(4) 0.3677(3) 0.0815(3) 0.0312(9) Uani 1 1 d . . . H28A H 0.2250 0.3445 0.0454 0.037 Uiso 1 1 calc R . . C29 C 0.3947(4) 0.4641(3) 0.0889(3) 0.0314(9) Uani 1 1 d . . . C30 C 0.5182(4) 0.4942(3) 0.1394(3) 0.0314(9) Uani 1 1 d . . . H30A H 0.5803 0.5583 0.1438 0.038 Uiso 1 1 calc R . . C31 C 0.5469(4) 0.4297(3) 0.1817(3) 0.0292(9) Uani 1 1 d . . . C32 C 0.6672(4) 0.4491(3) 0.2411(3) 0.0270(8) Uani 1 1 d . . . C33 C 0.7744(4) 0.5373(3) 0.2580(3) 0.0326(9) Uani 1 1 d . . . H33A H 0.7741 0.5886 0.2301 0.039 Uiso 1 1 calc R . . C34 C 0.8807(4) 0.5486(4) 0.3162(3) 0.0375(10) Uani 1 1 d . . . H34A H 0.9549 0.6075 0.3275 0.045 Uiso 1 1 calc R . . C35 C 0.8800(4) 0.4752(4) 0.3578(3) 0.0388(10) Uani 1 1 d . . . H35A H 0.9522 0.4834 0.3987 0.047 Uiso 1 1 calc R . . C36 C 0.7717(4) 0.3891(4) 0.3389(3) 0.0355(10) Uani 1 1 d . . . H36A H 0.7708 0.3383 0.3676 0.043 Uiso 1 1 calc R . . C37 C 0.2165(5) 0.5665(4) -0.0302(3) 0.0392(10) Uani 1 1 d . . . H37A H 0.2733 0.6347 -0.0144 0.047 Uiso 1 1 calc R . . C38 C 0.0928(5) 0.5375(4) -0.0869(3) 0.0398(11) Uani 1 1 d . . . C39 C 0.0089(5) 0.4370(4) -0.1151(3) 0.0437(11) Uani 1 1 d . . . H39A H 0.0298 0.3852 -0.0961 0.052 Uiso 1 1 calc R . . C40 C -0.1040(5) 0.4143(5) -0.1707(4) 0.0503(13) Uani 1 1 d . . . H40A H -0.1607 0.3460 -0.1889 0.060 Uiso 1 1 calc R . . C41 C -0.0562(5) 0.5802(5) -0.1739(3) 0.0503(13) Uani 1 1 d . . . H41A H -0.0780 0.6302 -0.1954 0.060 Uiso 1 1 calc R . . C42 C 0.0581(5) 0.6104(4) -0.1171(3) 0.0435(11) Uani 1 1 d . . . H42A H 0.1120 0.6795 -0.0991 0.052 Uiso 1 1 calc R . . N100 N 0.8340(5) 0.7871(4) 0.1367(4) 0.0674(15) Uani 1 1 d . . . O11 O 0.7924(8) 0.7351(5) 0.1818(5) 0.122(2) Uani 1 1 d U . . O12 O 0.9399(5) 0.7823(4) 0.0997(5) 0.0937(18) Uani 1 1 d . . . O13 O 0.7807(5) 0.8377(4) 0.1096(4) 0.0761(13) Uani 1 1 d . . . N200 N 0.3636(5) -0.1243(3) 0.2718(3) 0.0550(12) Uani 1 1 d . . . O21 O 0.4149(7) -0.1646(5) 0.3144(4) 0.108(2) Uani 1 1 d . . . O22 O 0.3032(7) -0.0704(5) 0.3100(4) 0.102(2) Uani 1 1 d . . . O23 O 0.3796(5) -0.1330(4) 0.1917(3) 0.0744(13) Uani 1 1 d . . . H30C H 0.527(8) 0.766(6) 0.289(6) 0.089 Uiso 1 1 d . . . O30 O 0.5822(6) 0.7263(4) 0.2863(3) 0.0809(15) Uani 1 1 d . . . H30D H 0.6413 0.7052 0.3021 0.097 Uiso 1 1 calc R . . O40 O 0.3585(4) 0.5766(3) 0.3235(3) 0.0561(10) Uani 1 1 d . . . H40C H 0.294(7) 0.575(5) 0.285(5) 0.067 Uiso 1 1 d . . . H40D H 0.425(7) 0.626(5) 0.306(4) 0.067 Uiso 1 1 d . . . H50B H 1.178(7) -0.335(5) 0.447(5) 0.067 Uiso 1 1 d . . . O50 O 1.1961(4) -0.3769(3) 0.4591(3) 0.0559(10) Uani 1 1 d . . . H50A H 1.258(6) -0.371(5) 0.410(5) 0.067 Uiso 1 1 d . . . O60 O 0.5006(4) 0.7414(3) 0.0787(3) 0.0482(9) Uani 1 1 d . . . H60A H 0.473(6) 0.780(5) 0.119(4) 0.058 Uiso 1 1 d . . . H60B H 0.573(7) 0.762(5) 0.089(5) 0.058 Uiso 1 1 d . . . O70 O 1.105(2) 0.7898(18) 0.0712(16) 0.093(6) Uiso 0.25 1 d P . . 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 0.02582(19) 0.02632(19) 0.02390(19) 0.00387(13) 0.00510(12) 0.00902(13) N1 0.0280(18) 0.0296(18) 0.0305(18) 0.0039(14) 0.0060(14) 0.0097(14) N2 0.0245(17) 0.0306(18) 0.0294(18) 0.0039(14) 0.0084(14) 0.0099(14) N3 0.0246(17) 0.0316(18) 0.0256(17) 0.0038(14) 0.0023(13) 0.0075(14) N4 0.038(2) 0.047(2) 0.040(2) 0.0199(18) 0.0106(17) 0.0193(18) N5 0.034(2) 0.033(2) 0.046(2) 0.0111(17) 0.0031(17) 0.0098(16) N6 0.050(3) 0.037(2) 0.092(4) -0.004(3) -0.005(3) 0.019(2) N7 0.0289(18) 0.0309(18) 0.0277(18) 0.0020(14) 0.0070(14) 0.0091(15) N8 0.0240(17) 0.0311(18) 0.0242(17) 0.0030(14) 0.0072(13) 0.0101(14) N9 0.0289(18) 0.0325(18) 0.0224(16) 0.0048(14) 0.0050(13) 0.0106(15) N10 0.037(2) 0.043(2) 0.035(2) 0.0132(17) 0.0026(16) 0.0177(17) N11 0.041(2) 0.051(2) 0.0295(19) 0.0128(17) 0.0094(16) 0.0237(19) N12 0.045(2) 0.084(4) 0.036(2) 0.012(2) 0.0083(19) 0.035(3) C1 0.036(2) 0.032(2) 0.039(2) 0.0032(19) 0.0057(19) 0.0135(19) C2 0.047(3) 0.041(3) 0.042(3) 0.000(2) 0.011(2) 0.021(2) C3 0.048(3) 0.050(3) 0.031(2) 0.000(2) 0.011(2) 0.021(2) C4 0.036(2) 0.042(3) 0.028(2) 0.0036(19) 0.0068(18) 0.012(2) C5 0.026(2) 0.031(2) 0.029(2) 0.0011(17) 0.0045(16) 0.0087(17) C6 0.025(2) 0.032(2) 0.028(2) 0.0049(17) 0.0045(16) 0.0080(17) C7 0.031(2) 0.037(2) 0.030(2) 0.0086(18) 0.0066(17) 0.0089(18) C8 0.030(2) 0.031(2) 0.038(2) 0.0107(18) 0.0049(18) 0.0071(18) C9 0.029(2) 0.036(2) 0.035(2) 0.0074(18) 0.0050(17) 0.0141(18) C10 0.027(2) 0.030(2) 0.030(2) 0.0037(17) 0.0056(16) 0.0111(17) C11 0.026(2) 0.034(2) 0.029(2) 0.0039(17) 0.0026(16) 0.0097(17) C12 0.035(2) 0.041(2) 0.036(2) 0.0021(19) 0.0042(19) 0.019(2) C13 0.039(3) 0.051(3) 0.035(2) -0.004(2) 0.008(2) 0.021(2) C14 0.039(2) 0.054(3) 0.027(2) 0.002(2) 0.0056(19) 0.015(2) C15 0.035(2) 0.037(2) 0.026(2) 0.0043(18) 0.0039(17) 0.0108(19) C16 0.034(2) 0.043(3) 0.046(3) 0.017(2) 0.005(2) 0.013(2) C17 0.035(2) 0.032(2) 0.057(3) 0.009(2) -0.005(2) 0.010(2) C18 0.048(3) 0.035(3) 0.059(3) 0.003(2) 0.003(2) 0.014(2) C19 0.056(3) 0.040(3) 0.077(4) -0.003(3) 0.007(3) 0.016(3) C20 0.047(3) 0.047(3) 0.089(5) 0.012(3) -0.019(3) 0.020(3) C21 0.046(3) 0.047(3) 0.065(4) 0.015(3) -0.004(3) 0.017(2) C22 0.041(3) 0.030(2) 0.041(3) 0.0055(19) 0.009(2) 0.0051(19) C23 0.043(3) 0.043(3) 0.046(3) 0.008(2) 0.008(2) -0.002(2) C24 0.030(2) 0.053(3) 0.044(3) -0.002(2) 0.005(2) -0.001(2) C25 0.031(2) 0.046(3) 0.037(2) 0.002(2) 0.0038(19) 0.011(2) C26 0.029(2) 0.031(2) 0.026(2) -0.0020(16) 0.0033(16) 0.0085(17) C27 0.028(2) 0.031(2) 0.024(2) 0.0016(16) 0.0043(16) 0.0129(17) C28 0.028(2) 0.041(2) 0.025(2) 0.0038(17) 0.0023(16) 0.0168(18) C29 0.036(2) 0.036(2) 0.024(2) 0.0042(17) 0.0057(17) 0.0192(19) C30 0.033(2) 0.034(2) 0.026(2) 0.0049(17) 0.0063(17) 0.0121(18) C31 0.031(2) 0.031(2) 0.026(2) 0.0041(16) 0.0066(16) 0.0138(17) C32 0.027(2) 0.031(2) 0.0205(19) 0.0022(16) 0.0053(15) 0.0103(17) C33 0.034(2) 0.033(2) 0.028(2) 0.0043(17) 0.0082(17) 0.0100(18) C34 0.029(2) 0.040(2) 0.032(2) -0.0027(19) 0.0045(18) 0.0057(19) C35 0.031(2) 0.051(3) 0.029(2) 0.002(2) -0.0019(18) 0.015(2) C36 0.035(2) 0.043(3) 0.027(2) 0.0064(18) 0.0013(18) 0.013(2) C37 0.042(3) 0.049(3) 0.032(2) 0.011(2) 0.0076(19) 0.023(2) C38 0.043(3) 0.058(3) 0.029(2) 0.011(2) 0.0108(19) 0.031(2) C39 0.043(3) 0.059(3) 0.036(3) 0.016(2) 0.011(2) 0.025(2) C40 0.041(3) 0.069(4) 0.042(3) 0.011(3) 0.011(2) 0.023(3) C41 0.054(3) 0.072(4) 0.040(3) 0.014(3) 0.008(2) 0.044(3) C42 0.047(3) 0.058(3) 0.033(2) 0.009(2) 0.003(2) 0.032(2) N100 0.055(3) 0.041(3) 0.104(5) 0.027(3) -0.001(3) 0.009(2) O11 0.199(6) 0.101(4) 0.100(4) 0.058(4) 0.061(4) 0.068(4) O12 0.059(3) 0.070(3) 0.152(6) 0.034(3) 0.004(3) 0.020(2) O13 0.091(3) 0.063(3) 0.091(4) 0.031(3) 0.018(3) 0.040(3) N200 0.074(3) 0.041(2) 0.056(3) 0.017(2) 0.022(3) 0.022(2) O21 0.143(6) 0.140(5) 0.082(4) 0.066(4) 0.030(4) 0.072(5) O22 0.160(6) 0.106(4) 0.093(4) 0.050(3) 0.078(4) 0.094(4) O23 0.108(4) 0.097(3) 0.038(2) 0.018(2) 0.023(2) 0.061(3) O30 0.110(4) 0.073(3) 0.060(3) 0.026(2) -0.007(3) 0.026(3) O40 0.055(2) 0.064(3) 0.050(2) 0.0160(19) -0.0042(18) 0.021(2) O50 0.061(2) 0.059(3) 0.053(2) 0.0184(19) 0.0047(19) 0.025(2) O60 0.053(2) 0.048(2) 0.043(2) 0.0072(16) 0.0014(18) 0.0197(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N2 1.972(4) . ? Ru1 N8 1.973(4) . ? Ru1 N9 2.061(4) . ? Ru1 N7 2.062(4) . ? Ru1 N1 2.074(3) . ? Ru1 N3 2.075(3) . ? N1 C1 1.349(6) . ? N1 C5 1.355(6) . ? N2 C6 1.360(5) . ? N2 C10 1.363(5) . ? N3 C15 1.356(6) . ? N3 C11 1.364(6) . ? N4 C8 1.359(6) . ? N4 N5 1.366(5) . ? N4 H4B 0.8800 . ? N5 C16 1.278(6) . ? N6 C19 1.337(9) . ? N6 C20 1.339(9) . ? N7 C22 1.348(6) . ? N7 C26 1.366(6) . ? N8 C27 1.357(5) . ? N8 C31 1.357(6) . ? N9 C36 1.347(6) . ? N9 C32 1.369(6) . ? N10 N11 1.357(5) . ? N10 C29 1.365(6) . ? N10 H10A 0.8800 . ? N11 C37 1.284(6) . ? N12 C41 1.341(8) . ? N12 C40 1.353(8) . ? C1 C2 1.388(7) . ? C1 H1A 0.9500 . ? C2 C3 1.369(8) . ? C2 H2A 0.9500 . ? C3 C4 1.384(7) . ? C3 H3A 0.9500 . ? C4 C5 1.391(6) . ? C4 H4A 0.9500 . ? C5 C6 1.487(6) . ? C6 C7 1.370(6) . ? C7 C8 1.405(6) . ? C7 H7A 0.9500 . ? C8 C9 1.413(6) . ? C9 C10 1.373(6) . ? C9 H9A 0.9500 . ? C10 C11 1.487(6) . ? C11 C12 1.387(6) . ? C12 C13 1.394(7) . ? C12 H12A 0.9500 . ? C13 C14 1.383(8) . ? C13 H13A 0.9500 . ? C14 C15 1.379(6) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.460(7) . ? C16 H16A 0.9500 . ? C17 C21 1.389(8) . ? C17 C18 1.396(8) . ? C18 C19 1.379(8) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C21 1.392(8) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.380(7) . ? C22 H22A 0.9500 . ? C23 C24 1.378(8) . ? C23 H23A 0.9500 . ? C24 C25 1.390(7) . ? C24 H24A 0.9500 . ? C25 C26 1.393(6) . ? C25 H25A 0.9500 . ? C26 C27 1.478(6) . ? C27 C28 1.374(6) . ? C28 C29 1.402(6) . ? C28 H28A 0.9500 . ? C29 C30 1.413(6) . ? C30 C31 1.366(6) . ? C30 H30A 0.9500 . ? C31 C32 1.481(6) . ? C32 C33 1.398(6) . ? C33 C34 1.382(6) . ? C33 H33A 0.9500 . ? C34 C35 1.373(7) . ? C34 H34A 0.9500 . ? C35 C36 1.384(7) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C38 1.463(7) . ? C37 H37A 0.9500 . ? C38 C42 1.391(7) . ? C38 C39 1.400(8) . ? C39 C40 1.376(7) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 C42 1.380(7) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? N100 O11 1.167(8) . ? N100 O13 1.195(7) . ? N100 O12 1.317(8) . ? N200 O21 1.203(7) . ? N200 O22 1.210(6) . ? N200 O23 1.248(6) . ? O30 H30C 0.93(8) . ? O30 H30D 0.8400 . ? O40 H40C 0.90(7) . ? O40 H40D 0.96(7) . ? O50 H50B 0.75(7) . ? O50 H50A 1.04(7) . ? O60 H60A 0.85(7) . ? O60 H60B 0.75(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ru1 N8 177.38(14) . . ? N2 Ru1 N9 98.49(14) . . ? N8 Ru1 N9 79.36(14) . . ? N2 Ru1 N7 103.06(15) . . ? N8 Ru1 N7 79.03(14) . . ? N9 Ru1 N7 158.32(15) . . ? N2 Ru1 N1 78.96(14) . . ? N8 Ru1 N1 99.49(14) . . ? N9 Ru1 N1 90.43(14) . . ? N7 Ru1 N1 91.37(14) . . ? N2 Ru1 N3 78.97(14) . . ? N8 Ru1 N3 102.58(14) . . ? N9 Ru1 N3 93.29(13) . . ? N7 Ru1 N3 93.11(13) . . ? N1 Ru1 N3 157.93(15) . . ? C1 N1 C5 118.7(4) . . ? C1 N1 Ru1 127.1(3) . . ? C5 N1 Ru1 114.2(3) . . ? C6 N2 C10 120.1(4) . . ? C6 N2 Ru1 119.6(3) . . ? C10 N2 Ru1 120.0(3) . . ? C15 N3 C11 118.8(4) . . ? C15 N3 Ru1 127.3(3) . . ? C11 N3 Ru1 113.8(3) . . ? C8 N4 N5 118.9(4) . . ? C8 N4 H4B 120.5 . . ? N5 N4 H4B 120.5 . . ? C16 N5 N4 116.3(4) . . ? C19 N6 C20 116.6(5) . . ? C22 N7 C26 119.2(4) . . ? C22 N7 Ru1 126.5(3) . . ? C26 N7 Ru1 114.2(3) . . ? C27 N8 C31 120.7(4) . . ? C27 N8 Ru1 119.5(3) . . ? C31 N8 Ru1 119.6(3) . . ? C36 N9 C32 119.2(4) . . ? C36 N9 Ru1 127.1(3) . . ? C32 N9 Ru1 113.7(3) . . ? N11 N10 C29 118.5(4) . . ? N11 N10 H10A 120.8 . . ? C29 N10 H10A 120.8 . . ? C37 N11 N10 117.0(4) . . ? C41 N12 C40 116.9(5) . . ? N1 C1 C2 122.0(5) . . ? N1 C1 H1A 119.0 . . ? C2 C1 H1A 119.0 . . ? C3 C2 C1 118.9(5) . . ? C3 C2 H2A 120.5 . . ? C1 C2 H2A 120.5 . . ? C2 C3 C4 120.0(4) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C3 C4 C5 118.7(5) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? N1 C5 C4 121.6(4) . . ? N1 C5 C6 115.4(4) . . ? C4 C5 C6 123.0(4) . . ? N2 C6 C7 121.5(4) . . ? N2 C6 C5 111.7(4) . . ? C7 C6 C5 126.8(4) . . ? C6 C7 C8 119.3(4) . . ? C6 C7 H7A 120.4 . . ? C8 C7 H7A 120.4 . . ? N4 C8 C7 118.9(4) . . ? N4 C8 C9 122.3(4) . . ? C7 C8 C9 118.8(4) . . ? C10 C9 C8 119.2(4) . . ? C10 C9 H9A 120.4 . . ? C8 C9 H9A 120.4 . . ? N2 C10 C9 121.1(4) . . ? N2 C10 C11 111.2(4) . . ? C9 C10 C11 127.7(4) . . ? N3 C11 C12 121.0(4) . . ? N3 C11 C10 115.8(4) . . ? C12 C11 C10 123.2(4) . . ? C11 C12 C13 119.3(5) . . ? C11 C12 H12A 120.4 . . ? C13 C12 H12A 120.4 . . ? C14 C13 C12 119.7(4) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C15 C14 C13 118.6(4) . . ? C15 C14 H14A 120.7 . . ? C13 C14 H14A 120.7 . . ? N3 C15 C14 122.6(4) . . ? N3 C15 H15A 118.7 . . ? C14 C15 H15A 118.7 . . ? N5 C16 C17 120.2(5) . . ? N5 C16 H16A 119.9 . . ? C17 C16 H16A 119.9 . . ? C21 C17 C18 118.0(5) . . ? C21 C17 C16 119.4(5) . . ? C18 C17 C16 122.6(5) . . ? C19 C18 C17 118.5(6) . . ? C19 C18 H18A 120.8 . . ? C17 C18 H18A 120.8 . . ? N6 C19 C18 124.5(6) . . ? N6 C19 H19A 117.7 . . ? C18 C19 H19A 117.7 . . ? N6 C20 C21 123.5(6) . . ? N6 C20 H20A 118.2 . . ? C21 C20 H20A 118.2 . . ? C17 C21 C20 118.9(6) . . ? C17 C21 H21A 120.5 . . ? C20 C21 H21A 120.5 . . ? N7 C22 C23 122.4(5) . . ? N7 C22 H22A 118.8 . . ? C23 C22 H22A 118.8 . . ? C24 C23 C22 118.5(5) . . ? C24 C23 H23A 120.7 . . ? C22 C23 H23A 120.7 . . ? C23 C24 C25 120.4(5) . . ? C23 C24 H24A 119.8 . . ? C25 C24 H24A 119.8 . . ? C24 C25 C26 118.5(5) . . ? C24 C25 H25A 120.8 . . ? C26 C25 H25A 120.8 . . ? N7 C26 C25 121.0(4) . . ? N7 C26 C27 115.2(4) . . ? C25 C26 C27 123.8(4) . . ? N8 C27 C28 120.9(4) . . ? N8 C27 C26 112.0(4) . . ? C28 C27 C26 127.0(4) . . ? C27 C28 C29 119.1(4) . . ? C27 C28 H28A 120.5 . . ? C29 C28 H28A 120.5 . . ? N10 C29 C28 122.1(4) . . ? N10 C29 C30 118.9(4) . . ? C28 C29 C30 119.0(4) . . ? C31 C30 C29 119.0(4) . . ? C31 C30 H30A 120.5 . . ? C29 C30 H30A 120.5 . . ? N8 C31 C30 121.2(4) . . ? N8 C31 C32 111.6(4) . . ? C30 C31 C32 127.2(4) . . ? N9 C32 C33 120.6(4) . . ? N9 C32 C31 115.8(4) . . ? C33 C32 C31 123.6(4) . . ? C34 C33 C32 118.8(4) . . ? C34 C33 H33A 120.6 . . ? C32 C33 H33A 120.6 . . ? C35 C34 C33 120.5(4) . . ? C35 C34 H34A 119.7 . . ? C33 C34 H34A 119.7 . . ? C34 C35 C36 118.6(4) . . ? C34 C35 H35A 120.7 . . ? C36 C35 H35A 120.7 . . ? N9 C36 C35 122.2(4) . . ? N9 C36 H36A 118.9 . . ? C35 C36 H36A 118.9 . . ? N11 C37 C38 119.7(5) . . ? N11 C37 H37A 120.2 . . ? C38 C37 H37A 120.2 . . ? C42 C38 C39 118.1(5) . . ? C42 C38 C37 119.8(5) . . ? C39 C38 C37 122.0(4) . . ? C40 C39 C38 119.1(5) . . ? C40 C39 H39A 120.5 . . ? C38 C39 H39A 120.5 . . ? N12 C40 C39 123.2(6) . . ? N12 C40 H40A 118.4 . . ? C39 C40 H40A 118.4 . . ? N12 C41 C42 123.9(5) . . ? N12 C41 H41A 118.0 . . ? C42 C41 H41A 118.0 . . ? C41 C42 C38 118.7(5) . . ? C41 C42 H42A 120.7 . . ? C38 C42 H42A 120.7 . . ? O11 N100 O13 126.0(7) . . ? O11 N100 O12 120.3(6) . . ? O13 N100 O12 112.9(6) . . ? O21 N200 O22 118.4(6) . . ? O21 N200 O23 120.4(5) . . ? O22 N200 O23 121.1(5) . . ? H30C O30 H30D 159.4 . . ? H40C O40 H40D 95(6) . . ? H50B O50 H50A 85(6) . . ? H60A O60 H60B 105(7) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.228 _refine_diff_density_min -0.859 _refine_diff_density_rms 0.086 # start Validation Reply Form _vrf_PLAT430_jb1220 ; PROBLEM: Short Inter D...A Contact O12 .. O70 .. 1.84 Ang. RESPONSE: O70 is only 25% occupancy ; # end Validation Reply Form # Attachment 'Ru_1_2_PF6_JZ.CIF' data_jb643 _database_code_depnum_ccdc_archive 'CCDC 692944' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H32 N12 Ru, 2(F6 P)' _chemical_formula_sum 'C42 H32 F12 N12 P2 Ru' _chemical_formula_weight 1095.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall -C2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.324(5) _cell_length_b 17.924(4) _cell_length_c 10.753(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.08(3) _cell_angle_gamma 90.00 _cell_volume 4165.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.747 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2200 _exptl_absorpt_coefficient_mu 0.559 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17314 _diffrn_reflns_av_R_equivalents 0.1765 _diffrn_reflns_av_sigmaI/netI 0.0950 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3698 _reflns_number_gt 3241 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1006P)^2^+15.5980P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3698 _refine_ls_number_parameters 367 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_gt 0.0739 _refine_ls_wR_factor_ref 0.1947 _refine_ls_wR_factor_gt 0.1865 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.5000 0.73351(3) 0.7500 0.0299(2) Uani 1 2 d S . . N1 N 0.4941(2) 0.8156(3) 0.8800(5) 0.0345(10) Uani 1 1 d . . . N2 N 0.5849(2) 0.7319(3) 0.8898(4) 0.0314(10) Uani 1 1 d . . . N3 N 0.5420(2) 0.6533(3) 0.6738(4) 0.0325(10) Uani 1 1 d . . . C1 C 0.4454(3) 0.8592(3) 0.8647(6) 0.0381(13) Uani 1 1 d . . . H1A H 0.4091 0.8539 0.7860 0.046 Uiso 1 1 calc R . . C2 C 0.4458(3) 0.9119(4) 0.9593(6) 0.0427(14) Uani 1 1 d . . . H2A H 0.4099 0.9408 0.9469 0.051 Uiso 1 1 calc R . . C3 C 0.4982(3) 0.9216(4) 1.0705(6) 0.0431(14) Uani 1 1 d . . . H3A H 0.4996 0.9577 1.1362 0.052 Uiso 1 1 calc R . . N4 N 0.7538(2) 0.7098(3) 1.1972(5) 0.0427(12) Uani 1 1 d . . . H4B H 0.7783 0.6737 1.1918 0.051 Uiso 1 1 calc R . . C4 C 0.5497(3) 0.8777(3) 1.0859(5) 0.0377(13) Uani 1 1 d . . . H4A H 0.5867 0.8836 1.1629 0.045 Uiso 1 1 calc R . . N5 N 0.7712(2) 0.7544(3) 1.3080(5) 0.0390(11) Uani 1 1 d . . . C5 C 0.5471(2) 0.8261(3) 0.9903(5) 0.0347(12) Uani 1 1 d . . . C6 C 0.5990(3) 0.7780(3) 0.9973(5) 0.0323(11) Uani 1 1 d . . . N6 N 0.8966(3) 0.8650(3) 1.7623(5) 0.0483(13) Uani 1 1 d . . . C7 C 0.6562(3) 0.7745(3) 1.1006(6) 0.0359(13) Uani 1 1 d . . . H7A H 0.6668 0.8080 1.1743 0.043 Uiso 1 1 calc R . . C8 C 0.6979(3) 0.7212(3) 1.0942(5) 0.0363(13) Uani 1 1 d . . . C9 C 0.6835(3) 0.6743(3) 0.9810(6) 0.0377(13) Uani 1 1 d . . . H9A H 0.7124 0.6386 0.9748 0.045 Uiso 1 1 calc R . . C10 C 0.6256(2) 0.6821(3) 0.8792(5) 0.0319(11) Uani 1 1 d . . . C11 C 0.6022(2) 0.6388(3) 0.7536(5) 0.0314(11) Uani 1 1 d . . . C12 C 0.6377(3) 0.5882(4) 0.7165(6) 0.0413(13) Uani 1 1 d . . . H12A H 0.6792 0.5783 0.7746 0.050 Uiso 1 1 calc R . . C13 C 0.6123(3) 0.5521(4) 0.5938(6) 0.0451(14) Uani 1 1 d . . . H13A H 0.6360 0.5175 0.5661 0.054 Uiso 1 1 calc R . . C14 C 0.5520(3) 0.5675(4) 0.5131(6) 0.0440(14) Uani 1 1 d . . . H14A H 0.5339 0.5440 0.4281 0.053 Uiso 1 1 calc R . . C15 C 0.5181(3) 0.6163(3) 0.5547(5) 0.0371(13) Uani 1 1 d . . . H15A H 0.4762 0.6250 0.4983 0.044 Uiso 1 1 calc R . . C16 C 0.8184(3) 0.7342(4) 1.4069(6) 0.0407(14) Uani 1 1 d . . . H16A H 0.8383 0.6887 1.4017 0.049 Uiso 1 1 calc R . . C17 C 0.8434(3) 0.7794(3) 1.5297(6) 0.0379(13) Uani 1 1 d . . . C18 C 0.8135(3) 0.8408(4) 1.5511(6) 0.0454(15) Uani 1 1 d . . . H18A H 0.7745 0.8552 1.4864 0.054 Uiso 1 1 calc R . . C19 C 0.8406(3) 0.8817(4) 1.6681(6) 0.0486(15) Uani 1 1 d . . . H19A H 0.8189 0.9235 1.6826 0.058 Uiso 1 1 calc R . . C20 C 0.9239(3) 0.8051(4) 1.7389(6) 0.0498(16) Uani 1 1 d . . . H20A H 0.9628 0.7916 1.8049 0.060 Uiso 1 1 calc R . . C21 C 0.9005(3) 0.7606(4) 1.6262(6) 0.0429(14) Uani 1 1 d . . . H21A H 0.9228 0.7185 1.6151 0.052 Uiso 1 1 calc R . . P1 P 0.68494(8) 1.00547(10) 1.40523(16) 0.0441(4) Uani 1 1 d . . . F1 F 0.6874(4) 1.0709(5) 1.5020(9) 0.093(3) Uani 0.822(14) 1 d P A 1 F2 F 0.6880(3) 0.9389(4) 1.3088(6) 0.077(2) Uani 0.822(14) 1 d P A 1 F3 F 0.6837(2) 1.0659(4) 1.2953(7) 0.070(3) Uani 0.822(14) 1 d P A 1 F4 F 0.6899(3) 0.9452(4) 1.5166(8) 0.068(2) Uani 0.822(14) 1 d P A 1 F5 F 0.6131(6) 1.0071(7) 1.3522(13) 0.099(4) Uani 0.822(14) 1 d PU A 1 F6 F 0.7591(4) 1.0076(5) 1.4508(10) 0.058(2) Uani 0.822(14) 1 d P A 1 F1' F 0.6792(12) 1.0988(17) 1.374(3) 0.064(8) Uani 0.178(14) 1 d PU A 2 F2' F 0.668(2) 0.990(3) 1.262(4) 0.118(15) Uani 0.178(14) 1 d PU A 2 F3' F 0.6729(16) 0.9244(18) 1.437(4) 0.074(9) Uani 0.178(14) 1 d PU A 2 F4' F 0.7537(14) 1.0104(18) 1.487(3) 0.023(6) Uani 0.178(14) 1 d PU A 2 F5' F 0.6084(15) 0.9938(18) 1.340(3) 0.020(5) Uani 0.178(14) 1 d PU A 2 F6' F 0.667(3) 1.035(3) 1.519(5) 0.115(15) Uani 0.178(14) 1 d PU A 2 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 0.0221(4) 0.0300(4) 0.0254(3) 0.000 -0.0051(2) 0.000 N1 0.022(2) 0.034(3) 0.036(2) 0.0034(19) -0.0028(17) -0.0003(18) N2 0.025(2) 0.030(2) 0.027(2) -0.0022(17) -0.0036(17) 0.0017(18) N3 0.031(2) 0.029(2) 0.026(2) -0.0007(17) -0.0027(17) -0.0030(18) C1 0.029(3) 0.038(3) 0.037(3) 0.002(2) 0.001(2) 0.003(2) C2 0.032(3) 0.048(4) 0.042(3) -0.001(3) 0.008(2) 0.006(3) C3 0.045(3) 0.039(3) 0.038(3) -0.003(2) 0.007(3) 0.008(3) N4 0.027(2) 0.045(3) 0.036(3) -0.006(2) -0.010(2) 0.007(2) C4 0.035(3) 0.040(3) 0.029(3) -0.003(2) 0.002(2) 0.001(2) N5 0.027(2) 0.042(3) 0.034(3) -0.003(2) -0.0044(19) 0.001(2) C5 0.029(3) 0.035(3) 0.030(3) 0.005(2) -0.002(2) 0.002(2) C6 0.030(3) 0.029(3) 0.030(3) -0.002(2) 0.003(2) -0.001(2) N6 0.047(3) 0.049(3) 0.033(3) -0.001(2) -0.002(2) 0.001(2) C7 0.030(3) 0.034(3) 0.032(3) -0.004(2) -0.003(2) -0.003(2) C8 0.025(3) 0.046(3) 0.027(3) 0.002(2) -0.003(2) 0.002(2) C9 0.026(3) 0.039(3) 0.039(3) 0.000(2) 0.002(2) 0.000(2) C10 0.022(2) 0.033(3) 0.032(3) 0.004(2) 0.000(2) 0.004(2) C11 0.031(3) 0.027(3) 0.027(2) 0.001(2) 0.001(2) 0.001(2) C12 0.036(3) 0.043(3) 0.037(3) 0.000(2) 0.005(2) 0.001(3) C13 0.052(4) 0.037(3) 0.043(3) -0.002(2) 0.013(3) 0.001(3) C14 0.057(4) 0.038(3) 0.033(3) -0.004(2) 0.011(3) -0.005(3) C15 0.041(3) 0.031(3) 0.025(3) 0.001(2) -0.004(2) -0.006(2) C16 0.036(3) 0.044(3) 0.031(3) 0.000(2) -0.002(2) 0.003(3) C17 0.030(3) 0.039(3) 0.034(3) 0.000(2) -0.001(2) -0.005(2) C18 0.037(3) 0.045(4) 0.037(3) 0.004(3) -0.006(2) 0.001(3) C19 0.054(4) 0.042(4) 0.037(3) -0.005(3) 0.004(3) 0.002(3) C20 0.046(4) 0.056(4) 0.028(3) 0.003(3) -0.008(2) -0.004(3) C21 0.041(3) 0.045(3) 0.031(3) -0.001(2) 0.001(2) 0.011(3) P1 0.0381(9) 0.0416(9) 0.0430(9) 0.0032(7) 0.0044(7) -0.0041(7) F1 0.099(6) 0.075(5) 0.113(6) -0.041(5) 0.046(5) 0.004(4) F2 0.078(4) 0.071(5) 0.066(4) -0.030(3) 0.009(3) -0.007(3) F3 0.046(3) 0.071(4) 0.079(5) 0.043(4) 0.006(3) -0.004(3) F4 0.057(3) 0.081(5) 0.063(4) 0.033(3) 0.019(3) 0.008(3) F5 0.045(4) 0.088(8) 0.139(8) 0.039(6) 0.006(4) -0.016(4) F6 0.045(3) 0.056(4) 0.068(6) 0.001(4) 0.017(3) 0.005(2) F1' 0.047(12) 0.068(14) 0.075(16) -0.004(12) 0.021(10) -0.010(10) F2' 0.13(2) 0.13(2) 0.093(19) -0.018(16) 0.039(15) 0.016(17) F3' 0.069(15) 0.057(14) 0.089(18) 0.015(13) 0.022(13) 0.013(11) F4' 0.020(7) 0.018(7) 0.024(7) 0.002(5) -0.001(4) 0.001(4) F5' 0.017(7) 0.019(7) 0.021(6) -0.002(4) 0.004(4) -0.004(4) F6' 0.14(2) 0.12(2) 0.095(19) -0.021(16) 0.057(16) -0.026(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N2 1.986(4) 2_656 ? Ru1 N2 1.986(4) . ? Ru1 N1 2.069(5) . ? Ru1 N1 2.069(5) 2_656 ? Ru1 N3 2.075(5) 2_656 ? Ru1 N3 2.075(5) . ? N1 C1 1.338(7) . ? N1 C5 1.367(7) . ? N2 C10 1.339(7) . ? N2 C6 1.357(7) . ? N3 C15 1.361(7) . ? N3 C11 1.366(7) . ? C1 C2 1.385(9) . ? C1 H1A 0.9500 . ? C2 C3 1.362(9) . ? C2 H2A 0.9500 . ? C3 C4 1.392(8) . ? C3 H3A 0.9500 . ? N4 N5 1.365(7) . ? N4 C8 1.372(7) . ? N4 H4B 0.8800 . ? C4 C5 1.368(8) . ? C4 H4A 0.9500 . ? N5 C16 1.263(8) . ? C5 C6 1.464(8) . ? C6 C7 1.381(8) . ? N6 C20 1.320(9) . ? N6 C19 1.351(8) . ? C7 C8 1.382(9) . ? C7 H7A 0.9500 . ? C8 C9 1.413(8) . ? C9 C10 1.390(7) . ? C9 H9A 0.9500 . ? C10 C11 1.474(7) . ? C11 C12 1.384(8) . ? C12 C13 1.387(8) . ? C12 H12A 0.9500 . ? C13 C14 1.375(9) . ? C13 H13A 0.9500 . ? C14 C15 1.362(9) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.470(8) . ? C16 H16A 0.9500 . ? C17 C18 1.367(9) . ? C17 C21 1.387(8) . ? C18 C19 1.387(9) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C21 1.381(9) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? P1 F2' 1.47(4) . ? P1 F6' 1.53(4) . ? P1 F3' 1.54(3) . ? P1 F5 1.554(12) . ? P1 F1 1.555(7) . ? P1 F4' 1.51(3) . ? P1 F4 1.584(6) . ? P1 F3 1.595(5) . ? P1 F6 1.612(8) . ? P1 F2 1.599(6) . ? P1 F5' 1.67(3) . ? P1 F1' 1.70(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ru1 N2 178.3(3) 2_656 . ? N2 Ru1 N1 102.81(18) 2_656 . ? N2 Ru1 N1 78.43(17) . . ? N2 Ru1 N1 78.43(17) 2_656 2_656 ? N2 Ru1 N1 102.81(18) . 2_656 ? N1 Ru1 N1 89.4(3) . 2_656 ? N2 Ru1 N3 78.68(17) 2_656 2_656 ? N2 Ru1 N3 100.12(18) . 2_656 ? N1 Ru1 N3 93.72(19) . 2_656 ? N1 Ru1 N3 157.02(17) 2_656 2_656 ? N2 Ru1 N3 100.12(18) 2_656 . ? N2 Ru1 N3 78.68(17) . . ? N1 Ru1 N3 157.02(17) . . ? N1 Ru1 N3 93.72(18) 2_656 . ? N3 Ru1 N3 92.2(3) 2_656 . ? C1 N1 C5 118.4(5) . . ? C1 N1 Ru1 126.9(4) . . ? C5 N1 Ru1 114.6(4) . . ? C10 N2 C6 121.8(4) . . ? C10 N2 Ru1 118.9(3) . . ? C6 N2 Ru1 119.3(4) . . ? C15 N3 C11 117.3(5) . . ? C15 N3 Ru1 128.4(4) . . ? C11 N3 Ru1 114.2(3) . . ? N1 C1 C2 122.5(5) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? C3 C2 C1 119.2(6) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C2 C3 C4 118.8(6) . . ? C2 C3 H3A 120.6 . . ? C4 C3 H3A 120.6 . . ? N5 N4 C8 119.8(5) . . ? N5 N4 H4B 120.1 . . ? C8 N4 H4B 120.1 . . ? C5 C4 C3 120.0(5) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C16 N5 N4 116.4(5) . . ? N1 C5 C4 121.1(5) . . ? N1 C5 C6 115.0(5) . . ? C4 C5 C6 123.9(5) . . ? N2 C6 C7 120.6(5) . . ? N2 C6 C5 112.6(5) . . ? C7 C6 C5 126.7(5) . . ? C20 N6 C19 115.8(5) . . ? C6 C7 C8 118.4(5) . . ? C6 C7 H7A 120.8 . . ? C8 C7 H7A 120.8 . . ? N4 C8 C7 122.4(5) . . ? N4 C8 C9 116.8(5) . . ? C7 C8 C9 120.7(5) . . ? C10 C9 C8 117.7(5) . . ? C10 C9 H9A 121.2 . . ? C8 C9 H9A 121.2 . . ? N2 C10 C9 120.7(5) . . ? N2 C10 C11 113.5(4) . . ? C9 C10 C11 125.8(5) . . ? N3 C11 C12 121.9(5) . . ? N3 C11 C10 114.5(5) . . ? C12 C11 C10 123.6(5) . . ? C11 C12 C13 119.4(5) . . ? C11 C12 H12A 120.3 . . ? C13 C12 H12A 120.3 . . ? C14 C13 C12 118.5(6) . . ? C14 C13 H13A 120.8 . . ? C12 C13 H13A 120.8 . . ? C15 C14 C13 120.3(6) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? N3 C15 C14 122.6(5) . . ? N3 C15 H15A 118.7 . . ? C14 C15 H15A 118.7 . . ? N5 C16 C17 121.6(6) . . ? N5 C16 H16A 119.2 . . ? C17 C16 H16A 119.2 . . ? C18 C17 C21 118.4(5) . . ? C18 C17 C16 122.6(5) . . ? C21 C17 C16 118.9(6) . . ? C17 C18 C19 119.4(6) . . ? C17 C18 H18A 120.3 . . ? C19 C18 H18A 120.3 . . ? N6 C19 C18 123.1(6) . . ? N6 C19 H19A 118.4 . . ? C18 C19 H19A 118.4 . . ? N6 C20 C21 125.3(6) . . ? N6 C20 H20A 117.4 . . ? C21 C20 H20A 117.4 . . ? C20 C21 C17 117.9(6) . . ? C20 C21 H21A 121.0 . . ? C17 C21 H21A 121.0 . . ? F2' P1 F6' 149(3) . . ? F2' P1 F3' 93(3) . . ? F6' P1 F3' 91(2) . . ? F2' P1 F5 77.5(19) . . ? F6' P1 F5 73(2) . . ? F3' P1 F5 80.6(13) . . ? F2' P1 F1 140(2) . . ? F3' P1 F1 121.6(16) . . ? F5 P1 F1 89.7(6) . . ? F2' P1 F4' 116(2) . . ? F6' P1 F4' 94(2) . . ? F3' P1 F4' 99.6(18) . . ? F5 P1 F4' 166.5(11) . . ? F1 P1 F4' 78.6(12) . . ? F2' P1 F4 125(2) . . ? F6' P1 F4 66(2) . . ? F5 P1 F4 93.0(5) . . ? F1 P1 F4 92.0(5) . . ? F4' P1 F4 80.8(12) . . ? F2' P1 F3 55(2) . . ? F6' P1 F3 115(2) . . ? F3' P1 F3 148.3(16) . . ? F5 P1 F3 89.9(5) . . ? F1 P1 F3 88.2(5) . . ? F4' P1 F3 96.4(12) . . ? F4 P1 F3 177.1(3) . . ? F2' P1 F6 99.5(19) . . ? F6' P1 F6 109(2) . . ? F3' P1 F6 102.7(12) . . ? F5 P1 F6 175.7(6) . . ? F1 P1 F6 90.8(5) . . ? F4 P1 F6 91.3(4) . . ? F3 P1 F6 85.8(4) . . ? F6' P1 F2 150(2) . . ? F3' P1 F2 60.0(16) . . ? F5 P1 F2 94.6(6) . . ? F1 P1 F2 175.7(4) . . ? F4' P1 F2 97.2(12) . . ? F4 P1 F2 88.4(4) . . ? F3 P1 F2 91.1(4) . . ? F6 P1 F2 84.9(4) . . ? F2' P1 F5' 73(2) . . ? F6' P1 F5' 79(2) . . ? F3' P1 F5' 73.8(17) . . ? F1 P1 F5' 98.1(9) . . ? F4' P1 F5' 170.0(15) . . ? F4 P1 F5' 89.8(11) . . ? F3 P1 F5' 93.0(11) . . ? F6 P1 F5' 171.0(9) . . ? F2 P1 F5' 86.2(9) . . ? F2' P1 F1' 90(2) . . ? F6' P1 F1' 78(2) . . ? F3' P1 F1' 164.1(15) . . ? F5 P1 F1' 85.2(10) . . ? F1 P1 F1' 50.9(11) . . ? F4' P1 F1' 92.5(15) . . ? F4 P1 F1' 142.8(12) . . ? F6 P1 F1' 91.8(9) . . ? F2 P1 F1' 128.8(12) . . ? F5' P1 F1' 92.7(14) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.554 _refine_diff_density_min -1.662 _refine_diff_density_rms 0.135 # start Validation Reply Form _vrf_PLAT221_jb643 ; PROBLEM: Large Solvent/Anion F Ueq(max)/Ueq(min) ... 5.95 Ratio RESPONSE: Related to disorder ; # end Validation Reply Form # Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Catherine E Housecroft' ; ? # Address for author 1 ; ; ? # Footnote for author 1 ; 'Jonathon E Beves' ; ? # Address 2 ; ; ? # Footnote 2 ; 'Edwin C. Constable' '' '' 'Cameron Kepert' '' '' 'Markus Neuburger' '' '' 'David J Price' '' '' 'Silvia Schaffner' '' '' 'Jennifer A Zampese' '' '' _publ_contact_author_name 'Catherine E Housecroft' _publ_contact_author_email CATHERINE.HOUSECROFT@UNIBAS.CH _publ_section_title ; Curly-curly, loop-loop: homoleptic metal(II) complexes of pyridinecarbaldehyde 4'-(2,2':6',2"-terpyridyl)hydrazones and their coordination polymers ; _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_address ; Chemical Crystallography Laboratory, Department of Chemistry, University of Nowhere, Nowhere, NO1 4T, UK. ; _publ_contact_author_fax '+44 1865 000000' _publ_contact_author_phone '+44 1865 000000' # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # 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 E. The figures will be sent by e-mail. ; _publ_requested_category EO # choose from: FI FM FO CI CM CO AD _publ_requested_coeditor_name 'Prof William Clegg' _publ_requested_journal 'Section E' # Attachment 'Fe_1_2_MN.cif' data_jb451 _database_code_depnum_ccdc_archive 'CCDC 692938' _audit_creation_date 06-12-08 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '12080929 jb451_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 10.2902(2) _cell_length_b 13.5226(3) _cell_length_c 20.1859(4) _cell_angle_alpha 89.1662(9) _cell_angle_beta 79.5970(12) _cell_angle_gamma 67.9900(11) _cell_volume 2557.00(9) _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 57.7998 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' 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 1 # Given Formula = C84 H64 F24 Fe2 N24 P4 # Dc = 1.36 Fooo = 1174.00 Mu = 4.43 M = 1050.57 # Found Formula = C94 H79 F24 Fe2 N29 P4 # Dc = 1.50 FOOO = 1174.00 Mu = 4.52 M = 1153.20 _chemical_formula_sum 'C94 H79 F24 Fe2 N29 P4' _chemical_formula_moiety '2(C42 H32 Fe N12), 4(F6 P), 5(C2 H3 N)' _chemical_compound_source ? _chemical_formula_weight 2306.40 _cell_measurement_reflns_used 11694 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_max 0.22 _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1174 _exptl_absorpt_coefficient_mu 0.452 # Sheldrick geometric approximatio 0.92 0.97 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.97 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _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 23137 _reflns_number_total 11743 _diffrn_reflns_av_R_equivalents 0.032 # Number of reflections with Friedels Law is 11743 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 11728 _diffrn_reflns_theta_min 1.873 _diffrn_reflns_theta_max 27.485 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.485 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min -17 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _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 0.53 _refine_ls_number_reflns 7102 _refine_ls_number_restraints 168 _refine_ls_number_parameters 703 #_refine_ls_R_factor_ref 0.0459 _refine_ls_wR_factor_ref 0.0534 _refine_ls_goodness_of_fit_ref 1.1656 #_reflns_number_all 11627 _refine_ls_R_factor_all 0.0831 _refine_ls_wR_factor_all 0.0743 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>2.3\s(I) _reflns_number_gt 7102 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_gt 0.0534 _refine_ls_shift/su_max 0.001298 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.896 0.851 0.579 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # 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). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: 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 atomsattached 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 0.26667(4) 0.23084(3) 0.757531(17) 0.0285 1.0000 Uani . . . . . . N1 N 0.1100(2) 0.31934(18) 0.71271(11) 0.0325 1.0000 Uani . . . . . . N2 N 0.1336(2) 0.30729(17) 0.83403(10) 0.0295 1.0000 Uani . . . . . . N3 N 0.3810(2) 0.17033(17) 0.82798(10) 0.0292 1.0000 Uani . . . . . . N4 N 0.3636(2) 0.33044(17) 0.73166(10) 0.0316 1.0000 Uani . . . . . . N5 N 0.3996(2) 0.15278(17) 0.68169(10) 0.0306 1.0000 Uani . . . . . . N6 N 0.2129(2) 0.10487(17) 0.75739(10) 0.0306 1.0000 Uani . . . . . . N7 N -0.1627(2) 0.4571(2) 1.00401(12) 0.0410 1.0000 Uani . . . . . . N8 N -0.2963(2) 0.52765(18) 1.00149(12) 0.0381 1.0000 Uani . . . . . . N9 N -0.8081(3) 0.7857(2) 1.07544(15) 0.0505 1.0000 Uani . . . . . . N10 N 0.6959(3) -0.0285(2) 0.51979(12) 0.0426 1.0000 Uani . . . . . . N11 N 0.7942(2) 0.0034(2) 0.48143(11) 0.0393 1.0000 Uani . . . . . . N12 N 1.2044(3) -0.0007(2) 0.29815(12) 0.0465 1.0000 Uani . . . . . . N13 N 0.8428(4) 0.2896(3) 0.5157(2) 0.0789 1.0000 Uani D U . . . . N14 N 0.4544(5) 0.3624(4) 0.1760(3) 0.0987 1.0000 Uani D U . . . . N15 N 0.3136(10) -0.0468(7) 0.9108(5) 0.0895 0.5000 Uani D U . . . . C1 C 0.1133(3) 0.3252(2) 0.64616(14) 0.0396 1.0000 Uani . . . . . . C2 C 0.0011(4) 0.3955(3) 0.61949(16) 0.0500 1.0000 Uani . . . . . . C3 C -0.1189(4) 0.4621(3) 0.66263(17) 0.0545 1.0000 Uani . . . . . . C4 C -0.1245(3) 0.4568(3) 0.73150(16) 0.0463 1.0000 Uani . . . . . . C5 C -0.0082(3) 0.3859(2) 0.75547(13) 0.0336 1.0000 Uani . . . . . . C6 C 0.0036(3) 0.3776(2) 0.82712(13) 0.0303 1.0000 Uani . . . . . . C7 C -0.0992(3) 0.4314(2) 0.88205(13) 0.0331 1.0000 Uani . . . . . . C8 C -0.0655(3) 0.4117(2) 0.94633(13) 0.0327 1.0000 Uani . . . . . . C9 C 0.0708(3) 0.3401(2) 0.95302(13) 0.0336 1.0000 Uani . . . . . . C10 C 0.1673(3) 0.2895(2) 0.89585(12) 0.0308 1.0000 Uani . . . . . . C11 C 0.3141(3) 0.2101(2) 0.89208(12) 0.0313 1.0000 Uani . . . . . . C12 C 0.3791(3) 0.1769(2) 0.94696(14) 0.0374 1.0000 Uani . . . . . . C13 C 0.5168(3) 0.1007(2) 0.93724(15) 0.0414 1.0000 Uani . . . . . . C14 C 0.5846(3) 0.0589(2) 0.87248(15) 0.0406 1.0000 Uani . . . . . . C15 C 0.5140(3) 0.0952(2) 0.81961(13) 0.0343 1.0000 Uani . . . . . . C16 C 0.3292(3) 0.4278(2) 0.76085(14) 0.0383 1.0000 Uani . . . . . . C17 C 0.4041(3) 0.4921(2) 0.73940(16) 0.0456 1.0000 Uani . . . . . . C18 C 0.5172(3) 0.4559(3) 0.68576(16) 0.0471 1.0000 Uani . . . . . . C19 C 0.5518(3) 0.3572(2) 0.65378(15) 0.0420 1.0000 Uani . . . . . . C20 C 0.4731(3) 0.2959(2) 0.67718(13) 0.0329 1.0000 Uani . . . . . . C21 C 0.4942(3) 0.1912(2) 0.64707(12) 0.0315 1.0000 Uani . . . . . . C22 C 0.5948(3) 0.1352(2) 0.59168(12) 0.0336 1.0000 Uani . . . . . . C23 C 0.5979(3) 0.0356(2) 0.57206(12) 0.0330 1.0000 Uani . . . . . . C24 C 0.4985(3) -0.0038(2) 0.60796(13) 0.0354 1.0000 Uani . . . . . . C25 C 0.4013(3) 0.0572(2) 0.66228(13) 0.0325 1.0000 Uani . . . . . . C26 C 0.2914(3) 0.0293(2) 0.70671(12) 0.0319 1.0000 Uani . . . . . . C27 C 0.2689(3) -0.0651(2) 0.69981(14) 0.0379 1.0000 Uani . . . . . . C28 C 0.1646(3) -0.0833(2) 0.74599(15) 0.0438 1.0000 Uani . . . . . . C29 C 0.0850(3) -0.0069(2) 0.79757(15) 0.0420 1.0000 Uani . . . . . . C30 C 0.1122(3) 0.0853(2) 0.80176(13) 0.0346 1.0000 Uani . . . . . . C31 C -0.3822(3) 0.5566(2) 1.05832(14) 0.0411 1.0000 Uani . . . . . . C32 C -0.5286(3) 0.6338(2) 1.06239(15) 0.0401 1.0000 Uani . . . . . . C33 C -0.6149(3) 0.6715(2) 1.12538(16) 0.0436 1.0000 Uani . . . . . . C34 C -0.7507(3) 0.7467(3) 1.12890(17) 0.0490 1.0000 Uani . . . . . . C35 C -0.7251(3) 0.7473(3) 1.01464(17) 0.0490 1.0000 Uani . . . . . . C36 C -0.5863(3) 0.6733(2) 1.00586(16) 0.0448 1.0000 Uani . . . . . . C37 C 0.8877(3) -0.0672(2) 0.43837(13) 0.0403 1.0000 Uani . . . . . . C38 C 0.9969(3) -0.0429(2) 0.39166(13) 0.0375 1.0000 Uani . . . . . . C39 C 1.0101(3) 0.0548(2) 0.39309(15) 0.0442 1.0000 Uani . . . . . . C40 C 1.1137(3) 0.0722(3) 0.34586(16) 0.0473 1.0000 Uani . . . . . . C41 C 1.1902(3) -0.0948(3) 0.29764(14) 0.0442 1.0000 Uani . . . . . . C42 C 1.0907(3) -0.1205(3) 0.34239(14) 0.0406 1.0000 Uani . . . . . . C43 C 0.8186(5) 0.3347(3) 0.4695(2) 0.0736 1.0000 Uani D U . . . . C44 C 0.7852(9) 0.3912(5) 0.4087(3) 0.1206 1.0000 Uani D U . . . . C45 C 0.4382(5) 0.2873(4) 0.1956(3) 0.0847 1.0000 Uani D U . . . . C46 C 0.4091(7) 0.1962(4) 0.2240(4) 0.1126 1.0000 Uani D U . . . . C47 C 0.2145(12) -0.0070(6) 0.9507(4) 0.0824 0.5000 Uani D U . . . . C48 C 0.0756(15) 0.0287(11) 0.9966(6) 0.1734 0.5000 Uani D U . . . . P1 P -0.01955(9) 0.71290(6) 0.84092(4) 0.0448 1.0000 Uani D U . . . . P2 P 0.36912(11) 0.32296(7) 0.46115(4) 0.0572 1.0000 Uani D U . . . . F1 F 0.0601(2) 0.59714(16) 0.86927(10) 0.0629 1.0000 Uani D U . . . . F2 F -0.0949(2) 0.82686(17) 0.81415(12) 0.0746 1.0000 Uani D U . . . . F3 F 0.0350(3) 0.7624(2) 0.89571(18) 0.1050 1.0000 Uani D U . . . . F4 F -0.0714(4) 0.6582(2) 0.78844(13) 0.0953 1.0000 Uani D U . . . . F5 F -0.1598(2) 0.7270(2) 0.89409(12) 0.0831 1.0000 Uani D U . . . . F6 F 0.1209(3) 0.6954(2) 0.78785(16) 0.1049 1.0000 Uani D U . . . . F11 F 0.2106(3) 0.4103(2) 0.47412(14) 0.0992 1.0000 Uani D U . . . . F12 F 0.5238(3) 0.2314(2) 0.44792(13) 0.0817 1.0000 Uani D U . . . . F13 F 0.3107(3) 0.2376(2) 0.49759(16) 0.1000 1.0000 Uani D U . . . . F14 F 0.4227(5) 0.4073(3) 0.4278(2) 0.1503 1.0000 Uani D U . . . . F15 F 0.3867(3) 0.35512(19) 0.53266(12) 0.0840 1.0000 Uani D U . . . . F16 F 0.3481(4) 0.2865(3) 0.39128(15) 0.1536 1.0000 Uani D U . . . . H7 H -0.1381 0.4409 1.0434 0.0367 1.0000 Uiso R . . . . . H10 H 0.6969 -0.0924 0.5117 0.0426 1.0000 Uiso R . . . . . H11 H 0.1954 0.2794 0.6165 0.0419 1.0000 Uiso R . . . . . H21 H 0.0073 0.3969 0.5724 0.0552 1.0000 Uiso R . . . . . H31 H -0.1966 0.5108 0.6460 0.0563 1.0000 Uiso R . . . . . H41 H -0.2057 0.5019 0.7617 0.0465 1.0000 Uiso R . . . . . H71 H -0.1889 0.4800 0.8770 0.0325 1.0000 Uiso R . . . . . H91 H 0.0957 0.3275 0.9953 0.0327 1.0000 Uiso R . . . . . H121 H 0.3304 0.2056 0.9910 0.0360 1.0000 Uiso R . . . . . H131 H 0.5631 0.0774 0.9738 0.0411 1.0000 Uiso R . . . . . H141 H 0.6776 0.0074 0.8643 0.0381 1.0000 Uiso R . . . . . H151 H 0.5595 0.0666 0.7754 0.0320 1.0000 Uiso R . . . . . H161 H 0.2508 0.4526 0.7974 0.0391 1.0000 Uiso R . . . . . H171 H 0.3777 0.5598 0.7611 0.0482 1.0000 Uiso R . . . . . H181 H 0.5708 0.4983 0.6708 0.0513 1.0000 Uiso R . . . . . H191 H 0.6271 0.3321 0.6166 0.0454 1.0000 Uiso R . . . . . H221 H 0.6583 0.1638 0.5681 0.0306 1.0000 Uiso R . . . . . H241 H 0.4978 -0.0702 0.5950 0.0343 1.0000 Uiso R . . . . . H271 H 0.3236 -0.1154 0.6640 0.0382 1.0000 Uiso R . . . . . H281 H 0.1473 -0.1466 0.7425 0.0440 1.0000 Uiso R . . . . . H291 H 0.0129 -0.0179 0.8293 0.0411 1.0000 Uiso R . . . . . H301 H 0.0579 0.1382 0.8371 0.0343 1.0000 Uiso R . . . . . H311 H -0.3518 0.5288 1.0991 0.0397 1.0000 Uiso R . . . . . H331 H -0.5809 0.6459 1.1652 0.0433 1.0000 Uiso R . . . . . H341 H -0.8096 0.7730 1.1716 0.0472 1.0000 Uiso R . . . . . H351 H -0.7637 0.7727 0.9754 0.0512 1.0000 Uiso R . . . . . H361 H -0.5313 0.6498 0.9623 0.0430 1.0000 Uiso R . . . . . H371 H 0.8875 -0.1373 0.4363 0.0393 1.0000 Uiso R . . . . . H391 H 0.9498 0.1080 0.4256 0.0444 1.0000 Uiso R . . . . . H401 H 1.1214 0.1395 0.3474 0.0484 1.0000 Uiso R . . . . . H411 H 1.2539 -0.1471 0.2644 0.0423 1.0000 Uiso R . . . . . H421 H 1.0855 -0.1892 0.3399 0.0418 1.0000 Uiso R . . . . . H441 H 0.8206 0.4483 0.4067 0.1573 1.0000 Uiso R . . . . . H442 H 0.6829 0.4193 0.4134 0.1572 1.0000 Uiso R . . . . . H443 H 0.8298 0.3422 0.3698 0.1572 1.0000 Uiso R . . . . . H461 H 0.4816 0.1336 0.1983 0.1570 1.0000 Uiso R . . . . . H462 H 0.4169 0.1922 0.2715 0.1571 1.0000 Uiso R . . . . . H463 H 0.3150 0.2014 0.2185 0.1572 1.0000 Uiso R . . . . . H481 H 0.0657 0.0840 1.0294 0.1900 0.5000 Uiso R . . . . . H482 H 0.0658 -0.0321 1.0198 0.1900 0.5000 Uiso R . . . . . H483 H 0.0021 0.0565 0.9695 0.1900 0.5000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02597(17) 0.03208(19) 0.02457(17) 0.00138(13) -0.00016(12) -0.00975(13) N1 0.0312(11) 0.0364(11) 0.0314(11) 0.0047(9) -0.0053(8) -0.0148(9) N2 0.0253(10) 0.0313(11) 0.0289(10) 0.0026(8) -0.0017(8) -0.0089(8) N3 0.0235(9) 0.0327(11) 0.0298(10) 0.0023(8) -0.0010(8) -0.0105(8) N4 0.0294(10) 0.0350(11) 0.0284(10) 0.0056(8) -0.0051(8) -0.0102(9) N5 0.0283(10) 0.0334(11) 0.0281(10) 0.0036(8) -0.0021(8) -0.0109(9) N6 0.0253(10) 0.0353(11) 0.0290(10) 0.0036(8) -0.0029(8) -0.0101(8) N7 0.0280(11) 0.0487(14) 0.0345(12) -0.0071(10) -0.0019(9) -0.0027(10) N8 0.0298(11) 0.0361(12) 0.0420(12) -0.0055(10) -0.0014(9) -0.0076(9) N9 0.0331(12) 0.0461(14) 0.0647(17) -0.0066(13) -0.0053(12) -0.0079(11) N10 0.0394(12) 0.0495(14) 0.0351(12) -0.0085(10) 0.0091(10) -0.0196(11) N11 0.0367(12) 0.0482(14) 0.0276(11) -0.0008(9) 0.0020(9) -0.0136(10) N12 0.0373(13) 0.0557(16) 0.0376(13) 0.0055(11) 0.0011(10) -0.0115(11) N13 0.092(3) 0.069(2) 0.072(2) -0.0009(18) -0.014(2) -0.027(2) N14 0.099(3) 0.094(3) 0.099(3) -0.019(3) -0.019(2) -0.030(3) N15 0.114(6) 0.083(5) 0.104(6) 0.038(4) -0.055(5) -0.059(5) C1 0.0404(14) 0.0487(16) 0.0325(13) 0.0071(12) -0.0078(11) -0.0198(13) C2 0.0534(18) 0.067(2) 0.0355(15) 0.0138(14) -0.0166(13) -0.0256(16) C3 0.0424(17) 0.070(2) 0.0493(17) 0.0208(16) -0.0193(14) -0.0148(15) C4 0.0325(14) 0.0527(18) 0.0468(16) 0.0113(13) -0.0092(12) -0.0079(12) C5 0.0322(12) 0.0355(13) 0.0335(13) 0.0056(10) -0.0048(10) -0.0139(11) C6 0.0297(12) 0.0303(12) 0.0321(12) 0.0029(10) -0.0056(10) -0.0128(10) C7 0.0248(11) 0.0327(13) 0.0378(13) -0.0008(10) -0.0028(10) -0.0076(10) C8 0.0319(12) 0.0311(13) 0.0325(13) -0.0049(10) 0.0007(10) -0.0116(10) C9 0.0294(12) 0.0389(14) 0.0291(12) -0.0006(10) -0.0032(10) -0.0099(10) C10 0.0263(11) 0.0321(12) 0.0305(12) 0.0005(10) -0.0011(9) -0.0090(10) C11 0.0269(11) 0.0342(13) 0.0292(12) 0.0024(10) -0.0005(9) -0.0097(10) C12 0.0368(13) 0.0421(15) 0.0302(13) 0.0043(11) -0.0059(10) -0.0118(11) C13 0.0338(13) 0.0467(16) 0.0413(15) 0.0094(12) -0.0135(11) -0.0099(12) C14 0.0267(12) 0.0391(15) 0.0488(16) 0.0036(12) -0.0055(11) -0.0052(11) C15 0.0291(12) 0.0340(13) 0.0332(13) -0.0004(10) 0.0024(10) -0.0084(10) C16 0.0385(14) 0.0396(15) 0.0361(13) 0.0010(11) -0.0061(11) -0.0144(12) C17 0.0501(17) 0.0375(15) 0.0508(17) 0.0020(12) -0.0096(13) -0.0185(13) C18 0.0516(17) 0.0454(16) 0.0511(17) 0.0125(13) -0.0097(14) -0.0264(14) C19 0.0392(14) 0.0510(17) 0.0384(14) 0.0084(12) -0.0018(11) -0.0225(13) C20 0.0306(12) 0.0376(13) 0.0294(12) 0.0065(10) -0.0057(10) -0.0118(10) C21 0.0294(12) 0.0381(13) 0.0267(12) 0.0041(10) -0.0034(9) -0.0133(10) C22 0.0287(12) 0.0442(15) 0.0261(11) 0.0038(10) -0.0007(9) -0.0139(11) C23 0.0268(11) 0.0423(14) 0.0236(11) -0.0002(10) -0.0009(9) -0.0076(10) C24 0.0356(13) 0.0396(14) 0.0285(12) -0.0004(10) -0.0008(10) -0.0138(11) C25 0.0280(12) 0.0388(14) 0.0288(12) 0.0004(10) -0.0013(9) -0.0122(10) C26 0.0307(12) 0.0347(13) 0.0277(12) 0.0022(10) -0.0029(10) -0.0107(10) C27 0.0400(14) 0.0394(14) 0.0340(13) -0.0011(11) -0.0023(11) -0.0165(12) C28 0.0452(15) 0.0418(15) 0.0479(16) 0.0069(12) -0.0057(13) -0.0220(13) C29 0.0367(14) 0.0499(17) 0.0412(15) 0.0101(12) 0.0004(11) -0.0222(12) C30 0.0266(12) 0.0391(14) 0.0334(13) 0.0018(10) -0.0001(10) -0.0097(10) C31 0.0314(13) 0.0458(16) 0.0373(14) -0.0083(12) 0.0002(11) -0.0075(12) C32 0.0291(13) 0.0382(15) 0.0479(16) -0.0057(12) -0.0005(11) -0.0098(11) C33 0.0312(13) 0.0493(17) 0.0442(16) -0.0075(13) -0.0003(11) -0.0111(12) C34 0.0318(14) 0.0529(18) 0.0539(18) -0.0105(14) 0.0036(13) -0.0113(13) C35 0.0459(16) 0.0458(17) 0.0546(18) 0.0007(14) -0.0127(14) -0.0150(14) C36 0.0384(15) 0.0459(16) 0.0452(16) -0.0071(13) -0.0010(12) -0.0132(13) C37 0.0379(14) 0.0480(16) 0.0308(13) -0.0031(11) -0.0004(11) -0.0143(12) C38 0.0295(12) 0.0478(16) 0.0288(12) -0.0020(11) 0.0006(10) -0.0100(11) C39 0.0381(14) 0.0447(16) 0.0394(15) -0.0043(12) 0.0032(11) -0.0085(12) C40 0.0413(15) 0.0478(17) 0.0481(17) 0.0002(13) 0.0021(13) -0.0163(13) C41 0.0335(14) 0.0558(18) 0.0317(13) -0.0054(12) 0.0031(11) -0.0076(12) C42 0.0332(13) 0.0499(16) 0.0317(13) -0.0032(11) 0.0013(11) -0.0111(12) C43 0.097(3) 0.049(2) 0.067(2) -0.0076(18) -0.013(2) -0.019(2) C44 0.184(6) 0.077(3) 0.081(3) 0.010(3) -0.029(4) -0.026(4) C45 0.076(3) 0.068(3) 0.105(4) -0.014(2) -0.040(3) -0.010(2) C46 0.114(4) 0.079(3) 0.155(5) 0.020(3) -0.074(4) -0.026(3) C47 0.135(7) 0.041(4) 0.061(5) 0.012(3) -0.059(4) -0.005(4) C48 0.194(12) 0.117(10) 0.077(7) 0.024(7) -0.010(8) 0.082(9) P1 0.0474(4) 0.0410(4) 0.0430(4) 0.0061(3) -0.0041(3) -0.0155(3) P2 0.0726(6) 0.0494(5) 0.0348(4) 0.0085(3) -0.0054(4) -0.0088(4) F1 0.0754(14) 0.0527(11) 0.0573(12) 0.0166(9) -0.0142(10) -0.0202(10) F2 0.0688(14) 0.0511(12) 0.0834(16) 0.0209(11) -0.0010(11) -0.0064(10) F3 0.116(2) 0.0727(16) 0.140(3) -0.0144(16) -0.065(2) -0.0311(16) F4 0.139(2) 0.0848(17) 0.0735(16) 0.0013(13) -0.0512(17) -0.0404(17) F5 0.0577(13) 0.1103(19) 0.0645(14) 0.0241(13) 0.0063(10) -0.0216(13) F6 0.0726(16) 0.0768(16) 0.122(2) 0.0378(16) 0.0352(15) -0.0051(13) F11 0.0893(18) 0.0899(18) 0.0753(17) -0.0047(14) -0.0167(14) 0.0155(15) F12 0.0714(15) 0.0781(16) 0.0719(15) 0.0011(12) -0.0056(12) -0.0051(12) F13 0.119(2) 0.0662(15) 0.112(2) -0.0187(14) 0.0170(18) -0.0490(16) F14 0.170(3) 0.094(2) 0.142(3) 0.055(2) 0.048(3) -0.037(2) F15 0.117(2) 0.0647(14) 0.0648(14) -0.0059(11) -0.0315(14) -0.0211(14) F16 0.157(3) 0.163(3) 0.0591(16) -0.0406(18) -0.0497(19) 0.046(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2640(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 . 1.975(2) yes Fe1 . N2 . 1.884(2) yes Fe1 . N3 . 1.981(2) yes Fe1 . N4 . 1.970(2) yes Fe1 . N5 . 1.881(2) yes Fe1 . N6 . 1.979(2) yes N1 . C1 . 1.340(3) yes N1 . C5 . 1.363(3) yes N2 . C6 . 1.350(3) yes N2 . C10 . 1.349(3) yes N3 . C11 . 1.363(3) yes N3 . C15 . 1.346(3) yes N4 . C16 . 1.343(4) yes N4 . C20 . 1.368(3) yes N5 . C21 . 1.353(3) yes N5 . C25 . 1.348(3) yes N6 . C26 . 1.363(3) yes N6 . C30 . 1.345(3) yes N7 . N8 . 1.358(3) yes N7 . C8 . 1.369(3) yes N7 . H7 . 0.878 no N8 . C31 . 1.280(4) yes N9 . C34 . 1.331(4) yes N9 . C35 . 1.346(4) yes N10 . N11 . 1.358(3) yes N10 . C23 . 1.367(3) yes N10 . H10 . 0.878 no N11 . C37 . 1.275(4) yes N12 . C40 . 1.336(4) yes N12 . C41 . 1.335(4) yes N13 . C43 . 1.121(5) yes N14 . C45 . 1.143(6) yes N15 . C47 . 1.132(11) yes C1 . C2 . 1.383(4) yes C1 . H11 . 0.945 no C2 . C3 . 1.377(5) yes C2 . H21 . 0.943 no C3 . C4 . 1.383(5) yes C3 . H31 . 0.939 no C4 . C5 . 1.386(4) yes C4 . H41 . 0.942 no C5 . C6 . 1.473(4) yes C6 . C7 . 1.379(3) yes C7 . C8 . 1.400(4) yes C7 . H71 . 0.933 no C8 . C9 . 1.403(4) yes C9 . C10 . 1.373(3) yes C9 . H91 . 0.931 no C10 . C11 . 1.478(3) yes C11 . C12 . 1.380(4) yes C12 . C13 . 1.385(4) yes C12 . H121 . 0.946 no C13 . C14 . 1.383(4) yes C13 . H131 . 0.937 no C14 . C15 . 1.380(4) yes C14 . H141 . 0.935 no C15 . H151 . 0.942 no C16 . C17 . 1.382(4) yes C16 . H161 . 0.947 no C17 . C18 . 1.379(5) yes C17 . H171 . 0.942 no C18 . C19 . 1.383(5) yes C18 . H181 . 0.947 no C19 . C20 . 1.385(4) yes C19 . H191 . 0.938 no C20 . C21 . 1.473(4) yes C21 . C22 . 1.384(3) yes C22 . C23 . 1.396(4) yes C22 . H221 . 0.935 no C23 . C24 . 1.409(4) yes C24 . C25 . 1.377(4) yes C24 . H241 . 0.943 no C25 . C26 . 1.473(3) yes C26 . C27 . 1.393(4) yes C27 . C28 . 1.382(4) yes C27 . H271 . 0.940 no C28 . C29 . 1.383(4) yes C28 . H281 . 0.943 no C29 . C30 . 1.382(4) yes C29 . H291 . 0.945 no C30 . H301 . 0.952 no C31 . C32 . 1.464(4) yes C31 . H311 . 0.956 no C32 . C33 . 1.392(4) yes C32 . C36 . 1.389(4) yes C33 . C34 . 1.376(4) yes C33 . H331 . 0.945 no C34 . H341 . 0.946 no C35 . C36 . 1.384(4) yes C35 . H351 . 0.953 no C36 . H361 . 0.943 no C37 . C38 . 1.465(4) yes C37 . H371 . 0.951 no C38 . C39 . 1.379(4) yes C38 . C42 . 1.396(4) yes C39 . C40 . 1.384(4) yes C39 . H391 . 0.930 no C40 . H401 . 0.944 no C41 . C42 . 1.381(4) yes C41 . H411 . 0.942 no C42 . H421 . 0.953 no C43 . C44 . 1.462(7) yes C44 . H441 . 0.967 no C44 . H442 . 0.962 no C44 . H443 . 0.961 no C45 . C46 . 1.459(8) yes C46 . H461 . 0.971 no C46 . H462 . 0.977 no C46 . H463 . 0.971 no C47 . C48 . 1.466(13) yes C48 . H481 . 0.970 no C48 . H482 . 0.970 no C48 . H483 . 0.971 no P1 . F1 . 1.622(2) yes P1 . F2 . 1.581(2) yes P1 . F3 . 1.585(3) yes P1 . F4 . 1.574(3) yes P1 . F5 . 1.585(2) yes P1 . F6 . 1.576(2) yes P2 . F11 . 1.592(3) yes P2 . F12 . 1.586(2) yes P2 . F13 . 1.603(3) yes P2 . F14 . 1.541(3) yes P2 . F15 . 1.574(2) yes P2 . F16 . 1.578(3) 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 . 80.78(9) yes N1 . Fe1 . N3 . 161.57(9) yes N2 . Fe1 . N3 . 80.83(9) yes N1 . Fe1 . N4 . 88.93(9) yes N2 . Fe1 . N4 . 100.15(9) yes N3 . Fe1 . N4 . 93.00(8) yes N1 . Fe1 . N5 . 99.65(9) yes N2 . Fe1 . N5 . 179.23(9) yes N3 . Fe1 . N5 . 98.75(9) yes N4 . Fe1 . N5 . 80.51(9) yes N1 . Fe1 . N6 . 93.65(9) yes N2 . Fe1 . N6 . 98.33(9) yes N3 . Fe1 . N6 . 90.31(9) yes N4 . Fe1 . N6 . 161.52(9) yes N5 . Fe1 . N6 . 81.01(9) yes Fe1 . N1 . C1 . 126.80(19) yes Fe1 . N1 . C5 . 114.56(17) yes C1 . N1 . C5 . 118.4(2) yes Fe1 . N2 . C6 . 120.04(17) yes Fe1 . N2 . C10 . 119.80(16) yes C6 . N2 . C10 . 120.1(2) yes Fe1 . N3 . C11 . 114.77(16) yes Fe1 . N3 . C15 . 127.66(17) yes C11 . N3 . C15 . 117.6(2) yes Fe1 . N4 . C16 . 126.32(18) yes Fe1 . N4 . C20 . 115.09(17) yes C16 . N4 . C20 . 118.6(2) yes Fe1 . N5 . C21 . 120.51(18) yes Fe1 . N5 . C25 . 119.59(16) yes C21 . N5 . C25 . 119.9(2) yes Fe1 . N6 . C26 . 114.53(16) yes Fe1 . N6 . C30 . 127.70(18) yes C26 . N6 . C30 . 117.8(2) yes N8 . N7 . C8 . 121.3(2) yes N8 . N7 . H7 . 119.3 no C8 . N7 . H7 . 119.5 no N7 . N8 . C31 . 115.6(2) yes C34 . N9 . C35 . 116.3(3) yes N11 . N10 . C23 . 121.4(2) yes N11 . N10 . H10 . 119.4 no C23 . N10 . H10 . 119.2 no N10 . N11 . C37 . 115.3(3) yes C40 . N12 . C41 . 115.9(2) yes N1 . C1 . C2 . 122.5(3) yes N1 . C1 . H11 . 118.5 no C2 . C1 . H11 . 119.0 no C1 . C2 . C3 . 119.1(3) yes C1 . C2 . H21 . 119.9 no C3 . C2 . H21 . 120.9 no C2 . C3 . C4 . 119.2(3) yes C2 . C3 . H31 . 121.1 no C4 . C3 . H31 . 119.7 no C3 . C4 . C5 . 119.2(3) yes C3 . C4 . H41 . 120.3 no C5 . C4 . H41 . 120.4 no C4 . C5 . N1 . 121.5(2) yes C4 . C5 . C6 . 124.7(3) yes N1 . C5 . C6 . 113.8(2) yes C5 . C6 . N2 . 110.7(2) yes C5 . C6 . C7 . 127.4(2) yes N2 . C6 . C7 . 121.9(2) yes C6 . C7 . C8 . 118.1(2) yes C6 . C7 . H71 . 121.6 no C8 . C7 . H71 . 120.3 no C7 . C8 . N7 . 122.4(2) yes C7 . C8 . C9 . 119.7(2) yes N7 . C8 . C9 . 117.9(2) yes C8 . C9 . C10 . 118.7(2) yes C8 . C9 . H91 . 120.7 no C10 . C9 . H91 . 120.6 no C9 . C10 . N2 . 121.5(2) yes C9 . C10 . C11 . 127.1(2) yes N2 . C10 . C11 . 111.4(2) yes C10 . C11 . N3 . 113.2(2) yes C10 . C11 . C12 . 124.7(2) yes N3 . C11 . C12 . 122.1(2) yes C11 . C12 . C13 . 119.5(3) yes C11 . C12 . H121 . 120.5 no C13 . C12 . H121 . 120.0 no C12 . C13 . C14 . 118.7(3) yes C12 . C13 . H131 . 120.9 no C14 . C13 . H131 . 120.4 no C13 . C14 . C15 . 119.1(2) yes C13 . C14 . H141 . 120.7 no C15 . C14 . H141 . 120.1 no C14 . C15 . N3 . 123.0(2) yes C14 . C15 . H151 . 119.5 no N3 . C15 . H151 . 117.6 no N4 . C16 . C17 . 122.3(3) yes N4 . C16 . H161 . 118.4 no C17 . C16 . H161 . 119.4 no C16 . C17 . C18 . 119.1(3) yes C16 . C17 . H171 . 120.3 no C18 . C17 . H171 . 120.6 no C17 . C18 . C19 . 119.5(3) yes C17 . C18 . H181 . 120.3 no C19 . C18 . H181 . 120.2 no C18 . C19 . C20 . 119.1(3) yes C18 . C19 . H191 . 120.5 no C20 . C19 . H191 . 120.4 no C19 . C20 . N4 . 121.4(3) yes C19 . C20 . C21 . 125.3(2) yes N4 . C20 . C21 . 113.3(2) yes C20 . C21 . N5 . 110.5(2) yes C20 . C21 . C22 . 127.4(2) yes N5 . C21 . C22 . 122.0(2) yes C21 . C22 . C23 . 118.1(2) yes C21 . C22 . H221 . 120.6 no C23 . C22 . H221 . 121.3 no C22 . C23 . N10 . 123.2(2) yes C22 . C23 . C24 . 119.7(2) yes N10 . C23 . C24 . 117.1(2) yes C23 . C24 . C25 . 118.6(3) yes C23 . C24 . H241 . 120.9 no C25 . C24 . H241 . 120.5 no C24 . C25 . N5 . 121.7(2) yes C24 . C25 . C26 . 126.7(2) yes N5 . C25 . C26 . 111.6(2) yes C25 . C26 . N6 . 113.3(2) yes C25 . C26 . C27 . 124.7(2) yes N6 . C26 . C27 . 122.0(2) yes C26 . C27 . C28 . 119.2(3) yes C26 . C27 . H271 . 120.2 no C28 . C27 . H271 . 120.6 no C27 . C28 . C29 . 119.0(3) yes C27 . C28 . H281 . 120.9 no C29 . C28 . H281 . 120.1 no C28 . C29 . C30 . 119.2(2) yes C28 . C29 . H291 . 119.9 no C30 . C29 . H291 . 120.9 no C29 . C30 . N6 . 122.9(2) yes C29 . C30 . H301 . 119.7 no N6 . C30 . H301 . 117.4 no N8 . C31 . C32 . 120.8(3) yes N8 . C31 . H311 . 120.6 no C32 . C31 . H311 . 118.5 no C31 . C32 . C33 . 119.4(3) yes C31 . C32 . C36 . 123.0(3) yes C33 . C32 . C36 . 117.6(3) yes C32 . C33 . C34 . 119.1(3) yes C32 . C33 . H331 . 120.6 no C34 . C33 . H331 . 120.3 no C33 . C34 . N9 . 124.3(3) yes C33 . C34 . H341 . 119.4 no N9 . C34 . H341 . 116.2 no N9 . C35 . C36 . 123.7(3) yes N9 . C35 . H351 . 118.3 no C36 . C35 . H351 . 118.0 no C32 . C36 . C35 . 119.0(3) yes C32 . C36 . H361 . 120.2 no C35 . C36 . H361 . 120.8 no N11 . C37 . C38 . 121.3(3) yes N11 . C37 . H371 . 119.9 no C38 . C37 . H371 . 118.7 no C37 . C38 . C39 . 122.9(2) yes C37 . C38 . C42 . 119.2(3) yes C39 . C38 . C42 . 117.8(3) yes C38 . C39 . C40 . 119.3(3) yes C38 . C39 . H391 . 119.9 no C40 . C39 . H391 . 120.8 no C39 . C40 . N12 . 124.0(3) yes C39 . C40 . H401 . 118.3 no N12 . C40 . H401 . 117.7 no N12 . C41 . C42 . 124.8(3) yes N12 . C41 . H411 . 116.8 no C42 . C41 . H411 . 118.5 no C38 . C42 . C41 . 118.2(3) yes C38 . C42 . H421 . 120.4 no C41 . C42 . H421 . 121.3 no N13 . C43 . C44 . 178.3(5) yes C43 . C44 . H441 . 107.5 no C43 . C44 . H442 . 106.7 no H441 . C44 . H442 . 110.9 no C43 . C44 . H443 . 109.4 no H441 . C44 . H443 . 111.1 no H442 . C44 . H443 . 111.0 no N14 . C45 . C46 . 176.0(6) yes C45 . C46 . H461 . 105.7 no C45 . C46 . H462 . 110.6 no H461 . C46 . H462 . 109.9 no C45 . C46 . H463 . 110.2 no H461 . C46 . H463 . 109.8 no H462 . C46 . H463 . 110.6 no N15 . C47 . C48 . 168.0(12) yes C47 . C48 . H481 . 111.8 no C47 . C48 . H482 . 108.8 no H481 . C48 . H482 . 109.5 no C47 . C48 . H483 . 107.7 no H481 . C48 . H483 . 109.4 no H482 . C48 . H483 . 109.5 no F1 . P1 . F2 . 178.57(14) yes F1 . P1 . F3 . 87.23(14) yes F2 . P1 . F3 . 91.42(15) yes F1 . P1 . F4 . 89.85(13) yes F2 . P1 . F4 . 91.50(15) yes F3 . P1 . F4 . 177.02(16) yes F1 . P1 . F5 . 89.46(13) yes F2 . P1 . F5 . 90.99(13) yes F3 . P1 . F5 . 89.62(18) yes F4 . P1 . F5 . 89.73(16) yes F1 . P1 . F6 . 89.21(12) yes F2 . P1 . F6 . 90.36(13) yes F3 . P1 . F6 . 91.22(19) yes F4 . P1 . F6 . 89.37(19) yes F5 . P1 . F6 . 178.40(16) yes F11 . P2 . F12 . 177.04(18) yes F11 . P2 . F13 . 89.69(18) yes F12 . P2 . F13 . 87.78(15) yes F11 . P2 . F14 . 89.2(2) yes F12 . P2 . F14 . 93.35(18) yes F13 . P2 . F14 . 178.38(19) yes F11 . P2 . F15 . 89.55(15) yes F12 . P2 . F15 . 91.88(14) yes F13 . P2 . F15 . 87.21(16) yes F14 . P2 . F15 . 91.6(2) yes F11 . P2 . F16 . 90.30(16) yes F12 . P2 . F16 . 88.14(16) yes F13 . P2 . F16 . 89.8(2) yes F14 . P2 . F16 . 91.4(3) yes F15 . P2 . F16 . 177.0(2) yes # Attachment 'Fe_H2__2__JZ.CIF' data_jb1167 _database_code_depnum_ccdc_archive 'CCDC 692939' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H33 Fe N12, 3(F6 P), 3.5(C2 H3 N), 2.5(H2 O)' _chemical_formula_sum 'C49 H48.50 F18 Fe N15.50 O2.50 P3' _chemical_formula_weight 1385.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8794(18) _cell_length_b 16.055(3) _cell_length_c 23.710(5) _cell_angle_alpha 105.43(3) _cell_angle_beta 91.68(3) _cell_angle_gamma 97.54(3) _cell_volume 3222.7(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1398 _exptl_absorpt_coefficient_mu 0.411 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28413 _diffrn_reflns_av_R_equivalents 0.0753 _diffrn_reflns_av_sigmaI/netI 0.0632 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.05 _reflns_number_total 11375 _reflns_number_gt 8715 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1403P)^2^+7.9641P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11375 _refine_ls_number_parameters 983 _refine_ls_number_restraints 67 _refine_ls_R_factor_all 0.1226 _refine_ls_R_factor_gt 0.0952 _refine_ls_wR_factor_ref 0.2723 _refine_ls_wR_factor_gt 0.2477 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.91430(7) 0.73245(4) 0.87157(3) 0.0284(2) Uani 1 1 d . . . N1 N 0.6954(4) 0.6861(3) 0.85978(17) 0.0293(8) Uani 1 1 d . . . C1 C 0.6024(5) 0.6722(3) 0.9005(2) 0.0338(11) Uani 1 1 d . . . H1A H 0.6448 0.6800 0.9391 0.041 Uiso 1 1 calc R . . N2 N 0.8846(5) 0.7250(3) 0.79113(18) 0.0336(9) Uani 1 1 d . . . C2 C 0.4473(6) 0.6472(4) 0.8891(2) 0.0400(12) Uani 1 1 d . . . H2A H 0.3837 0.6395 0.9194 0.048 Uiso 1 1 calc R . . N3 N 1.1211(4) 0.7820(3) 0.85701(18) 0.0336(9) Uani 1 1 d . . . C3 C 0.3869(6) 0.6336(4) 0.8324(3) 0.0429(13) Uani 1 1 d . . . H3A H 0.2809 0.6150 0.8231 0.052 Uiso 1 1 calc R . . C4 C 0.4803(6) 0.6469(4) 0.7897(2) 0.0371(11) Uani 1 1 d . . . H4A H 0.4397 0.6383 0.7507 0.045 Uiso 1 1 calc R . . N4 N 0.8288(7) 0.6934(5) 0.6132(2) 0.080(2) Uani 1 1 d . . . H4B H 0.9084 0.7067 0.5944 0.096 Uiso 1 1 calc R . . C5 C 0.6350(5) 0.6733(3) 0.8041(2) 0.0313(10) Uani 1 1 d . . . N5 N 0.6902(7) 0.6631(5) 0.5836(2) 0.0711(18) Uani 1 1 d . . . C6 C 0.7463(6) 0.6920(3) 0.7627(2) 0.0339(11) Uani 1 1 d . . . N6 N 0.3829(12) 0.6088(5) 0.4086(3) 0.093(3) Uani 1 1 d . . . H6 H 0.389(14) 0.610(8) 0.369(6) 0.140 Uiso 1 1 d . . . N7 N 0.9771(4) 0.6158(3) 0.86395(18) 0.0317(9) Uani 1 1 d . . . C7 C 0.7219(6) 0.6799(4) 0.7034(2) 0.0450(13) Uani 1 1 d . . . H7A H 0.6242 0.6563 0.6842 0.054 Uiso 1 1 calc R . . C8 C 0.8437(7) 0.7030(5) 0.6717(3) 0.0545(16) Uani 1 1 d . . . N8 N 0.9509(4) 0.7401(3) 0.95173(17) 0.0300(8) Uani 1 1 d . . . N9 N 0.8584(5) 0.8495(3) 0.90644(18) 0.0327(9) Uani 1 1 d . . . C9 C 0.9856(7) 0.7385(5) 0.7020(3) 0.0539(16) Uani 1 1 d . . . H9A H 1.0693 0.7562 0.6817 0.065 Uiso 1 1 calc R . . C10 C 1.0029(6) 0.7475(4) 0.7609(2) 0.0410(12) Uani 1 1 d . . . N10 N 1.0875(6) 0.7756(3) 1.1254(2) 0.0502(12) Uani 1 1 d . . . H10D H 1.0669 0.8220 1.1518 0.060 Uiso 1 1 calc R . . N11 N 1.1664(5) 0.7179(3) 1.14177(19) 0.0414(11) Uani 1 1 d . . . C11 C 1.1410(6) 0.7843(4) 0.8010(2) 0.0382(12) Uani 1 1 d . . . N12 N 1.3632(8) 0.6200(4) 1.2968(2) 0.0675(17) Uani 1 1 d . . . C12 C 1.2770(6) 0.8197(4) 0.7846(3) 0.0486(14) Uani 1 1 d . . . H12A H 1.2883 0.8197 0.7449 0.058 Uiso 1 1 calc R . . C13 C 1.3979(7) 0.8556(4) 0.8266(3) 0.0528(15) Uani 1 1 d . . . H13A H 1.4922 0.8807 0.8160 0.063 Uiso 1 1 calc R . . C14 C 1.3774(6) 0.8538(4) 0.8837(3) 0.0474(14) Uani 1 1 d . . . H14A H 1.4575 0.8782 0.9133 0.057 Uiso 1 1 calc R . . C15 C 1.2395(6) 0.8161(4) 0.8975(2) 0.0400(12) Uani 1 1 d . . . H15A H 1.2272 0.8140 0.9367 0.048 Uiso 1 1 calc R . . C16 C 0.6830(10) 0.6578(7) 0.5287(3) 0.086(3) Uani 1 1 d . . . H16A H 0.7712 0.6724 0.5097 0.103 Uiso 1 1 calc R . . C17 C 0.5331(10) 0.6282(6) 0.4960(3) 0.079(2) Uani 1 1 d . . . C18 C 0.5182(12) 0.6343(6) 0.4390(3) 0.084(3) Uani 1 1 d . . . H18A H 0.6037 0.6566 0.4215 0.101 Uiso 1 1 calc R . . C19 C 0.2621(15) 0.5756(8) 0.4305(4) 0.110(4) Uani 1 1 d . . . H19A H 0.1687 0.5569 0.4072 0.132 Uiso 1 1 calc R . . C20 C 0.2703(13) 0.5680(8) 0.4859(4) 0.119(4) Uani 1 1 d . . . H20A H 0.1828 0.5447 0.5018 0.143 Uiso 1 1 calc R . . C21 C 0.4072(12) 0.5943(8) 0.5192(4) 0.110(4) Uani 1 1 d . . . H21A H 0.4141 0.5889 0.5581 0.132 Uiso 1 1 calc R . . C22 C 0.9826(5) 0.5513(3) 0.8149(2) 0.0373(11) Uani 1 1 d . . . H22A H 0.9466 0.5588 0.7787 0.045 Uiso 1 1 calc R . . C23 C 1.0381(6) 0.4742(4) 0.8142(3) 0.0454(13) Uani 1 1 d . . . H23A H 1.0400 0.4303 0.7784 0.054 Uiso 1 1 calc R . . C24 C 1.0905(6) 0.4626(4) 0.8666(3) 0.0461(13) Uani 1 1 d . . . H24A H 1.1294 0.4105 0.8673 0.055 Uiso 1 1 calc R . . C25 C 1.0857(6) 0.5274(3) 0.9177(2) 0.0400(12) Uani 1 1 d . . . H25A H 1.1218 0.5204 0.9540 0.048 Uiso 1 1 calc R . . C26 C 1.0278(5) 0.6033(3) 0.9159(2) 0.0329(10) Uani 1 1 d . . . C27 C 1.0158(5) 0.6766(3) 0.9673(2) 0.0303(10) Uani 1 1 d . . . C28 C 1.0628(6) 0.6856(4) 1.0249(2) 0.0382(11) Uani 1 1 d . . . H28A H 1.1097 0.6415 1.0353 0.046 Uiso 1 1 calc R . . C29 C 1.0399(6) 0.7611(4) 1.0674(2) 0.0366(11) Uani 1 1 d . . . C30 C 0.9673(6) 0.8251(4) 1.0511(2) 0.0378(11) Uani 1 1 d . . . H30A H 0.9466 0.8756 1.0796 0.045 Uiso 1 1 calc R . . C31 C 0.9274(5) 0.8122(3) 0.9926(2) 0.0315(10) Uani 1 1 d . . . C32 C 0.8625(5) 0.8746(3) 0.9659(2) 0.0326(10) Uani 1 1 d . . . C33 C 0.8104(6) 0.9498(4) 0.9973(2) 0.0402(12) Uani 1 1 d . . . H33A H 0.8134 0.9647 1.0390 0.048 Uiso 1 1 calc R . . C34 C 0.7538(6) 1.0031(4) 0.9669(3) 0.0450(13) Uani 1 1 d . . . H34A H 0.7145 1.0543 0.9871 0.054 Uiso 1 1 calc R . . C35 C 0.7559(6) 0.9801(3) 0.9060(3) 0.0432(13) Uani 1 1 d . . . H35A H 0.7219 1.0168 0.8843 0.052 Uiso 1 1 calc R . . C36 C 0.8079(6) 0.9035(3) 0.8775(2) 0.0371(11) Uani 1 1 d . . . H36A H 0.8082 0.8883 0.8360 0.045 Uiso 1 1 calc R . . C37 C 1.1920(6) 0.7297(4) 1.1966(2) 0.0439(13) Uani 1 1 d . . . H37A H 1.1543 0.7758 1.2240 0.053 Uiso 1 1 calc R . . C38 C 1.2808(6) 0.6707(4) 1.2169(2) 0.0419(13) Uani 1 1 d . . . C39 C 1.2860(8) 0.6730(5) 1.2761(3) 0.0576(17) Uani 1 1 d . . . H39A H 1.2335 0.7131 1.3024 0.069 Uiso 1 1 calc R . . C40 C 1.4354(10) 0.5637(5) 1.2602(3) 0.071(2) Uani 1 1 d . . . H40A H 1.4901 0.5264 1.2752 0.085 Uiso 1 1 calc R . . C41 C 1.4342(9) 0.5572(5) 1.2012(3) 0.0626(18) Uani 1 1 d . . . H41A H 1.4869 0.5158 1.1760 0.075 Uiso 1 1 calc R . . C42 C 1.3560(7) 0.6112(4) 1.1789(3) 0.0479(14) Uani 1 1 d . . . H42A H 1.3536 0.6077 1.1382 0.057 Uiso 1 1 calc R . . P1 P 1.3488(4) 0.9875(2) 1.26261(13) 0.1138(11) Uani 1 1 d . . . F11 F 1.4120(16) 0.9551(8) 1.2009(4) 0.217(6) Uani 1 1 d . . . F12 F 1.5093(11) 1.0414(9) 1.2868(5) 0.215(5) Uani 1 1 d . . . F13 F 1.3959(13) 0.9033(8) 1.2753(5) 0.213(5) Uani 1 1 d . . . F14 F 1.2956(13) 1.0226(10) 1.3233(4) 0.219(6) Uani 1 1 d . . . F15 F 1.3068(8) 1.0684(4) 1.2447(3) 0.120(2) Uani 1 1 d . . . F16 F 1.1903(10) 0.9369(5) 1.2356(6) 0.201(5) Uani 1 1 d . . . P2 P 0.8320(5) 0.5161(9) 0.3460(2) 0.068(2) Uani 0.555(18) 1 d P A 1 P2' P 0.8202(8) 0.4663(8) 0.3486(3) 0.056(3) Uani 0.445(18) 1 d P A 2 F21 F 0.839(3) 0.5983(16) 0.3934(9) 0.178(10) Uani 0.555(18) 1 d P A 1 F21' F 0.8373(18) 0.5414(17) 0.4101(6) 0.113(8) Uani 0.445(18) 1 d P A 2 F22' F 0.762(2) 0.5364(17) 0.3013(11) 0.116(9) Uani 0.445(18) 1 d P A 2 F22 F 0.775(3) 0.557(3) 0.3091(15) 0.216(17) Uani 0.555(18) 1 d P A 1 F23 F 0.9966(9) 0.5488(12) 0.3309(4) 0.092(5) Uani 0.555(18) 1 d P A 1 F23' F 0.9926(13) 0.4774(16) 0.3395(8) 0.119(9) Uani 0.445(18) 1 d P A 2 F24 F 0.824(2) 0.4299(18) 0.2917(9) 0.139(10) Uani 0.555(18) 1 d P A 1 F24' F 0.8022(17) 0.3922(17) 0.2916(9) 0.099(8) Uani 0.445(18) 1 d P A 2 F25 F 0.6547(6) 0.4689(5) 0.3585(2) 0.110(2) Uani 0.555(18) 1 d P A 1 F25' F 0.6547(6) 0.4689(5) 0.3585(2) 0.110(2) Uani 0.445(18) 1 d P A 2 F26 F 0.9078(15) 0.4674(18) 0.3887(7) 0.138(8) Uani 0.555(18) 1 d P A 1 F26' F 0.846(3) 0.3995(19) 0.3831(8) 0.144(10) Uani 0.445(18) 1 d P A 2 P3 P 0.5000 0.5000 1.0000 0.0483(5) Uani 1 2 d S . . F31 F 0.6526(6) 0.5485(4) 0.9851(3) 0.108(2) Uani 1 1 d . . . F32 F 0.4238(6) 0.5866(3) 1.01016(19) 0.0863(15) Uani 1 1 d . . . F33 F 0.4414(6) 0.4742(3) 0.93291(17) 0.0810(14) Uani 1 1 d . . . N100 N 0.8666(11) 0.9823(6) 1.1582(4) 0.102(3) Uani 1 1 d . . . C100 C 0.8709(18) 1.0072(9) 1.2698(5) 0.140(5) Uani 1 1 d . . . H10A H 0.9303 0.9665 1.2815 0.210 Uiso 1 1 calc R . . H10B H 0.7664 0.9977 1.2814 0.210 Uiso 1 1 calc R . . H10C H 0.9173 1.0673 1.2891 0.210 Uiso 1 1 calc R . . C101 C 0.8688(13) 0.9924(6) 1.2067(5) 0.095(3) Uani 1 1 d . . . P4 P 0.5876(12) 0.8799(5) 0.4398(4) 0.175(5) Uani 0.50 1 d PD . . F41 F 0.717(3) 0.8267(10) 0.4529(12) 0.271(15) Uani 0.50 1 d PD . . F42 F 0.4639(19) 0.9394(14) 0.4365(8) 0.217(11) Uani 0.50 1 d PD . . F43 F 0.525(3) 0.8524(15) 0.4948(8) 0.256(12) Uiso 0.50 1 d PD . . F44 F 0.490(3) 0.7993(10) 0.3965(7) 0.270(17) Uani 0.50 1 d PD . . F45 F 0.676(4) 0.959(2) 0.4908(10) 0.335(18) Uiso 0.50 1 d PD . . F46 F 0.677(3) 0.9122(17) 0.3909(10) 0.267(13) Uani 0.50 1 d PDU . . N300 N 0.4399(10) 0.8270(5) 1.0235(3) 0.091(2) Uani 1 1 d . . . C300 C 0.5629(9) 0.7822(6) 1.1086(4) 0.074(2) Uani 1 1 d . . . H30B H 0.5592 0.7186 1.0981 0.111 Uiso 1 1 calc R . . H30C H 0.5080 0.8010 1.1440 0.111 Uiso 1 1 calc R . . H30D H 0.6692 0.8101 1.1160 0.111 Uiso 1 1 calc R . . C301 C 0.4926(8) 0.8070(5) 1.0610(3) 0.0609(17) Uani 1 1 d . . . C201 C 0.7744(10) 0.7639(6) 0.2598(7) 0.115(5) Uani 1 1 d . . . N200 N 0.8296(13) 0.7599(11) 0.2125(6) 0.172(6) Uani 1 1 d . . . C200 C 0.678(2) 0.7716(17) 0.2994(10) 0.271(15) Uani 1 1 d . . . H20B H 0.7249 0.7650 0.3355 0.406 Uiso 1 1 calc R . . H20C H 0.5892 0.7262 0.2858 0.406 Uiso 1 1 calc R . . H20D H 0.6448 0.8293 0.3070 0.406 Uiso 1 1 calc R . . O1 O 1.0185(14) 0.8016(8) 0.4145(6) 0.092(4) Uani 0.50 1 d P B 3 C500 C 0.955(6) 0.990(4) 0.5812(17) 0.14(3) Uani 0.25 1 d P C 1 C501 C 0.867(5) 0.929(3) 0.5632(16) 0.111(15) Uani 0.25 1 d PD C 1 H50A H 0.7660 0.9470 0.5603 0.167 Uiso 0.25 1 calc PR C 1 H50B H 0.8653 0.8914 0.5897 0.167 Uiso 0.25 1 calc PR C 1 H50C H 0.8924 0.8970 0.5243 0.167 Uiso 0.25 1 calc PR C 1 N500 N 1.058(7) 1.023(4) 0.5943(14) 0.20(3) Uani 0.25 1 d PD C 1 N400 N 1.115(5) 0.766(3) 0.5718(18) 0.090(11) Uani 0.25 1 d PU D 1 C401 C 1.235(3) 0.823(2) 0.5773(11) 0.062(9) Uani 0.25 1 d P D 1 C400 C 1.396(4) 0.857(2) 0.5687(12) 0.076(10) Uani 0.25 1 d P D 1 H40B H 1.4184 0.9188 0.5894 0.113 Uiso 0.25 1 calc PR D 1 H40C H 1.4085 0.8485 0.5268 0.113 Uiso 0.25 1 calc PR D 1 H40D H 1.4656 0.8244 0.5843 0.113 Uiso 0.25 1 calc PR D 1 O1' O 1.149(4) 0.770(2) 0.4187(13) 0.118(11) Uani 0.25 1 d P E 4 O2 O 1.043(3) 0.718(2) 0.5209(13) 0.103(9) Uani 0.25 1 d P F 3 O3 O 1.453(6) 0.789(2) 0.6182(15) 0.18(2) Uani 0.25 1 d P G 3 O2" O 1.084(3) 0.8789(19) 0.4617(13) 0.105(9) Uani 0.25 1 d P H 5 O2' O 1.031(4) 0.750(2) 0.4712(15) 0.127(10) Uani 0.25 1 d PU I 6 O1" O 1.058(4) 0.847(2) 0.3630(17) 0.127(12) Uani 0.25 1 d P J 5 O3' O 1.130(6) 0.810(3) 0.586(2) 0.119(13) Uani 0.25 1 d PU K 4 O3" O 1.347(5) 0.820(2) 0.6146(16) 0.130(11) Uani 0.25 1 d PU L 5 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 0.0266(4) 0.0323(4) 0.0253(4) 0.0097(3) -0.0073(2) -0.0009(3) N1 0.029(2) 0.029(2) 0.029(2) 0.0084(16) -0.0070(16) 0.0018(15) C1 0.032(2) 0.037(3) 0.034(3) 0.015(2) -0.004(2) 0.003(2) N2 0.031(2) 0.039(2) 0.030(2) 0.0140(18) -0.0083(16) -0.0032(17) C2 0.032(3) 0.049(3) 0.045(3) 0.022(3) 0.003(2) 0.009(2) N3 0.029(2) 0.039(2) 0.031(2) 0.0105(18) -0.0066(16) -0.0025(17) C3 0.026(2) 0.051(3) 0.053(3) 0.020(3) -0.008(2) 0.004(2) C4 0.031(3) 0.044(3) 0.035(3) 0.011(2) -0.011(2) 0.001(2) N4 0.053(3) 0.150(7) 0.041(3) 0.045(4) -0.010(2) -0.011(4) C5 0.030(2) 0.032(2) 0.032(2) 0.012(2) -0.0087(19) 0.0026(19) N5 0.066(4) 0.115(5) 0.034(3) 0.037(3) -0.018(2) -0.011(3) C6 0.034(3) 0.040(3) 0.029(2) 0.015(2) -0.0084(19) -0.001(2) N6 0.154(8) 0.079(5) 0.043(4) 0.020(3) -0.055(5) 0.012(5) N7 0.0254(19) 0.035(2) 0.030(2) 0.0045(17) -0.0064(15) 0.0000(16) C7 0.035(3) 0.063(4) 0.036(3) 0.019(3) -0.013(2) -0.006(2) C8 0.048(3) 0.083(5) 0.033(3) 0.025(3) -0.009(2) -0.003(3) N8 0.029(2) 0.033(2) 0.027(2) 0.0094(17) -0.0063(15) 0.0020(16) N9 0.032(2) 0.031(2) 0.035(2) 0.0131(17) -0.0104(17) -0.0025(16) C9 0.041(3) 0.080(5) 0.042(3) 0.027(3) -0.005(2) -0.005(3) C10 0.032(3) 0.054(3) 0.037(3) 0.019(2) -0.008(2) -0.005(2) N10 0.069(3) 0.058(3) 0.027(2) 0.012(2) -0.002(2) 0.024(3) N11 0.049(3) 0.050(3) 0.029(2) 0.018(2) -0.0065(19) 0.007(2) C11 0.032(3) 0.045(3) 0.035(3) 0.012(2) -0.008(2) -0.002(2) N12 0.100(5) 0.064(4) 0.036(3) 0.017(3) -0.037(3) 0.001(3) C12 0.036(3) 0.067(4) 0.044(3) 0.026(3) -0.001(2) -0.007(3) C13 0.034(3) 0.063(4) 0.061(4) 0.025(3) -0.004(3) -0.010(3) C14 0.032(3) 0.047(3) 0.057(4) 0.011(3) -0.012(2) -0.006(2) C15 0.033(3) 0.046(3) 0.036(3) 0.009(2) -0.010(2) -0.004(2) C16 0.079(5) 0.141(8) 0.042(4) 0.048(5) -0.018(4) -0.013(5) C17 0.091(6) 0.113(7) 0.034(3) 0.035(4) -0.027(4) -0.003(5) C18 0.124(7) 0.093(6) 0.033(4) 0.024(4) -0.030(4) 0.002(5) C19 0.125(9) 0.124(9) 0.075(6) 0.040(6) -0.065(6) -0.017(7) C20 0.104(7) 0.164(11) 0.084(7) 0.061(7) -0.057(6) -0.044(7) C21 0.096(7) 0.175(11) 0.059(5) 0.061(6) -0.044(5) -0.035(7) C22 0.030(2) 0.040(3) 0.037(3) 0.007(2) -0.009(2) -0.002(2) C23 0.039(3) 0.040(3) 0.045(3) -0.005(2) -0.007(2) 0.002(2) C24 0.042(3) 0.037(3) 0.057(4) 0.010(3) -0.008(3) 0.007(2) C25 0.038(3) 0.036(3) 0.046(3) 0.013(2) -0.009(2) 0.005(2) C26 0.029(2) 0.035(3) 0.034(3) 0.010(2) -0.0069(19) -0.0010(19) C27 0.031(2) 0.030(2) 0.032(2) 0.013(2) -0.0056(19) 0.0024(18) C28 0.037(3) 0.045(3) 0.035(3) 0.017(2) -0.005(2) 0.004(2) C29 0.038(3) 0.045(3) 0.028(2) 0.014(2) -0.008(2) 0.004(2) C30 0.044(3) 0.040(3) 0.027(2) 0.007(2) -0.004(2) 0.007(2) C31 0.031(2) 0.032(3) 0.031(2) 0.011(2) -0.0052(19) 0.0015(19) C32 0.031(2) 0.032(3) 0.034(3) 0.011(2) -0.0076(19) 0.0024(19) C33 0.042(3) 0.039(3) 0.036(3) 0.007(2) -0.011(2) 0.005(2) C34 0.044(3) 0.036(3) 0.052(3) 0.010(2) -0.014(2) 0.005(2) C35 0.044(3) 0.033(3) 0.053(3) 0.016(2) -0.017(2) 0.001(2) C36 0.032(2) 0.043(3) 0.039(3) 0.020(2) -0.007(2) -0.002(2) C37 0.048(3) 0.060(4) 0.026(3) 0.014(2) -0.003(2) 0.011(3) C38 0.051(3) 0.047(3) 0.025(2) 0.011(2) -0.014(2) -0.001(2) C39 0.077(4) 0.063(4) 0.030(3) 0.011(3) -0.014(3) 0.009(3) C40 0.102(6) 0.052(4) 0.054(4) 0.010(3) -0.038(4) 0.011(4) C41 0.079(5) 0.054(4) 0.054(4) 0.012(3) -0.019(3) 0.017(3) C42 0.058(4) 0.049(3) 0.035(3) 0.014(3) -0.012(3) 0.001(3) P1 0.128(2) 0.142(3) 0.0857(19) 0.0720(19) -0.0252(17) -0.007(2) F11 0.360(16) 0.235(11) 0.107(6) 0.059(6) 0.026(7) 0.194(11) F12 0.120(7) 0.302(14) 0.195(10) 0.052(9) -0.038(6) -0.031(8) F13 0.222(10) 0.218(10) 0.257(12) 0.178(10) -0.055(9) 0.023(8) F14 0.212(10) 0.365(17) 0.123(7) 0.133(9) 0.069(7) 0.040(10) F15 0.150(6) 0.105(4) 0.116(5) 0.049(4) 0.008(4) 0.017(4) F16 0.132(7) 0.103(5) 0.352(15) 0.052(7) -0.066(8) 0.002(5) P2 0.045(2) 0.106(6) 0.049(2) 0.026(3) -0.0129(15) -0.009(3) P2' 0.044(2) 0.080(6) 0.034(2) -0.003(3) -0.0169(17) 0.014(3) F21 0.171(16) 0.168(18) 0.144(16) -0.010(13) 0.070(12) -0.062(14) F21' 0.079(9) 0.168(19) 0.055(8) -0.034(9) -0.021(6) 0.025(11) F22' 0.056(9) 0.130(14) 0.122(16) -0.029(13) -0.017(9) 0.011(8) F22 0.123(17) 0.34(4) 0.24(3) 0.21(3) 0.037(18) -0.01(2) F23 0.044(4) 0.165(13) 0.057(5) 0.039(6) -0.025(3) -0.029(6) F23' 0.046(6) 0.163(18) 0.104(12) -0.035(12) -0.016(7) 0.005(8) F24 0.114(11) 0.22(2) 0.063(9) 0.030(12) 0.011(7) -0.044(12) F24' 0.046(7) 0.153(17) 0.077(10) -0.023(10) -0.029(7) 0.051(10) F25 0.067(3) 0.196(7) 0.077(3) 0.049(4) 0.008(2) 0.023(3) F25' 0.067(3) 0.196(7) 0.077(3) 0.049(4) 0.008(2) 0.023(3) F26 0.080(8) 0.25(2) 0.109(10) 0.120(14) -0.033(7) -0.017(11) F26' 0.16(2) 0.21(2) 0.100(12) 0.083(15) 0.023(12) 0.102(18) P3 0.0629(14) 0.0558(13) 0.0353(11) 0.0221(10) -0.0014(9) 0.0217(11) F31 0.078(3) 0.147(5) 0.125(5) 0.091(4) 0.001(3) -0.002(3) F32 0.133(4) 0.076(3) 0.063(3) 0.024(2) -0.008(3) 0.057(3) F33 0.120(4) 0.088(3) 0.042(2) 0.022(2) -0.019(2) 0.039(3) N100 0.118(7) 0.090(6) 0.084(6) -0.004(4) 0.030(5) 0.021(5) C100 0.204(15) 0.134(11) 0.085(8) 0.012(7) 0.019(8) 0.071(10) C101 0.123(8) 0.073(6) 0.076(6) -0.002(5) 0.012(6) 0.014(5) P4 0.251(12) 0.102(5) 0.158(8) 0.009(5) 0.097(8) 0.009(7) F41 0.40(4) 0.069(10) 0.35(4) 0.061(15) -0.02(3) 0.066(16) F42 0.165(16) 0.33(3) 0.22(2) 0.16(2) 0.001(14) 0.124(19) F44 0.45(4) 0.140(15) 0.186(18) 0.079(14) -0.19(2) -0.10(2) F46 0.284(15) 0.267(15) 0.260(15) 0.096(10) 0.015(10) 0.021(10) N300 0.132(7) 0.078(5) 0.068(4) 0.020(4) -0.021(4) 0.039(5) C300 0.063(4) 0.089(6) 0.074(5) 0.034(4) -0.008(4) 0.007(4) C301 0.062(4) 0.062(4) 0.060(4) 0.015(3) 0.000(3) 0.015(3) C201 0.053(5) 0.059(5) 0.204(13) -0.004(6) 0.031(7) -0.012(4) N200 0.103(8) 0.280(18) 0.169(12) 0.082(12) 0.033(8) 0.108(10) C200 0.144(15) 0.29(3) 0.27(3) -0.09(2) 0.107(17) -0.049(16) O1 0.085(8) 0.083(8) 0.093(9) -0.003(7) 0.021(7) 0.011(7) C500 0.16(4) 0.14(4) 0.05(2) -0.04(2) 0.05(2) -0.09(3) C501 0.12(3) 0.12(3) 0.06(2) -0.03(2) 0.02(2) 0.01(3) N500 0.33(8) 0.19(5) 0.040(19) 0.04(3) 0.02(3) -0.09(5) N400 0.095(17) 0.096(18) 0.085(17) 0.047(15) 0.030(14) -0.014(14) C401 0.017(10) 0.13(3) 0.049(14) 0.048(16) 0.010(9) -0.007(12) C400 0.074(19) 0.09(2) 0.044(14) 0.010(14) 0.018(13) -0.040(17) O1' 0.16(3) 0.12(2) 0.097(19) 0.041(17) -0.011(18) 0.09(2) O2 0.070(15) 0.16(3) 0.095(19) 0.07(2) 0.006(13) 0.023(16) O3 0.27(5) 0.13(3) 0.11(2) -0.06(2) -0.03(3) 0.15(3) O2" 0.11(2) 0.096(19) 0.11(2) 0.025(16) -0.019(16) 0.017(16) O2' 0.143(18) 0.117(17) 0.110(16) 0.021(13) 0.056(14) -0.017(14) O1" 0.11(2) 0.12(2) 0.19(3) 0.11(3) 0.05(2) 0.050(19) O3' 0.14(2) 0.105(19) 0.13(2) 0.050(16) 0.038(16) 0.039(16) O3" 0.139(19) 0.112(17) 0.125(18) 0.024(15) -0.011(15) -0.015(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.887(4) . ? Fe1 N8 1.887(4) . ? Fe1 N1 1.971(4) . ? Fe1 N9 1.976(4) . ? Fe1 N3 1.981(4) . ? Fe1 N7 1.988(4) . ? N1 C1 1.333(6) . ? N1 C5 1.364(6) . ? C1 C2 1.381(7) . ? C1 H1A 0.9500 . ? N2 C10 1.353(7) . ? N2 C6 1.354(6) . ? C2 C3 1.383(8) . ? C2 H2A 0.9500 . ? N3 C15 1.355(6) . ? N3 C11 1.355(7) . ? C3 C4 1.371(8) . ? C3 H3A 0.9500 . ? C4 C5 1.387(7) . ? C4 H4A 0.9500 . ? N4 C8 1.354(8) . ? N4 N5 1.362(8) . ? N4 H4B 0.8800 . ? C5 C6 1.471(7) . ? N5 C16 1.281(8) . ? C6 C7 1.374(7) . ? N6 C19 1.316(14) . ? N6 C18 1.339(12) . ? N6 H6 0.95(13) . ? N7 C22 1.343(7) . ? N7 C26 1.372(6) . ? C7 C8 1.401(8) . ? C7 H7A 0.9500 . ? C8 C9 1.403(8) . ? N8 C31 1.342(7) . ? N8 C27 1.361(6) . ? N9 C36 1.351(6) . ? N9 C32 1.356(6) . ? C9 C10 1.368(8) . ? C9 H9A 0.9500 . ? C10 C11 1.482(7) . ? N10 N11 1.358(6) . ? N10 C29 1.376(7) . ? N10 H10D 0.8800 . ? N11 C37 1.273(7) . ? C11 C12 1.377(8) . ? N12 C40 1.322(10) . ? N12 C39 1.337(9) . ? C12 C13 1.394(8) . ? C12 H12A 0.9500 . ? C13 C14 1.381(9) . ? C13 H13A 0.9500 . ? C14 C15 1.380(8) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.475(11) . ? C16 H16A 0.9500 . ? C17 C21 1.372(13) . ? C17 C18 1.386(9) . ? C18 H18A 0.9500 . ? C19 C20 1.352(14) . ? C19 H19A 0.9500 . ? C20 C21 1.381(11) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.386(8) . ? C22 H22A 0.9500 . ? C23 C24 1.380(8) . ? C23 H23A 0.9500 . ? C24 C25 1.377(8) . ? C24 H24A 0.9500 . ? C25 C26 1.394(7) . ? C25 H25A 0.9500 . ? C26 C27 1.470(7) . ? C27 C28 1.379(7) . ? C28 C29 1.398(8) . ? C28 H28A 0.9500 . ? C29 C30 1.412(7) . ? C30 C31 1.375(7) . ? C30 H30A 0.9500 . ? C31 C32 1.485(7) . ? C32 C33 1.385(8) . ? C33 C34 1.388(8) . ? C33 H33A 0.9500 . ? C34 C35 1.392(8) . ? C34 H34A 0.9500 . ? C35 C36 1.380(8) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C38 1.471(8) . ? C37 H37A 0.9500 . ? C38 C42 1.384(9) . ? C38 C39 1.396(8) . ? C39 H39A 0.9500 . ? C40 C41 1.375(10) . ? C40 H40A 0.9500 . ? C41 C42 1.377(9) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? P1 F14 1.514(10) . ? P1 F15 1.554(7) . ? P1 F16 1.556(9) . ? P1 F11 1.565(10) . ? P1 F13 1.566(9) . ? P1 F12 1.572(10) . ? P2 F22 1.35(3) . ? P2 F21 1.48(2) . ? P2 F23 1.571(9) . ? P2 F24 1.61(2) . ? P2 F26 1.614(15) . ? P2 F25 1.724(8) . ? P2' F24' 1.53(2) . ? P2' F23' 1.546(14) . ? P2' F26' 1.546(19) . ? P2' F21' 1.615(15) . ? P2' F22' 1.89(3) . ? P3 F31 1.570(5) . ? P3 F31 1.570(5) 2_667 ? P3 F33 1.587(4) . ? P3 F33 1.587(4) 2_667 ? P3 F32 1.590(4) 2_667 ? P3 F32 1.590(4) . ? N100 C101 1.116(12) . ? C100 C101 1.451(15) . ? C100 H10A 0.9800 . ? C100 H10B 0.9800 . ? C100 H10C 0.9800 . ? P4 F44 1.557(13) . ? P4 F42 1.561(13) . ? P4 F43 1.578(16) . ? P4 F46 1.586(16) . ? P4 F41 1.592(15) . ? P4 F45 1.600(17) . ? N300 C301 1.131(9) . ? C300 C301 1.445(10) . ? C300 H30B 0.9800 . ? C300 H30C 0.9800 . ? C300 H30D 0.9800 . ? C201 N200 1.226(17) . ? C201 C200 1.28(2) . ? C200 H20B 0.9800 . ? C200 H20C 0.9800 . ? C200 H20D 0.9800 . ? C500 N500 0.99(5) . ? C500 C501 1.14(4) . ? C501 H50A 0.9800 . ? C501 H50B 0.9800 . ? C501 H50C 0.9800 . ? N400 C401 1.29(5) . ? C401 C400 1.50(3) . ? C400 H40B 0.9800 . ? C400 H40C 0.9800 . ? C400 H40D 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N8 178.15(18) . . ? N2 Fe1 N1 81.00(17) . . ? N8 Fe1 N1 100.76(17) . . ? N2 Fe1 N9 100.13(18) . . ? N8 Fe1 N9 80.56(17) . . ? N1 Fe1 N9 88.37(17) . . ? N2 Fe1 N3 80.35(17) . . ? N8 Fe1 N3 97.92(17) . . ? N1 Fe1 N3 161.16(16) . . ? N9 Fe1 N3 92.26(18) . . ? N2 Fe1 N7 98.59(18) . . ? N8 Fe1 N7 80.77(17) . . ? N1 Fe1 N7 93.54(16) . . ? N9 Fe1 N7 161.25(17) . . ? N3 Fe1 N7 91.88(17) . . ? C1 N1 C5 118.5(4) . . ? C1 N1 Fe1 127.1(3) . . ? C5 N1 Fe1 114.2(3) . . ? N1 C1 C2 122.9(5) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C10 N2 C6 119.7(4) . . ? C10 N2 Fe1 120.3(3) . . ? C6 N2 Fe1 119.9(3) . . ? C1 C2 C3 118.3(5) . . ? C1 C2 H2A 120.9 . . ? C3 C2 H2A 120.9 . . ? C15 N3 C11 118.2(4) . . ? C15 N3 Fe1 126.6(4) . . ? C11 N3 Fe1 115.2(3) . . ? C4 C3 C2 119.8(5) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C3 C4 C5 119.2(5) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? C8 N4 N5 119.9(6) . . ? C8 N4 H4B 120.1 . . ? N5 N4 H4B 120.1 . . ? N1 C5 C4 121.2(5) . . ? N1 C5 C6 114.3(4) . . ? C4 C5 C6 124.4(4) . . ? C16 N5 N4 116.7(6) . . ? N2 C6 C7 121.9(5) . . ? N2 C6 C5 110.4(4) . . ? C7 C6 C5 127.7(4) . . ? C19 N6 C18 122.3(7) . . ? C19 N6 H6 125(7) . . ? C18 N6 H6 112(8) . . ? C22 N7 C26 117.5(4) . . ? C22 N7 Fe1 128.3(3) . . ? C26 N7 Fe1 114.1(3) . . ? C6 C7 C8 118.8(5) . . ? C6 C7 H7A 120.6 . . ? C8 C7 H7A 120.6 . . ? N4 C8 C7 122.4(5) . . ? N4 C8 C9 119.0(6) . . ? C7 C8 C9 118.6(5) . . ? C31 N8 C27 120.3(4) . . ? C31 N8 Fe1 119.7(3) . . ? C27 N8 Fe1 119.6(3) . . ? C36 N9 C32 117.5(5) . . ? C36 N9 Fe1 127.0(4) . . ? C32 N9 Fe1 115.3(3) . . ? C10 C9 C8 119.7(5) . . ? C10 C9 H9A 120.2 . . ? C8 C9 H9A 120.2 . . ? N2 C10 C9 121.3(5) . . ? N2 C10 C11 110.4(4) . . ? C9 C10 C11 128.2(5) . . ? N11 N10 C29 119.7(5) . . ? N11 N10 H10D 120.1 . . ? C29 N10 H10D 120.1 . . ? C37 N11 N10 116.5(5) . . ? N3 C11 C12 121.9(5) . . ? N3 C11 C10 113.5(4) . . ? C12 C11 C10 124.7(5) . . ? C40 N12 C39 119.3(6) . . ? C11 C12 C13 119.7(5) . . ? C11 C12 H12A 120.1 . . ? C13 C12 H12A 120.1 . . ? C14 C13 C12 118.4(5) . . ? C14 C13 H13A 120.8 . . ? C12 C13 H13A 120.8 . . ? C15 C14 C13 119.3(5) . . ? C15 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? N3 C15 C14 122.5(5) . . ? N3 C15 H15A 118.8 . . ? C14 C15 H15A 118.8 . . ? N5 C16 C17 117.8(7) . . ? N5 C16 H16A 121.1 . . ? C17 C16 H16A 121.1 . . ? C21 C17 C18 118.1(8) . . ? C21 C17 C16 123.2(6) . . ? C18 C17 C16 118.7(8) . . ? N6 C18 C17 119.8(9) . . ? N6 C18 H18A 120.1 . . ? C17 C18 H18A 120.1 . . ? N6 C19 C20 120.4(9) . . ? N6 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C19 C20 C21 119.4(11) . . ? C19 C20 H20A 120.3 . . ? C21 C20 H20A 120.3 . . ? C17 C21 C20 120.0(8) . . ? C17 C21 H21A 120.0 . . ? C20 C21 H21A 120.0 . . ? N7 C22 C23 123.6(5) . . ? N7 C22 H22A 118.2 . . ? C23 C22 H22A 118.2 . . ? C24 C23 C22 118.6(5) . . ? C24 C23 H23A 120.7 . . ? C22 C23 H23A 120.7 . . ? C25 C24 C23 119.2(5) . . ? C25 C24 H24A 120.4 . . ? C23 C24 H24A 120.4 . . ? C24 C25 C26 119.8(5) . . ? C24 C25 H25A 120.1 . . ? C26 C25 H25A 120.1 . . ? N7 C26 C25 121.4(5) . . ? N7 C26 C27 113.8(4) . . ? C25 C26 C27 124.9(4) . . ? N8 C27 C28 121.2(5) . . ? N8 C27 C26 111.0(4) . . ? C28 C27 C26 127.8(5) . . ? C27 C28 C29 118.5(5) . . ? C27 C28 H28A 120.7 . . ? C29 C28 H28A 120.7 . . ? N10 C29 C28 121.7(5) . . ? N10 C29 C30 118.4(5) . . ? C28 C29 C30 119.9(4) . . ? C31 C30 C29 117.9(5) . . ? C31 C30 H30A 121.0 . . ? C29 C30 H30A 121.0 . . ? N8 C31 C30 122.1(5) . . ? N8 C31 C32 111.5(4) . . ? C30 C31 C32 126.4(5) . . ? N9 C32 C33 123.1(4) . . ? N9 C32 C31 112.4(4) . . ? C33 C32 C31 124.5(5) . . ? C32 C33 C34 118.6(5) . . ? C32 C33 H33A 120.7 . . ? C34 C33 H33A 120.7 . . ? C33 C34 C35 118.7(5) . . ? C33 C34 H34A 120.7 . . ? C35 C34 H34A 120.7 . . ? C36 C35 C34 119.4(5) . . ? C36 C35 H35A 120.3 . . ? C34 C35 H35A 120.3 . . ? N9 C36 C35 122.5(5) . . ? N9 C36 H36A 118.7 . . ? C35 C36 H36A 118.7 . . ? N11 C37 C38 118.8(5) . . ? N11 C37 H37A 120.6 . . ? C38 C37 H37A 120.6 . . ? C42 C38 C39 118.7(6) . . ? C42 C38 C37 122.3(5) . . ? C39 C38 C37 119.0(6) . . ? N12 C39 C38 121.6(7) . . ? N12 C39 H39A 119.2 . . ? C38 C39 H39A 119.2 . . ? N12 C40 C41 122.5(6) . . ? N12 C40 H40A 118.8 . . ? C41 C40 H40A 118.8 . . ? C40 C41 C42 119.3(7) . . ? C40 C41 H41A 120.3 . . ? C42 C41 H41A 120.3 . . ? C41 C42 C38 118.7(6) . . ? C41 C42 H42A 120.7 . . ? C38 C42 H42A 120.7 . . ? F14 P1 F15 90.5(6) . . ? F14 P1 F16 94.9(7) . . ? F15 P1 F16 88.9(5) . . ? F14 P1 F11 176.8(8) . . ? F15 P1 F11 88.7(4) . . ? F16 P1 F11 88.1(7) . . ? F14 P1 F13 94.4(7) . . ? F15 P1 F13 175.1(6) . . ? F16 P1 F13 90.7(5) . . ? F11 P1 F13 86.4(6) . . ? F14 P1 F12 87.2(7) . . ? F15 P1 F12 88.3(6) . . ? F16 P1 F12 176.6(7) . . ? F11 P1 F12 89.8(7) . . ? F13 P1 F12 91.8(7) . . ? F22 P2 F21 88(2) . . ? F22 P2 F23 88.6(12) . . ? F21 P2 F23 89.1(8) . . ? F22 P2 F24 88.9(18) . . ? F21 P2 F24 176.7(14) . . ? F23 P2 F24 89.9(8) . . ? F22 P2 F26 177.1(13) . . ? F21 P2 F26 92.7(13) . . ? F23 P2 F26 88.6(6) . . ? F24 P2 F26 90.4(13) . . ? F22 P2 F25 93.6(12) . . ? F21 P2 F25 96.9(7) . . ? F23 P2 F25 173.7(8) . . ? F24 P2 F25 84.2(8) . . ? F26 P2 F25 89.1(6) . . ? F24' P2' F23' 86.8(8) . . ? F24' P2' F26' 89.2(13) . . ? F23' P2' F26' 88.8(12) . . ? F24' P2' F21' 177.6(14) . . ? F23' P2' F21' 94.0(8) . . ? F26' P2' F21' 88.6(12) . . ? F24' P2' F22' 85.5(10) . . ? F23' P2' F22' 97.8(12) . . ? F26' P2' F22' 171.4(13) . . ? F21' P2' F22' 96.5(11) . . ? F31 P3 F31 180.000(2) . 2_667 ? F31 P3 F33 89.8(3) . . ? F31 P3 F33 90.2(3) 2_667 . ? F31 P3 F33 90.2(3) . 2_667 ? F31 P3 F33 89.8(3) 2_667 2_667 ? F33 P3 F33 180.000(3) . 2_667 ? F31 P3 F32 89.2(3) . 2_667 ? F31 P3 F32 90.8(3) 2_667 2_667 ? F33 P3 F32 90.9(2) . 2_667 ? F33 P3 F32 89.1(2) 2_667 2_667 ? F31 P3 F32 90.8(3) . . ? F31 P3 F32 89.2(3) 2_667 . ? F33 P3 F32 89.1(2) . . ? F33 P3 F32 90.9(2) 2_667 . ? F32 P3 F32 180.000(5) 2_667 . ? C101 C100 H10A 109.5 . . ? C101 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? C101 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? N100 C101 C100 179.0(12) . . ? F44 P4 F42 92.0(9) . . ? F44 P4 F43 91.9(9) . . ? F42 P4 F43 94.7(9) . . ? F44 P4 F46 95.5(14) . . ? F42 P4 F46 91.1(8) . . ? F43 P4 F46 170.4(14) . . ? F44 P4 F41 94.5(8) . . ? F42 P4 F41 171.8(14) . . ? F43 P4 F41 80.0(15) . . ? F46 P4 F41 93.3(9) . . ? F44 P4 F45 172.7(15) . . ? F42 P4 F45 87.6(17) . . ? F43 P4 F45 80.8(16) . . ? F46 P4 F45 91.8(10) . . ? F41 P4 F45 85.4(18) . . ? C301 C300 H30B 109.5 . . ? C301 C300 H30C 109.5 . . ? H30B C300 H30C 109.5 . . ? C301 C300 H30D 109.5 . . ? H30B C300 H30D 109.5 . . ? H30C C300 H30D 109.5 . . ? N300 C301 C300 178.9(9) . . ? N200 C201 C200 160.6(19) . . ? C201 C200 H20B 109.5 . . ? C201 C200 H20C 109.5 . . ? H20B C200 H20C 109.5 . . ? C201 C200 H20D 109.5 . . ? H20B C200 H20D 109.5 . . ? H20C C200 H20D 109.5 . . ? N500 C500 C501 157(10) . . ? C500 C501 H50A 109.5 . . ? C500 C501 H50B 109.5 . . ? H50A C501 H50B 109.5 . . ? C500 C501 H50C 109.5 . . ? H50A C501 H50C 109.5 . . ? H50B C501 H50C 109.5 . . ? N400 C401 C400 156(4) . . ? C401 C400 H40B 109.5 . . ? C401 C400 H40C 109.5 . . ? H40B C400 H40C 109.5 . . ? C401 C400 H40D 109.5 . . ? H40B C400 H40D 109.5 . . ? H40C C400 H40D 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.809 _refine_diff_density_min -1.039 _refine_diff_density_rms 0.103 # start Validation Reply Form _vrf_PLAT242_jb1167 ; PROBLEM: Check Low Ueq as Compared to Neighbors for P4 RESPONSE: PF6 anion disordered ; _vrf_PLAT430_jb1167 ; PROBLEM: Short Inter D...A Contact O1" .. N500 .. 2.44 Ang. RESPONSE: Refers to atoms of partial occupancy ; _vrf_PLAT432_jb1167 ; PROBLEM: Short Inter X...Y Contact F45 .. C501 .. 2.56 Ang. RESPONSE: Refers to atoms of partial occupancy ; _vrf_PLAT780_jb1167 ; PROBLEM: Coordinates do not Form a Properly Connected Set ? RESPONSE: There are two complexes and two sets of disordered solvent molecules ; # end Validation Reply Form # Attachment 'Ligand_1_JZ.CIF' data_jb999 _database_code_depnum_ccdc_archive 'CCDC 692940' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H16 N6, C H Cl3, H2 O' _chemical_formula_sum 'C22 H19 Cl3 N6 O' _chemical_formula_weight 489.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.957(2) _cell_length_b 10.336(2) _cell_length_c 12.413(3) _cell_angle_alpha 71.39(3) _cell_angle_beta 71.60(3) _cell_angle_gamma 88.82(3) _cell_volume 1144.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 0.428 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20589 _diffrn_reflns_av_R_equivalents 0.1144 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3989 _reflns_number_gt 3666 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+1.8426P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3989 _refine_ls_number_parameters 295 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1401 _refine_ls_wR_factor_gt 0.1367 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.4652(2) 1.1666(2) 0.7729(2) 0.0271(5) Uani 1 1 d . . . C1 C 0.1575(3) 0.5074(3) 0.6598(3) 0.0306(6) Uani 1 1 d . . . H1 H 0.0778 0.4598 0.6583 0.037 Uiso 1 1 calc R . . N2 N 0.3468(2) 0.8987(2) 0.69256(19) 0.0220(5) Uani 1 1 d . . . C2 C 0.2866(3) 0.4520(3) 0.6345(3) 0.0319(6) Uani 1 1 d . . . H2 H 0.2952 0.3683 0.6175 0.038 Uiso 1 1 calc R . . N3 N 0.1373(2) 0.6235(2) 0.6862(2) 0.0270(5) Uani 1 1 d . . . C3 C 0.4033(3) 0.5229(3) 0.6347(3) 0.0306(6) Uani 1 1 d . . . H3A H 0.4940 0.4883 0.6178 0.037 Uiso 1 1 calc R . . N4 N -0.0562(2) 0.9939(2) 0.8661(2) 0.0255(5) Uani 1 1 d . . . H4B H -0.1298 0.9345 0.8879 0.031 Uiso 1 1 calc R . . C4 C 0.3863(3) 0.6438(3) 0.6596(2) 0.0262(6) Uani 1 1 d . . . H4A H 0.4654 0.6945 0.6586 0.031 Uiso 1 1 calc R . . N5 N -0.0735(2) 1.1143(2) 0.8888(2) 0.0229(5) Uani 1 1 d . . . C5 C 0.2516(3) 0.6911(3) 0.6864(2) 0.0221(5) Uani 1 1 d . . . C6 C 0.2286(3) 0.8185(3) 0.7187(2) 0.0208(5) Uani 1 1 d . . . N6 N -0.2862(3) 1.5071(2) 1.0226(2) 0.0307(5) Uani 1 1 d . . . C7 C 0.0938(3) 0.8477(3) 0.7758(2) 0.0220(5) Uani 1 1 d . . . H7A H 0.0131 0.7880 0.7925 0.026 Uiso 1 1 calc R . . C8 C 0.0778(3) 0.9659(3) 0.8087(2) 0.0218(5) Uani 1 1 d . . . C9 C 0.2004(3) 1.0498(3) 0.7825(2) 0.0219(5) Uani 1 1 d . . . H9A H 0.1944 1.1315 0.8028 0.026 Uiso 1 1 calc R . . C10 C 0.3304(3) 1.0106(3) 0.7265(2) 0.0203(5) Uani 1 1 d . . . C11 C 0.4673(3) 1.0896(3) 0.7032(2) 0.0215(5) Uani 1 1 d . . . C12 C 0.5901(3) 1.0766(3) 0.6170(2) 0.0274(6) Uani 1 1 d . . . H12A H 0.5873 1.0233 0.5678 0.033 Uiso 1 1 calc R . . C13 C 0.7174(3) 1.1429(3) 0.6034(3) 0.0307(6) Uani 1 1 d . . . H13A H 0.8032 1.1351 0.5452 0.037 Uiso 1 1 calc R . . C14 C 0.7170(3) 1.2201(3) 0.6760(3) 0.0318(6) Uani 1 1 d . . . H14A H 0.8026 1.2652 0.6697 0.038 Uiso 1 1 calc R . . C15 C 0.5898(3) 1.2304(3) 0.7575(3) 0.0326(6) Uani 1 1 d . . . H15A H 0.5899 1.2856 0.8057 0.039 Uiso 1 1 calc R . . C16 C -0.1999(3) 1.1319(3) 0.9487(2) 0.0236(5) Uani 1 1 d . . . H16A H -0.2750 1.0620 0.9758 0.028 Uiso 1 1 calc R . . C17 C -0.2272(3) 1.2594(3) 0.9748(2) 0.0219(5) Uani 1 1 d . . . C18 C -0.3641(3) 1.2821(3) 1.0366(2) 0.0262(6) Uani 1 1 d . . . H18A H -0.4407 1.2138 1.0632 0.031 Uiso 1 1 calc R . . C19 C -0.3874(3) 1.4050(3) 1.0588(3) 0.0295(6) Uani 1 1 d . . . H19A H -0.4811 1.4175 1.1025 0.035 Uiso 1 1 calc R . . C20 C -0.1546(3) 1.4840(3) 0.9638(3) 0.0305(6) Uani 1 1 d . . . H20A H -0.0806 1.5547 0.9374 0.037 Uiso 1 1 calc R . . C21 C -0.1200(3) 1.3643(3) 0.9393(3) 0.0270(6) Uani 1 1 d . . . H21A H -0.0244 1.3531 0.8987 0.032 Uiso 1 1 calc R . . Cl1 Cl -0.13027(12) 0.83353(13) 0.48550(8) 0.0669(3) Uani 1 1 d . . . O1 O -0.2884(3) 0.7884(2) 1.0087(2) 0.0413(6) Uani 1 1 d . . . Cl2 Cl -0.22524(12) 0.55745(10) 0.65021(12) 0.0638(3) Uani 1 1 d . . . Cl3 Cl -0.25525(9) 0.78390(9) 0.74076(8) 0.0440(2) Uani 1 1 d . . . C22 C -0.1499(3) 0.7199(3) 0.6304(3) 0.0344(7) Uani 1 1 d . . . H22A H -0.0537 0.7092 0.6396 0.041 Uiso 1 1 calc R . . H1B H -0.284(4) 0.706(5) 1.024(4) 0.052 Uiso 1 1 d . . . H2B H -0.329(4) 0.795(4) 1.081(4) 0.052 Uiso 1 1 d . . . 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 N1 0.0248(12) 0.0286(12) 0.0291(12) -0.0120(10) -0.0076(10) -0.0007(9) C1 0.0298(15) 0.0296(14) 0.0338(16) -0.0155(12) -0.0069(12) -0.0021(11) N2 0.0219(11) 0.0232(11) 0.0200(11) -0.0066(9) -0.0062(9) 0.0005(9) C2 0.0383(16) 0.0280(14) 0.0322(15) -0.0164(12) -0.0090(13) 0.0053(12) N3 0.0251(12) 0.0272(12) 0.0306(12) -0.0134(10) -0.0075(10) 0.0005(9) C3 0.0289(14) 0.0346(15) 0.0322(15) -0.0166(13) -0.0103(12) 0.0105(12) N4 0.0191(11) 0.0245(11) 0.0333(13) -0.0148(10) -0.0036(9) 0.0006(9) C4 0.0242(13) 0.0306(14) 0.0269(14) -0.0135(12) -0.0085(11) 0.0032(11) N5 0.0237(11) 0.0227(11) 0.0235(11) -0.0092(9) -0.0078(9) 0.0031(9) C5 0.0248(13) 0.0234(13) 0.0178(12) -0.0064(10) -0.0066(10) 0.0008(10) C6 0.0219(12) 0.0224(12) 0.0178(12) -0.0060(10) -0.0067(10) 0.0013(10) N6 0.0389(14) 0.0259(12) 0.0278(12) -0.0093(10) -0.0111(11) 0.0079(10) C7 0.0219(12) 0.0216(12) 0.0225(13) -0.0070(10) -0.0073(10) -0.0010(10) C8 0.0221(13) 0.0236(13) 0.0179(12) -0.0056(10) -0.0057(10) 0.0030(10) C9 0.0248(13) 0.0200(12) 0.0206(13) -0.0067(10) -0.0068(10) 0.0013(10) C10 0.0218(12) 0.0205(12) 0.0168(12) -0.0040(10) -0.0059(10) -0.0008(10) C11 0.0226(13) 0.0196(12) 0.0198(12) -0.0030(10) -0.0070(10) 0.0007(10) C12 0.0267(14) 0.0285(14) 0.0256(14) -0.0099(11) -0.0053(11) -0.0008(11) C13 0.0226(13) 0.0337(15) 0.0288(15) -0.0069(12) -0.0019(11) -0.0019(11) C14 0.0253(14) 0.0305(15) 0.0379(16) -0.0078(13) -0.0109(12) -0.0055(11) C15 0.0315(15) 0.0331(15) 0.0383(16) -0.0181(13) -0.0117(13) -0.0007(12) C16 0.0222(13) 0.0245(13) 0.0235(13) -0.0072(11) -0.0071(11) 0.0010(10) C17 0.0229(13) 0.0244(13) 0.0187(12) -0.0070(10) -0.0076(10) 0.0046(10) C18 0.0228(13) 0.0280(14) 0.0254(14) -0.0068(11) -0.0066(11) 0.0021(11) C19 0.0284(14) 0.0327(15) 0.0270(14) -0.0115(12) -0.0073(12) 0.0100(12) C20 0.0338(15) 0.0249(14) 0.0320(15) -0.0084(12) -0.0108(12) -0.0005(11) C21 0.0233(13) 0.0251(13) 0.0296(15) -0.0080(11) -0.0056(11) 0.0026(11) Cl1 0.0674(7) 0.0859(8) 0.0321(5) -0.0026(5) -0.0131(4) 0.0103(5) O1 0.0447(13) 0.0298(11) 0.0388(13) -0.0185(10) 0.0086(10) -0.0093(10) Cl2 0.0668(6) 0.0471(5) 0.1007(9) -0.0336(5) -0.0493(6) 0.0058(4) Cl3 0.0389(4) 0.0509(5) 0.0410(5) -0.0173(4) -0.0097(3) 0.0087(3) C22 0.0308(15) 0.0423(17) 0.0344(16) -0.0132(14) -0.0158(13) 0.0050(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C11 1.345(3) . ? N1 C15 1.347(4) . ? C1 N3 1.338(4) . ? C1 C2 1.381(4) . ? C1 H1 0.9500 . ? N2 C10 1.342(3) . ? N2 C6 1.344(3) . ? C2 C3 1.388(4) . ? C2 H2 0.9500 . ? N3 C5 1.348(3) . ? C3 C4 1.375(4) . ? C3 H3A 0.9500 . ? N4 N5 1.357(3) . ? N4 C8 1.374(3) . ? N4 H4B 0.8800 . ? C4 C5 1.394(4) . ? C4 H4A 0.9500 . ? N5 C16 1.288(4) . ? C5 C6 1.489(4) . ? C6 C7 1.383(4) . ? N6 C19 1.337(4) . ? N6 C20 1.342(4) . ? C7 C8 1.398(4) . ? C7 H7A 0.9500 . ? C8 C9 1.400(4) . ? C9 C10 1.383(4) . ? C9 H9A 0.9500 . ? C10 C11 1.501(3) . ? C11 C12 1.384(4) . ? C12 C13 1.390(4) . ? C12 H12A 0.9500 . ? C13 C14 1.381(4) . ? C13 H13A 0.9500 . ? C14 C15 1.376(4) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.455(4) . ? C16 H16A 0.9500 . ? C17 C18 1.394(4) . ? C17 C21 1.398(4) . ? C18 C19 1.383(4) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C21 1.378(4) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? Cl1 C22 1.758(3) . ? O1 H1B 0.81(4) . ? O1 H2B 0.89(4) . ? Cl2 C22 1.765(3) . ? Cl3 C22 1.748(3) . ? C22 H22A 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 N1 C15 117.2(2) . . ? N3 C1 C2 124.3(3) . . ? N3 C1 H1 117.9 . . ? C2 C1 H1 117.9 . . ? C10 N2 C6 117.0(2) . . ? C1 C2 C3 117.7(3) . . ? C1 C2 H2 121.1 . . ? C3 C2 H2 121.1 . . ? C1 N3 C5 117.3(2) . . ? C4 C3 C2 119.3(3) . . ? C4 C3 H3A 120.4 . . ? C2 C3 H3A 120.4 . . ? N5 N4 C8 119.1(2) . . ? N5 N4 H4B 120.5 . . ? C8 N4 H4B 120.5 . . ? C3 C4 C5 119.3(3) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? C16 N5 N4 116.5(2) . . ? N3 C5 C4 122.1(2) . . ? N3 C5 C6 117.3(2) . . ? C4 C5 C6 120.5(2) . . ? N2 C6 C7 123.2(2) . . ? N2 C6 C5 115.5(2) . . ? C7 C6 C5 121.2(2) . . ? C19 N6 C20 116.1(2) . . ? C6 C7 C8 119.2(2) . . ? C6 C7 H7A 120.4 . . ? C8 C7 H7A 120.4 . . ? N4 C8 C7 118.9(2) . . ? N4 C8 C9 123.0(2) . . ? C7 C8 C9 118.1(2) . . ? C10 C9 C8 118.2(2) . . ? C10 C9 H9A 120.9 . . ? C8 C9 H9A 120.9 . . ? N2 C10 C9 124.2(2) . . ? N2 C10 C11 114.3(2) . . ? C9 C10 C11 121.5(2) . . ? N1 C11 C12 122.7(2) . . ? N1 C11 C10 117.1(2) . . ? C12 C11 C10 120.2(2) . . ? C11 C12 C13 119.0(3) . . ? C11 C12 H12A 120.5 . . ? C13 C12 H12A 120.5 . . ? C14 C13 C12 118.8(3) . . ? C14 C13 H13A 120.6 . . ? C12 C13 H13A 120.6 . . ? C15 C14 C13 118.6(3) . . ? C15 C14 H14A 120.7 . . ? C13 C14 H14A 120.7 . . ? N1 C15 C14 123.7(3) . . ? N1 C15 H15A 118.1 . . ? C14 C15 H15A 118.1 . . ? N5 C16 C17 119.7(2) . . ? N5 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C18 C17 C21 117.0(2) . . ? C18 C17 C16 120.5(2) . . ? C21 C17 C16 122.4(2) . . ? C19 C18 C17 119.3(3) . . ? C19 C18 H18A 120.3 . . ? C17 C18 H18A 120.3 . . ? N6 C19 C18 124.1(3) . . ? N6 C19 H19A 117.9 . . ? C18 C19 H19A 117.9 . . ? N6 C20 C21 124.3(3) . . ? N6 C20 H20A 117.9 . . ? C21 C20 H20A 117.9 . . ? C20 C21 C17 119.2(3) . . ? C20 C21 H21A 120.4 . . ? C17 C21 H21A 120.4 . . ? H1B O1 H2B 102(4) . . ? Cl3 C22 Cl1 110.99(17) . . ? Cl3 C22 Cl2 109.86(18) . . ? Cl1 C22 Cl2 110.52(17) . . ? Cl3 C22 H22A 108.5 . . ? Cl1 C22 H22A 108.5 . . ? Cl2 C22 H22A 108.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.510 _refine_diff_density_min -0.759 _refine_diff_density_rms 0.061 # Attachment 'Polymer.CIF' data_jb21ap-1 _database_code_depnum_ccdc_archive 'CCDC 692941' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[{Ru(tpyNHNCHpy)2}2Fe(NCS)2]An(NCS)2' _chemical_melting_point ? _chemical_formula_moiety 'Fe (N C S)2 Ru2 C84 H64 N24,Fe2 O4 C8 H22 (N C S)6,(NCS)2,C8 H26 O5' _chemical_formula_sum 'C116 H132 Fe3 N34 O13 Ru2 S10' _chemical_formula_weight 2900.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.812(8) _cell_length_b 15.073(8) _cell_length_c 18.604(10) _cell_angle_alpha 67.221(8) _cell_angle_beta 70.821(8) _cell_angle_gamma 73.834(8) _cell_volume 3322(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 986 _cell_measurement_theta_min 2.567 _cell_measurement_theta_max 20.1165 _exptl_crystal_description plate _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.770 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.905 _exptl_absorpt_correction_T_max 0.977 _exptl_absorpt_process_details 'SADABS, Bruker 1995' _exptl_special_details ; In a thin film of perfluoropolyether oil on a mohair fibre ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 48 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 28554 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.2446 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 26.37 _reflns_number_total 13366 _reflns_number_gt 5422 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1109P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13366 _refine_ls_number_parameters 750 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.2173 _refine_ls_R_factor_gt 0.0822 _refine_ls_wR_factor_ref 0.2416 _refine_ls_wR_factor_gt 0.1821 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.34446(6) 0.23985(5) 1.13850(4) 0.0288(2) Uani 1 1 d . . . Fe1 Fe 0.0000 0.5000 0.5000 0.0280(4) Uani 1 2 d S . . Fe2 Fe 0.04463(13) -0.03744(13) 1.07580(10) 0.0631(5) Uani 1 1 d . . . S1 S 0.3207(3) 0.6156(4) 0.4475(3) 0.1300(18) Uani 1 1 d . . . S2 S 0.3816(2) 0.0412(2) 0.9531(2) 0.0726(10) Uani 1 1 d . . . S3 S 0.0218(3) 0.0886(3) 1.2797(3) 0.1176(17) Uani 1 1 d . . . S4 S 0.2134(3) -0.2910(2) 1.25693(19) 0.0686(9) Uani 1 1 d . . . S5 S -0.2541(2) 0.4530(2) 1.22207(17) 0.0604(8) Uani 1 1 d . . . O1 O 0.0415(5) -0.0752(5) 0.9857(4) 0.059(2) Uani 1 1 d . . . O2 O -0.1016(6) -0.0901(6) 1.1360(5) 0.084(3) Uani 1 1 d . . . O70 O 0.8041(10) 0.2215(10) 1.4772(8) 0.155(5) Uiso 1 1 d . . . H70 H 0.8429 0.2196 1.4321 0.186 Uiso 1 1 calc R . . O76 O 0.508(2) 0.351(2) 0.4244(17) 0.357(10) Uiso 1 1 d D . . H76 H 0.5537 0.3025 0.4180 0.429 Uiso 1 1 calc . . . O77 O 0.4519(13) 0.2375(13) 0.5951(10) 0.213(7) Uiso 1 1 d D . . H77 H 0.5006 0.2527 0.5538 0.256 Uiso 1 1 calc R . . O80 O 0.669(3) -0.043(3) 1.556(3) 0.293(15) Uiso 0.50 1 d PD . . O730 O 0.788(3) 0.2198(17) 1.317(2) 0.085(11) Uiso 0.40(4) 1 d P . . O731 O 0.7340(16) 0.2322(10) 1.3518(11) 0.061(6) Uiso 0.60(4) 1 d P . . N1 N 0.3427(5) 0.0921(5) 1.1798(4) 0.0332(18) Uani 1 1 d . . . N2 N 0.4582(5) 0.1886(5) 1.1935(4) 0.0303(17) Uani 1 1 d . . . N3 N 0.3931(5) 0.3657(5) 1.1177(4) 0.0250(16) Uani 1 1 d . . . N4 N 0.6929(6) 0.0832(5) 1.3092(4) 0.043(2) Uani 1 1 d . . . H4 H 0.7245 0.1249 1.3114 0.052 Uiso 1 1 calc R . . N5 N 0.7232(6) -0.0139(5) 1.3419(4) 0.0365(18) Uani 1 1 d . . . N6 N 0.9297(6) -0.3409(5) 1.4607(4) 0.0312(17) Uani 1 1 d . . . N7 N 0.4191(5) 0.2409(5) 1.0229(4) 0.0281(16) Uani 1 1 d . . . N8 N 0.2285(5) 0.2920(5) 1.0867(4) 0.0270(16) Uani 1 1 d . . . N9 N 0.2223(5) 0.2575(5) 1.2342(4) 0.0281(17) Uani 1 1 d . . . N10 N -0.0171(5) 0.3966(5) 0.9807(4) 0.0326(18) Uani 1 1 d . . . H10 H -0.0807 0.4095 1.0098 0.039 Uiso 1 1 calc R . . N11 N -0.0001(6) 0.4110(5) 0.9025(4) 0.0318(17) Uani 1 1 d . . . N12 N -0.0273(5) 0.4948(5) 0.6232(4) 0.0297(17) Uani 1 1 d . . . N13 N 0.1485(6) 0.5355(5) 0.4740(4) 0.0338(18) Uani 1 1 d . . . N14 N 0.1798(8) 0.0138(8) 1.0153(6) 0.072(3) Uani 1 1 d . . . N15 N 0.0190(8) 0.0185(8) 1.1647(7) 0.075(3) Uani 1 1 d . . . N16 N 0.1165(8) -0.1675(8) 1.1365(7) 0.076(3) Uani 1 1 d . . . N17 N -0.2288(6) 0.4367(6) 1.0727(5) 0.052(2) Uani 1 1 d . . . C1 C 0.2804(7) 0.0467(7) 1.1703(5) 0.041(2) Uani 1 1 d . . . H1 H 0.2338 0.0841 1.1370 0.049 Uiso 1 1 calc R . . C2 C 0.2803(8) -0.0498(7) 1.2056(6) 0.045(3) Uani 1 1 d . . . H2 H 0.2332 -0.0787 1.1978 0.053 Uiso 1 1 calc R . . C3 C 0.3473(8) -0.1065(7) 1.2525(6) 0.050(3) Uani 1 1 d . . . H3 H 0.3473 -0.1746 1.2785 0.059 Uiso 1 1 calc R . . C4 C 0.4146(7) -0.0610(6) 1.2605(5) 0.035(2) Uani 1 1 d . . . H4A H 0.4638 -0.0984 1.2915 0.042 Uiso 1 1 calc R . . C5 C 0.4120(7) 0.0362(6) 1.2250(5) 0.030(2) Uani 1 1 d . . . C6 C 0.4797(6) 0.0921(6) 1.2309(5) 0.028(2) Uani 1 1 d . . . C7 C 0.5587(7) 0.0523(6) 1.2701(5) 0.036(2) Uani 1 1 d . . . H7 H 0.5756 -0.0163 1.2947 0.043 Uiso 1 1 calc R . . C8 C 0.6127(7) 0.1160(7) 1.2726(5) 0.034(2) Uani 1 1 d . . . C9 C 0.8070(7) -0.0406(7) 1.3662(5) 0.042(2) Uani 1 1 d . . . H9 H 0.8429 0.0074 1.3616 0.050 Uiso 1 1 calc R . . C10 C 0.8474(7) -0.1435(6) 1.4005(5) 0.031(2) Uani 1 1 d . . . C11 C 0.7849(7) -0.2145(7) 1.4305(5) 0.038(2) Uani 1 1 d . . . H11A H 0.7135 -0.1970 1.4297 0.046 Uiso 1 1 calc R . . C12 C 0.8288(7) -0.3105(7) 1.4612(5) 0.038(2) Uani 1 1 d . . . H12 H 0.7849 -0.3582 1.4843 0.046 Uiso 1 1 calc R . . C13 C 0.9868(8) -0.2721(7) 1.4320(5) 0.040(2) Uani 1 1 d . . . H13 H 1.0585 -0.2916 1.4315 0.048 Uiso 1 1 calc R . . C14 C 0.9497(7) -0.1745(7) 1.4029(6) 0.043(3) Uani 1 1 d . . . H14 H 0.9947 -0.1283 1.3844 0.051 Uiso 1 1 calc R . . C15 C 0.5879(6) 0.2169(6) 1.2358(5) 0.032(2) Uani 1 1 d . . . H15 H 0.6241 0.2608 1.2375 0.039 Uiso 1 1 calc R . . C16 C 0.5092(6) 0.2503(6) 1.1969(5) 0.0252(19) Uani 1 1 d . . . C17 C 0.4701(6) 0.3517(6) 1.1550(5) 0.028(2) Uani 1 1 d . . . C18 C 0.5051(7) 0.4315(6) 1.1506(5) 0.036(2) Uani 1 1 d . . . H18 H 0.5564 0.4215 1.1780 0.043 Uiso 1 1 calc R . . C19 C 0.4677(7) 0.5239(6) 1.1081(6) 0.040(2) Uani 1 1 d . . . H19 H 0.4922 0.5784 1.1054 0.048 Uiso 1 1 calc R . . C20 C 0.3924(7) 0.5367(7) 1.0686(5) 0.039(2) Uani 1 1 d . . . H20 H 0.3649 0.6002 1.0380 0.046 Uiso 1 1 calc R . . C21 C 0.3587(6) 0.4564(6) 1.0746(5) 0.031(2) Uani 1 1 d . . . H21 H 0.3082 0.4657 1.0467 0.037 Uiso 1 1 calc R . . C22 C 0.5200(7) 0.2112(6) 0.9943(5) 0.035(2) Uani 1 1 d . . . H22 H 0.5638 0.1828 1.0305 0.042 Uiso 1 1 calc R . . C23 C 0.5635(8) 0.2203(7) 0.9139(6) 0.042(2) Uani 1 1 d . . . H23 H 0.6356 0.1976 0.8954 0.050 Uiso 1 1 calc R . . C24 C 0.5010(7) 0.2625(7) 0.8616(6) 0.040(2) Uani 1 1 d . . . H24 H 0.5294 0.2716 0.8058 0.048 Uiso 1 1 calc R . . C25 C 0.3970(7) 0.2915(6) 0.8904(5) 0.031(2) Uani 1 1 d . . . H25 H 0.3528 0.3204 0.8546 0.037 Uiso 1 1 calc R . . C26 C 0.3561(6) 0.2788(6) 0.9713(5) 0.0260(19) Uani 1 1 d . . . C27 C 0.2466(7) 0.3058(6) 1.0078(5) 0.028(2) Uani 1 1 d . . . C28 C 0.1665(7) 0.3386(6) 0.9716(5) 0.031(2) Uani 1 1 d . . . H28 H 0.1796 0.3459 0.9164 0.038 Uiso 1 1 calc R . . C29 C 0.0656(6) 0.3614(6) 1.0154(5) 0.0263(19) Uani 1 1 d . . . C30 C -0.0764(7) 0.4400(6) 0.8719(5) 0.034(2) Uani 1 1 d . . . H30 H -0.1450 0.4484 0.9050 0.041 Uiso 1 1 calc R . . C31 C -0.0611(7) 0.4608(6) 0.7865(5) 0.031(2) Uani 1 1 d . . . C32 C 0.0389(7) 0.4502(7) 0.7379(5) 0.037(2) Uani 1 1 d . . . H32 H 0.0975 0.4311 0.7599 0.044 Uiso 1 1 calc R . . C33 C 0.0521(7) 0.4674(7) 0.6579(5) 0.036(2) Uani 1 1 d . . . H33 H 0.1210 0.4595 0.6252 0.044 Uiso 1 1 calc R . . C34 C -0.1226(7) 0.5071(6) 0.6706(5) 0.031(2) Uani 1 1 d . . . H34 H -0.1800 0.5289 0.6470 0.037 Uiso 1 1 calc R . . C35 C -0.1427(7) 0.4902(6) 0.7514(5) 0.033(2) Uani 1 1 d . . . H35 H -0.2124 0.4986 0.7827 0.039 Uiso 1 1 calc R . . C36 C 0.0478(6) 0.3486(6) 1.0965(5) 0.029(2) Uani 1 1 d . . . H36 H -0.0205 0.3644 1.1274 0.035 Uiso 1 1 calc R . . C37 C 0.1308(6) 0.3126(6) 1.1315(5) 0.0262(19) Uani 1 1 d . . . C38 C 0.1289(6) 0.2927(6) 1.2162(5) 0.0252(19) Uani 1 1 d . . . C39 C 0.0379(7) 0.3065(7) 1.2745(5) 0.034(2) Uani 1 1 d . . . H39 H -0.0271 0.3324 1.2607 0.041 Uiso 1 1 calc R . . C40 C 0.0432(8) 0.2823(7) 1.3518(5) 0.039(2) Uani 1 1 d . . . H40 H -0.0180 0.2908 1.3926 0.047 Uiso 1 1 calc R . . C41 C 0.1373(8) 0.2458(6) 1.3696(5) 0.038(2) Uani 1 1 d . . . H41 H 0.1419 0.2281 1.4234 0.045 Uiso 1 1 calc R . . C42 C 0.2244(7) 0.2346(6) 1.3112(5) 0.035(2) Uani 1 1 d . . . H42 H 0.2894 0.2096 1.3249 0.042 Uiso 1 1 calc R . . C50 C 0.2185(9) 0.5681(8) 0.4639(7) 0.055(3) Uani 1 1 d . . . C60 C 0.2637(9) 0.0249(7) 0.9899(6) 0.048(3) Uani 1 1 d . . . C61 C 0.0158(10) 0.0514(10) 1.2110(8) 0.078(4) Uani 1 1 d . . . C62 C 0.1560(9) -0.2201(9) 1.1880(7) 0.057(3) Uani 1 1 d . . . C63 C 0.0799(10) -0.1696(9) 0.9776(8) 0.078(4) Uani 1 1 d . . . H63A H 0.0356 -0.1828 0.9518 0.094 Uiso 1 1 calc R . . H63B H 0.0762 -0.2194 1.0316 0.094 Uiso 1 1 calc R . . C64 C 0.1919(11) -0.1777(11) 0.9272(9) 0.108(5) Uani 1 1 d . . . H64A H 0.2164 -0.2436 0.9231 0.162 Uiso 1 1 calc R . . H64B H 0.2361 -0.1651 0.9528 0.162 Uiso 1 1 calc R . . H64C H 0.1955 -0.1296 0.8732 0.162 Uiso 1 1 calc R . . C65 C -0.1256(12) -0.1703(14) 1.1938(9) 0.124(5) Uani 1 1 d . . . H65A H -0.1086 -0.1699 1.2413 0.149 Uiso 1 1 calc R . . H65B H -0.0761 -0.2248 1.1773 0.149 Uiso 1 1 calc R . . C66 C -0.2238(12) -0.1972(13) 1.2216(9) 0.124(5) Uani 1 1 d . . . H66A H -0.2218 -0.2610 1.2640 0.186 Uiso 1 1 calc R . . H66B H -0.2435 -0.2011 1.1770 0.186 Uiso 1 1 calc R . . H66C H -0.2751 -0.1482 1.2433 0.186 Uiso 1 1 calc R . . C71 C 0.8215(19) 0.1211(18) 1.5409(13) 0.155(8) Uiso 1 1 d . . . C74 C 0.384(3) 0.297(3) 0.380(2) 0.357(10) Uiso 1 1 d D . . H74A H 0.3371 0.3231 0.3440 0.536 Uiso 1 1 calc R . . H74B H 0.3450 0.2704 0.4354 0.536 Uiso 1 1 calc R . . H74C H 0.4381 0.2448 0.3640 0.536 Uiso 1 1 calc R . . C75 C 0.434(3) 0.375(2) 0.373(2) 0.357(10) Uiso 1 1 d D . . H75A H 0.3778 0.4285 0.3854 0.429 Uiso 1 1 calc R . . H75B H 0.4718 0.4014 0.3159 0.429 Uiso 1 1 calc R . . C78 C 0.431(2) 0.3031(19) 0.6398(15) 0.230(12) Uiso 1 1 d D . . H78A H 0.3802 0.2766 0.6911 0.276 Uiso 1 1 calc R . . H78B H 0.4963 0.2958 0.6541 0.276 Uiso 1 1 calc R . . C79 C 0.395(3) 0.403(2) 0.612(2) 0.313(18) Uiso 1 1 d D . . H79A H 0.3791 0.4297 0.6560 0.469 Uiso 1 1 calc R . . H79B H 0.3311 0.4143 0.5951 0.469 Uiso 1 1 calc R . . H79C H 0.4478 0.4345 0.5670 0.469 Uiso 1 1 calc R . . C81 C 0.580(3) -0.071(3) 1.544(4) 0.293(15) Uiso 0.50 1 d PD . . H81A H 0.5399 -0.1051 1.5986 0.352 Uiso 0.50 1 calc PR . . H81B H 0.6113 -0.1212 1.5168 0.352 Uiso 0.50 1 calc PR . . C82 C 0.5000 0.0000 1.5000 0.293(15) Uiso 1 2 d SD . . H82A H 0.4525 -0.0358 1.4975 0.440 Uiso 0.50 1 calc PR . . H82B H 0.5356 0.0354 1.4452 0.440 Uiso 0.50 1 calc PR . . H82C H 0.4604 0.0465 1.5287 0.440 Uiso 0.50 1 calc PR . . C90 C -0.2408(6) 0.4430(7) 1.1352(7) 0.044(3) Uani 1 1 d . . . C720 C 0.773(3) 0.053(2) 1.5380(19) 0.153(17) Uiso 0.60(3) 1 d P . . H72A H 0.6977 0.0699 1.5569 0.229 Uiso 0.60(3) 1 calc PR . . H72B H 0.7976 -0.0125 1.5726 0.229 Uiso 0.60(3) 1 calc PR . . H72C H 0.7909 0.0527 1.4825 0.229 Uiso 0.60(3) 1 calc PR . . C721 C 0.891(4) 0.054(3) 1.514(2) 0.118(19) Uiso 0.40(3) 1 d P . . H72D H 0.9604 0.0690 1.5014 0.177 Uiso 0.40(3) 1 calc PR . . H72E H 0.8774 0.0538 1.4660 0.177 Uiso 0.40(3) 1 calc PR . . H72F H 0.8858 -0.0098 1.5560 0.177 Uiso 0.40(3) 1 calc PR . . 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 0.0335(5) 0.0286(4) 0.0307(4) -0.0141(3) -0.0120(3) -0.0039(3) Fe1 0.0310(10) 0.0336(11) 0.0264(10) -0.0158(8) -0.0129(8) -0.0004(8) Fe2 0.0579(11) 0.0692(12) 0.0751(12) -0.0340(10) -0.0087(9) -0.0251(9) S1 0.089(3) 0.128(4) 0.210(5) -0.049(4) -0.071(3) -0.044(3) S2 0.0520(19) 0.0516(19) 0.112(3) -0.0283(19) -0.0149(19) -0.0105(15) S3 0.130(4) 0.118(3) 0.128(3) -0.089(3) 0.049(3) -0.081(3) S4 0.087(2) 0.058(2) 0.063(2) -0.0176(16) -0.0056(18) -0.0356(18) S5 0.077(2) 0.0612(19) 0.0478(18) -0.0194(15) -0.0191(15) -0.0134(16) O1 0.060(5) 0.052(5) 0.075(5) -0.031(4) 0.000(4) -0.030(4) O2 0.080(6) 0.081(6) 0.088(6) 0.000(5) -0.025(5) -0.043(5) N1 0.036(4) 0.035(4) 0.037(4) -0.020(4) -0.007(4) -0.012(4) N2 0.034(4) 0.031(4) 0.024(4) -0.008(3) -0.011(3) 0.001(3) N3 0.022(4) 0.028(4) 0.027(4) -0.012(3) -0.009(3) 0.001(3) N4 0.047(5) 0.035(5) 0.054(5) -0.011(4) -0.024(4) -0.007(4) N5 0.038(5) 0.023(4) 0.044(5) -0.005(4) -0.020(4) 0.005(4) N6 0.035(5) 0.038(5) 0.026(4) -0.017(3) -0.009(3) -0.003(4) N7 0.023(4) 0.029(4) 0.031(4) -0.013(3) -0.004(3) -0.001(3) N8 0.037(5) 0.022(4) 0.024(4) -0.010(3) -0.005(3) -0.008(3) N9 0.034(4) 0.032(4) 0.025(4) -0.011(3) -0.013(3) -0.007(3) N10 0.024(4) 0.055(5) 0.023(4) -0.024(4) -0.001(3) -0.003(4) N11 0.043(5) 0.032(4) 0.029(4) -0.018(3) -0.012(4) -0.002(4) N12 0.033(4) 0.032(4) 0.029(4) -0.015(3) -0.013(4) 0.000(3) N13 0.035(5) 0.039(5) 0.039(5) -0.022(4) -0.021(4) 0.002(4) N14 0.060(7) 0.088(8) 0.086(8) -0.046(6) 0.001(6) -0.035(6) N15 0.063(7) 0.085(8) 0.091(8) -0.051(7) -0.012(6) -0.011(6) N16 0.063(7) 0.087(8) 0.098(9) -0.037(7) -0.024(6) -0.030(6) N17 0.045(5) 0.065(6) 0.037(5) -0.021(5) -0.008(4) 0.005(4) C1 0.052(6) 0.040(6) 0.040(6) -0.017(5) -0.013(5) -0.014(5) C2 0.054(7) 0.046(7) 0.051(7) -0.031(5) -0.014(5) -0.013(5) C3 0.065(7) 0.036(6) 0.057(7) -0.027(5) -0.008(6) -0.015(6) C4 0.041(6) 0.032(6) 0.030(5) -0.012(4) -0.005(4) -0.004(4) C5 0.034(5) 0.025(5) 0.032(5) -0.008(4) -0.017(4) 0.004(4) C6 0.023(5) 0.028(5) 0.034(5) -0.013(4) -0.007(4) -0.003(4) C7 0.046(6) 0.021(5) 0.044(6) -0.008(4) -0.021(5) 0.001(4) C8 0.027(5) 0.036(6) 0.040(6) -0.015(4) -0.017(4) 0.006(4) C9 0.043(6) 0.034(6) 0.045(6) -0.007(5) -0.018(5) -0.002(5) C10 0.030(5) 0.035(5) 0.031(5) -0.011(4) -0.017(4) 0.001(4) C11 0.031(5) 0.042(6) 0.049(6) -0.019(5) -0.022(5) 0.003(5) C12 0.037(6) 0.044(6) 0.041(6) -0.014(5) -0.017(5) -0.008(5) C13 0.040(6) 0.043(6) 0.037(6) -0.009(5) -0.013(5) -0.008(5) C14 0.025(5) 0.043(6) 0.050(6) -0.003(5) -0.010(5) -0.007(5) C15 0.033(5) 0.031(5) 0.037(5) -0.010(4) -0.011(4) -0.008(4) C16 0.026(5) 0.027(5) 0.028(5) -0.013(4) -0.009(4) -0.005(4) C17 0.025(5) 0.034(5) 0.025(5) -0.013(4) -0.004(4) -0.001(4) C18 0.039(6) 0.030(5) 0.043(6) -0.009(4) -0.018(5) -0.008(4) C19 0.046(6) 0.025(5) 0.057(6) -0.013(5) -0.020(5) -0.012(5) C20 0.036(6) 0.032(6) 0.043(6) -0.007(5) -0.015(5) 0.002(4) C21 0.029(5) 0.027(5) 0.035(5) -0.009(4) -0.014(4) 0.003(4) C22 0.036(6) 0.029(5) 0.036(6) -0.005(4) -0.010(5) -0.009(4) C23 0.041(6) 0.036(6) 0.042(6) -0.016(5) -0.002(5) -0.001(5) C24 0.047(6) 0.047(6) 0.033(6) -0.027(5) 0.000(5) -0.009(5) C25 0.035(5) 0.031(5) 0.029(5) -0.019(4) -0.001(4) -0.005(4) C26 0.023(5) 0.033(5) 0.027(5) -0.019(4) -0.001(4) -0.008(4) C27 0.035(5) 0.032(5) 0.024(5) -0.011(4) -0.009(4) -0.015(4) C28 0.034(5) 0.033(5) 0.028(5) -0.013(4) -0.002(4) -0.008(4) C29 0.027(5) 0.032(5) 0.025(5) -0.015(4) -0.008(4) -0.002(4) C30 0.033(5) 0.048(6) 0.024(5) -0.014(4) -0.015(4) 0.002(4) C31 0.046(6) 0.029(5) 0.026(5) -0.010(4) -0.014(5) -0.010(4) C32 0.028(5) 0.047(6) 0.041(6) -0.021(5) -0.021(5) 0.008(4) C33 0.028(5) 0.059(6) 0.029(5) -0.024(5) -0.010(4) -0.002(5) C34 0.031(5) 0.038(5) 0.028(5) -0.018(4) -0.010(4) 0.000(4) C35 0.032(5) 0.032(5) 0.037(6) -0.013(4) -0.013(4) -0.002(4) C36 0.027(5) 0.042(6) 0.026(5) -0.018(4) -0.009(4) -0.003(4) C37 0.028(5) 0.031(5) 0.029(5) -0.013(4) -0.008(4) -0.012(4) C38 0.028(5) 0.024(5) 0.029(5) -0.013(4) -0.009(4) -0.004(4) C39 0.027(5) 0.047(6) 0.041(6) -0.028(5) -0.006(4) -0.007(4) C40 0.047(6) 0.047(6) 0.030(6) -0.019(5) -0.008(5) -0.013(5) C41 0.061(7) 0.043(6) 0.011(5) -0.009(4) -0.007(5) -0.014(5) C42 0.043(6) 0.040(6) 0.031(5) -0.012(4) -0.020(5) -0.010(5) C50 0.057(7) 0.048(7) 0.071(8) -0.027(6) -0.027(6) -0.004(6) C60 0.051(7) 0.046(7) 0.058(7) -0.023(5) -0.012(6) -0.016(6) C61 0.069(9) 0.089(10) 0.081(10) -0.046(8) 0.035(7) -0.058(8) C62 0.064(8) 0.060(8) 0.060(8) -0.025(6) -0.002(6) -0.039(7) C63 0.092(10) 0.064(9) 0.098(10) -0.040(8) -0.017(8) -0.030(8) C64 0.091(11) 0.097(12) 0.127(13) -0.071(10) 0.020(10) -0.010(9) C65 0.115(10) 0.157(12) 0.095(9) 0.003(8) -0.036(8) -0.068(9) C66 0.115(10) 0.157(12) 0.095(9) 0.003(8) -0.036(8) -0.068(9) C90 0.014(5) 0.053(7) 0.059(7) -0.018(6) -0.009(5) 0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N8 1.958(7) . ? Ru1 N2 1.970(7) . ? Ru1 N3 2.043(7) . ? Ru1 N7 2.053(7) . ? Ru1 N9 2.056(7) . ? Ru1 N1 2.059(7) . ? Fe1 N13 2.117(8) 2_566 ? Fe1 N13 2.117(8) . ? Fe1 N12 2.171(7) . ? Fe1 N12 2.171(7) 2_566 ? Fe1 N6 2.245(7) 1_464 ? Fe1 N6 2.245(7) 2_657 ? Fe2 O1 1.968(8) 2_557 ? Fe2 O1 1.984(7) . ? Fe2 N16 2.010(12) . ? Fe2 N14 2.024(10) . ? Fe2 N15 2.026(11) . ? Fe2 O2 2.163(8) . ? S1 C50 1.646(12) . ? S2 C60 1.594(11) . ? S3 C61 1.615(14) . ? S4 C62 1.597(14) . ? S5 C90 1.626(12) . ? O1 C63 1.422(13) . ? O1 Fe2 1.968(8) 2_557 ? O2 C65 1.308(15) . ? O70 C71 1.53(2) . ? O70 H70 0.8400 . ? O76 C75 1.512(18) . ? O76 H76 0.8400 . ? O77 C78 1.441(17) . ? O77 H77 0.8400 . ? O80 C81 1.51(2) . ? O730 O731 0.83(3) . ? N1 C1 1.329(10) . ? N1 C5 1.366(10) . ? N2 C6 1.342(10) . ? N2 C16 1.343(10) . ? N3 C21 1.333(10) . ? N3 C17 1.379(10) . ? N4 N5 1.351(10) . ? N4 C8 1.364(10) . ? N4 H4 0.8800 . ? N5 C9 1.284(11) . ? N6 C13 1.317(11) . ? N6 C12 1.338(10) . ? N6 Fe1 2.245(7) 1_646 ? N7 C22 1.332(10) . ? N7 C26 1.361(10) . ? N8 C27 1.347(10) . ? N8 C37 1.356(10) . ? N9 C42 1.345(10) . ? N9 C38 1.351(10) . ? N10 N11 1.334(9) . ? N10 C29 1.372(10) . ? N10 H10 0.8800 . ? N11 C30 1.254(10) . ? N12 C34 1.332(10) . ? N12 C33 1.340(10) . ? N13 C50 1.134(11) . ? N14 C60 1.133(12) . ? N15 C61 1.132(14) . ? N16 C62 1.166(14) . ? N17 C90 1.156(12) . ? C1 C2 1.345(13) . ? C1 H1 0.9500 . ? C2 C3 1.365(13) . ? C2 H2 0.9500 . ? C3 C4 1.373(12) . ? C3 H3 0.9500 . ? C4 C5 1.348(11) . ? C4 H4A 0.9500 . ? C5 C6 1.474(11) . ? C6 C7 1.380(11) . ? C7 C8 1.393(12) . ? C7 H7 0.9500 . ? C8 C15 1.399(12) . ? C9 C10 1.452(12) . ? C9 H9 0.9500 . ? C10 C14 1.369(11) . ? C10 C11 1.392(12) . ? C11 C12 1.374(12) . ? C11 H11A 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.366(13) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.374(11) . ? C15 H15 0.9500 . ? C16 C17 1.458(11) . ? C17 C18 1.382(11) . ? C18 C19 1.360(12) . ? C18 H18 0.9500 . ? C19 C20 1.392(12) . ? C19 H19 0.9500 . ? C20 C21 1.366(12) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.383(12) . ? C22 H22 0.9500 . ? C23 C24 1.365(12) . ? C23 H23 0.9500 . ? C24 C25 1.366(12) . ? C24 H24 0.9500 . ? C25 C26 1.378(11) . ? C25 H25 0.9500 . ? C26 C27 1.453(11) . ? C27 C28 1.359(11) . ? C28 C29 1.389(11) . ? C28 H28 0.9500 . ? C29 C36 1.390(11) . ? C30 C31 1.448(11) . ? C30 H30 0.9500 . ? C31 C35 1.370(11) . ? C31 C32 1.385(12) . ? C32 C33 1.365(11) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.366(11) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.379(11) . ? C36 H36 0.9500 . ? C37 C38 1.478(11) . ? C38 C39 1.390(11) . ? C39 C40 1.361(12) . ? C39 H39 0.9500 . ? C40 C41 1.358(12) . ? C40 H40 0.9500 . ? C41 C42 1.353(12) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C63 C64 1.522(16) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C66 1.398(17) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C71 C721 1.31(4) . ? C71 C720 1.40(3) . ? C74 C75 1.467(19) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C78 C79 1.385(18) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C81 C82 1.51(2) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C720 H72A 0.9800 . ? C720 H72B 0.9800 . ? C720 H72C 0.9800 . ? C721 H72D 0.9800 . ? C721 H72E 0.9800 . ? C721 H72F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 Ru1 N2 178.2(3) . . ? N8 Ru1 N3 100.7(3) . . ? N2 Ru1 N3 78.9(3) . . ? N8 Ru1 N7 78.6(3) . . ? N2 Ru1 N7 103.2(3) . . ? N3 Ru1 N7 91.2(3) . . ? N8 Ru1 N9 79.3(3) . . ? N2 Ru1 N9 98.9(3) . . ? N3 Ru1 N9 93.9(3) . . ? N7 Ru1 N9 157.9(3) . . ? N8 Ru1 N1 101.4(3) . . ? N2 Ru1 N1 79.0(3) . . ? N3 Ru1 N1 157.9(3) . . ? N7 Ru1 N1 92.9(3) . . ? N9 Ru1 N1 90.5(3) . . ? N13 Fe1 N13 180.00(11) 2_566 . ? N13 Fe1 N12 90.9(3) 2_566 . ? N13 Fe1 N12 89.1(3) . . ? N13 Fe1 N12 89.1(3) 2_566 2_566 ? N13 Fe1 N12 90.9(3) . 2_566 ? N12 Fe1 N12 180.000(1) . 2_566 ? N13 Fe1 N6 89.1(3) 2_566 1_464 ? N13 Fe1 N6 90.9(3) . 1_464 ? N12 Fe1 N6 92.6(2) . 1_464 ? N12 Fe1 N6 87.4(2) 2_566 1_464 ? N13 Fe1 N6 90.9(3) 2_566 2_657 ? N13 Fe1 N6 89.1(3) . 2_657 ? N12 Fe1 N6 87.4(2) . 2_657 ? N12 Fe1 N6 92.6(2) 2_566 2_657 ? N6 Fe1 N6 180.000(1) 1_464 2_657 ? O1 Fe2 O1 75.3(3) 2_557 . ? O1 Fe2 N16 169.2(3) 2_557 . ? O1 Fe2 N16 97.1(4) . . ? O1 Fe2 N14 94.9(4) 2_557 . ? O1 Fe2 N14 92.9(3) . . ? N16 Fe2 N14 93.1(4) . . ? O1 Fe2 N15 94.1(4) 2_557 . ? O1 Fe2 N15 168.1(4) . . ? N16 Fe2 N15 92.7(4) . . ? N14 Fe2 N15 93.3(4) . . ? O1 Fe2 O2 83.4(3) 2_557 . ? O1 Fe2 O2 85.2(3) . . ? N16 Fe2 O2 88.5(4) . . ? N14 Fe2 O2 177.7(4) . . ? N15 Fe2 O2 88.3(4) . . ? C63 O1 Fe2 129.0(7) . 2_557 ? C63 O1 Fe2 125.6(7) . . ? Fe2 O1 Fe2 104.7(3) 2_557 . ? C65 O2 Fe2 132.1(9) . . ? C71 O70 H70 109.5 . . ? C75 O76 H76 109.5 . . ? C78 O77 H77 109.5 . . ? C1 N1 C5 117.4(8) . . ? C1 N1 Ru1 127.9(6) . . ? C5 N1 Ru1 114.7(5) . . ? C6 N2 C16 121.0(7) . . ? C6 N2 Ru1 118.8(6) . . ? C16 N2 Ru1 120.1(6) . . ? C21 N3 C17 118.4(7) . . ? C21 N3 Ru1 128.1(6) . . ? C17 N3 Ru1 113.5(5) . . ? N5 N4 C8 119.4(7) . . ? N5 N4 H4 120.3 . . ? C8 N4 H4 120.3 . . ? C9 N5 N4 116.5(8) . . ? C13 N6 C12 116.0(8) . . ? C13 N6 Fe1 121.6(6) . 1_646 ? C12 N6 Fe1 122.3(6) . 1_646 ? C22 N7 C26 118.5(7) . . ? C22 N7 Ru1 127.3(6) . . ? C26 N7 Ru1 114.1(5) . . ? C27 N8 C37 121.0(7) . . ? C27 N8 Ru1 119.7(6) . . ? C37 N8 Ru1 119.2(5) . . ? C42 N9 C38 117.6(7) . . ? C42 N9 Ru1 128.1(6) . . ? C38 N9 Ru1 114.2(5) . . ? N11 N10 C29 119.2(7) . . ? N11 N10 H10 120.4 . . ? C29 N10 H10 120.4 . . ? C30 N11 N10 118.8(7) . . ? C34 N12 C33 116.6(7) . . ? C34 N12 Fe1 122.4(5) . . ? C33 N12 Fe1 120.5(6) . . ? C50 N13 Fe1 168.2(8) . . ? C60 N14 Fe2 166.5(11) . . ? C61 N15 Fe2 172.4(10) . . ? C62 N16 Fe2 153.8(10) . . ? N1 C1 C2 122.9(9) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C1 C2 C3 120.5(9) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C2 C3 C4 117.1(9) . . ? C2 C3 H3 121.4 . . ? C4 C3 H3 121.4 . . ? C5 C4 C3 120.9(9) . . ? C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C4 C5 N1 121.1(8) . . ? C4 C5 C6 125.1(8) . . ? N1 C5 C6 113.8(7) . . ? N2 C6 C7 121.3(8) . . ? N2 C6 C5 113.6(7) . . ? C7 C6 C5 125.1(8) . . ? C6 C7 C8 117.8(8) . . ? C6 C7 H7 121.1 . . ? C8 C7 H7 121.1 . . ? N4 C8 C7 121.9(8) . . ? N4 C8 C15 117.4(8) . . ? C7 C8 C15 120.7(8) . . ? N5 C9 C10 120.6(9) . . ? N5 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C14 C10 C11 117.4(8) . . ? C14 C10 C9 120.9(9) . . ? C11 C10 C9 121.7(8) . . ? C12 C11 C10 118.4(8) . . ? C12 C11 H11A 120.8 . . ? C10 C11 H11A 120.8 . . ? N6 C12 C11 124.1(9) . . ? N6 C12 H12 118.0 . . ? C11 C12 H12 118.0 . . ? N6 C13 C14 124.4(9) . . ? N6 C13 H13 117.8 . . ? C14 C13 H13 117.8 . . ? C13 C14 C10 119.7(9) . . ? C13 C14 H14 120.2 . . ? C10 C14 H14 120.2 . . ? C16 C15 C8 117.7(8) . . ? C16 C15 H15 121.1 . . ? C8 C15 H15 121.1 . . ? N2 C16 C15 121.4(8) . . ? N2 C16 C17 111.5(7) . . ? C15 C16 C17 127.1(8) . . ? N3 C17 C18 119.6(8) . . ? N3 C17 C16 115.8(7) . . ? C18 C17 C16 124.6(8) . . ? C19 C18 C17 121.4(8) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C18 C19 C20 118.2(8) . . ? C18 C19 H19 120.9 . . ? C20 C19 H19 120.9 . . ? C21 C20 C19 119.0(8) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? N3 C21 C20 123.3(8) . . ? N3 C21 H21 118.4 . . ? C20 C21 H21 118.4 . . ? N7 C22 C23 122.6(8) . . ? N7 C22 H22 118.7 . . ? C23 C22 H22 118.7 . . ? C24 C23 C22 118.8(9) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C23 C24 C25 119.2(9) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C24 C25 C26 120.3(8) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? N7 C26 C25 120.5(7) . . ? N7 C26 C27 115.2(7) . . ? C25 C26 C27 124.3(8) . . ? N8 C27 C28 120.5(8) . . ? N8 C27 C26 112.2(7) . . ? C28 C27 C26 127.3(8) . . ? C27 C28 C29 120.1(8) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? N10 C29 C28 121.9(7) . . ? N10 C29 C36 119.0(7) . . ? C28 C29 C36 119.0(8) . . ? N11 C30 C31 120.6(8) . . ? N11 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C35 C31 C32 118.1(8) . . ? C35 C31 C30 122.2(8) . . ? C32 C31 C30 119.8(8) . . ? C33 C32 C31 119.1(8) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? N12 C33 C32 123.3(8) . . ? N12 C33 H33 118.4 . . ? C32 C33 H33 118.4 . . ? N12 C34 C35 123.9(8) . . ? N12 C34 H34 118.1 . . ? C35 C34 H34 118.1 . . ? C34 C35 C31 119.1(8) . . ? C34 C35 H35 120.5 . . ? C31 C35 H35 120.5 . . ? C37 C36 C29 119.1(8) . . ? C37 C36 H36 120.5 . . ? C29 C36 H36 120.5 . . ? N8 C37 C36 120.3(7) . . ? N8 C37 C38 112.0(7) . . ? C36 C37 C38 127.7(8) . . ? N9 C38 C39 121.5(7) . . ? N9 C38 C37 115.2(7) . . ? C39 C38 C37 123.2(7) . . ? C40 C39 C38 119.1(8) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? C41 C40 C39 119.1(9) . . ? C41 C40 H40 120.4 . . ? C39 C40 H40 120.4 . . ? C42 C41 C40 120.2(8) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? N9 C42 C41 122.4(8) . . ? N9 C42 H42 118.8 . . ? C41 C42 H42 118.8 . . ? N13 C50 S1 179.0(10) . . ? N14 C60 S2 179.3(10) . . ? N15 C61 S3 173.6(15) . . ? N16 C62 S4 178.2(11) . . ? O1 C63 C64 111.4(10) . . ? O1 C63 H63A 109.4 . . ? C64 C63 H63A 109.4 . . ? O1 C63 H63B 109.4 . . ? C64 C63 H63B 109.4 . . ? H63A C63 H63B 108.0 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? O2 C65 C66 124.8(15) . . ? O2 C65 H65A 106.1 . . ? C66 C65 H65A 106.1 . . ? O2 C65 H65B 106.1 . . ? C66 C65 H65B 106.1 . . ? H65A C65 H65B 106.3 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C721 C71 C720 69(2) . . ? C721 C71 O70 115(3) . . ? C720 C71 O70 113(2) . . ? C75 C74 H74A 109.5 . . ? C75 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C75 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C74 C75 O76 118(3) . . ? C74 C75 H75A 107.7 . . ? O76 C75 H75A 107.7 . . ? C74 C75 H75B 107.7 . . ? O76 C75 H75B 107.7 . . ? H75A C75 H75B 107.1 . . ? C79 C78 O77 125(2) . . ? C79 C78 H78A 106.0 . . ? O77 C78 H78A 106.0 . . ? C79 C78 H78B 106.0 . . ? O77 C78 H78B 106.0 . . ? H78A C78 H78B 106.3 . . ? C78 C79 H79A 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C78 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? O80 C81 C82 125(3) . . ? O80 C81 H81A 106.2 . . ? C82 C81 H81A 106.2 . . ? O80 C81 H81B 106.2 . . ? C82 C81 H81B 106.2 . . ? H81A C81 H81B 106.4 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N17 C90 S5 178.2(9) . . ? C71 C720 H72A 109.5 . . ? C71 C720 H72B 109.5 . . ? H72A C720 H72B 109.5 . . ? C71 C720 H72C 109.5 . . ? H72A C720 H72C 109.5 . . ? H72B C720 H72C 109.5 . . ? C71 C721 H72D 109.5 . . ? C71 C721 H72E 109.5 . . ? H72D C721 H72E 109.5 . . ? C71 C721 H72F 109.5 . . ? H72D C721 H72F 109.5 . . ? H72E C721 H72F 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4 O730 0.88 1.92 2.80(2) 177.4 . N4 H4 O731 0.88 2.08 2.894(16) 154.0 . N10 H10 N17 0.88 2.01 2.893(11) 177.0 . O77 H77 O76 0.84 2.27 2.92(3) 134.3 . O76 H76 O731 0.84 2.52 3.28(4) 150.0 1_554 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.999 _refine_diff_density_min -0.905 _refine_diff_density_rms 0.140 # Attachment 'Ru[H2_1_]2_MN.cif' data_jb984 _database_code_depnum_ccdc_archive 'CCDC 692942' _audit_creation_date 07-11-14 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '11131708 jb984_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 11.0743(1) _cell_length_b 14.7284(1) _cell_length_c 15.5483(2) _cell_angle_alpha 77.6715(5) _cell_angle_beta 88.2000(5) _cell_angle_gamma 68.6393(5) _cell_volume 2304.36(4) _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 57.7998 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' 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' _cell_formula_units_Z 2 # Given Formula = C88 H88 N30 O30 Ru2 # Dc = 3.24 Fooo = 1136.00 Mu = 8.60 M = 2247.99 # Found Formula = C42 H40 N16 O15 Ru1 # Dc = 1.60 FOOO = 1136.00 Mu = 4.30 M = 1109.95 _chemical_formula_sum 'C42 H40 N16 O15 Ru1' _chemical_formula_moiety 'C42 H34 N12 Ru, 4(N O3), 3(H2 O)' _chemical_compound_source ? _chemical_formula_weight 1109.95 _cell_measurement_reflns_used 10973 _cell_measurement_theta_min 1 _cell_measurement_theta_max 28 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_min 0.09 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_max 0.36 _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.430 # Sheldrick geometric approximatio 0.89 0.96 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.96 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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 21783 _reflns_number_total 10975 _diffrn_reflns_av_R_equivalents 0.023 # Number of reflections with Friedels Law is 10975 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 10972 _diffrn_reflns_theta_min 1.342 _diffrn_reflns_theta_max 27.857 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.857 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _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 -14 _reflns_limit_h_max 14 _reflns_limit_k_min -18 _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 -0.64 _refine_diff_density_max 0.66 _refine_ls_number_reflns 9207 _refine_ls_number_restraints 0 _refine_ls_number_parameters 667 #_refine_ls_R_factor_ref 0.0309 _refine_ls_wR_factor_ref 0.0356 _refine_ls_goodness_of_fit_ref 1.0958 #_reflns_number_all 10901 _refine_ls_R_factor_all 0.0375 _refine_ls_wR_factor_all 0.0420 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 9207 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_gt 0.0356 _refine_ls_shift/su_max 0.001980 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.428 0.218 0.170 ; _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fih. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: 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 atomsattached 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 0.494871(13) 0.250876(10) 0.243638(8) 0.0196 1.0000 Uani . . . . . . N1 N 0.42372(13) 0.19760(10) 0.36046(9) 0.0209 1.0000 Uani . . . . . . N2 N 0.54143(13) 0.32317(10) 0.32306(9) 0.0204 1.0000 Uani . . . . . . N3 N 0.58275(14) 0.33432(11) 0.15794(9) 0.0232 1.0000 Uani . . . . . . N4 N 0.65837(14) 0.12285(11) 0.27025(9) 0.0213 1.0000 Uani . . . . . . N5 N 0.45172(13) 0.17003(10) 0.17180(9) 0.0193 1.0000 Uani . . . . . . N6 N 0.31468(14) 0.34730(11) 0.18938(9) 0.0222 1.0000 Uani . . . . . . N7 N 0.67209(15) 0.44589(12) 0.49739(10) 0.0268 1.0000 Uani . . . . . . N8 N 0.74075(15) 0.50407(11) 0.46927(10) 0.0254 1.0000 Uani . . . . . . N9 N 1.01450(17) 0.70746(12) 0.44977(11) 0.0323 1.0000 Uani . . . . . . N10 N 0.34946(14) -0.01465(11) 0.04817(10) 0.0245 1.0000 Uani . . . . . . N11 N 0.23762(14) 0.01953(12) -0.00110(9) 0.0242 1.0000 Uani . . . . . . N12 N -0.13289(16) 0.04554(14) -0.18985(11) 0.0348 1.0000 Uani . . . . . . N13 N 0.81913(16) 0.14802(12) 0.54477(11) 0.0302 1.0000 Uani . . . . . . N14 N 0.9805(2) 0.27910(17) 0.24723(13) 0.0457 1.0000 Uani . . . . . . N15 N 0.3437(2) 0.63932(14) 0.27169(13) 0.0484 1.0000 Uani . . . . . . N16 N 0.8211(2) 0.71116(13) 0.12766(13) 0.0411 1.0000 Uani . . . . . . C1 C 0.36115(18) 0.13297(14) 0.37440(12) 0.0270 1.0000 Uani . . . . . . C2 C 0.3272(2) 0.09680(15) 0.45780(14) 0.0327 1.0000 Uani . . . . . . C3 C 0.3581(2) 0.12809(15) 0.52867(13) 0.0323 1.0000 Uani . . . . . . C4 C 0.42024(18) 0.19597(14) 0.51525(12) 0.0269 1.0000 Uani . . . . . . C5 C 0.45213(16) 0.22988(12) 0.43057(11) 0.0212 1.0000 Uani . . . . . . C6 C 0.51983(16) 0.30118(12) 0.40950(11) 0.0203 1.0000 Uani . . . . . . C7 C 0.56194(16) 0.34253(13) 0.46883(11) 0.0227 1.0000 Uani . . . . . . C8 C 0.62954(16) 0.40550(13) 0.43725(11) 0.0231 1.0000 Uani . . . . . . C9 C 0.65397(17) 0.42575(13) 0.34764(12) 0.0246 1.0000 Uani . . . . . . C10 C 0.60715(16) 0.38368(12) 0.29168(11) 0.0221 1.0000 Uani . . . . . . C11 C 0.62344(17) 0.39471(13) 0.19578(11) 0.0238 1.0000 Uani . . . . . . C12 C 0.6754(2) 0.46080(15) 0.14625(13) 0.0317 1.0000 Uani . . . . . . C13 C 0.6897(2) 0.46397(17) 0.05714(13) 0.0380 1.0000 Uani . . . . . . C14 C 0.6518(2) 0.40105(17) 0.01915(13) 0.0373 1.0000 Uani . . . . . . C15 C 0.59788(19) 0.33804(15) 0.07120(12) 0.0303 1.0000 Uani . . . . . . C16 C 0.76223(17) 0.10472(14) 0.32309(12) 0.0274 1.0000 Uani . . . . . . C17 C 0.86354(18) 0.01302(15) 0.34136(12) 0.0306 1.0000 Uani . . . . . . C18 C 0.85831(18) -0.06201(14) 0.30361(12) 0.0291 1.0000 Uani . . . . . . C19 C 0.75177(17) -0.04493(13) 0.24897(11) 0.0252 1.0000 Uani . . . . . . C20 C 0.65246(16) 0.04794(12) 0.23303(10) 0.0205 1.0000 Uani . . . . . . C21 C 0.53366(16) 0.07480(12) 0.17685(10) 0.0201 1.0000 Uani . . . . . . C22 C 0.50149(17) 0.01234(13) 0.13471(11) 0.0223 1.0000 Uani . . . . . . C23 C 0.38132(17) 0.04966(13) 0.08765(10) 0.0216 1.0000 Uani . . . . . . C24 C 0.29633(16) 0.14806(13) 0.08373(11) 0.0223 1.0000 Uani . . . . . . C25 C 0.33466(16) 0.20663(12) 0.12777(10) 0.0204 1.0000 Uani . . . . . . C26 C 0.25670(16) 0.30993(13) 0.13630(11) 0.0219 1.0000 Uani . . . . . . C27 C 0.13424(18) 0.36547(14) 0.09639(12) 0.0274 1.0000 Uani . . . . . . C28 C 0.06895(19) 0.46086(15) 0.11103(13) 0.0336 1.0000 Uani . . . . . . C29 C 0.1294(2) 0.49913(15) 0.16282(13) 0.0343 1.0000 Uani . . . . . . C30 C 0.25160(19) 0.44075(13) 0.20061(12) 0.0278 1.0000 Uani . . . . . . C31 C 0.77943(17) 0.53985(13) 0.52713(12) 0.0260 1.0000 Uani . . . . . . C32 C 0.85829(17) 0.59980(13) 0.49911(12) 0.0258 1.0000 Uani . . . . . . C33 C 0.90597(19) 0.63685(15) 0.56044(13) 0.0303 1.0000 Uani . . . . . . C34 C 0.9839(2) 0.69100(15) 0.53362(13) 0.0328 1.0000 Uani . . . . . . C35 C 0.9704(2) 0.67320(15) 0.38849(13) 0.0332 1.0000 Uani . . . . . . C36 C 0.89128(19) 0.62016(14) 0.41148(13) 0.0302 1.0000 Uani . . . . . . C37 C 0.20972(17) -0.04466(14) -0.03302(12) 0.0256 1.0000 Uani . . . . . . C38 C 0.09004(18) -0.01201(14) -0.08716(11) 0.0266 1.0000 Uani . . . . . . C39 C 0.00753(19) 0.08843(15) -0.10925(13) 0.0308 1.0000 Uani . . . . . . C40 C -0.1037(2) 0.11504(17) -0.16061(13) 0.0359 1.0000 Uani . . . . . . C41 C -0.05626(19) -0.05080(17) -0.17071(13) 0.0331 1.0000 Uani . . . . . . C42 C 0.05654(19) -0.08210(15) -0.11894(12) 0.0291 1.0000 Uani . . . . . . O1 O 0.82800(15) 0.18669(12) 0.60817(9) 0.0375 1.0000 Uani . . . . . . O2 O 0.74437(16) 0.10144(12) 0.54821(10) 0.0417 1.0000 Uani . . . . . . O3 O 0.88316(19) 0.15795(16) 0.48001(11) 0.0538 1.0000 Uani . . . . . . O4 O 0.9355(2) 0.36069(16) 0.27147(12) 0.0591 1.0000 Uani . . . . . . O5 O 1.0860(2) 0.21563(17) 0.27834(14) 0.0668 1.0000 Uani . . . . . . O6 O 0.9245(3) 0.26572(19) 0.1867(2) 0.0964 1.0000 Uani . . . . . . O7 O 0.35020(19) 0.67245(15) 0.19226(11) 0.0526 1.0000 Uani . . . . . . O8 O 0.4322(2) 0.62600(18) 0.32571(13) 0.0786 1.0000 Uani . . . . . . O9 O 0.2452(3) 0.62119(19) 0.29743(16) 0.0872 1.0000 Uani . . . . . . O10 O 0.7930(4) 0.7469(2) 0.19310(18) 0.1053 1.0000 Uani . . . . . . O11 O 0.91870(17) 0.71491(13) 0.08704(13) 0.0508 1.0000 Uani . . . . . . O12 O 0.75380(18) 0.67023(14) 0.10044(13) 0.0510 1.0000 Uani . . . . . . O13 O 0.48410(15) 0.77570(11) 0.07589(10) 0.0364 1.0000 Uani . . . . . . O14 O 0.34814(15) 0.92351(14) 0.28469(10) 0.0447 1.0000 Uani . . . . . . O15 O 0.5704(2) 0.7555(2) 0.28783(14) 0.0788 1.0000 Uani . . . . . . H1 H 0.6566 0.4323 0.5527 0.0372 1.0000 Uiso R . . . . . H2 H 1.0649 0.7399 0.4340 0.0410 1.0000 Uiso R . . . . . H3 H 0.4002 -0.0769 0.0564 0.0319 1.0000 Uiso R . . . . . H4 H -0.2047 0.0643 -0.2221 0.0427 1.0000 Uiso R . . . . . H5 H 0.4531 0.7443 0.1139 0.0545 1.0000 Uiso R . . . . . H6 H 0.5619 0.7500 0.0860 0.0546 1.0000 Uiso R . . . . . H7 H 0.4089 0.8731 0.2795 0.0674 1.0000 Uiso R . . . . . H8 H 0.3265 0.9129 0.3364 0.0669 1.0000 Uiso R . . . . . H9 H 0.6318 0.7496 0.2569 0.1087 1.0000 Uiso R . . . . . H10 H 0.5519 0.7065 0.2890 0.1089 1.0000 Uiso R . . . . . H11 H 0.3433 0.1117 0.3256 0.0348 1.0000 Uiso R . . . . . H21 H 0.2848 0.0521 0.4647 0.0411 1.0000 Uiso R . . . . . H31 H 0.3363 0.1051 0.5847 0.0401 1.0000 Uiso R . . . . . H41 H 0.4398 0.2187 0.5621 0.0329 1.0000 Uiso R . . . . . H71 H 0.5450 0.3298 0.5285 0.0285 1.0000 Uiso R . . . . . H91 H 0.7000 0.4666 0.3262 0.0303 1.0000 Uiso R . . . . . H121 H 0.7016 0.5027 0.1736 0.0387 1.0000 Uiso R . . . . . H131 H 0.7253 0.5086 0.0234 0.0458 1.0000 Uiso R . . . . . H141 H 0.6614 0.4002 -0.0411 0.0447 1.0000 Uiso R . . . . . H151 H 0.5696 0.2961 0.0470 0.0355 1.0000 Uiso R . . . . . H161 H 0.7623 0.1580 0.3487 0.0329 1.0000 Uiso R . . . . . H171 H 0.9322 0.0030 0.3797 0.0335 1.0000 Uiso R . . . . . H181 H 0.9259 -0.1246 0.3147 0.0331 1.0000 Uiso R . . . . . H191 H 0.7469 -0.0949 0.2236 0.0294 1.0000 Uiso R . . . . . H221 H 0.5580 -0.0529 0.1380 0.0279 1.0000 Uiso R . . . . . H241 H 0.2159 0.1733 0.0516 0.0283 1.0000 Uiso R . . . . . H271 H 0.0963 0.3388 0.0610 0.0326 1.0000 Uiso R . . . . . H281 H -0.0150 0.4989 0.0863 0.0375 1.0000 Uiso R . . . . . H291 H 0.0894 0.5647 0.1718 0.0392 1.0000 Uiso R . . . . . H301 H 0.2946 0.4655 0.2370 0.0312 1.0000 Uiso R . . . . . H311 H 0.7600 0.5255 0.5869 0.0329 1.0000 Uiso R . . . . . H331 H 0.8846 0.6261 0.6195 0.0386 1.0000 Uiso R . . . . . H341 H 1.0154 0.7162 0.5740 0.0411 1.0000 Uiso R . . . . . H351 H 0.9976 0.6855 0.3308 0.0404 1.0000 Uiso R . . . . . H361 H 0.8607 0.5967 0.3692 0.0371 1.0000 Uiso R . . . . . H371 H 0.2642 -0.1129 -0.0220 0.0325 1.0000 Uiso R . . . . . H391 H 0.0278 0.1374 -0.0898 0.0374 1.0000 Uiso R . . . . . H401 H -0.1601 0.1819 -0.1758 0.0425 1.0000 Uiso R . . . . . H411 H -0.0779 -0.0972 -0.1934 0.0420 1.0000 Uiso R . . . . . H421 H 0.1115 -0.1515 -0.1057 0.0378 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 0.02140(7) 0.01937(7) 0.02103(7) -0.00605(5) -0.00125(4) -0.00973(5) N1 0.0209(6) 0.0206(7) 0.0236(7) -0.0053(5) -0.0008(5) -0.0101(5) N2 0.0208(6) 0.0205(7) 0.0225(6) -0.0056(5) -0.0001(5) -0.0101(5) N3 0.0242(7) 0.0240(7) 0.0227(7) -0.0045(5) -0.0010(5) -0.0103(6) N4 0.0210(6) 0.0223(7) 0.0210(6) -0.0047(5) -0.0018(5) -0.0082(5) N5 0.0206(6) 0.0192(6) 0.0201(6) -0.0048(5) -0.0007(5) -0.0091(5) N6 0.0247(7) 0.0203(7) 0.0228(6) -0.0053(5) -0.0011(5) -0.0092(6) N7 0.0333(8) 0.0315(8) 0.0264(7) -0.0101(6) 0.0022(6) -0.0223(7) N8 0.0246(7) 0.0249(7) 0.0320(7) -0.0089(6) -0.0008(6) -0.0135(6) N9 0.0346(8) 0.0287(8) 0.0386(9) -0.0004(7) -0.0075(7) -0.0205(7) N10 0.0247(7) 0.0252(7) 0.0277(7) -0.0103(6) -0.0014(6) -0.0112(6) N11 0.0248(7) 0.0301(8) 0.0223(7) -0.0085(6) 0.0011(5) -0.0137(6) N12 0.0276(8) 0.0517(11) 0.0270(8) -0.0053(7) -0.0023(6) -0.0182(8) N13 0.0309(8) 0.0298(8) 0.0340(8) -0.0043(6) -0.0045(6) -0.0170(7) N14 0.0412(10) 0.0562(12) 0.0411(10) -0.0106(9) -0.0023(8) -0.0189(9) N15 0.0782(15) 0.0289(9) 0.0364(10) -0.0105(7) 0.0169(10) -0.0171(10) N16 0.0461(11) 0.0279(9) 0.0466(10) -0.0081(7) -0.0046(8) -0.0099(8) C1 0.0308(9) 0.0270(9) 0.0310(9) -0.0096(7) 0.0010(7) -0.0176(7) C2 0.0373(10) 0.0301(9) 0.0393(10) -0.0063(8) 0.0036(8) -0.0230(8) C3 0.0369(10) 0.0367(10) 0.0286(9) -0.0036(7) 0.0055(7) -0.0217(9) C4 0.0299(9) 0.0303(9) 0.0255(8) -0.0072(7) 0.0008(7) -0.0162(7) C5 0.0205(7) 0.0210(8) 0.0247(8) -0.0068(6) -0.0007(6) -0.0093(6) C6 0.0199(7) 0.0210(8) 0.0224(7) -0.0066(6) 0.0007(6) -0.0092(6) C7 0.0236(8) 0.0247(8) 0.0229(7) -0.0066(6) 0.0005(6) -0.0117(7) C8 0.0213(8) 0.0248(8) 0.0276(8) -0.0108(6) -0.0015(6) -0.0103(7) C9 0.0254(8) 0.0241(8) 0.0292(8) -0.0072(7) 0.0013(6) -0.0141(7) C10 0.0228(8) 0.0211(8) 0.0246(8) -0.0040(6) 0.0002(6) -0.0110(6) C11 0.0245(8) 0.0240(8) 0.0250(8) -0.0049(6) -0.0018(6) -0.0111(7) C12 0.0368(10) 0.0352(10) 0.0284(9) -0.0027(7) -0.0001(7) -0.0216(8) C13 0.0437(11) 0.0450(12) 0.0291(9) 0.0010(8) 0.0023(8) -0.0256(10) C14 0.0454(12) 0.0464(12) 0.0221(8) -0.0035(8) 0.0032(8) -0.0215(10) C15 0.0355(10) 0.0331(10) 0.0239(8) -0.0069(7) 0.0000(7) -0.0138(8) C16 0.0240(8) 0.0319(9) 0.0272(8) -0.0069(7) -0.0045(7) -0.0104(7) C17 0.0244(8) 0.0376(10) 0.0271(8) -0.0031(7) -0.0058(7) -0.0099(8) C18 0.0250(8) 0.0295(9) 0.0273(8) -0.0007(7) -0.0003(7) -0.0065(7) C19 0.0268(8) 0.0238(8) 0.0248(8) -0.0043(6) 0.0026(6) -0.0098(7) C20 0.0219(7) 0.0226(8) 0.0186(7) -0.0038(6) 0.0011(6) -0.0104(6) C21 0.0228(7) 0.0224(8) 0.0177(7) -0.0048(6) 0.0022(6) -0.0111(6) C22 0.0248(8) 0.0210(8) 0.0237(8) -0.0071(6) 0.0029(6) -0.0103(6) C23 0.0256(8) 0.0264(8) 0.0188(7) -0.0080(6) 0.0033(6) -0.0148(7) C24 0.0232(8) 0.0252(8) 0.0215(7) -0.0060(6) -0.0003(6) -0.0116(7) C25 0.0216(7) 0.0223(8) 0.0191(7) -0.0045(6) -0.0003(6) -0.0101(6) C26 0.0239(8) 0.0234(8) 0.0198(7) -0.0047(6) -0.0006(6) -0.0103(7) C27 0.0263(8) 0.0291(9) 0.0250(8) -0.0047(7) -0.0045(7) -0.0082(7) C28 0.0286(9) 0.0323(10) 0.0316(9) -0.0078(8) -0.0060(7) -0.0006(8) C29 0.0372(10) 0.0238(9) 0.0356(10) -0.0092(7) -0.0034(8) -0.0021(8) C30 0.0323(9) 0.0226(8) 0.0288(8) -0.0088(7) -0.0021(7) -0.0082(7) C31 0.0275(8) 0.0262(9) 0.0296(8) -0.0097(7) -0.0003(7) -0.0138(7) C32 0.0248(8) 0.0220(8) 0.0328(9) -0.0068(7) -0.0034(7) -0.0103(7) C33 0.0354(10) 0.0316(9) 0.0304(9) -0.0070(7) -0.0039(7) -0.0191(8) C34 0.0386(10) 0.0311(10) 0.0350(10) -0.0043(8) -0.0089(8) -0.0207(8) C35 0.0402(11) 0.0316(10) 0.0317(9) -0.0039(7) -0.0019(8) -0.0191(8) C36 0.0349(10) 0.0283(9) 0.0324(9) -0.0065(7) -0.0045(7) -0.0170(8) C37 0.0263(8) 0.0295(9) 0.0262(8) -0.0097(7) 0.0018(7) -0.0141(7) C38 0.0270(8) 0.0356(10) 0.0227(8) -0.0082(7) 0.0030(6) -0.0170(8) C39 0.0310(9) 0.0352(10) 0.0302(9) -0.0091(7) 0.0031(7) -0.0159(8) C40 0.0322(10) 0.0415(11) 0.0308(9) -0.0045(8) 0.0016(8) -0.0117(9) C41 0.0315(10) 0.0484(12) 0.0281(9) -0.0095(8) 0.0012(7) -0.0242(9) C42 0.0299(9) 0.0364(10) 0.0271(8) -0.0088(7) 0.0005(7) -0.0180(8) O1 0.0480(9) 0.0466(9) 0.0333(7) -0.0136(6) 0.0022(6) -0.0326(7) O2 0.0521(9) 0.0477(9) 0.0440(8) -0.0125(7) 0.0029(7) -0.0388(8) O3 0.0691(12) 0.0807(13) 0.0442(9) -0.0281(9) 0.0186(8) -0.0583(11) O4 0.0630(12) 0.0691(13) 0.0464(10) -0.0246(9) -0.0014(8) -0.0183(10) O5 0.0497(11) 0.0728(14) 0.0637(12) -0.0095(10) -0.0179(9) -0.0072(10) O6 0.0825(16) 0.0678(15) 0.134(2) -0.0484(15) -0.0602(16) -0.0017(12) O7 0.0615(11) 0.0637(11) 0.0323(8) -0.0023(7) 0.0074(7) -0.0273(9) O8 0.0798(15) 0.0742(15) 0.0411(10) -0.0093(10) -0.0101(10) 0.0184(12) O9 0.151(2) 0.0894(17) 0.0737(14) -0.0471(13) 0.0649(16) -0.0932(18) O10 0.185(3) 0.098(2) 0.0787(17) -0.0623(16) 0.0505(19) -0.084(2) O11 0.0417(9) 0.0414(9) 0.0656(11) -0.0086(8) -0.0091(8) -0.0117(7) O12 0.0482(10) 0.0505(10) 0.0616(11) -0.0215(8) 0.0021(8) -0.0212(8) O13 0.0371(8) 0.0337(7) 0.0373(7) -0.0058(6) -0.0023(6) -0.0124(6) O14 0.0364(8) 0.0631(11) 0.0336(8) 0.0031(7) -0.0045(6) -0.0241(8) O15 0.0699(14) 0.1030(18) 0.0516(11) -0.0400(12) -0.0061(10) -0.0042(13) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3472(3) 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 . 2.0707(14) yes Ru1 . N2 . 1.9815(13) yes Ru1 . N3 . 2.0792(15) yes Ru1 . N4 . 2.0572(14) yes Ru1 . N5 . 1.9773(13) yes Ru1 . N6 . 2.0592(14) yes N1 . C1 . 1.348(2) yes N1 . C5 . 1.366(2) yes N2 . C6 . 1.349(2) yes N2 . C10 . 1.351(2) yes N3 . C11 . 1.368(2) yes N3 . C15 . 1.346(2) yes N4 . C16 . 1.346(2) yes N4 . C20 . 1.373(2) yes N5 . C21 . 1.352(2) yes N5 . C25 . 1.352(2) yes N6 . C26 . 1.371(2) yes N6 . C30 . 1.344(2) yes N7 . N8 . 1.341(2) yes N7 . C8 . 1.385(2) yes N7 . H1 . 0.866 no N8 . C31 . 1.289(2) yes N9 . C34 . 1.331(3) yes N9 . C35 . 1.348(2) yes N9 . H2 . 0.857 no N10 . N11 . 1.347(2) yes N10 . C23 . 1.380(2) yes N10 . H3 . 0.868 no N11 . C37 . 1.288(2) yes N12 . C40 . 1.344(3) yes N12 . C41 . 1.334(3) yes N12 . H4 . 0.875 no N13 . O1 . 1.262(2) yes N13 . O2 . 1.247(2) yes N13 . O3 . 1.227(2) yes N14 . O4 . 1.257(3) yes N14 . O5 . 1.232(3) yes N14 . O6 . 1.231(3) yes N15 . O7 . 1.237(2) yes N15 . O8 . 1.243(3) yes N15 . O9 . 1.250(3) yes N16 . O10 . 1.224(3) yes N16 . O11 . 1.247(3) yes N16 . O12 . 1.247(3) yes C1 . C2 . 1.388(3) yes C1 . H11 . 0.932 no C2 . C3 . 1.378(3) yes C2 . H21 . 0.926 no C3 . C4 . 1.385(3) yes C3 . H31 . 0.924 no C4 . C5 . 1.388(2) yes C4 . H41 . 0.926 no C5 . C6 . 1.478(2) yes C6 . C7 . 1.383(2) yes C7 . C8 . 1.396(2) yes C7 . H71 . 0.934 no C8 . C9 . 1.400(2) yes C9 . C10 . 1.379(2) yes C9 . H91 . 0.928 no C10 . C11 . 1.478(2) yes C11 . C12 . 1.390(3) yes C12 . C13 . 1.382(3) yes C12 . H121 . 0.946 no C13 . C14 . 1.385(3) yes C13 . H131 . 0.944 no C14 . C15 . 1.387(3) yes C14 . H141 . 0.942 no C15 . H151 . 0.932 no C16 . C17 . 1.384(3) yes C16 . H161 . 0.953 no C17 . C18 . 1.376(3) yes C17 . H171 . 0.930 no C18 . C19 . 1.390(2) yes C18 . H181 . 0.937 no C19 . C20 . 1.385(2) yes C19 . H191 . 0.925 no C20 . C21 . 1.482(2) yes C21 . C22 . 1.383(2) yes C22 . C23 . 1.402(2) yes C22 . H221 . 0.927 no C23 . C24 . 1.401(2) yes C24 . C25 . 1.389(2) yes C24 . H241 . 0.943 no C25 . C26 . 1.483(2) yes C26 . C27 . 1.386(2) yes C27 . C28 . 1.391(3) yes C27 . H271 . 0.928 no C28 . C29 . 1.384(3) yes C28 . H281 . 0.937 no C29 . C30 . 1.380(3) yes C29 . H291 . 0.944 no C30 . H301 . 0.955 no C31 . C32 . 1.451(2) yes C31 . H311 . 0.944 no C32 . C33 . 1.396(2) yes C32 . C36 . 1.398(3) yes C33 . C34 . 1.375(3) yes C33 . H331 . 0.936 no C34 . H341 . 0.929 no C35 . C36 . 1.365(3) yes C35 . H351 . 0.939 no C36 . H361 . 0.928 no C37 . C38 . 1.459(2) yes C37 . H371 . 0.946 no C38 . C39 . 1.400(3) yes C38 . C42 . 1.398(2) yes C39 . C40 . 1.373(3) yes C39 . H391 . 0.936 no C40 . H401 . 0.937 no C41 . C42 . 1.381(3) yes C41 . H411 . 0.937 no C42 . H421 . 0.960 no O13 . H5 . 0.818 no O13 . H6 . 0.810 no O14 . H7 . 0.818 no O14 . H8 . 0.830 no O15 . H9 . 0.809 no O15 . H10 . 0.816 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Ru1 . N2 . 79.42(6) yes N1 . Ru1 . N3 . 158.07(5) yes N2 . Ru1 . N3 . 78.65(6) yes N1 . Ru1 . N4 . 88.38(6) yes N2 . Ru1 . N4 . 97.63(6) yes N3 . Ru1 . N4 . 95.13(6) yes N1 . Ru1 . N5 . 97.21(5) yes N2 . Ru1 . N5 . 175.74(6) yes N3 . Ru1 . N5 . 104.72(6) yes N4 . Ru1 . N5 . 79.58(6) yes N1 . Ru1 . N6 . 94.20(6) yes N2 . Ru1 . N6 . 103.81(6) yes N3 . Ru1 . N6 . 90.40(6) yes N4 . Ru1 . N6 . 158.51(6) yes N5 . Ru1 . N6 . 78.93(6) yes Ru1 . N1 . C1 . 127.73(12) yes Ru1 . N1 . C5 . 113.45(11) yes C1 . N1 . C5 . 118.72(15) yes Ru1 . N2 . C6 . 118.39(11) yes Ru1 . N2 . C10 . 119.43(11) yes C6 . N2 . C10 . 121.72(14) yes Ru1 . N3 . C11 . 114.18(11) yes Ru1 . N3 . C15 . 127.52(12) yes C11 . N3 . C15 . 118.23(16) yes Ru1 . N4 . C16 . 127.02(12) yes Ru1 . N4 . C20 . 113.85(11) yes C16 . N4 . C20 . 118.99(15) yes Ru1 . N5 . C21 . 118.64(11) yes Ru1 . N5 . C25 . 119.39(11) yes C21 . N5 . C25 . 121.47(14) yes Ru1 . N6 . C26 . 114.73(11) yes Ru1 . N6 . C30 . 126.64(12) yes C26 . N6 . C30 . 118.63(15) yes N8 . N7 . C8 . 119.07(15) yes N8 . N7 . H1 . 120.4 no C8 . N7 . H1 . 120.5 no N7 . N8 . C31 . 117.37(16) yes C34 . N9 . C35 . 121.98(17) yes C34 . N9 . H2 . 119.5 no C35 . N9 . H2 . 118.6 no N11 . N10 . C23 . 119.46(15) yes N11 . N10 . H3 . 120.6 no C23 . N10 . H3 . 120.0 no N10 . N11 . C37 . 116.90(16) yes C40 . N12 . C41 . 122.02(17) yes C40 . N12 . H4 . 118.8 no C41 . N12 . H4 . 119.2 no O1 . N13 . O2 . 119.68(17) yes O1 . N13 . O3 . 119.40(16) yes O2 . N13 . O3 . 120.92(17) yes O4 . N14 . O5 . 120.5(2) yes O4 . N14 . O6 . 119.8(2) yes O5 . N14 . O6 . 119.4(2) yes O7 . N15 . O8 . 121.0(2) yes O7 . N15 . O9 . 118.9(3) yes O8 . N15 . O9 . 120.1(2) yes O10 . N16 . O11 . 120.2(2) yes O10 . N16 . O12 . 121.1(2) yes O11 . N16 . O12 . 118.7(2) yes N1 . C1 . C2 . 122.12(16) yes N1 . C1 . H11 . 117.2 no C2 . C1 . H11 . 120.7 no C1 . C2 . C3 . 119.02(17) yes C1 . C2 . H21 . 119.5 no C3 . C2 . H21 . 121.5 no C2 . C3 . C4 . 119.60(18) yes C2 . C3 . H31 . 120.5 no C4 . C3 . H31 . 119.9 no C3 . C4 . C5 . 119.15(16) yes C3 . C4 . H41 . 120.4 no C5 . C4 . H41 . 120.4 no C4 . C5 . N1 . 121.37(15) yes C4 . C5 . C6 . 123.34(15) yes N1 . C5 . C6 . 115.28(14) yes C5 . C6 . N2 . 113.09(14) yes C5 . C6 . C7 . 126.40(15) yes N2 . C6 . C7 . 120.49(15) yes C6 . C7 . C8 . 118.38(16) yes C6 . C7 . H71 . 121.4 no C8 . C7 . H71 . 120.2 no C7 . C8 . N7 . 117.86(16) yes C7 . C8 . C9 . 120.48(15) yes N7 . C8 . C9 . 121.65(16) yes C8 . C9 . C10 . 118.24(15) yes C8 . C9 . H91 . 121.1 no C10 . C9 . H91 . 120.7 no C9 . C10 . N2 . 120.66(16) yes C9 . C10 . C11 . 126.71(15) yes N2 . C10 . C11 . 112.61(14) yes C10 . C11 . N3 . 114.76(15) yes C10 . C11 . C12 . 123.72(16) yes N3 . C11 . C12 . 121.52(16) yes C11 . C12 . C13 . 119.44(18) yes C11 . C12 . H121 . 120.1 no C13 . C12 . H121 . 120.4 no C12 . C13 . C14 . 119.14(19) yes C12 . C13 . H131 . 119.6 no C14 . C13 . H131 . 121.3 no C13 . C14 . C15 . 119.07(18) yes C13 . C14 . H141 . 121.6 no C15 . C14 . H141 . 119.3 no C14 . C15 . N3 . 122.56(18) yes C14 . C15 . H151 . 120.8 no N3 . C15 . H151 . 116.7 no N4 . C16 . C17 . 122.31(17) yes N4 . C16 . H161 . 116.7 no C17 . C16 . H161 . 121.0 no C16 . C17 . C18 . 118.82(17) yes C16 . C17 . H171 . 119.6 no C18 . C17 . H171 . 121.6 no C17 . C18 . C19 . 119.80(17) yes C17 . C18 . H181 . 120.4 no C19 . C18 . H181 . 119.8 no C18 . C19 . C20 . 119.25(17) yes C18 . C19 . H191 . 120.6 no C20 . C19 . H191 . 120.2 no C19 . C20 . N4 . 120.83(15) yes C19 . C20 . C21 . 124.24(15) yes N4 . C20 . C21 . 114.92(14) yes C20 . C21 . N5 . 112.74(14) yes C20 . C21 . C22 . 126.52(15) yes N5 . C21 . C22 . 120.71(15) yes C21 . C22 . C23 . 118.49(15) yes C21 . C22 . H221 . 120.6 no C23 . C22 . H221 . 120.9 no C22 . C23 . N10 . 117.60(15) yes C22 . C23 . C24 . 120.40(15) yes N10 . C23 . C24 . 121.97(15) yes C23 . C24 . C25 . 118.10(15) yes C23 . C24 . H241 . 120.4 no C25 . C24 . H241 . 121.5 no C24 . C25 . N5 . 120.81(15) yes C24 . C25 . C26 . 126.68(15) yes N5 . C25 . C26 . 112.46(14) yes C25 . C26 . N6 . 114.37(14) yes C25 . C26 . C27 . 124.24(15) yes N6 . C26 . C27 . 121.37(16) yes C26 . C27 . C28 . 119.08(17) yes C26 . C27 . H271 . 120.2 no C28 . C27 . H271 . 120.8 no C27 . C28 . C29 . 119.25(17) yes C27 . C28 . H281 . 120.5 no C29 . C28 . H281 . 120.2 no C28 . C29 . C30 . 119.21(18) yes C28 . C29 . H291 . 121.4 no C30 . C29 . H291 . 119.4 no C29 . C30 . N6 . 122.40(17) yes C29 . C30 . H301 . 120.5 no N6 . C30 . H301 . 117.1 no N8 . C31 . C32 . 118.49(17) yes N8 . C31 . H311 . 121.1 no C32 . C31 . H311 . 120.4 no C31 . C32 . C33 . 120.19(17) yes C31 . C32 . C36 . 121.61(16) yes C33 . C32 . C36 . 118.19(17) yes C32 . C33 . C34 . 119.68(18) yes C32 . C33 . H331 . 120.8 no C34 . C33 . H331 . 119.5 no C33 . C34 . N9 . 120.22(17) yes C33 . C34 . H341 . 120.1 no N9 . C34 . H341 . 119.7 no N9 . C35 . C36 . 120.10(19) yes N9 . C35 . H351 . 117.9 no C36 . C35 . H351 . 121.9 no C32 . C36 . C35 . 119.82(17) yes C32 . C36 . H361 . 120.1 no C35 . C36 . H361 . 120.1 no N11 . C37 . C38 . 119.41(17) yes N11 . C37 . H371 . 122.0 no C38 . C37 . H371 . 118.6 no C37 . C38 . C39 . 121.74(17) yes C37 . C38 . C42 . 119.66(17) yes C39 . C38 . C42 . 118.60(17) yes C38 . C39 . C40 . 119.30(19) yes C38 . C39 . H391 . 120.8 no C40 . C39 . H391 . 119.9 no C39 . C40 . N12 . 120.4(2) yes C39 . C40 . H401 . 120.3 no N12 . C40 . H401 . 119.2 no N12 . C41 . C42 . 120.16(18) yes N12 . C41 . H411 . 120.1 no C42 . C41 . H411 . 119.8 no C38 . C42 . C41 . 119.48(19) yes C38 . C42 . H421 . 120.8 no C41 . C42 . H421 . 119.8 no H5 . O13 . H6 . 105.3 no H7 . O14 . H8 . 106.3 no H9 . O15 . H10 . 105.8 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag N9 . H2 . O1 2_766 176 0.86 1.89 2.751(2) yes N10 . H3 . O13 1_545 169 0.87 1.98 2.839(2) yes N12 . H4 . O14 2_565 168 0.88 1.82 2.685(2) yes O13 . H5 . O7 . 170 0.82 2.03 2.843(2) yes O13 . H6 . O12 . 171 0.81 2.01 2.814(2) yes O14 . H7 . O15 . 168 0.82 1.97 2.775(2) yes O14 . H8 . O2 2_666 173 0.83 1.94 2.763(2) yes O15 . H9 . O10 . 171 0.81 2.01 2.808(2) yes O15 . H10 . O8 . 151 0.82 2.07 2.815(2) yes # Attachment 'Ru_1_2_NO3_JZ.CIF' data_jb1220 _database_code_depnum_ccdc_archive 'CCDC 692943' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H32 N12 Ru, 2(N O3), 4.25(H2 O)' _chemical_formula_sum 'C42 H40.5 N14 O10.25 Ru' _chemical_formula_weight 1005.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.840(2) _cell_length_b 14.336(3) _cell_length_c 15.614(3) _cell_angle_alpha 105.45(3) _cell_angle_beta 92.24(3) _cell_angle_gamma 107.05(3) _cell_volume 2217.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 0.429 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32184 _diffrn_reflns_av_R_equivalents 0.0965 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.05 _reflns_number_total 7769 _reflns_number_gt 7180 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+6.1660P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7769 _refine_ls_number_parameters 629 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1502 _refine_ls_wR_factor_gt 0.1469 _refine_ls_goodness_of_fit_ref 1.186 _refine_ls_restrained_S_all 1.193 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.49965(3) 0.25230(2) 0.24603(2) 0.02581(13) Uani 1 1 d . . . N1 N 0.4313(3) 0.3108(3) 0.3641(2) 0.0301(8) Uani 1 1 d . . . N2 N 0.5441(3) 0.1730(3) 0.3211(2) 0.0287(7) Uani 1 1 d . . . N3 N 0.5844(3) 0.1609(3) 0.1577(2) 0.0285(7) Uani 1 1 d . . . N4 N 0.6711(4) 0.0334(3) 0.4904(3) 0.0386(9) Uani 1 1 d . . . H4B H 0.6476 0.0419 0.5445 0.046 Uiso 1 1 calc R . . N5 N 0.7501(4) -0.0245(3) 0.4626(3) 0.0383(9) Uani 1 1 d . . . N6 N 1.0635(5) -0.2245(4) 0.4615(4) 0.0634(15) Uani 1 1 d . . . N7 N 0.3135(3) 0.1652(3) 0.1865(2) 0.0305(8) Uani 1 1 d . . . N8 N 0.4596(3) 0.3374(3) 0.1752(2) 0.0270(7) Uani 1 1 d . . . N9 N 0.6678(3) 0.3751(3) 0.2811(2) 0.0283(7) Uani 1 1 d . . . N10 N 0.3643(4) 0.5305(3) 0.0499(3) 0.0370(8) Uani 1 1 d . . . H10A H 0.4190 0.5921 0.0580 0.044 Uiso 1 1 calc R . . N11 N 0.2479(4) 0.4993(3) -0.0018(3) 0.0380(9) Uani 1 1 d . . . N12 N -0.1384(4) 0.4846(4) -0.2007(3) 0.0524(12) Uani 1 1 d . . . C1 C 0.3723(4) 0.3834(3) 0.3805(3) 0.0368(10) Uani 1 1 d . . . H1A H 0.3596 0.4130 0.3345 0.044 Uiso 1 1 calc R . . C2 C 0.3295(5) 0.4163(4) 0.4624(3) 0.0440(12) Uani 1 1 d . . . H2A H 0.2878 0.4673 0.4723 0.053 Uiso 1 1 calc R . . C3 C 0.3485(5) 0.3740(4) 0.5288(3) 0.0440(12) Uani 1 1 d . . . H3A H 0.3195 0.3954 0.5852 0.053 Uiso 1 1 calc R . . C4 C 0.4098(4) 0.3000(4) 0.5137(3) 0.0368(10) Uani 1 1 d . . . H4A H 0.4232 0.2700 0.5592 0.044 Uiso 1 1 calc R . . C5 C 0.4515(4) 0.2704(3) 0.4306(3) 0.0301(9) Uani 1 1 d . . . C6 C 0.5202(4) 0.1928(3) 0.4080(3) 0.0290(9) Uani 1 1 d . . . C7 C 0.5606(4) 0.1465(3) 0.4649(3) 0.0329(9) Uani 1 1 d . . . H7A H 0.5425 0.1609 0.5252 0.040 Uiso 1 1 calc R . . C8 C 0.6293(4) 0.0776(3) 0.4331(3) 0.0335(9) Uani 1 1 d . . . C9 C 0.6528(4) 0.0571(3) 0.3427(3) 0.0331(9) Uani 1 1 d . . . H9A H 0.6979 0.0101 0.3193 0.040 Uiso 1 1 calc R . . C10 C 0.6096(4) 0.1058(3) 0.2889(3) 0.0296(9) Uani 1 1 d . . . C11 C 0.6276(4) 0.0974(3) 0.1935(3) 0.0309(9) Uani 1 1 d . . . C12 C 0.6828(4) 0.0289(4) 0.1423(3) 0.0374(10) Uani 1 1 d . . . H12A H 0.7116 -0.0156 0.1676 0.045 Uiso 1 1 calc R . . C13 C 0.6955(5) 0.0261(4) 0.0532(3) 0.0435(12) Uani 1 1 d . . . H13A H 0.7333 -0.0203 0.0174 0.052 Uiso 1 1 calc R . . C14 C 0.6528(5) 0.0912(4) 0.0172(3) 0.0418(11) Uani 1 1 d . . . H14A H 0.6618 0.0908 -0.0431 0.050 Uiso 1 1 calc R . . C15 C 0.5971(4) 0.1567(3) 0.0709(3) 0.0340(9) Uani 1 1 d . . . H15A H 0.5663 0.2006 0.0459 0.041 Uiso 1 1 calc R . . C16 C 0.7963(4) -0.0563(4) 0.5216(3) 0.0400(10) Uani 1 1 d . . . H16A H 0.7726 -0.0414 0.5805 0.048 Uiso 1 1 calc R . . C17 C 0.8856(5) -0.1156(4) 0.4989(4) 0.0424(11) Uani 1 1 d . . . C18 C 0.9261(5) -0.1382(4) 0.4141(4) 0.0496(13) Uani 1 1 d . . . H18A H 0.8936 -0.1174 0.3674 0.060 Uiso 1 1 calc R . . C19 C 1.0144(6) -0.1914(4) 0.3998(5) 0.0615(16) Uani 1 1 d . . . H19A H 1.0424 -0.2054 0.3422 0.074 Uiso 1 1 calc R . . C20 C 1.0237(6) -0.2028(4) 0.5424(5) 0.0622(17) Uani 1 1 d . . . H20A H 1.0566 -0.2260 0.5873 0.075 Uiso 1 1 calc R . . C21 C 0.9368(5) -0.1480(4) 0.5644(4) 0.0526(13) Uani 1 1 d . . . H21A H 0.9129 -0.1330 0.6232 0.063 Uiso 1 1 calc R . . C22 C 0.2441(5) 0.0753(3) 0.1976(3) 0.0395(11) Uani 1 1 d . . . H22A H 0.2847 0.0447 0.2324 0.047 Uiso 1 1 calc R . . C23 C 0.1163(5) 0.0261(4) 0.1601(4) 0.0485(13) Uani 1 1 d . . . H23A H 0.0691 -0.0368 0.1695 0.058 Uiso 1 1 calc R . . C24 C 0.0585(5) 0.0703(4) 0.1089(4) 0.0489(13) Uani 1 1 d . . . H24A H -0.0299 0.0383 0.0834 0.059 Uiso 1 1 calc R . . C25 C 0.1288(4) 0.1615(4) 0.0941(3) 0.0399(11) Uani 1 1 d . . . H25A H 0.0901 0.1915 0.0576 0.048 Uiso 1 1 calc R . . C26 C 0.2574(4) 0.2079(3) 0.1340(3) 0.0308(9) Uani 1 1 d . . . C27 C 0.3406(4) 0.3071(3) 0.1270(3) 0.0282(8) Uani 1 1 d . . . C28 C 0.3068(4) 0.3677(3) 0.0815(3) 0.0312(9) Uani 1 1 d . . . H28A H 0.2250 0.3445 0.0454 0.037 Uiso 1 1 calc R . . C29 C 0.3947(4) 0.4641(3) 0.0889(3) 0.0314(9) Uani 1 1 d . . . C30 C 0.5182(4) 0.4942(3) 0.1394(3) 0.0314(9) Uani 1 1 d . . . H30A H 0.5803 0.5583 0.1438 0.038 Uiso 1 1 calc R . . C31 C 0.5469(4) 0.4297(3) 0.1817(3) 0.0292(9) Uani 1 1 d . . . C32 C 0.6672(4) 0.4491(3) 0.2411(3) 0.0270(8) Uani 1 1 d . . . C33 C 0.7744(4) 0.5373(3) 0.2580(3) 0.0326(9) Uani 1 1 d . . . H33A H 0.7741 0.5886 0.2301 0.039 Uiso 1 1 calc R . . C34 C 0.8807(4) 0.5486(4) 0.3162(3) 0.0375(10) Uani 1 1 d . . . H34A H 0.9549 0.6075 0.3275 0.045 Uiso 1 1 calc R . . C35 C 0.8800(4) 0.4752(4) 0.3578(3) 0.0388(10) Uani 1 1 d . . . H35A H 0.9522 0.4834 0.3987 0.047 Uiso 1 1 calc R . . C36 C 0.7717(4) 0.3891(4) 0.3389(3) 0.0355(10) Uani 1 1 d . . . H36A H 0.7708 0.3383 0.3676 0.043 Uiso 1 1 calc R . . C37 C 0.2165(5) 0.5665(4) -0.0302(3) 0.0392(10) Uani 1 1 d . . . H37A H 0.2733 0.6347 -0.0144 0.047 Uiso 1 1 calc R . . C38 C 0.0928(5) 0.5375(4) -0.0869(3) 0.0398(11) Uani 1 1 d . . . C39 C 0.0089(5) 0.4370(4) -0.1151(3) 0.0437(11) Uani 1 1 d . . . H39A H 0.0298 0.3852 -0.0961 0.052 Uiso 1 1 calc R . . C40 C -0.1040(5) 0.4143(5) -0.1707(4) 0.0503(13) Uani 1 1 d . . . H40A H -0.1607 0.3460 -0.1889 0.060 Uiso 1 1 calc R . . C41 C -0.0562(5) 0.5802(5) -0.1739(3) 0.0503(13) Uani 1 1 d . . . H41A H -0.0780 0.6302 -0.1954 0.060 Uiso 1 1 calc R . . C42 C 0.0581(5) 0.6104(4) -0.1171(3) 0.0435(11) Uani 1 1 d . . . H42A H 0.1120 0.6795 -0.0991 0.052 Uiso 1 1 calc R . . N100 N 0.8340(5) 0.7871(4) 0.1367(4) 0.0674(15) Uani 1 1 d . . . O11 O 0.7924(8) 0.7351(5) 0.1818(5) 0.122(2) Uani 1 1 d U . . O12 O 0.9399(5) 0.7823(4) 0.0997(5) 0.0937(18) Uani 1 1 d . . . O13 O 0.7807(5) 0.8377(4) 0.1096(4) 0.0761(13) Uani 1 1 d . . . N200 N 0.3636(5) -0.1243(3) 0.2718(3) 0.0550(12) Uani 1 1 d . . . O21 O 0.4149(7) -0.1646(5) 0.3144(4) 0.108(2) Uani 1 1 d . . . O22 O 0.3032(7) -0.0704(5) 0.3100(4) 0.102(2) Uani 1 1 d . . . O23 O 0.3796(5) -0.1330(4) 0.1917(3) 0.0744(13) Uani 1 1 d . . . H30C H 0.527(8) 0.766(6) 0.289(6) 0.089 Uiso 1 1 d . . . O30 O 0.5822(6) 0.7263(4) 0.2863(3) 0.0809(15) Uani 1 1 d . . . H30D H 0.6413 0.7052 0.3021 0.097 Uiso 1 1 calc R . . O40 O 0.3585(4) 0.5766(3) 0.3235(3) 0.0561(10) Uani 1 1 d . . . H40C H 0.294(7) 0.575(5) 0.285(5) 0.067 Uiso 1 1 d . . . H40D H 0.425(7) 0.626(5) 0.306(4) 0.067 Uiso 1 1 d . . . H50B H 1.178(7) -0.335(5) 0.447(5) 0.067 Uiso 1 1 d . . . O50 O 1.1961(4) -0.3769(3) 0.4591(3) 0.0559(10) Uani 1 1 d . . . H50A H 1.258(6) -0.371(5) 0.410(5) 0.067 Uiso 1 1 d . . . O60 O 0.5006(4) 0.7414(3) 0.0787(3) 0.0482(9) Uani 1 1 d . . . H60A H 0.473(6) 0.780(5) 0.119(4) 0.058 Uiso 1 1 d . . . H60B H 0.573(7) 0.762(5) 0.089(5) 0.058 Uiso 1 1 d . . . O70 O 1.105(2) 0.7898(18) 0.0712(16) 0.093(6) Uiso 0.25 1 d P . . 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 0.02582(19) 0.02632(19) 0.02390(19) 0.00387(13) 0.00510(12) 0.00902(13) N1 0.0280(18) 0.0296(18) 0.0305(18) 0.0039(14) 0.0060(14) 0.0097(14) N2 0.0245(17) 0.0306(18) 0.0294(18) 0.0039(14) 0.0084(14) 0.0099(14) N3 0.0246(17) 0.0316(18) 0.0256(17) 0.0038(14) 0.0023(13) 0.0075(14) N4 0.038(2) 0.047(2) 0.040(2) 0.0199(18) 0.0106(17) 0.0193(18) N5 0.034(2) 0.033(2) 0.046(2) 0.0111(17) 0.0031(17) 0.0098(16) N6 0.050(3) 0.037(2) 0.092(4) -0.004(3) -0.005(3) 0.019(2) N7 0.0289(18) 0.0309(18) 0.0277(18) 0.0020(14) 0.0070(14) 0.0091(15) N8 0.0240(17) 0.0311(18) 0.0242(17) 0.0030(14) 0.0072(13) 0.0101(14) N9 0.0289(18) 0.0325(18) 0.0224(16) 0.0048(14) 0.0050(13) 0.0106(15) N10 0.037(2) 0.043(2) 0.035(2) 0.0132(17) 0.0026(16) 0.0177(17) N11 0.041(2) 0.051(2) 0.0295(19) 0.0128(17) 0.0094(16) 0.0237(19) N12 0.045(2) 0.084(4) 0.036(2) 0.012(2) 0.0083(19) 0.035(3) C1 0.036(2) 0.032(2) 0.039(2) 0.0032(19) 0.0057(19) 0.0135(19) C2 0.047(3) 0.041(3) 0.042(3) 0.000(2) 0.011(2) 0.021(2) C3 0.048(3) 0.050(3) 0.031(2) 0.000(2) 0.011(2) 0.021(2) C4 0.036(2) 0.042(3) 0.028(2) 0.0036(19) 0.0068(18) 0.012(2) C5 0.026(2) 0.031(2) 0.029(2) 0.0011(17) 0.0045(16) 0.0087(17) C6 0.025(2) 0.032(2) 0.028(2) 0.0049(17) 0.0045(16) 0.0080(17) C7 0.031(2) 0.037(2) 0.030(2) 0.0086(18) 0.0066(17) 0.0089(18) C8 0.030(2) 0.031(2) 0.038(2) 0.0107(18) 0.0049(18) 0.0071(18) C9 0.029(2) 0.036(2) 0.035(2) 0.0074(18) 0.0050(17) 0.0141(18) C10 0.027(2) 0.030(2) 0.030(2) 0.0037(17) 0.0056(16) 0.0111(17) C11 0.026(2) 0.034(2) 0.029(2) 0.0039(17) 0.0026(16) 0.0097(17) C12 0.035(2) 0.041(2) 0.036(2) 0.0021(19) 0.0042(19) 0.019(2) C13 0.039(3) 0.051(3) 0.035(2) -0.004(2) 0.008(2) 0.021(2) C14 0.039(2) 0.054(3) 0.027(2) 0.002(2) 0.0056(19) 0.015(2) C15 0.035(2) 0.037(2) 0.026(2) 0.0043(18) 0.0039(17) 0.0108(19) C16 0.034(2) 0.043(3) 0.046(3) 0.017(2) 0.005(2) 0.013(2) C17 0.035(2) 0.032(2) 0.057(3) 0.009(2) -0.005(2) 0.010(2) C18 0.048(3) 0.035(3) 0.059(3) 0.003(2) 0.003(2) 0.014(2) C19 0.056(3) 0.040(3) 0.077(4) -0.003(3) 0.007(3) 0.016(3) C20 0.047(3) 0.047(3) 0.089(5) 0.012(3) -0.019(3) 0.020(3) C21 0.046(3) 0.047(3) 0.065(4) 0.015(3) -0.004(3) 0.017(2) C22 0.041(3) 0.030(2) 0.041(3) 0.0055(19) 0.009(2) 0.0051(19) C23 0.043(3) 0.043(3) 0.046(3) 0.008(2) 0.008(2) -0.002(2) C24 0.030(2) 0.053(3) 0.044(3) -0.002(2) 0.005(2) -0.001(2) C25 0.031(2) 0.046(3) 0.037(2) 0.002(2) 0.0038(19) 0.011(2) C26 0.029(2) 0.031(2) 0.026(2) -0.0020(16) 0.0033(16) 0.0085(17) C27 0.028(2) 0.031(2) 0.024(2) 0.0016(16) 0.0043(16) 0.0129(17) C28 0.028(2) 0.041(2) 0.025(2) 0.0038(17) 0.0023(16) 0.0168(18) C29 0.036(2) 0.036(2) 0.024(2) 0.0042(17) 0.0057(17) 0.0192(19) C30 0.033(2) 0.034(2) 0.026(2) 0.0049(17) 0.0063(17) 0.0121(18) C31 0.031(2) 0.031(2) 0.026(2) 0.0041(16) 0.0066(16) 0.0138(17) C32 0.027(2) 0.031(2) 0.0205(19) 0.0022(16) 0.0053(15) 0.0103(17) C33 0.034(2) 0.033(2) 0.028(2) 0.0043(17) 0.0082(17) 0.0100(18) C34 0.029(2) 0.040(2) 0.032(2) -0.0027(19) 0.0045(18) 0.0057(19) C35 0.031(2) 0.051(3) 0.029(2) 0.002(2) -0.0019(18) 0.015(2) C36 0.035(2) 0.043(3) 0.027(2) 0.0064(18) 0.0013(18) 0.013(2) C37 0.042(3) 0.049(3) 0.032(2) 0.011(2) 0.0076(19) 0.023(2) C38 0.043(3) 0.058(3) 0.029(2) 0.011(2) 0.0108(19) 0.031(2) C39 0.043(3) 0.059(3) 0.036(3) 0.016(2) 0.011(2) 0.025(2) C40 0.041(3) 0.069(4) 0.042(3) 0.011(3) 0.011(2) 0.023(3) C41 0.054(3) 0.072(4) 0.040(3) 0.014(3) 0.008(2) 0.044(3) C42 0.047(3) 0.058(3) 0.033(2) 0.009(2) 0.003(2) 0.032(2) N100 0.055(3) 0.041(3) 0.104(5) 0.027(3) -0.001(3) 0.009(2) O11 0.199(6) 0.101(4) 0.100(4) 0.058(4) 0.061(4) 0.068(4) O12 0.059(3) 0.070(3) 0.152(6) 0.034(3) 0.004(3) 0.020(2) O13 0.091(3) 0.063(3) 0.091(4) 0.031(3) 0.018(3) 0.040(3) N200 0.074(3) 0.041(2) 0.056(3) 0.017(2) 0.022(3) 0.022(2) O21 0.143(6) 0.140(5) 0.082(4) 0.066(4) 0.030(4) 0.072(5) O22 0.160(6) 0.106(4) 0.093(4) 0.050(3) 0.078(4) 0.094(4) O23 0.108(4) 0.097(3) 0.038(2) 0.018(2) 0.023(2) 0.061(3) O30 0.110(4) 0.073(3) 0.060(3) 0.026(2) -0.007(3) 0.026(3) O40 0.055(2) 0.064(3) 0.050(2) 0.0160(19) -0.0042(18) 0.021(2) O50 0.061(2) 0.059(3) 0.053(2) 0.0184(19) 0.0047(19) 0.025(2) O60 0.053(2) 0.048(2) 0.043(2) 0.0072(16) 0.0014(18) 0.0197(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N2 1.972(4) . ? Ru1 N8 1.973(4) . ? Ru1 N9 2.061(4) . ? Ru1 N7 2.062(4) . ? Ru1 N1 2.074(3) . ? Ru1 N3 2.075(3) . ? N1 C1 1.349(6) . ? N1 C5 1.355(6) . ? N2 C6 1.360(5) . ? N2 C10 1.363(5) . ? N3 C15 1.356(6) . ? N3 C11 1.364(6) . ? N4 C8 1.359(6) . ? N4 N5 1.366(5) . ? N4 H4B 0.8800 . ? N5 C16 1.278(6) . ? N6 C19 1.337(9) . ? N6 C20 1.339(9) . ? N7 C22 1.348(6) . ? N7 C26 1.366(6) . ? N8 C27 1.357(5) . ? N8 C31 1.357(6) . ? N9 C36 1.347(6) . ? N9 C32 1.369(6) . ? N10 N11 1.357(5) . ? N10 C29 1.365(6) . ? N10 H10A 0.8800 . ? N11 C37 1.284(6) . ? N12 C41 1.341(8) . ? N12 C40 1.353(8) . ? C1 C2 1.388(7) . ? C1 H1A 0.9500 . ? C2 C3 1.369(8) . ? C2 H2A 0.9500 . ? C3 C4 1.384(7) . ? C3 H3A 0.9500 . ? C4 C5 1.391(6) . ? C4 H4A 0.9500 . ? C5 C6 1.487(6) . ? C6 C7 1.370(6) . ? C7 C8 1.405(6) . ? C7 H7A 0.9500 . ? C8 C9 1.413(6) . ? C9 C10 1.373(6) . ? C9 H9A 0.9500 . ? C10 C11 1.487(6) . ? C11 C12 1.387(6) . ? C12 C13 1.394(7) . ? C12 H12A 0.9500 . ? C13 C14 1.383(8) . ? C13 H13A 0.9500 . ? C14 C15 1.379(6) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.460(7) . ? C16 H16A 0.9500 . ? C17 C21 1.389(8) . ? C17 C18 1.396(8) . ? C18 C19 1.379(8) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C21 1.392(8) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.380(7) . ? C22 H22A 0.9500 . ? C23 C24 1.378(8) . ? C23 H23A 0.9500 . ? C24 C25 1.390(7) . ? C24 H24A 0.9500 . ? C25 C26 1.393(6) . ? C25 H25A 0.9500 . ? C26 C27 1.478(6) . ? C27 C28 1.374(6) . ? C28 C29 1.402(6) . ? C28 H28A 0.9500 . ? C29 C30 1.413(6) . ? C30 C31 1.366(6) . ? C30 H30A 0.9500 . ? C31 C32 1.481(6) . ? C32 C33 1.398(6) . ? C33 C34 1.382(6) . ? C33 H33A 0.9500 . ? C34 C35 1.373(7) . ? C34 H34A 0.9500 . ? C35 C36 1.384(7) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C38 1.463(7) . ? C37 H37A 0.9500 . ? C38 C42 1.391(7) . ? C38 C39 1.400(8) . ? C39 C40 1.376(7) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 C42 1.380(7) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? N100 O11 1.167(8) . ? N100 O13 1.195(7) . ? N100 O12 1.317(8) . ? N200 O21 1.203(7) . ? N200 O22 1.210(6) . ? N200 O23 1.248(6) . ? O30 H30C 0.93(8) . ? O30 H30D 0.8400 . ? O40 H40C 0.90(7) . ? O40 H40D 0.96(7) . ? O50 H50B 0.75(7) . ? O50 H50A 1.04(7) . ? O60 H60A 0.85(7) . ? O60 H60B 0.75(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ru1 N8 177.38(14) . . ? N2 Ru1 N9 98.49(14) . . ? N8 Ru1 N9 79.36(14) . . ? N2 Ru1 N7 103.06(15) . . ? N8 Ru1 N7 79.03(14) . . ? N9 Ru1 N7 158.32(15) . . ? N2 Ru1 N1 78.96(14) . . ? N8 Ru1 N1 99.49(14) . . ? N9 Ru1 N1 90.43(14) . . ? N7 Ru1 N1 91.37(14) . . ? N2 Ru1 N3 78.97(14) . . ? N8 Ru1 N3 102.58(14) . . ? N9 Ru1 N3 93.29(13) . . ? N7 Ru1 N3 93.11(13) . . ? N1 Ru1 N3 157.93(15) . . ? C1 N1 C5 118.7(4) . . ? C1 N1 Ru1 127.1(3) . . ? C5 N1 Ru1 114.2(3) . . ? C6 N2 C10 120.1(4) . . ? C6 N2 Ru1 119.6(3) . . ? C10 N2 Ru1 120.0(3) . . ? C15 N3 C11 118.8(4) . . ? C15 N3 Ru1 127.3(3) . . ? C11 N3 Ru1 113.8(3) . . ? C8 N4 N5 118.9(4) . . ? C8 N4 H4B 120.5 . . ? N5 N4 H4B 120.5 . . ? C16 N5 N4 116.3(4) . . ? C19 N6 C20 116.6(5) . . ? C22 N7 C26 119.2(4) . . ? C22 N7 Ru1 126.5(3) . . ? C26 N7 Ru1 114.2(3) . . ? C27 N8 C31 120.7(4) . . ? C27 N8 Ru1 119.5(3) . . ? C31 N8 Ru1 119.6(3) . . ? C36 N9 C32 119.2(4) . . ? C36 N9 Ru1 127.1(3) . . ? C32 N9 Ru1 113.7(3) . . ? N11 N10 C29 118.5(4) . . ? N11 N10 H10A 120.8 . . ? C29 N10 H10A 120.8 . . ? C37 N11 N10 117.0(4) . . ? C41 N12 C40 116.9(5) . . ? N1 C1 C2 122.0(5) . . ? N1 C1 H1A 119.0 . . ? C2 C1 H1A 119.0 . . ? C3 C2 C1 118.9(5) . . ? C3 C2 H2A 120.5 . . ? C1 C2 H2A 120.5 . . ? C2 C3 C4 120.0(4) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C3 C4 C5 118.7(5) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? N1 C5 C4 121.6(4) . . ? N1 C5 C6 115.4(4) . . ? C4 C5 C6 123.0(4) . . ? N2 C6 C7 121.5(4) . . ? N2 C6 C5 111.7(4) . . ? C7 C6 C5 126.8(4) . . ? C6 C7 C8 119.3(4) . . ? C6 C7 H7A 120.4 . . ? C8 C7 H7A 120.4 . . ? N4 C8 C7 118.9(4) . . ? N4 C8 C9 122.3(4) . . ? C7 C8 C9 118.8(4) . . ? C10 C9 C8 119.2(4) . . ? C10 C9 H9A 120.4 . . ? C8 C9 H9A 120.4 . . ? N2 C10 C9 121.1(4) . . ? N2 C10 C11 111.2(4) . . ? C9 C10 C11 127.7(4) . . ? N3 C11 C12 121.0(4) . . ? N3 C11 C10 115.8(4) . . ? C12 C11 C10 123.2(4) . . ? C11 C12 C13 119.3(5) . . ? C11 C12 H12A 120.4 . . ? C13 C12 H12A 120.4 . . ? C14 C13 C12 119.7(4) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C15 C14 C13 118.6(4) . . ? C15 C14 H14A 120.7 . . ? C13 C14 H14A 120.7 . . ? N3 C15 C14 122.6(4) . . ? N3 C15 H15A 118.7 . . ? C14 C15 H15A 118.7 . . ? N5 C16 C17 120.2(5) . . ? N5 C16 H16A 119.9 . . ? C17 C16 H16A 119.9 . . ? C21 C17 C18 118.0(5) . . ? C21 C17 C16 119.4(5) . . ? C18 C17 C16 122.6(5) . . ? C19 C18 C17 118.5(6) . . ? C19 C18 H18A 120.8 . . ? C17 C18 H18A 120.8 . . ? N6 C19 C18 124.5(6) . . ? N6 C19 H19A 117.7 . . ? C18 C19 H19A 117.7 . . ? N6 C20 C21 123.5(6) . . ? N6 C20 H20A 118.2 . . ? C21 C20 H20A 118.2 . . ? C17 C21 C20 118.9(6) . . ? C17 C21 H21A 120.5 . . ? C20 C21 H21A 120.5 . . ? N7 C22 C23 122.4(5) . . ? N7 C22 H22A 118.8 . . ? C23 C22 H22A 118.8 . . ? C24 C23 C22 118.5(5) . . ? C24 C23 H23A 120.7 . . ? C22 C23 H23A 120.7 . . ? C23 C24 C25 120.4(5) . . ? C23 C24 H24A 119.8 . . ? C25 C24 H24A 119.8 . . ? C24 C25 C26 118.5(5) . . ? C24 C25 H25A 120.8 . . ? C26 C25 H25A 120.8 . . ? N7 C26 C25 121.0(4) . . ? N7 C26 C27 115.2(4) . . ? C25 C26 C27 123.8(4) . . ? N8 C27 C28 120.9(4) . . ? N8 C27 C26 112.0(4) . . ? C28 C27 C26 127.0(4) . . ? C27 C28 C29 119.1(4) . . ? C27 C28 H28A 120.5 . . ? C29 C28 H28A 120.5 . . ? N10 C29 C28 122.1(4) . . ? N10 C29 C30 118.9(4) . . ? C28 C29 C30 119.0(4) . . ? C31 C30 C29 119.0(4) . . ? C31 C30 H30A 120.5 . . ? C29 C30 H30A 120.5 . . ? N8 C31 C30 121.2(4) . . ? N8 C31 C32 111.6(4) . . ? C30 C31 C32 127.2(4) . . ? N9 C32 C33 120.6(4) . . ? N9 C32 C31 115.8(4) . . ? C33 C32 C31 123.6(4) . . ? C34 C33 C32 118.8(4) . . ? C34 C33 H33A 120.6 . . ? C32 C33 H33A 120.6 . . ? C35 C34 C33 120.5(4) . . ? C35 C34 H34A 119.7 . . ? C33 C34 H34A 119.7 . . ? C34 C35 C36 118.6(4) . . ? C34 C35 H35A 120.7 . . ? C36 C35 H35A 120.7 . . ? N9 C36 C35 122.2(4) . . ? N9 C36 H36A 118.9 . . ? C35 C36 H36A 118.9 . . ? N11 C37 C38 119.7(5) . . ? N11 C37 H37A 120.2 . . ? C38 C37 H37A 120.2 . . ? C42 C38 C39 118.1(5) . . ? C42 C38 C37 119.8(5) . . ? C39 C38 C37 122.0(4) . . ? C40 C39 C38 119.1(5) . . ? C40 C39 H39A 120.5 . . ? C38 C39 H39A 120.5 . . ? N12 C40 C39 123.2(6) . . ? N12 C40 H40A 118.4 . . ? C39 C40 H40A 118.4 . . ? N12 C41 C42 123.9(5) . . ? N12 C41 H41A 118.0 . . ? C42 C41 H41A 118.0 . . ? C41 C42 C38 118.7(5) . . ? C41 C42 H42A 120.7 . . ? C38 C42 H42A 120.7 . . ? O11 N100 O13 126.0(7) . . ? O11 N100 O12 120.3(6) . . ? O13 N100 O12 112.9(6) . . ? O21 N200 O22 118.4(6) . . ? O21 N200 O23 120.4(5) . . ? O22 N200 O23 121.1(5) . . ? H30C O30 H30D 159.4 . . ? H40C O40 H40D 95(6) . . ? H50B O50 H50A 85(6) . . ? H60A O60 H60B 105(7) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.228 _refine_diff_density_min -0.859 _refine_diff_density_rms 0.086 # start Validation Reply Form _vrf_PLAT430_jb1220 ; PROBLEM: Short Inter D...A Contact O12 .. O70 .. 1.84 Ang. RESPONSE: O70 is only 25% occupancy ; # end Validation Reply Form # Attachment 'Ru_1_2_PF6_JZ.CIF' data_jb643 _database_code_depnum_ccdc_archive 'CCDC 692944' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H32 N12 Ru, 2(F6 P)' _chemical_formula_sum 'C42 H32 F12 N12 P2 Ru' _chemical_formula_weight 1095.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall -C2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.324(5) _cell_length_b 17.924(4) _cell_length_c 10.753(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.08(3) _cell_angle_gamma 90.00 _cell_volume 4165.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.747 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2200 _exptl_absorpt_coefficient_mu 0.559 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17314 _diffrn_reflns_av_R_equivalents 0.1765 _diffrn_reflns_av_sigmaI/netI 0.0950 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3698 _reflns_number_gt 3241 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1006P)^2^+15.5980P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3698 _refine_ls_number_parameters 367 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_gt 0.0739 _refine_ls_wR_factor_ref 0.1947 _refine_ls_wR_factor_gt 0.1865 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.5000 0.73351(3) 0.7500 0.0299(2) Uani 1 2 d S . . N1 N 0.4941(2) 0.8156(3) 0.8800(5) 0.0345(10) Uani 1 1 d . . . N2 N 0.5849(2) 0.7319(3) 0.8898(4) 0.0314(10) Uani 1 1 d . . . N3 N 0.5420(2) 0.6533(3) 0.6738(4) 0.0325(10) Uani 1 1 d . . . C1 C 0.4454(3) 0.8592(3) 0.8647(6) 0.0381(13) Uani 1 1 d . . . H1A H 0.4091 0.8539 0.7860 0.046 Uiso 1 1 calc R . . C2 C 0.4458(3) 0.9119(4) 0.9593(6) 0.0427(14) Uani 1 1 d . . . H2A H 0.4099 0.9408 0.9469 0.051 Uiso 1 1 calc R . . C3 C 0.4982(3) 0.9216(4) 1.0705(6) 0.0431(14) Uani 1 1 d . . . H3A H 0.4996 0.9577 1.1362 0.052 Uiso 1 1 calc R . . N4 N 0.7538(2) 0.7098(3) 1.1972(5) 0.0427(12) Uani 1 1 d . . . H4B H 0.7783 0.6737 1.1918 0.051 Uiso 1 1 calc R . . C4 C 0.5497(3) 0.8777(3) 1.0859(5) 0.0377(13) Uani 1 1 d . . . H4A H 0.5867 0.8836 1.1629 0.045 Uiso 1 1 calc R . . N5 N 0.7712(2) 0.7544(3) 1.3080(5) 0.0390(11) Uani 1 1 d . . . C5 C 0.5471(2) 0.8261(3) 0.9903(5) 0.0347(12) Uani 1 1 d . . . C6 C 0.5990(3) 0.7780(3) 0.9973(5) 0.0323(11) Uani 1 1 d . . . N6 N 0.8966(3) 0.8650(3) 1.7623(5) 0.0483(13) Uani 1 1 d . . . C7 C 0.6562(3) 0.7745(3) 1.1006(6) 0.0359(13) Uani 1 1 d . . . H7A H 0.6668 0.8080 1.1743 0.043 Uiso 1 1 calc R . . C8 C 0.6979(3) 0.7212(3) 1.0942(5) 0.0363(13) Uani 1 1 d . . . C9 C 0.6835(3) 0.6743(3) 0.9810(6) 0.0377(13) Uani 1 1 d . . . H9A H 0.7124 0.6386 0.9748 0.045 Uiso 1 1 calc R . . C10 C 0.6256(2) 0.6821(3) 0.8792(5) 0.0319(11) Uani 1 1 d . . . C11 C 0.6022(2) 0.6388(3) 0.7536(5) 0.0314(11) Uani 1 1 d . . . C12 C 0.6377(3) 0.5882(4) 0.7165(6) 0.0413(13) Uani 1 1 d . . . H12A H 0.6792 0.5783 0.7746 0.050 Uiso 1 1 calc R . . C13 C 0.6123(3) 0.5521(4) 0.5938(6) 0.0451(14) Uani 1 1 d . . . H13A H 0.6360 0.5175 0.5661 0.054 Uiso 1 1 calc R . . C14 C 0.5520(3) 0.5675(4) 0.5131(6) 0.0440(14) Uani 1 1 d . . . H14A H 0.5339 0.5440 0.4281 0.053 Uiso 1 1 calc R . . C15 C 0.5181(3) 0.6163(3) 0.5547(5) 0.0371(13) Uani 1 1 d . . . H15A H 0.4762 0.6250 0.4983 0.044 Uiso 1 1 calc R . . C16 C 0.8184(3) 0.7342(4) 1.4069(6) 0.0407(14) Uani 1 1 d . . . H16A H 0.8383 0.6887 1.4017 0.049 Uiso 1 1 calc R . . C17 C 0.8434(3) 0.7794(3) 1.5297(6) 0.0379(13) Uani 1 1 d . . . C18 C 0.8135(3) 0.8408(4) 1.5511(6) 0.0454(15) Uani 1 1 d . . . H18A H 0.7745 0.8552 1.4864 0.054 Uiso 1 1 calc R . . C19 C 0.8406(3) 0.8817(4) 1.6681(6) 0.0486(15) Uani 1 1 d . . . H19A H 0.8189 0.9235 1.6826 0.058 Uiso 1 1 calc R . . C20 C 0.9239(3) 0.8051(4) 1.7389(6) 0.0498(16) Uani 1 1 d . . . H20A H 0.9628 0.7916 1.8049 0.060 Uiso 1 1 calc R . . C21 C 0.9005(3) 0.7606(4) 1.6262(6) 0.0429(14) Uani 1 1 d . . . H21A H 0.9228 0.7185 1.6151 0.052 Uiso 1 1 calc R . . P1 P 0.68494(8) 1.00547(10) 1.40523(16) 0.0441(4) Uani 1 1 d . . . F1 F 0.6874(4) 1.0709(5) 1.5020(9) 0.093(3) Uani 0.822(14) 1 d P A 1 F2 F 0.6880(3) 0.9389(4) 1.3088(6) 0.077(2) Uani 0.822(14) 1 d P A 1 F3 F 0.6837(2) 1.0659(4) 1.2953(7) 0.070(3) Uani 0.822(14) 1 d P A 1 F4 F 0.6899(3) 0.9452(4) 1.5166(8) 0.068(2) Uani 0.822(14) 1 d P A 1 F5 F 0.6131(6) 1.0071(7) 1.3522(13) 0.099(4) Uani 0.822(14) 1 d PU A 1 F6 F 0.7591(4) 1.0076(5) 1.4508(10) 0.058(2) Uani 0.822(14) 1 d P A 1 F1' F 0.6792(12) 1.0988(17) 1.374(3) 0.064(8) Uani 0.178(14) 1 d PU A 2 F2' F 0.668(2) 0.990(3) 1.262(4) 0.118(15) Uani 0.178(14) 1 d PU A 2 F3' F 0.6729(16) 0.9244(18) 1.437(4) 0.074(9) Uani 0.178(14) 1 d PU A 2 F4' F 0.7537(14) 1.0104(18) 1.487(3) 0.023(6) Uani 0.178(14) 1 d PU A 2 F5' F 0.6084(15) 0.9938(18) 1.340(3) 0.020(5) Uani 0.178(14) 1 d PU A 2 F6' F 0.667(3) 1.035(3) 1.519(5) 0.115(15) Uani 0.178(14) 1 d PU A 2 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 0.0221(4) 0.0300(4) 0.0254(3) 0.000 -0.0051(2) 0.000 N1 0.022(2) 0.034(3) 0.036(2) 0.0034(19) -0.0028(17) -0.0003(18) N2 0.025(2) 0.030(2) 0.027(2) -0.0022(17) -0.0036(17) 0.0017(18) N3 0.031(2) 0.029(2) 0.026(2) -0.0007(17) -0.0027(17) -0.0030(18) C1 0.029(3) 0.038(3) 0.037(3) 0.002(2) 0.001(2) 0.003(2) C2 0.032(3) 0.048(4) 0.042(3) -0.001(3) 0.008(2) 0.006(3) C3 0.045(3) 0.039(3) 0.038(3) -0.003(2) 0.007(3) 0.008(3) N4 0.027(2) 0.045(3) 0.036(3) -0.006(2) -0.010(2) 0.007(2) C4 0.035(3) 0.040(3) 0.029(3) -0.003(2) 0.002(2) 0.001(2) N5 0.027(2) 0.042(3) 0.034(3) -0.003(2) -0.0044(19) 0.001(2) C5 0.029(3) 0.035(3) 0.030(3) 0.005(2) -0.002(2) 0.002(2) C6 0.030(3) 0.029(3) 0.030(3) -0.002(2) 0.003(2) -0.001(2) N6 0.047(3) 0.049(3) 0.033(3) -0.001(2) -0.002(2) 0.001(2) C7 0.030(3) 0.034(3) 0.032(3) -0.004(2) -0.003(2) -0.003(2) C8 0.025(3) 0.046(3) 0.027(3) 0.002(2) -0.003(2) 0.002(2) C9 0.026(3) 0.039(3) 0.039(3) 0.000(2) 0.002(2) 0.000(2) C10 0.022(2) 0.033(3) 0.032(3) 0.004(2) 0.000(2) 0.004(2) C11 0.031(3) 0.027(3) 0.027(2) 0.001(2) 0.001(2) 0.001(2) C12 0.036(3) 0.043(3) 0.037(3) 0.000(2) 0.005(2) 0.001(3) C13 0.052(4) 0.037(3) 0.043(3) -0.002(2) 0.013(3) 0.001(3) C14 0.057(4) 0.038(3) 0.033(3) -0.004(2) 0.011(3) -0.005(3) C15 0.041(3) 0.031(3) 0.025(3) 0.001(2) -0.004(2) -0.006(2) C16 0.036(3) 0.044(3) 0.031(3) 0.000(2) -0.002(2) 0.003(3) C17 0.030(3) 0.039(3) 0.034(3) 0.000(2) -0.001(2) -0.005(2) C18 0.037(3) 0.045(4) 0.037(3) 0.004(3) -0.006(2) 0.001(3) C19 0.054(4) 0.042(4) 0.037(3) -0.005(3) 0.004(3) 0.002(3) C20 0.046(4) 0.056(4) 0.028(3) 0.003(3) -0.008(2) -0.004(3) C21 0.041(3) 0.045(3) 0.031(3) -0.001(2) 0.001(2) 0.011(3) P1 0.0381(9) 0.0416(9) 0.0430(9) 0.0032(7) 0.0044(7) -0.0041(7) F1 0.099(6) 0.075(5) 0.113(6) -0.041(5) 0.046(5) 0.004(4) F2 0.078(4) 0.071(5) 0.066(4) -0.030(3) 0.009(3) -0.007(3) F3 0.046(3) 0.071(4) 0.079(5) 0.043(4) 0.006(3) -0.004(3) F4 0.057(3) 0.081(5) 0.063(4) 0.033(3) 0.019(3) 0.008(3) F5 0.045(4) 0.088(8) 0.139(8) 0.039(6) 0.006(4) -0.016(4) F6 0.045(3) 0.056(4) 0.068(6) 0.001(4) 0.017(3) 0.005(2) F1' 0.047(12) 0.068(14) 0.075(16) -0.004(12) 0.021(10) -0.010(10) F2' 0.13(2) 0.13(2) 0.093(19) -0.018(16) 0.039(15) 0.016(17) F3' 0.069(15) 0.057(14) 0.089(18) 0.015(13) 0.022(13) 0.013(11) F4' 0.020(7) 0.018(7) 0.024(7) 0.002(5) -0.001(4) 0.001(4) F5' 0.017(7) 0.019(7) 0.021(6) -0.002(4) 0.004(4) -0.004(4) F6' 0.14(2) 0.12(2) 0.095(19) -0.021(16) 0.057(16) -0.026(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N2 1.986(4) 2_656 ? Ru1 N2 1.986(4) . ? Ru1 N1 2.069(5) . ? Ru1 N1 2.069(5) 2_656 ? Ru1 N3 2.075(5) 2_656 ? Ru1 N3 2.075(5) . ? N1 C1 1.338(7) . ? N1 C5 1.367(7) . ? N2 C10 1.339(7) . ? N2 C6 1.357(7) . ? N3 C15 1.361(7) . ? N3 C11 1.366(7) . ? C1 C2 1.385(9) . ? C1 H1A 0.9500 . ? C2 C3 1.362(9) . ? C2 H2A 0.9500 . ? C3 C4 1.392(8) . ? C3 H3A 0.9500 . ? N4 N5 1.365(7) . ? N4 C8 1.372(7) . ? N4 H4B 0.8800 . ? C4 C5 1.368(8) . ? C4 H4A 0.9500 . ? N5 C16 1.263(8) . ? C5 C6 1.464(8) . ? C6 C7 1.381(8) . ? N6 C20 1.320(9) . ? N6 C19 1.351(8) . ? C7 C8 1.382(9) . ? C7 H7A 0.9500 . ? C8 C9 1.413(8) . ? C9 C10 1.390(7) . ? C9 H9A 0.9500 . ? C10 C11 1.474(7) . ? C11 C12 1.384(8) . ? C12 C13 1.387(8) . ? C12 H12A 0.9500 . ? C13 C14 1.375(9) . ? C13 H13A 0.9500 . ? C14 C15 1.362(9) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.470(8) . ? C16 H16A 0.9500 . ? C17 C18 1.367(9) . ? C17 C21 1.387(8) . ? C18 C19 1.387(9) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C21 1.381(9) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? P1 F2' 1.47(4) . ? P1 F6' 1.53(4) . ? P1 F3' 1.54(3) . ? P1 F5 1.554(12) . ? P1 F1 1.555(7) . ? P1 F4' 1.51(3) . ? P1 F4 1.584(6) . ? P1 F3 1.595(5) . ? P1 F6 1.612(8) . ? P1 F2 1.599(6) . ? P1 F5' 1.67(3) . ? P1 F1' 1.70(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ru1 N2 178.3(3) 2_656 . ? N2 Ru1 N1 102.81(18) 2_656 . ? N2 Ru1 N1 78.43(17) . . ? N2 Ru1 N1 78.43(17) 2_656 2_656 ? N2 Ru1 N1 102.81(18) . 2_656 ? N1 Ru1 N1 89.4(3) . 2_656 ? N2 Ru1 N3 78.68(17) 2_656 2_656 ? N2 Ru1 N3 100.12(18) . 2_656 ? N1 Ru1 N3 93.72(19) . 2_656 ? N1 Ru1 N3 157.02(17) 2_656 2_656 ? N2 Ru1 N3 100.12(18) 2_656 . ? N2 Ru1 N3 78.68(17) . . ? N1 Ru1 N3 157.02(17) . . ? N1 Ru1 N3 93.72(18) 2_656 . ? N3 Ru1 N3 92.2(3) 2_656 . ? C1 N1 C5 118.4(5) . . ? C1 N1 Ru1 126.9(4) . . ? C5 N1 Ru1 114.6(4) . . ? C10 N2 C6 121.8(4) . . ? C10 N2 Ru1 118.9(3) . . ? C6 N2 Ru1 119.3(4) . . ? C15 N3 C11 117.3(5) . . ? C15 N3 Ru1 128.4(4) . . ? C11 N3 Ru1 114.2(3) . . ? N1 C1 C2 122.5(5) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? C3 C2 C1 119.2(6) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C2 C3 C4 118.8(6) . . ? C2 C3 H3A 120.6 . . ? C4 C3 H3A 120.6 . . ? N5 N4 C8 119.8(5) . . ? N5 N4 H4B 120.1 . . ? C8 N4 H4B 120.1 . . ? C5 C4 C3 120.0(5) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C16 N5 N4 116.4(5) . . ? N1 C5 C4 121.1(5) . . ? N1 C5 C6 115.0(5) . . ? C4 C5 C6 123.9(5) . . ? N2 C6 C7 120.6(5) . . ? N2 C6 C5 112.6(5) . . ? C7 C6 C5 126.7(5) . . ? C20 N6 C19 115.8(5) . . ? C6 C7 C8 118.4(5) . . ? C6 C7 H7A 120.8 . . ? C8 C7 H7A 120.8 . . ? N4 C8 C7 122.4(5) . . ? N4 C8 C9 116.8(5) . . ? C7 C8 C9 120.7(5) . . ? C10 C9 C8 117.7(5) . . ? C10 C9 H9A 121.2 . . ? C8 C9 H9A 121.2 . . ? N2 C10 C9 120.7(5) . . ? N2 C10 C11 113.5(4) . . ? C9 C10 C11 125.8(5) . . ? N3 C11 C12 121.9(5) . . ? N3 C11 C10 114.5(5) . . ? C12 C11 C10 123.6(5) . . ? C11 C12 C13 119.4(5) . . ? C11 C12 H12A 120.3 . . ? C13 C12 H12A 120.3 . . ? C14 C13 C12 118.5(6) . . ? C14 C13 H13A 120.8 . . ? C12 C13 H13A 120.8 . . ? C15 C14 C13 120.3(6) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? N3 C15 C14 122.6(5) . . ? N3 C15 H15A 118.7 . . ? C14 C15 H15A 118.7 . . ? N5 C16 C17 121.6(6) . . ? N5 C16 H16A 119.2 . . ? C17 C16 H16A 119.2 . . ? C18 C17 C21 118.4(5) . . ? C18 C17 C16 122.6(5) . . ? C21 C17 C16 118.9(6) . . ? C17 C18 C19 119.4(6) . . ? C17 C18 H18A 120.3 . . ? C19 C18 H18A 120.3 . . ? N6 C19 C18 123.1(6) . . ? N6 C19 H19A 118.4 . . ? C18 C19 H19A 118.4 . . ? N6 C20 C21 125.3(6) . . ? N6 C20 H20A 117.4 . . ? C21 C20 H20A 117.4 . . ? C20 C21 C17 117.9(6) . . ? C20 C21 H21A 121.0 . . ? C17 C21 H21A 121.0 . . ? F2' P1 F6' 149(3) . . ? F2' P1 F3' 93(3) . . ? F6' P1 F3' 91(2) . . ? F2' P1 F5 77.5(19) . . ? F6' P1 F5 73(2) . . ? F3' P1 F5 80.6(13) . . ? F2' P1 F1 140(2) . . ? F3' P1 F1 121.6(16) . . ? F5 P1 F1 89.7(6) . . ? F2' P1 F4' 116(2) . . ? F6' P1 F4' 94(2) . . ? F3' P1 F4' 99.6(18) . . ? F5 P1 F4' 166.5(11) . . ? F1 P1 F4' 78.6(12) . . ? F2' P1 F4 125(2) . . ? F6' P1 F4 66(2) . . ? F5 P1 F4 93.0(5) . . ? F1 P1 F4 92.0(5) . . ? F4' P1 F4 80.8(12) . . ? F2' P1 F3 55(2) . . ? F6' P1 F3 115(2) . . ? F3' P1 F3 148.3(16) . . ? F5 P1 F3 89.9(5) . . ? F1 P1 F3 88.2(5) . . ? F4' P1 F3 96.4(12) . . ? F4 P1 F3 177.1(3) . . ? F2' P1 F6 99.5(19) . . ? F6' P1 F6 109(2) . . ? F3' P1 F6 102.7(12) . . ? F5 P1 F6 175.7(6) . . ? F1 P1 F6 90.8(5) . . ? F4 P1 F6 91.3(4) . . ? F3 P1 F6 85.8(4) . . ? F6' P1 F2 150(2) . . ? F3' P1 F2 60.0(16) . . ? F5 P1 F2 94.6(6) . . ? F1 P1 F2 175.7(4) . . ? F4' P1 F2 97.2(12) . . ? F4 P1 F2 88.4(4) . . ? F3 P1 F2 91.1(4) . . ? F6 P1 F2 84.9(4) . . ? F2' P1 F5' 73(2) . . ? F6' P1 F5' 79(2) . . ? F3' P1 F5' 73.8(17) . . ? F1 P1 F5' 98.1(9) . . ? F4' P1 F5' 170.0(15) . . ? F4 P1 F5' 89.8(11) . . ? F3 P1 F5' 93.0(11) . . ? F6 P1 F5' 171.0(9) . . ? F2 P1 F5' 86.2(9) . . ? F2' P1 F1' 90(2) . . ? F6' P1 F1' 78(2) . . ? F3' P1 F1' 164.1(15) . . ? F5 P1 F1' 85.2(10) . . ? F1 P1 F1' 50.9(11) . . ? F4' P1 F1' 92.5(15) . . ? F4 P1 F1' 142.8(12) . . ? F6 P1 F1' 91.8(9) . . ? F2 P1 F1' 128.8(12) . . ? F5' P1 F1' 92.7(14) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.554 _refine_diff_density_min -1.662 _refine_diff_density_rms 0.135 # start Validation Reply Form _vrf_PLAT221_jb643 ; PROBLEM: Large Solvent/Anion F Ueq(max)/Ueq(min) ... 5.95 Ratio RESPONSE: Related to disorder ; # end Validation Reply Form