Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'C. E. Housecroft' 'Jonathon E. Beves' 'E. Constable' 'Emma L. Dunphy' 'Cameron Kepert' 'Markus Neuburger' 'David J. Price' 'Silvia Schaffner' _publ_contact_author_name 'C. E. Housecroft' _publ_contact_author_address ; Departement Chemie University of Basel Spitalstrasse 51 Basel CH-4056 SWITZERLAND ; _publ_contact_author_email CATHERINE.HOUSECROFT@UNIBAS.CH _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Vectorial property dependence in bis{4'-(n-pyridyl)-2,2':6',2"-terpyridine}iron(II) and ruthenium(II) complexes with n = 2, 3 and 4 ; _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' # Attachment 'Fe_2pytpy_2.cif' data_jb1125 _database_code_depnum_ccdc_archive 'CCDC 662661' _audit_creation_date 07-06-27 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '6260926 jb1125_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 15.7521(6) _cell_length_b 16.1814(6) _cell_length_c 17.3664(6) _cell_angle_alpha 94.145(2) _cell_angle_beta 99.444(2) _cell_angle_gamma 109.4686(16) _cell_volume 4078.3(3) _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' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 # Given Formula = C160 H130 F48 Fe4 N32 O9 P8 # Dc = 1.64 Fooo = 2042.00 Mu = 5.53 M = 2014.04 # Found Formula = C160 H130 F48 Fe4 N32 O9 P8 # Dc = 1.64 FOOO = 2042.00 Mu = 5.53 M = 2014.04 _chemical_formula_sum 'C160 H130 F48 Fe4 N32 O9 P8' _chemical_formula_moiety '4(C40 H28 Fe N8), 8(F6 P), 8(H2 O), H2 O' _chemical_compound_source ? _chemical_formula_weight 4028.08 _cell_measurement_reflns_used 15846 _cell_measurement_theta_min 1 _cell_measurement_theta_max 28 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2042 _exptl_absorpt_coefficient_mu 0.553 # Sheldrick geometric approximatio 0.85 0.96 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.85 _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 '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 32121 _reflns_number_total 18648 _diffrn_reflns_av_R_equivalents 0.045 # Number of reflections with Friedels Law is 18648 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 19385 _diffrn_reflns_theta_min 1.200 _diffrn_reflns_theta_max 27.840 _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.056 _diffrn_measured_fraction_theta_full 0.975 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -20 _reflns_limit_h_max 20 _reflns_limit_k_min -21 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.64 _refine_diff_density_max 0.73 _refine_ls_number_reflns 12869 _refine_ls_number_restraints 1517 _refine_ls_number_parameters 1180 _refine_ls_wR_factor_ref 0.0842 _refine_ls_goodness_of_fit_ref 1.0087 _refine_ls_R_factor_all 0.1172 _refine_ls_wR_factor_all 0.1214 _reflns_threshold_expression I>1.0\s(I) _reflns_number_gt 12869 _refine_ls_R_factor_gt 0.0776 _refine_ls_wR_factor_gt 0.0842 _refine_ls_shift/su_max 0.013387 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.88 1.92 1.25 ; 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 0.59813(3) 0.81878(3) 0.25568(2) 0.0302 1.0000 Uani . . . . . . Fe2 Fe 0.92986(3) 0.67009(3) 0.70887(2) 0.0317 1.0000 Uani . . . . . . N1 N 0.5292(2) 0.69024(19) 0.24060(16) 0.0349 1.0000 Uani . . . . . . N2 N 0.57046(19) 0.79898(18) 0.14510(14) 0.0311 1.0000 Uani . . . . . . N3 N 0.65750(19) 0.94121(18) 0.23469(15) 0.0318 1.0000 Uani . . . . . . N4 N 0.48666(19) 0.84240(19) 0.27348(15) 0.0337 1.0000 Uani . . . . . . N5 N 0.62588(19) 0.84010(18) 0.36623(15) 0.0314 1.0000 Uani . . . . . . N6 N 0.7176(2) 0.80096(19) 0.27412(15) 0.0330 1.0000 Uani . . . . . . N7 N 0.4859(2) 0.8301(2) -0.13704(16) 0.0431 1.0000 Uani . . . . . . N8 N 0.7755(2) 0.8863(2) 0.64831(17) 0.0418 1.0000 Uani . . . . . . N51 N 0.9875(2) 0.79993(19) 0.71526(16) 0.0348 1.0000 Uani . . . . . . N52 N 0.96170(19) 0.69872(19) 0.81876(15) 0.0328 1.0000 Uani . . . . . . N53 N 0.8807(2) 0.55047(19) 0.73912(16) 0.0352 1.0000 Uani . . . . . . N54 N 1.0428(2) 0.65314(18) 0.68825(16) 0.0339 1.0000 Uani . . . . . . N55 N 0.8974(2) 0.64277(19) 0.59867(16) 0.0373 1.0000 Uani . . . . . . N56 N 0.8050(2) 0.67698(19) 0.69290(15) 0.0348 1.0000 Uani . . . . . . N57 N 1.0376(3) 0.8562(3) 1.0899(2) 0.0703 1.0000 Uani . . . . . . N58 N 0.8933(4) 0.5752(2) 0.3128(2) 0.0672 1.0000 Uani . . . . . . C1 C 0.5108(3) 0.6381(2) 0.2964(2) 0.0428 1.0000 Uani . . . . . . C2 C 0.4589(3) 0.5494(3) 0.2799(2) 0.0556 1.0000 Uani . . . . . . C3 C 0.4243(3) 0.5114(3) 0.2019(2) 0.0560 1.0000 Uani . . . . . . C4 C 0.4422(3) 0.5648(3) 0.1427(2) 0.0488 1.0000 Uani . . . . . . C5 C 0.4954(2) 0.6535(2) 0.16334(18) 0.0358 1.0000 Uani . . . . . . C6 C 0.5201(2) 0.7169(2) 0.10679(18) 0.0323 1.0000 Uani . . . . . . C7 C 0.4940(2) 0.7011(2) 0.02591(18) 0.0339 1.0000 Uani . . . . . . C8 C 0.5220(2) 0.7716(2) -0.01735(18) 0.0353 1.0000 Uani . . . . . . C9 C 0.5768(2) 0.8548(2) 0.02214(18) 0.0336 1.0000 Uani . . . . . . C10 C 0.5989(2) 0.8675(2) 0.10407(17) 0.0307 1.0000 Uani . . . . . . C11 C 0.6503(2) 0.9500(2) 0.15658(18) 0.0322 1.0000 Uani . . . . . . C12 C 0.6872(2) 1.0323(2) 0.13173(19) 0.0376 1.0000 Uani . . . . . . C13 C 0.7311(3) 1.1064(2) 0.1870(2) 0.0425 1.0000 Uani . . . . . . C14 C 0.7382(3) 1.0973(2) 0.2663(2) 0.0412 1.0000 Uani . . . . . . C15 C 0.7011(2) 1.0136(2) 0.28773(19) 0.0359 1.0000 Uani . . . . . . C16 C 0.4147(2) 0.8399(2) 0.2184(2) 0.0382 1.0000 Uani . . . . . . C17 C 0.3375(3) 0.8514(3) 0.2378(2) 0.0437 1.0000 Uani . . . . . . C18 C 0.3336(3) 0.8682(3) 0.3166(2) 0.0419 1.0000 Uani . . . . . . C19 C 0.4079(3) 0.8723(3) 0.3738(2) 0.0402 1.0000 Uani . . . . . . C20 C 0.4833(2) 0.8591(2) 0.35069(18) 0.0328 1.0000 Uani . . . . . . C21 C 0.5653(2) 0.8592(2) 0.40527(18) 0.0331 1.0000 Uani . . . . . . C22 C 0.5854(3) 0.8763(2) 0.48702(19) 0.0369 1.0000 Uani . . . . . . C23 C 0.6679(2) 0.8738(2) 0.52906(18) 0.0343 1.0000 Uani . . . . . . C24 C 0.7287(2) 0.8533(2) 0.48706(18) 0.0350 1.0000 Uani . . . . . . C25 C 0.7060(2) 0.8376(2) 0.40579(18) 0.0325 1.0000 Uani . . . . . . C26 C 0.7605(2) 0.8161(2) 0.35161(17) 0.0316 1.0000 Uani . . . . . . C27 C 0.8468(2) 0.8108(2) 0.37428(19) 0.0353 1.0000 Uani . . . . . . C28 C 0.8907(2) 0.7881(2) 0.3171(2) 0.0377 1.0000 Uani . . . . . . C29 C 0.8458(2) 0.7710(2) 0.23910(19) 0.0363 1.0000 Uani . . . . . . C30 C 0.7600(3) 0.7779(2) 0.21981(19) 0.0367 1.0000 Uani . . . . . . C31 C 0.4919(2) 0.7584(2) -0.10487(19) 0.0371 1.0000 Uani . . . . . . C32 C 0.4713(2) 0.6772(3) -0.1493(2) 0.0405 1.0000 Uani . . . . . . C33 C 0.4437(3) 0.6701(3) -0.2307(2) 0.0511 1.0000 Uani . . . . . . C34 C 0.4372(3) 0.7420(3) -0.2645(2) 0.0516 1.0000 Uani . . . . . . C35 C 0.4577(3) 0.8206(3) -0.2161(2) 0.0533 1.0000 Uani . . . . . . C36 C 0.6932(2) 0.8914(2) 0.61660(18) 0.0353 1.0000 Uani . . . . . . C37 C 0.6373(3) 0.9119(3) 0.6620(2) 0.0430 1.0000 Uani . . . . . . C38 C 0.6671(3) 0.9294(3) 0.7435(2) 0.0479 1.0000 Uani . . . . . . C39 C 0.7505(3) 0.9247(3) 0.7763(2) 0.0488 1.0000 Uani . . . . . . C40 C 0.8024(3) 0.9027(3) 0.7265(2) 0.0453 1.0000 Uani . . . . . . C51 C 0.9951(3) 0.8484(3) 0.6547(2) 0.0449 1.0000 Uani . . . . . . C52 C 1.0349(3) 0.9398(3) 0.6666(3) 0.0536 1.0000 Uani . . . . . . C53 C 1.0689(3) 0.9827(3) 0.7423(3) 0.0546 1.0000 Uani . . . . . . C54 C 1.0628(3) 0.9346(3) 0.8051(2) 0.0470 1.0000 Uani . . . . . . C55 C 1.0210(2) 0.8439(2) 0.7902(2) 0.0386 1.0000 Uani . . . . . . C56 C 1.0056(2) 0.7849(2) 0.8508(2) 0.0373 1.0000 Uani . . . . . . C57 C 1.0283(2) 0.8089(3) 0.9315(2) 0.0416 1.0000 Uani . . . . . . C58 C 1.0050(2) 0.7432(3) 0.9807(2) 0.0416 1.0000 Uani . . . . . . C59 C 0.9608(3) 0.6563(3) 0.9473(2) 0.0419 1.0000 Uani . . . . . . C60 C 0.9387(2) 0.6355(2) 0.86514(19) 0.0366 1.0000 Uani . . . . . . C61 C 0.8886(3) 0.5488(2) 0.8183(2) 0.0381 1.0000 Uani . . . . . . C62 C 0.8490(3) 0.4708(3) 0.8488(2) 0.0485 1.0000 Uani . . . . . . C63 C 0.8018(3) 0.3941(3) 0.7989(3) 0.0596 1.0000 Uani . . . . . . C64 C 0.7960(3) 0.3950(3) 0.7181(3) 0.0591 1.0000 Uani . . . . . . C65 C 0.8361(3) 0.4736(3) 0.6906(2) 0.0482 1.0000 Uani . . . . . . C66 C 1.1177(2) 0.6610(2) 0.7419(2) 0.0372 1.0000 Uani . . . . . . C67 C 1.1959(3) 0.6519(3) 0.7213(2) 0.0452 1.0000 Uani . . . . . . C68 C 1.1977(3) 0.6355(3) 0.6430(2) 0.0471 1.0000 Uani . . . . . . C69 C 1.1213(3) 0.6272(3) 0.5870(2) 0.0463 1.0000 Uani . . . . . . C70 C 1.0438(3) 0.6353(2) 0.61040(19) 0.0387 1.0000 Uani . . . . . . C71 C 0.9579(3) 0.6279(2) 0.55815(19) 0.0375 1.0000 Uani . . . . . . C72 C 0.9356(3) 0.6086(2) 0.4762(2) 0.0434 1.0000 Uani . . . . . . C73 C 0.8498(3) 0.6029(2) 0.4363(2) 0.0442 1.0000 Uani . . . . . . C74 C 0.7881(3) 0.6198(2) 0.4798(2) 0.0431 1.0000 Uani . . . . . . C75 C 0.8142(3) 0.6403(2) 0.56125(19) 0.0380 1.0000 Uani . . . . . . C76 C 0.7600(3) 0.6597(2) 0.61698(19) 0.0380 1.0000 Uani . . . . . . C77 C 0.6716(3) 0.6596(3) 0.5957(2) 0.0452 1.0000 Uani . . . . . . C78 C 0.6276(3) 0.6784(3) 0.6534(2) 0.0454 1.0000 Uani . . . . . . C79 C 0.6730(3) 0.6960(3) 0.7312(2) 0.0420 1.0000 Uani . . . . . . C80 C 0.7625(3) 0.6948(2) 0.7491(2) 0.0383 1.0000 Uani . . . . . . C81 C 1.0279(3) 0.7719(4) 1.0675(2) 0.0543 1.0000 Uani . . . . . . C82 C 1.0412(3) 0.7166(5) 1.1203(2) 0.0703 1.0000 Uani . . . . . . C83 C 1.0669(3) 0.7519(6) 1.2016(3) 0.0880 1.0000 Uani . . . . . . C84 C 1.0773(3) 0.8379(6) 1.2229(3) 0.0967 1.0000 Uani . . . . . . C85 C 1.0610(4) 0.8869(5) 1.1659(3) 0.0877 1.0000 Uani . . . . . . C86 C 0.8246(4) 0.5808(2) 0.3487(2) 0.0538 1.0000 Uani . . . . . . C87 C 0.7377(4) 0.5660(3) 0.3082(2) 0.0629 1.0000 Uani . . . . . . C88 C 0.7195(5) 0.5466(3) 0.2256(3) 0.0831 1.0000 Uani . . . . . . C89 C 0.7884(5) 0.5415(3) 0.1886(3) 0.0852 1.0000 Uani . . . . . . C90 C 0.8730(5) 0.5556(3) 0.2333(3) 0.0753 1.0000 Uani . . . . . . P1 P 0.73644(7) 0.68001(8) 0.98840(6) 0.0510 1.0000 Uani . . . . . . P2 P 0.24270(8) 0.69184(9) -0.01653(6) 0.0522 1.0000 Uani . . . . . . P3 P 0.14366(8) 0.86982(8) 0.47790(5) 0.0497 1.0000 Uani . . . . . . P4 P 0.38641(8) 0.62536(7) 0.48879(6) 0.0472 1.0000 Uani . . . . . . F1 F 0.6670(2) 0.6194(2) 1.0347(3) 0.0948 1.0000 Uani . . . . . . F2 F 0.8069(2) 0.7435(2) 0.94309(16) 0.0715 1.0000 Uani . . . . . . F3 F 0.7480(2) 0.5971(2) 0.9422(2) 0.0900 1.0000 Uani . . . . . . F4 F 0.7256(2) 0.76517(19) 1.03216(14) 0.0616 1.0000 Uani . . . . . . F5 F 0.6530(2) 0.6731(3) 0.92049(18) 0.0972 1.0000 Uani . . . . . . F6 F 0.81976(18) 0.6871(2) 1.05660(14) 0.0612 1.0000 Uani . . . . . . F11 F 0.2914(3) 0.6427(4) 0.0408(3) 0.1265 1.0000 Uani . . . . . . F12 F 0.19482(19) 0.7447(2) -0.07063(16) 0.0674 1.0000 Uani . . . . . . F13 F 0.2072(3) 0.7295(4) 0.05497(19) 0.1146 1.0000 Uani . . . . . . F14 F 0.2829(2) 0.6613(3) -0.08563(19) 0.0879 1.0000 Uani . . . . . . F15 F 0.1526(2) 0.6110(3) -0.0353(4) 0.1406 1.0000 Uani . . . . . . F16 F 0.3341(2) 0.7773(2) 0.0062(2) 0.0904 1.0000 Uani . . . . . . F21 F 0.1601(2) 0.9528(2) 0.54084(17) 0.0802 1.0000 Uani . . . . . . F22 F 0.1258(3) 0.7886(2) 0.4147(2) 0.1042 1.0000 Uani . . . . . . F23 F 0.1665(3) 0.8197(3) 0.5478(2) 0.1076 1.0000 Uani . . . . . . F24 F 0.1196(3) 0.9224(2) 0.40910(18) 0.1061 1.0000 Uani . . . . . . F26 F 0.0383(2) 0.8319(3) 0.48355(19) 0.0951 1.0000 Uani . . . . . . F31 F 0.3481(3) 0.53647(19) 0.4303(2) 0.0831 1.0000 Uani . . . . . . F32 F 0.4261(4) 0.7153(2) 0.5469(2) 0.1237 1.0000 Uani . . . . . . F33 F 0.3843(2) 0.67809(19) 0.41569(15) 0.0680 1.0000 Uani . . . . . . F34 F 0.3893(3) 0.5766(3) 0.56436(19) 0.0957 1.0000 Uani . . . . . . F35 F 0.2838(2) 0.6166(3) 0.49113(19) 0.1056 1.0000 Uani . . . . . . F36 F 0.4883(2) 0.6329(3) 0.48395(19) 0.0929 1.0000 Uani . . . . . . O1 O 0.5320(3) 1.0114(2) -0.0733(2) 0.0688 1.0000 Uani . . . . . . O2 O 0.7230(2) 1.0607(3) -0.06161(19) 0.0692 1.0000 Uani . . . . . . O3 O 0.8188(3) 0.9539(3) -0.0009(3) 0.0973 1.0000 Uani . . . . . . O4 O 0.9904(7) 0.9854(6) 0.0284(6) 0.1027 0.5000 Uani . . . . . . O5 O 0.4018(3) 0.8819(4) 0.5799(3) 0.1002 1.0000 Uani . . . . . . F25 F 0.2488(2) 0.9123(3) 0.4722(2) 0.1020 1.0000 Uani . . . . . . H1 H 0.5110 0.9577 -0.0871 0.0801 1.0000 Uiso R . . . . . H2 H 0.5880 1.0291 -0.0692 0.0801 0.5000 Uiso R . . . . . H3 H 0.7416 1.1166 -0.0599 0.0813 1.0000 Uiso R . . . . . H4 H 0.7586 1.0417 -0.0339 0.0813 0.5000 Uiso R . . . . . H5 H 0.8750 0.9721 0.0059 0.1182 0.5000 Uiso R . . . . . H6 H 0.7931 0.9014 0.0084 0.1141 1.0000 Uiso R . . . . . H7 H 1.0151 1.0312 0.0605 0.1215 0.5000 Uiso R . . . . . H8 H 1.0027 0.9445 0.0469 0.1215 0.5000 Uiso R . . . . . H9 H 0.4059 0.8335 0.5682 0.1270 1.0000 Uiso R . . . . . H10 H 0.3593 0.8872 0.5490 0.1270 1.0000 Uiso R . . . . . H12 H 0.5194 1.0226 -0.0307 0.0801 0.5000 Uiso R . . . . . H14 H 0.6692 1.0310 -0.0599 0.0813 0.5000 Uiso R . . . . . H15 H 0.7995 0.9912 -0.0188 0.1182 0.5000 Uiso R . . . . . H20 H 0.5350 0.6652 0.3491 0.0473 1.0000 Uiso R . . . . . H21 H 0.4474 0.5152 0.3211 0.0617 1.0000 Uiso R . . . . . H31 H 0.3902 0.4513 0.1886 0.0592 1.0000 Uiso R . . . . . H41 H 0.4181 0.5412 0.0898 0.0544 1.0000 Uiso R . . . . . H71 H 0.4585 0.6448 0.0003 0.0403 1.0000 Uiso R . . . . . H91 H 0.5989 0.9035 -0.0062 0.0388 1.0000 Uiso R . . . . . H131 H 0.7574 1.1634 0.1723 0.0489 1.0000 Uiso R . . . . . H141 H 0.7678 1.1472 0.3060 0.0479 1.0000 Uiso R . . . . . H151 H 0.7056 1.0077 0.3414 0.0414 1.0000 Uiso R . . . . . H161 H 0.4178 0.8299 0.1649 0.0450 1.0000 Uiso R . . . . . H171 H 0.2886 0.8479 0.1976 0.0521 1.0000 Uiso R . . . . . H181 H 0.2821 0.8770 0.3308 0.0511 1.0000 Uiso R . . . . . H191 H 0.4087 0.8847 0.4274 0.0460 1.0000 Uiso R . . . . . H221 H 0.5433 0.8896 0.5143 0.0430 1.0000 Uiso R . . . . . H241 H 0.7853 0.8512 0.5147 0.0408 1.0000 Uiso R . . . . . H271 H 0.8762 0.8242 0.4279 0.0421 1.0000 Uiso R . . . . . H281 H 0.9493 0.7844 0.3312 0.0444 1.0000 Uiso R . . . . . H291 H 0.8746 0.7563 0.1988 0.0421 1.0000 Uiso R . . . . . H301 H 0.7298 0.7661 0.1667 0.0435 1.0000 Uiso R . . . . . H321 H 0.4770 0.6294 -0.1249 0.0454 1.0000 Uiso R . . . . . H331 H 0.4293 0.6156 -0.2626 0.0572 1.0000 Uiso R . . . . . H341 H 0.4192 0.7379 -0.3196 0.0561 1.0000 Uiso R . . . . . H351 H 0.4524 0.8710 -0.2386 0.0593 1.0000 Uiso R . . . . . H371 H 0.5806 0.9141 0.6386 0.0503 1.0000 Uiso R . . . . . H381 H 0.6295 0.9429 0.7755 0.0561 1.0000 Uiso R . . . . . H391 H 0.7725 0.9357 0.8310 0.0543 1.0000 Uiso R . . . . . H401 H 0.8591 0.8991 0.7492 0.0529 1.0000 Uiso R . . . . . H511 H 0.9720 0.8184 0.6026 0.0558 1.0000 Uiso R . . . . . H521 H 1.0388 0.9720 0.6239 0.0654 1.0000 Uiso R . . . . . H531 H 1.0954 1.0443 0.7507 0.0646 1.0000 Uiso R . . . . . H541 H 1.0851 0.9617 0.8567 0.0531 1.0000 Uiso R . . . . . H571 H 1.0582 0.8687 0.9532 0.0512 1.0000 Uiso R . . . . . H591 H 0.9453 0.6119 0.9789 0.0505 1.0000 Uiso R . . . . . H621 H 0.8549 0.4715 0.9038 0.0579 1.0000 Uiso R . . . . . H631 H 0.7747 0.3418 0.8192 0.0663 1.0000 Uiso R . . . . . H641 H 0.7646 0.3421 0.6837 0.0643 1.0000 Uiso R . . . . . H651 H 0.8306 0.4735 0.6362 0.0528 1.0000 Uiso R . . . . . H661 H 1.1167 0.6727 0.7953 0.0433 1.0000 Uiso R . . . . . H671 H 1.2479 0.6582 0.7605 0.0553 1.0000 Uiso R . . . . . H681 H 1.2501 0.6300 0.6276 0.0566 1.0000 Uiso R . . . . . H691 H 1.1205 0.6159 0.5330 0.0560 1.0000 Uiso R . . . . . H721 H 0.9784 0.5986 0.4485 0.0501 1.0000 Uiso R . . . . . H741 H 0.7307 0.6177 0.4554 0.0494 1.0000 Uiso R . . . . . H771 H 0.6420 0.6474 0.5421 0.0537 1.0000 Uiso R . . . . . H781 H 0.5667 0.6786 0.6399 0.0539 1.0000 Uiso R . . . . . H791 H 0.6451 0.7087 0.7722 0.0513 1.0000 Uiso R . . . . . H801 H 0.7944 0.7055 0.8023 0.0448 1.0000 Uiso R . . . . . H821 H 1.0329 0.6568 1.1025 0.0953 1.0000 Uiso R . . . . . H831 H 1.0758 0.7157 1.2391 0.1035 1.0000 Uiso R . . . . . H841 H 1.0953 0.8623 1.2764 0.1071 1.0000 Uiso R . . . . . H851 H 1.0685 0.9468 1.1822 0.0924 1.0000 Uiso R . . . . . H871 H 0.6921 0.5702 0.3351 0.0695 1.0000 Uiso R . . . . . H881 H 0.6603 0.5364 0.1962 0.0875 1.0000 Uiso R . . . . . H891 H 0.7783 0.5290 0.1341 0.0964 1.0000 Uiso R . . . . . H901 H 0.9203 0.5515 0.2080 0.0905 1.0000 Uiso R . . . . . H902 H 0.6811 1.0373 0.0776 0.0449 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0350(3) 0.0338(3) 0.0196(2) 0.00342(16) 0.00482(17) 0.00944(19) Fe2 0.0377(3) 0.0328(2) 0.0212(2) 0.00261(17) 0.00580(17) 0.0084(2) N1 0.0380(15) 0.0340(14) 0.0270(13) 0.0015(11) 0.0078(11) 0.0051(12) N2 0.0335(14) 0.0385(15) 0.0196(11) 0.0044(10) 0.0056(10) 0.0104(12) N3 0.0367(14) 0.0327(14) 0.0236(12) 0.0021(10) 0.0031(10) 0.0107(11) N4 0.0355(14) 0.0374(15) 0.0264(12) 0.0025(11) 0.0031(11) 0.0126(12) N5 0.0368(14) 0.0328(14) 0.0229(12) 0.0039(10) 0.0041(10) 0.0110(11) N6 0.0400(15) 0.0373(14) 0.0216(12) 0.0048(10) 0.0067(11) 0.0130(12) N7 0.0420(16) 0.061(2) 0.0231(13) 0.0074(12) 0.0041(11) 0.0142(15) N8 0.0451(17) 0.0491(18) 0.0279(13) 0.0046(12) 0.0047(12) 0.0134(14) N51 0.0366(14) 0.0329(14) 0.0320(13) 0.0018(11) 0.0057(11) 0.0094(12) N52 0.0332(14) 0.0409(15) 0.0237(12) 0.0031(11) 0.0060(10) 0.0126(12) N53 0.0372(15) 0.0345(14) 0.0290(13) 0.0052(11) 0.0033(11) 0.0076(12) N54 0.0401(15) 0.0296(14) 0.0301(13) 0.0019(10) 0.0117(11) 0.0080(12) N55 0.0454(16) 0.0361(15) 0.0235(12) 0.0019(11) 0.0038(11) 0.0072(13) N56 0.0387(15) 0.0328(14) 0.0261(13) 0.0064(10) 0.0011(11) 0.0057(12) N57 0.051(2) 0.089(3) 0.048(2) -0.0272(19) 0.0151(16) 0.000(2) N58 0.119(3) 0.046(2) 0.0327(16) 0.0054(14) 0.0192(19) 0.022(2) C1 0.056(2) 0.0415(19) 0.0258(15) 0.0045(13) 0.0091(14) 0.0108(16) C2 0.075(3) 0.045(2) 0.0372(19) 0.0102(16) 0.0157(19) 0.005(2) C3 0.073(3) 0.0356(19) 0.042(2) 0.0024(15) 0.0102(19) -0.0029(19) C4 0.060(2) 0.0388(19) 0.0358(18) 0.0021(15) 0.0091(16) 0.0035(17) C5 0.0416(18) 0.0374(17) 0.0251(14) 0.0036(12) 0.0062(13) 0.0101(14) C6 0.0358(16) 0.0342(16) 0.0247(14) 0.0023(12) 0.0057(12) 0.0100(13) C7 0.0345(16) 0.0366(17) 0.0250(14) -0.0004(12) 0.0020(12) 0.0079(13) C8 0.0324(16) 0.0472(19) 0.0237(14) 0.0015(13) 0.0041(12) 0.0121(14) C9 0.0339(16) 0.0447(18) 0.0216(13) 0.0050(12) 0.0051(12) 0.0131(14) C10 0.0305(15) 0.0376(17) 0.0242(14) 0.0044(12) 0.0047(11) 0.0126(13) C11 0.0349(16) 0.0382(17) 0.0238(13) 0.0075(12) 0.0069(12) 0.0120(14) C12 0.0421(18) 0.0415(18) 0.0270(15) 0.0065(13) 0.0054(13) 0.0124(15) C13 0.050(2) 0.0337(17) 0.0390(18) 0.0069(14) 0.0091(15) 0.0073(15) C14 0.0449(19) 0.0348(18) 0.0358(17) -0.0004(13) 0.0032(14) 0.0071(15) C15 0.0426(18) 0.0360(17) 0.0244(14) 0.0026(12) 0.0043(13) 0.0091(14) C16 0.0405(18) 0.0428(19) 0.0287(15) 0.0042(13) 0.0044(13) 0.0124(15) C17 0.0377(18) 0.056(2) 0.0352(17) 0.0090(15) 0.0017(14) 0.0165(16) C18 0.0392(18) 0.052(2) 0.0390(18) 0.0077(15) 0.0120(15) 0.0201(16) C19 0.0465(19) 0.0436(19) 0.0291(15) 0.0037(13) 0.0093(14) 0.0133(16) C20 0.0341(16) 0.0394(17) 0.0229(13) 0.0050(12) 0.0053(12) 0.0102(14) C21 0.0394(17) 0.0337(16) 0.0244(14) 0.0039(12) 0.0052(12) 0.0113(14) C22 0.0438(18) 0.0392(18) 0.0274(15) 0.0017(13) 0.0105(13) 0.0133(15) C23 0.0426(18) 0.0330(16) 0.0229(14) 0.0029(12) 0.0046(13) 0.0087(14) C24 0.0376(17) 0.0411(18) 0.0242(14) 0.0035(12) 0.0049(12) 0.0121(14) C25 0.0380(17) 0.0333(16) 0.0251(14) 0.0045(12) 0.0083(12) 0.0100(13) C26 0.0392(17) 0.0318(16) 0.0206(13) 0.0030(11) 0.0063(12) 0.0082(13) C27 0.0394(17) 0.0408(18) 0.0252(14) 0.0060(12) 0.0049(12) 0.0136(14) C28 0.0346(17) 0.0401(18) 0.0383(17) 0.0049(14) 0.0080(14) 0.0126(14) C29 0.0401(18) 0.0384(17) 0.0306(15) 0.0013(13) 0.0138(13) 0.0116(14) C30 0.0456(19) 0.0353(17) 0.0249(14) 0.0017(12) 0.0074(13) 0.0091(14) C31 0.0334(16) 0.0480(19) 0.0264(15) 0.0035(13) 0.0068(12) 0.0099(15) C32 0.0348(17) 0.049(2) 0.0310(16) -0.0007(14) 0.0038(13) 0.0091(15) C33 0.041(2) 0.070(3) 0.0307(17) -0.0073(17) 0.0081(15) 0.0060(18) C34 0.0409(19) 0.080(3) 0.0222(15) 0.0036(17) -0.0009(14) 0.0099(19) C35 0.048(2) 0.077(3) 0.0276(16) 0.0106(17) 0.0014(15) 0.015(2) C36 0.0439(18) 0.0373(17) 0.0203(13) 0.0019(12) 0.0061(12) 0.0091(14) C37 0.047(2) 0.049(2) 0.0325(17) 0.0041(14) 0.0126(15) 0.0141(17) C38 0.057(2) 0.050(2) 0.0360(18) 0.0030(16) 0.0214(17) 0.0121(18) C39 0.062(2) 0.049(2) 0.0220(15) 0.0021(14) 0.0022(15) 0.0059(18) C40 0.046(2) 0.050(2) 0.0321(17) 0.0030(15) 0.0009(15) 0.0106(17) C51 0.055(2) 0.0420(19) 0.0372(17) 0.0060(15) 0.0147(16) 0.0131(17) C52 0.066(3) 0.042(2) 0.057(2) 0.0136(18) 0.024(2) 0.0183(19) C53 0.058(2) 0.038(2) 0.060(2) 0.0034(18) 0.013(2) 0.0072(18) C54 0.045(2) 0.0400(19) 0.050(2) -0.0079(16) 0.0057(16) 0.0111(16) C55 0.0323(16) 0.0444(19) 0.0341(16) -0.0013(14) 0.0100(13) 0.0069(14) C56 0.0340(17) 0.0422(18) 0.0305(15) -0.0022(13) 0.0021(13) 0.0101(14) C57 0.0352(17) 0.051(2) 0.0364(17) -0.0082(15) 0.0059(14) 0.0160(16) C58 0.0331(17) 0.063(2) 0.0282(16) -0.0042(15) 0.0032(13) 0.0204(16) C59 0.0421(19) 0.059(2) 0.0276(15) 0.0089(15) 0.0097(14) 0.0198(17) C60 0.0391(17) 0.0468(19) 0.0250(14) 0.0047(13) 0.0058(13) 0.0170(15) C61 0.0411(18) 0.0422(19) 0.0317(16) 0.0106(14) 0.0061(13) 0.0150(15) C62 0.055(2) 0.049(2) 0.0375(18) 0.0158(16) 0.0075(16) 0.0125(18) C63 0.066(3) 0.044(2) 0.057(2) 0.0240(19) 0.003(2) 0.004(2) C64 0.074(3) 0.0313(19) 0.051(2) 0.0048(16) -0.007(2) 0.0004(19) C65 0.061(2) 0.0393(19) 0.0350(17) 0.0044(14) -0.0020(16) 0.0115(17) C66 0.0401(18) 0.0377(18) 0.0310(16) 0.0029(13) 0.0072(13) 0.0101(15) C67 0.043(2) 0.044(2) 0.0451(19) 0.0044(16) 0.0116(16) 0.0108(16) C68 0.050(2) 0.044(2) 0.051(2) 0.0094(16) 0.0164(17) 0.0180(17) C69 0.060(2) 0.043(2) 0.0386(18) 0.0044(15) 0.0178(17) 0.0173(17) C70 0.051(2) 0.0317(16) 0.0290(15) 0.0040(12) 0.0095(14) 0.0082(15) C71 0.052(2) 0.0326(16) 0.0254(14) 0.0038(12) 0.0110(14) 0.0106(15) C72 0.066(2) 0.0363(18) 0.0274(16) 0.0038(13) 0.0127(15) 0.0150(17) C73 0.067(2) 0.0312(17) 0.0248(15) 0.0018(12) 0.0045(15) 0.0067(16) C74 0.051(2) 0.0379(18) 0.0292(16) 0.0057(13) -0.0021(14) 0.0054(16) C75 0.0481(19) 0.0324(17) 0.0293(15) 0.0071(12) 0.0040(14) 0.0099(15) C76 0.0456(19) 0.0325(17) 0.0290(15) 0.0075(12) 0.0036(14) 0.0058(14) C77 0.048(2) 0.046(2) 0.0352(17) 0.0066(15) 0.0020(15) 0.0121(17) C78 0.0378(18) 0.045(2) 0.048(2) 0.0137(16) 0.0030(15) 0.0086(16) C79 0.0419(19) 0.0436(19) 0.0432(18) 0.0123(15) 0.0160(15) 0.0136(16) C80 0.0470(19) 0.0374(18) 0.0294(15) 0.0083(13) 0.0087(14) 0.0121(15) C81 0.0279(17) 0.092(3) 0.0326(18) -0.0047(19) 0.0059(14) 0.0102(19) C82 0.052(2) 0.135(4) 0.0294(18) 0.015(2) 0.0103(17) 0.039(3) C83 0.045(2) 0.179(6) 0.037(2) 0.011(3) 0.0061(19) 0.038(3) C84 0.041(2) 0.174(6) 0.043(3) -0.034(3) 0.0054(19) 0.007(3) C85 0.058(3) 0.124(4) 0.046(3) -0.038(3) 0.014(2) -0.005(3) C86 0.092(3) 0.0318(18) 0.0236(16) 0.0037(13) 0.0040(18) 0.0072(19) C87 0.087(3) 0.049(2) 0.0348(19) 0.0062(17) -0.002(2) 0.007(2) C88 0.123(4) 0.052(3) 0.040(2) 0.008(2) -0.015(3) 0.000(3) C89 0.158(4) 0.047(2) 0.0266(19) 0.0032(17) 0.012(3) 0.007(3) C90 0.141(4) 0.049(2) 0.035(2) 0.0072(18) 0.025(3) 0.029(3) P1 0.0438(6) 0.0676(7) 0.0386(5) -0.0086(5) 0.0003(4) 0.0229(5) P2 0.0496(6) 0.0758(8) 0.0442(5) 0.0253(5) 0.0199(4) 0.0302(6) P3 0.0536(6) 0.0565(6) 0.0273(4) 0.0055(4) 0.0058(4) 0.0053(5) P4 0.0501(6) 0.0533(6) 0.0303(4) 0.0043(4) 0.0063(4) 0.0089(5) F1 0.0658(19) 0.088(2) 0.136(3) 0.032(2) 0.043(2) 0.0200(17) F2 0.0796(18) 0.103(2) 0.0518(14) 0.0243(14) 0.0284(13) 0.0473(17) F3 0.0656(18) 0.085(2) 0.105(2) -0.0398(19) -0.0028(17) 0.0283(16) F4 0.0758(17) 0.0766(18) 0.0417(12) -0.0008(12) 0.0141(12) 0.0395(15) F5 0.0766(19) 0.163(3) 0.0556(16) -0.0360(19) -0.0196(14) 0.072(2) F6 0.0556(14) 0.0880(19) 0.0404(12) 0.0106(12) 0.0017(10) 0.0288(13) F11 0.094(2) 0.205(4) 0.152(3) 0.132(3) 0.069(2) 0.102(3) F12 0.0652(16) 0.091(2) 0.0573(15) 0.0327(14) 0.0143(12) 0.0360(15) F13 0.112(2) 0.232(4) 0.0517(17) 0.042(2) 0.0391(17) 0.112(3) F14 0.082(2) 0.118(3) 0.0695(18) -0.0156(18) 0.0221(16) 0.0455(19) F15 0.0564(19) 0.087(3) 0.280(5) 0.070(3) 0.033(3) 0.0179(18) F16 0.0548(17) 0.083(2) 0.123(3) -0.0185(19) -0.0009(17) 0.0262(16) F21 0.097(2) 0.0756(19) 0.0519(15) -0.0102(14) 0.0104(15) 0.0151(17) F22 0.148(3) 0.073(2) 0.075(2) -0.0197(17) 0.018(2) 0.024(2) F23 0.141(3) 0.089(2) 0.068(2) 0.0330(18) -0.022(2) 0.024(2) F24 0.157(3) 0.089(2) 0.0459(16) 0.0249(16) -0.0062(19) 0.019(2) F26 0.0585(17) 0.131(3) 0.0650(18) 0.0024(19) 0.0047(14) -0.0002(18) F31 0.102(2) 0.0526(16) 0.0783(19) -0.0078(14) 0.0188(17) 0.0085(15) F32 0.204(4) 0.075(2) 0.0564(18) -0.0225(16) 0.019(2) 0.012(2) F33 0.0854(19) 0.0680(17) 0.0480(14) 0.0182(12) 0.0071(13) 0.0243(15) F34 0.093(2) 0.117(3) 0.0603(17) 0.0505(18) 0.0117(16) 0.010(2) F35 0.0704(19) 0.201(4) 0.0598(18) 0.015(2) 0.0285(15) 0.060(2) F36 0.0495(15) 0.162(3) 0.0626(17) 0.032(2) 0.0079(13) 0.0288(19) O1 0.073(2) 0.0592(19) 0.069(2) 0.0044(16) -0.0042(17) 0.0266(17) O2 0.070(2) 0.077(2) 0.0530(18) 0.0062(16) 0.0116(15) 0.0168(17) O3 0.106(3) 0.069(2) 0.122(4) 0.017(2) 0.037(3) 0.029(2) O4 0.135(5) 0.078(5) 0.113(6) 0.010(4) 0.062(5) 0.043(4) O5 0.098(3) 0.151(4) 0.077(3) 0.028(3) 0.027(2) 0.069(3) F25 0.0652(19) 0.115(3) 0.110(3) -0.005(2) 0.0346(19) 0.0072(19) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2388(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 . 1.974(3) yes Fe1 . N2 . 1.877(2) yes Fe1 . N3 . 1.978(3) yes Fe1 . N4 . 1.983(3) yes Fe1 . N5 . 1.877(3) yes Fe1 . N6 . 1.976(3) yes Fe2 . N51 . 1.978(3) yes Fe2 . N52 . 1.874(3) yes Fe2 . N53 . 1.976(3) yes Fe2 . N54 . 1.972(3) yes Fe2 . N55 . 1.878(3) yes Fe2 . N56 . 1.983(3) yes N1 . C1 . 1.335(4) yes N1 . C5 . 1.370(4) yes N2 . C6 . 1.354(4) yes N2 . C10 . 1.351(4) yes N3 . C11 . 1.364(4) yes N3 . C15 . 1.339(4) yes N4 . C16 . 1.346(4) yes N4 . C20 . 1.362(4) yes N5 . C21 . 1.358(4) yes N5 . C25 . 1.349(4) yes N6 . C26 . 1.367(4) yes N6 . C30 . 1.341(4) yes N7 . C31 . 1.349(5) yes N7 . C35 . 1.353(4) yes N8 . C36 . 1.355(5) yes N8 . C40 . 1.334(4) yes N51 . C51 . 1.354(5) yes N51 . C55 . 1.367(4) yes N52 . C56 . 1.360(5) yes N52 . C60 . 1.340(4) yes N53 . C61 . 1.363(4) yes N53 . C65 . 1.350(5) yes N54 . C66 . 1.341(5) yes N54 . C70 . 1.366(4) yes N55 . C71 . 1.347(5) yes N55 . C75 . 1.350(5) yes N56 . C76 . 1.351(4) yes N56 . C80 . 1.337(5) yes N57 . C81 . 1.343(7) yes N57 . C85 . 1.322(6) yes N58 . C86 . 1.357(7) yes N58 . C90 . 1.354(6) yes C1 . C2 . 1.376(6) yes C1 . H20 . 0.943 no C2 . C3 . 1.387(6) yes C2 . H21 . 0.940 no C3 . C4 . 1.394(5) yes C3 . H31 . 0.931 no C4 . C5 . 1.384(5) yes C4 . H41 . 0.934 no C5 . C6 . 1.474(5) yes C6 . C7 . 1.377(4) yes C7 . C8 . 1.399(5) yes C7 . H71 . 0.928 no C8 . C9 . 1.388(5) yes C8 . C31 . 1.493(4) yes C9 . C10 . 1.391(4) yes C9 . H91 . 0.955 no C10 . C11 . 1.460(5) yes C11 . C12 . 1.395(5) yes C12 . C13 . 1.379(5) yes C12 . H902 . 0.941 no C13 . C14 . 1.386(5) yes C13 . H131 . 0.950 no C14 . C15 . 1.389(5) yes C14 . H141 . 0.953 no C15 . H151 . 0.938 no C16 . C17 . 1.380(5) yes C16 . H161 . 0.944 no C17 . C18 . 1.390(5) yes C17 . H171 . 0.934 no C18 . C19 . 1.386(5) yes C18 . H181 . 0.936 no C19 . C20 . 1.388(5) yes C19 . H191 . 0.935 no C20 . C21 . 1.471(5) yes C21 . C22 . 1.389(4) yes C22 . C23 . 1.397(5) yes C22 . H221 . 0.947 no C23 . C24 . 1.402(5) yes C23 . C36 . 1.488(4) yes C24 . C25 . 1.381(4) yes C24 . H241 . 0.954 no C25 . C26 . 1.469(4) yes C26 . C27 . 1.386(5) yes C27 . C28 . 1.393(5) yes C27 . H271 . 0.943 no C28 . C29 . 1.383(5) yes C28 . H281 . 0.939 no C29 . C30 . 1.380(5) yes C29 . H291 . 0.951 no C30 . H301 . 0.940 no C31 . C32 . 1.383(5) yes C32 . C33 . 1.395(5) yes C32 . H321 . 0.930 no C33 . C34 . 1.366(7) yes C33 . H331 . 0.943 no C34 . C35 . 1.383(6) yes C34 . H341 . 0.943 no C35 . H351 . 0.951 no C36 . C37 . 1.375(5) yes C37 . C38 . 1.393(5) yes C37 . H371 . 0.931 no C38 . C39 . 1.373(6) yes C38 . H381 . 0.940 no C39 . C40 . 1.387(6) yes C39 . H391 . 0.940 no C40 . H401 . 0.937 no C51 . C52 . 1.385(6) yes C51 . H511 . 0.947 no C52 . C53 . 1.373(6) yes C52 . H521 . 0.936 no C53 . C54 . 1.384(6) yes C53 . H531 . 0.933 no C54 . C55 . 1.380(5) yes C54 . H541 . 0.924 no C55 . C56 . 1.467(5) yes C56 . C57 . 1.381(5) yes C57 . C58 . 1.403(6) yes C57 . H571 . 0.941 no C58 . C59 . 1.377(6) yes C58 . C81 . 1.492(5) yes C59 . C60 . 1.401(5) yes C59 . H591 . 0.927 no C60 . C61 . 1.462(5) yes C61 . C62 . 1.395(5) yes C62 . C63 . 1.365(6) yes C62 . H621 . 0.943 no C63 . C64 . 1.392(6) yes C63 . H631 . 0.935 no C64 . C65 . 1.377(6) yes C64 . H641 . 0.940 no C65 . H651 . 0.935 no C66 . C67 . 1.387(5) yes C66 . H661 . 0.938 no C67 . C68 . 1.374(6) yes C67 . H671 . 0.948 no C68 . C69 . 1.379(6) yes C68 . H681 . 0.936 no C69 . C70 . 1.391(6) yes C69 . H691 . 0.939 no C70 . C71 . 1.463(5) yes C71 . C72 . 1.394(5) yes C72 . C73 . 1.384(6) yes C72 . H721 . 0.938 no C73 . C74 . 1.406(6) yes C73 . C86 . 1.494(5) yes C74 . C75 . 1.389(5) yes C74 . H741 . 0.922 no C75 . C76 . 1.473(5) yes C76 . C77 . 1.381(6) yes C77 . C78 . 1.379(6) yes C77 . H771 . 0.945 no C78 . C79 . 1.383(5) yes C78 . H781 . 0.951 no C79 . C80 . 1.399(5) yes C79 . H791 . 0.940 no C80 . H801 . 0.949 no C81 . C82 . 1.365(7) yes C82 . C83 . 1.423(7) yes C82 . H821 . 0.954 no C83 . C84 . 1.362(11) yes C83 . H831 . 0.931 no C84 . C85 . 1.356(11) yes C84 . H841 . 0.941 no C85 . H851 . 0.952 no C86 . C87 . 1.366(7) yes C87 . C88 . 1.407(6) yes C87 . H871 . 0.936 no C88 . C89 . 1.370(10) yes C88 . H881 . 0.942 no C89 . C90 . 1.365(10) yes C89 . H891 . 0.929 no C90 . H901 . 0.943 no P1 . F1 . 1.579(3) yes P1 . F2 . 1.597(3) yes P1 . F3 . 1.592(3) yes P1 . F4 . 1.598(3) yes P1 . F5 . 1.583(3) yes P1 . F6 . 1.584(3) yes P2 . F11 . 1.576(3) yes P2 . F12 . 1.580(3) yes P2 . F13 . 1.604(3) yes P2 . F14 . 1.568(3) yes P2 . F15 . 1.543(4) yes P2 . F16 . 1.597(4) yes P3 . F21 . 1.590(3) yes P3 . F22 . 1.567(3) yes P3 . F23 . 1.566(3) yes P3 . F24 . 1.584(3) yes P3 . F26 . 1.588(3) yes P3 . F25 . 1.592(3) yes P4 . F31 . 1.573(3) yes P4 . F32 . 1.581(3) yes P4 . F33 . 1.582(3) yes P4 . F34 . 1.582(3) yes P4 . F35 . 1.582(3) yes P4 . F36 . 1.585(3) yes O1 . H1 . 0.820 no O1 . H2 . 0.820 no O1 . H12 . 0.820 no O2 . H3 . 0.850 no O2 . H4 . 0.830 no O2 . H14 . 0.830 no O3 . H5 . 0.820 no O3 . H6 . 0.850 no O3 . H15 . 0.820 no O4 . O4 2_775 1.167(17) yes O4 . H7 . 0.830 no O4 . H8 . 0.820 no O5 . H9 . 0.820 no O5 . H10 . 0.820 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Fe1 . N2 . 81.17(11) yes N1 . Fe1 . N3 . 162.17(11) yes N2 . Fe1 . N3 . 81.00(11) yes N1 . Fe1 . N4 . 90.20(12) yes N2 . Fe1 . N4 . 98.55(11) yes N3 . Fe1 . N4 . 92.11(12) yes N1 . Fe1 . N5 . 99.49(12) yes N2 . Fe1 . N5 . 179.26(12) yes N3 . Fe1 . N5 . 98.33(11) yes N4 . Fe1 . N5 . 81.13(12) yes N1 . Fe1 . N6 . 92.17(12) yes N2 . Fe1 . N6 . 99.31(11) yes N3 . Fe1 . N6 . 91.04(12) yes N4 . Fe1 . N6 . 162.13(11) yes N5 . Fe1 . N6 . 81.01(11) yes N51 . Fe2 . N52 . 81.28(12) yes N51 . Fe2 . N53 . 161.78(11) yes N52 . Fe2 . N53 . 80.53(12) yes N51 . Fe2 . N54 . 91.28(12) yes N52 . Fe2 . N54 . 99.73(12) yes N53 . Fe2 . N54 . 92.91(12) yes N51 . Fe2 . N55 . 98.13(12) yes N52 . Fe2 . N55 . 179.19(13) yes N53 . Fe2 . N55 . 100.05(12) yes N54 . Fe2 . N55 . 80.82(13) yes N51 . Fe2 . N56 . 91.75(12) yes N52 . Fe2 . N56 . 98.46(12) yes N53 . Fe2 . N56 . 89.79(12) yes N54 . Fe2 . N56 . 161.80(11) yes N55 . Fe2 . N56 . 80.99(13) yes Fe1 . N1 . C1 . 127.3(2) yes Fe1 . N1 . C5 . 114.2(2) yes C1 . N1 . C5 . 118.5(3) yes Fe1 . N2 . C6 . 120.1(2) yes Fe1 . N2 . C10 . 119.6(2) yes C6 . N2 . C10 . 120.3(3) yes Fe1 . N3 . C11 . 114.1(2) yes Fe1 . N3 . C15 . 127.4(2) yes C11 . N3 . C15 . 118.6(3) yes Fe1 . N4 . C16 . 127.1(2) yes Fe1 . N4 . C20 . 114.6(2) yes C16 . N4 . C20 . 118.3(3) yes Fe1 . N5 . C21 . 119.3(2) yes Fe1 . N5 . C25 . 119.8(2) yes C21 . N5 . C25 . 120.9(3) yes Fe1 . N6 . C26 . 114.3(2) yes Fe1 . N6 . C30 . 127.3(2) yes C26 . N6 . C30 . 118.4(3) yes C31 . N7 . C35 . 117.6(4) yes C36 . N8 . C40 . 117.8(3) yes Fe2 . N51 . C51 . 127.4(2) yes Fe2 . N51 . C55 . 114.6(2) yes C51 . N51 . C55 . 118.0(3) yes Fe2 . N52 . C56 . 119.2(2) yes Fe2 . N52 . C60 . 120.4(2) yes C56 . N52 . C60 . 120.4(3) yes Fe2 . N53 . C61 . 114.3(2) yes Fe2 . N53 . C65 . 127.3(2) yes C61 . N53 . C65 . 118.2(3) yes Fe2 . N54 . C66 . 126.8(2) yes Fe2 . N54 . C70 . 114.7(2) yes C66 . N54 . C70 . 118.5(3) yes Fe2 . N55 . C71 . 119.6(2) yes Fe2 . N55 . C75 . 119.3(2) yes C71 . N55 . C75 . 121.1(3) yes Fe2 . N56 . C76 . 114.6(2) yes Fe2 . N56 . C80 . 126.4(2) yes C76 . N56 . C80 . 118.9(3) yes C81 . N57 . C85 . 118.8(6) yes C86 . N58 . C90 . 117.1(5) yes N1 . C1 . C2 . 123.0(3) yes N1 . C1 . H20 . 116.6 no C2 . C1 . H20 . 120.4 no C1 . C2 . C3 . 119.1(4) yes C1 . C2 . H21 . 120.2 no C3 . C2 . H21 . 120.7 no C2 . C3 . C4 . 118.8(4) yes C2 . C3 . H31 . 121.4 no C4 . C3 . H31 . 119.8 no C3 . C4 . C5 . 119.2(3) yes C3 . C4 . H41 . 120.5 no C5 . C4 . H41 . 120.3 no C4 . C5 . N1 . 121.4(3) yes C4 . C5 . C6 . 124.7(3) yes N1 . C5 . C6 . 113.9(3) yes C5 . C6 . N2 . 110.7(3) yes C5 . C6 . C7 . 127.7(3) yes N2 . C6 . C7 . 121.5(3) yes C6 . C7 . C8 . 118.9(3) yes C6 . C7 . H71 . 120.9 no C8 . C7 . H71 . 120.3 no C7 . C8 . C9 . 119.2(3) yes C7 . C8 . C31 . 120.7(3) yes C9 . C8 . C31 . 120.1(3) yes C8 . C9 . C10 . 119.4(3) yes C8 . C9 . H91 . 120.9 no C10 . C9 . H91 . 119.7 no C9 . C10 . N2 . 120.6(3) yes C9 . C10 . C11 . 128.0(3) yes N2 . C10 . C11 . 111.4(3) yes C10 . C11 . N3 . 113.9(3) yes C10 . C11 . C12 . 124.8(3) yes N3 . C11 . C12 . 121.3(3) yes C11 . C12 . C13 . 119.5(3) yes C11 . C12 . H902 . 120.2 no C13 . C12 . H902 . 120.3 no C12 . C13 . C14 . 119.0(3) yes C12 . C13 . H131 . 121.8 no C14 . C13 . H131 . 119.1 no C13 . C14 . C15 . 119.0(3) yes C13 . C14 . H141 . 121.1 no C15 . C14 . H141 . 119.9 no C14 . C15 . N3 . 122.6(3) yes C14 . C15 . H151 . 118.7 no N3 . C15 . H151 . 118.7 no N4 . C16 . C17 . 122.1(3) yes N4 . C16 . H161 . 118.3 no C17 . C16 . H161 . 119.6 no C16 . C17 . C18 . 119.8(3) yes C16 . C17 . H171 . 119.2 no C18 . C17 . H171 . 121.0 no C17 . C18 . C19 . 118.6(3) yes C17 . C18 . H181 . 121.0 no C19 . C18 . H181 . 120.5 no C18 . C19 . C20 . 119.1(3) yes C18 . C19 . H191 . 121.4 no C20 . C19 . H191 . 119.6 no C19 . C20 . N4 . 122.2(3) yes C19 . C20 . C21 . 124.6(3) yes N4 . C20 . C21 . 113.3(3) yes C20 . C21 . N5 . 111.7(3) yes C20 . C21 . C22 . 128.3(3) yes N5 . C21 . C22 . 120.0(3) yes C21 . C22 . C23 . 120.0(3) yes C21 . C22 . H221 . 120.1 no C23 . C22 . H221 . 119.9 no C22 . C23 . C24 . 118.6(3) yes C22 . C23 . C36 . 122.5(3) yes C24 . C23 . C36 . 118.9(3) yes C23 . C24 . C25 . 119.2(3) yes C23 . C24 . H241 . 119.8 no C25 . C24 . H241 . 120.9 no C24 . C25 . N5 . 121.3(3) yes C24 . C25 . C26 . 127.4(3) yes N5 . C25 . C26 . 111.3(3) yes C25 . C26 . N6 . 113.5(3) yes C25 . C26 . C27 . 125.0(3) yes N6 . C26 . C27 . 121.6(3) yes C26 . C27 . C28 . 119.4(3) yes C26 . C27 . H271 . 120.0 no C28 . C27 . H271 . 120.5 no C27 . C28 . C29 . 118.5(3) yes C27 . C28 . H281 . 120.7 no C29 . C28 . H281 . 120.8 no C28 . C29 . C30 . 119.7(3) yes C28 . C29 . H291 . 120.1 no C30 . C29 . H291 . 120.2 no C29 . C30 . N6 . 122.5(3) yes C29 . C30 . H301 . 119.3 no N6 . C30 . H301 . 118.2 no C8 . C31 . N7 . 115.7(3) yes C8 . C31 . C32 . 121.5(3) yes N7 . C31 . C32 . 122.8(3) yes C31 . C32 . C33 . 118.1(4) yes C31 . C32 . H321 . 120.1 no C33 . C32 . H321 . 121.7 no C32 . C33 . C34 . 120.0(4) yes C32 . C33 . H331 . 120.1 no C34 . C33 . H331 . 119.9 no C33 . C34 . C35 . 118.5(3) yes C33 . C34 . H341 . 120.6 no C35 . C34 . H341 . 120.9 no C34 . C35 . N7 . 123.0(4) yes C34 . C35 . H351 . 119.5 no N7 . C35 . H351 . 117.4 no C23 . C36 . N8 . 115.1(3) yes C23 . C36 . C37 . 122.4(3) yes N8 . C36 . C37 . 122.4(3) yes C36 . C37 . C38 . 118.7(4) yes C36 . C37 . H371 . 120.6 no C38 . C37 . H371 . 120.6 no C37 . C38 . C39 . 119.3(4) yes C37 . C38 . H381 . 120.0 no C39 . C38 . H381 . 120.7 no C38 . C39 . C40 . 118.4(3) yes C38 . C39 . H391 . 121.5 no C40 . C39 . H391 . 120.0 no C39 . C40 . N8 . 123.2(4) yes C39 . C40 . H401 . 118.1 no N8 . C40 . H401 . 118.7 no N51 . C51 . C52 . 122.2(4) yes N51 . C51 . H511 . 118.5 no C52 . C51 . H511 . 119.3 no C51 . C52 . C53 . 119.0(4) yes C51 . C52 . H521 . 120.8 no C53 . C52 . H521 . 120.2 no C52 . C53 . C54 . 119.9(4) yes C52 . C53 . H531 . 119.4 no C54 . C53 . H531 . 120.7 no C53 . C54 . C55 . 118.8(4) yes C53 . C54 . H541 . 121.9 no C55 . C54 . H541 . 119.3 no C54 . C55 . N51 . 122.0(3) yes C54 . C55 . C56 . 124.9(3) yes N51 . C55 . C56 . 113.0(3) yes C55 . C56 . N52 . 111.9(3) yes C55 . C56 . C57 . 127.1(3) yes N52 . C56 . C57 . 120.9(3) yes C56 . C57 . C58 . 119.2(4) yes C56 . C57 . H571 . 120.4 no C58 . C57 . H571 . 120.4 no C57 . C58 . C59 . 119.2(3) yes C57 . C58 . C81 . 117.8(4) yes C59 . C58 . C81 . 123.0(4) yes C58 . C59 . C60 . 119.4(4) yes C58 . C59 . H591 . 120.5 no C60 . C59 . H591 . 120.2 no C59 . C60 . N52 . 120.9(3) yes C59 . C60 . C61 . 128.0(3) yes N52 . C60 . C61 . 111.1(3) yes C60 . C61 . N53 . 113.5(3) yes C60 . C61 . C62 . 125.1(3) yes N53 . C61 . C62 . 121.3(3) yes C61 . C62 . C63 . 119.8(4) yes C61 . C62 . H621 . 119.7 no C63 . C62 . H621 . 120.5 no C62 . C63 . C64 . 119.0(4) yes C62 . C63 . H631 . 119.9 no C64 . C63 . H631 . 121.1 no C63 . C64 . C65 . 119.2(4) yes C63 . C64 . H641 . 119.2 no C65 . C64 . H641 . 121.6 no C64 . C65 . N53 . 122.4(4) yes C64 . C65 . H651 . 118.3 no N53 . C65 . H651 . 119.3 no N54 . C66 . C67 . 122.6(3) yes N54 . C66 . H661 . 118.4 no C67 . C66 . H661 . 119.0 no C66 . C67 . C68 . 119.1(4) yes C66 . C67 . H671 . 120.6 no C68 . C67 . H671 . 120.2 no C67 . C68 . C69 . 119.1(4) yes C67 . C68 . H681 . 120.7 no C69 . C68 . H681 . 120.3 no C68 . C69 . C70 . 119.8(3) yes C68 . C69 . H691 . 121.0 no C70 . C69 . H691 . 119.2 no C69 . C70 . N54 . 120.9(3) yes C69 . C70 . C71 . 126.0(3) yes N54 . C70 . C71 . 113.1(3) yes C70 . C71 . N55 . 111.7(3) yes C70 . C71 . C72 . 127.8(4) yes N55 . C71 . C72 . 120.5(4) yes C71 . C72 . C73 . 119.8(4) yes C71 . C72 . H721 . 119.9 no C73 . C72 . H721 . 120.3 no C72 . C73 . C74 . 118.7(3) yes C72 . C73 . C86 . 120.2(4) yes C74 . C73 . C86 . 121.1(4) yes C73 . C74 . C75 . 119.4(4) yes C73 . C74 . H741 . 121.4 no C75 . C74 . H741 . 119.3 no C74 . C75 . N55 . 120.5(4) yes C74 . C75 . C76 . 127.7(4) yes N55 . C75 . C76 . 111.8(3) yes C75 . C76 . N56 . 113.3(3) yes C75 . C76 . C77 . 124.6(3) yes N56 . C76 . C77 . 122.1(3) yes C76 . C77 . C78 . 119.3(3) yes C76 . C77 . H771 . 120.1 no C78 . C77 . H771 . 120.6 no C77 . C78 . C79 . 119.0(4) yes C77 . C78 . H781 . 120.5 no C79 . C78 . H781 . 120.5 no C78 . C79 . C80 . 119.1(4) yes C78 . C79 . H791 . 121.4 no C80 . C79 . H791 . 119.5 no C79 . C80 . N56 . 121.6(3) yes C79 . C80 . H801 . 120.4 no N56 . C80 . H801 . 118.0 no C58 . C81 . N57 . 115.6(4) yes C58 . C81 . C82 . 122.0(5) yes N57 . C81 . C82 . 122.4(4) yes C81 . C82 . C83 . 117.4(6) yes C81 . C82 . H821 . 120.3 no C83 . C82 . H821 . 122.3 no C82 . C83 . C84 . 119.1(6) yes C82 . C83 . H831 . 119.5 no C84 . C83 . H831 . 121.4 no C83 . C84 . C85 . 119.0(5) yes C83 . C84 . H841 . 119.9 no C85 . C84 . H841 . 121.2 no C84 . C85 . N57 . 123.3(7) yes C84 . C85 . H851 . 117.4 no N57 . C85 . H851 . 119.2 no C73 . C86 . N58 . 115.5(4) yes C73 . C86 . C87 . 121.6(4) yes N58 . C86 . C87 . 122.9(4) yes C86 . C87 . C88 . 118.4(6) yes C86 . C87 . H871 . 120.4 no C88 . C87 . H871 . 121.2 no C87 . C88 . C89 . 119.3(6) yes C87 . C88 . H881 . 120.2 no C89 . C88 . H881 . 120.4 no C88 . C89 . C90 . 118.8(4) yes C88 . C89 . H891 . 121.1 no C90 . C89 . H891 . 120.1 no C89 . C90 . N58 . 123.5(6) yes C89 . C90 . H901 . 118.9 no N58 . C90 . H901 . 117.6 no F1 . P1 . F2 . 178.5(2) yes F1 . P1 . F3 . 92.5(2) yes F2 . P1 . F3 . 89.06(19) yes F1 . P1 . F4 . 89.37(19) yes F2 . P1 . F4 . 89.12(16) yes F3 . P1 . F4 . 177.9(2) yes F1 . P1 . F5 . 89.7(2) yes F2 . P1 . F5 . 90.6(2) yes F3 . P1 . F5 . 89.61(18) yes F4 . P1 . F5 . 89.39(16) yes F1 . P1 . F6 . 90.20(19) yes F2 . P1 . F6 . 89.51(16) yes F3 . P1 . F6 . 90.58(17) yes F4 . P1 . F6 . 90.42(15) yes F5 . P1 . F6 . 179.77(16) yes F11 . P2 . F12 . 177.3(3) yes F11 . P2 . F13 . 90.5(2) yes F12 . P2 . F13 . 87.23(18) yes F11 . P2 . F14 . 90.1(2) yes F12 . P2 . F14 . 92.06(18) yes F13 . P2 . F14 . 176.1(3) yes F11 . P2 . F15 . 91.6(3) yes F12 . P2 . F15 . 89.8(2) yes F13 . P2 . F15 . 89.4(3) yes F14 . P2 . F15 . 94.5(3) yes F11 . P2 . F16 . 88.6(2) yes F12 . P2 . F16 . 89.89(19) yes F13 . P2 . F16 . 87.9(2) yes F14 . P2 . F16 . 88.3(2) yes F15 . P2 . F16 . 177.3(3) yes F21 . P3 . F22 . 178.8(2) yes F21 . P3 . F23 . 88.4(2) yes F22 . P3 . F23 . 92.6(2) yes F21 . P3 . F24 . 90.0(2) yes F22 . P3 . F24 . 89.0(2) yes F23 . P3 . F24 . 178.2(2) yes F21 . P3 . F26 . 90.4(2) yes F22 . P3 . F26 . 88.9(2) yes F23 . P3 . F26 . 89.3(2) yes F24 . P3 . F26 . 89.9(2) yes F21 . P3 . F25 . 87.6(2) yes F22 . P3 . F25 . 93.0(2) yes F23 . P3 . F25 . 92.5(2) yes F24 . P3 . F25 . 88.3(2) yes F26 . P3 . F25 . 177.3(2) yes F31 . P4 . F32 . 179.2(2) yes F31 . P4 . F33 . 89.15(17) yes F32 . P4 . F33 . 90.36(19) yes F31 . P4 . F34 . 93.4(2) yes F32 . P4 . F34 . 87.1(2) yes F33 . P4 . F34 . 177.4(2) yes F31 . P4 . F35 . 88.5(2) yes F32 . P4 . F35 . 92.1(3) yes F33 . P4 . F35 . 90.27(19) yes F34 . P4 . F35 . 89.3(2) yes F31 . P4 . F36 . 90.1(2) yes F32 . P4 . F36 . 89.2(3) yes F33 . P4 . F36 . 88.81(18) yes F34 . P4 . F36 . 91.7(2) yes F35 . P4 . F36 . 178.41(19) yes H1 . O1 . H2 . 109.5 no H1 . O1 . H12 . 109.5 no H2 . O1 . H12 . 109.5 no H3 . O2 . H4 . 114.6 no H3 . O2 . H14 . 122.5 no H4 . O2 . H14 . 109.5 no H5 . O3 . H6 . 116.5 no H5 . O3 . H15 . 109.5 no H6 . O3 . H15 . 133.8 no O4 2_775 O4 . H7 . 98.8 no O4 2_775 O4 . H8 . 127.2 no H7 . O4 . H8 . 109.5 no H9 . O5 . H10 . 109.5 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 O1 . H1 . N7 . 165 0.82 2.06 2.863(2) yes O1 . H2 . O2 . 175 0.82 1.99 2.811(2) yes O2 . H4 . O3 . 157 0.83 2.02 2.803(2) yes O3 . H5 . O4 . 166 0.82 1.73 2.534(2) yes O3 . H5 . O4 2_775 156 0.82 2.20 2.966(2) yes O4 . H8 . N57 1_554 177 0.82 1.86 2.676(2) yes O4 2_775 H8 . N57 1_554 147 1.79 1.86 3.494(2) yes O1 . H12 . O1 2_675 154 0.82 2.13 2.893(2) yes O2 . H14 . O1 . 153 0.83 2.05 2.811(2) yes O3 . H15 . O2 . 166 0.82 2.00 2.803(2) yes # Attachment 'Fe_3pytpy_2.cif' data_jb1010_173k _database_code_depnum_ccdc_archive 'CCDC 662662' _audit_creation_date 07-05-31 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '5311019 jb1010_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 9.3867(2) _cell_length_b 10.4130(2) _cell_length_c 21.3789(3) _cell_angle_alpha 93.6804(10) _cell_angle_beta 100.2623(10) _cell_angle_gamma 110.4597(8) _cell_volume 1908.30(6) _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 2 # Given Formula = C40 H28 F12 Fe1 N8 P2 # Dc = 1.68 Fooo = 976.00 Mu = 5.83 M = 966.49 # Found Formula = C40 H28 F12 Fe1 N8 P2 # Dc = 1.68 FOOO = 976.00 Mu = 5.83 M = 966.49 _chemical_formula_sum 'C40 H28 F12 Fe1 N8 P2' _chemical_formula_moiety 'C40 H28 Fe N8, 2(F6 P)' _chemical_compound_source ? _chemical_formula_weight 966.49 _cell_measurement_reflns_used 9107 _cell_measurement_theta_min 1 _cell_measurement_theta_max 28 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.29 _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 0.583 # Sheldrick geometric approximatio 0.94 0.99 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.99 # 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 18035 _reflns_number_total 9126 _diffrn_reflns_av_R_equivalents 0.026 # Number of reflections with Friedels Law is 9126 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9131 _diffrn_reflns_theta_min 1.955 _diffrn_reflns_theta_max 27.907 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.907 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min -13 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _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 -0.62 _refine_diff_density_max 0.86 _refine_ls_number_reflns 5829 _refine_ls_number_restraints 0 _refine_ls_number_parameters 571 #_refine_ls_R_factor_ref 0.0375 _refine_ls_wR_factor_ref 0.0434 _refine_ls_goodness_of_fit_ref 1.1183 #_reflns_number_all 9037 _refine_ls_R_factor_all 0.0648 _refine_ls_wR_factor_all 0.0678 # 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 5829 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_gt 0.0434 _refine_ls_shift/su_max 0.000421 _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: 0.417 0.235 0.196 ; 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 0.73318(4) 0.44480(3) 0.239152(14) 0.0221 1.0000 Uani . . . . . . N1 N 0.8861(2) 0.3552(2) 0.23357(9) 0.0236 1.0000 Uani . . . . . . N2 N 0.6528(2) 0.3522(2) 0.15448(9) 0.0230 1.0000 Uani . . . . . . N3 N 0.5552(2) 0.5051(2) 0.21608(9) 0.0252 1.0000 Uani . . . . . . N4 N 0.8788(2) 0.6168(2) 0.21861(9) 0.0234 1.0000 Uani . . . . . . N5 N 0.8105(2) 0.5453(2) 0.32194(9) 0.0232 1.0000 Uani . . . . . . N6 N 0.6178(2) 0.3042(2) 0.28766(9) 0.0248 1.0000 Uani . . . . . . N35 N 0.5279(3) 0.0557(2) -0.13628(10) 0.0356 1.0000 Uani . . . . . . N39 N 0.9100(3) 0.8577(3) 0.60551(11) 0.0454 1.0000 Uani . . . . . . C1 C 1.0099(3) 0.3654(3) 0.27864(11) 0.0287 1.0000 Uani . . . . . . C2 C 1.1155(3) 0.3057(3) 0.26817(12) 0.0320 1.0000 Uani . . . . . . C3 C 1.0942(3) 0.2329(3) 0.20908(13) 0.0336 1.0000 Uani . . . . . . C4 C 0.9655(3) 0.2193(3) 0.16155(12) 0.0298 1.0000 Uani . . . . . . C5 C 0.8640(3) 0.2814(2) 0.17475(10) 0.0237 1.0000 Uani . . . . . . C6 C 0.7277(3) 0.2805(2) 0.12839(10) 0.0238 1.0000 Uani . . . . . . C7 C 0.6791(3) 0.2231(2) 0.06422(10) 0.0249 1.0000 Uani . . . . . . C8 C 0.5497(3) 0.2377(2) 0.02593(10) 0.0242 1.0000 Uani . . . . . . C9 C 0.4740(3) 0.3113(3) 0.05471(11) 0.0282 1.0000 Uani . . . . . . C10 C 0.5285(3) 0.3682(2) 0.11870(10) 0.0253 1.0000 Uani . . . . . . C11 C 0.4702(3) 0.4573(3) 0.15504(11) 0.0270 1.0000 Uani . . . . . . C12 C 0.3442(3) 0.4919(3) 0.13058(11) 0.0344 1.0000 Uani . . . . . . C13 C 0.3038(3) 0.5799(3) 0.16926(12) 0.0359 1.0000 Uani . . . . . . C14 C 0.3890(3) 0.6281(3) 0.23098(12) 0.0337 1.0000 Uani . . . . . . C15 C 0.5131(3) 0.5890(3) 0.25285(11) 0.0294 1.0000 Uani . . . . . . C16 C 0.9097(3) 0.6422(3) 0.16043(11) 0.0268 1.0000 Uani . . . . . . C17 C 1.0158(3) 0.7662(3) 0.15088(12) 0.0305 1.0000 Uani . . . . . . C18 C 1.0938(3) 0.8692(3) 0.20273(12) 0.0321 1.0000 Uani . . . . . . C19 C 1.0632(3) 0.8443(3) 0.26318(12) 0.0303 1.0000 Uani . . . . . . C20 C 0.9569(3) 0.7178(2) 0.26971(11) 0.0253 1.0000 Uani . . . . . . C21 C 0.9148(3) 0.6753(2) 0.33059(11) 0.0248 1.0000 Uani . . . . . . C22 C 0.9695(3) 0.7548(2) 0.39053(11) 0.0267 1.0000 Uani . . . . . . C23 C 0.9104(3) 0.6995(3) 0.44272(11) 0.0273 1.0000 Uani . . . . . . C24 C 0.7996(3) 0.5655(3) 0.43268(11) 0.0292 1.0000 Uani . . . . . . C25 C 0.7528(3) 0.4898(2) 0.37164(10) 0.0251 1.0000 Uani . . . . . . C26 C 0.6418(3) 0.3475(3) 0.35149(11) 0.0264 1.0000 Uani . . . . . . C27 C 0.5694(3) 0.2612(3) 0.39233(12) 0.0368 1.0000 Uani . . . . . . C28 C 0.4750(3) 0.1251(3) 0.36864(13) 0.0407 1.0000 Uani . . . . . . C29 C 0.4549(3) 0.0801(3) 0.30435(13) 0.0361 1.0000 Uani . . . . . . C30 C 0.5249(3) 0.1722(3) 0.26500(11) 0.0291 1.0000 Uani . . . . . . C31 C 0.4971(3) 0.1817(2) -0.04371(11) 0.0250 1.0000 Uani . . . . . . C32 C 0.3709(3) 0.1999(3) -0.08211(12) 0.0360 1.0000 Uani . . . . . . C33 C 0.3268(3) 0.1473(3) -0.14633(12) 0.0413 1.0000 Uani . . . . . . C34 C 0.4081(3) 0.0769(3) -0.17099(12) 0.0354 1.0000 Uani . . . . . . C36 C 0.5701(3) 0.1080(3) -0.07403(11) 0.0314 1.0000 Uani . . . . . . C37 C 0.9671(3) 0.7837(3) 0.50708(11) 0.0288 1.0000 Uani . . . . . . C38 C 0.8654(3) 0.7842(3) 0.54707(12) 0.0386 1.0000 Uani . . . . . . C40 C 1.0609(4) 0.9329(3) 0.62565(13) 0.0408 1.0000 Uani . . . . . . C41 C 1.1696(4) 0.9423(3) 0.58953(14) 0.0426 1.0000 Uani . . . . . . C42 C 1.1225(3) 0.8666(3) 0.52879(13) 0.0385 1.0000 Uani . . . . . . P1 P 0.38986(8) 0.69858(8) 0.41503(3) 0.0358 1.0000 Uani . . . . . . P2 P 1.0000 0.5000 0.0000 0.0244 1.0000 Uani S . . . . . P3 P 0.0000 0.0000 0.0000 0.0285 1.0000 Uani S . . . . . F1 F 0.3370(3) 0.5581(2) 0.36899(10) 0.0711 1.0000 Uani . . . . . . F2 F 0.4491(4) 0.8377(2) 0.46319(12) 0.0957 1.0000 Uani . . . . . . F3 F 0.4807(3) 0.6362(3) 0.46780(10) 0.0712 1.0000 Uani . . . . . . F4 F 0.2977(4) 0.7567(4) 0.36263(12) 0.0975 1.0000 Uani . . . . . . F5 F 0.2428(2) 0.6388(3) 0.44653(10) 0.0641 1.0000 Uani . . . . . . F6 F 0.5376(2) 0.7582(2) 0.38421(10) 0.0698 1.0000 Uani . . . . . . F7 F 0.85945(16) 0.54375(16) 0.01470(7) 0.0326 1.0000 Uani . . . . . . F8 F 0.87659(17) 0.35589(15) -0.03830(7) 0.0338 1.0000 Uani . . . . . . F9 F 0.99440(17) 0.56753(16) -0.06512(7) 0.0326 1.0000 Uani . . . . . . F10 F -0.1514(2) 0.0177(2) 0.01724(9) 0.0504 1.0000 Uani . . . . . . F11 F 0.0767(2) 0.02004(19) 0.07470(8) 0.0476 1.0000 Uani . . . . . . F12 F 0.0760(2) 0.16276(17) 0.00042(9) 0.0471 1.0000 Uani . . . . . . H11 H 1.0223 0.4168 0.3191 0.0330 1.0000 Uiso R . . . . . H21 H 1.2020 0.3152 0.3014 0.0394 1.0000 Uiso R . . . . . H31 H 1.1666 0.1914 0.2007 0.0416 1.0000 Uiso R . . . . . H41 H 0.9465 0.1690 0.1201 0.0367 1.0000 Uiso R . . . . . H71 H 0.7328 0.1731 0.0469 0.0290 1.0000 Uiso R . . . . . H91 H 0.3853 0.3226 0.0310 0.0333 1.0000 Uiso R . . . . . H121 H 0.2868 0.4557 0.0876 0.0431 1.0000 Uiso R . . . . . H131 H 0.2172 0.6056 0.1530 0.0452 1.0000 Uiso R . . . . . H141 H 0.3620 0.6874 0.2588 0.0432 1.0000 Uiso R . . . . . H151 H 0.5722 0.6207 0.2959 0.0366 1.0000 Uiso R . . . . . H161 H 0.8542 0.5687 0.1253 0.0350 1.0000 Uiso R . . . . . H171 H 1.0349 0.7790 0.1086 0.0389 1.0000 Uiso R . . . . . H181 H 1.1677 0.9560 0.1976 0.0394 1.0000 Uiso R . . . . . H191 H 1.1142 0.9147 0.2997 0.0366 1.0000 Uiso R . . . . . H221 H 1.0455 0.8467 0.3964 0.0323 1.0000 Uiso R . . . . . H241 H 0.7563 0.5258 0.4669 0.0340 1.0000 Uiso R . . . . . H271 H 0.5864 0.2960 0.4366 0.0422 1.0000 Uiso R . . . . . H281 H 0.4274 0.0636 0.3962 0.0456 1.0000 Uiso R . . . . . H291 H 0.3930 -0.0134 0.2864 0.0426 1.0000 Uiso R . . . . . H301 H 0.5096 0.1435 0.2200 0.0343 1.0000 Uiso R . . . . . H321 H 0.3154 0.2477 -0.0638 0.0444 1.0000 Uiso R . . . . . H331 H 0.2408 0.1590 -0.1733 0.0490 1.0000 Uiso R . . . . . H341 H 0.3790 0.0400 -0.2152 0.0412 1.0000 Uiso R . . . . . H361 H 0.6556 0.0924 -0.0487 0.0367 1.0000 Uiso R . . . . . H381 H 0.7582 0.7301 0.5321 0.0452 1.0000 Uiso R . . . . . H401 H 1.0907 0.9829 0.6677 0.0472 1.0000 Uiso R . . . . . H411 H 1.2748 1.0000 0.6055 0.0487 1.0000 Uiso R . . . . . H421 H 1.1953 0.8708 0.5024 0.0439 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02344(16) 0.02684(17) 0.01589(15) 0.00069(11) 0.00362(12) 0.00977(13) N1 0.0249(9) 0.0252(10) 0.0199(9) 0.0027(7) 0.0048(7) 0.0080(8) N2 0.0238(9) 0.0269(10) 0.0188(8) 0.0016(7) 0.0049(7) 0.0098(8) N3 0.0253(9) 0.0329(10) 0.0184(9) 0.0025(7) 0.0052(7) 0.0117(8) N4 0.0252(9) 0.0287(10) 0.0192(8) 0.0029(7) 0.0056(7) 0.0132(8) N5 0.0229(9) 0.0263(10) 0.0192(9) 0.0011(7) 0.0036(7) 0.0084(8) N6 0.0245(9) 0.0282(10) 0.0204(9) 0.0007(7) 0.0040(7) 0.0090(8) N35 0.0431(13) 0.0422(12) 0.0222(10) -0.0042(9) 0.0025(9) 0.0203(11) N39 0.0519(15) 0.0587(16) 0.0229(10) -0.0072(10) 0.0066(10) 0.0198(13) C1 0.0286(12) 0.0319(12) 0.0235(11) 0.0021(9) 0.0032(9) 0.0100(10) C2 0.0297(12) 0.0352(13) 0.0304(12) 0.0053(10) -0.0003(10) 0.0141(11) C3 0.0328(13) 0.0367(14) 0.0362(13) 0.0055(11) 0.0056(10) 0.0193(11) C4 0.0333(13) 0.0299(12) 0.0268(11) 0.0015(9) 0.0057(10) 0.0131(10) C5 0.0252(11) 0.0237(11) 0.0214(10) 0.0028(8) 0.0064(8) 0.0073(9) C6 0.0255(11) 0.0243(11) 0.0207(10) 0.0027(8) 0.0069(8) 0.0073(9) C7 0.0272(11) 0.0253(11) 0.0213(10) -0.0008(8) 0.0060(9) 0.0091(9) C8 0.0255(11) 0.0257(11) 0.0193(10) 0.0007(8) 0.0061(8) 0.0066(9) C9 0.0244(11) 0.0396(14) 0.0197(10) 0.0003(9) 0.0013(9) 0.0131(10) C10 0.0240(11) 0.0329(12) 0.0187(10) -0.0001(9) 0.0034(8) 0.0114(9) C11 0.0266(11) 0.0326(12) 0.0209(10) 0.0001(9) 0.0041(9) 0.0107(10) C12 0.0332(13) 0.0515(16) 0.0210(11) -0.0027(10) 0.0004(10) 0.0226(12) C13 0.0343(13) 0.0503(16) 0.0290(12) 0.0029(11) 0.0038(10) 0.0247(12) C14 0.0382(14) 0.0438(15) 0.0258(11) -0.0007(10) 0.0089(10) 0.0231(12) C15 0.0332(13) 0.0381(13) 0.0201(10) 0.0005(9) 0.0068(9) 0.0170(11) C16 0.0327(12) 0.0324(12) 0.0208(10) 0.0037(9) 0.0068(9) 0.0182(10) C17 0.0365(13) 0.0360(13) 0.0263(11) 0.0102(10) 0.0131(10) 0.0184(11) C18 0.0346(13) 0.0322(13) 0.0299(12) 0.0070(10) 0.0086(10) 0.0115(11) C19 0.0311(12) 0.0319(13) 0.0264(11) 0.0037(10) 0.0051(10) 0.0102(10) C20 0.0269(11) 0.0304(12) 0.0205(10) 0.0039(9) 0.0054(9) 0.0127(10) C21 0.0258(11) 0.0285(12) 0.0212(10) 0.0027(9) 0.0056(9) 0.0112(9) C22 0.0282(11) 0.0268(12) 0.0227(11) 0.0001(9) 0.0034(9) 0.0087(9) C23 0.0286(12) 0.0308(12) 0.0212(11) -0.0008(9) 0.0023(9) 0.0116(10) C24 0.0346(13) 0.0334(13) 0.0195(10) 0.0030(9) 0.0075(9) 0.0115(11) C25 0.0277(11) 0.0285(12) 0.0183(10) 0.0030(8) 0.0042(8) 0.0098(9) C26 0.0275(11) 0.0311(12) 0.0189(10) 0.0008(9) 0.0056(9) 0.0090(10) C27 0.0400(15) 0.0391(14) 0.0246(11) 0.0026(10) 0.0094(11) 0.0054(12) C28 0.0427(15) 0.0383(15) 0.0331(13) 0.0057(11) 0.0115(12) 0.0033(12) C29 0.0334(13) 0.0323(13) 0.0349(13) 0.0009(10) 0.0075(11) 0.0033(11) C30 0.0282(12) 0.0301(12) 0.0249(11) -0.0022(9) 0.0037(9) 0.0077(10) C31 0.0250(11) 0.0258(11) 0.0205(10) 0.0007(8) 0.0049(8) 0.0053(9) C32 0.0361(14) 0.0521(16) 0.0231(11) -0.0042(11) 0.0041(10) 0.0232(13) C33 0.0404(15) 0.0618(19) 0.0247(12) -0.0019(12) -0.0006(11) 0.0275(14) C34 0.0417(15) 0.0417(15) 0.0209(11) -0.0025(10) 0.0045(10) 0.0152(12) C36 0.0333(13) 0.0368(13) 0.0226(11) -0.0011(10) 0.0018(9) 0.0141(11) C37 0.0344(13) 0.0298(12) 0.0213(11) 0.0009(9) 0.0037(9) 0.0125(10) C38 0.0360(14) 0.0485(16) 0.0236(12) -0.0044(11) 0.0048(10) 0.0086(12) C40 0.0545(17) 0.0402(15) 0.0251(12) -0.0091(11) -0.0009(12) 0.0214(13) C41 0.0414(15) 0.0403(15) 0.0356(14) -0.0100(12) -0.0013(12) 0.0097(13) C42 0.0367(14) 0.0420(15) 0.0316(13) -0.0043(11) 0.0069(11) 0.0100(12) P1 0.0377(4) 0.0434(4) 0.0271(3) 0.0021(3) 0.0113(3) 0.0142(3) P2 0.0232(4) 0.0299(4) 0.0191(4) 0.0030(3) 0.0042(3) 0.0089(3) P3 0.0373(5) 0.0316(5) 0.0250(4) 0.0069(3) 0.0110(4) 0.0202(4) F1 0.0921(16) 0.0506(12) 0.0485(11) -0.0112(9) 0.0223(11) -0.0012(11) F2 0.161(3) 0.0561(13) 0.0687(15) -0.0071(11) 0.0645(17) 0.0221(15) F3 0.0674(14) 0.1156(19) 0.0436(11) 0.0109(11) 0.0043(10) 0.0532(14) F4 0.111(2) 0.170(3) 0.0682(15) 0.0692(17) 0.0433(15) 0.100(2) F5 0.0518(11) 0.0975(17) 0.0538(11) 0.0278(11) 0.0295(9) 0.0289(11) F6 0.0578(12) 0.0693(13) 0.0591(12) -0.0171(10) 0.0334(10) -0.0104(10) F7 0.0296(7) 0.0446(9) 0.0280(7) 0.0048(6) 0.0077(6) 0.0182(7) F8 0.0322(8) 0.0333(8) 0.0287(7) -0.0012(6) 0.0035(6) 0.0056(6) F9 0.0322(7) 0.0424(8) 0.0244(7) 0.0107(6) 0.0068(6) 0.0136(7) F10 0.0438(10) 0.0609(11) 0.0562(11) -0.0003(9) 0.0188(8) 0.0285(9) F11 0.0673(12) 0.0526(10) 0.0288(8) 0.0065(7) 0.0041(8) 0.0319(9) F12 0.0600(11) 0.0313(9) 0.0513(10) 0.0101(7) 0.0113(8) 0.0180(8) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2763(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 . 1.9817(19) yes Fe1 . N2 . 1.8859(18) yes Fe1 . N3 . 1.977(2) yes Fe1 . N4 . 1.968(2) yes Fe1 . N5 . 1.8784(18) yes Fe1 . N6 . 1.969(2) yes N1 . C1 . 1.339(3) yes N1 . C5 . 1.374(3) yes N2 . C6 . 1.347(3) yes N2 . C10 . 1.345(3) yes N3 . C11 . 1.362(3) yes N3 . C15 . 1.342(3) yes N4 . C16 . 1.349(3) yes N4 . C20 . 1.366(3) yes N5 . C21 . 1.342(3) yes N5 . C25 . 1.350(3) yes N6 . C26 . 1.363(3) yes N6 . C30 . 1.346(3) yes N35 . C34 . 1.327(4) yes N35 . C36 . 1.339(3) yes N39 . C38 . 1.338(3) yes N39 . C40 . 1.330(4) yes C1 . C2 . 1.382(3) yes C1 . H11 . 0.954 no C2 . C3 . 1.376(4) yes C2 . H21 . 0.950 no C3 . C4 . 1.392(4) yes C3 . H31 . 0.958 no C4 . C5 . 1.381(3) yes C4 . H41 . 0.954 no C5 . C6 . 1.469(3) yes C6 . C7 . 1.389(3) yes C7 . C8 . 1.400(3) yes C7 . H71 . 0.943 no C8 . C9 . 1.394(3) yes C8 . C31 . 1.492(3) yes C9 . C10 . 1.385(3) yes C9 . H91 . 0.943 no C10 . C11 . 1.476(3) yes C11 . C12 . 1.380(3) yes C12 . C13 . 1.387(4) yes C12 . H121 . 0.956 no C13 . C14 . 1.375(4) yes C13 . H131 . 0.957 no C14 . C15 . 1.380(4) yes C14 . H141 . 0.956 no C15 . H151 . 0.957 no C16 . C17 . 1.381(4) yes C16 . H161 . 0.964 no C17 . C18 . 1.387(4) yes C17 . H171 . 0.961 no C18 . C19 . 1.394(3) yes C18 . H181 . 0.955 no C19 . C20 . 1.380(3) yes C19 . H191 . 0.962 no C20 . C21 . 1.477(3) yes C21 . C22 . 1.387(3) yes C22 . C23 . 1.401(3) yes C22 . H221 . 0.957 no C23 . C24 . 1.394(3) yes C23 . C37 . 1.485(3) yes C24 . C25 . 1.392(3) yes C24 . H241 . 0.947 no C25 . C26 . 1.464(3) yes C26 . C27 . 1.385(3) yes C27 . C28 . 1.386(4) yes C27 . H271 . 0.957 no C28 . C29 . 1.381(4) yes C28 . H281 . 0.948 no C29 . C30 . 1.385(4) yes C29 . H291 . 0.954 no C30 . H301 . 0.958 no C31 . C32 . 1.393(3) yes C31 . C36 . 1.394(3) yes C32 . C33 . 1.378(3) yes C32 . H321 . 0.950 no C33 . C34 . 1.372(4) yes C33 . H331 . 0.955 no C34 . H341 . 0.951 no C36 . H361 . 0.954 no C37 . C38 . 1.391(4) yes C37 . C42 . 1.383(4) yes C38 . H381 . 0.948 no C40 . C41 . 1.367(4) yes C40 . H401 . 0.953 no C41 . C42 . 1.387(4) yes C41 . H411 . 0.944 no C42 . H421 . 0.952 no P1 . F1 . 1.578(2) yes P1 . F2 . 1.584(2) yes P1 . F3 . 1.600(2) yes P1 . F4 . 1.574(2) yes P1 . F5 . 1.5911(19) yes P1 . F6 . 1.5872(19) yes P2 . F7 2_765 1.6114(14) yes P2 . F9 2_765 1.6002(13) yes P2 . F8 2_765 1.5979(14) yes P2 . F7 . 1.6114(14) yes P2 . F8 . 1.5979(14) yes P2 . F9 . 1.6002(13) yes P3 . F11 2_555 1.5984(16) yes P3 . F10 2_555 1.5967(16) yes P3 . F12 2_555 1.5912(16) yes P3 . F10 . 1.5967(16) yes P3 . F11 . 1.5984(16) yes P3 . F12 . 1.5912(16) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Fe1 . N2 . 80.74(8) yes N1 . Fe1 . N3 . 161.65(8) yes N2 . Fe1 . N3 . 80.93(8) yes N1 . Fe1 . N4 . 89.71(8) yes N2 . Fe1 . N4 . 97.24(8) yes N3 . Fe1 . N4 . 91.97(8) yes N1 . Fe1 . N5 . 101.73(8) yes N2 . Fe1 . N5 . 176.84(9) yes N3 . Fe1 . N5 . 96.57(8) yes N4 . Fe1 . N5 . 80.87(8) yes N1 . Fe1 . N6 . 92.47(8) yes N2 . Fe1 . N6 . 101.10(8) yes N3 . Fe1 . N6 . 91.66(8) yes N4 . Fe1 . N6 . 161.64(8) yes N5 . Fe1 . N6 . 80.84(8) yes Fe1 . N1 . C1 . 127.54(16) yes Fe1 . N1 . C5 . 114.39(15) yes C1 . N1 . C5 . 118.0(2) yes Fe1 . N2 . C6 . 119.99(15) yes Fe1 . N2 . C10 . 119.48(15) yes C6 . N2 . C10 . 120.29(19) yes Fe1 . N3 . C11 . 114.74(15) yes Fe1 . N3 . C15 . 127.42(16) yes C11 . N3 . C15 . 117.8(2) yes Fe1 . N4 . C16 . 126.68(16) yes Fe1 . N4 . C20 . 115.09(15) yes C16 . N4 . C20 . 118.2(2) yes Fe1 . N5 . C21 . 119.84(15) yes Fe1 . N5 . C25 . 119.65(16) yes C21 . N5 . C25 . 120.35(19) yes Fe1 . N6 . C26 . 114.59(16) yes Fe1 . N6 . C30 . 127.19(16) yes C26 . N6 . C30 . 118.2(2) yes C34 . N35 . C36 . 116.9(2) yes C38 . N39 . C40 . 116.9(2) yes N1 . C1 . C2 . 122.8(2) yes N1 . C1 . H11 . 116.3 no C2 . C1 . H11 . 120.9 no C1 . C2 . C3 . 119.2(2) yes C1 . C2 . H21 . 120.3 no C3 . C2 . H21 . 120.4 no C2 . C3 . C4 . 119.2(2) yes C2 . C3 . H31 . 120.6 no C4 . C3 . H31 . 120.3 no C3 . C4 . C5 . 119.0(2) yes C3 . C4 . H41 . 121.5 no C5 . C4 . H41 . 119.5 no C4 . C5 . N1 . 121.8(2) yes C4 . C5 . C6 . 124.8(2) yes N1 . C5 . C6 . 113.38(19) yes C5 . C6 . N2 . 111.40(19) yes C5 . C6 . C7 . 127.7(2) yes N2 . C6 . C7 . 120.8(2) yes C6 . C7 . C8 . 120.1(2) yes C6 . C7 . H71 . 119.5 no C8 . C7 . H71 . 120.4 no C7 . C8 . C9 . 117.5(2) yes C7 . C8 . C31 . 121.7(2) yes C9 . C8 . C31 . 120.7(2) yes C8 . C9 . C10 . 120.1(2) yes C8 . C9 . H91 . 120.6 no C10 . C9 . H91 . 119.3 no C9 . C10 . N2 . 121.2(2) yes C9 . C10 . C11 . 127.0(2) yes N2 . C10 . C11 . 111.69(19) yes C10 . C11 . N3 . 113.1(2) yes C10 . C11 . C12 . 124.5(2) yes N3 . C11 . C12 . 122.3(2) yes C11 . C12 . C13 . 118.8(2) yes C11 . C12 . H121 . 119.9 no C13 . C12 . H121 . 121.2 no C12 . C13 . C14 . 119.0(2) yes C12 . C13 . H131 . 120.0 no C14 . C13 . H131 . 120.9 no C13 . C14 . C15 . 119.4(2) yes C13 . C14 . H141 . 120.4 no C15 . C14 . H141 . 120.1 no C14 . C15 . N3 . 122.5(2) yes C14 . C15 . H151 . 120.2 no N3 . C15 . H151 . 117.3 no N4 . C16 . C17 . 122.4(2) yes N4 . C16 . H161 . 116.6 no C17 . C16 . H161 . 121.0 no C16 . C17 . C18 . 119.2(2) yes C16 . C17 . H171 . 119.4 no C18 . C17 . H171 . 121.4 no C17 . C18 . C19 . 119.0(2) yes C17 . C18 . H181 . 121.1 no C19 . C18 . H181 . 119.9 no C18 . C19 . C20 . 119.1(2) yes C18 . C19 . H191 . 120.5 no C20 . C19 . H191 . 120.4 no C19 . C20 . N4 . 122.1(2) yes C19 . C20 . C21 . 125.3(2) yes N4 . C20 . C21 . 112.6(2) yes C20 . C21 . N5 . 111.55(19) yes C20 . C21 . C22 . 126.9(2) yes N5 . C21 . C22 . 121.5(2) yes C21 . C22 . C23 . 119.1(2) yes C21 . C22 . H221 . 120.9 no C23 . C22 . H221 . 120.0 no C22 . C23 . C24 . 118.7(2) yes C22 . C23 . C37 . 119.7(2) yes C24 . C23 . C37 . 121.6(2) yes C23 . C24 . C25 . 119.3(2) yes C23 . C24 . H241 . 120.6 no C25 . C24 . H241 . 120.1 no C24 . C25 . N5 . 121.0(2) yes C24 . C25 . C26 . 127.9(2) yes N5 . C25 . C26 . 111.14(19) yes C25 . C26 . N6 . 113.6(2) yes C25 . C26 . C27 . 124.6(2) yes N6 . C26 . C27 . 121.8(2) yes C26 . C27 . C28 . 119.5(2) yes C26 . C27 . H271 . 119.6 no C28 . C27 . H271 . 120.9 no C27 . C28 . C29 . 118.5(3) yes C27 . C28 . H281 . 120.7 no C29 . C28 . H281 . 120.7 no C28 . C29 . C30 . 119.6(2) yes C28 . C29 . H291 . 121.1 no C30 . C29 . H291 . 119.3 no C29 . C30 . N6 . 122.2(2) yes C29 . C30 . H301 . 120.7 no N6 . C30 . H301 . 117.0 no C8 . C31 . C32 . 121.6(2) yes C8 . C31 . C36 . 122.2(2) yes C32 . C31 . C36 . 116.2(2) yes C31 . C32 . C33 . 119.8(2) yes C31 . C32 . H321 . 119.8 no C33 . C32 . H321 . 120.4 no C32 . C33 . C34 . 118.9(2) yes C32 . C33 . H331 . 120.8 no C34 . C33 . H331 . 120.3 no C33 . C34 . N35 . 123.6(2) yes C33 . C34 . H341 . 119.8 no N35 . C34 . H341 . 116.6 no C31 . C36 . N35 . 124.6(2) yes C31 . C36 . H361 . 118.0 no N35 . C36 . H361 . 117.3 no C23 . C37 . C38 . 121.2(2) yes C23 . C37 . C42 . 121.1(2) yes C38 . C37 . C42 . 117.8(2) yes C37 . C38 . N39 . 123.7(3) yes C37 . C38 . H381 . 118.5 no N39 . C38 . H381 . 117.8 no N39 . C40 . C41 . 123.9(2) yes N39 . C40 . H401 . 115.7 no C41 . C40 . H401 . 120.4 no C40 . C41 . C42 . 118.9(3) yes C40 . C41 . H411 . 120.6 no C42 . C41 . H411 . 120.6 no C41 . C42 . C37 . 118.8(3) yes C41 . C42 . H421 . 120.9 no C37 . C42 . H421 . 120.3 no F1 . P1 . F2 . 177.31(17) yes F1 . P1 . F3 . 88.77(13) yes F2 . P1 . F3 . 88.66(15) yes F1 . P1 . F4 . 90.21(16) yes F2 . P1 . F4 . 92.37(18) yes F3 . P1 . F4 . 178.76(17) yes F1 . P1 . F5 . 90.90(13) yes F2 . P1 . F5 . 89.80(14) yes F3 . P1 . F5 . 87.58(12) yes F4 . P1 . F5 . 91.75(13) yes F1 . P1 . F6 . 89.29(11) yes F2 . P1 . F6 . 89.99(13) yes F3 . P1 . F6 . 91.92(14) yes F4 . P1 . F6 . 88.76(14) yes F5 . P1 . F6 . 179.46(13) yes F7 2_765 P2 . F9 2_765 90.29(7) yes F7 2_765 P2 . F8 2_765 89.86(8) yes F9 2_765 P2 . F8 2_765 89.76(8) yes F7 2_765 P2 . F7 . 179.993 yes F9 2_765 P2 . F7 . 89.71(7) yes F8 2_765 P2 . F7 . 90.14(8) yes F7 2_765 P2 . F8 . 90.14(8) yes F9 2_765 P2 . F8 . 90.24(8) yes F8 2_765 P2 . F8 . 179.993 yes F7 . P2 . F8 . 89.86(8) yes F7 2_765 P2 . F9 . 89.71(7) yes F9 2_765 P2 . F9 . 179.993 yes F8 2_765 P2 . F9 . 90.24(8) yes F7 . P2 . F9 . 90.29(7) yes F8 . P2 . F9 . 89.76(8) yes F11 2_555 P3 . F10 2_555 90.14(10) yes F11 2_555 P3 . F12 2_555 89.43(9) yes F10 2_555 P3 . F12 2_555 89.72(10) yes F11 2_555 P3 . F10 . 89.86(10) yes F10 2_555 P3 . F10 . 179.993 yes F12 2_555 P3 . F10 . 90.28(10) yes F11 2_555 P3 . F11 . 179.993 yes F10 2_555 P3 . F11 . 89.86(10) yes F12 2_555 P3 . F11 . 90.57(9) yes F10 . P3 . F11 . 90.14(10) yes F11 2_555 P3 . F12 . 90.57(9) yes F10 2_555 P3 . F12 . 90.28(10) yes F12 2_555 P3 . F12 . 179.993 yes F10 . P3 . F12 . 89.72(10) yes F11 . P3 . F12 . 89.43(9) yes # Attachment 'Fe_4_pytpy_2_PF6.cif' data_jb421_173k _database_code_depnum_ccdc_archive 'CCDC 662663' _audit_creation_date 07-07-16 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '3271628 jb421_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 8.7704(2) _cell_length_b 8.7704(2) _cell_length_c 56.5252(14) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4347.91(18) _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z+1/2 -x+1/2,-y+1/2,-z+1/2 -y+3/4,x+1/4,z+1/4 y+3/4,-x+1/4,-z+1/4 -y+5/4,x+3/4,z+3/4 y+5/4,-x+3/4,-z+3/4 -x+1/2,-y,z+1/2 x+1/2,y,-z+1/2 -x+1,-y+1/2,z+1 x+1,y+1/2,-z+1 y+3/4,-x+3/4,z+3/4 -y+3/4,x+3/4,-z+3/4 y+5/4,-x+5/4,z+5/4 -y+5/4,x+5/4,-z+5/4 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 4 # Given Formula = C44 H34 F12 Fe1 N10 P2 # Dc = 1.60 Fooo = 2128.00 Mu = 5.20 M = 262.15 # Found Formula = C44 H34 F12 Fe1 N10 P2 # Dc = 1.60 FOOO = 2128.00 Mu = 5.20 M = 262.15 _chemical_formula_sum 'C44 H34 F12 Fe1 N10 P2' _chemical_formula_moiety 'C40 H28 Fe N8, 2(F6 P), 2(C2 H3 N)' _chemical_compound_source ? _chemical_formula_weight 1048.59 _cell_measurement_reflns_used 5511 _cell_measurement_theta_min 1 _cell_measurement_theta_max 30 _cell_measurement_temperature 173 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.24 _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 0.520 # Sheldrick geometric approximatio 0.90 0.90 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.90 # 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 34009 _reflns_number_total 3188 _diffrn_reflns_av_R_equivalents 0.086 # Number of reflections with Friedels Law is 3188 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3171 _diffrn_reflns_theta_min 3.363 _diffrn_reflns_theta_max 30.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.000 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -79 _diffrn_reflns_limit_l_max 79 _reflns_limit_h_min -8 _reflns_limit_h_max 8 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 79 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.04 _refine_diff_density_max 1.51 _refine_ls_number_reflns 2431 _refine_ls_number_restraints 335 _refine_ls_number_parameters 204 _refine_ls_wR_factor_ref 0.0578 _refine_ls_goodness_of_fit_ref 0.9421 _refine_ls_R_factor_all 0.1160 _refine_ls_wR_factor_all 0.0590 _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 2431 _refine_ls_R_factor_gt 0.0998 _refine_ls_wR_factor_gt 0.0578 _refine_ls_shift/su_max 0.000717 _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: 9.75 -2.63 4.11 5.05 -1.29 ; 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 0.0000 0.2500 0.6250 0.0175 1.0000 Uani S T . . . . N1 N -0.08246(18) 0.04271(18) 0.61931(3) 0.0206 1.0000 Uani . . . . . . N2 N 0.0000 0.2500 0.59170(4) 0.0208 1.0000 Uani S T . . . . N3 N 0.0000 0.2500 0.46690(5) 0.0486 1.0000 Uani S T . . . . C1 C -0.1240(2) -0.0610(2) 0.63557(4) 0.0260 1.0000 Uani . . . . . . C2 C -0.1898(3) -0.2000(2) 0.62945(4) 0.0333 1.0000 Uani . . . . . . C3 C -0.2116(3) -0.2343(3) 0.60580(5) 0.0370 1.0000 Uani . . . . . . C4 C -0.1664(3) -0.1300(3) 0.58879(4) 0.0318 1.0000 Uani . . . . . . C5 C -0.1021(2) 0.0069(2) 0.59603(3) 0.0230 1.0000 Uani . . . . . . C6 C -0.0518(2) 0.1270(2) 0.57981(3) 0.0229 1.0000 Uani . . . . . . C7 C -0.0535(2) 0.1239(2) 0.55525(3) 0.0282 1.0000 Uani . . . . . . C8 C 0.0000 0.2500 0.54272(4) 0.0284 1.0000 Uani S T . . . . C9 C 0.0000 0.2500 0.51656(5) 0.0317 1.0000 Uani S T . . . . C10 C -0.1121(3) 0.1740(4) 0.50386(4) 0.0440 1.0000 Uani . . . . . . C11 C -0.1053(4) 0.1782(4) 0.47913(4) 0.0507 1.0000 Uani . . . . . . P1 P 0.52525(17) 0.4033(2) 0.54723(2) 0.0445 0.5000 Uani D U . . . . F1 F 0.4391(5) 0.2747(5) 0.53220(7) 0.0680 0.5000 Uani D U . . . . F2 F 0.6150(7) 0.5305(7) 0.56193(9) 0.0780 0.5000 Uani D U . . . . F3 F 0.6378(6) 0.4315(8) 0.52575(7) 0.1087 0.5000 Uani D U . . . . F4 F 0.4161(5) 0.3753(6) 0.56921(7) 0.0740 0.5000 Uani D U . . . . F5 F 0.4098(6) 0.5272(5) 0.53706(9) 0.0775 0.5000 Uani D U . . . . F6 F 0.6364(6) 0.2762(6) 0.55767(9) 0.0918 0.5000 Uani D U . . . . N4 N 0.400(2) -0.0722(17) 0.56806(17) 0.1122 0.5000 Uani D U . . . . C12 C 0.4624(11) -0.0843(12) 0.55001(12) 0.0771 0.5000 Uani D U . . . . C13 C 0.5319(11) -0.0947(15) 0.52633(14) 0.0810 0.5000 Uani D U . . . . H11 H -0.1075 -0.0382 0.6522 0.0315 1.0000 Uiso R . . . . . H21 H -0.2199 -0.2720 0.6416 0.0403 1.0000 Uiso R . . . . . H31 H -0.2579 -0.3302 0.6012 0.0448 1.0000 Uiso R . . . . . H41 H -0.1795 -0.1522 0.5721 0.0385 1.0000 Uiso R . . . . . H71 H -0.0915 0.0350 0.5469 0.0342 1.0000 Uiso R . . . . . H101 H -0.1930 0.1195 0.5119 0.0532 1.0000 Uiso R . . . . . H111 H -0.1838 0.1242 0.4704 0.0611 1.0000 Uiso R . . . . . H131 H 0.6326 -0.1398 0.5276 0.0973 0.5000 Uiso R . . . . . H132 H 0.5404 0.0067 0.5196 0.0973 0.5000 Uiso R . . . . . H133 H 0.4686 -0.1576 0.5162 0.0973 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 0.01902(19) 0.01902(19) 0.0144(2) 0.0000 0.0000 0.0000 N1 0.0192(7) 0.0224(7) 0.0202(7) 0.0008(5) 0.0003(5) -0.0004(5) N2 0.0234(10) 0.0202(10) 0.0188(8) 0.0000 0.0000 -0.0020(9) N3 0.068(2) 0.059(2) 0.0186(10) 0.0000 0.0000 0.0125(19) C1 0.0261(9) 0.0254(9) 0.0264(9) 0.0042(7) 0.0058(7) 0.0039(7) C2 0.0372(11) 0.0236(9) 0.0392(12) 0.0078(8) 0.0081(9) -0.0023(8) C3 0.0411(12) 0.0236(10) 0.0463(13) -0.0002(9) 0.0015(10) -0.0071(9) C4 0.0386(11) 0.0247(10) 0.0321(10) -0.0033(8) -0.0027(8) -0.0054(8) C5 0.0243(8) 0.0225(9) 0.0221(8) -0.0007(6) 0.0010(6) -0.0013(7) C6 0.0260(9) 0.0215(8) 0.0212(8) 0.0003(6) -0.0007(6) -0.0003(7) C7 0.0341(10) 0.0305(10) 0.0201(8) -0.0049(7) -0.0025(7) -0.0018(8) C8 0.0340(15) 0.0351(15) 0.0162(10) 0.0000 0.0000 0.0020(13) C9 0.0424(16) 0.0359(15) 0.0168(10) 0.0000 0.0000 0.0039(14) C10 0.0511(15) 0.0588(16) 0.0223(10) -0.0031(10) -0.0054(9) -0.0013(12) C11 0.0642(17) 0.0648(18) 0.0230(10) -0.0078(11) -0.0085(11) 0.0020(14) P1 0.0361(6) 0.0655(9) 0.0319(6) -0.0036(6) -0.0069(5) 0.0002(6) F1 0.081(3) 0.061(2) 0.062(2) -0.0097(18) -0.0334(19) -0.008(2) F2 0.097(3) 0.102(4) 0.036(3) -0.009(2) -0.020(3) -0.039(3) F3 0.090(3) 0.193(6) 0.043(2) -0.015(3) 0.017(2) -0.054(4) F4 0.059(2) 0.112(4) 0.051(2) 0.003(2) 0.0066(18) -0.011(2) F5 0.086(3) 0.067(3) 0.080(3) 0.013(2) -0.032(3) 0.007(2) F6 0.077(3) 0.126(4) 0.072(3) -0.019(3) -0.029(2) 0.048(3) N4 0.171(5) 0.133(6) 0.033(4) -0.005(4) 0.017(4) -0.080(5) C12 0.092(4) 0.096(5) 0.043(3) 0.000(3) -0.002(3) -0.050(4) C13 0.065(4) 0.131(6) 0.046(3) -0.001(4) 0.010(3) -0.019(4) _refine_ls_extinction_coef 1288.554 _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.959(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 Fe1 . N1 11_454 1.9828(16) yes Fe1 . N1 16_445 1.9828(16) yes Fe1 . N1 6_456 1.9828(16) yes Fe1 . N2 6_456 1.882(2) yes Fe1 . N1 . 1.9828(16) yes Fe1 . N2 . 1.882(2) yes N1 . C1 . 1.343(2) yes N1 . C5 . 1.364(2) yes N2 . C6 11_454 1.349(2) yes N2 . C6 . 1.349(2) yes N3 . C11 11_454 1.314(4) yes N3 . C11 . 1.314(4) yes C1 . C2 . 1.393(3) yes C1 . H11 . 0.970 no C2 . C3 . 1.383(3) yes C2 . H21 . 0.970 no C3 . C4 . 1.385(3) yes C3 . H31 . 0.970 no C4 . C5 . 1.388(3) yes C4 . H41 . 0.970 no C5 . C6 . 1.465(3) yes C6 . C7 . 1.389(3) yes C7 . C8 . 1.395(2) yes C7 . H71 . 0.970 no C8 . C9 . 1.478(3) yes C9 . C10 11_454 1.388(3) yes C9 . C10 . 1.388(3) yes C10 . C11 . 1.400(3) yes C10 . H101 . 0.970 no C11 . H111 . 0.970 no P1 . F1 . 1.602(3) yes P1 . F2 . 1.598(4) yes P1 . F3 . 1.584(4) yes P1 . F4 . 1.588(4) yes P1 . F5 . 1.593(4) yes P1 . F6 . 1.594(4) yes N4 . C12 . 1.165(13) yes C12 . C13 . 1.474(10) yes C13 . H131 . 0.970 no C13 . H132 . 0.970 no C13 . H133 . 0.970 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 11_454 Fe1 . N1 16_445 91.508(14) yes N1 11_454 Fe1 . N1 6_456 91.508(14) yes N1 16_445 Fe1 . N1 6_456 161.33(9) yes N1 11_454 Fe1 . N2 6_456 99.34(4) yes N1 16_445 Fe1 . N2 6_456 80.66(4) yes N1 6_456 Fe1 . N2 6_456 80.66(4) yes N1 11_454 Fe1 . N1 . 161.33(9) yes N1 16_445 Fe1 . N1 . 91.508(14) yes N1 6_456 Fe1 . N1 . 91.508(14) yes N2 6_456 Fe1 . N1 . 99.34(4) yes N1 11_454 Fe1 . N2 . 80.66(4) yes N1 16_445 Fe1 . N2 . 99.34(4) yes N1 6_456 Fe1 . N2 . 99.34(4) yes N2 6_456 Fe1 . N2 . 179.994 yes N1 . Fe1 . N2 . 80.66(4) yes Fe1 . N1 . C1 . 127.50(13) yes Fe1 . N1 . C5 . 114.45(12) yes C1 . N1 . C5 . 118.02(17) yes C6 11_454 N2 . Fe1 . 119.86(11) yes C6 11_454 N2 . C6 . 120.3(2) yes Fe1 . N2 . C6 . 119.86(11) yes C11 11_454 N3 . C11 . 116.5(3) yes N1 . C1 . C2 . 122.37(19) yes N1 . C1 . H11 . 118.8 no C2 . C1 . H11 . 118.8 no C1 . C2 . C3 . 119.15(19) yes C1 . C2 . H21 . 120.4 no C3 . C2 . H21 . 120.4 no C2 . C3 . C4 . 119.2(2) yes C2 . C3 . H31 . 120.4 no C4 . C3 . H31 . 120.4 no C3 . C4 . C5 . 118.9(2) yes C3 . C4 . H41 . 120.6 no C5 . C4 . H41 . 120.6 no C4 . C5 . N1 . 122.35(17) yes C4 . C5 . C6 . 124.07(18) yes N1 . C5 . C6 . 113.58(16) yes C5 . C6 . N2 . 111.39(16) yes C5 . C6 . C7 . 127.45(17) yes N2 . C6 . C7 . 121.15(18) yes C6 . C7 . C8 . 119.23(19) yes C6 . C7 . H71 . 120.4 no C8 . C7 . H71 . 120.4 no C7 . C8 . C7 11_454 119.0(2) yes C7 . C8 . C9 . 120.52(12) yes C7 11_454 C8 . C9 . 120.52(12) yes C8 . C9 . C10 11_454 121.16(15) yes C8 . C9 . C10 . 121.16(15) yes C10 11_454 C9 . C10 . 117.7(3) yes C9 . C10 . C11 . 118.3(3) yes C9 . C10 . H101 . 120.8 no C11 . C10 . H101 . 120.9 no C10 . C11 . N3 . 124.6(3) yes C10 . C11 . H111 . 117.7 no N3 . C11 . H111 . 117.7 no F1 . P1 . F2 . 178.6(3) yes F1 . P1 . F3 . 89.8(2) yes F2 . P1 . F3 . 89.0(3) yes F1 . P1 . F4 . 91.2(2) yes F2 . P1 . F4 . 89.9(3) yes F3 . P1 . F4 . 178.5(3) yes F1 . P1 . F5 . 89.4(2) yes F2 . P1 . F5 . 91.4(3) yes F3 . P1 . F5 . 90.7(3) yes F4 . P1 . F5 . 90.3(3) yes F1 . P1 . F6 . 89.6(2) yes F2 . P1 . F6 . 89.7(3) yes F3 . P1 . F6 . 90.7(3) yes F4 . P1 . F6 . 88.3(3) yes F5 . P1 . F6 . 178.2(3) yes N4 . C12 . C13 . 175.8(13) yes C12 . C13 . H131 . 109.5 no C12 . C13 . H132 . 109.4 no C12 . C13 . H133 . 109.5 no H131 . C13 . H132 . 109.5 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.5 no # Attachment 'Ru_2pytpy_2.CIF' data_jb512abs _database_code_depnum_ccdc_archive 'CCDC 662664' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Ru(tpy(2-py))2](PF6)2.4H2O' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H36 F12 N8 O2 P2 Ru' _chemical_formula_weight 1051.78 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' 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' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.124(4) _cell_length_b 16.170(4) _cell_length_c 17.526(4) _cell_angle_alpha 94.305(5) _cell_angle_beta 99.731(4) _cell_angle_gamma 113.697(4) _cell_volume 4071.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 980 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 27.64 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 0.568 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.840948 _exptl_absorpt_correction_T_max 0.970000 _exptl_absorpt_process_details 'SADABS, Bruker 1995' _exptl_special_details ; In a thin film of perfluoropolyether oil on a mohair fibre ; _diffrn_ambient_temperature 150(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 294 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 27431 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 28.03 _reflns_number_total 18394 _reflns_number_gt 13834 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0852P)^2^+12.2749P] 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 18394 _refine_ls_number_parameters 1157 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1718 _refine_ls_wR_factor_gt 0.1536 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _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 0.58488(2) 0.83780(2) 0.254287(19) 0.02371(10) Uani 1 1 d . . . Ru2 Ru 0.09228(2) 0.34131(2) 0.294995(19) 0.02185(9) Uani 1 1 d . . . P1 P 0.18667(9) 0.62588(10) -0.06264(8) 0.0371(3) Uani 1 1 d . . . P2 P 0.11928(14) 0.86476(10) 0.47840(8) 0.0589(5) Uani 1 1 d . . . P3 P 0.40683(8) 0.63333(8) 0.49123(7) 0.0294(3) Uani 1 1 d . . . P40 P 0.2471(5) 0.2406(5) 0.0059(4) 0.082(2) Uiso 0.390(6) 1 d P . . P41 P 0.21787(16) 0.17671(17) 0.00144(13) 0.0362(7) Uiso 0.610(6) 1 d P . . F1 F 0.2225(2) 0.5489(2) -0.04283(19) 0.0532(8) Uani 1 1 d . . . F2 F 0.2541(3) 0.6898(3) 0.0164(2) 0.0611(9) Uani 1 1 d . . . F3 F 0.2645(3) 0.6656(3) -0.1110(2) 0.0643(10) Uani 1 1 d . . . F4 F 0.1172(3) 0.5584(3) -0.14076(19) 0.0562(9) Uani 1 1 d . . . F5 F 0.1067(2) 0.5824(2) -0.01618(19) 0.0514(8) Uani 1 1 d . . . F6 F 0.1498(2) 0.7011(2) -0.0836(2) 0.0490(8) Uani 1 1 d . . . F7 F 0.1339(3) 0.9548(3) 0.5332(2) 0.0713(11) Uani 1 1 d . . . F12 F 0.1335(3) 0.8201(2) 0.5530(2) 0.0744(13) Uani 1 1 d . . . F13 F 0.4545(2) 0.7143(2) 0.56461(18) 0.0515(8) Uani 1 1 d . . . F14 F 0.3845(2) 0.70085(19) 0.43756(18) 0.0408(7) Uani 1 1 d . . . F15 F 0.50557(19) 0.6630(2) 0.46677(16) 0.0363(6) Uani 1 1 d . . . F16 F 0.36058(19) 0.55256(18) 0.41786(16) 0.0367(6) Uani 1 1 d . . . F17 F 0.4299(2) 0.5660(2) 0.54444(18) 0.0434(7) Uani 1 1 d . . . F18 F 0.3082(2) 0.6030(2) 0.5143(2) 0.0497(8) Uani 1 1 d . . . F20 F 0.2997(3) 0.1805(4) 0.0681(2) 0.0914(16) Uani 1 1 d . . . F21 F 0.3017(4) 0.2564(5) -0.0326(3) 0.116(2) Uani 1 1 d . . . F22 F 0.2245(4) 0.1054(4) -0.0542(4) 0.1106(18) Uani 1 1 d . . . F80 F 0.0038(5) 0.8315(5) 0.4907(5) 0.051(2) Uiso 0.483(10) 1 d P . . F81 F 0.0239(10) 0.8094(10) 0.4620(9) 0.126(5) Uiso 0.517(10) 1 d P . . F90 F 0.1317(7) 0.9065(6) 0.4016(5) 0.069(3) Uiso 0.483(10) 1 d P . . F91 F 0.0795(6) 0.9097(5) 0.4057(4) 0.055(2) Uiso 0.517(10) 1 d P . . F100 F 0.1309(8) 0.7766(6) 0.4287(5) 0.071(3) Uiso 0.483(10) 1 d P . . F101 F 0.0765(6) 0.7724(5) 0.4216(4) 0.050(2) Uiso 0.517(10) 1 d P . . F110 F 0.2408(8) 0.9126(7) 0.5002(7) 0.078(3) Uiso 0.483(10) 1 d P . . F111 F 0.2109(7) 0.9075(7) 0.4630(7) 0.080(3) Uiso 0.517(10) 1 d P . . F190 F 0.2346(7) 0.2898(7) 0.0550(6) 0.055(2) Uiso 0.390(6) 1 d P . . F191 F 0.1977(7) 0.2309(7) 0.0594(6) 0.100(3) Uiso 0.610(6) 1 d P . . F230 F 0.1643(8) 0.2269(9) -0.0561(7) 0.072(3) Uiso 0.390(6) 1 d P . . F231 F 0.1376(4) 0.1747(5) -0.0653(4) 0.0558(16) Uiso 0.610(6) 1 d P . . F240 F 0.1500(8) 0.1419(8) 0.0510(7) 0.068(3) Uiso 0.390(6) 1 d P . . F241 F 0.1405(7) 0.0863(8) 0.0263(6) 0.113(3) Uiso 0.610(6) 1 d P . . O20 O 0.3772(6) 0.8615(6) 0.5684(5) 0.125(3) Uiso 1 1 d . . . O210 O 0.2258(5) 0.9466(4) 0.0566(4) 0.058(2) Uiso 0.689(12) 1 d P . . O220 O 0.3653(4) 0.8931(4) 0.0490(4) 0.054(2) Uiso 0.699(13) 1 d P . . O230 O 0.4553(5) 0.3937(5) 0.0801(4) 0.056(2) Uiso 0.598(11) 1 d P . . N1 N 0.6991(3) 0.8075(2) 0.2707(2) 0.0250(7) Uani 1 1 d . . . N2 N 0.6177(2) 0.8527(2) 0.3700(2) 0.0238(7) Uani 1 1 d . . . N3 N 0.4828(3) 0.8716(2) 0.2846(2) 0.0283(8) Uani 1 1 d . . . N4 N 0.4889(3) 0.7018(2) 0.2244(2) 0.0261(8) Uani 1 1 d . . . N5 N 0.5534(3) 0.8248(3) 0.1385(2) 0.0274(8) Uani 1 1 d . . . N6 N 0.6666(3) 0.9691(2) 0.2371(2) 0.0263(8) Uani 1 1 d . . . N7 N 0.2164(2) 0.3320(2) 0.2974(2) 0.0240(7) Uani 1 1 d . . . N8 N 0.1424(2) 0.3621(2) 0.4097(2) 0.0223(7) Uani 1 1 d . . . N9 N -0.0110(3) 0.3610(2) 0.3389(2) 0.0264(8) Uani 1 1 d . . . N10 N 0.0214(3) 0.2002(2) 0.2727(2) 0.0276(8) Uani 1 1 d . . . N11 N 0.0520(2) 0.3194(2) 0.1797(2) 0.0244(7) Uani 1 1 d . . . N12 N 0.1421(2) 0.4742(2) 0.2705(2) 0.0247(7) Uani 1 1 d . . . N13 N 0.7785(3) 0.8907(3) 0.6470(2) 0.0415(10) Uani 1 1 d . . . N14 N 0.4758(3) 0.8720(4) -0.1416(3) 0.0523(13) Uani 1 1 d . . . N15 N 0.2069(3) 0.4417(3) 0.6996(2) 0.0331(9) Uani 1 1 d . . . N16 N -0.0660(4) 0.1846(3) -0.1034(3) 0.0472(11) Uani 1 1 d . . . C1 C 0.7369(3) 0.7825(3) 0.2160(3) 0.0310(10) Uani 1 1 d . . . H1 H 0.7074 0.7732 0.1623 0.037 Uiso 1 1 calc R . . C2 C 0.8180(3) 0.7696(3) 0.2349(3) 0.0335(10) Uani 1 1 d . . . H2 H 0.8423 0.7505 0.1947 0.040 Uiso 1 1 calc R . . C3 C 0.8622(3) 0.7848(3) 0.3120(3) 0.0333(10) Uani 1 1 d . . . H3 H 0.9185 0.7782 0.3258 0.040 Uiso 1 1 calc R . . C4 C 0.8238(3) 0.8100(3) 0.3699(3) 0.0285(9) Uani 1 1 d . . . H4 H 0.8537 0.8206 0.4236 0.034 Uiso 1 1 calc R . . C5 C 0.7420(3) 0.8195(3) 0.3488(2) 0.0260(9) Uani 1 1 d . . . C6 C 0.6941(3) 0.8427(3) 0.4054(2) 0.0248(9) Uani 1 1 d . . . C7 C 0.7186(3) 0.8529(3) 0.4855(3) 0.0268(9) Uani 1 1 d . . . H7 H 0.7717 0.8450 0.5096 0.032 Uiso 1 1 calc R . . C8 C 0.6653(3) 0.8748(3) 0.5317(3) 0.0273(9) Uani 1 1 d . . . C9 C 0.6938(3) 0.8866(3) 0.6185(3) 0.0299(10) Uani 1 1 d . . . C10 C 0.6363(4) 0.8918(3) 0.6665(3) 0.0319(10) Uani 1 1 d . . . H10 H 0.5760 0.8867 0.6448 0.038 Uiso 1 1 calc R . . C11 C 0.6676(4) 0.9044(3) 0.7466(3) 0.0398(12) Uani 1 1 d . . . H11 H 0.6290 0.9085 0.7807 0.048 Uiso 1 1 calc R . . C12 C 0.7553(4) 0.9112(3) 0.7771(3) 0.0396(12) Uani 1 1 d . . . H12 H 0.7783 0.9208 0.8321 0.048 Uiso 1 1 calc R . . C13 C 0.8083(4) 0.9037(4) 0.7258(3) 0.0434(12) Uani 1 1 d . . . H13 H 0.8684 0.9078 0.7464 0.052 Uiso 1 1 calc R . . C14 C 0.5874(3) 0.8857(3) 0.4947(3) 0.0282(9) Uani 1 1 d . . . H14 H 0.5503 0.9008 0.5248 0.034 Uiso 1 1 calc R . . C15 C 0.5645(3) 0.8741(3) 0.4132(3) 0.0262(9) Uani 1 1 d . . . C16 C 0.4861(3) 0.8820(3) 0.3633(3) 0.0295(9) Uani 1 1 d . . . C17 C 0.4169(3) 0.8968(3) 0.3917(3) 0.0351(11) Uani 1 1 d . . . H17 H 0.4194 0.9039 0.4465 0.042 Uiso 1 1 calc R . . C18 C 0.3442(4) 0.9011(3) 0.3400(4) 0.0409(12) Uani 1 1 d . . . H18 H 0.2964 0.9107 0.3589 0.049 Uiso 1 1 calc R . . C19 C 0.3420(4) 0.8913(3) 0.2605(3) 0.0400(12) Uani 1 1 d . . . H19 H 0.2928 0.8944 0.2242 0.048 Uiso 1 1 calc R . . C20 C 0.4118(3) 0.8771(3) 0.2347(3) 0.0332(10) Uani 1 1 d . . . H20 H 0.4102 0.8708 0.1800 0.040 Uiso 1 1 calc R . . C21 C 0.4553(3) 0.6422(3) 0.2732(3) 0.0296(9) Uani 1 1 d . . . H21 H 0.4771 0.6619 0.3282 0.035 Uiso 1 1 calc R . . C22 C 0.3900(3) 0.5534(3) 0.2458(3) 0.0333(10) Uani 1 1 d . . . H22 H 0.3676 0.5127 0.2815 0.040 Uiso 1 1 calc R . . C23 C 0.3574(3) 0.5242(3) 0.1658(3) 0.0349(10) Uani 1 1 d . . . H23 H 0.3135 0.4630 0.1461 0.042 Uiso 1 1 calc R . . C24 C 0.3895(3) 0.5848(3) 0.1152(3) 0.0340(10) Uani 1 1 d . . . H24 H 0.3669 0.5663 0.0602 0.041 Uiso 1 1 calc R . . C25 C 0.4552(3) 0.6731(3) 0.1453(3) 0.0282(9) Uani 1 1 d . . . C26 C 0.4926(3) 0.7436(3) 0.0957(3) 0.0286(9) Uani 1 1 d . . . C27 C 0.4692(3) 0.7336(3) 0.0147(3) 0.0322(10) Uani 1 1 d . . . H27 H 0.4272 0.6759 -0.0153 0.039 Uiso 1 1 calc R . . C28 C 0.5081(3) 0.8093(4) -0.0225(3) 0.0334(10) Uani 1 1 d . . . C29 C 0.4799(3) 0.7998(4) -0.1091(3) 0.0366(11) Uani 1 1 d . . . C30 C 0.4569(3) 0.7185(3) -0.1518(3) 0.0330(10) Uani 1 1 d . . . H30 H 0.4623 0.6700 -0.1271 0.040 Uiso 1 1 calc R . . C31 C 0.4259(4) 0.7060(4) -0.2305(3) 0.0470(14) Uani 1 1 d . . . H31 H 0.4097 0.6484 -0.2609 0.056 Uiso 1 1 calc R . . C32 C 0.4175(4) 0.7755(5) -0.2671(3) 0.0474(14) Uani 1 1 d . . . H32 H 0.3944 0.7662 -0.3221 0.057 Uiso 1 1 calc R . . C33 C 0.4435(4) 0.8592(5) -0.2217(3) 0.0471(14) Uani 1 1 d . . . H33 H 0.4392 0.9084 -0.2459 0.057 Uiso 1 1 calc R . . C34 C 0.5709(3) 0.8933(4) 0.0227(3) 0.0360(11) Uani 1 1 d . . . H34 H 0.5978 0.9455 -0.0015 0.043 Uiso 1 1 calc R . . C35 C 0.5930(3) 0.8989(3) 0.1032(3) 0.0307(10) Uani 1 1 d . . . C36 C 0.6583(3) 0.9805(3) 0.1591(3) 0.0298(9) Uani 1 1 d . . . C37 C 0.7079(4) 1.0639(3) 0.1376(3) 0.0353(11) Uani 1 1 d . . . H37 H 0.7018 1.0705 0.0838 0.042 Uiso 1 1 calc R . . C38 C 0.7664(4) 1.1373(3) 0.1946(3) 0.0372(11) Uani 1 1 d . . . H38 H 0.8002 1.1952 0.1805 0.045 Uiso 1 1 calc R . . C39 C 0.7750(4) 1.1256(3) 0.2725(3) 0.0353(11) Uani 1 1 d . . . H39 H 0.8153 1.1753 0.3126 0.042 Uiso 1 1 calc R . . C40 C 0.7243(3) 1.0408(3) 0.2914(3) 0.0290(9) Uani 1 1 d . . . H40 H 0.7309 1.0333 0.3450 0.035 Uiso 1 1 calc R . . C41 C 0.2513(3) 0.3162(3) 0.2357(3) 0.0269(9) Uani 1 1 d . . . H41 H 0.2150 0.3056 0.1843 0.032 Uiso 1 1 calc R . . C42 C 0.3368(3) 0.3148(3) 0.2442(3) 0.0312(10) Uani 1 1 d . . . H42 H 0.3586 0.3029 0.1995 0.037 Uiso 1 1 calc R . . C43 C 0.3907(3) 0.3308(3) 0.3186(3) 0.0323(10) Uani 1 1 d . . . H43 H 0.4506 0.3311 0.3256 0.039 Uiso 1 1 calc R . . C44 C 0.3559(3) 0.3466(3) 0.3832(3) 0.0293(9) Uani 1 1 d . . . H44 H 0.3916 0.3572 0.4349 0.035 Uiso 1 1 calc R . . C45 C 0.2693(3) 0.3466(3) 0.3714(2) 0.0234(8) Uani 1 1 d . . . C46 C 0.2263(3) 0.3625(3) 0.4355(2) 0.0228(8) Uani 1 1 d . . . C47 C 0.2654(3) 0.3806(3) 0.5149(2) 0.0252(9) Uani 1 1 d . . . H47 H 0.3244 0.3807 0.5327 0.030 Uiso 1 1 calc R . . C48 C 0.2177(3) 0.3987(3) 0.5692(2) 0.0250(9) Uani 1 1 d . . . C49 C 0.2596(3) 0.4247(3) 0.6546(3) 0.0271(9) Uani 1 1 d . . . C50 C 0.3473(4) 0.4308(3) 0.6864(3) 0.0351(10) Uani 1 1 d . . . H50 H 0.3837 0.4191 0.6533 0.042 Uiso 1 1 calc R . . C51 C 0.3812(4) 0.4541(4) 0.7667(3) 0.0414(12) Uani 1 1 d . . . H51 H 0.4409 0.4583 0.7896 0.050 Uiso 1 1 calc R . . C52 C 0.3268(4) 0.4709(4) 0.8129(3) 0.0404(12) Uani 1 1 d . . . H52 H 0.3478 0.4863 0.8683 0.048 Uiso 1 1 calc R . . C53 C 0.2414(4) 0.4649(3) 0.7771(3) 0.0364(11) Uani 1 1 d . . . H53 H 0.2048 0.4779 0.8091 0.044 Uiso 1 1 calc R . . C54 C 0.1301(3) 0.3957(3) 0.5401(3) 0.0259(9) Uani 1 1 d . . . H54 H 0.0955 0.4062 0.5755 0.031 Uiso 1 1 calc R . . C55 C 0.0933(3) 0.3774(3) 0.4601(3) 0.0245(8) Uani 1 1 d . . . C56 C 0.0046(3) 0.3753(3) 0.4192(3) 0.0269(9) Uani 1 1 d . . . C57 C -0.0597(3) 0.3871(3) 0.4571(3) 0.0325(10) Uani 1 1 d . . . H57 H -0.0490 0.3951 0.5127 0.039 Uiso 1 1 calc R . . C58 C -0.1391(3) 0.3873(3) 0.4136(3) 0.0377(11) Uani 1 1 d . . . H58 H -0.1837 0.3952 0.4389 0.045 Uiso 1 1 calc R . . C59 C -0.1536(3) 0.3760(3) 0.3326(3) 0.0362(11) Uani 1 1 d . . . H59 H -0.2076 0.3769 0.3017 0.043 Uiso 1 1 calc R . . C60 C -0.0882(3) 0.3634(3) 0.2974(3) 0.0304(10) Uani 1 1 d . . . H60 H -0.0980 0.3561 0.2418 0.036 Uiso 1 1 calc R . . C61 C 0.0043(3) 0.1424(3) 0.3257(3) 0.0340(10) Uani 1 1 d . . . H61 H 0.0245 0.1670 0.3800 0.041 Uiso 1 1 calc R . . C62 C -0.0418(4) 0.0480(3) 0.3037(3) 0.0429(13) Uani 1 1 d . . . H62 H -0.0528 0.0089 0.3422 0.051 Uiso 1 1 calc R . . C63 C -0.0713(4) 0.0120(3) 0.2250(4) 0.0462(13) Uani 1 1 d . . . H63 H -0.1028 -0.0523 0.2088 0.055 Uiso 1 1 calc R . . C64 C -0.0548(4) 0.0703(3) 0.1696(3) 0.0398(12) Uani 1 1 d . . . H64 H -0.0744 0.0463 0.1152 0.048 Uiso 1 1 calc R . . C65 C -0.0091(3) 0.1640(3) 0.1946(3) 0.0308(10) Uani 1 1 d . . . C66 C 0.0102(3) 0.2323(3) 0.1406(3) 0.0272(9) Uani 1 1 d . . . C67 C -0.0080(3) 0.2150(3) 0.0599(3) 0.0313(10) Uani 1 1 d . . . H67 H -0.0370 0.1538 0.0331 0.038 Uiso 1 1 calc R . . C68 C 0.0164(3) 0.2882(3) 0.0173(3) 0.0296(9) Uani 1 1 d . . . C69 C -0.0063(3) 0.2698(3) -0.0697(3) 0.0326(10) Uani 1 1 d . . . C70 C 0.0320(4) 0.3370(4) -0.1139(3) 0.0471(14) Uani 1 1 d . . . H70 H 0.0747 0.3969 -0.0889 0.057 Uiso 1 1 calc R . . C71 C 0.0074(4) 0.3161(5) -0.1953(3) 0.0530(15) Uani 1 1 d . . . H71 H 0.0320 0.3618 -0.2265 0.064 Uiso 1 1 calc R . . C72 C -0.0524(4) 0.2294(5) -0.2294(3) 0.0478(15) Uani 1 1 d . . . H72 H -0.0698 0.2133 -0.2849 0.057 Uiso 1 1 calc R . . C73 C -0.0869(5) 0.1657(4) -0.1822(3) 0.0521(15) Uani 1 1 d . . . H73 H -0.1277 0.1049 -0.2064 0.063 Uiso 1 1 calc R . . C74 C 0.0605(3) 0.3769(3) 0.0585(3) 0.0283(9) Uani 1 1 d . . . H74 H 0.0784 0.4276 0.0311 0.034 Uiso 1 1 calc R . . C75 C 0.0782(3) 0.3911(3) 0.1396(2) 0.0257(9) Uani 1 1 d . . . C76 C 0.1255(3) 0.4795(3) 0.1924(3) 0.0261(9) Uani 1 1 d . . . C77 C 0.1520(3) 0.5638(3) 0.1659(3) 0.0333(10) Uani 1 1 d . . . H77 H 0.1407 0.5664 0.1114 0.040 Uiso 1 1 calc R . . C78 C 0.1949(4) 0.6432(3) 0.2200(3) 0.0401(12) Uani 1 1 d . . . H78 H 0.2135 0.7011 0.2028 0.048 Uiso 1 1 calc R . . C79 C 0.2106(4) 0.6382(3) 0.2991(3) 0.0375(11) Uani 1 1 d . . . H79 H 0.2398 0.6922 0.3370 0.045 Uiso 1 1 calc R . . C80 C 0.1828(3) 0.5523(3) 0.3219(3) 0.0286(9) Uani 1 1 d . . . H80 H 0.1931 0.5487 0.3764 0.034 Uiso 1 1 calc R . . O231 O 0.5010(3) 0.4684(3) 0.0256(3) 0.070(4) Uiso 0.402(11) 1 d PR . . O211 O 0.2748(16) 0.8808(15) 0.0580(13) 0.101(8) Uiso 0.311(12) 1 d P . . O221 O 0.472(2) 0.985(2) 0.062(2) 0.162(14) Uiso 0.301(13) 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 0.02457(18) 0.02262(17) 0.02001(17) 0.00414(13) 0.00349(13) 0.00642(14) Ru2 0.02066(17) 0.02090(17) 0.01920(17) 0.00453(12) 0.00135(12) 0.00488(13) P1 0.0349(7) 0.0523(8) 0.0312(6) 0.0179(6) 0.0094(5) 0.0228(6) P2 0.0835(12) 0.0330(7) 0.0230(6) 0.0052(5) 0.0052(7) -0.0102(8) P3 0.0283(6) 0.0271(6) 0.0256(6) 0.0038(5) 0.0046(5) 0.0050(5) F1 0.057(2) 0.066(2) 0.0449(19) 0.0113(16) 0.0004(16) 0.0384(18) F2 0.060(2) 0.058(2) 0.056(2) -0.0002(17) -0.0023(18) 0.0231(18) F3 0.050(2) 0.088(3) 0.073(3) 0.037(2) 0.0333(19) 0.035(2) F4 0.058(2) 0.072(2) 0.0372(18) 0.0138(16) -0.0020(15) 0.0298(19) F5 0.0496(19) 0.072(2) 0.0472(19) 0.0350(17) 0.0207(15) 0.0313(18) F6 0.0486(19) 0.059(2) 0.056(2) 0.0301(17) 0.0222(16) 0.0309(16) F7 0.088(3) 0.053(2) 0.056(2) 0.0053(18) 0.016(2) 0.013(2) F12 0.114(4) 0.046(2) 0.0358(19) 0.0057(15) -0.004(2) 0.014(2) F13 0.061(2) 0.0453(18) 0.0328(16) -0.0071(14) 0.0057(15) 0.0108(16) F14 0.0389(16) 0.0335(15) 0.0454(17) 0.0129(13) 0.0027(13) 0.0120(13) F15 0.0267(14) 0.0419(16) 0.0332(14) 0.0132(12) 0.0044(11) 0.0069(12) F16 0.0350(15) 0.0295(14) 0.0352(15) -0.0007(11) 0.0020(12) 0.0065(12) F17 0.0363(16) 0.0403(16) 0.0416(17) 0.0184(13) 0.0030(13) 0.0041(13) F18 0.0422(18) 0.057(2) 0.054(2) 0.0141(16) 0.0247(15) 0.0187(16) F20 0.069(3) 0.167(5) 0.056(2) 0.029(3) 0.013(2) 0.065(3) F21 0.097(4) 0.186(6) 0.042(2) 0.001(3) 0.015(3) 0.039(4) F22 0.068(3) 0.124(5) 0.116(4) -0.015(4) -0.006(3) 0.032(3) N1 0.0285(19) 0.0207(17) 0.0224(17) 0.0034(14) 0.0057(14) 0.0067(15) N2 0.0266(18) 0.0174(16) 0.0254(18) 0.0045(14) 0.0076(14) 0.0062(14) N3 0.030(2) 0.0219(18) 0.0297(19) 0.0049(15) 0.0037(16) 0.0083(15) N4 0.0238(18) 0.0261(18) 0.0264(19) 0.0044(15) 0.0062(15) 0.0082(15) N5 0.0225(18) 0.0306(19) 0.0238(18) 0.0037(15) 0.0023(14) 0.0070(15) N6 0.0267(19) 0.0269(18) 0.0231(18) 0.0055(14) 0.0037(15) 0.0096(15) N7 0.0244(18) 0.0217(17) 0.0221(17) 0.0051(14) 0.0036(14) 0.0062(14) N8 0.0218(17) 0.0189(16) 0.0215(17) 0.0066(13) 0.0030(13) 0.0039(14) N9 0.0235(18) 0.0206(17) 0.0296(19) 0.0057(14) 0.0014(15) 0.0052(14) N10 0.0248(19) 0.0235(18) 0.0285(19) 0.0053(15) 0.0036(15) 0.0048(15) N11 0.0236(18) 0.0236(17) 0.0228(17) 0.0059(14) 0.0032(14) 0.0071(14) N12 0.0210(17) 0.0235(17) 0.0245(18) 0.0054(14) 0.0007(14) 0.0056(14) N13 0.052(3) 0.044(3) 0.029(2) 0.0075(19) 0.0092(19) 0.021(2) N14 0.040(3) 0.076(4) 0.032(2) 0.009(2) 0.006(2) 0.017(3) N15 0.037(2) 0.033(2) 0.030(2) 0.0023(16) 0.0051(17) 0.0164(18) N16 0.060(3) 0.046(3) 0.027(2) -0.0001(19) 0.004(2) 0.017(2) C1 0.037(3) 0.029(2) 0.027(2) 0.0080(18) 0.0134(19) 0.011(2) C2 0.036(3) 0.032(2) 0.040(3) 0.010(2) 0.020(2) 0.015(2) C3 0.030(2) 0.033(2) 0.039(3) 0.009(2) 0.010(2) 0.014(2) C4 0.029(2) 0.024(2) 0.029(2) 0.0082(18) 0.0060(18) 0.0084(18) C5 0.030(2) 0.0200(19) 0.023(2) 0.0053(16) 0.0070(17) 0.0055(17) C6 0.026(2) 0.0186(19) 0.025(2) 0.0047(16) 0.0059(17) 0.0047(16) C7 0.028(2) 0.022(2) 0.026(2) 0.0046(17) 0.0021(17) 0.0070(17) C8 0.032(2) 0.021(2) 0.024(2) 0.0032(16) 0.0062(18) 0.0073(18) C9 0.038(3) 0.022(2) 0.025(2) 0.0048(17) 0.0066(19) 0.0091(19) C10 0.038(3) 0.030(2) 0.028(2) 0.0050(18) 0.006(2) 0.015(2) C11 0.052(3) 0.031(2) 0.037(3) 0.005(2) 0.017(2) 0.015(2) C12 0.052(3) 0.032(3) 0.026(2) 0.0042(19) 0.002(2) 0.012(2) C13 0.045(3) 0.049(3) 0.037(3) 0.018(2) 0.006(2) 0.020(3) C14 0.035(2) 0.022(2) 0.027(2) 0.0014(17) 0.0110(19) 0.0094(18) C15 0.027(2) 0.0189(19) 0.030(2) 0.0047(17) 0.0095(18) 0.0060(17) C16 0.032(2) 0.020(2) 0.033(2) 0.0040(17) 0.0070(19) 0.0083(18) C17 0.034(3) 0.027(2) 0.042(3) 0.002(2) 0.011(2) 0.011(2) C18 0.032(3) 0.033(3) 0.060(3) 0.006(2) 0.013(2) 0.015(2) C19 0.035(3) 0.033(3) 0.050(3) 0.007(2) 0.001(2) 0.016(2) C20 0.035(3) 0.028(2) 0.034(2) 0.0049(19) 0.002(2) 0.013(2) C21 0.032(2) 0.031(2) 0.025(2) 0.0063(18) 0.0082(18) 0.0113(19) C22 0.035(3) 0.029(2) 0.036(3) 0.0088(19) 0.014(2) 0.010(2) C23 0.029(2) 0.028(2) 0.040(3) 0.002(2) 0.006(2) 0.0055(19) C24 0.028(2) 0.034(2) 0.032(2) 0.001(2) 0.0041(19) 0.007(2) C25 0.024(2) 0.031(2) 0.026(2) 0.0051(18) 0.0052(17) 0.0086(18) C26 0.023(2) 0.031(2) 0.026(2) 0.0036(18) 0.0033(17) 0.0063(18) C27 0.028(2) 0.038(3) 0.023(2) -0.0008(19) 0.0007(18) 0.009(2) C28 0.027(2) 0.044(3) 0.023(2) 0.005(2) 0.0034(18) 0.010(2) C29 0.022(2) 0.052(3) 0.024(2) 0.006(2) 0.0032(18) 0.005(2) C30 0.024(2) 0.041(3) 0.028(2) 0.009(2) 0.0067(18) 0.006(2) C31 0.029(3) 0.064(4) 0.037(3) 0.001(3) 0.010(2) 0.009(3) C32 0.034(3) 0.080(4) 0.024(2) 0.004(3) 0.001(2) 0.023(3) C33 0.040(3) 0.070(4) 0.028(3) 0.010(3) 0.004(2) 0.022(3) C34 0.028(2) 0.042(3) 0.027(2) 0.010(2) 0.0051(19) 0.002(2) C35 0.027(2) 0.034(2) 0.025(2) 0.0064(18) 0.0039(18) 0.0070(19) C36 0.031(2) 0.033(2) 0.024(2) 0.0081(18) 0.0030(18) 0.0125(19) C37 0.040(3) 0.035(3) 0.026(2) 0.0088(19) 0.006(2) 0.011(2) C38 0.044(3) 0.027(2) 0.034(3) 0.012(2) 0.008(2) 0.007(2) C39 0.041(3) 0.027(2) 0.031(2) 0.0029(19) 0.004(2) 0.009(2) C40 0.032(2) 0.028(2) 0.023(2) 0.0039(17) 0.0008(18) 0.0106(19) C41 0.031(2) 0.023(2) 0.022(2) 0.0028(16) 0.0044(17) 0.0067(18) C42 0.034(2) 0.030(2) 0.028(2) 0.0033(18) 0.0093(19) 0.012(2) C43 0.027(2) 0.034(2) 0.036(3) 0.005(2) 0.0066(19) 0.013(2) C44 0.030(2) 0.029(2) 0.029(2) 0.0063(18) 0.0041(18) 0.0125(19) C45 0.027(2) 0.0183(19) 0.0198(19) 0.0043(15) 0.0019(16) 0.0058(16) C46 0.023(2) 0.0171(18) 0.026(2) 0.0068(16) 0.0043(16) 0.0059(16) C47 0.025(2) 0.021(2) 0.025(2) 0.0048(16) 0.0004(17) 0.0068(17) C48 0.030(2) 0.0181(19) 0.024(2) 0.0044(16) 0.0043(17) 0.0076(17) C49 0.035(2) 0.022(2) 0.022(2) 0.0045(16) 0.0049(18) 0.0096(18) C50 0.037(3) 0.038(3) 0.029(2) 0.004(2) 0.006(2) 0.015(2) C51 0.041(3) 0.049(3) 0.029(3) 0.002(2) 0.000(2) 0.019(2) C52 0.051(3) 0.039(3) 0.024(2) -0.002(2) 0.000(2) 0.016(2) C53 0.050(3) 0.036(3) 0.023(2) 0.0010(19) 0.010(2) 0.018(2) C54 0.029(2) 0.022(2) 0.026(2) 0.0042(16) 0.0091(17) 0.0074(17) C55 0.025(2) 0.0207(19) 0.026(2) 0.0061(16) 0.0076(17) 0.0065(17) C56 0.026(2) 0.021(2) 0.030(2) 0.0059(17) 0.0043(18) 0.0058(17) C57 0.029(2) 0.030(2) 0.038(3) 0.0043(19) 0.011(2) 0.0099(19) C58 0.030(3) 0.031(2) 0.055(3) 0.007(2) 0.014(2) 0.014(2) C59 0.026(2) 0.029(2) 0.050(3) 0.005(2) 0.001(2) 0.0105(19) C60 0.026(2) 0.023(2) 0.037(2) 0.0079(18) 0.0005(19) 0.0067(18) C61 0.034(3) 0.031(2) 0.034(2) 0.011(2) 0.011(2) 0.008(2) C62 0.045(3) 0.028(2) 0.046(3) 0.016(2) 0.013(2) 0.003(2) C63 0.045(3) 0.022(2) 0.056(3) 0.008(2) 0.007(3) 0.000(2) C64 0.039(3) 0.029(2) 0.037(3) 0.000(2) 0.000(2) 0.004(2) C65 0.029(2) 0.025(2) 0.033(2) 0.0034(18) 0.0039(19) 0.0057(18) C66 0.023(2) 0.027(2) 0.026(2) 0.0042(17) -0.0001(17) 0.0069(17) C67 0.025(2) 0.034(2) 0.029(2) 0.0000(19) 0.0017(18) 0.0083(19) C68 0.025(2) 0.037(2) 0.026(2) 0.0047(18) 0.0037(17) 0.0127(19) C69 0.026(2) 0.044(3) 0.025(2) 0.000(2) 0.0008(18) 0.015(2) C70 0.050(3) 0.047(3) 0.029(3) 0.005(2) 0.003(2) 0.008(3) C71 0.048(3) 0.071(4) 0.031(3) 0.017(3) 0.006(2) 0.015(3) C72 0.034(3) 0.085(4) 0.021(2) 0.000(3) 0.001(2) 0.025(3) C73 0.059(4) 0.055(4) 0.035(3) -0.007(3) -0.001(3) 0.022(3) C74 0.028(2) 0.034(2) 0.022(2) 0.0073(18) 0.0025(17) 0.0129(19) C75 0.023(2) 0.028(2) 0.023(2) 0.0052(17) 0.0025(16) 0.0085(17) C76 0.025(2) 0.025(2) 0.028(2) 0.0073(17) 0.0043(17) 0.0101(17) C77 0.037(3) 0.031(2) 0.030(2) 0.0128(19) 0.005(2) 0.013(2) C78 0.044(3) 0.025(2) 0.045(3) 0.012(2) 0.005(2) 0.009(2) C79 0.039(3) 0.021(2) 0.041(3) 0.0038(19) -0.003(2) 0.007(2) C80 0.027(2) 0.025(2) 0.028(2) 0.0020(17) -0.0010(17) 0.0076(18) _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 1.977(4) . ? Ru1 N5 1.980(4) . ? Ru1 N3 2.065(4) . ? Ru1 N1 2.069(4) . ? Ru1 N6 2.077(4) . ? Ru1 N4 2.079(4) . ? Ru2 N11 1.974(4) . ? Ru2 N8 1.985(3) . ? Ru2 N7 2.060(4) . ? Ru2 N10 2.070(4) . ? Ru2 N9 2.071(4) . ? Ru2 N12 2.077(4) . ? P1 F3 1.581(4) . ? P1 F5 1.592(3) . ? P1 F6 1.594(3) . ? P1 F2 1.595(4) . ? P1 F1 1.605(3) . ? P1 F4 1.611(4) . ? P2 F81 1.398(15) . ? P2 F111 1.441(10) . ? P2 F101 1.554(7) . ? P2 F90 1.557(9) . ? P2 F12 1.568(4) . ? P2 F7 1.593(4) . ? P2 F91 1.674(7) . ? P2 F100 1.705(9) . ? P2 F110 1.751(11) . ? P2 F80 1.775(8) . ? P3 F18 1.598(3) . ? P3 F17 1.598(3) . ? P3 F16 1.599(3) . ? P3 F14 1.601(3) . ? P3 F13 1.601(3) . ? P3 F15 1.611(3) . ? P40 P41 0.938(7) . ? P40 F21 1.159(8) . ? P40 F190 1.223(11) . ? P40 F191 1.307(11) . ? P40 F230 1.500(13) . ? P40 F231 1.831(9) . ? P40 F20 1.833(8) . ? P40 F240 2.053(13) . ? P40 F22 2.215(9) . ? P41 F191 1.454(10) . ? P41 F240 1.472(11) . ? P41 F22 1.502(6) . ? P41 F231 1.579(7) . ? P41 F20 1.585(5) . ? P41 F241 1.643(11) . ? P41 F230 1.678(12) . ? P41 F21 1.683(6) . ? P41 F190 1.886(10) . ? F80 F81 0.778(15) . ? F81 F101 1.459(19) . ? F90 F91 0.877(9) . ? F90 F111 1.517(13) . ? F100 F101 0.839(10) . ? F110 F111 0.720(12) . ? F190 F191 0.915(11) . ? F191 F240 1.313(14) . ? F230 F231 0.766(12) . ? F240 F241 0.910(12) . ? O210 O211 1.56(2) . ? O220 O211 1.43(2) . ? O220 O221 1.73(4) . ? O230 O231 1.616(8) . ? N1 C1 1.338(6) . ? N1 C5 1.386(6) . ? N2 C15 1.359(6) . ? N2 C6 1.360(6) . ? N3 C20 1.356(6) . ? N3 C16 1.367(6) . ? N4 C21 1.348(6) . ? N4 C25 1.370(6) . ? N5 C26 1.349(6) . ? N5 C35 1.362(6) . ? N6 C40 1.336(6) . ? N6 C36 1.383(6) . ? N7 C41 1.352(6) . ? N7 C45 1.373(5) . ? N8 C46 1.350(5) . ? N8 C55 1.352(5) . ? N9 C60 1.348(6) . ? N9 C56 1.372(6) . ? N10 C61 1.351(6) . ? N10 C65 1.371(6) . ? N11 C75 1.358(5) . ? N11 C66 1.358(6) . ? N12 C80 1.342(5) . ? N12 C76 1.365(6) . ? N13 C9 1.346(7) . ? N13 C13 1.353(7) . ? N14 C29 1.356(8) . ? N14 C33 1.382(7) . ? N15 C49 1.340(6) . ? N15 C53 1.340(6) . ? N16 C69 1.339(7) . ? N16 C73 1.347(7) . ? C1 C2 1.395(7) . ? C2 C3 1.371(7) . ? C3 C4 1.389(7) . ? C4 C5 1.382(6) . ? C5 C6 1.468(6) . ? C6 C7 1.370(6) . ? C7 C8 1.401(6) . ? C8 C14 1.395(7) . ? C8 C9 1.487(6) . ? C9 C10 1.373(7) . ? C10 C11 1.380(7) . ? C11 C12 1.381(8) . ? C12 C13 1.371(8) . ? C14 C15 1.392(6) . ? C15 C16 1.468(7) . ? C16 C17 1.391(7) . ? C17 C18 1.384(7) . ? C18 C19 1.383(8) . ? C19 C20 1.375(7) . ? C21 C22 1.384(6) . ? C22 C23 1.385(7) . ? C23 C24 1.376(7) . ? C24 C25 1.386(6) . ? C25 C26 1.480(6) . ? C26 C27 1.387(6) . ? C27 C28 1.400(7) . ? C28 C34 1.399(7) . ? C28 C29 1.486(6) . ? C29 C30 1.340(7) . ? C30 C31 1.356(7) . ? C31 C32 1.377(9) . ? C32 C33 1.381(9) . ? C34 C35 1.383(6) . ? C35 C36 1.466(6) . ? C36 C37 1.383(7) . ? C37 C38 1.378(7) . ? C38 C39 1.385(7) . ? C39 C40 1.385(6) . ? C41 C42 1.371(7) . ? C42 C43 1.381(7) . ? C43 C44 1.398(7) . ? C44 C45 1.376(6) . ? C45 C46 1.474(6) . ? C46 C47 1.383(6) . ? C47 C48 1.403(6) . ? C48 C54 1.398(6) . ? C48 C49 1.487(6) . ? C49 C50 1.392(7) . ? C50 C51 1.385(7) . ? C51 C52 1.378(8) . ? C52 C53 1.375(8) . ? C54 C55 1.386(6) . ? C55 C56 1.475(6) . ? C56 C57 1.388(6) . ? C57 C58 1.377(7) . ? C58 C59 1.385(8) . ? C59 C60 1.381(7) . ? C61 C62 1.390(7) . ? C62 C63 1.379(8) . ? C63 C64 1.387(7) . ? C64 C65 1.388(6) . ? C65 C66 1.479(6) . ? C66 C67 1.379(6) . ? C67 C68 1.404(7) . ? C68 C74 1.392(6) . ? C68 C69 1.485(6) . ? C69 C70 1.382(7) . ? C70 C71 1.391(7) . ? C71 C72 1.358(9) . ? C72 C73 1.371(9) . ? C74 C75 1.384(6) . ? C75 C76 1.472(6) . ? C76 C77 1.397(6) . ? C77 C78 1.381(7) . ? C78 C79 1.382(7) . ? C79 C80 1.391(6) . ? O231 O231 1.417(8) 2_665 ? 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 N5 179.12(15) . . ? N2 Ru1 N3 78.63(15) . . ? N5 Ru1 N3 101.45(15) . . ? N2 Ru1 N1 79.06(14) . . ? N5 Ru1 N1 100.87(15) . . ? N3 Ru1 N1 157.66(15) . . ? N2 Ru1 N6 100.16(14) . . ? N5 Ru1 N6 78.96(15) . . ? N3 Ru1 N6 94.39(14) . . ? N1 Ru1 N6 90.53(14) . . ? N2 Ru1 N4 102.26(14) . . ? N5 Ru1 N4 78.62(15) . . ? N3 Ru1 N4 89.28(14) . . ? N1 Ru1 N4 94.43(14) . . ? N6 Ru1 N4 157.57(14) . . ? N11 Ru2 N8 175.13(15) . . ? N11 Ru2 N7 95.89(14) . . ? N8 Ru2 N7 79.24(14) . . ? N11 Ru2 N10 78.82(15) . . ? N8 Ru2 N10 101.02(14) . . ? N7 Ru2 N10 90.71(14) . . ? N11 Ru2 N9 106.44(15) . . ? N8 Ru2 N9 78.44(15) . . ? N7 Ru2 N9 157.66(14) . . ? N10 Ru2 N9 94.35(14) . . ? N11 Ru2 N12 78.70(14) . . ? N8 Ru2 N12 101.57(14) . . ? N7 Ru2 N12 93.83(14) . . ? N10 Ru2 N12 157.41(15) . . ? N9 Ru2 N12 89.81(14) . . ? F3 P1 F5 177.9(2) . . ? F3 P1 F6 90.58(19) . . ? F5 P1 F6 90.34(17) . . ? F3 P1 F2 92.0(2) . . ? F5 P1 F2 89.9(2) . . ? F6 P1 F2 91.6(2) . . ? F3 P1 F1 89.5(2) . . ? F5 P1 F1 89.54(19) . . ? F6 P1 F1 179.0(2) . . ? F2 P1 F1 89.34(19) . . ? F3 P1 F4 89.6(2) . . ? F5 P1 F4 88.5(2) . . ? F6 P1 F4 89.65(19) . . ? F2 P1 F4 178.0(2) . . ? F1 P1 F4 89.36(19) . . ? F81 P2 F111 157.2(9) . . ? F81 P2 F101 59.0(8) . . ? F111 P2 F101 102.0(5) . . ? F81 P2 F90 102.0(7) . . ? F111 P2 F90 60.7(5) . . ? F101 P2 F90 83.4(4) . . ? F81 P2 F12 90.6(6) . . ? F111 P2 F12 104.0(5) . . ? F101 P2 F12 93.8(3) . . ? F90 P2 F12 163.1(5) . . ? F81 P2 F7 105.6(7) . . ? F111 P2 F7 92.1(4) . . ? F101 P2 F7 164.2(4) . . ? F90 P2 F7 97.5(4) . . ? F12 P2 F7 89.7(2) . . ? F81 P2 F91 78.0(6) . . ? F111 P2 F91 89.6(5) . . ? F101 P2 F91 87.8(4) . . ? F90 P2 F91 31.2(4) . . ? F12 P2 F91 165.6(4) . . ? F7 P2 F91 85.0(3) . . ? F81 P2 F100 87.2(8) . . ? F111 P2 F100 76.7(5) . . ? F101 P2 F100 29.4(3) . . ? F90 P2 F100 83.9(5) . . ? F12 P2 F100 85.6(4) . . ? F7 P2 F100 166.4(4) . . ? F91 P2 F100 102.4(4) . . ? F81 P2 F110 168.1(7) . . ? F111 P2 F110 23.6(5) . . ? F101 P2 F110 112.1(5) . . ? F90 P2 F110 83.8(5) . . ? F12 P2 F110 81.9(4) . . ? F7 P2 F110 83.7(4) . . ? F91 P2 F110 110.7(4) . . ? F100 P2 F110 83.0(5) . . ? F81 P2 F80 25.0(7) . . ? F111 P2 F80 168.4(5) . . ? F101 P2 F80 83.7(4) . . ? F90 P2 F80 110.6(5) . . ? F12 P2 F80 85.5(3) . . ? F7 P2 F80 81.2(3) . . ? F91 P2 F80 80.5(4) . . ? F100 P2 F80 111.1(5) . . ? F110 P2 F80 160.3(5) . . ? F18 P3 F17 90.26(18) . . ? F18 P3 F16 89.50(17) . . ? F17 P3 F16 90.03(17) . . ? F18 P3 F14 90.22(18) . . ? F17 P3 F14 179.50(19) . . ? F16 P3 F14 89.85(16) . . ? F18 P3 F13 91.23(19) . . ? F17 P3 F13 89.75(18) . . ? F16 P3 F13 179.24(19) . . ? F14 P3 F13 90.37(18) . . ? F18 P3 F15 179.18(19) . . ? F17 P3 F15 89.98(16) . . ? F16 P3 F15 89.71(16) . . ? F14 P3 F15 89.54(16) . . ? F13 P3 F15 89.56(18) . . ? P41 P40 F21 106.3(7) . . ? P41 P40 F190 121.0(8) . . ? F21 P40 F190 131.6(9) . . ? P41 P40 F191 78.8(7) . . ? F21 P40 F191 170.0(8) . . ? F190 P40 F191 42.2(6) . . ? P41 P40 F230 83.6(7) . . ? F21 P40 F230 98.7(7) . . ? F190 P40 F230 96.2(8) . . ? F191 P40 F230 90.3(7) . . ? P41 P40 F231 59.6(4) . . ? F21 P40 F231 102.8(6) . . ? F190 P40 F231 109.0(7) . . ? F191 P40 F231 87.1(6) . . ? F230 P40 F231 24.1(5) . . ? P41 P40 F20 59.8(4) . . ? F21 P40 F20 93.1(5) . . ? F190 P40 F20 101.5(6) . . ? F191 P40 F20 81.9(6) . . ? F230 P40 F20 143.4(7) . . ? F231 P40 F20 119.4(5) . . ? P41 P40 F240 40.5(5) . . ? F21 P40 F240 146.6(7) . . ? F190 P40 F240 80.7(7) . . ? F191 P40 F240 38.5(6) . . ? F230 P40 F240 83.3(6) . . ? F231 P40 F240 66.6(4) . . ? F20 P40 F240 68.5(4) . . ? P41 P40 F22 31.8(4) . . ? F21 P40 F22 74.9(5) . . ? F190 P40 F22 152.9(7) . . ? F191 P40 F22 110.6(6) . . ? F230 P40 F22 82.9(6) . . ? F231 P40 F22 62.1(3) . . ? F20 P40 F22 66.9(3) . . ? F240 P40 F22 72.2(4) . . ? P40 P41 F191 61.9(6) . . ? P40 P41 F240 115.1(7) . . ? F191 P41 F240 53.3(6) . . ? P40 P41 F22 128.9(5) . . ? F191 P41 F22 169.1(5) . . ? F240 P41 F22 115.7(6) . . ? P40 P41 F231 89.6(5) . . ? F191 P41 F231 92.7(5) . . ? F240 P41 F231 89.1(5) . . ? F22 P41 F231 86.5(3) . . ? P40 P41 F20 89.4(5) . . ? F191 P41 F20 87.2(4) . . ? F240 P41 F20 91.7(5) . . ? F22 P41 F20 93.8(3) . . ? F231 P41 F20 178.9(4) . . ? P40 P41 F241 148.4(6) . . ? F191 P41 F241 86.7(5) . . ? F240 P41 F241 33.4(5) . . ? F22 P41 F241 82.3(5) . . ? F231 P41 F241 87.9(5) . . ? F20 P41 F241 93.2(4) . . ? P40 P41 F230 62.7(6) . . ? F191 P41 F230 78.8(6) . . ? F240 P41 F230 98.9(6) . . ? F22 P41 F230 104.5(5) . . ? F231 P41 F230 27.0(4) . . ? F20 P41 F230 152.0(5) . . ? F241 P41 F230 109.8(6) . . ? P40 P41 F21 41.4(5) . . ? F191 P41 F21 102.9(5) . . ? F240 P41 F21 156.2(6) . . ? F22 P41 F21 88.0(3) . . ? F231 P41 F21 93.4(3) . . ? F20 P41 F21 85.6(3) . . ? F241 P41 F21 170.2(5) . . ? F230 P41 F21 74.3(5) . . ? P40 P41 F190 33.8(5) . . ? F191 P41 F190 28.2(4) . . ? F240 P41 F190 81.5(6) . . ? F22 P41 F190 162.7(4) . . ? F231 P41 F190 92.5(4) . . ? F20 P41 F190 86.9(4) . . ? F241 P41 F190 114.9(5) . . ? F230 P41 F190 69.3(5) . . ? F21 P41 F190 74.8(4) . . ? P41 F20 P40 30.8(2) . . ? P40 F21 P41 32.3(4) . . ? P41 F22 P40 19.2(2) . . ? F81 F80 P2 49.3(13) . . ? F80 F81 P2 105.7(16) . . ? F80 F81 F101 168.7(19) . . ? P2 F81 F101 65.8(8) . . ? F91 F90 F111 131.7(11) . . ? F91 F90 P2 81.8(9) . . ? F111 F90 P2 55.9(5) . . ? F90 F91 P2 67.0(8) . . ? F101 F100 P2 65.2(8) . . ? F100 F101 F81 137.3(12) . . ? F100 F101 P2 85.4(9) . . ? F81 F101 P2 55.2(6) . . ? F111 F110 P2 53.3(12) . . ? F110 F111 P2 103.1(15) . . ? F110 F111 F90 161.6(17) . . ? P2 F111 F90 63.4(5) . . ? F191 F190 P40 73.8(9) . . ? F191 F190 P41 48.6(8) . . ? P40 F190 P41 25.2(4) . . ? F190 F191 P40 64.0(9) . . ? F190 F191 F240 167.0(14) . . ? P40 F191 F240 103.2(9) . . ? F190 F191 P41 103.2(11) . . ? P40 F191 P41 39.3(4) . . ? F240 F191 P41 64.1(7) . . ? F231 F230 P40 103.0(13) . . ? F231 F230 P41 69.3(10) . . ? P40 F230 P41 33.7(4) . . ? F230 F231 P41 83.7(11) . . ? F230 F231 P40 53.0(10) . . ? P41 F231 P40 30.8(2) . . ? F241 F240 F191 146.2(15) . . ? F241 F240 P41 83.6(11) . . ? F191 F240 P41 62.6(6) . . ? F241 F240 P40 108.0(12) . . ? F191 F240 P40 38.3(6) . . ? P41 F240 P40 24.4(3) . . ? F240 F241 P41 63.0(10) . . ? O211 O220 O221 135.9(15) . . ? C1 N1 C5 118.3(4) . . ? C1 N1 Ru1 128.0(3) . . ? C5 N1 Ru1 113.6(3) . . ? C15 N2 C6 120.7(4) . . ? C15 N2 Ru1 119.8(3) . . ? C6 N2 Ru1 119.5(3) . . ? C20 N3 C16 119.0(4) . . ? C20 N3 Ru1 126.6(3) . . ? C16 N3 Ru1 114.1(3) . . ? C21 N4 C25 118.3(4) . . ? C21 N4 Ru1 127.6(3) . . ? C25 N4 Ru1 114.1(3) . . ? C26 N5 C35 120.9(4) . . ? C26 N5 Ru1 119.9(3) . . ? C35 N5 Ru1 119.2(3) . . ? C40 N6 C36 118.3(4) . . ? C40 N6 Ru1 127.8(3) . . ? C36 N6 Ru1 113.9(3) . . ? C41 N7 C45 118.0(4) . . ? C41 N7 Ru2 127.9(3) . . ? C45 N7 Ru2 114.1(3) . . ? C46 N8 C55 121.4(4) . . ? C46 N8 Ru2 118.7(3) . . ? C55 N8 Ru2 119.9(3) . . ? C60 N9 C56 118.4(4) . . ? C60 N9 Ru2 127.1(3) . . ? C56 N9 Ru2 114.5(3) . . ? C61 N10 C65 118.5(4) . . ? C61 N10 Ru2 127.3(3) . . ? C65 N10 Ru2 114.2(3) . . ? C75 N11 C66 120.3(4) . . ? C75 N11 Ru2 119.5(3) . . ? C66 N11 Ru2 119.5(3) . . ? C80 N12 C76 118.4(4) . . ? C80 N12 Ru2 127.6(3) . . ? C76 N12 Ru2 113.9(3) . . ? C9 N13 C13 118.1(5) . . ? C29 N14 C33 118.0(5) . . ? C49 N15 C53 117.8(4) . . ? C69 N16 C73 117.8(5) . . ? N1 C1 C2 122.4(4) . . ? C3 C2 C1 119.2(4) . . ? C2 C3 C4 119.4(5) . . ? C5 C4 C3 119.5(4) . . ? C4 C5 N1 121.1(4) . . ? C4 C5 C6 123.8(4) . . ? N1 C5 C6 115.1(4) . . ? N2 C6 C7 120.7(4) . . ? N2 C6 C5 112.4(4) . . ? C7 C6 C5 126.9(4) . . ? C6 C7 C8 120.1(4) . . ? C14 C8 C7 118.7(4) . . ? C14 C8 C9 122.2(4) . . ? C7 C8 C9 119.1(4) . . ? N13 C9 C10 122.2(4) . . ? N13 C9 C8 116.0(4) . . ? C10 C9 C8 121.8(4) . . ? C9 C10 C11 118.9(5) . . ? C10 C11 C12 119.8(5) . . ? C13 C12 C11 118.2(5) . . ? N13 C13 C12 122.8(5) . . ? C15 C14 C8 119.5(4) . . ? N2 C15 C14 120.3(4) . . ? N2 C15 C16 111.7(4) . . ? C14 C15 C16 128.0(4) . . ? N3 C16 C17 120.5(4) . . ? N3 C16 C15 115.6(4) . . ? C17 C16 C15 123.9(4) . . ? C18 C17 C16 119.8(5) . . ? C19 C18 C17 119.3(5) . . ? C20 C19 C18 119.2(5) . . ? N3 C20 C19 122.2(5) . . ? N4 C21 C22 122.0(4) . . ? C21 C22 C23 119.5(4) . . ? C24 C23 C22 119.2(4) . . ? C23 C24 C25 119.4(5) . . ? N4 C25 C24 121.7(4) . . ? N4 C25 C26 115.0(4) . . ? C24 C25 C26 123.3(4) . . ? N5 C26 C27 120.6(4) . . ? N5 C26 C25 112.4(4) . . ? C27 C26 C25 127.0(4) . . ? C26 C27 C28 119.3(4) . . ? C34 C28 C27 119.4(4) . . ? C34 C28 C29 121.2(4) . . ? C27 C28 C29 119.4(4) . . ? C30 C29 N14 122.7(5) . . ? C30 C29 C28 117.9(5) . . ? N14 C29 C28 119.4(5) . . ? C29 C30 C31 119.3(5) . . ? C30 C31 C32 121.0(6) . . ? C31 C32 C33 118.2(5) . . ? C32 C33 N14 120.7(6) . . ? C35 C34 C28 118.8(4) . . ? N5 C35 C34 121.0(4) . . ? N5 C35 C36 112.9(4) . . ? C34 C35 C36 126.1(4) . . ? N6 C36 C37 121.2(4) . . ? N6 C36 C35 115.0(4) . . ? C37 C36 C35 123.8(4) . . ? C38 C37 C36 119.7(4) . . ? C37 C38 C39 119.1(4) . . ? C38 C39 C40 119.3(5) . . ? N6 C40 C39 122.5(4) . . ? N7 C41 C42 122.9(4) . . ? C41 C42 C43 119.3(4) . . ? C42 C43 C44 118.9(4) . . ? C45 C44 C43 119.4(4) . . ? N7 C45 C44 121.6(4) . . ? N7 C45 C46 114.9(4) . . ? C44 C45 C46 123.6(4) . . ? N8 C46 C47 120.4(4) . . ? N8 C46 C45 113.0(4) . . ? C47 C46 C45 126.5(4) . . ? C46 C47 C48 120.0(4) . . ? C54 C48 C47 117.8(4) . . ? C54 C48 C49 120.3(4) . . ? C47 C48 C49 121.9(4) . . ? N15 C49 C50 121.8(4) . . ? N15 C49 C48 115.6(4) . . ? C50 C49 C48 122.6(4) . . ? C51 C50 C49 119.4(5) . . ? C52 C51 C50 118.7(5) . . ? C53 C52 C51 118.5(5) . . ? N15 C53 C52 123.7(5) . . ? C55 C54 C48 120.5(4) . . ? N8 C55 C54 119.8(4) . . ? N8 C55 C56 112.2(4) . . ? C54 C55 C56 127.9(4) . . ? N9 C56 C57 121.1(4) . . ? N9 C56 C55 115.0(4) . . ? C57 C56 C55 124.0(4) . . ? C58 C57 C56 119.5(5) . . ? C57 C58 C59 119.5(5) . . ? C60 C59 C58 118.9(5) . . ? N9 C60 C59 122.5(5) . . ? N10 C61 C62 122.2(5) . . ? C63 C62 C61 119.0(5) . . ? C62 C63 C64 119.6(5) . . ? C63 C64 C65 119.2(5) . . ? N10 C65 C64 121.5(4) . . ? N10 C65 C66 114.9(4) . . ? C64 C65 C66 123.6(4) . . ? N11 C66 C67 120.8(4) . . ? N11 C66 C65 112.1(4) . . ? C67 C66 C65 127.0(4) . . ? C66 C67 C68 119.8(4) . . ? C74 C68 C67 118.5(4) . . ? C74 C68 C69 121.7(4) . . ? C67 C68 C69 119.8(4) . . ? N16 C69 C70 121.6(5) . . ? N16 C69 C68 116.5(4) . . ? C70 C69 C68 121.8(5) . . ? C69 C70 C71 119.3(5) . . ? C72 C71 C70 119.1(6) . . ? C71 C72 C73 118.6(5) . . ? N16 C73 C72 123.5(6) . . ? C75 C74 C68 119.8(4) . . ? N11 C75 C74 120.8(4) . . ? N11 C75 C76 112.1(4) . . ? C74 C75 C76 127.1(4) . . ? N12 C76 C77 121.3(4) . . ? N12 C76 C75 115.4(4) . . ? C77 C76 C75 123.3(4) . . ? C78 C77 C76 119.2(4) . . ? C77 C78 C79 119.7(4) . . ? C78 C79 C80 118.5(4) . . ? N12 C80 C79 122.9(4) . . ? O231 O231 O230 153.2(6) 2_665 . ? O220 O211 O210 132.3(16) . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.220 _refine_diff_density_min -1.213 _refine_diff_density_rms 0.128 data_CRYSTALS_cif _database_code_depnum_ccdc_archive 'CCDC 666047' _audit_creation_date 07-08-17 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '8171209 jb1123_173k' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 8.56310(10) _cell_length_b 15.5219(2) _cell_length_c 19.7088(2) _cell_angle_alpha 103.5494(7) _cell_angle_beta 97.4740(7) _cell_angle_gamma 101.6026(6) _cell_volume 2451.09(5) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ru -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 # Given Formula = C84 H68 F48 N16 O1 P8 Ru2 # Dc = 1.82 Fooo = 1332.00 Mu = 5.87 M = 1339.70 # Found Formula = C84 H68 F48 N16 O1 P8 Ru2 # Dc = 1.82 FOOO = 1332.00 Mu = 5.87 M = 1339.70 _chemical_formula_sum 'C84 H68 F48 N16 O1 P8 Ru2' _chemical_formula_moiety '2(C42 H34 N8 Ru), 8(F6 P), H2 O' _chemical_compound_source ? _chemical_formula_weight 2679.41 _cell_measurement_reflns_used 11688 _cell_measurement_theta_min 1 _cell_measurement_theta_max 28 _cell_measurement_temperature 173 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_max 0.52 _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 0.587 # Sheldrick geometric approximatio 0.95 0.98 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 0.98 # 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 23178 _reflns_number_total 11707 _diffrn_reflns_av_R_equivalents 0.025 # Number of reflections with Friedels Law is 11707 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 11714 _diffrn_reflns_theta_min 1.515 _diffrn_reflns_theta_max 27.895 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.895 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min -20 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _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 -0.93 _refine_diff_density_max 0.67 _refine_ls_number_reflns 8538 _refine_ls_number_restraints 1226 _refine_ls_number_parameters 811 #_refine_ls_R_factor_ref 0.0364 _refine_ls_wR_factor_ref 0.0378 _refine_ls_goodness_of_fit_ref 1.2304 #_reflns_number_all 11639 _refine_ls_R_factor_all 0.0539 _refine_ls_wR_factor_all 0.0481 # 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 8538 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_gt 0.0378 _refine_ls_shift/su_max 0.001821 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.09 1.41 1.10 0.491 0.221 ; _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. ; # End of 'script/refcif.dat' 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 0.57554(3) 0.609411(15) 0.252468(12) 0.0190 1.0000 Uani . . . . . . N1 N 0.4303(3) 0.50163(15) 0.17103(12) 0.0216 1.0000 Uani . . . . . . N2 N 0.5434(3) 0.51011(15) 0.29997(11) 0.0196 1.0000 Uani . . . . . . N3 N 0.7146(3) 0.67553(15) 0.35252(11) 0.0203 1.0000 Uani . . . . . . N4 N 0.3864(3) 0.66928(15) 0.27794(12) 0.0213 1.0000 Uani . . . . . . N5 N 0.6116(3) 0.71245(15) 0.20808(11) 0.0204 1.0000 Uani . . . . . . N6 N 0.7750(3) 0.58987(15) 0.20655(11) 0.0211 1.0000 Uani . . . . . . N7 N 0.3263(3) 0.15826(16) 0.41471(14) 0.0297 1.0000 Uani . . . . . . N8 N 0.7487(3) 1.10451(17) 0.15247(15) 0.0352 1.0000 Uani . . . . . . C1 C 0.3809(4) 0.5019(2) 0.10340(15) 0.0270 1.0000 Uani . . . . . . C2 C 0.2824(4) 0.4260(2) 0.05343(16) 0.0342 1.0000 Uani . . . . . . C3 C 0.2341(4) 0.3464(2) 0.07288(17) 0.0370 1.0000 Uani . . . . . . C4 C 0.2875(4) 0.3437(2) 0.14143(16) 0.0315 1.0000 Uani . . . . . . C5 C 0.3861(3) 0.42195(19) 0.18989(15) 0.0232 1.0000 Uani . . . . . . C6 C 0.4514(3) 0.42605(18) 0.26361(14) 0.0214 1.0000 Uani . . . . . . C7 C 0.4292(3) 0.35584(19) 0.29634(15) 0.0243 1.0000 Uani . . . . . . C8 C 0.5002(3) 0.37223(19) 0.36759(15) 0.0229 1.0000 Uani . . . . . . C9 C 0.5933(3) 0.45971(19) 0.40386(15) 0.0241 1.0000 Uani . . . . . . C10 C 0.6151(3) 0.52721(18) 0.36868(14) 0.0214 1.0000 Uani . . . . . . C11 C 0.7169(3) 0.62045(18) 0.39780(14) 0.0216 1.0000 Uani . . . . . . C12 C 0.8128(4) 0.6508(2) 0.46479(15) 0.0268 1.0000 Uani . . . . . . C13 C 0.9102(4) 0.7390(2) 0.48733(15) 0.0300 1.0000 Uani . . . . . . C14 C 0.9047(4) 0.79547(19) 0.44256(15) 0.0278 1.0000 Uani . . . . . . C15 C 0.8055(3) 0.76191(18) 0.37636(15) 0.0238 1.0000 Uani . . . . . . C16 C 0.2703(3) 0.64180(19) 0.31362(15) 0.0257 1.0000 Uani . . . . . . C17 C 0.1545(4) 0.6902(2) 0.32986(17) 0.0306 1.0000 Uani . . . . . . C18 C 0.1583(4) 0.7699(2) 0.30932(18) 0.0331 1.0000 Uani . . . . . . C19 C 0.2755(4) 0.7985(2) 0.27193(17) 0.0296 1.0000 Uani . . . . . . C20 C 0.3877(3) 0.74692(18) 0.25657(14) 0.0224 1.0000 Uani . . . . . . C21 C 0.5154(3) 0.77208(18) 0.21707(14) 0.0222 1.0000 Uani . . . . . . C22 C 0.5444(3) 0.84793(19) 0.19092(15) 0.0251 1.0000 Uani . . . . . . C23 C 0.6727(3) 0.86194(19) 0.15518(15) 0.0245 1.0000 Uani . . . . . . C24 C 0.7709(4) 0.79977(19) 0.14650(15) 0.0260 1.0000 Uani . . . . . . C25 C 0.7372(3) 0.72503(18) 0.17383(14) 0.0227 1.0000 Uani . . . . . . C26 C 0.8272(3) 0.65274(18) 0.17097(14) 0.0228 1.0000 Uani . . . . . . C27 C 0.9542(4) 0.6472(2) 0.13431(15) 0.0279 1.0000 Uani . . . . . . C28 C 1.0288(4) 0.5760(2) 0.13347(17) 0.0324 1.0000 Uani . . . . . . C29 C 0.9766(4) 0.5125(2) 0.16942(16) 0.0305 1.0000 Uani . . . . . . C30 C 0.8501(3) 0.52144(19) 0.20531(15) 0.0254 1.0000 Uani . . . . . . C31 C 0.4793(3) 0.29887(19) 0.40481(15) 0.0253 1.0000 Uani . . . . . . C32 C 0.5925(4) 0.3014(2) 0.46321(18) 0.0364 1.0000 Uani . . . . . . C33 C 0.5668(5) 0.2320(2) 0.4964(2) 0.0452 1.0000 Uani . . . . . . C34 C 0.4325(4) 0.1607(2) 0.47174(18) 0.0378 1.0000 Uani . . . . . . C35 C 0.3460(4) 0.22544(19) 0.38181(16) 0.0273 1.0000 Uani . . . . . . C36 C 0.1863(5) 0.0783(2) 0.3868(2) 0.0438 1.0000 Uani . . . . . . C37 C 0.7060(3) 0.94407(19) 0.12843(16) 0.0262 1.0000 Uani . . . . . . C38 C 0.7226(4) 0.9397(2) 0.05849(17) 0.0375 1.0000 Uani . . . . . . C39 C 0.7516(5) 1.0195(3) 0.03765(19) 0.0494 1.0000 Uani . . . . . . C40 C 0.7654(5) 1.1013(2) 0.08552(19) 0.0438 1.0000 Uani . . . . . . C41 C 0.7190(4) 1.0282(2) 0.17430(16) 0.0305 1.0000 Uani . . . . . . C42 C 0.7671(6) 1.1938(2) 0.2044(2) 0.0544 1.0000 Uani . . . . . . P1 P 0.23762(12) 0.06032(7) 0.17791(5) 0.0414 1.0000 Uani D U . . . . P2 P 0.30629(17) 0.68692(7) -0.00986(6) 0.0595 1.0000 Uani D U . . . . P3 P 0.70960(10) 1.00687(6) 0.39593(4) 0.0330 1.0000 Uani . . . . . . P4 P 1.01793(9) 0.41552(5) 0.36139(4) 0.0276 1.0000 Uani . . . . . . F41 F 0.8043(3) 1.10852(15) 0.40479(15) 0.0677 1.0000 Uani . . . . . . F42 F 0.6147(3) 0.90401(14) 0.38787(13) 0.0504 1.0000 Uani . . . . . . F43 F 0.7780(4) 0.97259(19) 0.32593(13) 0.0716 1.0000 Uani . . . . . . F44 F 0.6475(4) 1.03781(19) 0.46855(16) 0.0796 1.0000 Uani . . . . . . F45 F 0.8642(3) 0.99035(16) 0.44074(13) 0.0560 1.0000 Uani . . . . . . F46 F 0.5565(3) 1.02346(19) 0.35222(18) 0.0844 1.0000 Uani . . . . . . F51 F 0.9448(2) 0.41203(15) 0.43131(10) 0.0421 1.0000 Uani . . . . . . F52 F 1.0922(3) 0.41932(15) 0.29150(10) 0.0453 1.0000 Uani . . . . . . F53 F 1.0554(3) 0.31782(14) 0.35709(12) 0.0491 1.0000 Uani . . . . . . F54 F 0.9823(3) 0.51372(13) 0.36608(11) 0.0423 1.0000 Uani . . . . . . F55 F 0.8422(2) 0.36859(13) 0.31322(10) 0.0410 1.0000 Uani . . . . . . F56 F 1.1948(2) 0.46375(16) 0.40939(11) 0.0472 1.0000 Uani . . . . . . F1 F 0.3476(3) 0.0026(2) 0.13921(14) 0.0803 1.0000 Uani D U . . . . F2 F 0.1327(4) 0.1210(3) 0.21777(15) 0.1159 1.0000 Uani D U . . . . F3 F 0.1042(7) 0.0291(5) 0.1106(3) 0.0897 0.5000 Uani D U . . . . F4 F 0.3721(7) 0.0952(5) 0.2480(3) 0.0791 0.5000 Uani D U . . . . F5 F 0.1543(10) -0.0181(4) 0.2077(4) 0.1240 0.5000 Uani D U . . . . F6 F 0.3286(9) 0.1408(4) 0.1506(4) 0.0913 0.5000 Uani D U . . . . F13 F 0.2314(11) 0.1149(4) 0.1206(3) 0.1105 0.5000 Uani D U . . . . F14 F 0.2431(11) 0.0030(4) 0.2332(3) 0.1108 0.5000 Uani D U . . . . F15 F 0.0873(7) -0.0139(5) 0.1300(4) 0.1101 0.5000 Uani D U . . . . F16 F 0.3895(8) 0.1343(5) 0.2247(4) 0.1186 0.5000 Uani D U . . . . F21 F 0.4901(5) 0.6802(3) 0.0275(2) 0.0547 0.5000 Uani D U . . . . F22 F 0.1519(6) 0.6969(4) -0.0461(4) 0.0834 0.5000 Uani D U . . . . F23 F 0.3860(7) 0.7936(3) 0.0097(3) 0.0679 0.5000 Uani D U . . . . F24 F 0.2549(10) 0.5825(3) -0.0238(4) 0.1197 0.5000 Uani D U . . . . F25 F 0.2696(7) 0.7016(5) 0.0662(3) 0.0906 0.5000 Uani D U . . . . F26 F 0.3763(8) 0.6747(6) -0.0821(2) 0.1103 0.5000 Uani D U . . . . F31 F 0.1994(10) 0.7623(4) 0.0212(4) 0.1275 0.5000 Uani D U . . . . F32 F 0.3581(8) 0.6038(4) -0.0438(4) 0.1125 0.5000 Uani D U . . . . F33 F 0.2036(9) 0.6854(4) -0.0848(3) 0.0850 0.5000 Uani D U . . . . F34 F 0.3579(11) 0.6870(4) 0.0669(3) 0.1565 0.5000 Uani D U . . . . F35 F 0.1327(8) 0.6114(4) -0.0078(3) 0.0912 0.5000 Uani D U . . . . F36 F 0.4350(9) 0.7604(5) -0.0141(5) 0.1434 0.5000 Uani D U . . . . O1 O 1.0497(14) 0.8272(7) 0.0539(7) 0.1357 0.5000 Uani . . . . . . H11 H 0.4156 0.5557 0.0904 0.0340 1.0000 Uiso R . . . . . H21 H 0.2505 0.4282 0.0072 0.0390 1.0000 Uiso R . . . . . H31 H 0.1679 0.2952 0.0404 0.0420 1.0000 Uiso R . . . . . H41 H 0.2575 0.2903 0.1553 0.0350 1.0000 Uiso R . . . . . H71 H 0.3672 0.2977 0.2708 0.0298 1.0000 Uiso R . . . . . H91 H 0.6413 0.4726 0.4515 0.0302 1.0000 Uiso R . . . . . H121 H 0.8117 0.6117 0.4944 0.0310 1.0000 Uiso R . . . . . H131 H 0.9778 0.7598 0.5321 0.0341 1.0000 Uiso R . . . . . H141 H 0.9684 0.8552 0.4569 0.0320 1.0000 Uiso R . . . . . H151 H 0.8005 0.8001 0.3465 0.0291 1.0000 Uiso R . . . . . H161 H 0.2676 0.5883 0.3271 0.0299 1.0000 Uiso R . . . . . H171 H 0.0755 0.6695 0.3548 0.0358 1.0000 Uiso R . . . . . H181 H 0.0815 0.8034 0.3203 0.0409 1.0000 Uiso R . . . . . H191 H 0.2797 0.8516 0.2569 0.0369 1.0000 Uiso R . . . . . H221 H 0.4784 0.8891 0.1975 0.0291 1.0000 Uiso R . . . . . H241 H 0.8577 0.8085 0.1233 0.0319 1.0000 Uiso R . . . . . H271 H 0.9876 0.6910 0.1112 0.0328 1.0000 Uiso R . . . . . H281 H 1.1130 0.5711 0.1084 0.0410 1.0000 Uiso R . . . . . H291 H 1.0259 0.4640 0.1693 0.0380 1.0000 Uiso R . . . . . H301 H 0.8128 0.4785 0.2294 0.0310 1.0000 Uiso R . . . . . H321 H 0.6857 0.3491 0.4797 0.0451 1.0000 Uiso R . . . . . H331 H 0.6405 0.2333 0.5363 0.0560 1.0000 Uiso R . . . . . H341 H 0.4138 0.1140 0.4942 0.0469 1.0000 Uiso R . . . . . H351 H 0.2677 0.2220 0.3434 0.0337 1.0000 Uiso R . . . . . H361 H 0.0977 0.0959 0.3629 0.0651 1.0000 Uiso R . . . . . H362 H 0.1533 0.0550 0.4250 0.0651 1.0000 Uiso R . . . . . H363 H 0.2180 0.0320 0.3539 0.0652 1.0000 Uiso R . . . . . H381 H 0.7138 0.8833 0.0262 0.0460 1.0000 Uiso R . . . . . H391 H 0.7607 1.0176 -0.0090 0.0590 1.0000 Uiso R . . . . . H401 H 0.7862 1.1545 0.0721 0.0530 1.0000 Uiso R . . . . . H411 H 0.7065 1.0330 0.2212 0.0372 1.0000 Uiso R . . . . . H421 H 0.7516 1.1850 0.2495 0.0801 1.0000 Uiso R . . . . . H422 H 0.8730 1.2303 0.2085 0.0802 1.0000 Uiso R . . . . . H423 H 0.6896 1.2237 0.1880 0.0802 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 0.01922(10) 0.01865(10) 0.01983(10) 0.00634(7) 0.00315(7) 0.00518(7) N1 0.0212(11) 0.0217(11) 0.0235(11) 0.0064(9) 0.0036(9) 0.0084(9) N2 0.0195(10) 0.0201(11) 0.0206(11) 0.0061(9) 0.0038(9) 0.0068(9) N3 0.0208(11) 0.0200(10) 0.0202(10) 0.0047(8) 0.0050(8) 0.0054(8) N4 0.0199(11) 0.0193(10) 0.0226(11) 0.0037(9) 0.0022(9) 0.0036(8) N5 0.0192(11) 0.0218(11) 0.0196(10) 0.0062(9) 0.0014(8) 0.0046(9) N6 0.0209(11) 0.0233(11) 0.0192(10) 0.0052(9) 0.0023(8) 0.0073(9) N7 0.0354(13) 0.0236(12) 0.0338(13) 0.0117(10) 0.0148(11) 0.0055(10) N8 0.0408(15) 0.0245(12) 0.0394(15) 0.0119(11) 0.0024(12) 0.0053(11) C1 0.0293(14) 0.0316(15) 0.0231(13) 0.0087(11) 0.0045(11) 0.0127(12) C2 0.0391(17) 0.0388(17) 0.0219(14) 0.0055(12) -0.0045(12) 0.0128(14) C3 0.0397(17) 0.0331(16) 0.0299(16) 0.0000(13) -0.0052(13) 0.0073(14) C4 0.0343(16) 0.0250(14) 0.0305(15) 0.0046(12) -0.0009(12) 0.0044(12) C5 0.0231(13) 0.0229(13) 0.0241(13) 0.0057(10) 0.0039(10) 0.0075(10) C6 0.0210(12) 0.0191(12) 0.0233(13) 0.0055(10) 0.0026(10) 0.0044(10) C7 0.0247(13) 0.0191(12) 0.0287(14) 0.0071(11) 0.0045(11) 0.0037(10) C8 0.0213(13) 0.0235(13) 0.0277(14) 0.0106(11) 0.0074(11) 0.0075(10) C9 0.0254(13) 0.0248(13) 0.0232(13) 0.0084(11) 0.0042(11) 0.0064(11) C10 0.0225(13) 0.0214(12) 0.0213(12) 0.0065(10) 0.0048(10) 0.0064(10) C11 0.0212(12) 0.0219(13) 0.0219(12) 0.0057(10) 0.0047(10) 0.0049(10) C12 0.0299(14) 0.0263(14) 0.0226(13) 0.0070(11) 0.0013(11) 0.0046(11) C13 0.0324(15) 0.0288(14) 0.0233(14) 0.0012(11) -0.0007(12) 0.0052(12) C14 0.0302(15) 0.0214(13) 0.0269(14) 0.0014(11) 0.0034(11) 0.0019(11) C15 0.0268(13) 0.0202(12) 0.0258(13) 0.0066(10) 0.0078(11) 0.0060(10) C16 0.0222(13) 0.0243(13) 0.0294(14) 0.0074(11) 0.0056(11) 0.0025(11) C17 0.0240(14) 0.0326(15) 0.0364(16) 0.0087(13) 0.0113(12) 0.0069(12) C18 0.0259(14) 0.0314(15) 0.0467(18) 0.0111(13) 0.0137(13) 0.0123(12) C19 0.0256(14) 0.0263(14) 0.0392(16) 0.0102(12) 0.0070(12) 0.0091(11) C20 0.0214(12) 0.0207(12) 0.0244(13) 0.0062(10) 0.0027(10) 0.0044(10) C21 0.0220(12) 0.0210(12) 0.0229(13) 0.0051(10) 0.0024(10) 0.0058(10) C22 0.0253(13) 0.0224(13) 0.0274(13) 0.0069(11) 0.0030(11) 0.0062(11) C23 0.0267(14) 0.0226(13) 0.0245(13) 0.0091(11) 0.0030(11) 0.0047(11) C24 0.0278(14) 0.0279(14) 0.0249(13) 0.0093(11) 0.0089(11) 0.0074(11) C25 0.0241(13) 0.0229(13) 0.0207(12) 0.0059(10) 0.0036(10) 0.0051(10) C26 0.0217(13) 0.0246(13) 0.0228(13) 0.0074(10) 0.0033(10) 0.0067(10) C27 0.0267(14) 0.0337(15) 0.0251(14) 0.0098(12) 0.0055(11) 0.0088(12) C28 0.0291(15) 0.0409(17) 0.0325(15) 0.0113(13) 0.0113(12) 0.0154(13) C29 0.0314(15) 0.0347(16) 0.0302(15) 0.0091(12) 0.0065(12) 0.0177(13) C30 0.0263(14) 0.0254(13) 0.0247(13) 0.0059(11) 0.0022(11) 0.0095(11) C31 0.0267(14) 0.0248(13) 0.0291(14) 0.0120(11) 0.0084(11) 0.0089(11) C32 0.0372(17) 0.0299(15) 0.0416(18) 0.0165(13) -0.0007(14) 0.0039(13) C33 0.051(2) 0.0415(19) 0.0452(19) 0.0242(16) -0.0039(16) 0.0082(16) C34 0.0496(19) 0.0316(16) 0.0410(18) 0.0206(14) 0.0132(15) 0.0136(14) C35 0.0305(14) 0.0262(14) 0.0275(14) 0.0100(11) 0.0093(11) 0.0062(11) C36 0.051(2) 0.0332(17) 0.0432(19) 0.0132(15) 0.0141(16) -0.0059(15) C37 0.0258(14) 0.0261(14) 0.0290(14) 0.0127(11) 0.0041(11) 0.0057(11) C38 0.0503(19) 0.0322(16) 0.0302(16) 0.0110(13) 0.0081(14) 0.0068(14) C39 0.073(3) 0.047(2) 0.0327(17) 0.0239(16) 0.0106(17) 0.0081(18) C40 0.057(2) 0.0328(17) 0.0447(19) 0.0245(15) 0.0047(16) 0.0041(15) C41 0.0363(16) 0.0271(14) 0.0290(15) 0.0110(12) 0.0055(12) 0.0059(12) C42 0.076(3) 0.0240(16) 0.061(2) 0.0088(16) 0.013(2) 0.0103(17) P1 0.0437(5) 0.0444(5) 0.0368(5) 0.0073(4) 0.0030(4) 0.0192(4) P2 0.0920(9) 0.0335(5) 0.0452(6) 0.0184(4) -0.0122(6) 0.0045(5) P3 0.0345(4) 0.0290(4) 0.0329(4) 0.0091(3) 0.0011(3) 0.0046(3) P4 0.0255(4) 0.0312(4) 0.0298(4) 0.0123(3) 0.0056(3) 0.0099(3) F41 0.0691(16) 0.0333(11) 0.0890(19) 0.0234(12) -0.0088(14) -0.0075(11) F42 0.0406(11) 0.0372(11) 0.0724(15) 0.0181(10) 0.0112(10) 0.0028(9) F43 0.0900(19) 0.0772(17) 0.0398(12) 0.0092(12) 0.0255(13) 0.0013(15) F44 0.108(2) 0.0679(17) 0.0760(18) 0.0123(14) 0.0509(17) 0.0380(16) F45 0.0496(13) 0.0512(13) 0.0611(14) 0.0178(11) -0.0127(11) 0.0099(10) F46 0.0571(16) 0.0688(17) 0.120(2) 0.0422(17) -0.0325(16) 0.0099(13) F51 0.0384(10) 0.0593(13) 0.0357(10) 0.0214(9) 0.0139(8) 0.0134(9) F52 0.0471(12) 0.0652(14) 0.0374(10) 0.0235(10) 0.0191(9) 0.0260(10) F53 0.0552(13) 0.0418(11) 0.0634(14) 0.0238(10) 0.0145(11) 0.0277(10) F54 0.0476(11) 0.0313(10) 0.0516(12) 0.0136(9) 0.0106(9) 0.0138(9) F55 0.0324(10) 0.0418(11) 0.0420(11) 0.0036(9) -0.0016(8) 0.0081(8) F56 0.0279(10) 0.0649(14) 0.0459(12) 0.0185(10) 0.0002(8) 0.0048(9) F1 0.0820(19) 0.094(2) 0.0617(16) -0.0086(14) 0.0021(14) 0.0556(16) F2 0.100(2) 0.185(4) 0.0660(19) -0.011(2) 0.0059(17) 0.100(2) F3 0.055(3) 0.159(6) 0.035(3) -0.011(4) -0.007(2) 0.036(4) F4 0.061(3) 0.131(6) 0.036(3) -0.003(3) -0.006(2) 0.042(4) F5 0.182(6) 0.086(4) 0.066(4) 0.011(4) 0.031(4) -0.046(5) F6 0.121(5) 0.064(4) 0.085(5) 0.026(3) 0.021(4) 0.004(4) F13 0.225(6) 0.059(4) 0.064(4) 0.031(3) 0.034(5) 0.052(4) F14 0.219(6) 0.076(4) 0.041(3) 0.024(3) 0.016(4) 0.037(5) F15 0.051(3) 0.137(6) 0.100(6) 0.001(4) -0.005(4) -0.028(4) F16 0.092(4) 0.081(5) 0.119(6) -0.055(4) -0.010(5) -0.007(4) F21 0.058(3) 0.066(3) 0.042(2) 0.008(2) -0.003(2) 0.035(2) F22 0.040(3) 0.077(4) 0.118(5) 0.039(4) -0.034(3) -0.005(3) F23 0.063(3) 0.037(2) 0.092(4) 0.034(3) -0.030(3) -0.006(2) F24 0.173(5) 0.039(3) 0.102(5) 0.028(3) -0.090(5) -0.014(4) F25 0.064(3) 0.138(6) 0.064(3) 0.036(4) 0.033(3) -0.012(4) F26 0.113(4) 0.188(6) 0.031(3) 0.028(3) 0.004(3) 0.049(5) F31 0.235(6) 0.067(4) 0.092(4) 0.011(3) 0.052(5) 0.062(4) F32 0.065(3) 0.081(4) 0.191(7) 0.012(5) 0.028(4) 0.041(3) F33 0.150(5) 0.037(3) 0.055(3) 0.023(2) -0.017(3) 0.003(3) F34 0.247(6) 0.057(4) 0.103(5) 0.042(4) -0.114(5) -0.035(5) F35 0.130(5) 0.074(4) 0.056(3) 0.024(3) 0.021(3) -0.018(4) F36 0.087(5) 0.107(6) 0.200(7) 0.052(5) -0.008(5) -0.051(5) O1 0.137(6) 0.109(6) 0.155(7) 0.023(6) 0.069(6) 0.005(5) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2166(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 . N1 . 2.075(2) yes Ru1 . N2 . 1.975(2) yes Ru1 . N3 . 2.076(2) yes Ru1 . N4 . 2.083(2) yes Ru1 . N5 . 1.986(2) yes Ru1 . N6 . 2.076(2) yes N1 . C1 . 1.346(4) yes N1 . C5 . 1.369(3) yes N2 . C6 . 1.356(3) yes N2 . C10 . 1.353(3) yes N3 . C11 . 1.374(3) yes N3 . C15 . 1.347(3) yes N4 . C16 . 1.347(4) yes N4 . C20 . 1.365(3) yes N5 . C21 . 1.354(3) yes N5 . C25 . 1.347(3) yes N6 . C26 . 1.368(3) yes N6 . C30 . 1.345(3) yes N7 . C34 . 1.338(4) yes N7 . C35 . 1.346(4) yes N7 . C36 . 1.481(4) yes N8 . C40 . 1.336(4) yes N8 . C41 . 1.341(4) yes N8 . C42 . 1.482(4) yes C1 . C2 . 1.382(4) yes C1 . H11 . 0.934 no C2 . C3 . 1.378(5) yes C2 . H21 . 0.928 no C3 . C4 . 1.382(4) yes C3 . H31 . 0.921 no C4 . C5 . 1.391(4) yes C4 . H41 . 0.931 no C5 . C6 . 1.469(4) yes C6 . C7 . 1.385(4) yes C7 . C8 . 1.398(4) yes C7 . H71 . 0.935 no C8 . C9 . 1.397(4) yes C8 . C31 . 1.487(4) yes C9 . C10 . 1.381(4) yes C9 . H91 . 0.933 no C10 . C11 . 1.469(4) yes C11 . C12 . 1.382(4) yes C12 . C13 . 1.388(4) yes C12 . H121 . 0.934 no C13 . C14 . 1.385(4) yes C13 . H131 . 0.936 no C14 . C15 . 1.382(4) yes C14 . H141 . 0.933 no C15 . H151 . 0.930 no C16 . C17 . 1.385(4) yes C16 . H161 . 0.927 no C17 . C18 . 1.385(4) yes C17 . H171 . 0.937 no C18 . C19 . 1.383(4) yes C18 . H181 . 0.933 no C19 . C20 . 1.388(4) yes C19 . H191 . 0.936 no C20 . C21 . 1.466(4) yes C21 . C22 . 1.383(4) yes C22 . C23 . 1.388(4) yes C22 . H221 . 0.933 no C23 . C24 . 1.398(4) yes C23 . C37 . 1.481(4) yes C24 . C25 . 1.385(4) yes C24 . H241 . 0.925 no C25 . C26 . 1.479(4) yes C26 . C27 . 1.388(4) yes C27 . C28 . 1.381(4) yes C27 . H271 . 0.924 no C28 . C29 . 1.380(4) yes C28 . H281 . 0.931 no C29 . C30 . 1.381(4) yes C29 . H291 . 0.934 no C30 . H301 . 0.935 no C31 . C32 . 1.392(4) yes C31 . C35 . 1.381(4) yes C32 . C33 . 1.382(4) yes C32 . H321 . 0.935 no C33 . C34 . 1.369(5) yes C33 . H331 . 0.936 no C34 . H341 . 0.932 no C35 . H351 . 0.928 no C36 . H361 . 0.961 no C36 . H362 . 0.959 no C36 . H363 . 0.957 no C37 . C38 . 1.391(4) yes C37 . C41 . 1.378(4) yes C38 . C39 . 1.381(5) yes C38 . H381 . 0.936 no C39 . C40 . 1.366(5) yes C39 . H391 . 0.927 no C40 . H401 . 0.917 no C41 . H411 . 0.932 no C42 . H421 . 0.952 no C42 . H422 . 0.950 no C42 . H423 . 0.949 no P1 . F1 . 1.574(2) yes P1 . F2 . 1.578(3) yes P1 . F3 . 1.544(5) yes P1 . F4 . 1.585(4) yes P1 . F5 . 1.559(5) yes P1 . F6 . 1.578(5) yes P1 . F13 . 1.564(5) yes P1 . F14 . 1.561(5) yes P1 . F15 . 1.566(5) yes P1 . F16 . 1.566(5) yes P2 . F21 . 1.683(4) yes P2 . F22 . 1.473(4) yes P2 . F23 . 1.592(4) yes P2 . F24 . 1.539(4) yes P2 . F25 . 1.545(5) yes P2 . F26 . 1.601(5) yes P2 . F31 . 1.680(5) yes P2 . F32 . 1.488(5) yes P2 . F33 . 1.610(5) yes P2 . F34 . 1.520(5) yes P2 . F35 . 1.710(5) yes P2 . F36 . 1.444(5) yes P3 . F41 . 1.580(2) yes P3 . F42 . 1.600(2) yes P3 . F43 . 1.588(3) yes P3 . F44 . 1.594(3) yes P3 . F45 . 1.593(2) yes P3 . F46 . 1.573(2) yes P4 . F51 . 1.594(2) yes P4 . F52 . 1.599(2) yes P4 . F53 . 1.597(2) yes P4 . F54 . 1.598(2) yes P4 . F55 . 1.600(2) yes P4 . F56 . 1.609(2) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Ru1 . N2 . 78.44(9) yes N1 . Ru1 . N3 . 157.46(9) yes N2 . Ru1 . N3 . 79.10(9) yes N1 . Ru1 . N4 . 94.90(8) yes N2 . Ru1 . N4 . 100.86(9) yes N3 . Ru1 . N4 . 91.13(8) yes N1 . Ru1 . N5 . 103.61(9) yes N2 . Ru1 . N5 . 177.93(9) yes N3 . Ru1 . N5 . 98.86(9) yes N4 . Ru1 . N5 . 78.74(9) yes N1 . Ru1 . N6 . 88.99(9) yes N2 . Ru1 . N6 . 101.78(9) yes N3 . Ru1 . N6 . 93.76(8) yes N4 . Ru1 . N6 . 157.35(9) yes N5 . Ru1 . N6 . 78.66(9) yes Ru1 . N1 . C1 . 127.29(19) yes Ru1 . N1 . C5 . 114.28(17) yes C1 . N1 . C5 . 118.4(2) yes Ru1 . N2 . C6 . 119.98(18) yes Ru1 . N2 . C10 . 119.09(18) yes C6 . N2 . C10 . 120.9(2) yes Ru1 . N3 . C11 . 113.65(17) yes Ru1 . N3 . C15 . 128.56(18) yes C11 . N3 . C15 . 117.7(2) yes Ru1 . N4 . C16 . 127.89(19) yes Ru1 . N4 . C20 . 113.66(17) yes C16 . N4 . C20 . 118.4(2) yes Ru1 . N5 . C21 . 118.92(18) yes Ru1 . N5 . C25 . 119.53(18) yes C21 . N5 . C25 . 121.4(2) yes Ru1 . N6 . C26 . 114.09(17) yes Ru1 . N6 . C30 . 127.54(19) yes C26 . N6 . C30 . 118.3(2) yes C34 . N7 . C35 . 121.6(3) yes C34 . N7 . C36 . 118.6(3) yes C35 . N7 . C36 . 119.8(3) yes C40 . N8 . C41 . 121.1(3) yes C40 . N8 . C42 . 119.9(3) yes C41 . N8 . C42 . 119.0(3) yes N1 . C1 . C2 . 122.4(3) yes N1 . C1 . H11 . 117.9 no C2 . C1 . H11 . 119.7 no C1 . C2 . C3 . 119.2(3) yes C1 . C2 . H21 . 120.4 no C3 . C2 . H21 . 120.4 no C2 . C3 . C4 . 119.4(3) yes C2 . C3 . H31 . 120.5 no C4 . C3 . H31 . 120.1 no C3 . C4 . C5 . 119.3(3) yes C3 . C4 . H41 . 120.6 no C5 . C4 . H41 . 120.1 no C4 . C5 . N1 . 121.2(3) yes C4 . C5 . C6 . 123.7(3) yes N1 . C5 . C6 . 115.1(2) yes C5 . C6 . N2 . 112.2(2) yes C5 . C6 . C7 . 127.4(3) yes N2 . C6 . C7 . 120.4(2) yes C6 . C7 . C8 . 119.7(3) yes C6 . C7 . H71 . 120.1 no C8 . C7 . H71 . 120.2 no C7 . C8 . C9 . 118.6(2) yes C7 . C8 . C31 . 121.5(3) yes C9 . C8 . C31 . 119.9(3) yes C8 . C9 . C10 . 119.7(3) yes C8 . C9 . H91 . 120.4 no C10 . C9 . H91 . 119.9 no C9 . C10 . N2 . 120.6(2) yes C9 . C10 . C11 . 126.3(2) yes N2 . C10 . C11 . 113.0(2) yes C10 . C11 . N3 . 115.0(2) yes C10 . C11 . C12 . 123.2(2) yes N3 . C11 . C12 . 121.8(2) yes C11 . C12 . C13 . 119.6(3) yes C11 . C12 . H121 . 119.8 no C13 . C12 . H121 . 120.6 no C12 . C13 . C14 . 118.8(3) yes C12 . C13 . H131 . 120.4 no C14 . C13 . H131 . 120.8 no C13 . C14 . C15 . 119.2(3) yes C13 . C14 . H141 . 120.2 no C15 . C14 . H141 . 120.6 no C14 . C15 . N3 . 122.9(3) yes C14 . C15 . H151 . 119.3 no N3 . C15 . H151 . 117.9 no N4 . C16 . C17 . 122.2(3) yes N4 . C16 . H161 . 118.6 no C17 . C16 . H161 . 119.2 no C16 . C17 . C18 . 119.2(3) yes C16 . C17 . H171 . 120.3 no C18 . C17 . H171 . 120.5 no C17 . C18 . C19 . 119.3(3) yes C17 . C18 . H181 . 120.0 no C19 . C18 . H181 . 120.7 no C18 . C19 . C20 . 119.1(3) yes C18 . C19 . H191 . 121.0 no C20 . C19 . H191 . 120.0 no C19 . C20 . N4 . 121.8(3) yes C19 . C20 . C21 . 122.6(2) yes N4 . C20 . C21 . 115.6(2) yes C20 . C21 . N5 . 112.9(2) yes C20 . C21 . C22 . 126.8(2) yes N5 . C21 . C22 . 120.3(2) yes C21 . C22 . C23 . 119.2(3) yes C21 . C22 . H221 . 120.0 no C23 . C22 . H221 . 120.8 no C22 . C23 . C24 . 119.7(3) yes C22 . C23 . C37 . 119.3(3) yes C24 . C23 . C37 . 120.9(3) yes C23 . C24 . C25 . 118.9(3) yes C23 . C24 . H241 . 120.8 no C25 . C24 . H241 . 120.4 no C24 . C25 . N5 . 120.5(2) yes C24 . C25 . C26 . 127.1(3) yes N5 . C25 . C26 . 112.4(2) yes C25 . C26 . N6 . 115.2(2) yes C25 . C26 . C27 . 123.2(2) yes N6 . C26 . C27 . 121.6(2) yes C26 . C27 . C28 . 119.0(3) yes C26 . C27 . H271 . 119.7 no C28 . C27 . H271 . 121.3 no C27 . C28 . C29 . 119.5(3) yes C27 . C28 . H281 . 119.7 no C29 . C28 . H281 . 120.8 no C28 . C29 . C30 . 119.1(3) yes C28 . C29 . H291 . 120.5 no C30 . C29 . H291 . 120.4 no C29 . C30 . N6 . 122.4(3) yes C29 . C30 . H301 . 119.9 no N6 . C30 . H301 . 117.6 no C8 . C31 . C32 . 121.6(3) yes C8 . C31 . C35 . 120.4(3) yes C32 . C31 . C35 . 118.0(3) yes C31 . C32 . C33 . 119.4(3) yes C31 . C32 . H321 . 120.6 no C33 . C32 . H321 . 120.0 no C32 . C33 . C34 . 120.5(3) yes C32 . C33 . H331 . 120.5 no C34 . C33 . H331 . 119.0 no C33 . C34 . N7 . 119.5(3) yes C33 . C34 . H341 . 120.9 no N7 . C34 . H341 . 119.6 no C31 . C35 . N7 . 121.0(3) yes C31 . C35 . H351 . 120.2 no N7 . C35 . H351 . 118.8 no N7 . C36 . H361 . 109.5 no N7 . C36 . H362 . 110.0 no H361 . C36 . H362 . 109.7 no N7 . C36 . H363 . 108.7 no H361 . C36 . H363 . 109.5 no H362 . C36 . H363 . 109.5 no C23 . C37 . C38 . 122.7(3) yes C23 . C37 . C41 . 118.8(3) yes C38 . C37 . C41 . 118.5(3) yes C37 . C38 . C39 . 119.0(3) yes C37 . C38 . H381 . 120.2 no C39 . C38 . H381 . 120.8 no C38 . C39 . C40 . 120.1(3) yes C38 . C39 . H391 . 120.0 no C40 . C39 . H391 . 119.9 no C39 . C40 . N8 . 120.3(3) yes C39 . C40 . H401 . 120.4 no N8 . C40 . H401 . 119.3 no C37 . C41 . N8 . 121.0(3) yes C37 . C41 . H411 . 120.3 no N8 . C41 . H411 . 118.8 no N8 . C42 . H421 . 110.1 no N8 . C42 . H422 . 108.9 no H421 . C42 . H422 . 109.7 no N8 . C42 . H423 . 109.5 no H421 . C42 . H423 . 109.5 no H422 . C42 . H423 . 109.1 no F1 . P1 . F2 . 178.02(19) yes F1 . P1 . F3 . 91.4(2) yes F2 . P1 . F3 . 90.0(2) yes F1 . P1 . F4 . 90.4(2) yes F2 . P1 . F4 . 88.2(2) yes F3 . P1 . F4 . 178.1(3) yes F1 . P1 . F5 . 93.9(3) yes F2 . P1 . F5 . 87.5(3) yes F3 . P1 . F5 . 91.7(4) yes F4 . P1 . F5 . 88.8(3) yes F1 . P1 . F6 . 85.8(3) yes F2 . P1 . F6 . 92.8(3) yes F3 . P1 . F6 . 90.9(3) yes F4 . P1 . F6 . 88.6(3) yes F5 . P1 . F6 . 177.4(4) yes F1 . P1 . F13 . 91.6(3) yes F2 . P1 . F13 . 88.0(3) yes F1 . P1 . F14 . 87.0(3) yes F2 . P1 . F14 . 93.5(3) yes F1 . P1 . F15 . 87.4(3) yes F2 . P1 . F15 . 94.5(3) yes F1 . P1 . F16 . 91.7(3) yes F2 . P1 . F16 . 86.3(3) yes F13 . P1 . F14 . 178.2(3) yes F13 . P1 . F15 . 88.8(4) yes F14 . P1 . F15 . 89.9(4) yes F13 . P1 . F16 . 90.7(4) yes F14 . P1 . F16 . 90.6(4) yes F15 . P1 . F16 . 179.0(4) yes F21 . P2 . F22 . 175.5(3) yes F21 . P2 . F23 . 84.6(2) yes F22 . P2 . F23 . 92.7(3) yes F21 . P2 . F24 . 86.7(3) yes F22 . P2 . F24 . 96.0(3) yes F23 . P2 . F24 . 171.2(3) yes F21 . P2 . F25 . 84.9(3) yes F22 . P2 . F25 . 98.5(4) yes F23 . P2 . F25 . 87.8(3) yes F24 . P2 . F25 . 91.6(4) yes F21 . P2 . F26 . 85.4(3) yes F22 . P2 . F26 . 91.0(3) yes F23 . P2 . F26 . 89.1(3) yes F24 . P2 . F26 . 90.0(4) yes F25 . P2 . F26 . 170.1(3) yes F31 . P2 . F32 . 165.0(4) yes F31 . P2 . F33 . 82.0(3) yes F32 . P2 . F33 . 90.9(3) yes F31 . P2 . F34 . 86.7(4) yes F32 . P2 . F34 . 97.5(4) yes F33 . P2 . F34 . 164.2(5) yes F31 . P2 . F35 . 81.5(3) yes F32 . P2 . F35 . 84.5(3) yes F33 . P2 . F35 . 82.2(3) yes F34 . P2 . F35 . 85.3(3) yes F31 . P2 . F36 . 90.3(4) yes F32 . P2 . F36 . 103.2(4) yes F33 . P2 . F36 . 91.7(4) yes F34 . P2 . F36 . 99.3(4) yes F35 . P2 . F36 . 170.3(4) yes F41 . P3 . F42 . 179.33(14) yes F41 . P3 . F43 . 90.92(15) yes F42 . P3 . F43 . 89.45(14) yes F41 . P3 . F44 . 90.48(16) yes F42 . P3 . F44 . 89.12(14) yes F43 . P3 . F44 . 176.42(17) yes F41 . P3 . F45 . 89.86(13) yes F42 . P3 . F45 . 89.59(12) yes F43 . P3 . F45 . 88.58(15) yes F44 . P3 . F45 . 88.12(16) yes F41 . P3 . F46 . 90.12(14) yes F42 . P3 . F46 . 90.43(14) yes F43 . P3 . F46 . 91.85(18) yes F44 . P3 . F46 . 91.45(19) yes F45 . P3 . F46 . 179.57(18) yes F51 . P4 . F52 . 179.70(12) yes F51 . P4 . F53 . 89.97(12) yes F52 . P4 . F53 . 90.06(12) yes F51 . P4 . F54 . 90.09(11) yes F52 . P4 . F54 . 89.88(11) yes F53 . P4 . F54 . 179.44(12) yes F51 . P4 . F55 . 90.42(11) yes F52 . P4 . F55 . 89.88(11) yes F53 . P4 . F55 . 90.86(12) yes F54 . P4 . F55 . 89.70(11) yes F51 . P4 . F56 . 89.97(11) yes F52 . P4 . F56 . 89.73(12) yes F53 . P4 . F56 . 89.74(12) yes F54 . P4 . F56 . 89.70(12) yes F55 . P4 . F56 . 179.29(12) yes