Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global #=========================================================================== # 1. SUBMISSION DETAILS _publ_contact_autor ; Prof R W Saalfrank Institut fur Organische Chemie Universitat Erlangen-Nurnberg Henkestr. 42 D-91054 Erlangen GERMANY ; _publ_contact_author_phone '049 9131 852-22554' _publ_contact_author_fax '049 9131 852-21165' _publ_contact_author_email 'SAALFRNK@ORGANIK.UNI-ERLANGEN.DE' _publ_requested_journal 'J. Chem. Soc. Dalton Trans.' _journal_coden_Cambridge 186 _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission as supplementary material. ; #=========================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; Metal- and ligand control in di- and octanuclear cluster formation ; loop_ _publ_author_name _publ_author_address 'Saalfrank, R. W.' ; Institut f\"ur Organische Chemie Universit\"at Erlangen-N\"urnberg Henkestr. 42 D-91054 Erlangen Bundesrepublik Deutschland ; 'Seitz, V.' ; Institut f\"ur Organische Chemie Universit\"at Erlangen-N\"urnberg Henkestr. 42 D-91054 Erlangen Bundesrepublik Deutschland ; 'Heinemann, F. W.' ; Institut f\"ur Anorganische Chemie II Universit\"at Erlangen-N\"urnberg Egerlandstr. 1 D-91058 Erlangen Bundesrepublik Deutschland ; 'G\"obel, C.' ; Institut f\"ur Anorganische Chemie Universit\"at G\"ottingen Tammannstr. 4 D-37077 G\"ottingen Bundesrepublik Deutschland ; 'Herbst-Irmer, R.' ; Institut f\"ur Anorganische Chemie Universit\"at G\"ottingen Tammannstr. 4 D-37077 G\"ottingen Bundesrepublik Deutschland ; #=========================================================================== # 3. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_experimental ; source of material: see actual publication ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #=========================================================================== # 4.1 RESULTS FOR K-4c data_rs9909 _database_code_CSD 152453 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H39 Cl6 F6 Fe2 K N3 O12 P S6' _chemical_formula_weight 1694.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.114(3) _cell_length_b 17.853(3) _cell_length_c 31.886(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.55(1) _cell_angle_gamma 90.00 _cell_volume 6779(2) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 61 _cell_measurement_theta_min 7.10 _cell_measurement_theta_max 11.45 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.90 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.660 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3416 _exptl_absorpt_coefficient_mu 1.013 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.4112 _exptl_absorpt_correction_T_max 0.5696 _exptl_absorpt_process_details ; North A C T, Phillips D C, Mathews F S, Acta Cryst. A24 (1968), 351-359. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 'Siemens P4' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16301 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0970 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 26.00 _reflns_number_total 13310 _reflns_number_gt 7582 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCAnS 2.20 (Siemens An. X-Ray Instr.,1996)' _computing_cell_refinement 'XSCAnS 2.20 (Siemens An. X-Ray Instr.,1996)' _computing_data_reduction 'XSCAnS 2.20 (Siemens An. X-Ray Instr.,1996)' _computing_structure_solution 'SHELXTL 5.1 (Bruker AXS, 1998)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS, 1998)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS, 1998)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS, 1998)' _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. One thiophene group (S4 C35 C36 C37 C38) is disordered where S4 and C36 interchange their positions with s.o.f.'s of 0.594(6) and 0.406(6), respectively, for the alternative sites. ; _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^)+(0.0890P)^2^+0.8350P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13310 _refine_ls_number_parameters 875 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1383 _refine_ls_R_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.1889 _refine_ls_wR_factor_gt 0.1544 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 K1 K 0.00992(11) 0.17792(8) 0.42276(4) 0.0326(3) Uani 1 1 d . . . Fe1 Fe -0.14529(7) 0.28253(5) 0.48510(2) 0.0266(2) Uani 1 1 d . . . Fe2 Fe 0.15735(7) 0.07209(5) 0.35881(2) 0.0298(2) Uani 1 1 d . . . S1 S -0.38627(17) 0.49321(11) 0.46820(5) 0.0508(5) Uani 1 1 d . . . S2 S -0.07419(17) -0.12657(13) 0.22994(6) 0.0608(6) Uani 1 1 d . . . S3 S -0.36800(16) 0.26823(12) 0.58751(6) 0.0545(5) Uani 1 1 d . . . S4 S 0.5368(2) -0.08867(16) 0.44532(9) 0.0492(9) Uani 0.594(6) 1 d P A 1 S4A S 0.5241(3) -0.0277(2) 0.36775(11) 0.0590(12) Uani 0.406(6) 1 d P A 2 S5 S -0.04276(18) 0.42486(11) 0.61398(6) 0.0531(5) Uani 1 1 d . . . S6 S 0.2698(2) 0.09015(12) 0.22556(6) 0.0624(6) Uani 1 1 d . . . N1 N -0.1945(4) 0.1586(3) 0.35697(14) 0.0316(11) Uani 1 1 d . . . N2 N 0.0948(4) 0.0830(3) 0.49592(14) 0.0275(10) Uani 1 1 d . . . N3 N 0.1449(4) 0.3071(3) 0.41246(14) 0.0275(10) Uani 1 1 d . . . O1 O -0.2089(3) 0.2267(2) 0.43117(11) 0.0301(9) Uani 1 1 d . . . O2 O -0.2659(3) 0.3571(2) 0.46583(12) 0.0340(10) Uani 1 1 d . . . O3 O -0.0068(3) 0.0948(2) 0.35024(12) 0.0366(10) Uani 1 1 d . . . O4 O 0.1070(3) -0.0196(2) 0.32564(12) 0.0354(10) Uani 1 1 d . . . O5 O -0.0448(3) 0.1936(2) 0.50015(11) 0.0297(9) Uani 1 1 d . . . O6 O -0.2321(3) 0.2408(2) 0.52650(11) 0.0305(9) Uani 1 1 d . . . O7 O 0.1392(3) 0.0496(2) 0.41857(11) 0.0307(9) Uani 1 1 d . . . O8 O 0.3095(3) 0.0299(2) 0.37566(13) 0.0366(10) Uani 1 1 d . . . O9 O -0.0297(3) 0.3205(2) 0.45347(11) 0.0293(9) Uani 1 1 d . . . O10 O -0.0778(3) 0.3525(2) 0.53184(12) 0.0339(9) Uani 1 1 d . . . O11 O 0.1807(4) 0.1777(2) 0.37831(12) 0.0353(10) Uani 1 1 d . . . O12 O 0.1994(4) 0.1088(2) 0.30491(12) 0.0380(10) Uani 1 1 d . . . C1 C -0.2000(5) 0.1092(3) 0.32499(18) 0.0316(13) Uani 1 1 d . . . C2 C -0.2989(6) 0.0961(4) 0.2954(2) 0.0472(18) Uani 1 1 d . . . H2A H -0.3015 0.0596 0.2744 0.057 Uiso 1 1 calc R . . C3 C -0.3920(6) 0.1384(4) 0.2982(2) 0.056(2) Uani 1 1 d . . . H3A H -0.4581 0.1315 0.2786 0.067 Uiso 1 1 calc R . . C4 C -0.3877(6) 0.1912(4) 0.3302(2) 0.0495(18) Uani 1 1 d . . . H4A H -0.4497 0.2209 0.3320 0.059 Uiso 1 1 calc R . . C5 C -0.2875(5) 0.1987(3) 0.35973(18) 0.0314(13) Uani 1 1 d . . . C6 C -0.2731(5) 0.2506(3) 0.39751(17) 0.0290(13) Uani 1 1 d . . . C7 C -0.3298(5) 0.3188(3) 0.39414(18) 0.0336(14) Uani 1 1 d . . . H7A H -0.3739 0.3315 0.3681 0.040 Uiso 1 1 calc R . . C8 C -0.3236(5) 0.3694(3) 0.42823(18) 0.0305(13) Uani 1 1 d . . . C9 C -0.3835(5) 0.4409(3) 0.42343(18) 0.0320(13) Uani 1 1 d . . . C10 C -0.4378(5) 0.4768(4) 0.3879(2) 0.0378(15) Uani 1 1 d . . . H10A H -0.4463 0.4567 0.3606 0.045 Uiso 1 1 calc R . . C11 C -0.4797(5) 0.5473(4) 0.3966(2) 0.0431(16) Uani 1 1 d . . . H11A H -0.5172 0.5794 0.3757 0.052 Uiso 1 1 calc R . . C12 C -0.4592(6) 0.5628(4) 0.4385(3) 0.056(2) Uani 1 1 d . . . H12 H -0.4822 0.6067 0.4500 0.067 Uiso 1 1 calc R . . C13 C -0.0906(5) 0.0685(3) 0.32438(17) 0.0302(13) Uani 1 1 d . . . C14 C -0.0833(5) 0.0092(3) 0.29681(18) 0.0354(14) Uani 1 1 d . . . H14A H -0.1471 -0.0055 0.2777 0.042 Uiso 1 1 calc R . . C15 C 0.0189(5) -0.0294(3) 0.29713(18) 0.0319(13) Uani 1 1 d . . . C16 C 0.0339(5) -0.0830(3) 0.26367(19) 0.0358(14) Uani 1 1 d . . . C17 C 0.1417(5) -0.1056(3) 0.25526(17) 0.0284(12) Uani 1 1 d . . . H17 H 0.2108 -0.0895 0.2702 0.034 Uiso 1 1 calc R . . C18 C 0.1250(7) -0.1569(4) 0.2200(2) 0.0507(18) Uani 1 1 d . . . H18A H 0.1838 -0.1777 0.2089 0.061 Uiso 1 1 calc R . . C19 C 0.0158(7) -0.1722(5) 0.2046(2) 0.058(2) Uani 1 1 d . . . H19 H -0.0074 -0.2050 0.1821 0.069 Uiso 1 1 calc R . . C20 C 0.1702(4) 0.0290(3) 0.49285(16) 0.0265(12) Uani 1 1 d . . . C21 C 0.2057(5) -0.0227(3) 0.52548(18) 0.0311(13) Uani 1 1 d . . . H21A H 0.2587 -0.0591 0.5226 0.037 Uiso 1 1 calc R . . C22 C 0.1604(5) -0.0183(3) 0.56176(18) 0.0330(14) Uani 1 1 d . . . H22A H 0.1819 -0.0524 0.5838 0.040 Uiso 1 1 calc R . . C23 C 0.0822(5) 0.0370(3) 0.56561(17) 0.0289(12) Uani 1 1 d . . . H23A H 0.0504 0.0403 0.5900 0.035 Uiso 1 1 calc R . . C24 C 0.0523(4) 0.0876(3) 0.53186(16) 0.0237(11) Uani 1 1 d . . . C25 C -0.0357(4) 0.1476(3) 0.53116(16) 0.0251(12) Uani 1 1 d . . . C26 C -0.1033(5) 0.1512(3) 0.56240(16) 0.0285(13) Uani 1 1 d . . . H26A H -0.0857 0.1207 0.5863 0.034 Uiso 1 1 calc R . . C27 C -0.1957(5) 0.1987(3) 0.55887(17) 0.0267(12) Uani 1 1 d . . . C28 C -0.2625(5) 0.2024(3) 0.59265(17) 0.0301(13) Uani 1 1 d . . . C29 C -0.2573(5) 0.1614(4) 0.62995(18) 0.0350(14) Uani 1 1 d . . . H29A H -0.2045 0.1242 0.6389 0.042 Uiso 1 1 calc R . . C30 C -0.3413(6) 0.1828(4) 0.6526(2) 0.0464(17) Uani 1 1 d . . . H30A H -0.3518 0.1602 0.6779 0.056 Uiso 1 1 calc R . . C31 C -0.4056(6) 0.2400(5) 0.6338(2) 0.060(2) Uani 1 1 d . . . H31 H -0.4638 0.2615 0.6450 0.072 Uiso 1 1 calc R . . C32 C 0.2103(5) 0.0262(3) 0.45088(17) 0.0254(12) Uani 1 1 d . . . C33 C 0.3172(5) 0.0005(4) 0.44878(18) 0.0340(14) Uani 1 1 d . . . H33A H 0.3623 -0.0175 0.4735 0.041 Uiso 1 1 calc R . . C34 C 0.3596(5) 0.0005(3) 0.41054(18) 0.0316(13) Uani 1 1 d . A . C35 C 0.4685(5) -0.0345(4) 0.4088(2) 0.0389(15) Uani 1 1 d . . . C36 C 0.5241(3) -0.0277(2) 0.36775(11) 0.0590(12) Uani 0.594(6) 1 d P A 1 H36 H 0.5035 0.0008 0.3432 0.071 Uiso 0.594(6) 1 calc PR A 1 C36A C 0.5368(2) -0.08867(16) 0.44532(9) 0.0492(9) Uani 0.41 1 d P A 2 H36A H 0.5247 -0.1014 0.4724 0.059 Uiso 0.406(6) 1 calc PR A 2 C37 C 0.6314(6) -0.1128(5) 0.4195(3) 0.068(2) Uani 1 1 d . . . H37 H 0.6889 -0.1458 0.4304 0.081 Uiso 1 1 calc R A 1 C38 C 0.6217(7) -0.0818(5) 0.3806(3) 0.068(2) Uani 1 1 d . A . H38 H 0.6718 -0.0927 0.3626 0.082 Uiso 1 1 calc R B 1 C39 C 0.2205(5) 0.3067(3) 0.38629(18) 0.0311(13) Uani 1 1 d . . . C40 C 0.2900(5) 0.3662(4) 0.3828(2) 0.0393(15) Uani 1 1 d . . . H40A H 0.3414 0.3638 0.3644 0.047 Uiso 1 1 calc R . . C41 C 0.2828(6) 0.4294(4) 0.4066(2) 0.0513(19) Uani 1 1 d . . . H41A H 0.3281 0.4706 0.4042 0.062 Uiso 1 1 calc R . . C42 C 0.2069(5) 0.4311(4) 0.43469(19) 0.0394(15) Uani 1 1 d . . . H42A H 0.2014 0.4730 0.4516 0.047 Uiso 1 1 calc R . . C43 C 0.1391(5) 0.3682(3) 0.43668(16) 0.0296(13) Uani 1 1 d . . . C44 C 0.0547(5) 0.3639(3) 0.46584(17) 0.0285(13) Uani 1 1 d . . . C45 C 0.0744(5) 0.4034(3) 0.50390(18) 0.0343(14) Uani 1 1 d . . . H45A H 0.1354 0.4358 0.5092 0.041 Uiso 1 1 calc R . . C46 C 0.0058(5) 0.3962(3) 0.53479(18) 0.0317(13) Uani 1 1 d . . . C47 C 0.0315(5) 0.4405(3) 0.57414(18) 0.0357(14) Uani 1 1 d . . . C48 C 0.1174(6) 0.4963(3) 0.58606(18) 0.0446(17) Uani 1 1 d . . . H48 H 0.1690 0.5115 0.5695 0.053 Uiso 1 1 calc R . . C49 C 0.1108(7) 0.5242(5) 0.6271(2) 0.063(2) Uani 1 1 d . . . H49A H 0.1577 0.5617 0.6405 0.076 Uiso 1 1 calc R . . C50 C 0.0296(7) 0.4911(4) 0.6452(2) 0.0536(19) Uani 1 1 d . . . H50 H 0.0156 0.5038 0.6721 0.064 Uiso 1 1 calc R . . C51 C 0.2213(5) 0.2343(3) 0.36185(18) 0.0325(14) Uani 1 1 d . . . C52 C 0.2594(5) 0.2326(4) 0.32319(18) 0.0342(14) Uani 1 1 d . . . H52A H 0.2950 0.2746 0.3147 0.041 Uiso 1 1 calc R . . C53 C 0.2456(5) 0.1695(3) 0.29676(17) 0.0290(13) Uani 1 1 d . . . C54 C 0.2831(5) 0.1700(4) 0.25560(19) 0.0380(15) Uani 1 1 d . . . C55 C 0.3283(6) 0.2271(5) 0.2358(2) 0.0538(19) Uani 1 1 d . . . H55A H 0.3401 0.2751 0.2471 0.065 Uiso 1 1 calc R . . C56 C 0.3553(7) 0.2051(6) 0.1961(2) 0.065(2) Uani 1 1 d . . . H56A H 0.3880 0.2363 0.1785 0.079 Uiso 1 1 calc R . . C57 C 0.3279(8) 0.1343(6) 0.1875(2) 0.075(3) Uani 1 1 d . . . H57 H 0.3394 0.1105 0.1627 0.090 Uiso 1 1 calc R . . C58 C 0.0987(7) 0.2534(5) 0.6325(3) 0.073(3) Uani 1 1 d . . . H58A H 0.1203 0.2924 0.6536 0.087 Uiso 1 1 calc R . . H58B H 0.0195 0.2596 0.6208 0.087 Uiso 1 1 calc R . . Cl1 Cl 0.1762(2) 0.26367(14) 0.59158(7) 0.0800(7) Uani 1 1 d . . . Cl2 Cl 0.1195(2) 0.16654(14) 0.65719(7) 0.0808(7) Uani 1 1 d . . . C59 C -0.4965(9) -0.2449(7) 0.5312(3) 0.111(4) Uani 1 1 d . . . H59A H -0.5605 -0.2460 0.5080 0.133 Uiso 1 1 calc R . . H59B H -0.5024 -0.2877 0.5494 0.133 Uiso 1 1 calc R . . Cl3 Cl -0.5029(3) -0.1645(2) 0.56024(12) 0.1306(13) Uani 1 1 d . . . Cl4 Cl -0.3737(2) -0.2537(2) 0.51010(9) 0.1130(11) Uani 1 1 d . . . C60 C -0.1636(9) 0.3266(6) 0.7016(4) 0.100(3) Uani 1 1 d . . . H60A H -0.1997 0.3001 0.7219 0.120 Uiso 1 1 calc R . . H60B H -0.1691 0.2956 0.6763 0.120 Uiso 1 1 calc R . . Cl5 Cl -0.2351(2) 0.41037(19) 0.68779(8) 0.0996(9) Uani 1 1 d . . . Cl6 Cl -0.0242(2) 0.33926(17) 0.72341(9) 0.0953(8) Uani 1 1 d . . . P1 P 0.4964(2) -0.08611(13) 0.23622(6) 0.0649(6) Uani 1 1 d . . . F11 F 0.4455(7) -0.0397(4) 0.27062(15) 0.141(3) Uani 1 1 d . . . F12 F 0.5326(5) -0.0110(3) 0.21622(18) 0.0985(19) Uani 1 1 d . . . F13 F 0.5434(4) -0.1339(3) 0.20083(13) 0.0656(12) Uani 1 1 d . . . F14 F 0.4590(5) -0.1619(3) 0.25529(17) 0.102(2) Uani 1 1 d . . . F15 F 0.3779(4) -0.0806(3) 0.20479(14) 0.0734(14) Uani 1 1 d . . . F16 F 0.6142(5) -0.0911(3) 0.26704(18) 0.109(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0363(7) 0.0349(7) 0.0278(6) -0.0009(5) 0.0090(5) 0.0018(6) Fe1 0.0279(4) 0.0302(5) 0.0223(4) 0.0022(3) 0.0062(3) 0.0042(4) Fe2 0.0327(4) 0.0334(5) 0.0238(4) -0.0026(4) 0.0068(3) 0.0026(4) S1 0.0635(12) 0.0516(11) 0.0362(9) -0.0077(8) 0.0061(8) 0.0213(9) S2 0.0558(12) 0.0732(14) 0.0528(11) -0.0233(10) 0.0082(9) -0.0013(11) S3 0.0510(11) 0.0658(13) 0.0528(10) 0.0154(10) 0.0257(9) 0.0274(10) S4 0.0330(14) 0.0586(19) 0.0546(17) -0.0043(13) 0.0045(11) 0.0114(12) S4A 0.046(2) 0.083(3) 0.052(2) -0.0107(19) 0.0178(16) -0.0005(19) S5 0.0754(13) 0.0502(11) 0.0381(9) -0.0050(8) 0.0223(9) -0.0006(10) S6 0.0967(16) 0.0550(12) 0.0422(10) -0.0072(9) 0.0306(11) 0.0157(12) N1 0.035(3) 0.034(3) 0.025(2) 0.004(2) 0.004(2) 0.009(2) N2 0.026(2) 0.032(3) 0.025(2) -0.001(2) 0.0072(19) -0.001(2) N3 0.031(2) 0.025(3) 0.028(2) 0.001(2) 0.009(2) -0.001(2) O1 0.030(2) 0.034(2) 0.0259(19) 0.0019(17) 0.0037(17) 0.0064(18) O2 0.034(2) 0.041(2) 0.027(2) 0.0005(18) 0.0062(18) 0.0134(19) O3 0.034(2) 0.041(3) 0.034(2) -0.0119(19) 0.0022(18) 0.006(2) O4 0.037(2) 0.035(2) 0.033(2) -0.0058(19) 0.0028(19) 0.0050(19) O5 0.032(2) 0.034(2) 0.0248(19) 0.0052(17) 0.0112(17) 0.0087(18) O6 0.026(2) 0.041(2) 0.0251(19) 0.0050(18) 0.0060(16) 0.0051(18) O7 0.030(2) 0.038(2) 0.0240(19) 0.0040(18) 0.0053(17) 0.0069(18) O8 0.033(2) 0.046(3) 0.033(2) -0.004(2) 0.0106(18) 0.008(2) O9 0.032(2) 0.035(2) 0.0221(19) -0.0036(17) 0.0079(17) -0.0010(19) O10 0.039(2) 0.037(2) 0.028(2) -0.0040(18) 0.0110(18) -0.003(2) O11 0.048(3) 0.029(2) 0.033(2) -0.0043(19) 0.017(2) -0.001(2) O12 0.052(3) 0.037(3) 0.027(2) -0.0039(19) 0.0110(19) 0.000(2) C1 0.034(3) 0.033(3) 0.026(3) -0.004(3) 0.001(2) 0.005(3) C2 0.045(4) 0.059(5) 0.034(3) -0.016(3) -0.001(3) 0.010(4) C3 0.037(4) 0.078(6) 0.046(4) -0.023(4) -0.008(3) 0.016(4) C4 0.038(4) 0.062(5) 0.043(4) -0.010(4) -0.007(3) 0.012(3) C5 0.031(3) 0.031(3) 0.031(3) -0.001(3) 0.001(2) 0.005(3) C6 0.028(3) 0.030(3) 0.029(3) 0.005(2) 0.006(2) 0.002(3) C7 0.037(3) 0.040(4) 0.024(3) 0.005(3) 0.007(3) 0.010(3) C8 0.034(3) 0.032(3) 0.029(3) 0.006(2) 0.013(3) 0.004(3) C9 0.035(3) 0.029(3) 0.032(3) 0.003(3) 0.006(3) 0.002(3) C10 0.039(3) 0.037(4) 0.037(3) 0.002(3) 0.004(3) 0.007(3) C11 0.042(4) 0.035(4) 0.051(4) 0.009(3) 0.004(3) 0.011(3) C12 0.063(5) 0.036(4) 0.067(5) -0.009(4) 0.008(4) 0.013(4) C13 0.036(3) 0.031(3) 0.023(3) 0.002(2) 0.004(2) 0.004(3) C14 0.040(3) 0.035(4) 0.029(3) -0.003(3) -0.001(3) 0.008(3) C15 0.040(3) 0.025(3) 0.030(3) -0.001(3) 0.005(3) 0.002(3) C16 0.044(4) 0.031(3) 0.032(3) 0.000(3) 0.003(3) 0.000(3) C17 0.039(3) 0.026(3) 0.023(3) -0.005(2) 0.012(2) 0.003(3) C18 0.062(5) 0.049(4) 0.045(4) -0.005(3) 0.021(4) 0.005(4) C19 0.069(5) 0.066(5) 0.038(4) -0.018(4) 0.010(4) -0.007(4) C20 0.023(3) 0.032(3) 0.024(3) -0.004(2) 0.002(2) -0.002(2) C21 0.026(3) 0.034(3) 0.033(3) 0.005(3) 0.004(2) 0.010(3) C22 0.035(3) 0.035(3) 0.028(3) 0.010(3) 0.002(3) -0.001(3) C23 0.030(3) 0.030(3) 0.026(3) 0.001(2) 0.005(2) 0.003(3) C24 0.025(3) 0.025(3) 0.021(3) 0.000(2) 0.004(2) 0.001(2) C25 0.024(3) 0.028(3) 0.024(3) -0.001(2) 0.004(2) 0.002(2) C26 0.034(3) 0.032(3) 0.020(3) 0.005(2) 0.004(2) 0.002(3) C27 0.028(3) 0.027(3) 0.025(3) 0.002(2) 0.004(2) -0.001(2) C28 0.029(3) 0.035(3) 0.028(3) 0.001(3) 0.010(2) 0.002(3) C29 0.044(4) 0.037(4) 0.027(3) 0.000(3) 0.016(3) 0.000(3) C30 0.054(4) 0.057(5) 0.033(3) -0.002(3) 0.021(3) -0.003(4) C31 0.051(4) 0.080(6) 0.057(5) 0.002(4) 0.037(4) 0.014(4) C32 0.028(3) 0.024(3) 0.025(3) -0.001(2) 0.008(2) 0.000(2) C33 0.026(3) 0.044(4) 0.032(3) 0.000(3) 0.004(2) 0.008(3) C34 0.028(3) 0.031(3) 0.036(3) -0.007(3) 0.005(3) -0.002(3) C35 0.027(3) 0.044(4) 0.047(4) -0.009(3) 0.011(3) -0.003(3) C36 0.046(2) 0.083(3) 0.052(2) -0.0107(19) 0.0178(16) -0.0005(19) C36A 0.0330(14) 0.0586(19) 0.0546(17) -0.0043(13) 0.0045(11) 0.0114(12) C37 0.027(4) 0.073(6) 0.098(7) -0.020(5) -0.004(4) 0.011(4) C38 0.048(5) 0.085(6) 0.079(6) -0.032(5) 0.031(4) -0.004(4) C39 0.031(3) 0.032(3) 0.032(3) -0.002(3) 0.008(3) 0.002(3) C40 0.039(4) 0.044(4) 0.038(3) -0.007(3) 0.017(3) -0.005(3) C41 0.060(5) 0.039(4) 0.063(5) -0.007(4) 0.032(4) -0.016(4) C42 0.045(4) 0.043(4) 0.033(3) -0.004(3) 0.014(3) -0.008(3) C43 0.040(3) 0.029(3) 0.019(3) 0.002(2) 0.004(2) 0.002(3) C44 0.034(3) 0.031(3) 0.022(3) 0.004(2) 0.009(2) 0.004(3) C45 0.038(3) 0.036(3) 0.030(3) -0.011(3) 0.009(3) -0.008(3) C46 0.038(3) 0.031(3) 0.026(3) 0.001(2) 0.004(3) 0.007(3) C47 0.045(4) 0.035(4) 0.030(3) 0.001(3) 0.015(3) 0.003(3) C48 0.081(5) 0.032(3) 0.024(3) -0.016(3) 0.018(3) -0.021(4) C49 0.068(5) 0.068(6) 0.054(5) -0.029(4) 0.014(4) -0.015(4) C50 0.077(5) 0.055(5) 0.032(3) -0.011(3) 0.015(4) 0.009(4) C51 0.031(3) 0.038(4) 0.028(3) -0.003(3) 0.004(2) 0.001(3) C52 0.031(3) 0.042(4) 0.033(3) 0.000(3) 0.016(3) -0.002(3) C53 0.029(3) 0.036(4) 0.023(3) -0.002(2) 0.004(2) 0.009(3) C54 0.038(3) 0.045(4) 0.033(3) 0.002(3) 0.011(3) 0.011(3) C55 0.054(4) 0.072(5) 0.042(4) -0.004(4) 0.027(3) -0.003(4) C56 0.070(5) 0.092(7) 0.044(4) 0.000(5) 0.033(4) -0.001(5) C57 0.088(7) 0.104(8) 0.043(4) -0.009(5) 0.041(4) 0.017(6) C58 0.059(5) 0.069(6) 0.088(6) -0.027(5) 0.010(5) 0.017(4) Cl1 0.0970(18) 0.0762(16) 0.0660(13) 0.0035(12) 0.0128(13) 0.0206(14) Cl2 0.0969(18) 0.0776(16) 0.0661(14) 0.0006(12) 0.0097(13) -0.0020(14) C59 0.084(7) 0.164(12) 0.082(7) -0.005(8) 0.009(6) -0.069(8) Cl3 0.145(3) 0.131(3) 0.132(3) -0.044(2) 0.067(2) -0.065(2) Cl4 0.0843(19) 0.152(3) 0.096(2) 0.032(2) -0.0015(16) 0.0278(19) C60 0.090(8) 0.095(8) 0.118(9) -0.016(7) 0.023(7) -0.019(7) Cl5 0.0916(18) 0.147(3) 0.0597(14) -0.0079(16) 0.0125(13) 0.0164(18) Cl6 0.0877(18) 0.112(2) 0.0849(17) 0.0036(16) 0.0138(15) -0.0014(16) P1 0.0935(17) 0.0631(14) 0.0346(10) -0.0023(9) 0.0027(11) 0.0216(13) F11 0.233(8) 0.147(6) 0.038(3) -0.009(3) 0.012(4) 0.108(6) F12 0.112(4) 0.063(3) 0.101(4) 0.005(3) -0.030(4) -0.012(3) F13 0.075(3) 0.075(3) 0.050(2) -0.007(2) 0.020(2) 0.006(3) F14 0.139(5) 0.098(4) 0.082(4) 0.037(3) 0.057(4) 0.035(4) F15 0.066(3) 0.102(4) 0.054(3) 0.004(3) 0.017(2) 0.006(3) F16 0.123(5) 0.103(5) 0.079(4) -0.009(3) -0.039(4) 0.028(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic= ) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O5 2.684(4) . ? K1 O11 2.713(4) . ? K1 O3 2.724(4) . ? K1 O7 2.791(4) . ? K1 O9 2.800(4) . ? K1 O1 2.850(4) . ? K1 N3 2.881(5) . ? K1 N2 2.914(5) . ? K1 N1 2.958(5) . ? K1 Fe2 3.5001(15) . ? K1 Fe1 3.5133(16) . ? Fe1 O6 1.978(4) . ? Fe1 O9 1.988(4) . ? Fe1 O2 1.989(4) . ? Fe1 O10 2.001(4) . ? Fe1 O5 2.004(4) . ? Fe1 O1 2.015(4) . ? Fe2 O8 1.972(4) . ? Fe2 O4 1.983(4) . ? Fe2 O11 1.989(4) . ? Fe2 O12 1.991(4) . ? Fe2 O7 1.998(4) . ? Fe2 O3 1.999(4) . ? S1 C12 1.708(7) . ? S1 C9 1.711(6) . ? S2 C19 1.681(8) . ? S2 C16 1.720(6) . ? S3 C31 1.699(7) . ? S3 C28 1.722(6) . ? S4 C37 1.589(8) . ? S4 C35 1.620(7) . ? S4A C38 1.524(9) . ? S4A C35 1.582(7) . ? S5 C50 1.686(8) . ? S5 C47 1.708(6) . ? S6 C57 1.703(9) . ? S6 C54 1.709(7) . ? N1 C1 1.340(7) . ? N1 C5 1.351(7) . ? N2 C24 1.342(7) . ? N2 C20 1.344(7) . ? N3 C43 1.345(7) . ? N3 C39 1.347(7) . ? O1 C6 1.278(6) . ? O2 C8 1.291(7) . ? O3 C13 1.274(7) . ? O4 C15 1.281(7) . ? O5 C25 1.275(6) . ? O6 C27 1.288(6) . ? O7 C32 1.286(6) . ? O8 C34 1.278(7) . ? O9 C44 1.286(7) . ? O10 C46 1.268(7) . ? O11 C51 1.278(7) . ? O12 C53 1.269(7) . ? C1 C2 1.402(8) . ? C1 C13 1.514(8) . ? C2 C3 1.374(9) . ? C3 C4 1.383(9) . ? C4 C5 1.400(8) . ? C5 C6 1.505(8) . ? C6 C7 1.393(8) . ? C7 C8 1.404(8) . ? C8 C9 1.463(8) . ? C9 C10 1.363(8) . ? C10 C11 1.402(9) . ? C11 C12 1.343(10) . ? C13 C14 1.390(8) . ? C14 C15 1.415(8) . ? C15 C16 1.470(8) . ? C16 C17 1.438(8) . ? C17 C18 1.435(8) . ? C18 C19 1.352(10) . ? C20 C21 1.398(8) . ? C20 C32 1.506(7) . ? C21 C22 1.370(8) . ? C22 C23 1.389(8) . ? C23 C24 1.402(7) . ? C24 C25 1.508(7) . ? C25 C26 1.402(7) . ? C26 C27 1.393(8) . ? C27 C28 1.462(7) . ? C28 C29 1.388(8) . ? C29 C30 1.405(8) . ? C30 C31 1.355(10) . ? C32 C33 1.387(8) . ? C33 C34 1.408(8) . ? C34 C35 1.470(8) . ? C37 C38 1.341(12) . ? C39 C40 1.374(8) . ? C39 C51 1.509(8) . ? C40 C41 1.372(9) . ? C41 C42 1.396(9) . ? C42 C43 1.401(8) . ? C43 C44 1.505(8) . ? C44 C45 1.385(8) . ? C45 C46 1.406(8) . ? C46 C47 1.467(8) . ? C47 C48 1.441(9) . ? C48 C49 1.417(9) . ? C49 C50 1.362(11) . ? C51 C52 1.393(8) . ? C52 C53 1.398(8) . ? C53 C54 1.465(8) . ? C54 C55 1.365(9) . ? C55 C56 1.419(9) . ? C56 C57 1.324(12) . ? C58 Cl2 1.737(9) . ? C58 Cl1 1.752(9) . ? C59 Cl3 1.716(12) . ? C59 Cl4 1.749(11) . ? C60 Cl6 1.719(11) . ? C60 Cl5 1.743(11) . ? P1 F16 1.580(6) . ? P1 F12 1.581(6) . ? P1 F14 1.584(6) . ? P1 F11 1.586(6) . ? P1 F15 1.596(5) . ? P1 F13 1.600(5) . ? 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 O5 K1 O11 145.13(13) . . ? O5 K1 O3 147.65(14) . . ? O11 K1 O3 60.08(12) . . ? O5 K1 O7 111.40(12) . . ? O11 K1 O7 59.05(12) . . ? O3 K1 O7 57.82(12) . . ? O5 K1 O9 59.77(11) . . ? O11 K1 O9 112.33(12) . . ? O3 K1 O9 143.26(13) . . ? O7 K1 O9 153.66(12) . . ? O5 K1 O1 59.40(11) . . ? O11 K1 O1 149.43(13) . . ? O3 K1 O1 108.70(12) . . ? O7 K1 O1 142.67(13) . . ? O9 K1 O1 57.79(11) . . ? O5 K1 N3 105.19(13) . . ? O11 K1 N3 55.84(13) . . ? O3 K1 N3 107.16(13) . . ? O7 K1 N3 108.43(13) . . ? O9 K1 N3 56.59(12) . . ? O1 K1 N3 108.86(13) . . ? O5 K1 N2 55.61(12) . . ? O11 K1 N2 103.09(13) . . ? O3 K1 N2 108.85(13) . . ? O7 K1 N2 56.11(12) . . ? O9 K1 N2 107.86(12) . . ? O1 K1 N2 107.48(12) . . ? N3 K1 N2 115.63(14) . . ? O5 K1 N1 110.41(13) . . ? O11 K1 N1 104.40(13) . . ? O3 K1 N1 53.97(13) . . ? O7 K1 N1 105.93(13) . . ? O9 K1 N1 100.33(13) . . ? O1 K1 N1 55.25(12) . . ? N3 K1 N1 115.57(14) . . ? N2 K1 N1 128.79(14) . . ? O5 K1 Fe2 146.11(9) . . ? O11 K1 Fe2 34.49(9) . . ? O3 K1 Fe2 34.71(9) . . ? O7 K1 Fe2 34.78(8) . . ? O9 K1 Fe2 146.40(9) . . ? O1 K1 Fe2 143.38(9) . . ? N3 K1 Fe2 90.27(10) . . ? N2 K1 Fe2 90.55(10) . . ? N1 K1 Fe2 88.51(10) . . ? O5 K1 Fe1 34.57(8) . . ? O11 K1 Fe1 146.56(10) . . ? O3 K1 Fe1 143.67(10) . . ? O7 K1 Fe1 145.72(9) . . ? O9 K1 Fe1 34.42(8) . . ? O1 K1 Fe1 34.98(8) . . ? N3 K1 Fe1 90.73(10) . . ? N2 K1 Fe1 90.18(9) . . ? N1 K1 Fe1 89.89(10) . . ? Fe2 K1 Fe1 178.36(5) . . ? O6 Fe1 O9 167.62(16) . . ? O6 Fe1 O2 90.44(16) . . ? O9 Fe1 O2 99.25(17) . . ? O6 Fe1 O10 86.14(16) . . ? O9 Fe1 O10 86.29(16) . . ? O2 Fe1 O10 89.36(17) . . ? O6 Fe1 O5 85.19(15) . . ? O9 Fe1 O5 86.45(16) . . ? O2 Fe1 O5 169.63(17) . . ? O10 Fe1 O5 99.71(17) . . ? O6 Fe1 O1 102.49(16) . . ? O9 Fe1 O1 86.02(15) . . ? O2 Fe1 O1 85.57(16) . . ? O10 Fe1 O1 169.99(16) . . ? O5 Fe1 O1 86.20(16) . . ? O6 Fe1 K1 125.64(12) . . ? O9 Fe1 K1 52.76(12) . . ? O2 Fe1 K1 128.32(11) . . ? O10 Fe1 K1 124.43(12) . . ? O5 Fe1 K1 49.46(10) . . ? O1 Fe1 K1 54.20(11) . . ? O8 Fe2 O4 90.63(17) . . ? O8 Fe2 O11 101.79(18) . . ? O4 Fe2 O11 163.98(17) . . ? O8 Fe2 O12 89.25(18) . . ? O4 Fe2 O12 85.04(17) . . ? O11 Fe2 O12 85.05(17) . . ? O8 Fe2 O7 85.65(16) . . ? O4 Fe2 O7 105.44(17) . . ? O11 Fe2 O7 85.77(16) . . ? O12 Fe2 O7 168.37(17) . . ? O8 Fe2 O3 166.27(18) . . ? O4 Fe2 O3 83.86(17) . . ? O11 Fe2 O3 86.09(17) . . ? O12 Fe2 O3 102.74(18) . . ? O7 Fe2 O3 83.72(16) . . ? O8 Fe2 K1 126.76(12) . . ? O4 Fe2 K1 128.04(12) . . ? O11 Fe2 K1 50.56(12) . . ? O12 Fe2 K1 124.31(13) . . ? O7 Fe2 K1 52.83(11) . . ? O3 Fe2 K1 50.90(11) . . ? C12 S1 C9 91.2(3) . . ? C19 S2 C16 91.9(3) . . ? C31 S3 C28 91.6(3) . . ? C37 S4 C35 96.3(4) . . ? C38 S4A C35 98.9(5) . . ? C50 S5 C47 92.1(3) . . ? C57 S6 C54 90.3(4) . . ? C1 N1 C5 118.2(5) . . ? C1 N1 K1 122.3(4) . . ? C5 N1 K1 119.4(4) . . ? C24 N2 C20 118.6(5) . . ? C24 N2 K1 120.9(3) . . ? C20 N2 K1 120.2(3) . . ? C43 N3 C39 118.2(5) . . ? C43 N3 K1 119.5(4) . . ? C39 N3 K1 122.1(4) . . ? C6 O1 Fe1 129.1(4) . . ? C6 O1 K1 117.2(3) . . ? Fe1 O1 K1 90.82(14) . . ? C8 O2 Fe1 130.0(4) . . ? C13 O3 Fe2 132.0(4) . . ? C13 O3 K1 132.6(4) . . ? Fe2 O3 K1 94.40(15) . . ? C15 O4 Fe2 128.7(4) . . ? C25 O5 Fe1 131.2(3) . . ? C25 O5 K1 130.1(3) . . ? Fe1 O5 K1 95.97(14) . . ? C27 O6 Fe1 127.5(4) . . ? C32 O7 Fe2 130.9(3) . . ? C32 O7 K1 121.9(3) . . ? Fe2 O7 K1 92.39(14) . . ? C34 O8 Fe2 131.7(4) . . ? C44 O9 Fe1 130.1(3) . . ? C44 O9 K1 118.5(3) . . ? Fe1 O9 K1 92.82(15) . . ? C46 O10 Fe1 130.6(4) . . ? C51 O11 Fe2 131.7(4) . . ? C51 O11 K1 126.9(4) . . ? Fe2 O11 K1 94.95(16) . . ? C53 O12 Fe2 130.6(4) . . ? N1 C1 C2 122.6(5) . . ? N1 C1 C13 113.8(5) . . ? C2 C1 C13 123.6(5) . . ? C3 C2 C1 118.4(6) . . ? C2 C3 C4 120.1(6) . . ? C3 C4 C5 118.2(6) . . ? N1 C5 C4 122.5(6) . . ? N1 C5 C6 113.8(5) . . ? C4 C5 C6 123.8(5) . . ? O1 C6 C7 124.9(5) . . ? O1 C6 C5 115.5(5) . . ? C7 C6 C5 119.6(5) . . ? C6 C7 C8 123.1(5) . . ? O2 C8 C7 123.6(5) . . ? O2 C8 C9 114.8(5) . . ? C7 C8 C9 121.6(5) . . ? C10 C9 C8 130.8(6) . . ? C10 C9 S1 110.9(5) . . ? C8 C9 S1 118.3(4) . . ? C9 C10 C11 113.3(6) . . ? C12 C11 C10 112.0(6) . . ? C11 C12 S1 112.6(5) . . ? O3 C13 C14 123.7(5) . . ? O3 C13 C1 114.2(5) . . ? C14 C13 C1 122.1(5) . . ? C13 C14 C15 121.5(6) . . ? O4 C15 C14 123.6(5) . . ? O4 C15 C16 114.0(5) . . ? C14 C15 C16 122.4(5) . . ? C17 C16 C15 123.7(5) . . ? C17 C16 S2 111.7(4) . . ? C15 C16 S2 124.6(5) . . ? C18 C17 C16 108.8(6) . . ? C19 C18 C17 113.7(6) . . ? C18 C19 S2 113.9(6) . . ? N2 C20 C21 122.6(5) . . ? N2 C20 C32 115.0(5) . . ? C21 C20 C32 122.3(5) . . ? C22 C21 C20 118.3(5) . . ? C21 C22 C23 120.0(5) . . ? C22 C23 C24 118.4(5) . . ? N2 C24 C23 122.0(5) . . ? N2 C24 C25 114.3(5) . . ? C23 C24 C25 123.5(5) . . ? O5 C25 C26 122.9(5) . . ? O5 C25 C24 115.5(5) . . ? C26 C25 C24 121.6(5) . . ? C27 C26 C25 122.4(5) . . ? O6 C27 C26 125.0(5) . . ? O6 C27 C28 114.2(5) . . ? C26 C27 C28 120.8(5) . . ? C29 C28 C27 131.6(6) . . ? C29 C28 S3 110.9(4) . . ? C27 C28 S3 117.5(4) . . ? C28 C29 C30 112.0(6) . . ? C31 C30 C29 112.9(6) . . ? C30 C31 S3 112.6(5) . . ? O7 C32 C33 124.3(5) . . ? O7 C32 C20 115.1(5) . . ? C33 C32 C20 120.6(5) . . ? C32 C33 C34 122.3(5) . . ? O8 C34 C33 124.3(5) . . ? O8 C34 C35 115.3(5) . . ? C33 C34 C35 120.4(5) . . ? C34 C35 S4A 121.3(5) . . ? C34 C35 S4 124.7(5) . . ? S4A C35 S4 113.7(4) . . ? C38 C37 S4 114.7(6) . . ? C37 C38 S4A 116.3(6) . . ? N3 C39 C40 122.9(5) . . ? N3 C39 C51 113.2(5) . . ? C40 C39 C51 123.9(5) . . ? C41 C40 C39 119.2(6) . . ? C40 C41 C42 119.4(6) . . ? C41 C42 C43 118.1(6) . . ? N3 C43 C42 122.1(5) . . ? N3 C43 C44 115.3(5) . . ? C42 C43 C44 122.6(5) . . ? O9 C44 C45 125.1(5) . . ? O9 C44 C43 115.7(5) . . ? C45 C44 C43 119.2(5) . . ? C44 C45 C46 122.5(6) . . ? O10 C46 C45 124.8(5) . . ? O10 C46 C47 115.8(5) . . ? C45 C46 C47 119.4(6) . . ? C48 C47 C46 128.9(5) . . ? C48 C47 S5 111.7(4) . . ? C46 C47 S5 119.3(5) . . ? C49 C48 C47 109.0(6) . . ? C50 C49 C48 114.0(7) . . ? C49 C50 S5 113.0(5) . . ? O11 C51 C52 124.1(6) . . ? O11 C51 C39 115.2(5) . . ? C52 C51 C39 120.7(6) . . ? C51 C52 C53 122.0(6) . . ? O12 C53 C52 124.9(5) . . ? O12 C53 C54 114.2(5) . . ? C52 C53 C54 120.9(6) . . ? C55 C54 C53 129.4(6) . . ? C55 C54 S6 111.6(5) . . ? C53 C54 S6 119.0(5) . . ? C54 C55 C56 112.5(7) . . ? C57 C56 C55 111.1(8) . . ? C56 C57 S6 114.5(6) . . ? Cl2 C58 Cl1 112.2(4) . . ? Cl3 C59 Cl4 114.1(6) . . ? Cl6 C60 Cl5 113.3(6) . . ? F16 P1 F12 90.8(3) . . ? F16 P1 F14 90.1(4) . . ? F12 P1 F14 178.8(3) . . ? F16 P1 F11 91.2(4) . . ? F12 P1 F11 90.5(4) . . ? F14 P1 F11 90.3(4) . . ? F16 P1 F15 179.5(4) . . ? F12 P1 F15 88.8(3) . . ? F14 P1 F15 90.3(3) . . ? F11 P1 F15 89.1(3) . . ? F16 P1 F13 90.6(3) . . ? F12 P1 F13 90.4(3) . . ? F14 P1 F13 88.8(3) . . ? F11 P1 F13 178.0(4) . . ? F15 P1 F13 89.1(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.977 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.100 #======END OF DATA FOR K-4c # 4.2 RESULTS FOR K-4d data_rs9910 _database_code_CSD 152454 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H75 Cl4 Fe3 K N3 O15' _chemical_formula_weight 1931.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 16.179(3) _cell_length_b 16.179(3) _cell_length_c 20.981(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4756.2(15) _cell_formula_units_Z 2 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 52 _cell_measurement_theta_min 3.85 _cell_measurement_theta_max 9.00 _exptl_crystal_description 'hexagonal prism' _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1986 _exptl_absorpt_coefficient_mu 0.673 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.8928 _exptl_absorpt_correction_T_max 0.9504 _exptl_absorpt_process_details ; North A C T, Phillips D C, Mathews F S, Acta Cryst. A24 (1968) 351-359. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 'Siemens P4' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7058 _diffrn_reflns_av_R_equivalents 0.1152 _diffrn_reflns_av_sigmaI/netI 0.2971 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5538 _reflns_number_gt 1745 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCAnS 2.20 (Siemens An. X-Ray Instr.,1996)' _computing_cell_refinement 'XSCAnS 2.20 (Siemens An. X-Ray Instr.,1996)' _computing_data_reduction 'XSCAnS 2.20 (Siemens An. X-Ray Instr.,1996)' _computing_structure_solution 'SHELXTL 5.1 (Bruker AXS, 1998)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS, 1998)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS, 1998)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS, 1998)' _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. The compound crystallizes with 3 molecules acetone per asymmetric unit, that seem to be disordered. The xyz coordinates of the solvate molecule have been fixed during the refinement while the Uij components have been refined using DELU and SIMU restraints. No H atoms havve been included for the acetone molecules. ; _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^)+(0.1000P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5538 _refine_ls_number_parameters 373 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.3206 _refine_ls_R_factor_gt 0.1286 _refine_ls_wR_factor_ref 0.3489 _refine_ls_wR_factor_gt 0.2664 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.146 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.6667 0.3333 0.38570(14) 0.0505(12) Uani 1 3 d S . . Fe2 Fe 0.6667 0.3333 0.04211(14) 0.0481(12) Uani 1 3 d S . . K1 K 0.6667 0.3333 0.2137(2) 0.0491(16) Uani 1 3 d S . . N1 N 0.8678(8) 0.4637(9) 0.2121(4) 0.044(3) Uani 1 1 d . . . O1 O 0.7731(8) 0.4187(7) 0.3251(4) 0.050(3) Uani 1 1 d . . . O2 O 0.7684(8) 0.3342(8) 0.4389(4) 0.054(3) Uani 1 1 d . . . O3 O 0.7790(7) 0.3981(8) 0.1036(3) 0.050(3) Uani 1 1 d . . . O4 O 0.7522(8) 0.4402(8) -0.0156(4) 0.051(3) Uani 1 1 d . . . C1 C 0.9180(12) 0.5039(12) 0.1585(6) 0.050(4) Uani 1 1 d . . . C2 C 1.0123(11) 0.5707(11) 0.1586(5) 0.053(5) Uani 1 1 d . . . H2A H 1.0437 0.5985 0.1207 0.063 Uiso 1 1 calc R . . C3 C 1.0602(12) 0.5966(13) 0.2153(6) 0.070(6) Uani 1 1 d . . . H3A H 1.1251 0.6408 0.2168 0.084 Uiso 1 1 calc R . . C4 C 1.0096(12) 0.5553(12) 0.2697(6) 0.057(5) Uani 1 1 d . . . H4A H 1.0406 0.5735 0.3089 0.069 Uiso 1 1 calc R . . C5 C 0.9165(12) 0.4890(12) 0.2680(6) 0.053(5) Uani 1 1 d . . . C6 C 0.8592(12) 0.4399(12) 0.3247(6) 0.046(4) Uani 1 1 d . . . C7 C 0.9050(12) 0.4219(11) 0.3744(6) 0.065(5) Uani 1 1 d . . . H7A H 0.9699 0.4439 0.3702 0.078 Uiso 1 1 calc R . . C8 C 0.8589(12) 0.3721(12) 0.4309(6) 0.052(5) Uani 1 1 d . . . C9 C 0.9129(12) 0.3563(12) 0.4811(6) 0.054(5) Uani 1 1 d . . . C10 C 1.0114(12) 0.4049(16) 0.4812(8) 0.101(9) Uani 1 1 d . . . H10A H 1.0453 0.4489 0.4493 0.122 Uiso 1 1 calc R . . C11 C 1.0578(14) 0.3879(17) 0.5278(8) 0.115(9) Uani 1 1 d . . . H11A H 1.1242 0.4200 0.5267 0.138 Uiso 1 1 calc R . . C12 C 1.0123(15) 0.3256(17) 0.5766(7) 0.098(8) Uani 1 1 d . . . C13 C 1.0615(17) 0.310(2) 0.6247(9) 0.167(14) Uani 1 1 d . . . H13A H 1.1279 0.3429 0.6239 0.201 Uiso 1 1 calc R . . C14 C 1.0134(17) 0.245(2) 0.6748(10) 0.155(13) Uani 1 1 d . . . H14A H 1.0465 0.2321 0.7056 0.186 Uiso 1 1 calc R . . C15 C 0.9168(16) 0.2027(16) 0.6761(8) 0.110(9) Uani 1 1 d . . . H15A H 0.8839 0.1603 0.7090 0.132 Uiso 1 1 calc R . . C16 C 0.8650(13) 0.2200(15) 0.6305(6) 0.088(7) Uani 1 1 d . . . H16A H 0.7993 0.1940 0.6345 0.106 Uiso 1 1 calc R . . C17 C 0.9134(12) 0.2765(13) 0.5794(6) 0.060(5) Uani 1 1 d . . . C18 C 0.8644(11) 0.2970(11) 0.5317(5) 0.051(4) Uani 1 1 d . . . H18A H 0.7985 0.2701 0.5345 0.061 Uiso 1 1 calc R . . C19 C 0.8617(11) 0.4733(11) 0.0992(6) 0.043(4) Uani 1 1 d . . . C20 C 0.8960(12) 0.5246(12) 0.0434(5) 0.066(6) Uani 1 1 d . . . H20A H 0.9586 0.5750 0.0425 0.079 Uiso 1 1 calc R . . C21 C 0.8388(12) 0.5035(12) -0.0142(6) 0.050(5) Uani 1 1 d . . . C22 C 0.8798(13) 0.5509(12) -0.0740(5) 0.053(5) Uani 1 1 d . . . C23 C 0.9712(14) 0.6176(13) -0.0793(6) 0.065(6) Uani 1 1 d . . . H23A H 1.0098 0.6361 -0.0432 0.078 Uiso 1 1 calc R . . C24 C 1.0107(12) 0.6607(13) -0.1382(6) 0.057(5) Uani 1 1 d . . . C25 C 1.1062(16) 0.7307(14) -0.1449(7) 0.086(7) Uani 1 1 d . . . H25A H 1.1433 0.7514 -0.1082 0.103 Uiso 1 1 calc R . . C26 C 1.1500(15) 0.7718(15) -0.2024(8) 0.086(6) Uani 1 1 d . . . H26A H 1.2141 0.8183 -0.2052 0.103 Uiso 1 1 calc R . . C27 C 1.0920(15) 0.7391(15) -0.2544(8) 0.084(7) Uani 1 1 d . . . H27A H 1.1182 0.7646 -0.2940 0.101 Uiso 1 1 calc R . . C28 C 1.0003(13) 0.6729(13) -0.2520(7) 0.069(6) Uani 1 1 d . . . H28A H 0.9646 0.6525 -0.2893 0.083 Uiso 1 1 calc R . . C29 C 0.9568(13) 0.6333(13) -0.1926(6) 0.063(5) Uani 1 1 d . . . C30 C 0.8645(14) 0.5662(13) -0.1860(6) 0.074(6) Uani 1 1 d . . . H30A H 0.8260 0.5465 -0.2221 0.089 Uiso 1 1 calc R . . C31 C 0.8249(11) 0.5261(11) -0.1294(5) 0.053(5) Uani 1 1 d . . . H31A H 0.7602 0.4814 -0.1274 0.063 Uiso 1 1 calc R . . Fe3 Fe 0.6667 0.3333 -0.33756(16) 0.0557(13) Uani 1 3 d S . . Cl1 Cl 0.6291(4) 0.1921(4) -0.37077(19) 0.0797(16) Uani 1 1 d . . . Cl2 Cl 0.6667 0.3333 -0.2331(3) 0.072(3) Uani 1 3 d S . . O40 O 0.9091 0.2402 0.9678 0.63(3) Uani 1 1 d U . . C40 C 0.9145 0.1802 0.9415 0.50(3) Uani 1 1 d U . . C41 C 0.9496 0.1814 0.8766 0.44(3) Uani 1 1 d U . . C42 C 0.8862 0.0806 0.9700 0.71(4) Uani 1 1 d U . . 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 0.0673(19) 0.0673(19) 0.0170(16) 0.000 0.000 0.0336(10) Fe2 0.0628(19) 0.0628(19) 0.0185(16) 0.000 0.000 0.0314(9) K1 0.065(3) 0.065(3) 0.018(2) 0.000 0.000 0.0323(13) N1 0.050(8) 0.064(9) 0.015(5) 0.003(5) -0.007(5) 0.026(7) O1 0.075(8) 0.075(9) 0.021(4) 0.004(5) -0.001(5) 0.053(7) O2 0.068(8) 0.074(9) 0.019(4) 0.005(5) 0.002(5) 0.035(7) O3 0.058(8) 0.082(9) 0.011(4) 0.006(5) -0.004(4) 0.036(7) O4 0.063(8) 0.072(8) 0.019(4) 0.007(5) 0.005(5) 0.035(7) C1 0.074(13) 0.061(12) 0.018(6) 0.002(7) 0.000(7) 0.035(11) C2 0.059(12) 0.047(11) 0.017(6) 0.009(7) -0.009(7) 0.000(10) C3 0.054(12) 0.092(15) 0.042(9) 0.001(9) -0.025(8) 0.019(11) C4 0.062(13) 0.071(13) 0.032(8) -0.001(8) -0.004(8) 0.028(11) C5 0.046(11) 0.077(13) 0.026(7) 0.004(8) 0.000(7) 0.023(10) C6 0.052(11) 0.072(12) 0.020(6) -0.010(7) -0.006(7) 0.034(10) C7 0.077(14) 0.078(14) 0.022(7) 0.009(8) -0.006(8) 0.026(12) C8 0.055(12) 0.070(13) 0.028(7) 0.006(8) -0.002(8) 0.029(11) C9 0.057(12) 0.087(14) 0.017(6) 0.009(7) -0.006(7) 0.034(11) C10 0.032(11) 0.19(2) 0.057(10) 0.057(13) 0.006(9) 0.034(14) C11 0.058(14) 0.21(3) 0.059(11) 0.056(14) -0.008(10) 0.056(16) C12 0.080(16) 0.18(2) 0.038(9) 0.049(12) 0.012(10) 0.065(17) C13 0.083(19) 0.30(4) 0.068(13) 0.082(19) -0.003(13) 0.06(2) C14 0.060(16) 0.28(4) 0.099(17) 0.10(2) 0.014(14) 0.07(2) C15 0.097(19) 0.14(2) 0.051(11) 0.053(13) -0.002(12) 0.030(17) C16 0.059(13) 0.15(2) 0.028(8) 0.026(10) -0.009(8) 0.029(13) C17 0.039(11) 0.099(15) 0.034(8) 0.015(9) -0.009(8) 0.027(11) C18 0.058(11) 0.076(13) 0.018(6) 0.013(7) -0.004(7) 0.034(10) C19 0.037(10) 0.052(11) 0.031(7) 0.001(7) 0.013(7) 0.016(9) C20 0.077(13) 0.076(13) 0.009(6) 0.006(7) 0.004(7) 0.012(11) C21 0.049(11) 0.057(12) 0.030(7) 0.009(8) 0.013(8) 0.017(10) C22 0.070(13) 0.059(12) 0.013(6) 0.004(7) 0.004(7) 0.019(11) C23 0.101(16) 0.078(14) 0.012(6) 0.002(8) -0.010(8) 0.041(13) C24 0.040(11) 0.065(13) 0.039(8) 0.005(8) 0.001(8) 0.007(10) C25 0.110(19) 0.089(16) 0.047(10) 0.017(10) -0.023(11) 0.041(15) C26 0.079(16) 0.104(18) 0.064(11) 0.016(12) 0.018(11) 0.038(14) C27 0.085(16) 0.114(19) 0.039(9) 0.037(11) 0.015(10) 0.040(15) C28 0.064(14) 0.071(14) 0.049(9) 0.016(9) 0.009(9) 0.017(12) C29 0.066(13) 0.079(14) 0.024(7) 0.002(8) -0.004(8) 0.020(12) C30 0.090(16) 0.076(14) 0.028(8) 0.018(9) -0.004(9) 0.020(13) C31 0.033(10) 0.071(12) 0.030(7) -0.001(8) 0.002(7) 0.008(9) Fe3 0.068(2) 0.068(2) 0.0304(18) 0.000 0.000 0.0342(10) Cl1 0.097(4) 0.082(4) 0.061(2) -0.008(3) 0.001(3) 0.046(3) Cl2 0.094(4) 0.094(4) 0.027(3) 0.000 0.000 0.047(2) O40 0.38(5) 0.70(6) 0.41(4) 0.17(4) 0.00(4) -0.03(4) C40 0.29(4) 0.61(5) 0.27(3) 0.25(3) -0.14(3) -0.02(4) C41 0.18(4) 0.63(6) 0.32(3) 0.25(4) -0.13(3) 0.05(4) C42 0.44(6) 0.60(6) 0.55(6) 0.39(5) -0.17(5) -0.16(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic= ) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O2 1.983(10) . ? Fe1 O2 1.983(10) 3_665 ? Fe1 O2 1.983(10) 2_655 ? Fe1 O1 2.028(10) 3_665 ? Fe1 O1 2.028(10) . ? Fe1 O1 2.028(10) 2_655 ? Fe1 K1 3.608(6) . ? Fe2 O4 1.994(10) 3_665 ? Fe2 O4 1.994(10) . ? Fe2 O4 1.994(10) 2_655 ? Fe2 O3 2.040(9) 3_665 ? Fe2 O3 2.040(9) . ? Fe2 O3 2.040(9) 2_655 ? Fe2 K1 3.600(6) . ? K1 O3 2.799(9) 3_665 ? K1 O3 2.799(9) . ? K1 O3 2.799(9) 2_655 ? K1 O1 2.821(10) 3_665 ? K1 O1 2.821(10) . ? K1 O1 2.821(10) 2_655 ? K1 N1 2.859(12) 3_665 ? K1 N1 2.859(12) . ? K1 N1 2.859(12) 2_655 ? N1 C1 1.349(16) . ? N1 C5 1.357(15) . ? O1 C6 1.256(16) . ? O2 C8 1.285(17) . ? O3 C19 1.285(15) . ? O4 C21 1.256(16) . ? C1 C2 1.36(2) . ? C1 C19 1.473(18) . ? C2 C3 1.366(17) . ? C3 C4 1.369(19) . ? C4 C5 1.34(2) . ? C5 C6 1.472(18) . ? C6 C7 1.393(19) . ? C7 C8 1.419(18) . ? C8 C9 1.469(18) . ? C9 C10 1.38(2) . ? C9 C18 1.382(18) . ? C10 C11 1.34(2) . ? C11 C12 1.37(2) . ? C12 C13 1.39(2) . ? C12 C17 1.39(2) . ? C13 C14 1.41(3) . ? C14 C15 1.36(3) . ? C15 C16 1.39(2) . ? C16 C17 1.37(2) . ? C17 C18 1.414(18) . ? C19 C20 1.383(17) . ? C20 C21 1.454(19) . ? C21 C22 1.447(17) . ? C22 C23 1.33(2) . ? C22 C31 1.395(18) . ? C23 C24 1.407(18) . ? C24 C29 1.369(19) . ? C24 C25 1.39(2) . ? C25 C26 1.39(2) . ? C26 C27 1.36(2) . ? C27 C28 1.33(2) . ? C28 C29 1.417(19) . ? C29 C30 1.34(2) . ? C30 C31 1.351(17) . ? Fe3 Cl1 2.165(5) . ? Fe3 Cl1 2.165(5) 2_655 ? Fe3 Cl1 2.165(5) 3_665 ? Fe3 Cl2 2.191(6) . ? O40 C40 1.15625(18) . ? C40 C41 1.4729(2) . ? C40 C42 1.5585(2) . ? 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 O2 Fe1 O2 91.4(4) . 3_665 ? O2 Fe1 O2 91.4(4) . 2_655 ? O2 Fe1 O2 91.4(4) 3_665 2_655 ? O2 Fe1 O1 98.4(4) . 3_665 ? O2 Fe1 O1 85.9(4) 3_665 3_665 ? O2 Fe1 O1 169.9(4) 2_655 3_665 ? O2 Fe1 O1 85.9(4) . . ? O2 Fe1 O1 169.9(4) 3_665 . ? O2 Fe1 O1 98.4(4) 2_655 . ? O1 Fe1 O1 84.9(4) 3_665 . ? O2 Fe1 O1 169.9(4) . 2_655 ? O2 Fe1 O1 98.4(4) 3_665 2_655 ? O2 Fe1 O1 85.9(4) 2_655 2_655 ? O1 Fe1 O1 84.9(4) 3_665 2_655 ? O1 Fe1 O1 84.9(4) . 2_655 ? O2 Fe1 K1 124.3(3) . . ? O2 Fe1 K1 124.3(3) 3_665 . ? O2 Fe1 K1 124.3(3) 2_655 . ? O1 Fe1 K1 51.2(3) 3_665 . ? O1 Fe1 K1 51.2(3) . . ? O1 Fe1 K1 51.2(3) 2_655 . ? O4 Fe2 O4 87.0(4) 3_665 . ? O4 Fe2 O4 87.0(4) 3_665 2_655 ? O4 Fe2 O4 87.0(4) . 2_655 ? O4 Fe2 O3 83.4(4) 3_665 3_665 ? O4 Fe2 O3 161.0(4) . 3_665 ? O4 Fe2 O3 108.7(4) 2_655 3_665 ? O4 Fe2 O3 108.7(4) 3_665 . ? O4 Fe2 O3 83.4(4) . . ? O4 Fe2 O3 161.0(4) 2_655 . ? O3 Fe2 O3 84.2(4) 3_665 . ? O4 Fe2 O3 161.0(4) 3_665 2_655 ? O4 Fe2 O3 108.7(4) . 2_655 ? O4 Fe2 O3 83.4(4) 2_655 2_655 ? O3 Fe2 O3 84.2(4) 3_665 2_655 ? O3 Fe2 O3 84.2(4) . 2_655 ? O4 Fe2 K1 127.4(3) 3_665 . ? O4 Fe2 K1 127.4(3) . . ? O4 Fe2 K1 127.4(3) 2_655 . ? O3 Fe2 K1 50.8(3) 3_665 . ? O3 Fe2 K1 50.8(3) . . ? O3 Fe2 K1 50.8(3) 2_655 . ? O3 K1 O3 58.5(3) 3_665 . ? O3 K1 O3 58.5(3) 3_665 2_655 ? O3 K1 O3 58.5(3) . 2_655 ? O3 K1 O1 112.2(3) 3_665 3_665 ? O3 K1 O1 140.4(3) . 3_665 ? O3 K1 O1 154.7(3) 2_655 3_665 ? O3 K1 O1 154.7(3) 3_665 . ? O3 K1 O1 112.2(3) . . ? O3 K1 O1 140.4(3) 2_655 . ? O1 K1 O1 58.0(4) 3_665 . ? O3 K1 O1 140.4(3) 3_665 2_655 ? O3 K1 O1 154.7(3) . 2_655 ? O3 K1 O1 112.2(3) 2_655 2_655 ? O1 K1 O1 58.0(4) 3_665 2_655 ? O1 K1 O1 58.0(4) . 2_655 ? O3 K1 N1 55.1(3) 3_665 3_665 ? O3 K1 N1 103.4(3) . 3_665 ? O3 K1 N1 108.1(3) 2_655 3_665 ? O1 K1 N1 57.1(3) 3_665 3_665 ? O1 K1 N1 111.5(3) . 3_665 ? O1 K1 N1 101.9(3) 2_655 3_665 ? O3 K1 N1 108.1(3) 3_665 . ? O3 K1 N1 55.1(3) . . ? O3 K1 N1 103.4(3) 2_655 . ? O1 K1 N1 101.9(3) 3_665 . ? O1 K1 N1 57.1(3) . . ? O1 K1 N1 111.5(3) 2_655 . ? N1 K1 N1 119.986(9) 3_665 . ? O3 K1 N1 103.4(3) 3_665 2_655 ? O3 K1 N1 108.1(3) . 2_655 ? O3 K1 N1 55.1(3) 2_655 2_655 ? O1 K1 N1 111.5(3) 3_665 2_655 ? O1 K1 N1 101.9(3) . 2_655 ? O1 K1 N1 57.1(3) 2_655 2_655 ? N1 K1 N1 119.986(9) 3_665 2_655 ? N1 K1 N1 119.986(9) . 2_655 ? O3 K1 Fe2 34.4(2) 3_665 . ? O3 K1 Fe2 34.4(2) . . ? O3 K1 Fe2 34.4(2) 2_655 . ? O1 K1 Fe2 145.9(2) 3_665 . ? O1 K1 Fe2 145.9(2) . . ? O1 K1 Fe2 145.9(2) 2_655 . ? N1 K1 Fe2 89.3(2) 3_665 . ? N1 K1 Fe2 89.3(2) . . ? N1 K1 Fe2 89.3(2) 2_655 . ? O3 K1 Fe1 145.6(2) 3_665 . ? O3 K1 Fe1 145.6(2) . . ? O3 K1 Fe1 145.6(2) 2_655 . ? O1 K1 Fe1 34.1(2) 3_665 . ? O1 K1 Fe1 34.1(2) . . ? O1 K1 Fe1 34.1(2) 2_655 . ? N1 K1 Fe1 90.7(2) 3_665 . ? N1 K1 Fe1 90.7(2) . . ? N1 K1 Fe1 90.7(2) 2_655 . ? Fe2 K1 Fe1 180.0 . . ? C1 N1 C5 117.2(13) . . ? C1 N1 K1 123.7(9) . . ? C5 N1 K1 119.2(9) . . ? C6 O1 Fe1 129.7(9) . . ? C6 O1 K1 116.7(8) . . ? Fe1 O1 K1 94.8(4) . . ? C8 O2 Fe1 132.4(9) . . ? C19 O3 Fe2 132.8(8) . . ? C19 O3 K1 126.0(8) . . ? Fe2 O3 K1 94.9(4) . . ? C21 O4 Fe2 134.4(9) . . ? N1 C1 C2 123.3(13) . . ? N1 C1 C19 114.8(14) . . ? C2 C1 C19 121.9(13) . . ? C1 C2 C3 118.9(13) . . ? C2 C3 C4 117.9(16) . . ? C5 C4 C3 121.7(14) . . ? C4 C5 N1 120.9(13) . . ? C4 C5 C6 124.1(13) . . ? N1 C5 C6 114.9(14) . . ? O1 C6 C7 124.7(14) . . ? O1 C6 C5 117.8(13) . . ? C7 C6 C5 117.4(15) . . ? C6 C7 C8 124.2(16) . . ? O2 C8 C7 122.0(14) . . ? O2 C8 C9 117.3(13) . . ? C7 C8 C9 120.6(15) . . ? C10 C9 C18 119.2(14) . . ? C10 C9 C8 121.3(15) . . ? C18 C9 C8 119.4(15) . . ? C11 C10 C9 119.3(17) . . ? C10 C11 C12 123.1(19) . . ? C11 C12 C13 122(2) . . ? C11 C12 C17 119.8(17) . . ? C13 C12 C17 118.0(18) . . ? C12 C13 C14 122(2) . . ? C15 C14 C13 117(2) . . ? C14 C15 C16 122.8(19) . . ? C17 C16 C15 118.1(17) . . ? C16 C17 C12 121.7(15) . . ? C16 C17 C18 120.6(16) . . ? C12 C17 C18 117.2(15) . . ? C9 C18 C17 121.1(15) . . ? O3 C19 C20 123.0(14) . . ? O3 C19 C1 115.8(12) . . ? C20 C19 C1 121.2(14) . . ? C19 C20 C21 123.1(15) . . ? O4 C21 C22 116.1(14) . . ? O4 C21 C20 122.0(13) . . ? C22 C21 C20 121.8(15) . . ? C23 C22 C31 117.0(13) . . ? C23 C22 C21 122.1(14) . . ? C31 C22 C21 120.9(16) . . ? C22 C23 C24 121.4(14) . . ? C29 C24 C25 116.6(15) . . ? C29 C24 C23 121.0(16) . . ? C25 C24 C23 122.4(15) . . ? C26 C25 C24 124.7(17) . . ? C27 C26 C25 115.0(19) . . ? C28 C27 C26 124.0(17) . . ? C27 C28 C29 120.0(17) . . ? C30 C29 C24 116.5(14) . . ? C30 C29 C28 123.8(15) . . ? C24 C29 C28 119.6(17) . . ? C29 C30 C31 123.1(15) . . ? C30 C31 C22 121.0(15) . . ? Cl1 Fe3 Cl1 110.16(13) . 2_655 ? Cl1 Fe3 Cl1 110.16(13) . 3_665 ? Cl1 Fe3 Cl1 110.16(13) 2_655 3_665 ? Cl1 Fe3 Cl2 108.77(14) . . ? Cl1 Fe3 Cl2 108.77(14) 2_655 . ? Cl1 Fe3 Cl2 108.77(14) 3_665 . ? O40 C40 C41 128.312(5) . . ? O40 C40 C42 125.457(11) . . ? C41 C40 C42 106.225(7) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.665 _refine_diff_density_min -0.713 _refine_diff_density_rms 0.129 #======END OF DATA FOR K-4d # 4.3 RESULTS FOR Ba-4a data_rs9903 _database_code_CSD 152455 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65.25 H85.50 Ba Cl8.50 Fe4 N3 O14' _chemical_formula_weight 1797.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ba' 'Ba' -0.3244 2.2819 '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 17.835(4) _cell_length_b 22.145(3) _cell_length_c 22.985(4) _cell_angle_alpha 112.21(2) _cell_angle_beta 94.67(2) _cell_angle_gamma 94.07(2) _cell_volume 8326(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 57 _cell_measurement_theta_min 1.90 _cell_measurement_theta_max 11.60 _exptl_crystal_description fragment _exptl_crystal_colour black _exptl_crystal_size_max 0.90 _exptl_crystal_size_mid 0.80 _exptl_crystal_size_min 0.60 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3658 _exptl_absorpt_coefficient_mu 1.475 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.1177 _exptl_absorpt_correction_T_max 0.1484 _exptl_absorpt_process_details ; North A C T, Phillips D C, Mathews F S, Acta Cryst. A24 (1968), 351-359. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Siemens P4' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 8.10 _diffrn_reflns_number 30685 _diffrn_reflns_av_R_equivalents 0.0729 _diffrn_reflns_av_sigmaI/netI 0.0784 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 25032 _reflns_number_gt 13931 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCAnS 2.20 (Siemens An. X-Ray Instr.,1996)' _computing_cell_refinement 'XSCAnS 2.20 (Siemens An. X-Ray Instr.,1996)' _computing_data_reduction 'XSCAnS 2.20 (Siemens An. X-Ray Instr.,1996)' _computing_structure_solution 'SHELXTL 5.1 (Bruker AXS, 1998)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS, 1998)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS, 1998)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS, 1998)' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00040(12) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 25032 _refine_ls_number_parameters 1759 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1536 _refine_ls_R_factor_gt 0.0823 _refine_ls_wR_factor_ref 0.2464 _refine_ls_wR_factor_gt 0.2041 _refine_ls_goodness_of_fit_ref 1.304 _refine_ls_restrained_S_all 1.304 _refine_ls_shift/su_max 0.306 _refine_ls_shift/su_mean 0.015 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 Ba1 Ba 0.69397(3) 0.37890(3) 0.24395(3) 0.04401(17) Uani 1 1 d . . . Fe1 Fe 0.50370(8) 0.36342(8) 0.27944(8) 0.0522(4) Uani 1 1 d . . . Fe2 Fe 0.88677(8) 0.39190(8) 0.21044(8) 0.0534(4) Uani 1 1 d . . . N1 N 0.6427(4) 0.4030(4) 0.1335(4) 0.0431(19) Uani 1 1 d . . . N2 N 0.7357(5) 0.4834(4) 0.3664(4) 0.049(2) Uani 1 1 d . . . N3 N 0.7140(5) 0.2525(4) 0.2511(4) 0.048(2) Uani 1 1 d . . . O1 O 0.5444(4) 0.3858(4) 0.2102(3) 0.0499(17) Uani 1 1 d . . . O2 O 0.4185(4) 0.3163(4) 0.2139(4) 0.061(2) Uani 1 1 d . . . O3 O 0.7883(3) 0.3964(3) 0.1613(3) 0.0467(16) Uani 1 1 d . . . O4 O 0.9301(4) 0.4546(4) 0.1782(4) 0.062(2) Uani 1 1 d . . . O5 O 0.5963(4) 0.4222(3) 0.3334(3) 0.0483(17) Uani 1 1 d . . . O6 O 0.4487(4) 0.4397(4) 0.3221(4) 0.070(2) Uani 1 1 d . . . O7 O 0.8383(4) 0.4485(3) 0.2857(3) 0.0501(17) Uani 1 1 d . . . O8 O 0.9781(4) 0.4086(4) 0.2710(4) 0.073(2) Uani 1 1 d . . . O9 O 0.5792(4) 0.2971(4) 0.2607(3) 0.0536(18) Uani 1 1 d . . . O10 O 0.4640(4) 0.3205(4) 0.3330(4) 0.058(2) Uani 1 1 d . . . O11 O 0.8241(4) 0.3210(3) 0.2252(4) 0.0526(18) Uani 1 1 d . . . O12 O 0.9314(4) 0.3183(4) 0.1502(4) 0.065(2) Uani 1 1 d . . . C1 C 0.6908(6) 0.4268(5) 0.1039(5) 0.049(3) Uani 1 1 d . . . C2 C 0.6681(6) 0.4480(7) 0.0565(5) 0.066(3) Uani 1 1 d . . . H2A H 0.7033 0.4654 0.0377 0.079 Uiso 1 1 calc R . . C3 C 0.5908(6) 0.4425(7) 0.0379(6) 0.067(3) Uani 1 1 d . . . H3A H 0.5735 0.4555 0.0056 0.081 Uiso 1 1 calc R . . C4 C 0.5406(6) 0.4179(6) 0.0673(5) 0.057(3) Uani 1 1 d . . . H4A H 0.4889 0.4140 0.0551 0.069 Uiso 1 1 calc R . . C5 C 0.5672(6) 0.3986(6) 0.1160(5) 0.051(3) Uani 1 1 d . . . C6 C 0.5171(5) 0.3735(5) 0.1528(5) 0.049(3) Uani 1 1 d . . . C7 C 0.4463(6) 0.3386(6) 0.1250(6) 0.062(3) Uani 1 1 d . . . H7A H 0.4286 0.3343 0.0843 0.075 Uiso 1 1 calc R . . C8 C 0.4014(6) 0.3099(6) 0.1571(6) 0.055(3) Uani 1 1 d . . . C9 C 0.3316(7) 0.2623(7) 0.1220(8) 0.085(5) Uani 1 1 d . . . C10 C 0.2883(8) 0.2810(8) 0.0769(8) 0.109(6) Uani 1 1 d . . . H10A H 0.2665 0.3207 0.0989 0.164 Uiso 1 1 calc R . . H10B H 0.2486 0.2466 0.0534 0.164 Uiso 1 1 calc R . . H10C H 0.3208 0.2882 0.0483 0.164 Uiso 1 1 calc R . . C11 C 0.3590(13) 0.1985(10) 0.080(2) 0.39(3) Uani 1 1 d . . . H11A H 0.3162 0.1673 0.0571 0.591 Uiso 1 1 calc R . . H11B H 0.3887 0.1813 0.1056 0.591 Uiso 1 1 calc R . . H11C H 0.3894 0.2066 0.0505 0.591 Uiso 1 1 calc R . . C12 C 0.2857(13) 0.248(2) 0.1615(12) 0.39(3) Uani 1 1 d . . . H12A H 0.2697 0.2881 0.1901 0.589 Uiso 1 1 calc R . . H12B H 0.3132 0.2276 0.1852 0.589 Uiso 1 1 calc R . . H12C H 0.2421 0.2192 0.1368 0.589 Uiso 1 1 calc R . . C13 C 0.7743(6) 0.4314(5) 0.1276(5) 0.046(2) Uani 1 1 d . . . C14 C 0.8277(6) 0.4691(6) 0.1137(5) 0.057(3) Uani 1 1 d . . . H14A H 0.8128 0.4882 0.0854 0.068 Uiso 1 1 calc R . . C15 C 0.9042(6) 0.4812(6) 0.1396(5) 0.054(3) Uani 1 1 d . . . C16 C 0.9626(6) 0.5255(6) 0.1268(6) 0.063(3) Uani 1 1 d . . . C17 C 1.0347(8) 0.4908(10) 0.1116(9) 0.126(7) Uani 1 1 d . . . H17A H 1.0527 0.4794 0.1463 0.188 Uiso 1 1 calc R . . H17B H 1.0730 0.5197 0.1053 0.188 Uiso 1 1 calc R . . H17C H 1.0233 0.4517 0.0739 0.188 Uiso 1 1 calc R . . C18 C 0.9343(8) 0.5449(7) 0.0716(7) 0.088(5) Uani 1 1 d . . . H18A H 0.8899 0.5671 0.0813 0.133 Uiso 1 1 calc R . . H18B H 0.9224 0.5061 0.0336 0.133 Uiso 1 1 calc R . . H18C H 0.9732 0.5734 0.0654 0.133 Uiso 1 1 calc R . . C19 C 0.9798(10) 0.5892(8) 0.1872(7) 0.113(6) Uani 1 1 d . . . H19A H 0.9346 0.6105 0.1958 0.170 Uiso 1 1 calc R . . H19B H 1.0181 0.6180 0.1809 0.170 Uiso 1 1 calc R . . H19C H 0.9973 0.5784 0.2224 0.170 Uiso 1 1 calc R . . C20 C 0.8089(6) 0.5084(6) 0.3877(5) 0.053(3) Uani 1 1 d . . . C21 C 0.8290(7) 0.5596(6) 0.4459(6) 0.068(3) Uani 1 1 d . . . H21A H 0.8797 0.5748 0.4606 0.082 Uiso 1 1 calc R . . C22 C 0.7728(8) 0.5879(7) 0.4818(6) 0.083(4) Uani 1 1 d . . . H22A H 0.7850 0.6235 0.5202 0.100 Uiso 1 1 calc R . . C23 C 0.6985(7) 0.5627(6) 0.4599(5) 0.064(3) Uani 1 1 d . . . H23A H 0.6599 0.5801 0.4840 0.077 Uiso 1 1 calc R . . C24 C 0.6820(6) 0.5116(5) 0.4021(5) 0.050(3) Uani 1 1 d . . . C25 C 0.6024(6) 0.4824(5) 0.3738(5) 0.049(3) Uani 1 1 d . . . C26 C 0.5416(6) 0.5192(6) 0.3927(6) 0.061(3) Uani 1 1 d . . . H26A H 0.5512 0.5612 0.4241 0.073 Uiso 1 1 calc R . . C27 C 0.4680(6) 0.4953(6) 0.3665(6) 0.060(3) Uani 1 1 d . . . C28 C 0.4038(8) 0.5373(7) 0.3889(8) 0.086(4) Uani 1 1 d . . . C29 C 0.4189(11) 0.5987(10) 0.3888(15) 0.231(16) Uani 1 1 d . . . H29A H 0.4630 0.6210 0.4180 0.347 Uiso 1 1 calc R . . H29B H 0.3765 0.6230 0.4013 0.347 Uiso 1 1 calc R . . H29C H 0.4278 0.5951 0.3471 0.347 Uiso 1 1 calc R . . C30 C 0.3321(9) 0.5060(11) 0.3448(15) 0.252(18) Uani 1 1 d . . . H30A H 0.2922 0.5333 0.3584 0.377 Uiso 1 1 calc R . . H30B H 0.3181 0.4636 0.3455 0.377 Uiso 1 1 calc R . . H30C H 0.3402 0.5012 0.3026 0.377 Uiso 1 1 calc R . . C31 C 0.3935(17) 0.5402(17) 0.4508(13) 0.31(2) Uani 1 1 d . . . H31A H 0.4395 0.5593 0.4785 0.469 Uiso 1 1 calc R . . H31B H 0.3806 0.4966 0.4490 0.469 Uiso 1 1 calc R . . H31C H 0.3535 0.5665 0.4664 0.469 Uiso 1 1 calc R . . C32 C 0.8661(6) 0.4755(6) 0.3436(5) 0.057(3) Uani 1 1 d . . . C33 C 0.9394(7) 0.4767(7) 0.3669(6) 0.072(4) Uani 1 1 d . . . H33A H 0.9545 0.5000 0.4098 0.087 Uiso 1 1 calc R . . C34 C 0.9926(6) 0.4441(8) 0.3283(7) 0.080(4) Uani 1 1 d . . . C35 C 1.0769(8) 0.4486(11) 0.3552(8) 0.121(7) Uani 1 1 d . . . C36 C 1.0919(9) 0.4894(11) 0.4238(9) 0.160(10) Uani 1 1 d . . . H36A H 1.0683 0.4668 0.4470 0.240 Uiso 1 1 calc R . . H36B H 1.0715 0.5304 0.4323 0.240 Uiso 1 1 calc R . . H36C H 1.1455 0.4973 0.4364 0.240 Uiso 1 1 calc R . . C37 C 1.0937(14) 0.3821(13) 0.3386(15) 0.29(2) Uani 1 1 d . . . H37A H 1.0659 0.3623 0.3621 0.434 Uiso 1 1 calc R . . H37B H 1.1469 0.3817 0.3485 0.434 Uiso 1 1 calc R . . H37C H 1.0793 0.3578 0.2941 0.434 Uiso 1 1 calc R . . C38 C 1.1187(10) 0.4871(16) 0.3197(11) 0.244(17) Uani 1 1 d . . . H38A H 1.1722 0.4929 0.3326 0.366 Uiso 1 1 calc R . . H38B H 1.1004 0.5292 0.3300 0.366 Uiso 1 1 calc R . . H38C H 1.1090 0.4625 0.2749 0.366 Uiso 1 1 calc R . . C39 C 0.7780(6) 0.2223(5) 0.2311(5) 0.048(2) Uani 1 1 d . . . C40 C 0.7858(7) 0.1591(6) 0.2308(5) 0.061(3) Uani 1 1 d . . . H40A H 0.8297 0.1395 0.2194 0.074 Uiso 1 1 calc R . . C41 C 0.7282(7) 0.1274(6) 0.2472(6) 0.064(3) Uani 1 1 d . . . H41A H 0.7320 0.0849 0.2451 0.077 Uiso 1 1 calc R . . C42 C 0.6647(7) 0.1570(6) 0.2669(5) 0.059(3) Uani 1 1 d . . . H42A H 0.6265 0.1359 0.2798 0.071 Uiso 1 1 calc R . . C43 C 0.6590(6) 0.2197(5) 0.2670(5) 0.048(2) Uani 1 1 d . . . C44 C 0.5909(5) 0.2547(5) 0.2854(5) 0.045(2) Uani 1 1 d . . . C45 C 0.5465(6) 0.2413(6) 0.3264(5) 0.058(3) Uani 1 1 d . . . H45A H 0.5591 0.2090 0.3409 0.069 Uiso 1 1 calc R . . C46 C 0.4829(7) 0.2744(5) 0.3473(5) 0.056(3) Uani 1 1 d . . . C47 C 0.4341(10) 0.2553(8) 0.3893(8) 0.098(5) Uani 1 1 d . . . C48 C 0.3999(15) 0.1907(12) 0.3574(15) 0.261(19) Uani 1 1 d . . . H48A H 0.3650 0.1885 0.3224 0.392 Uiso 1 1 calc R . . H48B H 0.3732 0.1774 0.3860 0.392 Uiso 1 1 calc R . . H48C H 0.4381 0.1621 0.3421 0.392 Uiso 1 1 calc R . . C49 C 0.3817(13) 0.3035(11) 0.4126(11) 0.205(14) Uani 1 1 d . . . H49A H 0.3470 0.3024 0.3779 0.308 Uiso 1 1 calc R . . H49B H 0.4092 0.3464 0.4327 0.308 Uiso 1 1 calc R . . H49C H 0.3540 0.2937 0.4427 0.308 Uiso 1 1 calc R . . C50 C 0.4892(16) 0.2546(17) 0.4464(11) 0.255(17) Uani 1 1 d . . . H50A H 0.4603 0.2423 0.4744 0.383 Uiso 1 1 calc R . . H50B H 0.5158 0.2975 0.4690 0.383 Uiso 1 1 calc R . . H50C H 0.5249 0.2236 0.4305 0.383 Uiso 1 1 calc R . . C51 C 0.8331(6) 0.2602(5) 0.2114(5) 0.049(2) Uani 1 1 d . . . C52 C 0.8900(6) 0.2301(6) 0.1756(6) 0.065(3) Uani 1 1 d . . . H52A H 0.8965 0.1872 0.1706 0.078 Uiso 1 1 calc R . . C53 C 0.9369(6) 0.2601(7) 0.1475(6) 0.065(3) Uani 1 1 d . . . C54 C 0.9959(8) 0.2237(8) 0.1091(8) 0.090(5) Uani 1 1 d . . . C55 C 0.9798(16) 0.2219(13) 0.0420(10) 0.241(17) Uani 1 1 d . . . H55A H 0.9794 0.2659 0.0438 0.361 Uiso 1 1 calc R . . H55B H 0.9314 0.1975 0.0230 0.361 Uiso 1 1 calc R . . H55C H 1.0184 0.2012 0.0172 0.361 Uiso 1 1 calc R . . C56 C 0.9961(12) 0.1529(10) 0.1013(11) 0.188(12) Uani 1 1 d . . . H56A H 1.0076 0.1508 0.1420 0.283 Uiso 1 1 calc R . . H56B H 1.0336 0.1333 0.0746 0.283 Uiso 1 1 calc R . . H56C H 0.9471 0.1296 0.0825 0.283 Uiso 1 1 calc R . . C57 C 1.0686(11) 0.2586(14) 0.1372(15) 0.32(2) Uani 1 1 d . . . H57A H 1.0787 0.2590 0.1790 0.476 Uiso 1 1 calc R . . H57B H 1.0693 0.3029 0.1396 0.476 Uiso 1 1 calc R . . H57C H 1.1066 0.2374 0.1119 0.476 Uiso 1 1 calc R . . O120 O 0.6796(5) 0.5179(4) 0.2583(4) 0.077(3) Uani 1 1 d . . . C121 C 0.6128(9) 0.5484(7) 0.2486(7) 0.092(5) Uani 1 1 d . . . H12D H 0.5961 0.5744 0.2888 0.110 Uiso 1 1 calc R . . H12E H 0.5718 0.5154 0.2233 0.110 Uiso 1 1 calc R . . C122 C 0.6380(10) 0.5917(7) 0.2141(7) 0.100(6) Uani 1 1 d . . . H12F H 0.6282 0.5681 0.1686 0.121 Uiso 1 1 calc R . . H12G H 0.6119 0.6308 0.2260 0.121 Uiso 1 1 calc R . . C123 C 0.7211(10) 0.6091(8) 0.2346(8) 0.109(6) Uani 1 1 d . . . H12H H 0.7325 0.6557 0.2596 0.131 Uiso 1 1 calc R . . H12I H 0.7492 0.5976 0.1982 0.131 Uiso 1 1 calc R . . C124 C 0.7420(8) 0.5689(6) 0.2749(7) 0.082(4) Uani 1 1 d . . . H12J H 0.7891 0.5502 0.2647 0.098 Uiso 1 1 calc R . . H12K H 0.7470 0.5962 0.3197 0.098 Uiso 1 1 calc R . . O130 O 0.6611(5) 0.2611(4) 0.1231(4) 0.073(2) Uani 1 1 d . . . C131 C 0.7009(8) 0.2468(7) 0.0707(7) 0.087(4) Uani 1 1 d . . . H13A H 0.7503 0.2349 0.0803 0.105 Uiso 1 1 calc R . . H13B H 0.7082 0.2852 0.0603 0.105 Uiso 1 1 calc R . . C132 C 0.6580(8) 0.1913(8) 0.0155(6) 0.088(4) Uani 1 1 d . . . H13C H 0.6409 0.2060 -0.0176 0.105 Uiso 1 1 calc R . . H13D H 0.6892 0.1561 -0.0017 0.105 Uiso 1 1 calc R . . C133 C 0.5923(9) 0.1691(8) 0.0414(6) 0.099(5) Uani 1 1 d . . . H13E H 0.5451 0.1772 0.0229 0.118 Uiso 1 1 calc R . . H13F H 0.5907 0.1226 0.0326 0.118 Uiso 1 1 calc R . . C134 C 0.6040(9) 0.2070(7) 0.1086(7) 0.095(5) Uani 1 1 d . . . H13G H 0.5570 0.2233 0.1230 0.115 Uiso 1 1 calc R . . H13H H 0.6194 0.1793 0.1305 0.115 Uiso 1 1 calc R . . Fe5 Fe 0.40165(10) 0.23882(9) -0.37943(8) 0.0634(5) Uani 1 1 d . . . Cl51 Cl 0.3490(2) 0.2996(2) -0.42332(19) 0.0967(13) Uani 1 1 d . . . Cl52 Cl 0.4545(2) 0.1613(2) -0.44972(18) 0.0925(11) Uani 1 1 d . . . Cl53 Cl 0.4915(2) 0.2942(2) -0.30471(19) 0.1115(15) Uani 1 1 d . . . Cl54 Cl 0.3111(2) 0.1979(2) -0.3422(2) 0.1018(13) Uani 1 1 d . . . Fe6 Fe 0.20830(11) 0.01724(11) -0.08316(10) 0.0777(6) Uani 1 1 d . . . Cl61 Cl 0.16285(18) 0.08732(17) -0.00090(16) 0.0734(9) Uani 1 1 d . . . Cl62 Cl 0.2443(3) -0.06422(19) -0.06137(18) 0.0958(12) Uani 1 1 d . . . Cl63 Cl 0.1167(4) -0.0193(3) -0.1616(2) 0.166(3) Uani 1 1 d . . . Cl64 Cl 0.3016(4) 0.0623(4) -0.1095(5) 0.243(5) Uani 1 1 d . . . Ba2 Ba 0.80719(3) 0.12761(3) -0.25243(3) 0.04282(16) Uani 1 1 d . . . Fe3 Fe 0.99863(8) 0.15665(8) -0.28300(7) 0.0498(4) Uani 1 1 d . . . Fe4 Fe 0.61890(7) 0.09538(8) -0.21970(7) 0.0451(4) Uani 1 1 d . . . N4 N 0.8641(4) 0.0885(4) -0.1499(4) 0.046(2) Uani 1 1 d . . . N5 N 0.7746(4) 0.2504(4) -0.2548(4) 0.0384(18) Uani 1 1 d . . . N6 N 0.7893(5) 0.0059(4) -0.3627(4) 0.050(2) Uani 1 1 d . . . O13 O 0.9570(3) 0.1238(4) -0.2210(3) 0.0504(18) Uani 1 1 d . . . O14 O 1.0748(4) 0.2098(4) -0.2113(4) 0.057(2) Uani 1 1 d . . . O15 O 0.7182(3) 0.0973(4) -0.1679(3) 0.0487(17) Uani 1 1 d . . . O16 O 0.5771(4) 0.0346(4) -0.1829(4) 0.0554(19) Uani 1 1 d . . . O17 O 0.9141(4) 0.2148(4) -0.2672(3) 0.0494(17) Uani 1 1 d . . . O18 O 1.0307(4) 0.2018(4) -0.3372(3) 0.057(2) Uani 1 1 d . . . O19 O 0.6719(3) 0.1713(3) -0.2321(3) 0.0439(16) Uani 1 1 d . . . O20 O 0.5593(4) 0.1621(4) -0.1651(3) 0.0546(18) Uani 1 1 d . . . O21 O 0.9175(4) 0.0879(4) -0.3412(3) 0.0534(18) Uani 1 1 d . . . O22 O 1.0707(4) 0.0920(4) -0.3167(4) 0.064(2) Uani 1 1 d . . . O23 O 0.6789(4) 0.0411(4) -0.2896(3) 0.0512(18) Uani 1 1 d . . . O24 O 0.5335(3) 0.0639(4) -0.2870(3) 0.0495(17) Uani 1 1 d . . . C58 C 0.8180(5) 0.0597(6) -0.1233(5) 0.049(3) Uani 1 1 d . . . C59 C 0.8452(6) 0.0316(6) -0.0811(6) 0.061(3) Uani 1 1 d . . . H59A H 0.8122 0.0115 -0.0629 0.073 Uiso 1 1 calc R . . C60 C 0.9235(7) 0.0351(7) -0.0674(6) 0.078(4) Uani 1 1 d . . . H60A H 0.9435 0.0165 -0.0402 0.094 Uiso 1 1 calc R . . C61 C 0.9704(6) 0.0658(6) -0.0940(5) 0.061(3) Uani 1 1 d . . . H61A H 1.0226 0.0686 -0.0848 0.074 Uiso 1 1 calc R . . C62 C 0.9403(5) 0.0930(5) -0.1351(5) 0.050(3) Uani 1 1 d . . . C63 C 0.9859(5) 0.1278(6) -0.1660(5) 0.052(3) Uani 1 1 d . . . C64 C 1.0540(5) 0.1632(6) -0.1367(6) 0.058(3) Uani 1 1 d . . . H64A H 1.0745 0.1587 -0.1002 0.070 Uiso 1 1 calc R . . C65 C 1.0952(6) 0.2060(6) -0.1578(6) 0.054(3) Uani 1 1 d . . . C66 C 1.1645(6) 0.2501(6) -0.1180(6) 0.063(3) Uani 1 1 d . . . C67 C 1.1389(7) 0.2981(7) -0.0567(7) 0.087(4) Uani 1 1 d . . . H67A H 1.1030 0.3240 -0.0669 0.130 Uiso 1 1 calc R . . H67B H 1.1820 0.3265 -0.0302 0.130 Uiso 1 1 calc R . . H67C H 1.1158 0.2739 -0.0347 0.130 Uiso 1 1 calc R . . C68 C 1.2216(6) 0.2093(7) -0.1020(7) 0.080(4) Uani 1 1 d . . . H68A H 1.2376 0.1794 -0.1403 0.119 Uiso 1 1 calc R . . H68B H 1.1987 0.1849 -0.0801 0.119 Uiso 1 1 calc R . . H68C H 1.2646 0.2377 -0.0755 0.119 Uiso 1 1 calc R . . C69 C 1.1999(7) 0.2892(8) -0.1522(7) 0.088(5) Uani 1 1 d . . . H69A H 1.2158 0.2597 -0.1908 0.132 Uiso 1 1 calc R . . H69B H 1.2429 0.3177 -0.1258 0.132 Uiso 1 1 calc R . . H69C H 1.1634 0.3150 -0.1618 0.132 Uiso 1 1 calc R . . C70 C 0.7348(5) 0.0588(5) -0.1395(5) 0.044(2) Uani 1 1 d . . . C71 C 0.6828(6) 0.0187(6) -0.1252(5) 0.054(3) Uani 1 1 d . . . H71A H 0.7004 -0.0038 -0.1008 0.064 Uiso 1 1 calc R . . C72 C 0.6060(5) 0.0101(5) -0.1453(5) 0.047(2) Uani 1 1 d . . . C73 C 0.5503(6) -0.0327(6) -0.1269(5) 0.054(3) Uani 1 1 d . . . C74 C 0.5394(9) -0.1000(7) -0.1819(6) 0.093(5) Uani 1 1 d . . . H74A H 0.5868 -0.1183 -0.1865 0.140 Uiso 1 1 calc R . . H74B H 0.5217 -0.0950 -0.2202 0.140 Uiso 1 1 calc R . . H74C H 0.5030 -0.1287 -0.1734 0.140 Uiso 1 1 calc R . . C75 C 0.4749(7) -0.0029(8) -0.1181(8) 0.098(5) Uani 1 1 d . . . H75A H 0.4823 0.0389 -0.0832 0.146 Uiso 1 1 calc R . . H75B H 0.4385 -0.0318 -0.1097 0.146 Uiso 1 1 calc R . . H75C H 0.4566 0.0028 -0.1560 0.146 Uiso 1 1 calc R . . C76 C 0.5796(7) -0.0408(7) -0.0667(6) 0.073(4) Uani 1 1 d . . . H76A H 0.5857 0.0010 -0.0319 0.110 Uiso 1 1 calc R . . H76B H 0.6275 -0.0583 -0.0717 0.110 Uiso 1 1 calc R . . H76C H 0.5441 -0.0704 -0.0584 0.110 Uiso 1 1 calc R . . C77 C 0.7089(5) 0.2740(5) -0.2371(4) 0.045(2) Uani 1 1 d . . . C78 C 0.6886(6) 0.3318(5) -0.2412(5) 0.054(3) Uani 1 1 d . . . H78A H 0.6419 0.3462 -0.2308 0.065 Uiso 1 1 calc R . . C79 C 0.7401(6) 0.3671(5) -0.2611(5) 0.057(3) Uani 1 1 d . . . H79A H 0.7287 0.4068 -0.2628 0.069 Uiso 1 1 calc R . . C80 C 0.8086(6) 0.3444(5) -0.2787(5) 0.052(3) Uani 1 1 d . . . H80A H 0.8428 0.3677 -0.2931 0.063 Uiso 1 1 calc R . . C81 C 0.8247(5) 0.2854(5) -0.2741(5) 0.046(2) Uani 1 1 d . . . C82 C 0.8963(5) 0.2555(5) -0.2934(4) 0.041(2) Uani 1 1 d . . . C83 C 0.9350(6) 0.2698(5) -0.3349(5) 0.051(3) Uani 1 1 d . . . H83A H 0.9161 0.2987 -0.3515 0.061 Uiso 1 1 calc R . . C84 C 1.0033(5) 0.2436(5) -0.3552(5) 0.049(3) Uani 1 1 d . . . C85 C 1.0451(7) 0.2628(7) -0.4009(6) 0.075(4) Uani 1 1 d . . . C86 C 1.0050(16) 0.2173(13) -0.4653(9) 0.213(13) Uani 1 1 d . . . H86A H 1.0102 0.1725 -0.4712 0.319 Uiso 1 1 calc R . . H86B H 1.0271 0.2270 -0.4978 0.319 Uiso 1 1 calc R . . H86C H 0.9523 0.2236 -0.4673 0.319 Uiso 1 1 calc R . . C87 C 1.0350(12) 0.3294(10) -0.3979(12) 0.194(13) Uani 1 1 d . . . H87A H 1.0599 0.3612 -0.3585 0.291 Uiso 1 1 calc R . . H87B H 0.9820 0.3344 -0.4009 0.291 Uiso 1 1 calc R . . H87C H 1.0565 0.3358 -0.4323 0.291 Uiso 1 1 calc R . . C88 C 1.1241(10) 0.2490(15) -0.3973(13) 0.244(18) Uani 1 1 d . . . H88A H 1.1503 0.2774 -0.3569 0.366 Uiso 1 1 calc R . . H88B H 1.1479 0.2565 -0.4303 0.366 Uiso 1 1 calc R . . H88C H 1.1259 0.2041 -0.4022 0.366 Uiso 1 1 calc R . . C89 C 0.6579(5) 0.2317(5) -0.2159(5) 0.047(2) Uani 1 1 d . . . C90 C 0.5971(5) 0.2578(6) -0.1829(5) 0.054(3) Uani 1 1 d . . . H90A H 0.5877 0.3005 -0.1761 0.064 Uiso 1 1 calc R . . C91 C 0.5510(6) 0.2207(6) -0.1604(5) 0.054(3) Uani 1 1 d . . . C92 C 0.4800(6) 0.2458(6) -0.1303(5) 0.059(3) Uani 1 1 d . . . C93 C 0.4764(10) 0.2374(11) -0.0693(8) 0.146(9) Uani 1 1 d . . . H93A H 0.5187 0.2632 -0.0396 0.218 Uiso 1 1 calc R . . H93B H 0.4781 0.1919 -0.0762 0.218 Uiso 1 1 calc R . . H93C H 0.4301 0.2514 -0.0527 0.218 Uiso 1 1 calc R . . C94 C 0.4109(8) 0.2047(10) -0.1784(8) 0.151(9) Uani 1 1 d . . . H94A H 0.4128 0.1590 -0.1866 0.227 Uiso 1 1 calc R . . H94B H 0.4125 0.2114 -0.2172 0.227 Uiso 1 1 calc R . . H94C H 0.3649 0.2183 -0.1611 0.227 Uiso 1 1 calc R . . C95 C 0.4730(10) 0.3180(8) -0.1194(9) 0.122(7) Uani 1 1 d . . . H95A H 0.5149 0.3453 -0.0903 0.183 Uiso 1 1 calc R . . H95B H 0.4265 0.3303 -0.1021 0.183 Uiso 1 1 calc R . . H95C H 0.4731 0.3234 -0.1589 0.183 Uiso 1 1 calc R . . C96 C 0.7198(6) -0.0281(5) -0.3857(6) 0.054(3) Uani 1 1 d . . . C97 C 0.7066(7) -0.0832(6) -0.4398(6) 0.075(4) Uani 1 1 d . . . H97A H 0.6581 -0.1050 -0.4542 0.090 Uiso 1 1 calc R . . C98 C 0.7667(7) -0.1060(7) -0.4729(7) 0.085(4) Uani 1 1 d . . . H98A H 0.7596 -0.1435 -0.5100 0.103 Uiso 1 1 calc R . . C99 C 0.8380(6) -0.0717(6) -0.4496(6) 0.069(4) Uani 1 1 d . . . H99A H 0.8796 -0.0866 -0.4706 0.083 Uiso 1 1 calc R . . C100 C 0.8471(6) -0.0161(6) -0.3958(6) 0.059(3) Uani 1 1 d . . . C101 C 0.9211(6) 0.0259(6) -0.3685(5) 0.052(3) Uani 1 1 d . . . C102 C 0.9887(6) -0.0037(6) -0.3757(7) 0.075(4) Uani 1 1 d . . . H10D H 0.9861 -0.0486 -0.3992 0.090 Uiso 1 1 calc R . . C103 C 1.0593(6) 0.0311(6) -0.3493(6) 0.064(3) Uani 1 1 d . . . C104 C 1.1334(7) -0.0020(7) -0.3592(9) 0.097(5) Uani 1 1 d . . . C105 C 1.1201(11) -0.0706(10) -0.3671(19) 0.31(2) Uani 1 1 d . . . H10E H 1.0837 -0.0938 -0.4035 0.468 Uiso 1 1 calc R . . H10F H 1.1010 -0.0730 -0.3301 0.468 Uiso 1 1 calc R . . H10G H 1.1667 -0.0901 -0.3731 0.468 Uiso 1 1 calc R . . C106 C 1.1655(11) 0.0144(15) -0.4106(9) 0.223(16) Uani 1 1 d . . . H10H H 1.1323 -0.0063 -0.4493 0.335 Uiso 1 1 calc R . . H10I H 1.2144 -0.0012 -0.4164 0.335 Uiso 1 1 calc R . . H10J H 1.1705 0.0611 -0.3987 0.335 Uiso 1 1 calc R . . C107 C 1.1919(9) 0.0325(11) -0.3001(9) 0.151(9) Uani 1 1 d . . . H10K H 1.2375 0.0113 -0.3061 0.226 Uiso 1 1 calc R . . H10L H 1.1715 0.0297 -0.2637 0.226 Uiso 1 1 calc R . . H10M H 1.2031 0.0777 -0.2937 0.226 Uiso 1 1 calc R . . C108 C 0.6578(5) 0.0018(5) -0.3469(5) 0.049(3) Uani 1 1 d . . . C109 C 0.5832(6) -0.0136(6) -0.3751(5) 0.057(3) Uani 1 1 d . . . H10N H 0.5720 -0.0451 -0.4161 0.068 Uiso 1 1 calc R . . C110 C 0.5243(6) 0.0179(5) -0.3424(5) 0.051(3) Uani 1 1 d . . . C111 C 0.4410(6) -0.0020(6) -0.3723(6) 0.063(3) Uani 1 1 d . . . C112 C 0.3971(8) 0.0559(9) -0.3475(9) 0.141(8) Uani 1 1 d . . . H11D H 0.3978 0.0693 -0.3025 0.212 Uiso 1 1 calc R . . H11E H 0.3458 0.0440 -0.3672 0.212 Uiso 1 1 calc R . . H11F H 0.4197 0.0914 -0.3567 0.212 Uiso 1 1 calc R . . C113 C 0.4117(9) -0.0554(11) -0.3550(14) 0.219(16) Uani 1 1 d . . . H11G H 0.4162 -0.0408 -0.3097 0.328 Uiso 1 1 calc R . . H11H H 0.4403 -0.0920 -0.3719 0.328 Uiso 1 1 calc R . . H11I H 0.3595 -0.0685 -0.3719 0.328 Uiso 1 1 calc R . . C114 C 0.4343(9) -0.0208(12) -0.4431(8) 0.171(11) Uani 1 1 d . . . H11J H 0.3821 -0.0331 -0.4604 0.256 Uiso 1 1 calc R . . H11K H 0.4628 -0.0570 -0.4619 0.256 Uiso 1 1 calc R . . H11L H 0.4538 0.0160 -0.4521 0.256 Uiso 1 1 calc R . . O220 O 0.8411(5) 0.2359(4) -0.1296(4) 0.067(2) Uani 1 1 d . . . C221 C 0.8908(9) 0.2923(7) -0.1150(6) 0.095(5) Uani 1 1 d . . . H22B H 0.8702 0.3197 -0.1353 0.114 Uiso 1 1 calc R . . H22C H 0.9388 0.2804 -0.1305 0.114 Uiso 1 1 calc R . . C222 C 0.9024(8) 0.3285(7) -0.0465(6) 0.087(4) Uani 1 1 d . . . H22D H 0.9083 0.3755 -0.0358 0.105 Uiso 1 1 calc R . . H22E H 0.9467 0.3166 -0.0276 0.105 Uiso 1 1 calc R . . C223 C 0.8309(8) 0.3075(7) -0.0249(6) 0.085(4) Uani 1 1 d . . . H22F H 0.8422 0.3003 0.0138 0.102 Uiso 1 1 calc R . . H22G H 0.7957 0.3403 -0.0178 0.102 Uiso 1 1 calc R . . C224 C 0.7998(8) 0.2460(7) -0.0772(6) 0.091(5) Uani 1 1 d . . . H22H H 0.8028 0.2096 -0.0637 0.109 Uiso 1 1 calc R . . H22I H 0.7469 0.2481 -0.0894 0.109 Uiso 1 1 calc R . . O230 O 0.7272(5) 0.1261(5) -0.3720(4) 0.082(3) Uani 1 1 d . . . C231 C 0.7686(8) 0.1189(8) -0.4245(7) 0.096(5) Uani 1 1 d . . . H23B H 0.7580 0.0745 -0.4560 0.115 Uiso 1 1 calc R . . H23C H 0.8225 0.1274 -0.4105 0.115 Uiso 1 1 calc R . . C232 C 0.7454(8) 0.1667(8) -0.4528(7) 0.093(5) Uani 1 1 d . . . H23D H 0.7348 0.1455 -0.4985 0.112 Uiso 1 1 calc R . . H23E H 0.7846 0.2032 -0.4422 0.112 Uiso 1 1 calc R . . C233 C 0.6751(9) 0.1895(8) -0.4232(7) 0.099(5) Uani 1 1 d . . . H23F H 0.6342 0.1849 -0.4556 0.119 Uiso 1 1 calc R . . H23G H 0.6843 0.2352 -0.3946 0.119 Uiso 1 1 calc R . . C234 C 0.6545(7) 0.1463(6) -0.3871(6) 0.074(4) Uani 1 1 d . . . H23H H 0.6327 0.1710 -0.3490 0.088 Uiso 1 1 calc R . . H23I H 0.6190 0.1087 -0.4133 0.088 Uiso 1 1 calc R . . Fe7 Fe 0.30683(11) 0.49194(9) 0.09870(9) 0.0676(5) Uani 1 1 d . . . Cl71 Cl 0.4153(3) 0.5376(3) 0.1509(3) 0.187(3) Uani 1 1 d . . . Cl72 Cl 0.2432(3) 0.5647(2) 0.08034(19) 0.1116(15) Uani 1 1 d . . . Cl73 Cl 0.3292(2) 0.41626(17) 0.00813(16) 0.0770(9) Uani 1 1 d . . . Cl74 Cl 0.2397(4) 0.4529(3) 0.1530(3) 0.174(3) Uani 1 1 d . . . Fe8 Fe 0.8076(3) 0.31275(18) 0.45792(13) 0.1803(19) Uani 1 1 d . . . Cl81 Cl 0.8043(3) 0.3416(2) 0.55892(19) 0.1019(13) Uani 1 1 d . A . Cl82 Cl 0.7404(3) 0.3652(2) 0.4176(2) 0.1290(18) Uani 1 1 d . A . Cl83 Cl 0.8139(8) 0.2200(4) 0.4125(4) 0.141(6) Uani 0.541(11) 1 d P A 1 Cl84 Cl 0.9427(7) 0.3686(7) 0.4584(6) 0.168(6) Uani 0.541(11) 1 d P A 1 Cl85 Cl 0.7171(12) 0.2062(7) 0.4182(6) 0.228(12) Uani 0.459(11) 1 d P A 2 Cl86 Cl 0.8934(12) 0.2821(17) 0.4175(9) 0.31(2) Uani 0.459(11) 1 d P A 2 C300 C 1.061(2) 0.123(3) 0.279(2) 0.52(3) Uani 0.50 1 d PD . . Cl31 Cl 1.094(3) 0.196(2) 0.347(2) 0.73(5) Uani 0.50 1 d PD . . Cl32 Cl 1.154(3) 0.1083(18) 0.2584(15) 0.51(3) Uani 0.50 1 d PD . . 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 Ba1 0.0336(3) 0.0503(4) 0.0495(4) 0.0204(3) 0.0071(3) 0.0045(3) Fe1 0.0405(8) 0.0667(11) 0.0582(10) 0.0325(8) 0.0124(7) 0.0063(7) Fe2 0.0322(8) 0.0707(11) 0.0636(10) 0.0327(9) 0.0073(7) 0.0048(7) N1 0.031(4) 0.053(5) 0.047(5) 0.022(4) 0.004(4) 0.003(4) N2 0.048(5) 0.057(6) 0.053(5) 0.037(5) -0.006(4) 0.004(4) N3 0.054(5) 0.048(5) 0.050(5) 0.025(4) 0.009(4) 0.020(4) O1 0.037(4) 0.070(5) 0.047(4) 0.028(4) 0.003(3) 0.009(3) O2 0.038(4) 0.087(6) 0.066(5) 0.039(5) 0.006(4) -0.005(4) O3 0.030(3) 0.052(4) 0.058(4) 0.022(4) 0.003(3) -0.001(3) O4 0.037(4) 0.072(5) 0.082(6) 0.037(5) 0.007(4) -0.011(4) O5 0.039(4) 0.051(4) 0.056(4) 0.022(4) 0.007(3) 0.008(3) O6 0.052(5) 0.094(7) 0.083(6) 0.048(5) 0.026(4) 0.023(5) O7 0.046(4) 0.054(4) 0.045(4) 0.016(3) -0.005(3) 0.000(3) O8 0.040(4) 0.095(7) 0.093(7) 0.049(6) -0.008(4) 0.004(4) O9 0.046(4) 0.065(5) 0.059(5) 0.032(4) 0.013(3) 0.005(4) O10 0.049(4) 0.072(5) 0.067(5) 0.042(4) 0.024(4) 0.010(4) O11 0.040(4) 0.055(5) 0.073(5) 0.033(4) 0.013(3) 0.017(3) O12 0.048(4) 0.081(6) 0.075(6) 0.036(5) 0.025(4) 0.018(4) C1 0.040(5) 0.062(7) 0.045(6) 0.021(5) 0.010(5) 0.000(5) C2 0.051(7) 0.102(10) 0.060(7) 0.047(7) 0.013(6) 0.010(7) C3 0.046(6) 0.104(10) 0.071(8) 0.055(8) 0.005(6) 0.007(6) C4 0.048(6) 0.068(8) 0.063(7) 0.037(6) -0.006(5) 0.000(6) C5 0.038(5) 0.068(7) 0.045(6) 0.023(5) 0.003(5) 0.000(5) C6 0.036(5) 0.066(7) 0.056(6) 0.035(6) 0.012(5) 0.016(5) C7 0.043(6) 0.069(8) 0.083(9) 0.043(7) -0.007(6) 0.000(6) C8 0.034(5) 0.058(7) 0.082(8) 0.036(6) 0.002(5) 0.010(5) C9 0.044(7) 0.104(11) 0.132(13) 0.087(10) -0.032(7) -0.023(7) C10 0.068(9) 0.122(13) 0.153(16) 0.092(13) -0.047(10) -0.044(9) C11 0.12(2) 0.073(15) 0.85(9) 0.06(3) -0.16(4) -0.015(14) C12 0.17(2) 0.85(8) 0.21(3) 0.35(4) -0.13(2) -0.34(4) C13 0.047(6) 0.053(6) 0.038(5) 0.015(5) 0.013(4) 0.004(5) C14 0.047(6) 0.069(8) 0.057(7) 0.030(6) 0.010(5) -0.014(5) C15 0.047(6) 0.068(8) 0.048(6) 0.022(6) 0.016(5) 0.001(5) C16 0.041(6) 0.076(8) 0.071(8) 0.033(7) 0.002(6) -0.016(6) C17 0.070(10) 0.20(2) 0.149(17) 0.106(16) 0.048(11) 0.023(12) C18 0.080(9) 0.110(12) 0.107(11) 0.079(10) 0.014(8) -0.005(8) C19 0.139(15) 0.095(12) 0.087(11) 0.023(10) 0.013(11) -0.041(11) C20 0.049(6) 0.069(8) 0.040(6) 0.025(5) -0.006(5) 0.002(5) C21 0.069(8) 0.076(9) 0.059(8) 0.031(7) -0.010(6) -0.011(7) C22 0.098(11) 0.077(10) 0.053(8) 0.008(7) -0.005(7) -0.011(8) C23 0.070(8) 0.079(9) 0.049(7) 0.028(6) 0.014(6) 0.016(7) C24 0.064(7) 0.050(6) 0.038(6) 0.018(5) 0.004(5) 0.010(5) C25 0.056(6) 0.050(6) 0.050(6) 0.027(5) 0.013(5) 0.015(5) C26 0.060(7) 0.069(8) 0.060(7) 0.027(6) 0.021(6) 0.021(6) C27 0.056(7) 0.059(8) 0.071(8) 0.029(6) 0.024(6) 0.013(6) C28 0.070(9) 0.066(9) 0.123(13) 0.028(9) 0.043(9) 0.023(7) C29 0.117(17) 0.129(19) 0.49(5) 0.14(3) 0.15(2) 0.068(15) C30 0.047(11) 0.18(2) 0.43(5) 0.00(3) 0.022(18) 0.052(13) C31 0.36(4) 0.54(6) 0.27(3) 0.31(4) 0.28(3) 0.38(4) C32 0.037(6) 0.091(9) 0.058(7) 0.047(7) 0.000(5) -0.001(6) C33 0.058(7) 0.106(11) 0.051(7) 0.030(7) -0.006(6) 0.012(7) C34 0.033(6) 0.128(13) 0.102(11) 0.078(10) -0.014(7) 0.000(7) C35 0.049(9) 0.21(2) 0.094(12) 0.053(14) -0.025(8) 0.008(11) C36 0.060(10) 0.26(3) 0.17(2) 0.13(2) -0.072(12) -0.055(13) C37 0.19(3) 0.21(3) 0.37(5) 0.03(3) -0.14(3) 0.11(2) C38 0.054(11) 0.49(5) 0.17(2) 0.13(3) -0.016(13) -0.07(2) C39 0.043(6) 0.056(7) 0.046(6) 0.017(5) 0.010(5) 0.012(5) C40 0.069(8) 0.062(8) 0.065(7) 0.029(6) 0.020(6) 0.032(6) C41 0.068(8) 0.059(8) 0.076(8) 0.033(7) 0.024(7) 0.019(6) C42 0.065(7) 0.060(7) 0.061(7) 0.032(6) 0.010(6) 0.004(6) C43 0.055(6) 0.045(6) 0.047(6) 0.017(5) 0.015(5) 0.013(5) C44 0.045(6) 0.036(5) 0.046(6) 0.010(5) 0.001(4) -0.006(4) C45 0.072(8) 0.056(7) 0.052(6) 0.025(6) 0.024(6) 0.006(6) C46 0.082(8) 0.047(6) 0.038(6) 0.016(5) 0.022(5) -0.004(6) C47 0.127(14) 0.091(11) 0.105(12) 0.050(10) 0.079(11) 0.040(10) C48 0.26(3) 0.19(3) 0.38(4) 0.11(3) 0.27(3) 0.03(2) C49 0.26(3) 0.24(3) 0.26(3) 0.18(2) 0.23(2) 0.17(2) C50 0.25(3) 0.47(5) 0.14(2) 0.20(3) 0.11(2) 0.11(3) C51 0.044(6) 0.051(6) 0.054(6) 0.024(5) -0.001(5) 0.005(5) C52 0.060(7) 0.080(9) 0.074(8) 0.041(7) 0.033(6) 0.036(7) C53 0.049(7) 0.089(9) 0.064(8) 0.033(7) 0.019(6) 0.028(7) C54 0.072(9) 0.112(12) 0.108(12) 0.053(10) 0.053(9) 0.048(9) C55 0.37(4) 0.32(3) 0.139(19) 0.14(2) 0.17(2) 0.27(3) C56 0.22(2) 0.20(2) 0.27(3) 0.17(2) 0.18(2) 0.17(2) C57 0.073(14) 0.30(4) 0.35(4) -0.14(3) 0.07(2) 0.041(19) O120 0.100(7) 0.059(5) 0.072(6) 0.029(5) -0.011(5) 0.010(5) C121 0.109(12) 0.084(10) 0.075(9) 0.019(8) 0.001(8) 0.044(9) C122 0.157(16) 0.099(12) 0.070(9) 0.046(9) 0.030(10) 0.072(11) C123 0.135(15) 0.105(13) 0.115(14) 0.066(11) 0.034(12) 0.034(12) C124 0.102(11) 0.066(9) 0.081(10) 0.031(8) 0.018(8) 0.012(8) O130 0.100(7) 0.057(5) 0.058(5) 0.021(4) 0.010(5) -0.010(5) C131 0.090(10) 0.069(9) 0.083(10) 0.008(8) 0.023(8) -0.013(8) C132 0.085(10) 0.106(12) 0.064(9) 0.023(8) 0.017(8) 0.003(9) C133 0.107(12) 0.106(12) 0.065(9) 0.021(9) -0.002(9) -0.018(10) C134 0.095(11) 0.084(11) 0.078(10) 0.003(8) 0.017(9) -0.019(9) Fe5 0.0705(11) 0.0701(12) 0.0524(10) 0.0258(9) 0.0053(8) 0.0162(9) Cl51 0.118(3) 0.115(3) 0.089(3) 0.066(2) 0.030(2) 0.053(3) Cl52 0.092(3) 0.092(3) 0.079(2) 0.013(2) 0.010(2) 0.032(2) Cl53 0.090(3) 0.137(4) 0.079(3) 0.015(3) -0.013(2) 0.013(3) Cl54 0.099(3) 0.119(3) 0.119(3) 0.075(3) 0.036(2) 0.024(3) Fe6 0.0755(13) 0.0961(15) 0.0895(14) 0.0563(12) 0.0336(11) 0.0451(11) Cl61 0.0634(19) 0.079(2) 0.070(2) 0.0204(17) 0.0034(16) 0.0098(17) Cl62 0.128(3) 0.088(3) 0.083(2) 0.043(2) 0.002(2) 0.040(2) Cl63 0.210(6) 0.186(5) 0.077(3) 0.008(3) -0.014(3) 0.141(5) Cl64 0.178(6) 0.231(7) 0.485(14) 0.263(9) 0.234(8) 0.139(6) Ba2 0.0292(3) 0.0582(4) 0.0456(3) 0.0241(3) 0.0062(2) 0.0083(3) Fe3 0.0314(7) 0.0724(11) 0.0579(9) 0.0372(8) 0.0096(7) 0.0105(7) Fe4 0.0296(7) 0.0636(10) 0.0500(8) 0.0301(8) 0.0055(6) 0.0076(7) N4 0.038(4) 0.058(6) 0.053(5) 0.032(4) 0.007(4) 0.004(4) N5 0.028(4) 0.044(5) 0.047(5) 0.019(4) 0.010(3) 0.011(3) N6 0.045(5) 0.059(6) 0.049(5) 0.023(4) 0.008(4) 0.012(4) O13 0.034(4) 0.069(5) 0.057(4) 0.034(4) -0.001(3) 0.014(3) O14 0.033(4) 0.077(5) 0.076(5) 0.046(5) 0.005(4) -0.001(4) O15 0.033(3) 0.067(5) 0.056(4) 0.034(4) 0.007(3) 0.006(3) O16 0.032(4) 0.075(5) 0.074(5) 0.049(4) 0.000(3) -0.004(3) O17 0.042(4) 0.069(5) 0.050(4) 0.035(4) 0.013(3) 0.011(3) O18 0.043(4) 0.090(6) 0.065(5) 0.052(5) 0.024(4) 0.019(4) O19 0.038(4) 0.048(4) 0.049(4) 0.018(3) 0.011(3) 0.025(3) O20 0.044(4) 0.071(5) 0.056(5) 0.031(4) 0.013(3) 0.011(4) O21 0.037(4) 0.073(5) 0.056(4) 0.029(4) 0.004(3) 0.021(4) O22 0.038(4) 0.086(6) 0.086(6) 0.051(5) 0.013(4) 0.013(4) O23 0.036(4) 0.064(5) 0.053(4) 0.020(4) 0.009(3) 0.011(3) O24 0.031(3) 0.070(5) 0.049(4) 0.025(4) 0.000(3) 0.007(3) C58 0.034(5) 0.068(7) 0.056(6) 0.035(6) 0.001(5) 0.005(5) C59 0.040(6) 0.090(9) 0.072(8) 0.053(7) 0.005(5) 0.007(6) C60 0.054(7) 0.116(12) 0.095(10) 0.079(10) -0.007(7) 0.010(7) C61 0.039(6) 0.092(9) 0.074(8) 0.056(7) -0.002(5) 0.010(6) C62 0.035(5) 0.064(7) 0.059(7) 0.034(6) -0.001(5) 0.005(5) C63 0.032(5) 0.068(7) 0.073(7) 0.046(6) 0.009(5) 0.010(5) C64 0.036(6) 0.081(9) 0.076(8) 0.052(7) 0.003(5) 0.012(6) C65 0.035(5) 0.070(8) 0.071(8) 0.039(6) 0.015(5) 0.013(5) C66 0.038(6) 0.090(9) 0.070(8) 0.042(7) 0.002(5) 0.009(6) C67 0.064(8) 0.094(11) 0.096(11) 0.031(9) 0.003(8) 0.004(8) C68 0.035(6) 0.105(11) 0.113(11) 0.063(10) -0.011(7) 0.001(7) C69 0.062(8) 0.131(13) 0.089(10) 0.067(10) 0.009(7) -0.011(8) C70 0.039(5) 0.052(6) 0.047(6) 0.024(5) 0.007(4) 0.007(5) C71 0.041(6) 0.073(8) 0.068(7) 0.051(6) 0.003(5) 0.002(5) C72 0.039(5) 0.049(6) 0.054(6) 0.021(5) 0.005(5) -0.004(5) C73 0.041(6) 0.062(7) 0.064(7) 0.029(6) 0.018(5) -0.001(5) C74 0.106(12) 0.079(10) 0.079(10) 0.025(8) -0.003(9) -0.043(9) C75 0.048(7) 0.160(16) 0.122(13) 0.091(12) 0.025(8) 0.023(9) C76 0.078(9) 0.088(10) 0.071(8) 0.051(8) 0.015(7) -0.007(7) C77 0.044(6) 0.054(6) 0.033(5) 0.011(5) 0.003(4) 0.010(5) C78 0.049(6) 0.052(7) 0.069(7) 0.029(6) 0.015(5) 0.017(5) C79 0.063(7) 0.041(6) 0.073(8) 0.024(6) 0.016(6) 0.020(5) C80 0.057(6) 0.046(6) 0.063(7) 0.028(5) 0.018(5) 0.013(5) C81 0.037(5) 0.059(7) 0.041(6) 0.017(5) 0.006(4) 0.009(5) C82 0.024(4) 0.054(6) 0.042(5) 0.018(5) 0.006(4) -0.003(4) C83 0.048(6) 0.057(7) 0.055(6) 0.028(5) 0.010(5) 0.015(5) C84 0.037(5) 0.068(7) 0.044(6) 0.023(5) 0.009(4) 0.000(5) C85 0.070(8) 0.105(11) 0.071(9) 0.051(8) 0.032(7) 0.027(8) C86 0.31(4) 0.26(3) 0.094(15) 0.087(19) 0.088(19) 0.00(3) C87 0.22(2) 0.17(2) 0.33(3) 0.20(2) 0.21(2) 0.115(18) C88 0.097(14) 0.51(5) 0.34(4) 0.36(4) 0.131(19) 0.13(2) C89 0.031(5) 0.062(7) 0.048(6) 0.024(5) -0.002(4) 0.011(5) C90 0.043(6) 0.069(8) 0.063(7) 0.034(6) 0.023(5) 0.028(5) C91 0.046(6) 0.082(8) 0.033(5) 0.017(6) 0.006(5) 0.016(6) C92 0.049(6) 0.080(8) 0.053(7) 0.024(6) 0.021(5) 0.027(6) C93 0.143(16) 0.25(2) 0.109(13) 0.108(16) 0.095(13) 0.123(17) C94 0.047(9) 0.25(2) 0.116(15) 0.012(15) 0.023(9) 0.057(12) C95 0.130(14) 0.123(14) 0.151(16) 0.068(13) 0.104(13) 0.075(12) C96 0.035(5) 0.057(7) 0.073(8) 0.026(6) 0.012(5) 0.006(5) C97 0.058(8) 0.068(8) 0.079(9) 0.011(7) 0.000(7) -0.006(6) C98 0.053(8) 0.086(10) 0.097(11) 0.010(8) 0.023(7) 0.007(7) C99 0.041(6) 0.074(8) 0.073(8) 0.002(7) 0.014(6) 0.016(6) C100 0.048(6) 0.067(8) 0.065(7) 0.026(6) 0.017(6) 0.018(6) C101 0.039(5) 0.063(7) 0.066(7) 0.034(6) 0.020(5) 0.011(5) C102 0.047(7) 0.057(8) 0.115(11) 0.021(7) 0.027(7) 0.017(6) C103 0.038(6) 0.066(8) 0.101(10) 0.045(8) 0.022(6) 0.010(6) C104 0.041(7) 0.092(11) 0.159(16) 0.037(11) 0.043(9) 0.030(7) C105 0.082(14) 0.102(16) 0.76(8) 0.16(3) 0.10(3) 0.061(13) C106 0.120(16) 0.51(5) 0.125(17) 0.18(3) 0.091(14) 0.18(2) C107 0.095(13) 0.25(3) 0.132(16) 0.079(17) 0.016(11) 0.113(15) C108 0.038(5) 0.056(7) 0.061(7) 0.029(6) 0.012(5) 0.012(5) C109 0.047(6) 0.066(8) 0.056(7) 0.020(6) 0.012(5) 0.010(5) C110 0.039(6) 0.053(7) 0.064(7) 0.028(6) 0.005(5) -0.001(5) C111 0.049(7) 0.067(8) 0.061(7) 0.015(6) -0.005(6) 0.007(6) C112 0.048(8) 0.165(18) 0.140(16) -0.020(13) -0.023(9) 0.040(10) C113 0.070(12) 0.21(2) 0.45(4) 0.25(3) -0.091(18) -0.073(14) C114 0.067(11) 0.28(3) 0.094(13) -0.001(16) -0.021(10) 0.046(14) O220 0.078(6) 0.062(5) 0.059(5) 0.022(4) 0.008(4) -0.002(4) C221 0.101(11) 0.087(11) 0.065(9) 0.000(8) 0.018(8) -0.033(9) C222 0.094(11) 0.087(10) 0.064(9) 0.018(8) 0.001(8) -0.025(8) C223 0.105(11) 0.074(9) 0.065(9) 0.015(7) 0.013(8) 0.002(8) C224 0.087(10) 0.102(11) 0.064(9) 0.011(8) 0.029(8) -0.014(9) O230 0.093(7) 0.094(7) 0.058(5) 0.025(5) 0.003(5) 0.044(6) C231 0.083(10) 0.131(14) 0.093(11) 0.059(11) 0.015(9) 0.043(10) C232 0.079(10) 0.118(13) 0.095(11) 0.057(10) 0.002(8) 0.008(9) C233 0.121(14) 0.085(11) 0.076(10) 0.022(9) -0.021(9) 0.004(10) C234 0.078(9) 0.076(9) 0.066(8) 0.028(7) 0.000(7) 0.008(7) Fe7 0.0697(12) 0.0699(12) 0.0704(12) 0.0323(10) 0.0132(9) 0.0191(10) Cl71 0.084(3) 0.147(4) 0.197(6) -0.078(4) -0.047(3) 0.053(3) Cl72 0.152(4) 0.131(4) 0.085(3) 0.062(3) 0.041(3) 0.081(3) Cl73 0.078(2) 0.074(2) 0.070(2) 0.0180(17) 0.0097(17) 0.0047(18) Cl74 0.274(8) 0.128(4) 0.179(6) 0.093(4) 0.140(6) 0.063(5) Fe8 0.306(5) 0.199(3) 0.0781(18) 0.070(2) 0.047(2) 0.178(4) Cl81 0.126(3) 0.111(3) 0.076(2) 0.043(2) 0.011(2) 0.021(3) Cl82 0.193(5) 0.103(3) 0.112(3) 0.064(3) -0.005(3) 0.043(3) Cl83 0.260(16) 0.080(6) 0.091(6) 0.034(5) 0.024(8) 0.058(8) Cl84 0.159(11) 0.230(15) 0.150(11) 0.106(11) 0.052(8) 0.018(10) Cl85 0.39(3) 0.145(11) 0.131(10) 0.097(9) -0.150(14) -0.112(14) Cl86 0.21(2) 0.60(6) 0.182(18) 0.17(3) 0.095(16) 0.23(3) C300 0.37(6) 0.98(14) 0.20(6) 0.37(8) -0.19(4) -0.53(11) Cl31 0.79(9) 0.93(10) 0.71(8) 0.66(9) -0.01(7) -0.28(8) Cl32 0.67(7) 0.49(5) 0.25(3) 0.02(3) -0.02(4) 0.04(5) _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 Ba1 O11 2.717(6) . ? Ba1 O5 2.741(7) . ? Ba1 O1 2.749(6) . ? Ba1 O3 2.751(6) . ? Ba1 O9 2.784(7) . ? Ba1 O7 2.800(7) . ? Ba1 N1 2.877(8) . ? Ba1 N2 2.885(9) . ? Ba1 N3 2.909(8) . ? Ba1 O130 2.983(8) . ? Ba1 O120 3.001(8) . ? Ba1 Fe1 3.5771(18) . ? Fe1 O10 1.961(7) . ? Fe1 O2 1.969(8) . ? Fe1 O6 1.979(8) . ? Fe1 O1 2.009(7) . ? Fe1 O9 2.012(7) . ? Fe1 O5 2.025(7) . ? Fe2 O4 1.948(7) . ? Fe2 O12 1.966(8) . ? Fe2 O8 1.971(8) . ? Fe2 O11 2.012(7) . ? Fe2 O7 2.018(7) . ? Fe2 O3 2.039(6) . ? N1 C1 1.334(12) . ? N1 C5 1.359(12) . ? N2 C24 1.343(13) . ? N2 C20 1.356(13) . ? N3 C43 1.334(13) . ? N3 C39 1.387(12) . ? O1 C6 1.288(12) . ? O2 C8 1.269(13) . ? O3 C13 1.310(11) . ? O4 C15 1.309(12) . ? O5 C25 1.296(12) . ? O6 C27 1.269(14) . ? O7 C32 1.274(12) . ? O8 C34 1.247(16) . ? O9 C44 1.290(11) . ? O10 C46 1.246(12) . ? O11 C51 1.287(12) . ? O12 C53 1.276(14) . ? C1 C2 1.382(14) . ? C1 C13 1.526(14) . ? C2 C3 1.392(15) . ? C3 C4 1.365(15) . ? C4 C5 1.400(14) . ? C5 C6 1.493(13) . ? C6 C7 1.398(14) . ? C7 C8 1.403(15) . ? C8 C9 1.523(15) . ? C9 C12 1.38(2) . ? C9 C10 1.444(16) . ? C9 C11 1.52(3) . ? C13 C14 1.358(13) . ? C14 C15 1.409(14) . ? C15 C16 1.502(14) . ? C16 C17 1.542(19) . ? C16 C18 1.545(16) . ? C16 C19 1.549(18) . ? C20 C21 1.387(15) . ? C20 C32 1.520(15) . ? C21 C22 1.383(18) . ? C22 C23 1.376(17) . ? C23 C24 1.374(15) . ? C24 C25 1.502(15) . ? C25 C26 1.401(14) . ? C26 C27 1.376(16) . ? C27 C28 1.525(15) . ? C28 C29 1.37(2) . ? C28 C31 1.43(2) . ? C28 C30 1.51(2) . ? C32 C33 1.366(14) . ? C33 C34 1.398(18) . ? C34 C35 1.561(16) . ? C35 C37 1.44(3) . ? C35 C36 1.48(2) . ? C35 C38 1.58(3) . ? C39 C40 1.412(14) . ? C39 C51 1.456(14) . ? C40 C41 1.361(15) . ? C41 C42 1.371(15) . ? C42 C43 1.400(14) . ? C43 C44 1.491(13) . ? C44 C45 1.377(13) . ? C45 C46 1.412(15) . ? C46 C47 1.505(15) . ? C47 C48 1.40(3) . ? C47 C49 1.45(2) . ? C47 C50 1.58(3) . ? C51 C52 1.402(14) . ? C52 C53 1.376(16) . ? C53 C54 1.507(15) . ? C54 C57 1.43(3) . ? C54 C56 1.51(2) . ? C54 C55 1.53(2) . ? O120 C124 1.444(15) . ? O120 C121 1.451(15) . ? C121 C122 1.526(19) . ? C122 C123 1.49(2) . ? C123 C124 1.550(18) . ? O130 C131 1.394(15) . ? O130 C134 1.433(15) . ? C131 C132 1.495(17) . ? C132 C133 1.491(18) . ? C133 C134 1.441(18) . ? Fe5 Cl53 2.168(4) . ? Fe5 Cl51 2.183(4) . ? Fe5 Cl54 2.184(4) . ? Fe5 Cl52 2.197(4) . ? Fe6 Cl64 2.126(5) . ? Fe6 Cl62 2.171(4) . ? Fe6 Cl63 2.192(6) . ? Fe6 Cl61 2.202(4) . ? Ba2 O19 2.674(6) . ? Ba2 O13 2.727(6) . ? Ba2 O23 2.731(7) . ? Ba2 O17 2.749(7) . ? Ba2 N5 2.840(7) . ? Ba2 O15 2.842(6) . ? Ba2 O21 2.890(7) . ? Ba2 N6 2.893(9) . ? Ba2 O220 2.912(8) . ? Ba2 N4 2.935(8) . ? Ba2 O230 2.979(8) . ? Ba2 Fe4 3.5820(17) . ? Fe3 O18 1.963(7) . ? Fe3 O22 1.971(8) . ? Fe3 O14 1.972(8) . ? Fe3 O13 1.997(7) . ? Fe3 O21 2.008(8) . ? Fe3 O17 2.018(7) . ? Fe4 O24 1.963(7) . ? Fe4 O16 1.976(7) . ? Fe4 O20 1.981(7) . ? Fe4 O19 1.995(7) . ? Fe4 O15 2.040(6) . ? Fe4 O23 2.043(7) . ? N4 C58 1.325(12) . ? N4 C62 1.361(12) . ? N5 C77 1.347(11) . ? N5 C81 1.350(12) . ? N6 C100 1.341(13) . ? N6 C96 1.358(13) . ? O13 C63 1.294(12) . ? O14 C65 1.290(12) . ? O15 C70 1.292(11) . ? O16 C72 1.277(12) . ? O17 C82 1.302(11) . ? O18 C84 1.260(12) . ? O19 C89 1.296(11) . ? O20 C91 1.283(13) . ? O21 C101 1.285(12) . ? O22 C103 1.264(14) . ? O23 C108 1.280(12) . ? O24 C110 1.282(12) . ? C58 C59 1.408(13) . ? C58 C70 1.498(13) . ? C59 C60 1.396(15) . ? C60 C61 1.361(15) . ? C61 C62 1.392(13) . ? C62 C63 1.477(13) . ? C63 C64 1.370(14) . ? C64 C65 1.406(14) . ? C65 C66 1.512(15) . ? C66 C69 1.512(15) . ? C66 C68 1.520(15) . ? C66 C67 1.538(18) . ? C70 C71 1.381(13) . ? C71 C72 1.386(13) . ? C72 C73 1.517(13) . ? C73 C76 1.518(15) . ? C73 C74 1.532(17) . ? C73 C75 1.535(16) . ? C77 C78 1.389(14) . ? C77 C89 1.497(14) . ? C78 C79 1.380(14) . ? C79 C80 1.386(14) . ? C80 C81 1.397(14) . ? C81 C82 1.503(12) . ? C82 C83 1.338(13) . ? C83 C84 1.423(13) . ? C84 C85 1.502(14) . ? C85 C88 1.46(2) . ? C85 C87 1.48(2) . ? C85 C86 1.52(3) . ? C89 C90 1.405(13) . ? C90 C91 1.381(15) . ? C91 C92 1.532(13) . ? C92 C93 1.489(17) . ? C92 C95 1.537(18) . ? C92 C94 1.558(19) . ? C96 C97 1.363(16) . ? C96 C108 1.508(14) . ? C97 C98 1.379(17) . ? C98 C99 1.387(16) . ? C99 C100 1.362(16) . ? C100 C101 1.502(15) . ? C101 C102 1.405(14) . ? C102 C103 1.389(16) . ? C103 C104 1.547(15) . ? C104 C105 1.46(2) . ? C104 C106 1.50(2) . ? C104 C107 1.55(2) . ? C108 C109 1.391(14) . ? C109 C110 1.413(14) . ? C110 C111 1.545(14) . ? C111 C113 1.46(2) . ? C111 C112 1.497(18) . ? C111 C114 1.51(2) . ? O220 C221 1.392(14) . ? O220 C224 1.417(14) . ? C221 C222 1.460(17) . ? C222 C223 1.510(18) . ? C223 C224 1.468(17) . ? O230 C231 1.429(16) . ? O230 C234 1.460(14) . ? C231 C232 1.501(18) . ? C232 C233 1.50(2) . ? C233 C234 1.528(18) . ? Fe7 Cl71 2.152(5) . ? Fe7 Cl74 2.156(5) . ? Fe7 Cl72 2.182(4) . ? Fe7 Cl73 2.212(4) . ? Fe8 Cl86 1.889(16) . ? Fe8 Cl83 1.937(9) . ? Fe8 Cl82 2.116(5) . ? Fe8 Cl81 2.169(5) . ? Fe8 Cl85 2.569(14) . ? Fe8 Cl84 2.626(13) . ? C300 Cl31 1.79(2) . ? C300 Cl32 1.79(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Ba1 O5 140.8(2) . . ? O11 Ba1 O1 152.4(2) . . ? O5 Ba1 O1 58.8(2) . . ? O11 Ba1 O3 58.8(2) . . ? O5 Ba1 O3 152.6(2) . . ? O1 Ba1 O3 113.24(19) . . ? O11 Ba1 O9 111.2(2) . . ? O5 Ba1 O9 56.6(2) . . ? O1 Ba1 O9 58.8(2) . . ? O3 Ba1 O9 145.7(2) . . ? O11 Ba1 O7 56.6(2) . . ? O5 Ba1 O7 111.9(2) . . ? O1 Ba1 O7 145.6(2) . . ? O3 Ba1 O7 58.0(2) . . ? O9 Ba1 O7 148.2(2) . . ? O11 Ba1 N1 109.3(2) . . ? O5 Ba1 N1 109.9(2) . . ? O1 Ba1 N1 57.1(2) . . ? O3 Ba1 N1 56.1(2) . . ? O9 Ba1 N1 106.8(2) . . ? O7 Ba1 N1 105.0(2) . . ? O11 Ba1 N2 101.3(2) . . ? O5 Ba1 N2 56.2(2) . . ? O1 Ba1 N2 106.2(2) . . ? O3 Ba1 N2 108.5(2) . . ? O9 Ba1 N2 105.6(2) . . ? O7 Ba1 N2 55.7(2) . . ? N1 Ba1 N2 122.4(2) . . ? O11 Ba1 N3 55.8(2) . . ? O5 Ba1 N3 99.1(2) . . ? O1 Ba1 N3 110.6(2) . . ? O3 Ba1 N3 108.0(2) . . ? O9 Ba1 N3 55.6(2) . . ? O7 Ba1 N3 103.5(2) . . ? N1 Ba1 N3 127.2(2) . . ? N2 Ba1 N3 110.4(2) . . ? O11 Ba1 O130 73.6(2) . . ? O5 Ba1 O130 125.4(2) . . ? O1 Ba1 O130 78.8(2) . . ? O3 Ba1 O130 72.8(2) . . ? O9 Ba1 O130 73.0(2) . . ? O7 Ba1 O130 122.3(2) . . ? N1 Ba1 O130 63.9(2) . . ? N2 Ba1 O130 173.3(2) . . ? N3 Ba1 O130 63.3(2) . . ? O11 Ba1 O120 124.6(2) . . ? O5 Ba1 O120 75.6(2) . . ? O1 Ba1 O120 72.9(2) . . ? O3 Ba1 O120 77.0(2) . . ? O9 Ba1 O120 124.0(2) . . ? O7 Ba1 O120 72.6(2) . . ? N1 Ba1 O120 61.6(2) . . ? N2 Ba1 O120 60.9(2) . . ? N3 Ba1 O120 171.2(2) . . ? O130 Ba1 O120 125.5(2) . . ? O11 Ba1 Fe1 145.10(15) . . ? O5 Ba1 Fe1 34.26(15) . . ? O1 Ba1 Fe1 33.94(14) . . ? O3 Ba1 Fe1 147.03(14) . . ? O9 Ba1 Fe1 34.08(15) . . ? O7 Ba1 Fe1 146.00(15) . . ? N1 Ba1 Fe1 90.98(15) . . ? N2 Ba1 Fe1 90.38(17) . . ? N3 Ba1 Fe1 89.33(17) . . ? O130 Ba1 Fe1 91.64(18) . . ? O120 Ba1 Fe1 89.89(19) . . ? O10 Fe1 O2 89.0(3) . . ? O10 Fe1 O6 89.4(3) . . ? O2 Fe1 O6 94.3(4) . . ? O10 Fe1 O1 166.7(3) . . ? O2 Fe1 O1 83.8(3) . . ? O6 Fe1 O1 102.2(3) . . ? O10 Fe1 O9 85.7(3) . . ? O2 Fe1 O9 101.9(3) . . ? O6 Fe1 O9 163.0(3) . . ? O1 Fe1 O9 84.9(3) . . ? O10 Fe1 O5 103.9(3) . . ? O2 Fe1 O5 167.1(3) . . ? O6 Fe1 O5 84.6(3) . . ? O1 Fe1 O5 83.9(3) . . ? O9 Fe1 O5 80.8(3) . . ? O10 Fe1 Ba1 128.1(2) . . ? O2 Fe1 Ba1 122.7(2) . . ? O6 Fe1 Ba1 123.2(2) . . ? O1 Fe1 Ba1 49.80(18) . . ? O9 Fe1 Ba1 50.8(2) . . ? O5 Fe1 Ba1 49.64(19) . . ? O4 Fe2 O12 93.1(3) . . ? O4 Fe2 O8 90.9(3) . . ? O12 Fe2 O8 88.8(4) . . ? O4 Fe2 O11 166.3(3) . . ? O12 Fe2 O11 84.2(3) . . ? O8 Fe2 O11 102.5(3) . . ? O4 Fe2 O7 103.4(3) . . ? O12 Fe2 O7 162.6(3) . . ? O8 Fe2 O7 85.5(3) . . ? O11 Fe2 O7 81.0(3) . . ? O4 Fe2 O3 84.6(3) . . ? O12 Fe2 O3 104.1(3) . . ? O8 Fe2 O3 166.5(3) . . ? O11 Fe2 O3 83.0(3) . . ? O7 Fe2 O3 83.2(3) . . ? O4 Fe2 Ba1 124.9(2) . . ? O12 Fe2 Ba1 122.8(2) . . ? O8 Fe2 Ba1 126.1(3) . . ? O11 Fe2 Ba1 48.36(18) . . ? O7 Fe2 Ba1 50.75(19) . . ? O3 Fe2 Ba1 49.43(19) . . ? C1 N1 C5 118.5(9) . . ? C1 N1 Ba1 121.3(6) . . ? C5 N1 Ba1 119.5(6) . . ? C24 N2 C20 118.2(10) . . ? C24 N2 Ba1 120.2(7) . . ? C20 N2 Ba1 121.4(7) . . ? C43 N3 C39 118.8(8) . . ? C43 N3 Ba1 121.0(6) . . ? C39 N3 Ba1 119.8(6) . . ? C6 O1 Fe1 132.3(6) . . ? C6 O1 Ba1 122.7(6) . . ? Fe1 O1 Ba1 96.3(2) . . ? C8 O2 Fe1 134.3(7) . . ? C13 O3 Fe2 130.0(6) . . ? C13 O3 Ba1 123.8(6) . . ? Fe2 O3 Ba1 96.3(3) . . ? C15 O4 Fe2 134.6(7) . . ? C25 O5 Fe1 129.9(6) . . ? C25 O5 Ba1 122.2(6) . . ? Fe1 O5 Ba1 96.1(3) . . ? C27 O6 Fe1 133.7(8) . . ? C32 O7 Fe2 129.1(7) . . ? C32 O7 Ba1 124.1(6) . . ? Fe2 O7 Ba1 95.3(2) . . ? C34 O8 Fe2 132.0(8) . . ? C44 O9 Fe1 129.1(6) . . ? C44 O9 Ba1 123.8(6) . . ? Fe1 O9 Ba1 95.1(3) . . ? C46 O10 Fe1 133.6(7) . . ? C51 O11 Fe2 130.7(6) . . ? C51 O11 Ba1 128.3(6) . . ? Fe2 O11 Ba1 98.0(3) . . ? C53 O12 Fe2 131.1(7) . . ? N1 C1 C2 123.6(10) . . ? N1 C1 C13 115.0(9) . . ? C2 C1 C13 121.4(9) . . ? C1 C2 C3 117.9(10) . . ? C4 C3 C2 119.5(11) . . ? C3 C4 C5 119.9(10) . . ? N1 C5 C4 120.6(9) . . ? N1 C5 C6 115.3(9) . . ? C4 C5 C6 124.1(9) . . ? O1 C6 C7 123.9(10) . . ? O1 C6 C5 115.2(9) . . ? C7 C6 C5 120.9(10) . . ? C6 C7 C8 121.5(11) . . ? O2 C8 C7 123.9(10) . . ? O2 C8 C9 115.5(10) . . ? C7 C8 C9 120.3(11) . . ? C12 C9 C10 110.8(17) . . ? C12 C9 C11 108(2) . . ? C10 C9 C11 103(2) . . ? C12 C9 C8 113.4(15) . . ? C10 C9 C8 114.1(10) . . ? C11 C9 C8 107.4(12) . . ? O3 C13 C14 124.6(10) . . ? O3 C13 C1 114.2(8) . . ? C14 C13 C1 121.2(10) . . ? C13 C14 C15 124.0(11) . . ? O4 C15 C14 121.8(9) . . ? O4 C15 C16 114.2(9) . . ? C14 C15 C16 124.0(10) . . ? C15 C16 C17 109.1(11) . . ? C15 C16 C18 112.5(9) . . ? C17 C16 C18 109.5(11) . . ? C15 C16 C19 107.5(10) . . ? C17 C16 C19 110.4(12) . . ? C18 C16 C19 107.8(12) . . ? N2 C20 C21 121.5(11) . . ? N2 C20 C32 115.1(10) . . ? C21 C20 C32 123.4(10) . . ? C22 C21 C20 119.2(12) . . ? C23 C22 C21 119.0(12) . . ? C22 C23 C24 119.2(12) . . ? N2 C24 C23 122.7(11) . . ? N2 C24 C25 114.6(9) . . ? C23 C24 C25 122.7(10) . . ? O5 C25 C26 124.9(11) . . ? O5 C25 C24 114.7(9) . . ? C26 C25 C24 120.4(10) . . ? C27 C26 C25 122.4(12) . . ? O6 C27 C26 124.1(11) . . ? O6 C27 C28 115.6(11) . . ? C26 C27 C28 120.3(12) . . ? C29 C28 C31 111(2) . . ? C29 C28 C30 107.1(19) . . ? C31 C28 C30 110(2) . . ? C29 C28 C27 111.7(13) . . ? C31 C28 C27 107.3(13) . . ? C30 C28 C27 109.8(13) . . ? O7 C32 C33 125.9(11) . . ? O7 C32 C20 113.5(9) . . ? C33 C32 C20 120.7(11) . . ? C32 C33 C34 122.3(12) . . ? O8 C34 C33 124.6(10) . . ? O8 C34 C35 113.9(13) . . ? C33 C34 C35 121.5(14) . . ? C37 C35 C36 114.0(19) . . ? C37 C35 C34 105.9(17) . . ? C36 C35 C34 112.7(15) . . ? C37 C35 C38 115(2) . . ? C36 C35 C38 107.2(18) . . ? C34 C35 C38 101.7(13) . . ? N3 C39 C40 120.1(9) . . ? N3 C39 C51 115.1(9) . . ? C40 C39 C51 124.9(9) . . ? C41 C40 C39 119.1(10) . . ? C40 C41 C42 121.0(11) . . ? C41 C42 C43 118.3(11) . . ? N3 C43 C42 122.5(10) . . ? N3 C43 C44 115.5(9) . . ? C42 C43 C44 122.0(9) . . ? O9 C44 C45 125.0(10) . . ? O9 C44 C43 114.5(8) . . ? C45 C44 C43 120.5(10) . . ? C44 C45 C46 123.0(10) . . ? O10 C46 C45 123.2(9) . . ? O10 C46 C47 116.1(11) . . ? C45 C46 C47 120.8(11) . . ? C48 C47 C49 115(2) . . ? C48 C47 C46 110.0(14) . . ? C49 C47 C46 109.5(13) . . ? C48 C47 C50 106(2) . . ? C49 C47 C50 109.9(18) . . ? C46 C47 C50 106.6(15) . . ? O11 C51 C52 122.3(10) . . ? O11 C51 C39 116.7(9) . . ? C52 C51 C39 120.9(10) . . ? C53 C52 C51 124.1(11) . . ? O12 C53 C52 122.8(10) . . ? O12 C53 C54 116.6(11) . . ? C52 C53 C54 120.5(12) . . ? C57 C54 C53 108.4(14) . . ? C57 C54 C56 109.6(19) . . ? C53 C54 C56 115.5(12) . . ? C57 C54 C55 110(2) . . ? C53 C54 C55 107.8(12) . . ? C56 C54 C55 105.5(17) . . ? C124 O120 C121 105.3(10) . . ? C124 O120 Ba1 125.0(7) . . ? C121 O120 Ba1 129.7(8) . . ? O120 C121 C122 104.7(12) . . ? C123 C122 C121 104.5(12) . . ? C122 C123 C124 105.7(13) . . ? O120 C124 C123 104.4(12) . . ? C131 O130 C134 106.6(10) . . ? C131 O130 Ba1 126.3(7) . . ? C134 O130 Ba1 127.1(7) . . ? O130 C131 C132 109.8(11) . . ? C133 C132 C131 104.9(11) . . ? C134 C133 C132 105.5(12) . . ? O130 C134 C133 110.3(12) . . ? Cl53 Fe5 Cl51 112.4(2) . . ? Cl53 Fe5 Cl54 110.8(2) . . ? Cl51 Fe5 Cl54 106.13(17) . . ? Cl53 Fe5 Cl52 106.00(18) . . ? Cl51 Fe5 Cl52 110.12(17) . . ? Cl54 Fe5 Cl52 111.54(19) . . ? Cl64 Fe6 Cl62 109.0(2) . . ? Cl64 Fe6 Cl63 109.7(4) . . ? Cl62 Fe6 Cl63 109.4(2) . . ? Cl64 Fe6 Cl61 111.7(3) . . ? Cl62 Fe6 Cl61 109.78(16) . . ? Cl63 Fe6 Cl61 107.31(17) . . ? O19 Ba2 O13 154.9(2) . . ? O19 Ba2 O23 59.8(2) . . ? O13 Ba2 O23 136.5(2) . . ? O19 Ba2 O17 114.5(2) . . ? O13 Ba2 O17 59.9(2) . . ? O23 Ba2 O17 154.1(2) . . ? O19 Ba2 N5 57.7(2) . . ? O13 Ba2 N5 113.1(2) . . ? O23 Ba2 N5 110.2(2) . . ? O17 Ba2 N5 57.0(2) . . ? O19 Ba2 O15 58.80(19) . . ? O13 Ba2 O15 110.79(19) . . ? O23 Ba2 O15 55.7(2) . . ? O17 Ba2 O15 146.6(2) . . ? N5 Ba2 O15 109.2(2) . . ? O19 Ba2 O21 146.08(19) . . ? O13 Ba2 O21 54.80(19) . . ? O23 Ba2 O21 112.0(2) . . ? O17 Ba2 O21 56.9(2) . . ? N5 Ba2 O21 103.0(2) . . ? O15 Ba2 O21 147.8(2) . . ? O19 Ba2 N6 109.2(2) . . ? O13 Ba2 N6 95.2(2) . . ? O23 Ba2 N6 56.4(2) . . ? O17 Ba2 N6 109.5(2) . . ? N5 Ba2 N6 124.3(2) . . ? O15 Ba2 N6 103.1(2) . . ? O21 Ba2 N6 55.8(2) . . ? O19 Ba2 O220 77.9(2) . . ? O13 Ba2 O220 77.0(2) . . ? O23 Ba2 O220 124.7(2) . . ? O17 Ba2 O220 73.7(2) . . ? N5 Ba2 O220 66.6(2) . . ? O15 Ba2 O220 72.9(2) . . ? O21 Ba2 O220 122.6(2) . . ? N6 Ba2 O220 168.9(2) . . ? O19 Ba2 N4 110.0(2) . . ? O13 Ba2 N4 56.7(2) . . ? O23 Ba2 N4 95.3(2) . . ? O17 Ba2 N4 109.8(2) . . ? N5 Ba2 N4 132.5(2) . . ? O15 Ba2 N4 54.22(19) . . ? O21 Ba2 N4 103.4(2) . . ? N6 Ba2 N4 103.3(2) . . ? O220 Ba2 N4 65.9(2) . . ? O19 Ba2 O230 69.9(2) . . ? O13 Ba2 O230 129.7(2) . . ? O23 Ba2 O230 69.4(3) . . ? O17 Ba2 O230 84.8(2) . . ? N5 Ba2 O230 62.9(2) . . ? O15 Ba2 O230 117.6(2) . . ? O21 Ba2 O230 76.5(2) . . ? N6 Ba2 O230 62.1(2) . . ? O220 Ba2 O230 129.0(2) . . ? N4 Ba2 O230 162.8(3) . . ? O19 Ba2 Fe4 33.35(15) . . ? O13 Ba2 Fe4 145.03(14) . . ? O23 Ba2 Fe4 34.54(15) . . ? O17 Ba2 Fe4 147.77(14) . . ? N5 Ba2 Fe4 91.01(14) . . ? O15 Ba2 Fe4 34.65(13) . . ? O21 Ba2 Fe4 146.23(15) . . ? N6 Ba2 Fe4 90.88(17) . . ? O220 Ba2 Fe4 91.10(17) . . ? N4 Ba2 Fe4 88.39(15) . . ? O230 Ba2 Fe4 83.18(19) . . ? O18 Fe3 O22 89.7(3) . . ? O18 Fe3 O14 93.7(3) . . ? O22 Fe3 O14 90.5(3) . . ? O18 Fe3 O13 170.5(3) . . ? O22 Fe3 O13 99.7(3) . . ? O14 Fe3 O13 84.5(3) . . ? O18 Fe3 O21 101.9(3) . . ? O22 Fe3 O21 86.7(3) . . ? O14 Fe3 O21 164.1(3) . . ? O13 Fe3 O21 80.5(3) . . ? O18 Fe3 O17 85.3(3) . . ? O22 Fe3 O17 168.0(3) . . ? O14 Fe3 O17 100.6(3) . . ? O13 Fe3 O17 85.8(3) . . ? O21 Fe3 O17 83.7(3) . . ? O18 Fe3 Ba2 125.9(2) . . ? O22 Fe3 Ba2 128.3(2) . . ? O14 Fe3 Ba2 118.8(2) . . ? O13 Fe3 Ba2 48.49(17) . . ? O21 Fe3 Ba2 53.2(2) . . ? O17 Fe3 Ba2 49.21(19) . . ? O24 Fe4 O16 89.6(3) . . ? O24 Fe4 O20 90.4(3) . . ? O16 Fe4 O20 87.7(3) . . ? O24 Fe4 O19 104.0(3) . . ? O16 Fe4 O19 164.2(3) . . ? O20 Fe4 O19 84.4(3) . . ? O24 Fe4 O15 160.3(3) . . ? O16 Fe4 O15 85.2(3) . . ? O20 Fe4 O15 108.3(3) . . ? O19 Fe4 O15 84.5(3) . . ? O24 Fe4 O23 83.9(3) . . ? O16 Fe4 O23 105.9(3) . . ? O20 Fe4 O23 165.2(3) . . ? O19 Fe4 O23 83.8(3) . . ? O15 Fe4 O23 79.3(3) . . ? O24 Fe4 Ba2 121.3(2) . . ? O16 Fe4 Ba2 130.9(2) . . ? O20 Fe4 Ba2 125.2(2) . . ? O19 Fe4 Ba2 47.46(16) . . ? O15 Fe4 Ba2 52.41(18) . . ? O23 Fe4 Ba2 49.3(2) . . ? C58 N4 C62 119.6(8) . . ? C58 N4 Ba2 121.5(6) . . ? C62 N4 Ba2 118.4(6) . . ? C77 N5 C81 119.4(8) . . ? C77 N5 Ba2 120.3(6) . . ? C81 N5 Ba2 120.2(6) . . ? C100 N6 C96 117.5(10) . . ? C100 N6 Ba2 121.9(7) . . ? C96 N6 Ba2 120.3(7) . . ? C63 O13 Fe3 131.2(6) . . ? C63 O13 Ba2 124.1(6) . . ? Fe3 O13 Ba2 98.2(2) . . ? C65 O14 Fe3 132.6(7) . . ? C70 O15 Fe4 128.0(6) . . ? C70 O15 Ba2 125.2(6) . . ? Fe4 O15 Ba2 92.9(2) . . ? C72 O16 Fe4 133.2(6) . . ? C82 O17 Fe3 128.9(6) . . ? C82 O17 Ba2 122.1(5) . . ? Fe3 O17 Ba2 97.0(3) . . ? C84 O18 Fe3 134.1(6) . . ? C89 O19 Fe4 131.7(6) . . ? C89 O19 Ba2 125.8(6) . . ? Fe4 O19 Ba2 99.2(2) . . ? C91 O20 Fe4 131.1(6) . . ? C101 O21 Fe3 127.8(6) . . ? C101 O21 Ba2 116.5(6) . . ? Fe3 O21 Ba2 93.0(3) . . ? C103 O22 Fe3 130.5(7) . . ? C108 O23 Fe4 131.5(6) . . ? C108 O23 Ba2 124.0(6) . . ? Fe4 O23 Ba2 96.2(3) . . ? C110 O24 Fe4 132.5(6) . . ? N4 C58 C59 122.2(9) . . ? N4 C58 C70 116.9(8) . . ? C59 C58 C70 120.9(9) . . ? C60 C59 C58 117.8(10) . . ? C61 C60 C59 119.7(10) . . ? C60 C61 C62 120.0(10) . . ? N4 C62 C61 120.7(9) . . ? N4 C62 C63 114.9(8) . . ? C61 C62 C63 124.4(9) . . ? O13 C63 C64 122.8(9) . . ? O13 C63 C62 116.1(9) . . ? C64 C63 C62 121.0(10) . . ? C63 C64 C65 124.7(10) . . ? O14 C65 C64 121.4(10) . . ? O14 C65 C66 117.5(9) . . ? C64 C65 C66 121.1(10) . . ? C65 C66 C69 110.7(10) . . ? C65 C66 C68 110.0(10) . . ? C69 C66 C68 110.2(10) . . ? C65 C66 C67 107.7(9) . . ? C69 C66 C67 108.6(12) . . ? C68 C66 C67 109.6(11) . . ? O15 C70 C71 125.1(9) . . ? O15 C70 C58 113.9(8) . . ? C71 C70 C58 121.0(9) . . ? C70 C71 C72 123.6(9) . . ? O16 C72 C71 123.0(9) . . ? O16 C72 C73 114.8(9) . . ? C71 C72 C73 122.1(9) . . ? C72 C73 C76 112.4(9) . . ? C72 C73 C74 106.0(9) . . ? C76 C73 C74 109.1(10) . . ? C72 C73 C75 109.6(10) . . ? C76 C73 C75 109.4(10) . . ? C74 C73 C75 110.3(11) . . ? N5 C77 C78 122.3(9) . . ? N5 C77 C89 115.1(9) . . ? C78 C77 C89 122.5(9) . . ? C79 C78 C77 117.7(10) . . ? C78 C79 C80 121.1(10) . . ? C79 C80 C81 117.9(10) . . ? N5 C81 C80 121.5(9) . . ? N5 C81 C82 116.1(9) . . ? C80 C81 C82 122.4(9) . . ? O17 C82 C83 125.4(9) . . ? O17 C82 C81 113.5(8) . . ? C83 C82 C81 121.0(9) . . ? C82 C83 C84 124.3(10) . . ? O18 C84 C83 121.7(9) . . ? O18 C84 C85 116.5(9) . . ? C83 C84 C85 121.8(10) . . ? C88 C85 C87 114.5(17) . . ? C88 C85 C84 111.1(11) . . ? C87 C85 C84 113.9(11) . . ? C88 C85 C86 108.4(18) . . ? C87 C85 C86 104.5(17) . . ? C84 C85 C86 103.5(12) . . ? O19 C89 C90 124.2(10) . . ? O19 C89 C77 116.0(8) . . ? C90 C89 C77 119.7(9) . . ? C91 C90 C89 121.0(10) . . ? O20 C91 C90 125.5(9) . . ? O20 C91 C92 112.8(10) . . ? C90 C91 C92 121.6(10) . . ? C93 C92 C95 109.1(12) . . ? C93 C92 C91 111.5(10) . . ? C95 C92 C91 113.3(10) . . ? C93 C92 C94 109.7(14) . . ? C95 C92 C94 106.5(13) . . ? C91 C92 C94 106.6(9) . . ? N6 C96 C97 123.2(10) . . ? N6 C96 C108 113.8(10) . . ? C97 C96 C108 122.9(10) . . ? C96 C97 C98 118.7(12) . . ? C97 C98 C99 118.4(13) . . ? C100 C99 C98 120.0(11) . . ? N6 C100 C99 122.1(11) . . ? N6 C100 C101 114.0(10) . . ? C99 C100 C101 123.9(10) . . ? O21 C101 C102 124.5(10) . . ? O21 C101 C100 116.2(9) . . ? C102 C101 C100 119.2(11) . . ? C103 C102 C101 122.9(12) . . ? O22 C103 C102 124.9(10) . . ? O22 C103 C104 112.9(11) . . ? C102 C103 C104 122.2(12) . . ? C105 C104 C106 119(2) . . ? C105 C104 C103 110.9(12) . . ? C106 C104 C103 105.0(13) . . ? C105 C104 C107 107(2) . . ? C106 C104 C107 104.8(15) . . ? C103 C104 C107 109.7(12) . . ? O23 C108 C109 124.8(9) . . ? O23 C108 C96 116.3(9) . . ? C109 C108 C96 118.9(10) . . ? C108 C109 C110 120.7(11) . . ? O24 C110 C109 125.0(10) . . ? O24 C110 C111 114.3(9) . . ? C109 C110 C111 120.7(10) . . ? C113 C111 C112 111.1(16) . . ? C113 C111 C114 112.7(16) . . ? C112 C111 C114 105.5(13) . . ? C113 C111 C110 106.9(11) . . ? C112 C111 C110 109.4(10) . . ? C114 C111 C110 111.3(11) . . ? C221 O220 C224 107.1(10) . . ? C221 O220 Ba2 126.7(7) . . ? C224 O220 Ba2 125.4(7) . . ? O220 C221 C222 109.6(11) . . ? C221 C222 C223 103.2(11) . . ? C224 C223 C222 104.3(11) . . ? O220 C224 C223 109.7(11) . . ? C231 O230 C234 105.9(9) . . ? C231 O230 Ba2 119.6(7) . . ? C234 O230 Ba2 132.9(7) . . ? O230 C231 C232 108.9(12) . . ? C231 C232 C233 103.5(12) . . ? C232 C233 C234 106.8(12) . . ? O230 C234 C233 103.1(11) . . ? Cl71 Fe7 Cl74 110.9(3) . . ? Cl71 Fe7 Cl72 110.0(2) . . ? Cl74 Fe7 Cl72 106.3(2) . . ? Cl71 Fe7 Cl73 106.80(18) . . ? Cl74 Fe7 Cl73 113.2(2) . . ? Cl72 Fe7 Cl73 109.78(16) . . ? Cl86 Fe8 Cl83 58.4(10) . . ? Cl86 Fe8 Cl82 116.0(7) . . ? Cl83 Fe8 Cl82 120.7(4) . . ? Cl86 Fe8 Cl81 122.9(6) . . ? Cl83 Fe8 Cl81 114.3(3) . . ? Cl82 Fe8 Cl81 113.8(2) . . ? Cl86 Fe8 Cl85 100.8(12) . . ? Cl83 Fe8 Cl85 43.1(6) . . ? Cl82 Fe8 Cl85 97.0(4) . . ? Cl81 Fe8 Cl85 99.1(4) . . ? Cl86 Fe8 Cl84 46.2(11) . . ? Cl83 Fe8 Cl84 104.1(5) . . ? Cl82 Fe8 Cl84 99.8(4) . . ? Cl81 Fe8 Cl84 99.8(3) . . ? Cl85 Fe8 Cl84 147.0(6) . . ? Cl31 C300 Cl32 93(4) . . ? _diffrn_measured_fraction_theta_max 0.267 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.267 _refine_diff_density_max 1.693 _refine_diff_density_min -1.694 _refine_diff_density_rms 0.125 #======END OF DATA FOR Ba-4a # 4.4 RESULTS FOR La-4a data_rouge _database_code_CSD 152456 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69.50 H104 Cl13 Fe5 La N3 O17' _chemical_formula_weight 2132.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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 14.792(2) _cell_length_b 16.969(3) _cell_length_c 20.647(3) _cell_angle_alpha 68.83(2) _cell_angle_beta 84.05(2) _cell_angle_gamma 75.21(2) _cell_volume 4672.3(12) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 78110 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 26.37 _exptl_crystal_description block _exptl_crystal_colour rouge _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2172 _exptl_absorpt_coefficient_mu 1.633 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5612 _exptl_absorpt_correction_T_max 0.7360 _exptl_absorpt_process_details ? _exptl_special_details ; 'Intensities were measured with a Siemens CCD area detector' ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe-Siemens-Huber four circle diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 78110 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 26.37 _reflns_number_total 19088 _reflns_number_gt 12707 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (V. 4.202, Siemens 1996)' _computing_cell_refinement 'Siemens SAINT (V. 4.050, Siemens 1996)' _computing_data_reduction 'Siemens SAINT (V. 4.050, Siemens 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHELXTL (V. 5.10)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0417P)^2^+1.3076P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19088 _refine_ls_number_parameters 1350 _refine_ls_number_restraints 2287 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.0966 _refine_ls_wR_factor_gt 0.0861 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.30120(4) 0.48389(4) 0.28232(3) 0.01979(14) Uani 1 1 d . A . La1 La 0.257902(17) 0.298465(16) 0.260208(13) 0.01778(7) Uani 1 1 d . A . Fe2 Fe 0.21871(4) 0.11638(4) 0.22730(3) 0.02441(15) Uani 1 1 d . A . O1 O 0.1223(2) 0.2980(2) 0.34410(17) 0.0283(8) Uani 1 1 d D . . H11 H 0.082(2) 0.334(2) 0.341(3) 0.042(9) Uiso 1 1 d D . . H12 H 0.114(3) 0.263(3) 0.3756(18) 0.042(9) Uiso 1 1 d D . . O2 O 0.4283(2) 0.2199(2) 0.27796(16) 0.0298(8) Uani 1 1 d D . . H21 H 0.448(3) 0.210(3) 0.3115(16) 0.042(9) Uiso 1 1 d D . . H22 H 0.457(3) 0.205(3) 0.252(2) 0.042(9) Uiso 1 1 d D . . N1 N 0.3758(2) 0.3286(2) 0.13880(17) 0.0204(8) Uani 1 1 d . A . O11 O 0.4246(2) 0.51037(19) 0.27326(15) 0.0274(7) Uani 1 1 d . . . O12 O 0.35544(19) 0.41703(18) 0.22001(14) 0.0229(7) Uani 1 1 d . . . O13 O 0.30734(19) 0.19050(19) 0.17906(14) 0.0256(7) Uani 1 1 d . . . C105 C 0.4889(3) 0.5094(3) 0.2280(2) 0.0246(10) Uani 1 1 d D A . C101 C 0.5622(3) 0.5593(3) 0.2248(2) 0.0310(10) Uani 1 1 d DU . . C102 C 0.5658(6) 0.6251(5) 0.1542(3) 0.059(2) Uani 0.722(5) 1 d PDU A 1 H10A H 0.6134 0.6567 0.1527 0.088 Uiso 0.722(5) 1 calc PR A 1 H10B H 0.5046 0.6660 0.1434 0.088 Uiso 0.722(5) 1 calc PR A 1 H10C H 0.5817 0.5958 0.1200 0.088 Uiso 0.722(5) 1 calc PR A 1 C103 C 0.6572(4) 0.4947(4) 0.2442(4) 0.0446(17) Uani 0.722(5) 1 d PDU A 1 H10D H 0.6532 0.4524 0.2910 0.067 Uiso 0.722(5) 1 calc PR A 1 H10E H 0.7048 0.5261 0.2431 0.067 Uiso 0.722(5) 1 calc PR A 1 H10F H 0.6743 0.4641 0.2108 0.067 Uiso 0.722(5) 1 calc PR A 1 C104 C 0.5395(5) 0.6035(5) 0.2790(4) 0.0480(17) Uani 0.722(5) 1 d PDU A 1 H10G H 0.5383 0.5594 0.3254 0.072 Uiso 0.722(5) 1 calc PR A 1 H10H H 0.4782 0.6445 0.2694 0.072 Uiso 0.722(5) 1 calc PR A 1 H10I H 0.5874 0.6349 0.2772 0.072 Uiso 0.722(5) 1 calc PR A 1 C122 C 0.6475(8) 0.5346(11) 0.1815(9) 0.0480(17) Uani 0.278(5) 1 d PDU A 2 H12A H 0.6272 0.5415 0.1356 0.072 Uiso 0.278(5) 1 calc PR A 2 H12B H 0.6800 0.4739 0.2049 0.072 Uiso 0.278(5) 1 calc PR A 2 H12C H 0.6900 0.5725 0.1760 0.072 Uiso 0.278(5) 1 calc PR A 2 C123 C 0.5893(13) 0.5491(13) 0.2953(5) 0.059(2) Uani 0.278(5) 1 d PDU A 2 H12D H 0.6368 0.5818 0.2912 0.088 Uiso 0.278(5) 1 calc PR A 2 H12E H 0.6148 0.4874 0.3213 0.088 Uiso 0.278(5) 1 calc PR A 2 H12F H 0.5342 0.5714 0.3199 0.088 Uiso 0.278(5) 1 calc PR A 2 C124 C 0.5151(10) 0.6543(5) 0.1837(9) 0.0446(17) Uani 0.278(5) 1 d PDU A 2 H12G H 0.5001 0.6592 0.1371 0.067 Uiso 0.278(5) 1 calc PR A 2 H12H H 0.5578 0.6915 0.1800 0.067 Uiso 0.278(5) 1 calc PR A 2 H12I H 0.4575 0.6728 0.2079 0.067 Uiso 0.278(5) 1 calc PR A 2 C106 C 0.4920(3) 0.4681(3) 0.1802(2) 0.0240(10) Uani 1 1 d . . . H106 H 0.5421 0.4699 0.1474 0.029 Uiso 1 1 calc R A . C107 C 0.4264(3) 0.4249(3) 0.1781(2) 0.0212(9) Uani 1 1 d . A . C108 C 0.4315(3) 0.3836(3) 0.1260(2) 0.0231(10) Uani 1 1 d . . . C109 C 0.4875(3) 0.4025(3) 0.0674(2) 0.0330(11) Uani 1 1 d . A . H109 H 0.5261 0.4420 0.0600 0.040 Uiso 1 1 calc R . . C110 C 0.4865(3) 0.3635(3) 0.0204(2) 0.0377(12) Uani 1 1 d . . . H110 H 0.5236 0.3763 -0.0208 0.045 Uiso 1 1 calc R A . C111 C 0.4313(3) 0.3055(3) 0.0334(2) 0.0351(12) Uani 1 1 d . A . H111 H 0.4295 0.2776 0.0013 0.042 Uiso 1 1 calc R . . C112 C 0.3790(3) 0.2885(3) 0.0933(2) 0.0253(10) Uani 1 1 d . . . C113 C 0.3219(3) 0.2230(3) 0.1138(2) 0.0260(10) Uani 1 1 d D A . C114 C 0.2888(4) 0.2014(3) 0.0649(2) 0.0407(12) Uani 1 1 d DU . . H114 H 0.3069 0.2271 0.0179 0.049 Uiso 1 1 calc R A 1 O14 O 0.2078(2) 0.1029(2) 0.13885(16) 0.0362(8) Uani 1 1 d DU . . C115 C 0.2304(8) 0.1444(6) 0.0787(3) 0.0352(19) Uani 0.605(6) 1 d PDU A 1 C116 C 0.1988(5) 0.1177(5) 0.0236(3) 0.0456(19) Uani 0.605(6) 1 d PDU A 1 C117 C 0.2766(7) 0.0422(6) 0.0175(5) 0.069(3) Uani 0.605(6) 1 d PDU A 1 H11A H 0.2874 -0.0039 0.0631 0.104 Uiso 0.605(6) 1 calc PR A 1 H11B H 0.3340 0.0624 0.0008 0.104 Uiso 0.605(6) 1 calc PR A 1 H11C H 0.2583 0.0196 -0.0154 0.104 Uiso 0.605(6) 1 calc PR A 1 C118 C 0.1088(6) 0.0861(7) 0.0451(4) 0.065(3) Uani 0.605(6) 1 d PDU A 1 H11D H 0.0575 0.1345 0.0479 0.097 Uiso 0.605(6) 1 calc PR A 1 H11E H 0.1171 0.0395 0.0906 0.097 Uiso 0.605(6) 1 calc PR A 1 H11F H 0.0941 0.0640 0.0106 0.097 Uiso 0.605(6) 1 calc PR A 1 C119 C 0.1828(8) 0.1933(6) -0.0439(4) 0.063(3) Uani 0.605(6) 1 d PDU A 1 H11G H 0.1353 0.2417 -0.0370 0.095 Uiso 0.605(6) 1 calc PR A 1 H11H H 0.1614 0.1757 -0.0789 0.095 Uiso 0.605(6) 1 calc PR A 1 H11I H 0.2414 0.2116 -0.0599 0.095 Uiso 0.605(6) 1 calc PR A 1 C125 C 0.2457(12) 0.1329(9) 0.0801(4) 0.036(2) Uani 0.395(6) 1 d PDU A 2 C126 C 0.2254(8) 0.1097(7) 0.0195(5) 0.046(2) Uani 0.395(6) 1 d PDU A 2 C127 C 0.3010(8) 0.1197(9) -0.0371(6) 0.054(3) Uani 0.395(6) 1 d PDU A 2 H12J H 0.3604 0.0802 -0.0179 0.082 Uiso 0.395(6) 1 calc PR A 2 H12K H 0.3079 0.1798 -0.0546 0.082 Uiso 0.395(6) 1 calc PR A 2 H12L H 0.2831 0.1055 -0.0753 0.082 Uiso 0.395(6) 1 calc PR A 2 C128 C 0.2169(11) 0.0161(7) 0.0478(7) 0.061(4) Uani 0.395(6) 1 d PDU A 2 H12M H 0.2726 -0.0209 0.0746 0.091 Uiso 0.395(6) 1 calc PR A 2 H12N H 0.2111 -0.0029 0.0092 0.091 Uiso 0.395(6) 1 calc PR A 2 H12O H 0.1613 0.0115 0.0780 0.091 Uiso 0.395(6) 1 calc PR A 2 C129 C 0.1346(8) 0.1711(9) -0.0126(7) 0.064(4) Uani 0.395(6) 1 d PDU A 2 H12P H 0.1162 0.1540 -0.0489 0.095 Uiso 0.395(6) 1 calc PR A 2 H12Q H 0.1433 0.2306 -0.0329 0.095 Uiso 0.395(6) 1 calc PR A 2 H12R H 0.0856 0.1684 0.0234 0.095 Uiso 0.395(6) 1 calc PR A 2 N2 N 0.3012(2) 0.1971(2) 0.39652(17) 0.0182(7) Uani 1 1 d . A . O21 O 0.28205(19) 0.50972(18) 0.36732(14) 0.0243(7) Uani 1 1 d . . . O22 O 0.30163(18) 0.36067(17) 0.34622(14) 0.0205(6) Uani 1 1 d . . . O23 O 0.26110(19) 0.13428(17) 0.30893(14) 0.0214(6) Uani 1 1 d . . . O24 O 0.2884(2) -0.00286(18) 0.26812(15) 0.0276(7) Uani 1 1 d . . . C201 C 0.3085(3) 0.5119(3) 0.4763(2) 0.0286(11) Uani 1 1 d . . . C202 C 0.3875(3) 0.5576(3) 0.4446(3) 0.0415(13) Uani 1 1 d . . . H20A H 0.3720 0.5961 0.3967 0.062 Uiso 1 1 calc R . . H20B H 0.4457 0.5141 0.4448 0.062 Uiso 1 1 calc R . . H20C H 0.3955 0.5920 0.4720 0.062 Uiso 1 1 calc R . . C203 C 0.3317(4) 0.4539(3) 0.5504(2) 0.0458(14) Uani 1 1 d . . . H20D H 0.3410 0.4889 0.5769 0.069 Uiso 1 1 calc R . . H20E H 0.3891 0.4093 0.5512 0.069 Uiso 1 1 calc R . . H20F H 0.2802 0.4260 0.5713 0.069 Uiso 1 1 calc R . . C204 C 0.2174(3) 0.5783(3) 0.4750(3) 0.0415(13) Uani 1 1 d . . . H20G H 0.2024 0.6163 0.4269 0.062 Uiso 1 1 calc R . . H20H H 0.2238 0.6134 0.5023 0.062 Uiso 1 1 calc R . . H20I H 0.1671 0.5484 0.4950 0.062 Uiso 1 1 calc R . . C205 C 0.2988(3) 0.4630(3) 0.4302(2) 0.0241(10) Uani 1 1 d . . . C206 C 0.3078(3) 0.3733(3) 0.4548(2) 0.0248(10) Uani 1 1 d . . . H206 H 0.3153 0.3425 0.5033 0.030 Uiso 1 1 calc R . . C207 C 0.3064(3) 0.3272(3) 0.4125(2) 0.0198(9) Uani 1 1 d . . . C208 C 0.3100(3) 0.2329(3) 0.4427(2) 0.0215(9) Uani 1 1 d . . . C209 C 0.3218(3) 0.1855(3) 0.5125(2) 0.0292(11) Uani 1 1 d . . . H209 H 0.3269 0.2128 0.5444 0.035 Uiso 1 1 calc R . . C210 C 0.3259(3) 0.0978(3) 0.5351(2) 0.0352(12) Uani 1 1 d . . . H210 H 0.3334 0.0639 0.5831 0.042 Uiso 1 1 calc R . . C211 C 0.3190(3) 0.0602(3) 0.4887(2) 0.0303(11) Uani 1 1 d . A . H211 H 0.3225 -0.0004 0.5034 0.036 Uiso 1 1 calc R . . C212 C 0.3070(3) 0.1115(3) 0.4197(2) 0.0217(9) Uani 1 1 d . . . C213 C 0.2964(3) 0.0765(3) 0.3660(2) 0.0235(10) Uani 1 1 d . A . C214 C 0.3225(3) -0.0108(3) 0.3781(2) 0.0328(11) Uani 1 1 d . . . H214 H 0.3451 -0.0485 0.4229 0.039 Uiso 1 1 calc R A . C215 C 0.3180(3) -0.0478(3) 0.3284(2) 0.0279(10) Uani 1 1 d . A . C216 C 0.3442(4) -0.1451(3) 0.3463(3) 0.0379(12) Uani 1 1 d . . . C217 C 0.3742(5) -0.1668(4) 0.2819(3) 0.070(2) Uani 1 1 d . A . H21A H 0.3220 -0.1430 0.2494 0.105 Uiso 1 1 calc R . . H21B H 0.3930 -0.2301 0.2942 0.105 Uiso 1 1 calc R . . H21C H 0.4272 -0.1415 0.2600 0.105 Uiso 1 1 calc R . . C218 C 0.2542(5) -0.1747(4) 0.3762(4) 0.076(2) Uani 1 1 d . A . H21D H 0.2344 -0.1593 0.4177 0.114 Uiso 1 1 calc R . . H21E H 0.2658 -0.2379 0.3885 0.114 Uiso 1 1 calc R . . H21F H 0.2049 -0.1460 0.3413 0.114 Uiso 1 1 calc R . . C219 C 0.4214(4) -0.1900(3) 0.3992(3) 0.0540(16) Uani 1 1 d . A . H21G H 0.4728 -0.1604 0.3850 0.081 Uiso 1 1 calc R . . H21H H 0.4442 -0.2507 0.4022 0.081 Uiso 1 1 calc R . . H21I H 0.3970 -0.1879 0.4447 0.081 Uiso 1 1 calc R . . N3 N 0.0830(2) 0.3991(2) 0.19825(18) 0.0250(8) Uani 1 1 d . . . O32 O 0.18652(18) 0.46486(18) 0.24862(14) 0.0215(6) Uani 1 1 d . . . O33 O 0.1417(2) 0.23561(18) 0.21779(15) 0.0285(7) Uani 1 1 d . . . O31 O 0.2485(2) 0.60643(18) 0.23423(15) 0.0274(7) Uani 1 1 d D . . C306 C 0.1104(3) 0.6097(3) 0.1881(2) 0.0287(11) Uani 1 1 d D . . H306 H 0.0562 0.6460 0.1625 0.034 Uiso 1 1 calc R A . C305 C 0.1725(3) 0.6488(2) 0.2028(2) 0.0306(10) Uani 1 1 d DU A . C301 C 0.1546(9) 0.7468(4) 0.1838(7) 0.052(3) Uani 0.49(5) 1 d PDU A 1 C302 C 0.146(2) 0.7630(11) 0.2525(9) 0.070(4) Uani 0.49(5) 1 d PDU A 1 H30A H 0.1345 0.8256 0.2432 0.105 Uiso 0.49(5) 1 calc PR A 1 H30B H 0.2043 0.7331 0.2783 0.105 Uiso 0.49(5) 1 calc PR A 1 H30C H 0.0940 0.7408 0.2800 0.105 Uiso 0.49(5) 1 calc PR A 1 C303 C 0.2389(12) 0.7765(11) 0.1430(15) 0.067(5) Uani 0.49(5) 1 d PDU A 1 H30D H 0.2285 0.8396 0.1302 0.100 Uiso 0.49(5) 1 calc PR A 1 H30E H 0.2477 0.7614 0.1008 0.100 Uiso 0.49(5) 1 calc PR A 1 H30F H 0.2949 0.7476 0.1716 0.100 Uiso 0.49(5) 1 calc PR A 1 C304 C 0.0660(13) 0.7953(11) 0.1425(14) 0.064(4) Uani 0.49(5) 1 d PDU A 1 H30G H 0.0577 0.8579 0.1314 0.096 Uiso 0.49(5) 1 calc PR A 1 H30H H 0.0122 0.7766 0.1700 0.096 Uiso 0.49(5) 1 calc PR A 1 H30I H 0.0707 0.7827 0.0993 0.096 Uiso 0.49(5) 1 calc PR A 1 C321 C 0.1495(8) 0.7467(4) 0.1857(6) 0.051(2) Uani 0.51(5) 1 d PDU A 2 C322 C 0.105(2) 0.7620(11) 0.2514(9) 0.079(5) Uani 0.51(5) 1 d PDU A 2 H32A H 0.0885 0.8245 0.2434 0.118 Uiso 0.51(5) 1 calc PR A 2 H32B H 0.1492 0.7319 0.2897 0.118 Uiso 0.51(5) 1 calc PR A 2 H32C H 0.0483 0.7395 0.2634 0.118 Uiso 0.51(5) 1 calc PR A 2 C323 C 0.2403(11) 0.7769(10) 0.1687(15) 0.069(4) Uani 0.51(5) 1 d PDU A 2 H32D H 0.2268 0.8398 0.1580 0.104 Uiso 0.51(5) 1 calc PR A 2 H32E H 0.2707 0.7629 0.1284 0.104 Uiso 0.51(5) 1 calc PR A 2 H32F H 0.2820 0.7473 0.2086 0.104 Uiso 0.51(5) 1 calc PR A 2 C324 C 0.0848(17) 0.7952(10) 0.1241(12) 0.068(4) Uani 0.51(5) 1 d PDU A 2 H32G H 0.0714 0.8578 0.1153 0.102 Uiso 0.51(5) 1 calc PR A 2 H32H H 0.0262 0.7759 0.1343 0.102 Uiso 0.51(5) 1 calc PR A 2 H32I H 0.1149 0.7834 0.0829 0.102 Uiso 0.51(5) 1 calc PR A 2 C307 C 0.1222(3) 0.5215(3) 0.2082(2) 0.0212(9) Uani 1 1 d . A . C308 C 0.0571(3) 0.4850(3) 0.1834(2) 0.0232(10) Uani 1 1 d . A . C309 C -0.0241(3) 0.5356(3) 0.1485(2) 0.0323(11) Uani 1 1 d . . . H309 H -0.0399 0.5967 0.1384 0.039 Uiso 1 1 calc R A . C310 C -0.0815(3) 0.4974(3) 0.1285(3) 0.0428(13) Uani 1 1 d . A . H310 H -0.1369 0.5312 0.1034 0.051 Uiso 1 1 calc R . . C311 C -0.0571(3) 0.4090(3) 0.1457(3) 0.0424(13) Uani 1 1 d . . . H311 H -0.0967 0.3802 0.1338 0.051 Uiso 1 1 calc R A . C312 C 0.0250(3) 0.3620(3) 0.1802(2) 0.0303(11) Uani 1 1 d . A . C313 C 0.0549(3) 0.2664(3) 0.2013(2) 0.0313(11) Uani 1 1 d . A . C314 C -0.0058(3) 0.2161(3) 0.2041(3) 0.0419(13) Uani 1 1 d D . . H314 H -0.0668 0.2443 0.1860 0.050 Uiso 1 1 calc R A . O34 O 0.0999(2) 0.08143(19) 0.25397(16) 0.0307(7) Uani 1 1 d D . . C315 C 0.0182(3) 0.1250(3) 0.2324(3) 0.0365(11) Uani 1 1 d DU A . C316 C -0.0555(4) 0.0736(4) 0.2414(4) 0.0474(16) Uani 0.765(8) 1 d PDU A 1 C317 C -0.1316(5) 0.0957(6) 0.2919(5) 0.084(3) Uani 0.765(8) 1 d PDU A 1 H31A H -0.1046 0.0780 0.3378 0.126 Uiso 0.765(8) 1 calc PR A 1 H31B H -0.1806 0.0648 0.2952 0.126 Uiso 0.765(8) 1 calc PR A 1 H31C H -0.1588 0.1585 0.2751 0.126 Uiso 0.765(8) 1 calc PR A 1 C318 C -0.0098(6) -0.0229(4) 0.2693(6) 0.078(3) Uani 0.765(8) 1 d PDU A 1 H31D H 0.0213 -0.0369 0.3131 0.117 Uiso 0.765(8) 1 calc PR A 1 H31E H 0.0363 -0.0378 0.2354 0.117 Uiso 0.765(8) 1 calc PR A 1 H31F H -0.0577 -0.0562 0.2775 0.117 Uiso 0.765(8) 1 calc PR A 1 C319 C -0.0992(7) 0.0983(6) 0.1713(4) 0.080(3) Uani 0.765(8) 1 d PDU A 1 H31G H -0.1281 0.1608 0.1540 0.120 Uiso 0.765(8) 1 calc PR A 1 H31H H -0.1469 0.0657 0.1762 0.120 Uiso 0.765(8) 1 calc PR A 1 H31I H -0.0507 0.0845 0.1383 0.120 Uiso 0.765(8) 1 calc PR A 1 C326 C -0.0469(8) 0.0706(8) 0.2285(8) 0.052(3) Uani 0.235(8) 1 d PDU A 2 C327 C -0.0186(17) 0.0416(16) 0.1664(10) 0.068(5) Uani 0.235(8) 1 d PDU A 2 H32J H 0.0466 0.0083 0.1711 0.102 Uiso 0.235(8) 1 calc PR A 2 H32K H -0.0251 0.0927 0.1237 0.102 Uiso 0.235(8) 1 calc PR A 2 H32L H -0.0591 0.0050 0.1642 0.102 Uiso 0.235(8) 1 calc PR A 2 C328 C -0.0361(17) -0.0084(11) 0.2948(10) 0.057(5) Uani 0.235(8) 1 d PDU A 2 H32M H 0.0248 -0.0482 0.2943 0.086 Uiso 0.235(8) 1 calc PR A 2 H32N H -0.0860 -0.0382 0.2980 0.086 Uiso 0.235(8) 1 calc PR A 2 H32O H -0.0402 0.0101 0.3350 0.086 Uiso 0.235(8) 1 calc PR A 2 C329 C -0.1464(8) 0.1252(13) 0.2211(16) 0.075(5) Uani 0.235(8) 1 d PDU A 2 H32P H -0.1502 0.1785 0.1805 0.112 Uiso 0.235(8) 1 calc PR A 2 H32Q H -0.1648 0.1403 0.2629 0.112 Uiso 0.235(8) 1 calc PR A 2 H32R H -0.1883 0.0920 0.2152 0.112 Uiso 0.235(8) 1 calc PR A 2 Fe3 Fe 0.78197(15) 0.76461(15) 0.27130(11) 0.0394(4) Uani 0.742(6) 1 d PDU B 1 Cl31 Cl 0.8013(3) 0.6737(2) 0.2175(2) 0.0507(9) Uani 0.742(6) 1 d PDU B 1 Cl32 Cl 0.7996(3) 0.8903(2) 0.2009(3) 0.0736(11) Uani 0.742(6) 1 d PDU B 1 Cl33 Cl 0.64250(19) 0.77939(17) 0.31636(15) 0.0776(10) Uani 0.742(6) 1 d PD U B 1 Cl34 Cl 0.8773(3) 0.7121(2) 0.3574(2) 0.1241(16) Uani 0.742(6) 1 d PDU B 1 Fe4 Fe 0.7642(5) 0.7825(6) 0.2501(5) 0.077(2) Uani 0.258(6) 1 d PDU B 2 Cl41 Cl 0.8244(10) 0.6843(8) 0.2026(8) 0.086(4) Uani 0.258(6) 1 d PDU B 2 Cl42 Cl 0.8215(11) 0.8936(8) 0.1954(7) 0.093(4) Uani 0.258(6) 1 d PDU B 2 Cl43 Cl 0.8016(14) 0.7267(8) 0.3591(4) 0.181(6) Uani 0.258(6) 1 d PDU B 2 Cl44 Cl 0.6160(5) 0.8111(9) 0.2392(12) 0.220(9) Uani 0.258(6) 1 d PDU B 2 Fe5 Fe 0.20841(8) 0.59428(8) -0.00085(6) 0.0397(3) Uani 0.934(2) 1 d PDU C 1 Cl51 Cl 0.27301(10) 0.62468(14) -0.10370(7) 0.0623(6) Uani 0.934(2) 1 d PDU C 1 Cl52 Cl 0.19037(11) 0.46203(10) 0.03626(8) 0.0606(5) Uani 0.934(2) 1 d PDU C 1 Cl53 Cl 0.07201(10) 0.68421(11) -0.00816(8) 0.0541(5) Uani 0.934(2) 1 d PDU C 1 Cl54 Cl 0.29880(16) 0.60779(17) 0.06876(11) 0.0536(6) Uani 0.934(2) 1 d PDU C 1 Fe6 Fe 0.2231(10) 0.6068(10) -0.0171(7) 0.047(4) Uani 0.066(2) 1 d PDU C 2 Cl61 Cl 0.2421(13) 0.7104(12) -0.1129(9) 0.064(6) Uani 0.066(2) 1 d PDU C 2 Cl62 Cl 0.2869(11) 0.4830(10) -0.0293(10) 0.052(5) Uani 0.066(2) 1 d PDU C 2 Cl63 Cl 0.0747(10) 0.6174(13) 0.0048(10) 0.046(5) Uani 0.066(2) 1 d PDU C 2 Cl64 Cl 0.287(2) 0.621(2) 0.0668(13) 0.066(8) Uani 0.066(2) 1 d PDU C 2 Fe7 Fe 0.6367(4) 0.2282(3) 0.3920(3) 0.0342(7) Uani 0.74(3) 1 d PDU D 1 Cl71 Cl 0.7668(5) 0.1506(5) 0.4456(4) 0.0510(11) Uani 0.74(3) 1 d PDU D 1 Cl72 Cl 0.5774(10) 0.3408(3) 0.4215(3) 0.0729(18) Uani 0.74(3) 1 d PDU D 1 Cl73 Cl 0.6525(6) 0.2696(5) 0.2812(3) 0.0545(16) Uani 0.74(3) 1 d PDU D 1 Cl74 Cl 0.5390(6) 0.1418(6) 0.4227(5) 0.0448(14) Uani 0.74(3) 1 d PDU D 1 Fe8 Fe 0.6516(13) 0.2211(9) 0.3922(7) 0.0300(19) Uani 0.26(3) 1 d PDU D 2 Cl81 Cl 0.7804(15) 0.1300(17) 0.4376(13) 0.063(5) Uani 0.26(3) 1 d PDU D 2 Cl82 Cl 0.627(2) 0.3336(11) 0.4230(7) 0.063(4) Uani 0.26(3) 1 d PDU D 2 Cl83 Cl 0.6598(16) 0.2632(12) 0.2802(7) 0.042(3) Uani 0.26(3) 1 d PDU D 2 Cl84 Cl 0.5383(15) 0.1539(15) 0.4281(12) 0.034(3) Uani 0.26(3) 1 d PDU D 2 C1D C 0.0505(4) 0.4858(4) 0.4013(3) 0.0627(18) Uani 1 1 d D . . H1D1 H 0.0425 0.4503 0.4499 0.094 Uiso 1 1 calc R . . H1D2 H 0.0580 0.5426 0.3987 0.094 Uiso 1 1 calc R . . H1D3 H 0.1062 0.4564 0.3815 0.094 Uiso 1 1 calc R . . C2D C -0.0333(3) 0.4979(3) 0.3614(3) 0.0453(14) Uani 1 1 d D . . H2D1 H -0.0906 0.5218 0.3840 0.054 Uiso 1 1 calc R . . H2D2 H -0.0293 0.5394 0.3136 0.054 Uiso 1 1 calc R . . O1D O -0.0373(2) 0.4170(2) 0.35914(17) 0.0401(9) Uani 1 1 d D . . C3D C -0.1217(3) 0.4211(3) 0.3297(3) 0.0471(14) Uani 1 1 d D . . H3D1 H -0.1236 0.4577 0.2799 0.057 Uiso 1 1 calc R . . H3D2 H -0.1760 0.4473 0.3535 0.057 Uiso 1 1 calc R . . C4D C -0.1264(4) 0.3313(3) 0.3374(3) 0.0616(17) Uani 1 1 d D . . H4D1 H -0.0697 0.3037 0.3174 0.092 Uiso 1 1 calc R . . H4D2 H -0.1813 0.3341 0.3132 0.092 Uiso 1 1 calc R . . H4D3 H -0.1313 0.2971 0.3868 0.092 Uiso 1 1 calc R . . C1E C 0.5830(15) 0.0097(11) 0.2832(8) 0.073(5) Uani 0.373(8) 1 d PDU E 1 H1E1 H 0.5823 -0.0520 0.3021 0.110 Uiso 0.373(8) 1 calc PR E 1 H1E2 H 0.5524 0.0379 0.3162 0.110 Uiso 0.373(8) 1 calc PR E 1 H1E3 H 0.6479 0.0155 0.2754 0.110 Uiso 0.373(8) 1 calc PR E 1 C2E C 0.5320(10) 0.0521(8) 0.2158(7) 0.057(3) Uani 0.373(8) 1 d PDU E 1 H2E1 H 0.5626 0.0235 0.1825 0.069 Uiso 0.373(8) 1 calc PR E 1 H2E2 H 0.4668 0.0453 0.2234 0.069 Uiso 0.373(8) 1 calc PR E 1 O1E O 0.5317(10) 0.1411(8) 0.1880(8) 0.052(3) Uani 0.373(8) 1 d PDU E 1 C3E C 0.6190(15) 0.1575(14) 0.1609(14) 0.054(4) Uani 0.373(8) 1 d PDU E 1 H3E1 H 0.6668 0.1254 0.1973 0.064 Uiso 0.373(8) 1 calc PR E 1 H3E2 H 0.6157 0.2203 0.1478 0.064 Uiso 0.373(8) 1 calc PR E 1 C4E C 0.648(3) 0.131(3) 0.0986(19) 0.079(8) Uani 0.373(8) 1 d PDU E 1 H4E1 H 0.7091 0.1443 0.0813 0.118 Uiso 0.373(8) 1 calc PR E 1 H4E2 H 0.6017 0.1632 0.0621 0.118 Uiso 0.373(8) 1 calc PR E 1 H4E3 H 0.6538 0.0686 0.1115 0.118 Uiso 0.373(8) 1 calc PR E 1 C1G C 0.5257(7) 0.0159(6) 0.2940(5) 0.055(3) Uani 0.627(8) 1 d PDU E 2 H1G1 H 0.5536 -0.0435 0.3241 0.082 Uiso 0.627(8) 1 calc PR E 2 H1G2 H 0.4764 0.0150 0.2663 0.082 Uiso 0.627(8) 1 calc PR E 2 H1G3 H 0.4990 0.0515 0.3227 0.082 Uiso 0.627(8) 1 calc PR E 2 C2G C 0.5998(6) 0.0539(5) 0.2465(5) 0.056(3) Uani 0.627(8) 1 d PDU E 2 H2G1 H 0.6503 0.0547 0.2741 0.067 Uiso 0.627(8) 1 calc PR E 2 H2G2 H 0.6274 0.0183 0.2173 0.067 Uiso 0.627(8) 1 calc PR E 2 O1G O 0.5578(6) 0.1395(5) 0.2040(5) 0.047(2) Uani 0.627(8) 1 d PDU E 2 C3G C 0.6224(10) 0.1818(7) 0.1592(8) 0.049(2) Uani 0.627(8) 1 d PDU E 2 H3G1 H 0.6782 0.1721 0.1863 0.058 Uiso 0.627(8) 1 calc PR E 2 H3G2 H 0.5941 0.2451 0.1419 0.058 Uiso 0.627(8) 1 calc PR E 2 C4G C 0.6535(17) 0.1533(14) 0.0979(10) 0.061(4) Uani 0.627(8) 1 d PDU E 2 H4G1 H 0.6985 0.1858 0.0698 0.091 Uiso 0.627(8) 1 calc PR E 2 H4G2 H 0.5992 0.1644 0.0697 0.091 Uiso 0.627(8) 1 calc PR E 2 H4G3 H 0.6831 0.0910 0.1143 0.091 Uiso 0.627(8) 1 calc PR E 2 C1F C -0.0234(4) 0.2457(5) 0.5390(4) 0.093(2) Uani 1 1 d D . . H1F1 H -0.0500 0.2926 0.4967 0.139 Uiso 1 1 calc R . . H1F2 H -0.0254 0.2693 0.5761 0.139 Uiso 1 1 calc R . . H1F3 H -0.0598 0.2012 0.5532 0.139 Uiso 1 1 calc R . . C2F C 0.0750(4) 0.2062(4) 0.5252(3) 0.0578(16) Uani 1 1 d D . . H2F1 H 0.1133 0.2491 0.5172 0.069 Uiso 1 1 calc R . . H2F2 H 0.0996 0.1553 0.5666 0.069 Uiso 1 1 calc R . . O1F O 0.0839(2) 0.1798(2) 0.46752(17) 0.0465(9) Uani 1 1 d D . . C3F C 0.0497(4) 0.1061(4) 0.4787(3) 0.0633(18) Uani 1 1 d D . . H3F1 H -0.0160 0.1162 0.4953 0.076 Uiso 1 1 calc R . . H3F2 H 0.0870 0.0556 0.5149 0.076 Uiso 1 1 calc R . . C4F C 0.0547(4) 0.0871(4) 0.4141(3) 0.0649(18) Uani 1 1 d D . . H4F1 H 0.0113 0.1337 0.3803 0.097 Uiso 1 1 calc R . . H4F2 H 0.0376 0.0317 0.4240 0.097 Uiso 1 1 calc R . . H4F3 H 0.1185 0.0832 0.3951 0.097 Uiso 1 1 calc R . . C1L C 0.4642(18) 0.1242(15) -0.1304(10) 0.082(5) Uani 0.327(18) 1 d PDU F -1 H1L1 H 0.4826 0.1676 -0.1732 0.098 Uiso 0.327(18) 1 calc PR F -1 H1L2 H 0.3951 0.1350 -0.1288 0.098 Uiso 0.327(18) 1 calc PR F -1 Cl1L Cl 0.5035(12) 0.1348(8) -0.0573(8) 0.088(3) Uani 0.327(18) 1 d PDU F -1 Cl2L Cl 0.5135(11) 0.0182(11) -0.1315(6) 0.079(3) Uani 0.327(18) 1 d PDU F -1 C1M C 0.451(3) 0.090(2) -0.129(2) 0.076(5) Uani 0.173(18) 1 d PDU F -2 H1M1 H 0.3864 0.0861 -0.1123 0.091 Uiso 0.173(18) 1 calc PR F -2 H1M2 H 0.4479 0.1241 -0.1797 0.091 Uiso 0.173(18) 1 calc PR F -2 Cl1M Cl 0.497(2) 0.1415(13) -0.0854(19) 0.091(5) Uani 0.173(18) 1 d PDU F -2 Cl2M Cl 0.5201(19) -0.0151(17) -0.1163(14) 0.085(4) Uani 0.173(18) 1 d PDU F -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0233(3) 0.0170(3) 0.0206(3) -0.0064(3) -0.0034(3) -0.0064(3) La1 0.01861(13) 0.01649(13) 0.01985(13) -0.00686(10) -0.00104(10) -0.00578(10) Fe2 0.0294(4) 0.0192(3) 0.0276(4) -0.0083(3) -0.0072(3) -0.0081(3) O1 0.0223(17) 0.024(2) 0.0287(19) 0.0000(16) 0.0039(15) -0.0045(14) O2 0.0254(19) 0.039(2) 0.023(2) -0.0115(17) -0.0013(15) -0.0026(16) N1 0.0245(19) 0.0204(19) 0.0172(19) -0.0061(16) -0.0021(15) -0.0069(16) O11 0.0300(17) 0.0294(18) 0.0297(18) -0.0142(15) 0.0001(14) -0.0131(14) O12 0.0248(16) 0.0224(16) 0.0260(17) -0.0113(14) 0.0040(13) -0.0108(13) O13 0.0334(18) 0.0291(17) 0.0183(16) -0.0083(14) -0.0026(13) -0.0135(14) C105 0.026(2) 0.017(2) 0.028(3) -0.002(2) -0.007(2) -0.0059(19) C101 0.034(2) 0.029(2) 0.036(3) -0.011(2) -0.003(2) -0.017(2) C102 0.083(6) 0.064(5) 0.036(3) 0.003(3) -0.015(3) -0.053(4) C103 0.032(3) 0.044(4) 0.063(5) -0.015(3) -0.010(3) -0.020(2) C104 0.046(4) 0.055(4) 0.064(4) -0.033(4) 0.004(3) -0.031(3) C122 0.046(4) 0.055(4) 0.064(4) -0.033(4) 0.004(3) -0.031(3) C123 0.083(6) 0.064(5) 0.036(3) 0.003(3) -0.015(3) -0.053(4) C124 0.032(3) 0.044(4) 0.063(5) -0.015(3) -0.010(3) -0.020(2) C106 0.021(2) 0.027(2) 0.026(2) -0.007(2) -0.0029(18) -0.0103(19) C107 0.023(2) 0.019(2) 0.020(2) -0.0029(19) -0.0028(18) -0.0057(19) C108 0.024(2) 0.020(2) 0.023(2) -0.0034(19) -0.0021(19) -0.0063(19) C109 0.039(3) 0.039(3) 0.025(3) -0.009(2) 0.002(2) -0.020(2) C110 0.043(3) 0.051(3) 0.021(3) -0.011(2) 0.008(2) -0.019(3) C111 0.047(3) 0.042(3) 0.025(3) -0.018(2) 0.004(2) -0.017(3) C112 0.034(3) 0.023(2) 0.019(2) -0.008(2) -0.004(2) -0.005(2) C113 0.031(3) 0.020(2) 0.027(3) -0.010(2) -0.003(2) -0.003(2) C114 0.069(3) 0.037(3) 0.023(2) -0.011(2) -0.004(2) -0.023(2) O14 0.055(2) 0.0313(18) 0.0303(17) -0.0111(15) -0.0114(15) -0.0191(16) C115 0.055(4) 0.024(4) 0.031(3) -0.010(3) -0.017(3) -0.010(3) C116 0.071(5) 0.044(4) 0.034(3) -0.017(3) -0.011(4) -0.025(3) C117 0.098(6) 0.068(5) 0.060(6) -0.046(5) -0.001(5) -0.017(5) C118 0.079(5) 0.089(8) 0.044(5) -0.020(5) -0.019(5) -0.046(5) C119 0.092(7) 0.076(6) 0.031(5) -0.009(4) -0.024(5) -0.042(5) C125 0.061(5) 0.023(4) 0.031(4) -0.014(4) -0.012(4) -0.010(4) C126 0.074(6) 0.043(5) 0.035(4) -0.022(4) -0.012(4) -0.019(5) C127 0.080(7) 0.061(8) 0.044(6) -0.038(6) -0.005(5) -0.025(6) C128 0.106(11) 0.055(5) 0.047(8) -0.035(6) -0.005(7) -0.037(6) C129 0.071(7) 0.078(7) 0.046(8) -0.018(7) -0.020(6) -0.022(6) N2 0.0169(18) 0.0173(18) 0.0193(19) -0.0061(15) -0.0026(14) -0.0014(15) O21 0.0334(17) 0.0192(16) 0.0213(17) -0.0083(14) -0.0035(13) -0.0050(13) O22 0.0279(16) 0.0155(15) 0.0184(16) -0.0045(13) -0.0057(12) -0.0058(13) O23 0.0268(16) 0.0188(16) 0.0204(16) -0.0057(13) -0.0049(13) -0.0079(13) O24 0.0331(18) 0.0210(17) 0.0314(19) -0.0110(15) -0.0074(14) -0.0055(14) C201 0.045(3) 0.020(2) 0.024(3) -0.010(2) -0.009(2) -0.006(2) C202 0.050(3) 0.044(3) 0.043(3) -0.025(3) -0.007(3) -0.017(3) C203 0.078(4) 0.036(3) 0.029(3) -0.015(2) -0.017(3) -0.010(3) C204 0.049(3) 0.041(3) 0.041(3) -0.026(3) -0.004(3) -0.003(3) C205 0.022(2) 0.028(3) 0.025(3) -0.011(2) -0.0009(19) -0.005(2) C206 0.031(3) 0.023(2) 0.019(2) -0.006(2) -0.0047(19) -0.004(2) C207 0.016(2) 0.023(2) 0.021(2) -0.0076(19) -0.0011(17) -0.0060(18) C208 0.020(2) 0.018(2) 0.025(2) -0.0072(19) -0.0012(18) -0.0024(18) C209 0.041(3) 0.024(3) 0.021(2) -0.007(2) -0.008(2) -0.004(2) C210 0.055(3) 0.025(3) 0.020(3) -0.002(2) -0.006(2) -0.007(2) C211 0.041(3) 0.019(2) 0.028(3) -0.004(2) -0.006(2) -0.006(2) C212 0.026(2) 0.017(2) 0.022(2) -0.0063(19) -0.0011(18) -0.0058(19) C213 0.024(2) 0.020(2) 0.028(3) -0.008(2) -0.0018(19) -0.0074(19) C214 0.050(3) 0.022(3) 0.026(3) -0.007(2) -0.014(2) -0.005(2) C215 0.029(3) 0.021(2) 0.033(3) -0.008(2) -0.009(2) -0.005(2) C216 0.053(3) 0.022(3) 0.042(3) -0.015(2) -0.013(3) -0.004(2) C217 0.112(6) 0.038(4) 0.062(4) -0.033(3) -0.033(4) 0.015(4) C218 0.090(5) 0.034(3) 0.107(6) -0.015(4) -0.012(4) -0.031(4) C219 0.078(4) 0.024(3) 0.053(4) -0.011(3) -0.027(3) 0.006(3) N3 0.028(2) 0.023(2) 0.025(2) -0.0056(17) -0.0081(16) -0.0081(17) O32 0.0210(15) 0.0207(16) 0.0223(16) -0.0053(13) -0.0065(13) -0.0047(13) O33 0.0279(17) 0.0217(17) 0.0395(19) -0.0117(15) -0.0125(14) -0.0055(14) O31 0.0379(18) 0.0166(16) 0.0275(18) -0.0037(14) -0.0122(14) -0.0071(14) C306 0.033(3) 0.020(2) 0.032(3) -0.010(2) -0.011(2) 0.002(2) C305 0.046(3) 0.020(2) 0.027(2) -0.0085(19) -0.009(2) -0.0049(19) C301 0.074(5) 0.020(4) 0.064(5) -0.013(4) -0.033(4) -0.001(4) C302 0.087(11) 0.040(6) 0.094(6) -0.047(6) -0.037(7) 0.013(7) C303 0.095(7) 0.023(6) 0.072(10) 0.009(7) -0.038(7) -0.020(6) C304 0.083(6) 0.019(6) 0.082(9) -0.007(6) -0.039(7) 0.000(5) C321 0.070(5) 0.021(3) 0.064(4) -0.014(4) -0.036(4) 0.001(4) C322 0.105(11) 0.045(7) 0.094(6) -0.050(6) -0.043(7) 0.024(8) C323 0.103(6) 0.029(6) 0.085(10) -0.003(7) -0.059(6) -0.031(5) C324 0.097(8) 0.017(5) 0.087(7) -0.002(6) -0.063(7) -0.008(6) C307 0.022(2) 0.021(2) 0.019(2) -0.0063(19) -0.0017(18) -0.0022(19) C308 0.025(2) 0.022(2) 0.021(2) -0.0051(19) -0.0018(18) -0.0061(19) C309 0.035(3) 0.019(2) 0.039(3) -0.006(2) -0.013(2) 0.000(2) C310 0.034(3) 0.032(3) 0.059(4) -0.011(3) -0.028(3) 0.002(2) C311 0.038(3) 0.027(3) 0.064(4) -0.013(3) -0.025(3) -0.005(2) C312 0.029(3) 0.029(3) 0.034(3) -0.010(2) -0.014(2) -0.006(2) C313 0.033(3) 0.026(3) 0.036(3) -0.009(2) -0.015(2) -0.004(2) C314 0.037(3) 0.028(3) 0.065(4) -0.015(3) -0.025(3) -0.008(2) O34 0.0271(17) 0.0237(17) 0.043(2) -0.0098(15) -0.0074(15) -0.0079(14) C315 0.030(2) 0.034(3) 0.055(3) -0.022(2) -0.009(2) -0.011(2) C316 0.029(3) 0.035(3) 0.089(4) -0.030(3) -0.013(3) -0.009(3) C317 0.047(5) 0.096(7) 0.134(7) -0.063(6) 0.024(4) -0.036(4) C318 0.036(5) 0.035(3) 0.154(8) -0.014(4) -0.016(5) -0.016(3) C319 0.084(6) 0.077(5) 0.100(5) -0.023(4) -0.037(4) -0.048(5) C326 0.038(5) 0.041(6) 0.089(6) -0.026(5) -0.012(6) -0.019(4) C327 0.075(11) 0.071(12) 0.092(9) -0.042(8) -0.015(9) -0.050(9) C328 0.028(10) 0.050(8) 0.097(9) -0.021(7) 0.005(9) -0.022(7) C329 0.036(5) 0.056(9) 0.131(11) -0.016(9) -0.014(8) -0.027(6) Fe3 0.0379(7) 0.0329(9) 0.0519(10) -0.0220(8) -0.0078(7) -0.0026(6) Cl31 0.0688(19) 0.0395(13) 0.054(2) -0.0275(14) 0.0005(15) -0.0135(13) Cl32 0.078(2) 0.0429(15) 0.108(3) -0.0312(15) 0.0247(18) -0.0306(14) Cl33 0.0760(17) 0.0695(17) 0.086(2) -0.0333(15) 0.0357(15) -0.0208(13) Cl34 0.151(3) 0.092(2) 0.142(3) -0.073(2) -0.105(3) 0.038(2) Fe4 0.080(4) 0.058(4) 0.093(5) -0.028(4) 0.043(3) -0.030(3) Cl41 0.109(9) 0.068(6) 0.072(7) -0.031(6) 0.021(6) -0.003(6) Cl42 0.132(9) 0.107(6) 0.074(6) -0.027(5) -0.002(6) -0.094(7) Cl43 0.378(17) 0.122(9) 0.057(4) -0.042(5) 0.072(7) -0.093(11) Cl44 0.062(4) 0.177(12) 0.51(3) -0.229(15) 0.069(8) -0.054(5) Fe5 0.0278(5) 0.0550(7) 0.0264(6) -0.0050(5) -0.0006(4) -0.0059(4) Cl51 0.0406(9) 0.1203(17) 0.0290(8) -0.0204(9) 0.0046(6) -0.0345(10) Cl52 0.0611(10) 0.0504(10) 0.0554(10) -0.0066(8) -0.0058(8) -0.0027(8) Cl53 0.0412(8) 0.0576(11) 0.0513(10) -0.0137(9) -0.0099(7) 0.0054(8) Cl54 0.0382(10) 0.0845(14) 0.0320(10) -0.0135(10) -0.0046(9) -0.0125(10) Fe6 0.050(6) 0.054(7) 0.037(7) -0.006(5) -0.008(6) -0.023(6) Cl61 0.052(11) 0.081(11) 0.032(8) 0.011(9) -0.014(8) -0.006(10) Cl62 0.032(10) 0.071(9) 0.044(12) -0.016(9) -0.008(9) 0.001(8) Cl63 0.047(7) 0.039(11) 0.052(11) -0.020(9) 0.002(7) -0.005(7) Cl64 0.057(14) 0.120(17) 0.024(10) -0.030(11) 0.003(12) -0.022(15) Fe7 0.0382(14) 0.0263(11) 0.0332(12) -0.0031(9) -0.0084(9) -0.0063(9) Cl71 0.037(2) 0.057(3) 0.0500(17) 0.0012(19) -0.0138(14) -0.0186(16) Cl72 0.122(5) 0.0377(13) 0.0557(17) -0.0203(12) -0.005(3) -0.006(2) Cl73 0.057(3) 0.063(3) 0.0327(17) -0.0075(18) -0.0069(17) -0.006(2) Cl74 0.0346(18) 0.040(2) 0.052(3) 0.0003(18) -0.0167(18) -0.0116(15) Fe8 0.041(4) 0.027(3) 0.024(3) -0.004(3) -0.008(3) -0.015(3) Cl81 0.033(5) 0.047(7) 0.082(9) 0.021(6) -0.017(6) -0.019(4) Cl82 0.113(12) 0.050(5) 0.038(4) -0.025(4) 0.004(6) -0.029(6) Cl83 0.072(9) 0.032(6) 0.025(4) -0.009(4) 0.011(5) -0.023(5) Cl84 0.023(4) 0.051(7) 0.026(5) -0.009(5) 0.002(3) -0.013(4) C1D 0.046(4) 0.082(5) 0.082(5) -0.054(4) 0.001(3) -0.016(3) C2D 0.037(3) 0.050(4) 0.050(3) -0.021(3) 0.007(3) -0.010(3) O1D 0.0251(18) 0.039(2) 0.054(2) -0.0158(18) -0.0026(16) -0.0032(16) C3D 0.029(3) 0.054(4) 0.056(4) -0.016(3) -0.003(3) -0.010(3) C4D 0.045(3) 0.059(4) 0.079(5) -0.012(4) -0.010(3) -0.024(3) C1E 0.079(10) 0.056(8) 0.072(9) -0.018(6) -0.008(8) 0.005(10) C2E 0.051(6) 0.049(5) 0.067(6) -0.017(5) 0.000(5) -0.009(5) O1E 0.046(6) 0.049(4) 0.058(6) -0.020(4) 0.009(5) -0.009(4) C3E 0.047(5) 0.055(6) 0.060(5) -0.022(6) 0.006(5) -0.011(5) C4E 0.081(12) 0.088(16) 0.057(9) -0.027(10) 0.020(8) -0.009(12) C1G 0.045(6) 0.042(5) 0.073(6) -0.018(4) 0.000(5) -0.007(5) C2G 0.047(5) 0.047(4) 0.063(6) -0.012(4) -0.002(4) -0.003(4) O1G 0.040(4) 0.046(3) 0.052(4) -0.019(3) 0.004(3) -0.004(3) C3G 0.047(4) 0.044(5) 0.058(4) -0.023(4) 0.007(4) -0.012(4) C4G 0.056(6) 0.068(10) 0.060(6) -0.033(6) 0.009(5) -0.007(6) C1F 0.071(5) 0.116(7) 0.082(5) -0.044(5) 0.006(4) 0.004(5) C2F 0.050(4) 0.063(4) 0.050(4) -0.010(3) 0.007(3) -0.013(3) O1F 0.049(2) 0.044(2) 0.039(2) -0.0041(18) 0.0084(18) -0.0171(18) C3F 0.064(4) 0.051(4) 0.065(4) 0.000(3) 0.012(3) -0.030(3) C4F 0.064(4) 0.061(4) 0.072(5) -0.017(4) 0.016(3) -0.034(3) C1L 0.125(10) 0.061(8) 0.044(8) -0.011(8) 0.015(7) -0.011(8) Cl1L 0.143(7) 0.057(4) 0.061(6) -0.030(4) 0.017(6) -0.010(4) Cl2L 0.139(6) 0.045(6) 0.055(5) -0.010(4) -0.012(4) -0.031(6) C1M 0.115(10) 0.049(9) 0.053(9) -0.008(9) 0.003(9) -0.015(8) Cl1M 0.119(9) 0.060(7) 0.095(12) -0.026(9) 0.003(11) -0.028(6) Cl2M 0.111(8) 0.033(8) 0.097(10) 0.000(8) -0.034(8) -0.011(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic= ) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O21 1.934(3) . ? Fe1 O31 1.939(3) . ? Fe1 O11 1.964(3) . ? Fe1 O12 1.990(3) . ? Fe1 O22 2.028(3) . ? Fe1 O32 2.038(3) . ? Fe1 La1 3.5561(9) . ? La1 O1 2.510(3) . ? La1 O2 2.528(3) . ? La1 O22 2.574(3) . ? La1 O23 2.587(3) . ? La1 O33 2.604(3) . ? La1 O12 2.616(3) . ? La1 O32 2.681(3) . ? La1 N2 2.757(3) . ? La1 O13 2.824(3) . ? La1 N3 2.845(4) . ? La1 N1 2.865(3) . ? Fe2 O24 1.937(3) . ? Fe2 O14 1.948(3) . ? Fe2 O34 1.959(3) . ? Fe2 O13 1.990(3) . ? Fe2 O33 2.003(3) . ? Fe2 O23 2.003(3) . ? N1 C112 1.335(5) . ? N1 C108 1.336(5) . ? O11 C105 1.263(5) . ? O12 C107 1.291(5) . ? O13 C113 1.277(5) . ? C105 C106 1.395(6) . ? C105 C101 1.520(5) . ? C101 C123 1.487(7) . ? C101 C102 1.488(5) . ? C101 C104 1.525(6) . ? C101 C122 1.529(7) . ? C101 C103 1.533(6) . ? C101 C124 1.539(7) . ? C106 C107 1.368(5) . ? C107 C108 1.470(6) . ? C108 C109 1.379(6) . ? C109 C110 1.360(6) . ? C110 C111 1.372(6) . ? C111 C112 1.367(6) . ? C112 C113 1.481(6) . ? C113 C114 1.362(6) . ? C114 C125 1.388(8) . ? C114 C115 1.393(7) . ? O14 C115 1.246(7) . ? O14 C125 1.266(8) . ? C115 C116 1.520(7) . ? C116 C119 1.505(7) . ? C116 C117 1.521(7) . ? C116 C118 1.526(7) . ? C125 C126 1.520(7) . ? C126 C128 1.515(7) . ? C126 C129 1.517(7) . ? C126 C127 1.525(7) . ? N2 C208 1.334(5) . ? N2 C212 1.338(5) . ? O21 C205 1.264(5) . ? O22 C207 1.281(4) . ? O23 C213 1.286(5) . ? O24 C215 1.257(5) . ? C201 C203 1.508(6) . ? C201 C205 1.508(6) . ? C201 C204 1.516(6) . ? C201 C202 1.529(6) . ? C205 C206 1.396(6) . ? C206 C207 1.370(6) . ? C207 C208 1.482(5) . ? C208 C209 1.377(6) . ? C209 C210 1.376(6) . ? C210 C211 1.355(6) . ? C211 C212 1.378(6) . ? C212 C213 1.471(6) . ? C213 C214 1.366(6) . ? C214 C215 1.398(6) . ? C215 C216 1.508(6) . ? C216 C217 1.499(7) . ? C216 C219 1.513(7) . ? C216 C218 1.534(7) . ? N3 C312 1.336(5) . ? N3 C308 1.336(5) . ? O32 C307 1.281(5) . ? O33 C313 1.288(5) . ? O31 C305 1.267(5) . ? C306 C307 1.370(6) . ? C306 C305 1.375(6) . ? C305 C321 1.520(7) . ? C305 C301 1.520(7) . ? C301 C304 1.516(7) . ? C301 C303 1.522(7) . ? C301 C302 1.526(7) . ? C321 C324 1.520(7) . ? C321 C323 1.521(7) . ? C321 C322 1.525(7) . ? C307 C308 1.486(6) . ? C308 C309 1.381(6) . ? C309 C310 1.362(6) . ? C310 C311 1.369(6) . ? C311 C312 1.376(6) . ? C312 C313 1.477(6) . ? C313 C314 1.372(6) . ? C314 C315 1.403(6) . ? O34 C315 1.275(5) . ? C315 C316 1.519(6) . ? C315 C326 1.520(8) . ? C316 C318 1.518(6) . ? C316 C319 1.519(6) . ? C316 C317 1.523(6) . ? C326 C329 1.514(8) . ? C326 C327 1.518(8) . ? C326 C328 1.520(8) . ? Fe3 Cl31 2.154(3) . ? Fe3 Cl33 2.166(3) . ? Fe3 Cl34 2.163(3) . ? Fe3 Cl32 2.167(3) . ? Fe4 Cl44 2.138(7) . ? Fe4 Cl42 2.151(7) . ? Fe4 Cl43 2.172(7) . ? Fe4 Cl41 2.184(7) . ? Fe5 Cl54 2.1678(18) . ? Fe5 Cl52 2.172(2) . ? Fe5 Cl51 2.1744(18) . ? Fe5 Cl53 2.1788(19) . ? Fe6 Cl62 2.165(8) . ? Fe6 Cl64 2.166(8) . ? Fe6 Cl63 2.168(8) . ? Fe6 Cl61 2.169(8) . ? Fe7 Cl73 2.143(3) . ? Fe7 Cl72 2.160(3) . ? Fe7 Cl71 2.181(3) . ? Fe7 Cl74 2.205(3) . ? Fe8 Cl82 2.158(7) . ? Fe8 Cl83 2.160(7) . ? Fe8 Cl81 2.171(7) . ? Fe8 Cl84 2.182(7) . ? C1D C2D 1.490(5) . ? C2D O1D 1.406(5) . ? O1D C3D 1.420(5) . ? C3D C4D 1.492(6) . ? C1E C2E 1.497(8) . ? C2E O1E 1.407(8) . ? O1E C3E 1.407(8) . ? C3E C4E 1.499(8) . ? C1G C2G 1.504(7) . ? C2G O1G 1.413(7) . ? O1G C3G 1.404(6) . ? C3G C4G 1.503(7) . ? C1F C2F 1.484(6) . ? C2F O1F 1.400(5) . ? O1F C3F 1.400(5) . ? C3F C4F 1.472(6) . ? C1L Cl1L 1.754(12) . ? C1L Cl2L 1.767(12) . ? C1M Cl2M 1.750(13) . ? C1M Cl1M 1.756(13) . ? 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 O21 Fe1 O31 86.94(12) . . ? O21 Fe1 O11 88.25(12) . . ? O31 Fe1 O11 88.46(12) . . ? O21 Fe1 O12 157.22(12) . . ? O31 Fe1 O12 114.38(12) . . ? O11 Fe1 O12 84.60(12) . . ? O21 Fe1 O22 84.22(11) . . ? O31 Fe1 O22 156.62(12) . . ? O11 Fe1 O22 112.80(12) . . ? O12 Fe1 O22 78.73(11) . . ? O21 Fe1 O32 114.77(12) . . ? O31 Fe1 O32 85.22(12) . . ? O11 Fe1 O32 155.67(12) . . ? O12 Fe1 O32 76.76(11) . . ? O22 Fe1 O32 78.98(11) . . ? O21 Fe1 La1 125.69(8) . . ? O31 Fe1 La1 129.83(9) . . ? O11 Fe1 La1 124.67(9) . . ? O12 Fe1 La1 46.40(7) . . ? O22 Fe1 La1 45.38(8) . . ? O32 Fe1 La1 48.46(8) . . ? O1 La1 O2 131.34(10) . . ? O1 La1 O22 75.38(10) . . ? O2 La1 O22 80.21(10) . . ? O1 La1 O23 79.81(10) . . ? O2 La1 O23 73.98(10) . . ? O22 La1 O23 115.79(8) . . ? O1 La1 O33 74.96(11) . . ? O2 La1 O33 120.56(10) . . ? O22 La1 O33 150.33(9) . . ? O23 La1 O33 58.41(9) . . ? O1 La1 O12 124.16(10) . . ? O2 La1 O12 72.78(10) . . ? O22 La1 O12 58.82(8) . . ? O23 La1 O12 146.75(9) . . ? O33 La1 O12 143.46(9) . . ? O1 La1 O32 73.91(9) . . ? O2 La1 O32 125.67(10) . . ? O22 La1 O32 58.91(8) . . ? O23 La1 O32 153.67(8) . . ? O33 La1 O32 111.87(9) . . ? O12 La1 O32 56.33(8) . . ? O1 La1 N2 64.96(10) . . ? O2 La1 N2 66.39(10) . . ? O22 La1 N2 57.99(9) . . ? O23 La1 N2 57.82(9) . . ? O33 La1 N2 108.27(9) . . ? O12 La1 N2 108.17(9) . . ? O32 La1 N2 110.47(9) . . ? O1 La1 O13 125.13(10) . . ? O2 La1 O13 70.37(10) . . ? O22 La1 O13 150.58(8) . . ? O23 La1 O13 56.82(8) . . ? O33 La1 O13 54.93(9) . . ? O12 La1 O13 109.95(8) . . ? O32 La1 O13 141.29(8) . . ? N2 La1 O13 108.23(9) . . ? O1 La1 N3 65.50(10) . . ? O2 La1 N3 162.98(10) . . ? O22 La1 N3 110.07(9) . . ? O23 La1 N3 111.29(9) . . ? O33 La1 N3 56.25(9) . . ? O12 La1 N3 100.41(9) . . ? O32 La1 N3 55.83(9) . . ? N2 La1 N3 130.43(10) . . ? O13 La1 N3 98.45(9) . . ? O1 La1 N1 165.03(10) . . ? O2 La1 N1 63.62(10) . . ? O22 La1 N1 111.51(9) . . ? O23 La1 N1 107.42(9) . . ? O33 La1 N1 97.35(9) . . ? O12 La1 N1 55.84(9) . . ? O32 La1 N1 97.85(9) . . ? N2 La1 N1 130.01(9) . . ? O13 La1 N1 54.71(9) . . ? N3 La1 N1 99.54(10) . . ? O1 La1 Fe1 90.92(8) . . ? O2 La1 Fe1 91.69(8) . . ? O22 La1 Fe1 34.12(6) . . ? O23 La1 Fe1 149.67(6) . . ? O33 La1 Fe1 146.50(7) . . ? O12 La1 Fe1 33.43(6) . . ? O32 La1 Fe1 34.68(6) . . ? N2 La1 Fe1 92.05(7) . . ? O13 La1 Fe1 143.32(6) . . ? N3 La1 Fe1 90.27(7) . . ? N1 La1 Fe1 88.78(7) . . ? O24 Fe2 O14 92.48(13) . . ? O24 Fe2 O34 91.09(12) . . ? O14 Fe2 O34 86.85(13) . . ? O24 Fe2 O13 109.10(12) . . ? O14 Fe2 O13 86.85(12) . . ? O34 Fe2 O13 159.08(13) . . ? O24 Fe2 O33 161.28(13) . . ? O14 Fe2 O33 105.41(13) . . ? O34 Fe2 O33 84.54(12) . . ? O13 Fe2 O33 77.95(12) . . ? O24 Fe2 O23 85.51(12) . . ? O14 Fe2 O23 165.88(12) . . ? O34 Fe2 O23 107.14(12) . . ? O13 Fe2 O23 80.63(11) . . ? O33 Fe2 O23 78.46(12) . . ? O24 Fe2 La1 125.19(9) . . ? O14 Fe2 La1 129.23(9) . . ? O34 Fe2 La1 120.57(9) . . ? O13 Fe2 La1 51.73(8) . . ? O33 Fe2 La1 45.39(8) . . ? O23 Fe2 La1 44.90(8) . . ? C112 N1 C108 117.0(4) . . ? C112 N1 La1 122.4(3) . . ? C108 N1 La1 120.5(3) . . ? C105 O11 Fe1 132.0(3) . . ? C107 O12 Fe1 128.7(3) . . ? C107 O12 La1 130.7(2) . . ? Fe1 O12 La1 100.17(10) . . ? C113 O13 Fe2 127.7(3) . . ? C113 O13 La1 120.4(3) . . ? Fe2 O13 La1 94.69(11) . . ? O11 C105 C106 122.5(3) . . ? O11 C105 C101 117.4(4) . . ? C106 C105 C101 120.0(4) . . ? C123 C101 C102 134.8(7) . . ? C123 C101 C105 111.9(6) . . ? C102 C101 C105 110.2(4) . . ? C123 C101 C104 38.5(8) . . ? C102 C101 C104 110.3(5) . . ? C105 C101 C104 109.7(4) . . ? C123 C101 C122 111.5(8) . . ? C102 C101 C122 66.1(7) . . ? C105 C101 C122 111.6(6) . . ? C104 C101 C122 136.7(7) . . ? C123 C101 C103 69.8(8) . . ? C102 C101 C103 111.0(5) . . ? C105 C101 C103 108.8(4) . . ? C104 C101 C103 106.7(4) . . ? C122 C101 C103 47.4(7) . . ? C123 C101 C124 111.5(8) . . ? C102 C101 C124 40.8(7) . . ? C105 C101 C124 104.1(6) . . ? C104 C101 C124 75.4(7) . . ? C122 C101 C124 105.8(8) . . ? C103 C101 C124 143.6(7) . . ? C107 C106 C105 123.3(4) . . ? O12 C107 C106 124.5(4) . . ? O12 C107 C108 114.0(3) . . ? C106 C107 C108 121.5(4) . . ? N1 C108 C109 123.0(4) . . ? N1 C108 C107 114.9(4) . . ? C109 C108 C107 122.1(4) . . ? C110 C109 C108 118.7(4) . . ? C109 C110 C111 119.1(4) . . ? C112 C111 C110 118.9(4) . . ? N1 C112 C111 123.0(4) . . ? N1 C112 C113 114.2(4) . . ? C111 C112 C113 122.8(4) . . ? O13 C113 C114 124.6(4) . . ? O13 C113 C112 114.7(4) . . ? C114 C113 C112 120.6(4) . . ? C113 C114 C125 124.0(5) . . ? C113 C114 C115 124.8(5) . . ? C125 C114 C115 10.5(12) . . ? C115 O14 C125 11.6(13) . . ? C115 O14 Fe2 131.3(3) . . ? C125 O14 Fe2 131.4(4) . . ? O14 C115 C114 122.6(5) . . ? O14 C115 C116 113.4(5) . . ? C114 C115 C116 123.6(5) . . ? C119 C116 C115 110.1(6) . . ? C119 C116 C117 112.1(7) . . ? C115 C116 C117 105.7(6) . . ? C119 C116 C118 108.8(6) . . ? C115 C116 C118 111.8(6) . . ? C117 C116 C118 108.4(7) . . ? O14 C125 C114 121.4(6) . . ? O14 C125 C126 119.9(6) . . ? C114 C125 C126 117.1(6) . . ? C128 C126 C129 111.3(8) . . ? C128 C126 C125 107.7(7) . . ? C129 C126 C125 107.5(8) . . ? C128 C126 C127 109.3(8) . . ? C129 C126 C127 107.8(8) . . ? C125 C126 C127 113.3(7) . . ? C208 N2 C212 117.7(3) . . ? C208 N2 La1 121.0(3) . . ? C212 N2 La1 121.1(3) . . ? C205 O21 Fe1 132.6(3) . . ? C207 O22 Fe1 129.8(3) . . ? C207 O22 La1 128.8(2) . . ? Fe1 O22 La1 100.50(10) . . ? C213 O23 Fe2 128.4(3) . . ? C213 O23 La1 128.6(2) . . ? Fe2 O23 La1 101.97(11) . . ? C215 O24 Fe2 132.5(3) . . ? C203 C201 C205 113.4(4) . . ? C203 C201 C204 109.4(4) . . ? C205 C201 C204 108.3(4) . . ? C203 C201 C202 109.4(4) . . ? C205 C201 C202 106.1(4) . . ? C204 C201 C202 110.1(4) . . ? O21 C205 C206 122.5(4) . . ? O21 C205 C201 114.8(4) . . ? C206 C205 C201 122.7(4) . . ? C207 C206 C205 123.3(4) . . ? O22 C207 C206 124.0(4) . . ? O22 C207 C208 115.7(4) . . ? C206 C207 C208 120.4(4) . . ? N2 C208 C209 122.4(4) . . ? N2 C208 C207 114.4(4) . . ? C209 C208 C207 123.2(4) . . ? C210 C209 C208 118.7(4) . . ? C211 C210 C209 119.6(4) . . ? C210 C211 C212 118.6(4) . . ? N2 C212 C211 122.9(4) . . ? N2 C212 C213 114.8(4) . . ? C211 C212 C213 122.3(4) . . ? O23 C213 C214 124.5(4) . . ? O23 C213 C212 114.5(4) . . ? C214 C213 C212 120.9(4) . . ? C213 C214 C215 123.7(4) . . ? O24 C215 C214 122.4(4) . . ? O24 C215 C216 116.7(4) . . ? C214 C215 C216 120.9(4) . . ? C217 C216 C215 110.0(4) . . ? C217 C216 C219 109.2(5) . . ? C215 C216 C219 112.8(4) . . ? C217 C216 C218 109.9(5) . . ? C215 C216 C218 104.8(4) . . ? C219 C216 C218 110.0(5) . . ? C312 N3 C308 117.2(4) . . ? C312 N3 La1 120.7(3) . . ? C308 N3 La1 122.0(3) . . ? C307 O32 Fe1 128.2(3) . . ? C307 O32 La1 128.8(2) . . ? Fe1 O32 La1 96.86(10) . . ? C313 O33 Fe2 127.0(3) . . ? C313 O33 La1 131.3(3) . . ? Fe2 O33 La1 101.40(11) . . ? C305 O31 Fe1 133.8(3) . . ? C307 C306 C305 123.8(4) . . ? O31 C305 C306 123.0(4) . . ? O31 C305 C321 116.2(5) . . ? C306 C305 C321 120.7(5) . . ? O31 C305 C301 114.4(5) . . ? C306 C305 C301 122.7(6) . . ? C321 C305 C301 3.1(9) . . ? C304 C301 C305 112.6(8) . . ? C304 C301 C303 110.5(8) . . ? C305 C301 C303 108.3(8) . . ? C304 C301 C302 109.7(8) . . ? C305 C301 C302 106.1(8) . . ? C303 C301 C302 109.4(8) . . ? C324 C321 C305 112.3(8) . . ? C324 C321 C323 108.7(8) . . ? C305 C321 C323 108.4(8) . . ? C324 C321 C322 111.4(8) . . ? C305 C321 C322 105.9(7) . . ? C323 C321 C322 110.1(8) . . ? O32 C307 C306 125.0(4) . . ? O32 C307 C308 115.0(4) . . ? C306 C307 C308 120.0(4) . . ? N3 C308 C309 122.6(4) . . ? N3 C308 C307 114.5(4) . . ? C309 C308 C307 122.9(4) . . ? C310 C309 C308 119.6(4) . . ? C309 C310 C311 118.1(4) . . ? C310 C311 C312 119.7(4) . . ? N3 C312 C311 122.7(4) . . ? N3 C312 C313 114.8(4) . . ? C311 C312 C313 122.6(4) . . ? O33 C313 C314 124.0(4) . . ? O33 C313 C312 113.7(4) . . ? C314 C313 C312 122.3(4) . . ? C313 C314 C315 122.9(4) . . ? C315 O34 Fe2 128.3(3) . . ? O34 C315 C314 123.0(4) . . ? O34 C315 C316 116.7(4) . . ? C314 C315 C316 120.2(4) . . ? O34 C315 C326 114.5(6) . . ? C314 C315 C326 121.8(6) . . ? C316 C315 C326 11.3(7) . . ? C318 C316 C319 110.6(6) . . ? C318 C316 C315 109.3(5) . . ? C319 C316 C315 108.5(5) . . ? C318 C316 C317 109.4(6) . . ? C319 C316 C317 108.8(6) . . ? C315 C316 C317 110.2(5) . . ? C329 C326 C327 110.5(10) . . ? C329 C326 C315 108.9(9) . . ? C327 C326 C315 108.8(8) . . ? C329 C326 C328 111.0(10) . . ? C327 C326 C328 109.6(10) . . ? C315 C326 C328 107.9(9) . . ? Cl31 Fe3 Cl33 109.18(16) . . ? Cl31 Fe3 Cl34 109.59(17) . . ? Cl33 Fe3 Cl34 106.11(16) . . ? Cl31 Fe3 Cl32 110.93(19) . . ? Cl33 Fe3 Cl32 109.15(16) . . ? Cl34 Fe3 Cl32 111.7(2) . . ? Cl44 Fe4 Cl42 112.4(5) . . ? Cl44 Fe4 Cl43 110.6(5) . . ? Cl42 Fe4 Cl43 111.9(5) . . ? Cl44 Fe4 Cl41 106.6(5) . . ? Cl42 Fe4 Cl41 107.2(5) . . ? Cl43 Fe4 Cl41 107.8(5) . . ? Cl54 Fe5 Cl52 109.69(9) . . ? Cl54 Fe5 Cl51 108.35(9) . . ? Cl52 Fe5 Cl51 110.12(10) . . ? Cl54 Fe5 Cl53 111.14(9) . . ? Cl52 Fe5 Cl53 109.27(9) . . ? Cl51 Fe5 Cl53 108.24(8) . . ? Cl62 Fe6 Cl64 111.1(8) . . ? Cl62 Fe6 Cl63 110.0(6) . . ? Cl64 Fe6 Cl63 108.9(7) . . ? Cl62 Fe6 Cl61 108.8(7) . . ? Cl64 Fe6 Cl61 108.8(7) . . ? Cl63 Fe6 Cl61 109.2(7) . . ? Cl73 Fe7 Cl72 108.9(2) . . ? Cl73 Fe7 Cl71 112.7(3) . . ? Cl72 Fe7 Cl71 112.5(2) . . ? Cl73 Fe7 Cl74 107.7(2) . . ? Cl72 Fe7 Cl74 109.1(2) . . ? Cl71 Fe7 Cl74 105.8(2) . . ? Cl82 Fe8 Cl83 108.7(6) . . ? Cl82 Fe8 Cl81 110.0(5) . . ? Cl83 Fe8 Cl81 110.7(7) . . ? Cl82 Fe8 Cl84 110.9(6) . . ? Cl83 Fe8 Cl84 108.8(6) . . ? Cl81 Fe8 Cl84 107.8(6) . . ? O1D C2D C1D 108.8(4) . . ? C2D O1D C3D 112.2(4) . . ? O1D C3D C4D 109.0(4) . . ? O1E C2E C1E 110.4(10) . . ? C2E O1E C3E 113.7(11) . . ? O1E C3E C4E 112.5(12) . . ? O1G C2G C1G 108.2(7) . . ? C3G O1G C2G 112.5(7) . . ? O1G C3G C4G 115.0(8) . . ? O1F C2F C1F 112.4(5) . . ? C2F O1F C3F 114.2(4) . . ? O1F C3F C4F 110.6(4) . . ? Cl1L C1L Cl2L 109.5(10) . . ? Cl2M C1M Cl1M 110.5(13) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.629 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.087 #======END OF DATA FOR La-4a # 4.5 RESULTS FOR 7 data_rs9911 _database_code_CSD 152457 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C114 H192 Co8 N6 O53' _chemical_formula_weight 2966.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.001(6) _cell_length_b 31.448(7) _cell_length_c 20.135(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.78(2) _cell_angle_gamma 90.00 _cell_volume 15990(8) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 45 _cell_measurement_theta_min 4.15 _cell_measurement_theta_max 14.95 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6232 _exptl_absorpt_coefficient_mu 0.884 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.4594 _exptl_absorpt_correction_T_max 0.6251 _exptl_absorpt_process_details ; North A C T, Phillips D C, Mathews F S, Acta Cryst. A24 (1968), 351-359. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 'Siemens P4' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 13.5 _diffrn_reflns_number 15674 _diffrn_reflns_av_R_equivalents 0.1401 _diffrn_reflns_av_sigmaI/netI 0.3571 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14065 _reflns_number_gt 3781 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCAnS 2.20 (Siemens An. X-Ray Instr.,1996)' _computing_cell_refinement 'XSCAnS 2.20 (Siemens An. X-Ray Instr.,1996)' _computing_data_reduction 'XSCAnS 2.20 (Siemens An. X-Ray Instr.,1996)' _computing_structure_solution 'SHELXTL 5.1 (Bruker AXS, 1998)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS, 1998)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS, 1998)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS, 1998)' _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. The compound crystallizes with x solvent water ; _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^)+(0.1000P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14065 _refine_ls_number_parameters 736 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3730 _refine_ls_R_factor_gt 0.1489 _refine_ls_wR_factor_ref 0.3788 _refine_ls_wR_factor_gt 0.2955 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 0.464 _refine_ls_shift/su_mean 0.014 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 Co1 Co -0.04868(10) 0.22171(9) 0.34590(13) 0.0699(8) Uani 1 1 d . . . Co2 Co -0.08158(10) 0.20321(8) 0.15371(12) 0.0642(8) Uani 1 1 d . . . Co3 Co 0.03515(9) 0.18084(8) 0.50001(11) 0.0627(8) Uani 1 1 d . . . Co4 Co -0.00458(11) 0.11996(9) 0.14882(15) 0.0861(10) Uani 1 1 d . . . N1 N -0.1477(5) 0.1654(4) 0.1500(7) 0.055(4) Uani 1 1 d . . . N2 N -0.0324(6) 0.2838(5) 0.3483(9) 0.078(5) Uani 1 1 d . . . N3 N -0.0743(6) 0.0964(5) 0.3351(8) 0.068(4) Uani 1 1 d . . . O1 O -0.1015(5) 0.1836(4) 0.2839(6) 0.082(4) Uani 1 1 d . . . O2 O -0.1118(5) 0.2389(5) 0.3843(7) 0.091(5) Uani 1 1 d . . . O3 O -0.0844(5) 0.1640(4) 0.0643(5) 0.064(3) Uani 1 1 d . . . O4 O -0.0708(5) 0.1346(4) -0.0626(6) 0.072(4) Uani 1 1 d . . . O5 O -0.0623(5) 0.2460(4) 0.2291(6) 0.079(4) Uani 1 1 d . . . O6 O -0.1223(6) 0.2462(4) 0.0956(7) 0.081(5) Uani 1 1 d . . . O7 O 0.0079(4) 0.2327(4) 0.4414(6) 0.066(3) Uani 1 1 d . . . O8 O 0.0808(5) 0.2216(4) 0.5657(7) 0.078(4) Uani 1 1 d . . . O9 O -0.0213(5) 0.1425(4) 0.4342(6) 0.082(4) Uani 1 1 d . . . O10 O -0.0204(5) 0.1888(4) 0.5569(5) 0.073(4) Uani 1 1 d . . . O11 O -0.0497(4) 0.1090(4) 0.2146(5) 0.066(3) Uani 1 1 d . . . O12 O -0.0363(5) 0.0668(4) 0.1013(6) 0.082(4) Uani 1 1 d . . . O13 O -0.0059(4) 0.1808(4) 0.1772(5) 0.068(3) Uani 1 1 d . . . C1 C -0.1651(6) 0.1411(5) 0.0944(8) 0.048(4) Uani 1 1 d . . . C2 C -0.2096(7) 0.1171(6) 0.0862(8) 0.066(5) Uani 1 1 d . . . H2A H -0.2221 0.1012 0.0467 0.079 Uiso 1 1 calc R . . C3 C -0.2356(7) 0.1169(7) 0.1381(10) 0.079(6) Uani 1 1 d . . . H3B H -0.2640 0.0985 0.1350 0.095 Uiso 1 1 calc R . . C4 C -0.2224(7) 0.1410(7) 0.1905(9) 0.078(7) Uani 1 1 d . . . H4A H -0.2424 0.1426 0.2231 0.094 Uiso 1 1 calc R . . C5 C -0.1773(7) 0.1643(6) 0.1959(8) 0.071(6) Uani 1 1 d . . . C6 C -0.1522(7) 0.1885(7) 0.2606(9) 0.075(6) Uani 1 1 d . . . C7 C -0.1803(8) 0.2139(8) 0.2955(11) 0.120(9) Uani 1 1 d . . . H7A H -0.2169 0.2143 0.2790 0.144 Uiso 1 1 calc R . . C8 C -0.1593(11) 0.2392(9) 0.3540(11) 0.111(9) Uani 1 1 d . . . C9 C -0.1990(12) 0.2693(15) 0.3781(18) 0.196(19) Uani 1 1 d . . . C10 C -0.2343(14) 0.2339(15) 0.4101(19) 0.33(4) Uani 1 1 d . . . H10A H -0.2608 0.2484 0.4275 0.491 Uiso 1 1 calc R . . H10B H -0.2113 0.2185 0.4466 0.491 Uiso 1 1 calc R . . H10C H -0.2510 0.2145 0.3749 0.491 Uiso 1 1 calc R . . C11 C -0.1734(16) 0.2877(19) 0.439(2) 0.50(6) Uani 1 1 d . . . H11A H -0.1971 0.3070 0.4540 0.757 Uiso 1 1 calc R . . H11B H -0.1429 0.3030 0.4332 0.757 Uiso 1 1 calc R . . H11C H -0.1625 0.2660 0.4732 0.757 Uiso 1 1 calc R . . C12 C -0.2335(16) 0.2966(16) 0.318(2) 0.33(3) Uani 1 1 d . . . H12A H -0.2565 0.3150 0.3355 0.501 Uiso 1 1 calc R . . H12B H -0.2543 0.2780 0.2841 0.501 Uiso 1 1 calc R . . H12C H -0.2106 0.3134 0.2973 0.501 Uiso 1 1 calc R . . C13 C -0.1279(7) 0.1420(6) 0.0432(9) 0.057(5) Uani 1 1 d . . . C14 C -0.1448(6) 0.1229(5) -0.0187(9) 0.062(5) Uani 1 1 d . . . H14A H -0.1785 0.1111 -0.0281 0.074 Uiso 1 1 calc R . . C15 C -0.1155(8) 0.1191(6) -0.0721(9) 0.071(6) Uani 1 1 d . . . C16 C -0.1428(8) 0.1000(7) -0.1414(9) 0.073(6) Uani 1 1 d . . . C17 C -0.1696(12) 0.1384(9) -0.1832(10) 0.182(16) Uani 1 1 d . . . H17A H -0.1880 0.1291 -0.2279 0.273 Uiso 1 1 calc R . . H17B H -0.1432 0.1590 -0.1872 0.273 Uiso 1 1 calc R . . H17C H -0.1944 0.1511 -0.1605 0.273 Uiso 1 1 calc R . . C18 C -0.1034(12) 0.0780(13) -0.1689(13) 0.28(3) Uani 1 1 d . . . H18A H -0.0895 0.0544 -0.1398 0.421 Uiso 1 1 calc R . . H18B H -0.0752 0.0972 -0.1712 0.421 Uiso 1 1 calc R . . H18C H -0.1195 0.0677 -0.2140 0.421 Uiso 1 1 calc R . . C19 C -0.1768(13) 0.0641(10) -0.1354(12) 0.203(18) Uani 1 1 d . . . H19A H -0.1559 0.0419 -0.1092 0.304 Uiso 1 1 calc R . . H19B H -0.1933 0.0536 -0.1801 0.304 Uiso 1 1 calc R . . H19C H -0.2035 0.0731 -0.1128 0.304 Uiso 1 1 calc R . . C20 C -0.0081(9) 0.3055(9) 0.4076(12) 0.098(8) Uani 1 1 d . . . C21 C -0.0023(10) 0.3464(9) 0.4161(13) 0.123(10) Uani 1 1 d . . . H21A H 0.0153 0.3581 0.4577 0.147 Uiso 1 1 calc R . . C22 C -0.0242(11) 0.3722(8) 0.3582(16) 0.139(11) Uani 1 1 d . . . H22A H -0.0235 0.4016 0.3636 0.167 Uiso 1 1 calc R . . C23 C -0.0456(10) 0.3559(8) 0.2965(14) 0.129(11) Uani 1 1 d . . . H23A H -0.0575 0.3733 0.2586 0.154 Uiso 1 1 calc R . . C24 C -0.0492(8) 0.3144(8) 0.2919(10) 0.081(6) Uani 1 1 d . . . C25 C -0.0744(8) 0.2846(7) 0.2269(11) 0.088(7) Uani 1 1 d . . . C26 C -0.1067(8) 0.3053(6) 0.1681(11) 0.084(7) Uani 1 1 d . . . H26A H -0.1123 0.3344 0.1700 0.101 Uiso 1 1 calc R . . C27 C -0.1314(9) 0.2822(9) 0.1046(9) 0.086(7) Uani 1 1 d . . . C28 C -0.1753(11) 0.3101(8) 0.0596(11) 0.105(8) Uani 1 1 d . . . C29 C -0.2209(11) 0.3102(13) 0.0916(13) 0.25(3) Uani 1 1 d . . . H29A H -0.2130 0.3279 0.1316 0.375 Uiso 1 1 calc R . . H29B H -0.2278 0.2818 0.1043 0.375 Uiso 1 1 calc R . . H29C H -0.2516 0.3211 0.0596 0.375 Uiso 1 1 calc R . . C30 C -0.1492(14) 0.3536(8) 0.0458(14) 0.22(2) Uani 1 1 d . . . H30A H -0.1394 0.3696 0.0875 0.327 Uiso 1 1 calc R . . H30B H -0.1741 0.3697 0.0123 0.327 Uiso 1 1 calc R . . H30C H -0.1182 0.3480 0.0291 0.327 Uiso 1 1 calc R . . C31 C -0.1933(9) 0.2825(8) -0.0056(11) 0.151(12) Uani 1 1 d . . . H31A H -0.2090 0.2567 0.0056 0.226 Uiso 1 1 calc R . . H31B H -0.1632 0.2758 -0.0235 0.226 Uiso 1 1 calc R . . H31C H -0.2188 0.2980 -0.0393 0.226 Uiso 1 1 calc R . . C32 C 0.0137(7) 0.2708(7) 0.4614(12) 0.076(6) Uani 1 1 d . . . C33 C 0.0388(8) 0.2860(7) 0.5204(10) 0.088(7) Uani 1 1 d . . . H33A H 0.0363 0.3149 0.5290 0.106 Uiso 1 1 calc R . . C34 C 0.0707(9) 0.2591(8) 0.5732(10) 0.086(7) Uani 1 1 d . . . C35 C 0.0954(11) 0.2787(9) 0.6504(12) 0.115(9) Uani 1 1 d . . . C36 C 0.1421(12) 0.2494(9) 0.6848(13) 0.193(17) Uani 1 1 d . . . H36A H 0.1580 0.2598 0.7298 0.290 Uiso 1 1 calc R . . H36B H 0.1681 0.2492 0.6580 0.290 Uiso 1 1 calc R . . H36C H 0.1293 0.2210 0.6879 0.290 Uiso 1 1 calc R . . C37 C 0.0524(11) 0.2751(11) 0.6850(12) 0.187(16) Uani 1 1 d . . . H37A H 0.0635 0.2865 0.7304 0.281 Uiso 1 1 calc R . . H37B H 0.0430 0.2457 0.6875 0.281 Uiso 1 1 calc R . . H37C H 0.0222 0.2906 0.6600 0.281 Uiso 1 1 calc R . . C38 C 0.1106(11) 0.3264(9) 0.6402(12) 0.166(13) Uani 1 1 d . . . H38A H 0.1249 0.3392 0.6840 0.249 Uiso 1 1 calc R . . H38B H 0.0796 0.3417 0.6170 0.249 Uiso 1 1 calc R . . H38C H 0.1366 0.3273 0.6134 0.249 Uiso 1 1 calc R . . C39 C -0.0998(8) 0.0739(5) 0.2823(9) 0.066(6) Uani 1 1 d . . . C40 C -0.1481(6) 0.0568(5) 0.2794(8) 0.059(5) Uani 1 1 d . . . H40A H -0.1662 0.0431 0.2399 0.071 Uiso 1 1 calc R . . C41 C -0.1703(8) 0.0596(6) 0.3346(10) 0.076(6) Uani 1 1 d . . . H41A H -0.2016 0.0453 0.3349 0.091 Uiso 1 1 calc R . . C42 C -0.1453(7) 0.0840(6) 0.3893(9) 0.072(6) Uani 1 1 d . . . H42A H -0.1609 0.0883 0.4258 0.086 Uiso 1 1 calc R . . C43 C -0.0955(7) 0.1025(6) 0.3900(9) 0.064(5) Uani 1 1 d . . . C44 C -0.0664(6) 0.1298(6) 0.4439(9) 0.058(5) Uani 1 1 d . . . C45 C -0.0863(7) 0.1396(6) 0.4999(8) 0.067(5) Uani 1 1 d . . . H45A H -0.1179 0.1267 0.5023 0.081 Uiso 1 1 calc R . . C46 C -0.0638(7) 0.1666(7) 0.5521(9) 0.071(6) Uani 1 1 d . . . C47 C -0.0887(9) 0.1787(11) 0.6137(12) 0.132(11) Uani 1 1 d . . . C48 C -0.1444(11) 0.1532(10) 0.5991(12) 0.187(15) Uani 1 1 d . . . H48A H -0.1628 0.1602 0.6337 0.281 Uiso 1 1 calc R . . H48B H -0.1376 0.1231 0.6000 0.281 Uiso 1 1 calc R . . H48C H -0.1657 0.1610 0.5550 0.281 Uiso 1 1 calc R . . C49 C -0.0501(10) 0.1604(12) 0.6785(10) 0.215(19) Uani 1 1 d . . . H49A H -0.0628 0.1673 0.7182 0.322 Uiso 1 1 calc R . . H49B H -0.0156 0.1725 0.6829 0.322 Uiso 1 1 calc R . . H49C H -0.0481 0.1300 0.6744 0.322 Uiso 1 1 calc R . . C50 C -0.0929(13) 0.2265(8) 0.6169(19) 0.25(2) Uani 1 1 d . . . H50A H -0.1092 0.2342 0.6532 0.368 Uiso 1 1 calc R . . H50B H -0.1140 0.2369 0.5742 0.368 Uiso 1 1 calc R . . H50C H -0.0581 0.2388 0.6253 0.368 Uiso 1 1 calc R . . C51 C -0.0751(7) 0.0749(5) 0.2223(7) 0.050(4) Uani 1 1 d . . . C52 C -0.0853(7) 0.0420(6) 0.1780(9) 0.081(6) Uani 1 1 d . . . H52A H -0.1070 0.0202 0.1868 0.097 Uiso 1 1 calc R . . C53 C -0.0641(8) 0.0386(7) 0.1166(9) 0.080(6) Uani 1 1 d . . . C54 C -0.0790(14) 0.0009(11) 0.0718(17) 0.149(13) Uani 1 1 d . . . C55 C -0.0704(13) 0.0065(12) 0.0050(13) 0.24(2) Uani 1 1 d . . . H55A H -0.0770 -0.0198 -0.0198 0.353 Uiso 1 1 calc R . . H55B H -0.0344 0.0151 0.0086 0.353 Uiso 1 1 calc R . . H55C H -0.0939 0.0281 -0.0188 0.353 Uiso 1 1 calc R . . C56 C -0.046(2) -0.0328(10) 0.1017(17) 0.26(3) Uani 1 1 d . . . H56A H -0.0535 -0.0574 0.0727 0.389 Uiso 1 1 calc R . . H56B H -0.0524 -0.0393 0.1456 0.389 Uiso 1 1 calc R . . H56C H -0.0097 -0.0247 0.1071 0.389 Uiso 1 1 calc R . . C57 C -0.130(2) -0.017(2) 0.071(3) 0.62(4) Uani 1 1 d . . . H57A H -0.1354 -0.0422 0.0433 0.930 Uiso 1 1 calc R . . H57B H -0.1572 0.0033 0.0532 0.930 Uiso 1 1 calc R . . H57C H -0.1314 -0.0245 0.1171 0.930 Uiso 1 1 calc R . . O21 O -0.0230(13) 0.4172(9) -0.0483(15) 0.300 Uiso 1 1 d . . . O22 O -0.2790(12) 0.0357(9) 0.0026(15) 0.300 Uiso 1 1 d . . . O23 O 0.2450(13) -0.0065(10) 0.3309(15) 0.300 Uiso 1 1 d . . . O24 O -0.2989(12) 0.1328(9) 0.3462(15) 0.300 Uiso 1 1 d . . . O25 O 0.2457(12) 0.0922(9) 0.0230(15) 0.300 Uiso 1 1 d . . . O26 O 0.0821(12) 0.3494(10) -0.1107(15) 0.300 Uiso 1 1 d . . . O27 O -0.349(2) 0.0428(19) 0.058(3) 0.300 Uiso 0.50 1 d P . . O28 O 0.1451(13) 0.4300(9) 0.3018(15) 0.300 Uiso 1 1 d . . . O29 O 0.0482(12) 0.4546(9) 0.3089(15) 0.300 Uiso 1 1 d . . . O30 O 0.0565(12) 0.4869(10) 0.1630(15) 0.300 Uiso 1 1 d . . . O31 O -0.0137(12) 0.4720(9) 0.0510(15) 0.300 Uiso 1 1 d . . . O32 O -0.3198(12) 0.0776(10) 0.2434(15) 0.300 Uiso 1 1 d . . . O33 O -0.2686(12) -0.0079(10) -0.0796(15) 0.300 Uiso 1 1 d . . . O34 O 0.0270(12) 0.3949(9) -0.2719(16) 0.300 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0576(16) 0.083(2) 0.0719(18) -0.0093(15) 0.0208(14) 0.0151(15) Co2 0.0649(17) 0.0761(18) 0.0552(15) -0.0106(14) 0.0215(13) -0.0151(15) Co3 0.0523(15) 0.094(2) 0.0443(13) -0.0103(14) 0.0172(12) 0.0089(15) Co4 0.0772(19) 0.093(2) 0.111(2) 0.0310(18) 0.0681(18) 0.0152(17) N1 0.038(8) 0.065(10) 0.060(9) 0.011(8) 0.012(7) -0.001(7) N2 0.068(11) 0.082(13) 0.084(12) -0.028(11) 0.017(10) 0.019(10) N3 0.063(10) 0.069(11) 0.088(12) 0.013(9) 0.051(9) -0.003(8) O1 0.082(10) 0.093(10) 0.071(8) -0.013(8) 0.017(8) 0.037(8) O2 0.055(8) 0.146(14) 0.078(10) -0.033(9) 0.026(8) 0.014(10) O3 0.056(8) 0.095(10) 0.044(7) -0.004(6) 0.018(6) -0.023(7) O4 0.082(10) 0.079(9) 0.063(8) 0.000(7) 0.034(8) -0.001(8) O5 0.100(11) 0.046(8) 0.078(9) 0.012(7) -0.008(8) 0.018(8) O6 0.099(11) 0.060(9) 0.077(10) -0.015(8) 0.006(8) -0.012(9) O7 0.058(8) 0.074(9) 0.066(8) -0.038(7) 0.016(6) -0.005(7) O8 0.078(9) 0.079(10) 0.085(10) -0.023(8) 0.034(8) 0.004(8) O9 0.060(8) 0.140(12) 0.056(8) -0.028(8) 0.029(7) -0.016(8) O10 0.071(9) 0.107(11) 0.048(7) -0.016(7) 0.026(7) 0.018(8) O11 0.067(8) 0.083(9) 0.058(8) 0.005(7) 0.033(7) -0.005(7) O12 0.097(11) 0.079(10) 0.087(10) 0.010(8) 0.058(9) 0.007(8) O13 0.061(8) 0.103(10) 0.044(7) -0.006(7) 0.017(6) -0.018(7) C1 0.038(10) 0.050(11) 0.059(11) -0.001(9) 0.018(9) -0.001(9) C2 0.073(13) 0.073(13) 0.043(10) 0.004(10) -0.002(10) -0.002(12) C3 0.050(12) 0.115(18) 0.077(14) 0.025(13) 0.026(12) -0.019(12) C4 0.033(11) 0.15(2) 0.045(11) -0.001(13) 0.005(9) -0.015(12) C5 0.065(13) 0.115(17) 0.031(10) -0.004(10) 0.009(10) 0.017(12) C6 0.050(12) 0.120(18) 0.066(13) 0.005(12) 0.034(11) 0.005(12) C7 0.051(13) 0.21(3) 0.107(18) -0.065(19) 0.028(13) 0.002(16) C8 0.13(2) 0.16(2) 0.056(14) -0.032(16) 0.056(16) 0.01(2) C9 0.10(2) 0.35(5) 0.14(3) -0.11(3) 0.02(2) 0.08(3) C10 0.17(4) 0.60(9) 0.26(5) -0.21(6) 0.16(4) -0.17(5) C11 0.24(5) 0.85(13) 0.33(6) -0.46(8) -0.12(4) 0.28(7) C12 0.19(4) 0.57(9) 0.23(5) -0.15(6) 0.04(4) 0.17(5) C13 0.056(12) 0.065(13) 0.052(11) 0.001(10) 0.016(10) 0.020(10) C14 0.041(10) 0.084(13) 0.068(12) -0.011(11) 0.030(9) -0.012(10) C15 0.073(14) 0.072(14) 0.073(14) 0.008(11) 0.028(12) -0.011(12) C16 0.071(14) 0.109(17) 0.033(10) -0.023(11) 0.001(10) 0.002(13) C17 0.24(4) 0.23(3) 0.044(14) -0.026(18) -0.030(18) 0.12(3) C18 0.15(3) 0.55(7) 0.13(3) -0.24(4) 0.00(2) -0.04(4) C19 0.26(4) 0.25(4) 0.10(2) -0.08(2) 0.05(3) -0.15(4) C20 0.083(17) 0.11(2) 0.102(19) -0.053(18) 0.022(15) 0.004(16) C21 0.12(2) 0.10(2) 0.12(2) -0.048(18) -0.039(18) 0.022(18) C22 0.15(3) 0.072(19) 0.16(3) -0.06(2) -0.02(2) 0.020(18) C23 0.14(2) 0.060(17) 0.15(3) -0.029(17) -0.03(2) 0.027(16) C24 0.064(14) 0.091(18) 0.081(15) -0.011(14) 0.001(12) 0.011(13) C25 0.078(16) 0.070(17) 0.109(18) -0.008(15) 0.007(14) -0.014(13) C26 0.098(16) 0.048(13) 0.100(17) 0.034(12) 0.014(14) 0.051(12) C27 0.081(16) 0.13(2) 0.039(12) 0.014(15) 0.006(11) -0.029(17) C28 0.14(2) 0.09(2) 0.055(14) -0.002(13) -0.028(15) 0.023(17) C29 0.11(2) 0.51(7) 0.11(2) -0.06(3) -0.013(19) 0.17(4) C30 0.30(5) 0.10(2) 0.16(3) 0.02(2) -0.14(3) 0.05(3) C31 0.11(2) 0.24(3) 0.097(19) 0.07(2) 0.020(17) 0.10(2) C32 0.040(11) 0.081(17) 0.095(17) -0.018(15) -0.010(11) 0.004(12) C33 0.093(16) 0.112(19) 0.052(13) -0.009(13) 0.001(12) 0.042(15) C34 0.078(16) 0.13(2) 0.064(14) -0.038(15) 0.042(13) -0.041(16) C35 0.13(2) 0.11(2) 0.097(19) -0.075(17) 0.005(17) -0.004(18) C36 0.24(4) 0.15(3) 0.13(2) -0.04(2) -0.08(2) 0.10(3) C37 0.16(3) 0.32(4) 0.077(18) -0.10(2) 0.013(19) 0.01(3) C38 0.17(3) 0.22(4) 0.093(19) -0.08(2) 0.002(19) -0.06(3) C39 0.091(15) 0.054(12) 0.064(12) -0.031(10) 0.042(11) -0.047(11) C40 0.047(11) 0.082(13) 0.044(10) 0.011(9) 0.003(9) -0.016(10) C41 0.076(14) 0.084(15) 0.081(14) 0.001(12) 0.044(12) -0.021(12) C42 0.075(14) 0.103(16) 0.050(12) 0.002(11) 0.040(11) -0.010(12) C43 0.059(12) 0.089(15) 0.052(11) -0.001(10) 0.030(10) 0.011(11) C44 0.043(10) 0.076(14) 0.055(11) 0.006(10) 0.013(9) 0.010(10) C45 0.067(12) 0.098(15) 0.053(11) -0.014(11) 0.047(10) -0.005(11) C46 0.062(13) 0.117(18) 0.047(11) -0.006(11) 0.037(10) 0.002(12) C47 0.073(16) 0.25(3) 0.097(18) 0.01(2) 0.058(15) -0.02(2) C48 0.16(3) 0.31(4) 0.12(2) -0.09(3) 0.09(2) -0.08(3) C49 0.14(3) 0.47(6) 0.044(14) 0.03(2) 0.046(17) 0.01(3) C50 0.28(5) 0.08(2) 0.46(6) -0.11(3) 0.26(5) -0.01(3) C51 0.067(12) 0.056(12) 0.035(9) -0.015(8) 0.027(9) -0.020(10) C52 0.080(15) 0.094(16) 0.077(14) -0.004(12) 0.032(12) -0.025(12) C53 0.091(16) 0.103(18) 0.057(13) -0.019(12) 0.036(12) -0.008(14) C54 0.19(3) 0.15(3) 0.13(3) -0.07(2) 0.09(3) 0.01(3) C55 0.20(4) 0.41(6) 0.08(2) -0.09(3) -0.01(2) 0.06(4) C56 0.51(9) 0.13(3) 0.16(4) -0.05(3) 0.12(5) -0.02(4) C57 0.47(5) 0.79(8) 0.80(9) -0.74(7) 0.54(5) -0.512 _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 Co1 N2 1.996(16) . ? Co1 O1 2.018(14) . ? Co1 O2 2.046(12) . ? Co1 O13 2.049(11) 2 ? Co1 O7 2.153(11) . ? Co2 O6 1.929(15) . ? Co2 O5 2.001(13) . ? Co2 O13 2.037(11) . ? Co2 N1 2.077(13) . ? Co2 O3 2.169(11) . ? Co3 O4 2.002(13) 2 ? Co3 O8 2.014(14) . ? Co3 O7 2.039(13) . ? Co3 O10 2.061(11) . ? Co3 O3 2.094(10) 2 ? Co3 O9 2.106(12) . ? Co4 O11 1.996(10) . ? Co4 O13 2.000(12) . ? Co4 O12 2.003(14) . ? Co4 O9 2.070(11) 2 ? Co4 N3 2.132(14) 2 ? N1 C5 1.335(19) . ? N1 C1 1.342(18) . ? N2 C20 1.39(2) . ? N2 C24 1.47(2) . ? N3 C39 1.318(19) . ? N3 C43 1.360(18) . ? N3 Co4 2.132(14) 2 ? O1 C6 1.30(2) . ? O2 C8 1.24(3) . ? O3 C13 1.307(19) . ? O3 Co3 2.094(10) 2 ? O4 C15 1.232(19) . ? O4 Co3 2.002(13) 2 ? O5 C25 1.25(2) . ? O6 C27 1.18(3) . ? O7 C32 1.26(2) . ? O8 C34 1.22(2) . ? O9 C44 1.299(18) . ? O9 Co4 2.070(10) 2 ? O10 C46 1.31(2) . ? O11 C51 1.288(17) . ? O12 C53 1.23(2) . ? O13 Co1 2.049(11) 2 ? C1 C2 1.36(2) . ? C1 C13 1.57(2) . ? C2 C3 1.37(2) . ? C3 C4 1.28(2) . ? C4 C5 1.36(2) . ? C5 C6 1.52(2) . ? C6 C7 1.38(2) . ? C7 C8 1.42(3) . ? C8 C9 1.56(3) . ? C9 C11 1.38(4) . ? C9 C12 1.58(5) . ? C9 C10 1.66(5) . ? C13 C14 1.36(2) . ? C14 C15 1.46(2) . ? C15 C16 1.53(2) . ? C16 C18 1.45(3) . ? C16 C19 1.46(3) . ? C16 C17 1.54(3) . ? C20 C21 1.30(3) . ? C20 C32 1.55(3) . ? C21 C22 1.42(3) . ? C22 C23 1.34(3) . ? C23 C24 1.31(3) . ? C24 C25 1.62(3) . ? C25 C26 1.43(3) . ? C26 C27 1.48(3) . ? C27 C28 1.55(3) . ? C28 C29 1.48(4) . ? C28 C31 1.55(3) . ? C28 C30 1.58(4) . ? C32 C33 1.30(2) . ? C33 C34 1.46(3) . ? C34 C35 1.65(3) . ? C35 C37 1.46(3) . ? C35 C36 1.55(3) . ? C35 C38 1.58(3) . ? C39 C40 1.35(2) . ? C39 C51 1.498(19) . ? C40 C41 1.37(2) . ? C41 C42 1.37(2) . ? C42 C43 1.42(2) . ? C43 C44 1.45(2) . ? C44 C45 1.38(2) . ? C45 C46 1.37(2) . ? C46 C47 1.57(2) . ? C47 C50 1.51(4) . ? C47 C49 1.56(3) . ? C47 C48 1.62(3) . ? C51 C52 1.35(2) . ? C52 C53 1.47(2) . ? C53 C54 1.48(3) . ? C54 C56 1.40(4) . ? C54 C55 1.43(4) . ? C54 C57 1.44(5) . ? 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 Co1 O1 134.9(6) . . ? N2 Co1 O2 85.3(6) . . ? O1 Co1 O2 84.3(5) . . ? N2 Co1 O13 117.8(5) . 2 ? O1 Co1 O13 83.8(5) . 2 ? O2 Co1 O13 155.8(6) . 2 ? N2 Co1 O7 74.0(6) . . ? O1 Co1 O7 150.3(5) . . ? O2 Co1 O7 93.4(5) . . ? O13 Co1 O7 86.6(4) 2 . ? O6 Co2 O5 89.5(5) . . ? O6 Co2 O13 138.0(5) . . ? O5 Co2 O13 90.2(5) . . ? O6 Co2 N1 92.8(6) . . ? O5 Co2 N1 117.9(6) . . ? O13 Co2 N1 123.8(5) . . ? O6 Co2 O3 89.4(5) . . ? O5 Co2 O3 164.8(5) . . ? O13 Co2 O3 80.5(4) . . ? N1 Co2 O3 77.3(5) . . ? O4 Co3 O8 86.3(5) 2 . ? O4 Co3 O7 172.1(5) 2 . ? O8 Co3 O7 86.6(5) . . ? O4 Co3 O10 91.1(5) 2 . ? O8 Co3 O10 86.5(5) . . ? O7 Co3 O10 91.8(5) . . ? O4 Co3 O3 86.9(5) 2 2 ? O8 Co3 O3 102.4(5) . 2 ? O7 Co3 O3 91.4(4) . 2 ? O10 Co3 O3 170.7(5) . 2 ? O4 Co3 O9 97.5(5) 2 . ? O8 Co3 O9 172.4(5) . . ? O7 Co3 O9 90.0(5) . . ? O10 Co3 O9 86.8(5) . . ? O3 Co3 O9 84.4(4) 2 . ? O11 Co4 O13 85.6(5) . . ? O11 Co4 O12 86.2(5) . . ? O13 Co4 O12 154.4(5) . . ? O11 Co4 O9 161.8(5) . 2 ? O13 Co4 O9 86.2(5) . 2 ? O12 Co4 O9 94.4(5) . 2 ? O11 Co4 N3 122.4(5) . 2 ? O13 Co4 N3 111.7(5) . 2 ? O12 Co4 N3 93.2(5) . 2 ? O9 Co4 N3 75.8(5) 2 2 ? C5 N1 C1 115.2(14) . . ? C5 N1 Co2 126.7(13) . . ? C1 N1 Co2 117.9(10) . . ? C20 N2 C24 109.4(18) . . ? C20 N2 Co1 123.5(17) . . ? C24 N2 Co1 126.7(14) . . ? C39 N3 C43 120.5(15) . . ? C39 N3 Co4 126.2(11) . 2 ? C43 N3 Co4 112.9(13) . 2 ? C6 O1 Co1 129.4(13) . . ? C8 O2 Co1 127.7(13) . . ? C13 O3 Co3 122.8(10) . 2 ? C13 O3 Co2 115.2(10) . . ? Co3 O3 Co2 117.7(5) 2 . ? C15 O4 Co3 131.5(12) . 2 ? C25 O5 Co2 127.5(13) . . ? C27 O6 Co2 132.9(15) . . ? C32 O7 Co3 125.3(13) . . ? C32 O7 Co1 116.2(13) . . ? Co3 O7 Co1 117.2(6) . . ? C34 O8 Co3 125.7(15) . . ? C44 O9 Co4 119.7(11) . 2 ? C44 O9 Co3 126.9(11) . . ? Co4 O9 Co3 113.1(5) 2 . ? C46 O10 Co3 126.9(11) . . ? C51 O11 Co4 128.5(10) . . ? C53 O12 Co4 133.0(12) . . ? Co4 O13 Co2 110.2(5) . . ? Co4 O13 Co1 118.4(5) . 2 ? Co2 O13 Co1 114.4(6) . 2 ? N1 C1 C2 121.7(15) . . ? N1 C1 C13 113.5(14) . . ? C2 C1 C13 124.7(16) . . ? C1 C2 C3 118.0(17) . . ? C4 C3 C2 122.8(19) . . ? C3 C4 C5 116.1(18) . . ? N1 C5 C4 125.8(17) . . ? N1 C5 C6 112.4(17) . . ? C4 C5 C6 121.5(16) . . ? O1 C6 C7 120.1(19) . . ? O1 C6 C5 116.2(16) . . ? C7 C6 C5 123.7(18) . . ? C6 C7 C8 127(2) . . ? O2 C8 C7 123(2) . . ? O2 C8 C9 121(2) . . ? C7 C8 C9 116(2) . . ? C11 C9 C8 109(3) . . ? C11 C9 C12 121(5) . . ? C8 C9 C12 113(3) . . ? C11 C9 C10 97(4) . . ? C8 C9 C10 101(3) . . ? C12 C9 C10 113(3) . . ? O3 C13 C14 126.7(15) . . ? O3 C13 C1 114.6(14) . . ? C14 C13 C1 118.5(16) . . ? C13 C14 C15 126.8(16) . . ? O4 C15 C14 119.3(18) . . ? O4 C15 C16 120.8(17) . . ? C14 C15 C16 119.6(17) . . ? C18 C16 C19 99(2) . . ? C18 C16 C15 108.7(17) . . ? C19 C16 C15 112.8(17) . . ? C18 C16 C17 116(2) . . ? C19 C16 C17 117(2) . . ? C15 C16 C17 104.0(17) . . ? C21 C20 N2 128(3) . . ? C21 C20 C32 126(2) . . ? N2 C20 C32 106(2) . . ? C20 C21 C22 116(2) . . ? C23 C22 C21 123(2) . . ? C24 C23 C22 117(3) . . ? C23 C24 N2 126(2) . . ? C23 C24 C25 130(2) . . ? N2 C24 C25 103.6(18) . . ? O5 C25 C26 124.2(19) . . ? O5 C25 C24 119(2) . . ? C26 C25 C24 116.8(19) . . ? C25 C26 C27 122.7(18) . . ? O6 C27 C26 123(2) . . ? O6 C27 C28 127(2) . . ? C26 C27 C28 110(2) . . ? C29 C28 C27 108(2) . . ? C29 C28 C31 105(2) . . ? C27 C28 C31 102.2(18) . . ? C29 C28 C30 120(3) . . ? C27 C28 C30 108(2) . . ? C31 C28 C30 113(2) . . ? O7 C32 C33 129(2) . . ? O7 C32 C20 117(2) . . ? C33 C32 C20 114(2) . . ? C32 C33 C34 122(2) . . ? O8 C34 C33 125(2) . . ? O8 C34 C35 115(2) . . ? C33 C34 C35 120(2) . . ? C37 C35 C36 110(3) . . ? C37 C35 C38 112(2) . . ? C36 C35 C38 115(3) . . ? C37 C35 C34 104(2) . . ? C36 C35 C34 106.6(19) . . ? C38 C35 C34 107(2) . . ? N3 C39 C40 122.1(15) . . ? N3 C39 C51 114.1(14) . . ? C40 C39 C51 123.0(16) . . ? C39 C40 C41 120.3(17) . . ? C40 C41 C42 118.3(17) . . ? C41 C42 C43 119.7(15) . . ? N3 C43 C42 118.7(17) . . ? N3 C43 C44 116.9(16) . . ? C42 C43 C44 124.3(15) . . ? O9 C44 C45 125.5(17) . . ? O9 C44 C43 113.5(15) . . ? C45 C44 C43 121.0(16) . . ? C46 C45 C44 126.3(17) . . ? O10 C46 C45 126.0(14) . . ? O10 C46 C47 108.8(18) . . ? C45 C46 C47 125.0(18) . . ? C50 C47 C49 112(3) . . ? C50 C47 C46 109(2) . . ? C49 C47 C46 105(2) . . ? C50 C47 C48 116(3) . . ? C49 C47 C48 110(2) . . ? C46 C47 C48 105(2) . . ? O11 C51 C52 125.7(14) . . ? O11 C51 C39 116.5(14) . . ? C52 C51 C39 117.5(15) . . ? C51 C52 C53 123.8(17) . . ? O12 C53 C52 121.2(19) . . ? O12 C53 C54 121(2) . . ? C52 C53 C54 118(2) . . ? C56 C54 C55 106(3) . . ? C56 C54 C57 100(5) . . ? C55 C54 C57 113(4) . . ? C56 C54 C53 107(3) . . ? C55 C54 C53 113(3) . . ? C57 C54 C53 115(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.637 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.125 #======END OF ALL DATA