Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_gobal _journal_coden_Cambridge 186 loop_ _publ_author_name 'van Staveren, Dave R.' 'Thomas Weyhermuller' 'Nils Metzler-Nolte' _publ_contact_author_name 'Prof Nils Metzler-Nolte' _publ_contact_author_address ; Pharmazeutisch-Chemisches Institut University of Heidelberg Im Neuenheimer Feld 364 Heidelberg 69120 GERMANY ; _publ_contact_author_email 'NILS.METZLER-NOLTE@URZ.UNI-HEIDELBERG.DE' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Organometallic beta-turn mimetics. A Structural and Spectroscopic Study of Inter-strand Hydrogen Bonding in Ferrocene and Cobaltocenium Conjugates of Amino Acids and Dipeptides ; data_3b _database_code_CSD 180589 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[C21 H21 Co N O3]+, (C24 H20 B)-' _chemical_formula_analytical ? _chemical_formula_sum 'C45 H41 B Co N O3' _chemical_formula_weight 713.53 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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 'Orthorhombic' _symmetry_space_group_name_H-M 'P2(1)2(1)2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 13.992(2) _cell_length_b 39.148(7) _cell_length_c 13.195(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7228(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1826 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent parallelepiped' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method ? _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 0.518 _exptl_absorpt_correction_type 'not measured' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\w-scan, 0.5 deg./frame' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35109 _diffrn_reflns_av_R_equivalents 0.1995 _diffrn_reflns_av_sigmaI/netI 0.2114 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 24.00 _reflns_number_total 11307 _reflns_number_observed 5612 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'DENZO, Nonius Collect Software' _computing_cell_refinement 'DENZO, Nonius Collect Software' _computing_data_reduction 'DENZO, Nonius Collect Software' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 24 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0313P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 11283 _refine_ls_number_parameters 919 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1650 _refine_ls_R_factor_obs 0.0713 _refine_ls_wR_factor_all 0.1480 _refine_ls_wR_factor_obs 0.1206 _refine_ls_goodness_of_fit_all 0.922 _refine_ls_goodness_of_fit_obs 1.121 _refine_ls_restrained_S_all 0.931 _refine_ls_restrained_S_obs 1.121 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.74642(9) -0.10211(2) 0.83491(7) 0.0290(3) Uani 1 d . . N11 N 0.8687(4) -0.1891(2) 0.7629(5) 0.040(2) Uani 1 d . . H11 H 0.8355(4) -0.1870(2) 0.7067(5) 0.049 Uiso 1 calc R . O11 O 0.9392(4) -0.1626(2) 0.8976(4) 0.051(2) Uani 1 d . . O13 O 0.9326(4) -0.2342(2) 0.6224(4) 0.055(2) Uani 1 d . . O14 O 0.9845(4) -0.2706(2) 0.7421(4) 0.053(2) Uani 1 d . . C1 C 0.8594(5) -0.1277(2) 0.7762(5) 0.029(2) Uani 1 d . . C2 C 0.8883(6) -0.0959(2) 0.8169(6) 0.038(2) Uani 1 d . . H2 H 0.9332(6) -0.0928(2) 0.8701(6) 0.046 Uiso 1 calc R . C3 C 0.8398(6) -0.0697(2) 0.7662(6) 0.043(2) Uani 1 d . . H3 H 0.8465(6) -0.0459(2) 0.7784(6) 0.051 Uiso 1 calc R . C4 C 0.7785(5) -0.0852(2) 0.6926(5) 0.035(2) Uani 1 d . . H4 H 0.7364(5) -0.0735(2) 0.6479(5) 0.042 Uiso 1 calc R . C5 C 0.7916(5) -0.1208(2) 0.6982(5) 0.039(2) Uani 1 d . . H5 H 0.7607(5) -0.1374(2) 0.6571(5) 0.047 Uiso 1 calc R . C6 C 0.6356(6) -0.1311(2) 0.8827(6) 0.045(2) Uani 1 d . . H6 H 0.6141(6) -0.1516(2) 0.8516(6) 0.054 Uiso 1 calc R . C7 C 0.6037(6) -0.0982(2) 0.8621(6) 0.039(2) Uani 1 d . . H7 H 0.5552(6) -0.0924(2) 0.8148(6) 0.047 Uiso 1 calc R . C8 C 0.6545(5) -0.0751(2) 0.9220(6) 0.045(3) Uani 1 d . . H8 H 0.6474(5) -0.0509(2) 0.9217(6) 0.054 Uiso 1 calc R . C9 C 0.7180(5) -0.0939(3) 0.9827(5) 0.043(3) Uani 1 d . . H9 H 0.7609(5) -0.0845(3) 1.0311(5) 0.052 Uiso 1 calc R . C10 C 0.7078(5) -0.1282(3) 0.9605(6) 0.043(2) Uani 1 d . . H10 H 0.7420(5) -0.1465(3) 0.9909(6) 0.052 Uiso 1 calc R . C11 C 0.8920(5) -0.1616(2) 0.8177(6) 0.037(2) Uani 1 d . . C12 C 0.8993(6) -0.2223(2) 0.7978(6) 0.043(2) Uani 1 d . . H12 H 0.9484(6) -0.2197(2) 0.8523(6) 0.052 Uiso 1 calc R . C13 C 0.9412(6) -0.2426(2) 0.7091(7) 0.042(2) Uani 1 d . . C14 C 1.0261(5) -0.2936(2) 0.6672(6) 0.053(2) Uani 1 d . . H14A H 1.0555(5) -0.3131(2) 0.7017(6) 0.080 Uiso 1 calc R . H14B H 1.0749(5) -0.2813(2) 0.6281(6) 0.080 Uiso 1 calc R . H14C H 0.9760(5) -0.3017(2) 0.6213(6) 0.080 Uiso 1 calc R . C15 C 0.8147(6) -0.2434(2) 0.8374(7) 0.065(3) Uani 1 d . . H15A H 0.7671(6) -0.2459(2) 0.7824(7) 0.078 Uiso 1 calc R . H15B H 0.8378(6) -0.2666(2) 0.8550(7) 0.078 Uiso 1 calc R . C16 C 0.7664(7) -0.2284(2) 0.9281(7) 0.057(3) Uani 1 d . . C17 C 0.6647(7) -0.2266(3) 0.9274(8) 0.079(4) Uani 1 d . . H17 H 0.6311(7) -0.2338(3) 0.8686(8) 0.095 Uiso 1 calc R . C18 C 0.6126(8) -0.2146(3) 1.0109(8) 0.077(4) Uani 1 d . . H18 H 0.5449(8) -0.2128(3) 1.0088(8) 0.092 Uiso 1 calc R . C19 C 0.6638(9) -0.2055(3) 1.0963(9) 0.088(4) Uani 1 d . . H19 H 0.6301(9) -0.1981(3) 1.1548(9) 0.106 Uiso 1 calc R . C20 C 0.7603(10) -0.2067(3) 1.0992(8) 0.097(4) Uani 1 d . . H20 H 0.7934(10) -0.1993(3) 1.1580(8) 0.116 Uiso 1 calc R . C21 C 0.8125(8) -0.2193(3) 1.0140(7) 0.075(3) Uani 1 d . . H21 H 0.8801(8) -0.2212(3) 1.0177(7) 0.090 Uiso 1 calc R . Co2 Co 0.75296(9) -0.41415(2) 0.66186(7) 0.0293(3) Uani 1 d . . N32 N 0.7363(5) -0.3232(2) 0.5325(4) 0.044(2) Uani 1 d . . H32 H 0.7165(5) -0.3348(2) 0.4793(4) 0.053 Uiso 1 calc R . O32 O 0.8170(4) -0.3229(2) 0.6800(4) 0.057(2) Uani 1 d . . O34 O 0.6265(5) -0.2542(2) 0.6633(6) 0.076(2) Uani 1 d . . O35 O 0.5884(4) -0.3102(2) 0.6526(5) 0.052(2) Uani 1 d . . C22 C 0.8163(5) -0.3745(2) 0.5891(5) 0.029(2) Uani 1 d . . C23 C 0.7828(5) -0.3986(2) 0.5179(5) 0.033(2) Uani 1 d . . H23 H 0.7379(5) -0.3942(2) 0.4655(5) 0.039 Uiso 1 calc R . C24 C 0.8262(6) -0.4299(2) 0.5369(6) 0.042(2) Uani 1 d . . H24 H 0.8156(6) -0.4505(2) 0.5006(6) 0.051 Uiso 1 calc R . C25 C 0.8888(6) -0.4256(3) 0.6196(6) 0.056(3) Uani 1 d . . H25 H 0.9274(6) -0.4430(3) 0.6485(6) 0.067 Uiso 1 calc R . C26 C 0.8850(5) -0.3917(3) 0.6525(6) 0.045(3) Uani 1 d . . H26 H 0.9209(5) -0.3819(3) 0.7062(6) 0.054 Uiso 1 calc R . C27 C 0.6488(6) -0.3964(2) 0.7530(6) 0.045(2) Uani 1 d . . H27 H 0.6345(6) -0.3730(2) 0.7651(6) 0.055 Uiso 1 calc R . C28 C 0.7103(5) -0.4155(3) 0.8080(6) 0.046(3) Uani 1 d . . H28 H 0.7459(5) -0.4078(3) 0.8650(6) 0.056 Uiso 1 calc R . C29 C 0.7128(6) -0.4486(3) 0.7671(7) 0.058(3) Uani 1 d . . H29 H 0.7505(6) -0.4672(3) 0.7904(7) 0.069 Uiso 1 calc R . C30 C 0.6484(8) -0.4489(3) 0.6840(7) 0.068(3) Uani 1 d . . H30 H 0.6341(8) -0.4679(3) 0.6416(7) 0.082 Uiso 1 calc R . C31 C 0.6100(6) -0.4161(3) 0.6765(7) 0.057(3) Uani 1 d . . H31 H 0.5650(6) -0.4086(3) 0.6273(7) 0.069 Uiso 1 calc R . C32 C 0.7898(6) -0.3385(2) 0.6042(6) 0.041(2) Uani 1 d . . C33 C 0.7116(6) -0.2877(2) 0.5434(6) 0.053(3) Uani 1 d . . H33 H 0.7703(6) -0.2748(2) 0.5637(6) 0.063 Uiso 1 calc R . C34 C 0.6351(8) -0.2822(3) 0.6246(8) 0.066(3) Uani 1 d . . C35 C 0.5177(5) -0.3050(3) 0.7335(6) 0.062(3) Uani 1 d . . H35A H 0.4867(5) -0.3268(3) 0.7494(6) 0.093 Uiso 1 calc R . H35B H 0.4694(5) -0.2885(3) 0.7108(6) 0.093 Uiso 1 calc R . H35C H 0.5498(5) -0.2962(3) 0.7941(6) 0.093 Uiso 1 calc R . C36 C 0.6743(7) -0.2728(3) 0.4470(6) 0.069(3) Uani 1 d . . H36A H 0.6606(7) -0.2482(3) 0.4572(6) 0.083 Uiso 1 calc R . H36B H 0.6137(7) -0.2843(3) 0.4286(6) 0.083 Uiso 1 calc R . C37 C 0.7458(9) -0.2768(2) 0.3603(6) 0.058(2) Uani 1 d . . C38 C 0.7117(7) -0.2837(2) 0.2637(7) 0.060(3) Uani 1 d . . H38 H 0.6446(7) -0.2853(2) 0.2543(7) 0.072 Uiso 1 calc R . C39 C 0.7695(8) -0.2884(2) 0.1814(7) 0.067(3) Uani 1 d . . H39 H 0.7432(8) -0.2934(2) 0.1167(7) 0.080 Uiso 1 calc R . C40 C 0.8679(8) -0.2857(3) 0.1946(7) 0.071(3) Uani 1 d . . H40 H 0.9092(8) -0.2888(3) 0.1382(7) 0.085 Uiso 1 calc R . C41 C 0.9062(7) -0.2787(2) 0.2886(8) 0.068(3) Uani 1 d . . H41 H 0.9735(7) -0.2770(2) 0.2968(8) 0.081 Uiso 1 calc R . C42 C 0.8458(7) -0.2739(2) 0.3717(7) 0.058(3) Uani 1 d . . H42 H 0.8722(7) -0.2688(2) 0.4363(7) 0.070 Uiso 1 calc R . B1 B 0.7546(7) 0.0923(2) 0.8223(5) 0.022(2) Uani 1 d . . C51 C 0.6552(5) 0.0939(2) 0.7531(6) 0.025(2) Uani 1 d . . C52 C 0.6104(5) 0.0643(2) 0.7179(5) 0.029(2) Uani 1 d . . H52 H 0.6331(5) 0.0426(2) 0.7393(5) 0.035 Uiso 1 calc R . C53 C 0.5331(5) 0.0662(2) 0.6522(6) 0.033(2) Uani 1 d . . H53 H 0.5042(5) 0.0456(2) 0.6295(6) 0.040 Uiso 1 calc R . C54 C 0.4968(5) 0.0969(3) 0.6186(5) 0.039(3) Uani 1 d . . H54 H 0.4439(5) 0.0977(3) 0.5735(5) 0.047 Uiso 1 calc R . C55 C 0.5409(5) 0.1271(2) 0.6534(6) 0.034(2) Uani 1 d . . H55 H 0.5166(5) 0.1488(2) 0.6338(6) 0.041 Uiso 1 calc R . C56 C 0.6196(6) 0.1250(2) 0.7160(6) 0.036(3) Uani 1 d . . H56 H 0.6511(6) 0.1455(2) 0.7349(6) 0.043 Uiso 1 calc R . C61 C 0.7556(6) 0.1226(2) 0.9093(4) 0.025(2) Uani 1 d . . C62 C 0.6756(5) 0.1342(2) 0.9595(6) 0.028(2) Uani 1 d . . H62 H 0.6147(5) 0.1259(2) 0.9392(6) 0.034 Uiso 1 calc R . C63 C 0.6803(6) 0.1577(2) 1.0391(6) 0.036(2) Uani 1 d . . H63 H 0.6232(6) 0.1651(2) 1.0714(6) 0.044 Uiso 1 calc R . C64 C 0.7677(5) 0.1704(2) 1.0712(5) 0.034(2) Uani 1 d . . H64 H 0.7707(5) 0.1865(2) 1.1252(5) 0.041 Uiso 1 calc R . C65 C 0.8498(5) 0.1596(2) 1.0241(6) 0.033(2) Uani 1 d . . H65 H 0.9102(5) 0.1680(2) 1.0458(6) 0.040 Uiso 1 calc R . C66 C 0.8446(6) 0.1365(2) 0.9450(5) 0.028(2) Uani 1 d . . H66 H 0.9021(6) 0.1296(2) 0.9129(5) 0.034 Uiso 1 calc R . C71 C 0.7608(6) 0.0569(2) 0.8871(5) 0.026(2) Uani 1 d . . C72 C 0.6779(6) 0.0436(2) 0.9370(5) 0.029(2) Uani 1 d . . H72 H 0.6179(6) 0.0544(2) 0.9266(5) 0.034 Uiso 1 calc R . C73 C 0.6826(7) 0.0152(2) 1.0001(6) 0.039(2) Uani 1 d . . H73 H 0.6259(7) 0.0069(2) 1.0311(6) 0.047 Uiso 1 calc R . C74 C 0.7687(6) -0.0011(2) 1.0184(5) 0.038(2) Uani 1 d . . H74 H 0.7719(6) -0.0205(2) 1.0616(5) 0.046 Uiso 1 calc R . C75 C 0.8497(6) 0.0116(2) 0.9723(6) 0.042(3) Uani 1 d . . H75 H 0.9095(6) 0.0008(2) 0.9843(6) 0.051 Uiso 1 calc R . C76 C 0.8455(6) 0.0397(2) 0.9090(6) 0.032(2) Uani 1 d . . H76 H 0.9031(6) 0.0477(2) 0.8791(6) 0.039 Uiso 1 calc R . C81 C 0.8378(5) 0.0970(2) 0.7390(5) 0.026(2) Uani 1 d . . C82 C 0.8780(5) 0.0690(2) 0.6859(5) 0.024(2) Uani 1 d . . H82 H 0.8583(5) 0.0465(2) 0.7035(5) 0.029 Uiso 1 calc R . C83 C 0.9445(5) 0.0730(2) 0.6095(6) 0.029(2) Uani 1 d . . H83 H 0.9684(5) 0.0536(2) 0.5747(6) 0.035 Uiso 1 calc R . C84 C 0.9762(5) 0.1049(3) 0.5837(6) 0.034(2) Uani 1 d . . H84 H 1.0234(5) 0.1074(3) 0.5325(6) 0.041 Uiso 1 calc R . C85 C 0.9409(5) 0.1334(2) 0.6307(5) 0.031(2) Uani 1 d . . H85 H 0.9615(5) 0.1556(2) 0.6114(5) 0.037 Uiso 1 calc R . C86 C 0.8716(5) 0.1288(2) 0.7101(6) 0.029(2) Uani 1 d . . H86 H 0.8480(5) 0.1484(2) 0.7442(6) 0.035 Uiso 1 calc R . B2 B 1.2493(7) 0.0880(2) 0.3294(6) 0.026(2) Uani 1 d . . C91 C 1.2476(7) 0.0578(2) 0.4148(4) 0.028(2) Uani 1 d . . C92 C 1.3308(6) 0.0436(2) 0.4557(6) 0.038(3) Uani 1 d . . H92 H 1.3907(6) 0.0512(2) 0.4302(6) 0.046 Uiso 1 calc R . C93 C 1.3303(6) 0.0193(2) 0.5312(6) 0.031(2) Uani 1 d . . H93 H 1.3893(6) 0.0110(2) 0.5568(6) 0.038 Uiso 1 calc R . C94 C 1.2470(7) 0.0069(2) 0.5696(5) 0.042(2) Uani 1 d . . H94 H 1.2474(7) -0.0104(2) 0.6200(5) 0.051 Uiso 1 calc R . C95 C 1.1605(6) 0.0203(2) 0.5331(6) 0.037(3) Uani 1 d . . H95 H 1.1014(6) 0.0127(2) 0.5603(6) 0.044 Uiso 1 calc R . C96 C 1.1621(5) 0.0448(2) 0.4569(6) 0.026(2) Uani 1 d . . H96 H 1.1029(5) 0.0531(2) 0.4318(6) 0.031 Uiso 1 calc R . C101 C 1.3448(5) 0.0863(2) 0.2554(5) 0.028(2) Uani 1 d . . C102 C 1.3812(6) 0.1163(2) 0.2132(5) 0.031(2) Uani 1 d . . H102 H 1.3540(6) 0.1377(2) 0.2312(5) 0.037 Uiso 1 calc R . C103 C 1.4577(5) 0.1151(2) 0.1444(6) 0.031(2) Uani 1 d . . H103 H 1.4812(5) 0.1356(2) 0.1151(6) 0.038 Uiso 1 calc R . C104 C 1.4985(6) 0.0844(3) 0.1196(6) 0.047(3) Uani 1 d . . H104 H 1.5514(6) 0.0838(3) 0.0745(6) 0.056 Uiso 1 calc R . C105 C 1.4633(6) 0.0546(3) 0.1592(7) 0.043(3) Uani 1 d . . H105 H 1.4919(6) 0.0334(3) 0.1418(7) 0.052 Uiso 1 calc R . C106 C 1.3856(6) 0.0555(3) 0.2252(6) 0.036(3) Uani 1 d . . H106 H 1.3599(6) 0.0346(3) 0.2500(6) 0.043 Uiso 1 calc R . C111 C 1.2457(7) 0.1241(2) 0.3941(5) 0.031(2) Uani 1 d . . C112 C 1.3285(6) 0.1383(2) 0.4388(5) 0.030(2) Uani 1 d . . H112 H 1.3881(6) 0.1273(2) 0.4277(5) 0.036 Uiso 1 calc R . C113 C 1.3267(6) 0.1673(2) 0.4974(5) 0.030(2) Uani 1 d . . H113 H 1.3841(6) 0.1754(2) 0.5276(5) 0.037 Uiso 1 calc R . C114 C 1.2424(6) 0.1850(2) 0.5131(5) 0.034(2) Uani 1 d . . H114 H 1.2420(6) 0.2056(2) 0.5511(5) 0.041 Uiso 1 calc R . C115 C 1.1590(6) 0.1723(2) 0.4728(6) 0.034(2) Uani 1 d . . H115 H 1.1001(6) 0.1837(2) 0.4847(6) 0.041 Uiso 1 calc R . C116 C 1.1611(6) 0.1425(2) 0.4143(5) 0.029(2) Uani 1 d . . H116 H 1.1028(6) 0.1342(2) 0.3867(5) 0.035 Uiso 1 calc R . C121 C 1.1592(5) 0.0852(2) 0.2488(6) 0.025(2) Uani 1 d . . C122 C 1.1321(5) 0.1134(2) 0.1895(5) 0.028(2) Uani 1 d . . H122 H 1.1612(5) 0.1349(2) 0.2033(5) 0.033 Uiso 1 calc R . C123 C 1.0658(5) 0.1118(3) 0.1125(6) 0.038(3) Uani 1 d . . H123 H 1.0517(5) 0.1316(3) 0.0736(6) 0.046 Uiso 1 calc R . C124 C 1.0199(6) 0.0814(3) 0.0917(6) 0.037(3) Uani 1 d . . H124 H 0.9722(6) 0.0803(3) 0.0406(6) 0.045 Uiso 1 calc R . C125 C 1.0442(5) 0.0530(2) 0.1459(6) 0.036(3) Uani 1 d . . H125 H 1.0138(5) 0.0318(2) 0.1319(6) 0.043 Uiso 1 calc R . C126 C 1.1143(5) 0.0549(2) 0.2226(5) 0.030(2) Uani 1 d . . H126 H 1.1314(5) 0.0346(2) 0.2577(5) 0.036 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0231(5) 0.0441(7) 0.0199(5) -0.0002(5) 0.0024(7) 0.0010(7) N11 0.042(4) 0.034(5) 0.045(4) -0.007(4) -0.007(4) 0.001(4) O11 0.043(4) 0.073(5) 0.038(3) 0.001(3) -0.002(3) 0.001(3) O13 0.060(4) 0.076(5) 0.027(3) 0.016(3) 0.008(3) 0.022(4) O14 0.053(4) 0.063(5) 0.044(4) -0.004(4) -0.010(3) 0.020(4) C1 0.034(5) 0.035(6) 0.017(4) -0.008(4) 0.011(4) 0.000(4) C2 0.027(5) 0.042(7) 0.045(6) 0.013(5) 0.002(5) -0.007(5) C3 0.044(6) 0.034(6) 0.050(6) 0.011(5) 0.022(5) -0.013(5) C4 0.043(6) 0.046(6) 0.016(4) 0.009(4) -0.001(3) -0.004(5) C5 0.040(5) 0.061(7) 0.017(4) -0.004(4) 0.003(4) 0.004(5) C6 0.035(5) 0.054(7) 0.048(6) -0.002(5) 0.019(5) -0.004(5) C7 0.026(5) 0.057(7) 0.034(5) -0.004(5) 0.015(4) -0.001(5) C8 0.026(5) 0.078(8) 0.030(5) -0.004(5) -0.004(4) 0.013(5) C9 0.036(6) 0.076(8) 0.017(4) 0.006(5) 0.011(4) 0.010(5) C10 0.031(5) 0.058(7) 0.040(6) 0.024(5) 0.021(4) 0.005(5) C11 0.021(4) 0.064(7) 0.025(5) 0.000(5) 0.008(4) -0.001(5) C12 0.048(6) 0.042(6) 0.039(5) -0.002(5) 0.001(4) 0.011(5) C13 0.029(5) 0.056(7) 0.042(6) 0.002(5) 0.000(5) 0.007(5) C14 0.058(6) 0.055(6) 0.046(5) -0.014(6) -0.003(5) 0.020(5) C15 0.059(6) 0.065(7) 0.071(7) 0.002(7) 0.027(6) 0.003(6) C16 0.066(8) 0.057(7) 0.050(6) 0.003(5) 0.006(6) -0.002(6) C17 0.080(8) 0.080(9) 0.078(8) -0.026(7) 0.062(7) -0.015(7) C18 0.072(8) 0.097(10) 0.062(7) 0.005(7) 0.031(7) -0.011(7) C19 0.103(11) 0.079(10) 0.081(10) 0.031(8) 0.051(9) 0.002(8) C20 0.155(13) 0.067(8) 0.069(8) 0.011(6) 0.060(10) 0.009(10) C21 0.098(9) 0.082(9) 0.044(6) 0.006(6) 0.011(7) 0.004(8) Co2 0.0248(5) 0.0459(7) 0.0171(5) 0.0018(5) 0.0010(7) 0.0002(8) N32 0.056(5) 0.048(5) 0.029(4) -0.002(3) -0.008(4) 0.016(5) O32 0.059(4) 0.075(5) 0.038(4) -0.007(4) 0.000(3) -0.010(4) O34 0.073(5) 0.059(5) 0.094(6) 0.006(5) 0.021(5) -0.007(4) O35 0.053(4) 0.045(4) 0.058(4) 0.004(4) -0.006(4) -0.001(3) C22 0.020(4) 0.047(6) 0.021(4) -0.005(4) 0.001(4) -0.001(4) C23 0.033(5) 0.051(6) 0.015(4) 0.005(4) 0.001(4) 0.002(5) C24 0.042(5) 0.049(6) 0.036(5) 0.008(5) 0.024(5) 0.008(5) C25 0.031(5) 0.102(10) 0.036(6) 0.019(6) 0.010(5) 0.020(6) C26 0.015(4) 0.105(9) 0.015(4) 0.008(6) 0.003(4) -0.019(5) C27 0.041(5) 0.056(7) 0.039(5) 0.013(5) 0.025(5) -0.001(6) C28 0.034(5) 0.084(8) 0.021(5) 0.011(5) 0.010(4) 0.006(5) C29 0.062(7) 0.066(8) 0.044(6) 0.034(6) 0.021(5) 0.010(6) C30 0.111(9) 0.051(8) 0.042(7) -0.009(6) 0.026(7) -0.034(7) C31 0.025(5) 0.124(11) 0.024(5) 0.008(7) 0.000(5) -0.020(6) C32 0.044(5) 0.059(7) 0.021(4) -0.007(5) 0.001(4) -0.024(5) C33 0.055(6) 0.058(7) 0.044(6) -0.001(5) 0.011(5) 0.010(5) C34 0.085(8) 0.039(7) 0.074(8) 0.001(7) 0.002(6) 0.012(7) C35 0.032(5) 0.094(9) 0.060(6) 0.004(6) 0.005(5) -0.003(6) C36 0.097(8) 0.070(8) 0.040(6) 0.003(6) 0.007(6) 0.017(7) C37 0.090(7) 0.045(6) 0.039(5) 0.001(4) -0.013(7) -0.004(8) C38 0.072(7) 0.035(6) 0.072(7) 0.009(6) -0.008(6) 0.003(5) C39 0.098(9) 0.052(6) 0.050(6) -0.001(5) -0.021(7) -0.001(7) C40 0.095(9) 0.076(8) 0.041(6) -0.009(6) 0.015(6) -0.027(7) C41 0.082(8) 0.052(7) 0.070(7) -0.003(6) 0.009(7) -0.024(6) C42 0.072(7) 0.046(7) 0.057(7) -0.007(6) -0.018(6) -0.022(6) B1 0.011(4) 0.032(5) 0.023(4) -0.001(4) -0.005(5) -0.005(6) C51 0.016(4) 0.039(6) 0.020(5) -0.001(4) -0.003(4) -0.010(4) C52 0.024(5) 0.051(7) 0.012(4) 0.002(4) 0.001(4) -0.003(5) C53 0.018(4) 0.061(7) 0.021(5) 0.000(5) 0.004(4) 0.003(4) C54 0.012(4) 0.087(8) 0.017(4) -0.001(5) -0.001(4) -0.003(5) C55 0.024(5) 0.050(7) 0.028(5) 0.019(5) -0.012(4) 0.008(4) C56 0.027(5) 0.050(7) 0.031(5) 0.003(5) -0.010(4) -0.005(5) C61 0.025(4) 0.041(5) 0.010(3) 0.002(3) -0.004(4) 0.012(5) C62 0.013(4) 0.045(7) 0.026(5) 0.001(5) 0.006(4) -0.005(4) C63 0.039(5) 0.038(6) 0.032(5) -0.013(5) 0.011(5) 0.000(5) C64 0.036(6) 0.048(6) 0.018(4) -0.013(4) -0.005(4) -0.003(5) C65 0.019(5) 0.056(7) 0.024(5) 0.000(5) -0.006(4) 0.004(5) C66 0.027(5) 0.041(6) 0.016(4) -0.001(4) -0.007(4) 0.000(4) C71 0.020(4) 0.039(5) 0.018(3) -0.009(3) -0.008(4) -0.001(5) C72 0.027(5) 0.037(6) 0.022(5) -0.001(4) -0.002(4) 0.004(4) C73 0.047(6) 0.041(7) 0.029(5) -0.004(5) 0.008(5) 0.001(5) C74 0.048(7) 0.048(6) 0.019(4) 0.006(4) -0.009(4) 0.005(5) C75 0.030(5) 0.067(8) 0.030(5) -0.004(5) -0.007(4) 0.005(5) C76 0.030(5) 0.041(6) 0.026(5) -0.006(5) -0.006(4) -0.001(4) C81 0.020(5) 0.052(7) 0.005(4) -0.003(4) -0.001(4) -0.011(5) C82 0.024(4) 0.033(5) 0.015(5) 0.001(4) -0.006(4) -0.004(4) C83 0.029(5) 0.034(6) 0.024(5) -0.014(5) -0.005(4) 0.007(4) C84 0.023(5) 0.060(7) 0.020(5) -0.006(5) -0.004(4) -0.001(5) C85 0.025(5) 0.053(7) 0.015(4) 0.008(4) -0.012(4) 0.008(5) C86 0.032(5) 0.030(6) 0.024(5) -0.003(5) -0.002(4) 0.005(5) B2 0.023(4) 0.032(5) 0.022(4) 0.001(4) 0.003(6) 0.002(6) C91 0.028(4) 0.033(5) 0.021(3) -0.005(3) 0.001(5) 0.001(6) C92 0.038(6) 0.049(8) 0.027(5) -0.007(5) 0.000(5) -0.004(5) C93 0.033(5) 0.033(7) 0.029(5) 0.000(5) -0.008(5) 0.004(5) C94 0.046(5) 0.042(5) 0.039(4) 0.006(4) 0.000(6) -0.011(7) C95 0.019(5) 0.054(8) 0.036(6) -0.013(5) 0.005(5) -0.009(5) C96 0.017(5) 0.036(7) 0.024(5) -0.009(5) 0.004(4) 0.003(4) C101 0.027(5) 0.047(7) 0.010(4) -0.004(5) -0.004(4) 0.013(5) C102 0.025(5) 0.054(7) 0.013(4) -0.002(4) -0.012(4) -0.006(5) C103 0.025(5) 0.056(7) 0.013(5) -0.003(4) -0.003(4) -0.005(5) C104 0.032(6) 0.090(9) 0.018(5) -0.010(6) -0.008(4) -0.008(7) C105 0.037(6) 0.059(8) 0.033(5) -0.012(6) -0.009(5) 0.015(6) C106 0.019(5) 0.056(8) 0.032(5) -0.004(5) -0.012(4) -0.002(5) C111 0.042(5) 0.035(5) 0.016(4) 0.013(3) -0.020(5) -0.009(6) C112 0.022(5) 0.054(7) 0.015(4) -0.001(4) -0.003(4) 0.005(5) C113 0.031(5) 0.043(6) 0.018(5) 0.006(4) -0.007(4) -0.008(5) C114 0.035(5) 0.031(5) 0.037(4) -0.006(4) 0.002(5) -0.007(6) C115 0.041(6) 0.039(6) 0.023(5) 0.002(5) 0.013(4) 0.007(5) C116 0.023(5) 0.041(6) 0.023(5) 0.010(4) 0.008(4) 0.009(4) C121 0.020(5) 0.037(6) 0.018(5) -0.006(5) 0.008(4) 0.013(5) C122 0.013(4) 0.052(7) 0.019(5) -0.016(4) 0.000(4) 0.002(4) C123 0.020(5) 0.077(8) 0.018(5) -0.001(5) 0.009(4) 0.011(5) C124 0.020(5) 0.065(8) 0.026(5) -0.012(5) 0.004(4) 0.004(5) C125 0.021(5) 0.055(7) 0.033(5) -0.026(5) 0.006(4) 0.008(5) C126 0.026(5) 0.054(7) 0.011(4) -0.011(5) 0.000(4) 0.004(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 Co1 C2 2.014(8) . ? Co1 C9 2.016(7) . ? Co1 C10 2.020(8) . ? Co1 C6 2.022(8) . ? Co1 C8 2.023(8) . ? Co1 C1 2.027(7) . ? Co1 C3 2.034(8) . ? Co1 C7 2.034(7) . ? Co1 C4 2.042(7) . ? Co1 C5 2.047(7) . ? N11 C11 1.337(9) . ? N11 C12 1.445(9) . ? O11 C11 1.246(8) . ? O13 C13 1.198(9) . ? O14 C13 1.325(10) . ? O14 C14 1.456(8) . ? C1 C2 1.417(10) . ? C1 C5 1.426(10) . ? C1 C11 1.504(11) . ? C2 C3 1.399(10) . ? C3 C4 1.430(10) . ? C4 C5 1.410(10) . ? C6 C7 1.391(11) . ? C6 C10 1.444(10) . ? C7 C8 1.396(10) . ? C8 C9 1.404(10) . ? C9 C10 1.382(11) . ? C12 C13 1.532(11) . ? C12 C15 1.535(10) . ? C15 C16 1.494(11) . ? C16 C21 1.353(12) . ? C16 C17 1.424(13) . ? C17 C18 1.402(11) . ? C18 C19 1.383(13) . ? C19 C20 1.351(15) . ? C20 C21 1.428(12) . ? Co2 C31 2.012(8) . ? Co2 C27 2.014(8) . ? Co2 C29 2.015(8) . ? Co2 C28 2.020(7) . ? Co2 C30 2.020(9) . ? Co2 C22 2.029(8) . ? Co2 C25 2.031(8) . ? Co2 C24 2.037(7) . ? Co2 C23 2.038(7) . ? Co2 C26 2.050(7) . ? N32 C32 1.347(9) . ? N32 C33 1.441(9) . ? O32 C32 1.232(8) . ? O34 C34 1.215(10) . ? O35 C34 1.329(11) . ? O35 C35 1.470(8) . ? C22 C23 1.413(10) . ? C22 C26 1.441(10) . ? C22 C32 1.468(11) . ? C23 C24 1.390(10) . ? C24 C25 1.409(11) . ? C25 C26 1.398(12) . ? C27 C28 1.352(10) . ? C27 C31 1.383(11) . ? C28 C29 1.404(12) . ? C29 C30 1.419(12) . ? C30 C31 1.397(13) . ? C33 C36 1.494(10) . ? C33 C34 1.529(12) . ? C36 C37 1.528(12) . ? C37 C38 1.387(11) . ? C37 C42 1.412(13) . ? C38 C39 1.367(11) . ? C39 C40 1.392(11) . ? C40 C41 1.379(11) . ? C41 C42 1.397(11) . ? B1 C81 1.611(10) . ? B1 C71 1.629(10) . ? B1 C61 1.651(9) . ? B1 C51 1.665(11) . ? C51 C52 1.399(10) . ? C51 C56 1.401(11) . ? C52 C53 1.389(10) . ? C53 C54 1.377(11) . ? C54 C55 1.411(11) . ? C55 C56 1.379(10) . ? C61 C62 1.378(10) . ? C61 C66 1.440(10) . ? C62 C63 1.399(10) . ? C63 C64 1.386(10) . ? C64 C65 1.374(9) . ? C65 C66 1.382(10) . ? C71 C76 1.393(10) . ? C71 C72 1.433(10) . ? C72 C73 1.390(10) . ? C73 C74 1.386(10) . ? C74 C75 1.379(10) . ? C75 C76 1.384(10) . ? C81 C86 1.386(11) . ? C81 C82 1.417(10) . ? C82 C83 1.382(9) . ? C83 C84 1.368(10) . ? C84 C85 1.367(11) . ? C85 C86 1.438(10) . ? B2 C91 1.633(10) . ? B2 C111 1.652(10) . ? B2 C121 1.654(11) . ? B2 C101 1.655(11) . ? C91 C92 1.399(11) . ? C91 C96 1.414(10) . ? C92 C93 1.378(10) . ? C93 C94 1.360(10) . ? C94 C95 1.404(10) . ? C95 C96 1.389(10) . ? C101 C106 1.391(11) . ? C101 C102 1.398(11) . ? C102 C103 1.404(10) . ? C103 C104 1.368(11) . ? C104 C105 1.371(12) . ? C105 C106 1.394(11) . ? C111 C116 1.411(11) . ? C111 C112 1.414(11) . ? C112 C113 1.375(10) . ? C113 C114 1.383(10) . ? C114 C115 1.374(10) . ? C115 C116 1.399(10) . ? C121 C126 1.383(11) . ? C121 C122 1.408(10) . ? C122 C123 1.377(9) . ? C123 C124 1.379(11) . ? C124 C125 1.365(11) . ? C125 C126 1.412(10) . ? 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 C2 Co1 C9 106.8(3) . . ? C2 Co1 C10 114.9(3) . . ? C9 Co1 C10 40.1(3) . . ? C2 Co1 C6 149.3(4) . . ? C9 Co1 C6 68.7(3) . . ? C10 Co1 C6 41.9(3) . . ? C2 Co1 C8 129.1(4) . . ? C9 Co1 C8 40.7(3) . . ? C10 Co1 C8 68.2(3) . . ? C6 Co1 C8 68.3(3) . . ? C2 Co1 C1 41.0(3) . . ? C9 Co1 C1 127.1(3) . . ? C10 Co1 C1 105.8(3) . . ? C6 Co1 C1 116.0(3) . . ? C8 Co1 C1 166.4(3) . . ? C2 Co1 C3 40.4(3) . . ? C9 Co1 C3 117.3(4) . . ? C10 Co1 C3 148.5(4) . . ? C6 Co1 C3 168.9(4) . . ? C8 Co1 C3 109.6(4) . . ? C1 Co1 C3 68.7(3) . . ? C2 Co1 C7 168.3(3) . . ? C9 Co1 C7 67.9(3) . . ? C10 Co1 C7 68.3(3) . . ? C6 Co1 C7 40.1(3) . . ? C8 Co1 C7 40.3(3) . . ? C1 Co1 C7 150.5(3) . . ? C3 Co1 C7 131.5(4) . . ? C2 Co1 C4 68.6(3) . . ? C9 Co1 C4 151.8(4) . . ? C10 Co1 C4 167.9(4) . . ? C6 Co1 C4 129.6(3) . . ? C8 Co1 C4 119.5(3) . . ? C1 Co1 C4 68.8(3) . . ? C3 Co1 C4 41.1(3) . . ? C7 Co1 C4 110.7(3) . . ? C2 Co1 C5 68.6(3) . . ? C9 Co1 C5 166.1(4) . . ? C10 Co1 C5 128.7(4) . . ? C6 Co1 C5 108.1(3) . . ? C8 Co1 C5 152.1(3) . . ? C1 Co1 C5 41.0(3) . . ? C3 Co1 C5 68.4(3) . . ? C7 Co1 C5 119.0(3) . . ? C4 Co1 C5 40.3(3) . . ? C11 N11 C12 118.7(7) . . ? C13 O14 C14 118.0(6) . . ? C2 C1 C5 107.2(8) . . ? C2 C1 C11 123.5(7) . . ? C5 C1 C11 129.2(8) . . ? C2 C1 Co1 69.0(4) . . ? C5 C1 Co1 70.3(4) . . ? C11 C1 Co1 122.2(5) . . ? C3 C2 C1 109.0(8) . . ? C3 C2 Co1 70.6(5) . . ? C1 C2 Co1 70.0(4) . . ? C2 C3 C4 107.8(8) . . ? C2 C3 Co1 69.0(5) . . ? C4 C3 Co1 69.8(4) . . ? C5 C4 C3 107.7(7) . . ? C5 C4 Co1 70.0(4) . . ? C3 C4 Co1 69.2(4) . . ? C4 C5 C1 108.3(7) . . ? C4 C5 Co1 69.6(4) . . ? C1 C5 Co1 68.7(4) . . ? C7 C6 C10 106.8(8) . . ? C7 C6 Co1 70.4(5) . . ? C10 C6 Co1 69.0(4) . . ? C6 C7 C8 109.1(8) . . ? C6 C7 Co1 69.5(5) . . ? C8 C7 Co1 69.4(4) . . ? C7 C8 C9 107.8(9) . . ? C7 C8 Co1 70.3(5) . . ? C9 C8 Co1 69.4(4) . . ? C10 C9 C8 108.9(8) . . ? C10 C9 Co1 70.1(5) . . ? C8 C9 Co1 70.0(4) . . ? C9 C10 C6 107.4(8) . . ? C9 C10 Co1 69.8(5) . . ? C6 C10 Co1 69.2(4) . . ? O11 C11 N11 124.2(8) . . ? O11 C11 C1 119.7(8) . . ? N11 C11 C1 116.0(7) . . ? N11 C12 C13 109.7(7) . . ? N11 C12 C15 111.4(7) . . ? C13 C12 C15 106.0(7) . . ? O13 C13 O14 126.0(9) . . ? O13 C13 C12 123.2(9) . . ? O14 C13 C12 110.7(8) . . ? C16 C15 C12 114.2(8) . . ? C21 C16 C17 117.9(9) . . ? C21 C16 C15 124.0(10) . . ? C17 C16 C15 117.9(9) . . ? C18 C17 C16 122.1(10) . . ? C19 C18 C17 117.2(10) . . ? C20 C19 C18 122.2(12) . . ? C19 C20 C21 120.1(13) . . ? C16 C21 C20 120.4(11) . . ? C31 Co2 C27 40.2(3) . . ? C31 Co2 C29 68.4(4) . . ? C27 Co2 C29 67.6(4) . . ? C31 Co2 C28 67.3(3) . . ? C27 Co2 C28 39.2(3) . . ? C29 Co2 C28 40.7(3) . . ? C31 Co2 C30 40.6(4) . . ? C27 Co2 C30 67.8(4) . . ? C29 Co2 C30 41.2(3) . . ? C28 Co2 C30 68.3(4) . . ? C31 Co2 C22 120.5(4) . . ? C27 Co2 C22 109.5(3) . . ? C29 Co2 C22 163.7(4) . . ? C28 Co2 C22 126.9(4) . . ? C30 Co2 C22 154.2(4) . . ? C31 Co2 C25 161.6(5) . . ? C27 Co2 C25 156.6(4) . . ? C29 Co2 C25 107.6(4) . . ? C28 Co2 C25 122.2(3) . . ? C30 Co2 C25 124.7(5) . . ? C22 Co2 C25 68.4(4) . . ? C31 Co2 C24 124.5(4) . . ? C27 Co2 C24 162.2(4) . . ? C29 Co2 C24 119.7(4) . . ? C28 Co2 C24 156.0(4) . . ? C30 Co2 C24 106.1(4) . . ? C22 Co2 C24 68.2(3) . . ? C25 Co2 C24 40.5(3) . . ? C31 Co2 C23 107.7(3) . . ? C27 Co2 C23 127.0(3) . . ? C29 Co2 C23 154.0(4) . . ? C28 Co2 C23 163.4(4) . . ? C30 Co2 C23 119.0(4) . . ? C22 Co2 C23 40.7(3) . . ? C25 Co2 C23 67.6(3) . . ? C24 Co2 C23 39.9(3) . . ? C31 Co2 C26 156.7(5) . . ? C27 Co2 C26 122.7(4) . . ? C29 Co2 C26 125.4(4) . . ? C28 Co2 C26 109.6(3) . . ? C30 Co2 C26 162.0(5) . . ? C22 Co2 C26 41.4(3) . . ? C25 Co2 C26 40.1(3) . . ? C24 Co2 C26 68.1(3) . . ? C23 Co2 C26 68.3(3) . . ? C32 N32 C33 119.5(7) . . ? C34 O35 C35 114.7(7) . . ? C23 C22 C26 107.1(8) . . ? C23 C22 C32 130.3(7) . . ? C26 C22 C32 122.6(8) . . ? C23 C22 Co2 70.0(4) . . ? C26 C22 Co2 70.1(5) . . ? C32 C22 Co2 124.0(5) . . ? C24 C23 C22 108.9(7) . . ? C24 C23 Co2 70.0(4) . . ? C22 C23 Co2 69.3(4) . . ? C23 C24 C25 107.9(8) . . ? C23 C24 Co2 70.1(4) . . ? C25 C24 Co2 69.5(5) . . ? C26 C25 C24 109.2(9) . . ? C26 C25 Co2 70.7(5) . . ? C24 C25 Co2 70.0(5) . . ? C25 C26 C22 106.9(8) . . ? C25 C26 Co2 69.2(5) . . ? C22 C26 Co2 68.5(4) . . ? C28 C27 C31 109.4(9) . . ? C28 C27 Co2 70.6(5) . . ? C31 C27 Co2 69.8(5) . . ? C27 C28 C29 108.7(8) . . ? C27 C28 Co2 70.2(4) . . ? C29 C28 Co2 69.5(5) . . ? C28 C29 C30 106.8(9) . . ? C28 C29 Co2 69.8(5) . . ? C30 C29 Co2 69.6(5) . . ? C31 C30 C29 106.9(9) . . ? C31 C30 Co2 69.4(5) . . ? C29 C30 Co2 69.2(5) . . ? C27 C31 C30 108.1(9) . . ? C27 C31 Co2 70.0(5) . . ? C30 C31 Co2 70.0(5) . . ? O32 C32 N32 121.4(9) . . ? O32 C32 C22 120.4(8) . . ? N32 C32 C22 118.1(7) . . ? N32 C33 C36 112.0(7) . . ? N32 C33 C34 112.0(8) . . ? C36 C33 C34 107.3(8) . . ? O34 C34 O35 125.4(10) . . ? O34 C34 C33 119.4(10) . . ? O35 C34 C33 115.0(9) . . ? C33 C36 C37 111.7(8) . . ? C38 C37 C42 117.0(9) . . ? C38 C37 C36 118.9(10) . . ? C42 C37 C36 124.1(8) . . ? C39 C38 C37 123.6(9) . . ? C38 C39 C40 118.4(9) . . ? C41 C40 C39 120.8(9) . . ? C40 C41 C42 119.9(9) . . ? C41 C42 C37 120.3(8) . . ? C81 B1 C71 114.6(7) . . ? C81 B1 C61 112.7(6) . . ? C71 B1 C61 104.2(5) . . ? C81 B1 C51 103.0(5) . . ? C71 B1 C51 111.4(6) . . ? C61 B1 C51 111.1(7) . . ? C52 C51 C56 116.4(8) . . ? C52 C51 B1 121.6(7) . . ? C56 C51 B1 121.5(7) . . ? C53 C52 C51 120.7(9) . . ? C54 C53 C52 122.4(9) . . ? C53 C54 C55 117.7(7) . . ? C56 C55 C54 119.6(8) . . ? C55 C56 C51 123.1(9) . . ? C62 C61 C66 114.8(6) . . ? C62 C61 B1 124.4(8) . . ? C66 C61 B1 120.5(7) . . ? C61 C62 C63 122.7(8) . . ? C64 C63 C62 120.4(8) . . ? C65 C64 C63 119.3(7) . . ? C64 C65 C66 119.9(8) . . ? C65 C66 C61 122.8(8) . . ? C76 C71 C72 114.7(7) . . ? C76 C71 B1 124.4(8) . . ? C72 C71 B1 120.5(7) . . ? C73 C72 C71 121.9(8) . . ? C74 C73 C72 120.9(8) . . ? C75 C74 C73 118.1(8) . . ? C74 C75 C76 121.3(8) . . ? C75 C76 C71 123.1(8) . . ? C86 C81 C82 115.0(7) . . ? C86 C81 B1 122.5(8) . . ? C82 C81 B1 122.4(7) . . ? C83 C82 C81 122.7(8) . . ? C84 C83 C82 120.3(8) . . ? C85 C84 C83 120.9(8) . . ? C84 C85 C86 118.2(9) . . ? C81 C86 C85 122.9(8) . . ? C91 B2 C111 105.2(5) . . ? C91 B2 C121 112.6(7) . . ? C111 B2 C121 111.5(7) . . ? C91 B2 C101 112.9(7) . . ? C111 B2 C101 111.4(7) . . ? C121 B2 C101 103.5(5) . . ? C92 C91 C96 114.2(6) . . ? C92 C91 B2 122.7(8) . . ? C96 C91 B2 123.0(8) . . ? C93 C92 C91 123.3(8) . . ? C94 C93 C92 121.3(8) . . ? C93 C94 C95 118.6(7) . . ? C96 C95 C94 119.4(8) . . ? C95 C96 C91 123.1(8) . . ? C106 C101 C102 117.7(8) . . ? C106 C101 B2 122.4(8) . . ? C102 C101 B2 119.6(8) . . ? C101 C102 C103 120.4(9) . . ? C104 C103 C102 120.2(9) . . ? C103 C104 C105 120.4(9) . . ? C104 C105 C106 119.8(9) . . ? C101 C106 C105 121.4(9) . . ? C116 C111 C112 114.0(7) . . ? C116 C111 B2 124.1(8) . . ? C112 C111 B2 121.9(9) . . ? C113 C112 C111 123.1(8) . . ? C112 C113 C114 120.8(8) . . ? C115 C114 C113 119.1(7) . . ? C114 C115 C116 119.7(8) . . ? C115 C116 C111 123.2(8) . . ? C126 C121 C122 114.4(8) . . ? C126 C121 B2 124.3(7) . . ? C122 C121 B2 120.7(7) . . ? C123 C122 C121 123.6(9) . . ? C122 C123 C124 120.1(9) . . ? C125 C124 C123 118.8(8) . . ? C124 C125 C126 120.4(9) . . ? C121 C126 C125 122.6(9) . . ? _refine_diff_density_max 0.410 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.070 #===END data_4a _database_code_CSD 180590 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[C24 H26 Fe N2 O4] * 0.25 CH2Cl2' _chemical_formula_analytical ? _chemical_formula_sum 'C24.25 H26.50 Cl0.50 Fe N2 O4' _chemical_formula_weight 483.55 _chemical_melting_point ? _chemical_compound_source ? 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' '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 'Tetragonal' _symmetry_space_group_name_H-M 'P4(3)2(1)2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 17.2236(14) _cell_length_b 17.2236(14) _cell_length_c 16.9834(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5038.2(7) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6835 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent block' _exptl_crystal_colour 'yellow brown' _exptl_crystal_size_max 1.28 _exptl_crystal_size_mid 0.70 _exptl_crystal_size_min 0.60 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.275 _exptl_crystal_density_method ? _exptl_crystal_F_000 2020 _exptl_absorpt_coefficient_mu 0.682 _exptl_absorpt_correction_type 'SADABS, G.M. Sheldrick 1994' _exptl_absorpt_correction_T_min 0.585 _exptl_absorpt_correction_T_max 0.696 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Siemens SMART CCD-Detector' _diffrn_measurement_method '\w, 0.3 deg./frame' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54254 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 32.50 _reflns_number_total 9128 _reflns_number_observed 6621 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SAINT' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 6 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1187P)^2^+2.6729P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 9122 _refine_ls_number_parameters 300 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0972 _refine_ls_R_factor_obs 0.0703 _refine_ls_wR_factor_all 0.2124 _refine_ls_wR_factor_obs 0.1965 _refine_ls_goodness_of_fit_all 1.079 _refine_ls_goodness_of_fit_obs 1.182 _refine_ls_restrained_S_all 1.087 _refine_ls_restrained_S_obs 1.182 _refine_ls_shift/esd_max 0.008 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.27477(3) 0.55633(3) 0.02318(3) 0.03478(14) Uani 1 d . . C1 C 0.2094(2) 0.6511(2) -0.0003(2) 0.0370(7) Uani 1 d . . H1 H 0.2053(2) 0.6763(2) -0.0499(2) 0.044 Uiso 1 calc R . C2 C 0.2637(2) 0.6689(2) 0.0598(2) 0.0368(7) Uani 1 d . . H2 H 0.3020(2) 0.7086(2) 0.0577(2) 0.044 Uiso 1 calc R . C3 C 0.2510(2) 0.6173(2) 0.1234(2) 0.0344(7) Uani 1 d . . H3 H 0.2795(2) 0.6165(2) 0.1713(2) 0.041 Uiso 1 calc R . C4 C 0.1889(2) 0.5669(2) 0.1038(2) 0.0311(6) Uani 1 d . . H4 H 0.1687(2) 0.5264(2) 0.1357(2) 0.037 Uiso 1 calc R . C5 C 0.1621(2) 0.5886(2) 0.0268(2) 0.0243(5) Uani 1 d . . O6 O 0.08078(15) 0.5808(2) -0.08503(13) 0.0341(5) Uani 1 d . . C6 C 0.0999(2) 0.5525(2) -0.0211(2) 0.0261(5) Uani 1 d . . N7 N 0.0664(2) 0.4872(2) 0.00709(14) 0.0278(5) Uani 1 d D . H7 H 0.0682(26) 0.4693(24) 0.0604(19) 0.033 Uiso 1 d D . C8 C 0.0055(2) 0.4478(2) -0.0373(2) 0.0289(6) Uani 1 d . . H8 H 0.0238(2) 0.4389(2) -0.0924(2) 0.035 Uiso 1 calc R . O9 O -0.08872(13) 0.53952(14) 0.01580(12) 0.0295(5) Uani 1 d . . C9 C -0.0687(2) 0.4978(2) -0.0392(2) 0.0244(5) Uani 1 d . . N10 N -0.11234(15) 0.4870(2) -0.10367(14) 0.0263(5) Uani 1 d D . H10 H -0.0830(23) 0.4695(24) -0.1481(20) 0.032 Uiso 1 d D . C11 C -0.1876(2) 0.5238(2) -0.1125(2) 0.0250(5) Uani 1 d . . H11 H -0.1809(2) 0.5800(2) -0.1256(2) 0.030 Uiso 1 calc R . C12 C -0.2313(2) 0.4818(3) -0.1800(2) 0.0372(8) Uani 1 d . . H12A H -0.1983(2) 0.4811(3) -0.2277(2) 0.045 Uiso 1 calc R . H12B H -0.2415(2) 0.4273(3) -0.1645(2) 0.045 Uiso 1 calc R . C13 C -0.3074(2) 0.5217(2) -0.1986(2) 0.0332(7) Uani 1 d . . C14 C -0.3101(3) 0.5820(3) -0.2503(3) 0.0586(13) Uani 1 d . . H14 H -0.2640(3) 0.5978(3) -0.2766(3) 0.070 Uiso 1 calc R . C15 C -0.3793(3) 0.6208(3) -0.2652(4) 0.070(2) Uani 1 d . . H15 H -0.3801(3) 0.6629(3) -0.3014(4) 0.084 Uiso 1 calc R . C16 C -0.4459(3) 0.5989(3) -0.2280(3) 0.0563(11) Uani 1 d . . H16 H -0.4929(3) 0.6261(3) -0.2377(3) 0.068 Uiso 1 calc R . C17 C -0.4450(2) 0.5369(3) -0.1761(2) 0.0486(10) Uani 1 d . . H17 H -0.4914(2) 0.5213(3) -0.1503(2) 0.058 Uiso 1 calc R . C18 C -0.3753(2) 0.4972(2) -0.1618(2) 0.0363(7) Uani 1 d . . H18 H -0.3744(2) 0.4539(2) -0.1272(2) 0.044 Uiso 1 calc R . C19 C -0.0138(2) 0.3707(2) 0.0001(2) 0.0395(8) Uani 1 d . . H19A H -0.0557(14) 0.3457(9) -0.0295(12) 0.059 Uiso 1 calc R . H19B H -0.0305(19) 0.3791(3) 0.0546(7) 0.059 Uiso 1 calc R . H19C H 0.0323(6) 0.3373(7) -0.0005(18) 0.059 Uiso 1 calc R . C20 C -0.2340(2) 0.5153(2) -0.0367(2) 0.0306(6) Uani 1 d . . O20 O -0.2483(2) 0.4552(2) -0.0054(2) 0.0436(6) Uani 1 d . . O21 O -0.2585(2) 0.5844(2) -0.01218(15) 0.0433(6) Uani 1 d . . C22 C -0.3022(4) 0.5817(4) 0.0602(2) 0.076(2) Uani 1 d . . H22A H -0.3173(27) 0.6345(5) 0.0754(17) 0.114 Uiso 1 calc R . H22B H -0.2701(12) 0.5588(29) 0.1018(8) 0.114 Uiso 1 calc R . H22C H -0.3489(17) 0.5500(26) 0.0526(9) 0.114 Uiso 1 calc R . C23 C 0.3865(3) 0.5394(5) -0.0115(3) 0.073(2) Uani 1 d . . H23 H 0.4270(3) 0.5768(5) -0.0100(3) 0.087 Uiso 1 calc R . C24 C 0.3682(3) 0.4882(3) 0.0477(4) 0.066(2) Uani 1 d . . H24 H 0.3930(3) 0.4845(3) 0.0976(4) 0.079 Uiso 1 calc R . C25 C 0.3057(3) 0.4423(3) 0.0209(5) 0.079(2) Uani 1 d . . H25 H 0.2827(3) 0.4010(3) 0.0496(5) 0.095 Uiso 1 calc R . C26 C 0.2828(3) 0.4664(4) -0.0542(4) 0.074(2) Uani 1 d . . H26 H 0.2410(3) 0.4463(4) -0.0845(4) 0.089 Uiso 1 calc R . C27 C 0.3342(3) 0.5269(5) -0.0761(3) 0.077(2) Uani 1 d . . H27 H 0.3340(3) 0.5542(5) -0.1247(3) 0.093 Uiso 1 calc R . C30 C 0.2787(6) 0.7331(6) -0.2054(7) 0.028(2) Uiso 0.25 d PD . Cl1 Cl 0.3321(3) 0.7759(3) -0.1390(3) 0.0656(12) Uiso 0.25 d PD . Cl2 Cl 0.2013(7) 0.6778(7) -0.2023(7) 0.128(3) Uiso 0.25 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 Fe1 0.0239(2) 0.0450(3) 0.0355(2) -0.0117(2) -0.0006(2) 0.0046(2) C1 0.039(2) 0.041(2) 0.0311(15) 0.0083(14) -0.0003(13) -0.0013(14) C2 0.033(2) 0.036(2) 0.041(2) 0.0001(14) -0.0001(14) -0.0058(14) C3 0.0290(14) 0.048(2) 0.0265(14) -0.0070(13) -0.0027(12) -0.0012(14) C4 0.0311(15) 0.040(2) 0.0222(12) -0.0001(12) -0.0040(11) -0.0001(13) C5 0.0230(12) 0.0296(13) 0.0203(11) 0.0007(11) 0.0032(10) 0.0042(10) O6 0.0387(13) 0.0426(13) 0.0210(9) 0.0040(9) -0.0051(9) 0.0035(10) C6 0.0237(12) 0.0365(15) 0.0179(11) -0.0036(12) 0.0026(10) 0.0056(11) N7 0.0260(12) 0.0395(14) 0.0180(10) 0.0003(10) -0.0011(9) 0.0005(11) C8 0.0266(13) 0.041(2) 0.0194(11) -0.0069(12) 0.0002(10) 0.0011(13) O9 0.0279(10) 0.0403(13) 0.0203(9) -0.0075(9) -0.0005(8) 0.0025(9) C9 0.0244(13) 0.0308(13) 0.0179(11) -0.0013(10) -0.0016(10) -0.0014(11) N10 0.0228(11) 0.0377(14) 0.0184(10) -0.0051(10) -0.0001(9) -0.0005(10) C11 0.0232(13) 0.0352(15) 0.0166(10) -0.0025(11) 0.0011(10) -0.0021(11) C12 0.0283(15) 0.060(2) 0.0230(12) -0.0121(14) -0.0030(12) -0.0020(15) C13 0.031(2) 0.047(2) 0.0214(12) -0.0038(13) -0.0054(12) -0.0056(13) C14 0.041(2) 0.086(3) 0.049(2) 0.031(2) -0.014(2) -0.024(2) C15 0.067(3) 0.067(3) 0.077(4) 0.029(3) -0.043(3) -0.017(2) C16 0.051(2) 0.059(3) 0.059(2) -0.006(2) -0.030(2) 0.010(2) C17 0.029(2) 0.073(3) 0.044(2) -0.001(2) -0.004(2) 0.000(2) C18 0.034(2) 0.043(2) 0.032(2) 0.0018(14) -0.0039(13) -0.0047(14) C19 0.042(2) 0.035(2) 0.042(2) -0.0046(14) -0.003(2) 0.0023(14) C20 0.0232(13) 0.051(2) 0.0180(11) -0.0007(12) 0.0006(10) 0.0009(12) O20 0.0419(14) 0.056(2) 0.0331(12) 0.0088(12) 0.0017(11) -0.0111(13) O21 0.0458(15) 0.057(2) 0.0275(11) -0.0090(11) 0.0017(10) 0.0174(12) C22 0.082(4) 0.117(5) 0.029(2) -0.003(3) 0.009(2) 0.054(4) C23 0.027(2) 0.125(5) 0.066(3) -0.039(4) 0.002(2) 0.015(3) C24 0.039(2) 0.075(3) 0.083(4) -0.035(3) -0.014(2) 0.025(2) C25 0.056(3) 0.056(3) 0.126(5) -0.039(3) -0.017(3) 0.022(2) C26 0.043(2) 0.095(4) 0.084(4) -0.061(3) -0.011(2) 0.020(3) C27 0.048(3) 0.129(6) 0.055(3) -0.032(3) 0.013(2) 0.017(3) _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 C5 2.020(3) . ? Fe1 C1 2.023(4) . ? Fe1 C4 2.024(3) . ? Fe1 C23 2.033(4) . ? Fe1 C24 2.035(5) . ? Fe1 C26 2.035(5) . ? Fe1 C25 2.036(5) . ? Fe1 C27 2.037(5) . ? Fe1 C3 2.041(3) . ? Fe1 C2 2.046(4) . ? C1 C2 1.418(5) . ? C1 C5 1.427(5) . ? C2 C3 1.417(5) . ? C3 C4 1.418(5) . ? C4 C5 1.436(4) . ? C5 C6 1.482(4) . ? O6 C6 1.235(4) . ? C6 N7 1.351(4) . ? N7 C8 1.459(4) . ? C8 C19 1.510(5) . ? C8 C9 1.541(4) . ? O9 C9 1.228(4) . ? C9 N10 1.341(4) . ? N10 C11 1.450(4) . ? C11 C20 1.522(4) . ? C11 C12 1.550(4) . ? C12 C13 1.514(5) . ? C13 C14 1.361(6) . ? C13 C18 1.390(5) . ? C14 C15 1.389(8) . ? C15 C16 1.364(8) . ? C16 C17 1.385(7) . ? C17 C18 1.403(6) . ? C20 O20 1.190(5) . ? C20 O21 1.330(4) . ? O21 C22 1.442(5) . ? C23 C24 1.375(9) . ? C23 C27 1.436(8) . ? C24 C25 1.411(8) . ? C25 C26 1.399(10) . ? C26 C27 1.416(10) . ? C30 C30 1.54(2) 8_664 ? C30 Cl1 1.631(9) . ? C30 Cl2 1.639(10) . ? C30 Cl2 2.07(2) 8_664 ? Cl2 C30 2.07(2) 8_664 ? 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 C5 Fe1 C1 41.33(14) . . ? C5 Fe1 C4 41.60(12) . . ? C1 Fe1 C4 69.75(14) . . ? C5 Fe1 C23 163.2(2) . . ? C1 Fe1 C23 125.8(3) . . ? C4 Fe1 C23 154.3(2) . . ? C5 Fe1 C24 155.8(2) . . ? C1 Fe1 C24 161.1(2) . . ? C4 Fe1 C24 119.4(2) . . ? C23 Fe1 C24 39.5(3) . . ? C5 Fe1 C26 107.1(2) . . ? C1 Fe1 C26 121.6(2) . . ? C4 Fe1 C26 123.7(2) . . ? C23 Fe1 C26 68.9(2) . . ? C24 Fe1 C26 68.9(2) . . ? C5 Fe1 C25 121.2(2) . . ? C1 Fe1 C25 157.0(2) . . ? C4 Fe1 C25 106.9(2) . . ? C23 Fe1 C25 66.9(3) . . ? C24 Fe1 C25 40.6(2) . . ? C26 Fe1 C25 40.2(3) . . ? C5 Fe1 C27 125.2(2) . . ? C1 Fe1 C27 108.5(2) . . ? C4 Fe1 C27 161.8(2) . . ? C23 Fe1 C27 41.3(2) . . ? C24 Fe1 C27 68.2(3) . . ? C26 Fe1 C27 40.7(3) . . ? C25 Fe1 C27 67.2(3) . . ? C5 Fe1 C3 68.96(13) . . ? C1 Fe1 C3 68.8(2) . . ? C4 Fe1 C3 40.82(14) . . ? C23 Fe1 C3 120.3(2) . . ? C24 Fe1 C3 106.5(2) . . ? C26 Fe1 C3 160.6(3) . . ? C25 Fe1 C3 124.4(3) . . ? C27 Fe1 C3 156.8(2) . . ? C5 Fe1 C2 68.94(14) . . ? C1 Fe1 C2 40.8(2) . . ? C4 Fe1 C2 68.96(15) . . ? C23 Fe1 C2 108.2(2) . . ? C24 Fe1 C2 123.9(2) . . ? C26 Fe1 C2 157.5(3) . . ? C25 Fe1 C2 160.9(2) . . ? C27 Fe1 C2 122.3(3) . . ? C3 Fe1 C2 40.6(2) . . ? C2 C1 C5 108.0(3) . . ? C2 C1 Fe1 70.5(2) . . ? C5 C1 Fe1 69.3(2) . . ? C3 C2 C1 108.1(3) . . ? C3 C2 Fe1 69.6(2) . . ? C1 C2 Fe1 68.7(2) . . ? C2 C3 C4 108.7(3) . . ? C2 C3 Fe1 69.9(2) . . ? C4 C3 Fe1 68.9(2) . . ? C3 C4 C5 107.4(3) . . ? C3 C4 Fe1 70.3(2) . . ? C5 C4 Fe1 69.1(2) . . ? C1 C5 C4 107.8(3) . . ? C1 C5 C6 123.6(3) . . ? C4 C5 C6 128.5(3) . . ? C1 C5 Fe1 69.4(2) . . ? C4 C5 Fe1 69.3(2) . . ? C6 C5 Fe1 124.2(2) . . ? O6 C6 N7 121.8(3) . . ? O6 C6 C5 120.6(3) . . ? N7 C6 C5 117.6(3) . . ? C6 N7 C8 120.7(2) . . ? N7 C8 C19 110.4(3) . . ? N7 C8 C9 110.4(3) . . ? C19 C8 C9 108.5(3) . . ? O9 C9 N10 123.0(3) . . ? O9 C9 C8 122.9(3) . . ? N10 C9 C8 113.9(2) . . ? C9 N10 C11 121.7(2) . . ? N10 C11 C20 109.9(2) . . ? N10 C11 C12 107.9(3) . . ? C20 C11 C12 109.0(3) . . ? C13 C12 C11 111.3(3) . . ? C14 C13 C18 119.5(4) . . ? C14 C13 C12 120.7(4) . . ? C18 C13 C12 119.7(3) . . ? C13 C14 C15 120.9(4) . . ? C16 C15 C14 120.3(4) . . ? C15 C16 C17 119.9(4) . . ? C16 C17 C18 119.7(4) . . ? C13 C18 C17 119.6(4) . . ? O20 C20 O21 125.0(3) . . ? O20 C20 C11 124.7(3) . . ? O21 C20 C11 110.2(3) . . ? C20 O21 C22 113.8(4) . . ? C24 C23 C27 108.7(6) . . ? C24 C23 Fe1 70.3(3) . . ? C27 C23 Fe1 69.5(3) . . ? C23 C24 C25 107.3(6) . . ? C23 C24 Fe1 70.2(3) . . ? C25 C24 Fe1 69.8(3) . . ? C26 C25 C24 110.1(7) . . ? C26 C25 Fe1 69.9(3) . . ? C24 C25 Fe1 69.7(3) . . ? C25 C26 C27 106.4(5) . . ? C25 C26 Fe1 69.9(3) . . ? C27 C26 Fe1 69.7(3) . . ? C26 C27 C23 107.5(6) . . ? C26 C27 Fe1 69.6(3) . . ? C23 C27 Fe1 69.2(3) . . ? C30 C30 Cl1 144.4(11) 8_664 . ? C30 C30 Cl2 81.2(7) 8_664 . ? Cl1 C30 Cl2 134.4(9) . . ? C30 C30 Cl2 51.4(7) 8_664 8_664 ? Cl1 C30 Cl2 94.2(7) . 8_664 ? Cl2 C30 Cl2 129.4(8) . 8_664 ? C30 Cl2 C30 47.4(7) . 8_664 ? _refine_diff_density_max 1.799 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.117 #===END data_5b _database_code_CSD 180591 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[C19 H19 Co N O]+, (C24 H20 B)-' _chemical_formula_analytical ? _chemical_formula_sum 'C43 H39 B Co N O' _chemical_formula_weight 655.49 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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 'Triclinic' _symmetry_space_group_name_H-M 'P1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.4932(6) _cell_length_b 9.9247(8) _cell_length_c 9.9474(8) _cell_angle_alpha 97.90(2) _cell_angle_beta 92.80(2) _cell_angle_gamma 115.51(2) _cell_volume 831.65(15) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3874 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent platelet' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_method ? _exptl_crystal_F_000 344 _exptl_absorpt_coefficient_mu 0.552 _exptl_absorpt_correction_type 'SADABS, G.M. Sheldrick 1994' _exptl_absorpt_correction_T_min 0.711 _exptl_absorpt_correction_T_max 0.971 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Siemens SMART CCD-Detector' _diffrn_measurement_method '\w, 0.3 deg./frame' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8997 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 33.00 _reflns_number_total 5819 _reflns_number_observed 4921 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SAINT' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0521P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.022(11) _refine_ls_number_reflns 5814 _refine_ls_number_parameters 427 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_obs 0.0434 _refine_ls_wR_factor_all 0.0942 _refine_ls_wR_factor_obs 0.0895 _refine_ls_goodness_of_fit_all 1.014 _refine_ls_goodness_of_fit_obs 1.055 _refine_ls_restrained_S_all 1.015 _refine_ls_restrained_S_obs 1.055 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.31843(3) 0.58232(3) 0.89727(3) 0.02013(10) Uani 1 d . . O1 O 0.4815(2) 0.9513(2) 0.7586(2) 0.0276(4) Uani 1 d . . N1 N 0.2194(3) 0.8757(3) 0.7254(3) 0.0208(5) Uani 1 d . . H1 H 0.1343(41) 0.8040(43) 0.7017(35) 0.025 Uiso 1 d . . C1 C 0.3173(3) 0.6883(3) 0.7361(3) 0.0183(6) Uani 1 d . . C2 C 0.4420(4) 0.6446(4) 0.7357(3) 0.0225(6) Uani 1 d . . H2 H 0.5508(4) 0.7107(4) 0.7403(3) 0.027 Uiso 1 calc R . C3 C 0.3748(4) 0.4845(4) 0.7273(3) 0.0273(7) Uani 1 d . . H3 H 0.4307(4) 0.4247(4) 0.7259(3) 0.033 Uiso 1 calc R . C4 C 0.2096(4) 0.4301(4) 0.7213(3) 0.0252(7) Uani 1 d . . H4 H 0.1355(4) 0.3270(4) 0.7149(3) 0.030 Uiso 1 calc R . C5 C 0.1732(4) 0.5547(3) 0.7265(3) 0.0218(6) Uani 1 d . . H5 H 0.0710(4) 0.5500(3) 0.7240(3) 0.026 Uiso 1 calc R . C6 C 0.2506(5) 0.6660(5) 1.0655(4) 0.0354(8) Uani 1 d . . H6 H 0.1851(5) 0.7162(5) 1.0659(4) 0.043 Uiso 1 calc R . C7 C 0.1989(5) 0.5089(5) 1.0569(4) 0.0436(10) Uani 1 d . . H7 H 0.0927(5) 0.4348(5) 1.0502(4) 0.052 Uiso 1 calc R . C8 C 0.3337(5) 0.4808(4) 1.0602(4) 0.0416(10) Uani 1 d . . H8 H 0.3332(5) 0.3844(4) 1.0563(4) 0.050 Uiso 1 calc R . C9 C 0.4675(5) 0.6201(4) 1.0701(3) 0.0337(8) Uani 1 d . . H9 H 0.5733(5) 0.6345(4) 1.0739(3) 0.040 Uiso 1 calc R . C10 C 0.4162(4) 0.7366(4) 1.0735(3) 0.0295(8) Uani 1 d . . H10 H 0.4816(4) 0.8420(4) 1.0799(3) 0.035 Uiso 1 calc R . C11 C 0.3472(3) 0.8503(3) 0.7421(3) 0.0189(5) Uani 1 d . . C12 C 0.2365(3) 1.0279(3) 0.7110(3) 0.0230(6) Uani 1 d . . H12 H 0.3328(3) 1.1041(3) 0.7720(3) 0.028 Uiso 1 calc R . C13 C 0.2612(5) 1.0540(4) 0.5655(4) 0.0338(8) Uani 1 d . . H13A H 0.3532(5) 1.0402(4) 0.5403(4) 0.051 Uiso 1 calc R . H13B H 0.2784(5) 1.1575(4) 0.5590(4) 0.051 Uiso 1 calc R . H13C H 0.1680(5) 0.9813(4) 0.5033(4) 0.051 Uiso 1 calc R . C14 C 0.0964(3) 1.0463(3) 0.7619(3) 0.0188(5) Uani 1 d . . C15 C 0.0985(4) 1.0891(3) 0.9022(3) 0.0242(6) Uani 1 d . . H15 H 0.1880(4) 1.1085(3) 0.9631(3) 0.029 Uiso 1 calc R . C16 C -0.0288(4) 1.1035(3) 0.9534(3) 0.0292(6) Uani 1 d . . H16 H -0.0259(4) 1.1337(3) 1.0488(3) 0.035 Uiso 1 calc R . C17 C -0.1594(4) 1.0737(4) 0.8654(4) 0.0325(7) Uani 1 d . . H17 H -0.2478(4) 1.0806(4) 0.9005(4) 0.039 Uiso 1 calc R . C18 C -0.1620(3) 1.0339(3) 0.7261(4) 0.0287(7) Uani 1 d . . H18 H -0.2517(3) 1.0151(3) 0.6657(4) 0.034 Uiso 1 calc R . C19 C -0.0346(3) 1.0213(3) 0.6744(3) 0.0224(6) Uani 1 d . . H19 H -0.0367(3) 0.9954(3) 0.5785(3) 0.027 Uiso 1 calc R . B1 B 0.7993(4) 0.4958(3) 1.3975(3) 0.0172(6) Uani 1 d . . C20 C 0.6571(3) 0.3491(3) 1.2982(3) 0.0184(5) Uani 1 d . . C21 C 0.6762(3) 0.3010(3) 1.1645(3) 0.0245(6) Uani 1 d . . H21 H 0.7743(3) 0.3540(3) 1.1320(3) 0.029 Uiso 1 calc R . C22 C 0.5575(4) 0.1786(4) 1.0769(3) 0.0294(7) Uani 1 d . . H22 H 0.5753(4) 0.1500(4) 0.9865(3) 0.035 Uiso 1 calc R . C23 C 0.4134(4) 0.0984(3) 1.1214(3) 0.0271(7) Uani 1 d . . H23 H 0.3331(4) 0.0128(3) 1.0631(3) 0.033 Uiso 1 calc R . C24 C 0.3880(4) 0.1446(4) 1.2513(3) 0.0258(7) Uani 1 d . . H24 H 0.2890(4) 0.0917(4) 1.2824(3) 0.031 Uiso 1 calc R . C25 C 0.5069(3) 0.2682(3) 1.3366(3) 0.0223(5) Uani 1 d . . H25 H 0.4858(3) 0.2995(3) 1.4249(3) 0.027 Uiso 1 calc R . C26 C 0.7785(3) 0.4968(3) 1.5605(3) 0.0174(5) Uani 1 d . . C27 C 0.7302(4) 0.3638(3) 1.6182(3) 0.0231(6) Uani 1 d . . H27 H 0.7013(4) 0.2698(3) 1.5593(3) 0.028 Uiso 1 calc R . C28 C 0.7231(4) 0.3646(4) 1.7573(3) 0.0267(6) Uani 1 d . . H28 H 0.6874(4) 0.2718(4) 1.7909(3) 0.032 Uiso 1 calc R . C29 C 0.7676(4) 0.5001(4) 1.8484(3) 0.0261(6) Uani 1 d . . H29 H 0.7623(4) 0.5005(4) 1.9436(3) 0.031 Uiso 1 calc R . C30 C 0.8198(3) 0.6344(3) 1.7969(3) 0.0233(6) Uani 1 d . . H30 H 0.8527(3) 0.7284(3) 1.8569(3) 0.028 Uiso 1 calc R . C31 C 0.8239(3) 0.6305(3) 1.6560(3) 0.0198(5) Uani 1 d . . H31 H 0.8594(3) 0.7237(3) 1.6231(3) 0.024 Uiso 1 calc R . C32 C 0.8013(3) 0.6474(3) 1.3450(3) 0.0188(5) Uani 1 d . . C33 C 0.7052(3) 0.7143(3) 1.3933(3) 0.0199(6) Uani 1 d . . H33 H 0.6373(3) 0.6712(3) 1.4588(3) 0.024 Uiso 1 calc R . C34 C 0.7062(4) 0.8421(3) 1.3480(3) 0.0250(6) Uani 1 d . . H34 H 0.6407(4) 0.8849(3) 1.3841(3) 0.030 Uiso 1 calc R . C35 C 0.8015(4) 0.9068(3) 1.2511(3) 0.0262(6) Uani 1 d . . H35 H 0.8043(4) 0.9953(3) 1.2225(3) 0.031 Uiso 1 calc R . C36 C 0.8929(4) 0.8403(4) 1.1964(3) 0.0270(7) Uani 1 d . . H36 H 0.9570(4) 0.8817(4) 1.1281(3) 0.032 Uiso 1 calc R . C37 C 0.8906(4) 0.7122(4) 1.2419(3) 0.0242(6) Uani 1 d . . H37 H 0.9520(4) 0.6669(4) 1.2015(3) 0.029 Uiso 1 calc R . C38 C 0.9685(3) 0.4866(3) 1.3847(3) 0.0189(6) Uani 1 d . . C39 C 1.1139(3) 0.6154(3) 1.4039(3) 0.0233(6) Uani 1 d . . H39 H 1.1156(3) 0.7128(3) 1.4184(3) 0.028 Uiso 1 calc R . C40 C 1.2559(3) 0.6059(4) 1.4027(3) 0.0276(6) Uani 1 d . . H40 H 1.3519(3) 0.6963(4) 1.4162(3) 0.033 Uiso 1 calc R . C41 C 1.2592(4) 0.4672(4) 1.3820(3) 0.0296(7) Uani 1 d . . H41 H 1.3562(4) 0.4609(4) 1.3799(3) 0.036 Uiso 1 calc R . C42 C 1.1169(4) 0.3362(4) 1.3643(3) 0.0273(6) Uani 1 d . . H42 H 1.1165(4) 0.2394(4) 1.3511(3) 0.033 Uiso 1 calc R . C43 C 0.9759(3) 0.3470(3) 1.3657(3) 0.0247(6) Uani 1 d . . H43 H 0.8805(3) 0.2562(3) 1.3534(3) 0.030 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0250(2) 0.0187(2) 0.0154(2) 0.00123(12) -0.00154(13) 0.00939(15) O1 0.0180(10) 0.0215(10) 0.0392(12) 0.0022(8) 0.0022(9) 0.0060(9) N1 0.0142(10) 0.0142(11) 0.0327(13) 0.0052(9) 0.0037(9) 0.0047(9) C1 0.0194(13) 0.0190(14) 0.0167(13) 0.0029(11) 0.0005(11) 0.0089(12) C2 0.024(2) 0.027(2) 0.021(2) 0.0043(12) 0.0033(12) 0.0156(14) C3 0.042(2) 0.027(2) 0.021(2) -0.0007(12) 0.0005(14) 0.025(2) C4 0.034(2) 0.019(2) 0.021(2) -0.0012(11) -0.0068(13) 0.0128(14) C5 0.0232(15) 0.0198(14) 0.0213(15) 0.0012(11) -0.0029(12) 0.0097(13) C6 0.048(2) 0.040(2) 0.020(2) 0.0036(14) 0.009(2) 0.020(2) C7 0.055(3) 0.039(2) 0.023(2) 0.009(2) 0.012(2) 0.007(2) C8 0.080(3) 0.027(2) 0.018(2) 0.0040(13) -0.006(2) 0.025(2) C9 0.050(2) 0.034(2) 0.018(2) -0.0026(13) -0.0146(15) 0.022(2) C10 0.046(2) 0.021(2) 0.019(2) -0.0018(12) -0.0025(15) 0.015(2) C11 0.0225(13) 0.0183(13) 0.0162(11) 0.0033(9) 0.0032(10) 0.0091(11) C12 0.0204(13) 0.0145(13) 0.033(2) 0.0050(11) 0.0039(12) 0.0066(12) C13 0.043(2) 0.028(2) 0.038(2) 0.0131(15) 0.017(2) 0.019(2) C14 0.0196(13) 0.0136(12) 0.0253(13) 0.0067(10) 0.0033(11) 0.0082(11) C15 0.0293(15) 0.0194(13) 0.0260(14) 0.0052(10) 0.0006(12) 0.0125(12) C16 0.040(2) 0.026(2) 0.0280(15) 0.0084(12) 0.0099(13) 0.0188(14) C17 0.027(2) 0.031(2) 0.047(2) 0.0108(15) 0.0115(14) 0.0181(14) C18 0.0188(14) 0.0242(15) 0.042(2) 0.0034(12) -0.0028(13) 0.0102(12) C19 0.0222(13) 0.0157(12) 0.0264(14) 0.0026(10) -0.0004(11) 0.0063(11) B1 0.0171(14) 0.0143(13) 0.0180(14) 0.0025(11) 0.0015(12) 0.0051(12) C20 0.0215(13) 0.0172(12) 0.0180(12) 0.0051(9) 0.0027(10) 0.0092(11) C21 0.0218(13) 0.0287(15) 0.0197(13) 0.0013(10) 0.0033(11) 0.0088(12) C22 0.033(2) 0.037(2) 0.0172(13) -0.0056(12) -0.0013(12) 0.019(2) C23 0.0260(15) 0.0209(14) 0.031(2) -0.0037(11) -0.0112(12) 0.0112(13) C24 0.0214(14) 0.023(2) 0.029(2) 0.0058(12) 0.0015(12) 0.0067(13) C25 0.0245(14) 0.0229(14) 0.0202(13) 0.0026(10) 0.0032(10) 0.0115(12) C26 0.0161(12) 0.0198(13) 0.0182(12) 0.0039(10) 0.0013(10) 0.0095(11) C27 0.029(2) 0.0188(14) 0.0231(14) 0.0033(11) 0.0053(12) 0.0123(13) C28 0.037(2) 0.029(2) 0.0217(13) 0.0108(11) 0.0075(12) 0.0187(14) C29 0.034(2) 0.037(2) 0.0158(12) 0.0063(11) 0.0063(11) 0.0217(14) C30 0.0262(14) 0.0282(14) 0.0175(12) -0.0024(10) -0.0002(11) 0.0160(12) C31 0.0179(12) 0.0209(13) 0.0210(12) 0.0035(10) 0.0009(10) 0.0092(11) C32 0.0176(13) 0.0144(12) 0.0195(13) 0.0013(10) -0.0022(10) 0.0034(11) C33 0.0185(13) 0.0218(14) 0.0174(13) 0.0024(10) -0.0004(10) 0.0074(12) C34 0.0290(15) 0.0248(14) 0.0214(13) -0.0022(11) -0.0032(11) 0.0145(13) C35 0.031(2) 0.0148(12) 0.0299(15) 0.0048(10) -0.0070(12) 0.0084(12) C36 0.031(2) 0.024(2) 0.0238(15) 0.0106(12) 0.0046(12) 0.0078(14) C37 0.029(2) 0.025(2) 0.0212(14) 0.0063(11) 0.0062(12) 0.0137(14) C38 0.0211(13) 0.0232(14) 0.0141(12) 0.0043(10) 0.0018(10) 0.0111(12) C39 0.0239(13) 0.0275(14) 0.0168(12) 0.0038(10) 0.0015(10) 0.0099(12) C40 0.0192(13) 0.039(2) 0.0195(13) 0.0058(11) 0.0037(10) 0.0075(13) C41 0.026(2) 0.053(2) 0.0182(13) 0.0078(13) 0.0052(11) 0.025(2) C42 0.031(2) 0.033(2) 0.0237(14) 0.0055(11) 0.0024(12) 0.0194(14) C43 0.0257(14) 0.0240(14) 0.0255(14) 0.0026(11) 0.0003(12) 0.0127(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C6 2.022(4) . ? Co1 C7 2.031(4) . ? Co1 C1 2.037(3) . ? Co1 C10 2.039(3) . ? Co1 C4 2.041(3) . ? Co1 C2 2.043(3) . ? Co1 C3 2.043(3) . ? Co1 C5 2.045(3) . ? Co1 C8 2.053(4) . ? Co1 C9 2.056(3) . ? O1 C11 1.221(3) . ? N1 C11 1.349(4) . ? N1 C12 1.477(3) . ? C1 C5 1.425(4) . ? C1 C2 1.425(4) . ? C1 C11 1.499(4) . ? C2 C3 1.423(5) . ? C3 C4 1.417(5) . ? C4 C5 1.416(4) . ? C6 C7 1.407(6) . ? C6 C10 1.411(5) . ? C7 C8 1.422(6) . ? C8 C9 1.404(6) . ? C9 C10 1.433(5) . ? C12 C13 1.517(5) . ? C12 C14 1.519(4) . ? C14 C19 1.391(4) . ? C14 C15 1.398(4) . ? C15 C16 1.389(4) . ? C16 C17 1.377(5) . ? C17 C18 1.384(5) . ? C18 C19 1.384(4) . ? B1 C20 1.643(4) . ? B1 C26 1.643(4) . ? B1 C32 1.652(4) . ? B1 C38 1.657(4) . ? C20 C21 1.398(4) . ? C20 C25 1.406(4) . ? C21 C22 1.393(4) . ? C22 C23 1.385(5) . ? C23 C24 1.379(5) . ? C24 C25 1.388(4) . ? C26 C31 1.404(4) . ? C26 C27 1.412(4) . ? C27 C28 1.387(4) . ? C28 C29 1.395(4) . ? C29 C30 1.389(4) . ? C30 C31 1.399(4) . ? C32 C37 1.407(4) . ? C32 C33 1.408(4) . ? C33 C34 1.400(4) . ? C34 C35 1.383(4) . ? C35 C36 1.388(5) . ? C36 C37 1.399(4) . ? C38 C39 1.401(4) . ? C38 C43 1.406(4) . ? C39 C40 1.392(4) . ? C40 C41 1.378(5) . ? C41 C42 1.395(5) . ? C42 C43 1.389(4) . ? 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 C6 Co1 C7 40.6(2) . . ? C6 Co1 C1 113.09(14) . . ? C7 Co1 C1 142.2(2) . . ? C6 Co1 C10 40.7(2) . . ? C7 Co1 C10 68.4(2) . . ? C1 Co1 C10 110.65(13) . . ? C6 Co1 C4 136.5(2) . . ? C7 Co1 C4 110.2(2) . . ? C1 Co1 C4 68.46(13) . . ? C10 Co1 C4 176.7(2) . . ? C6 Co1 C2 142.67(15) . . ? C7 Co1 C2 176.3(2) . . ? C1 Co1 C2 40.90(12) . . ? C10 Co1 C2 113.19(14) . . ? C4 Co1 C2 68.35(14) . . ? C6 Co1 C3 176.3(2) . . ? C7 Co1 C3 136.0(2) . . ? C1 Co1 C3 68.75(13) . . ? C10 Co1 C3 142.4(2) . . ? C4 Co1 C3 40.61(14) . . ? C2 Co1 C3 40.76(13) . . ? C6 Co1 C5 110.52(15) . . ? C7 Co1 C5 112.6(2) . . ? C1 Co1 C5 40.87(12) . . ? C10 Co1 C5 136.81(14) . . ? C4 Co1 C5 40.55(13) . . ? C2 Co1 C5 68.65(13) . . ? C3 Co1 C5 68.56(14) . . ? C6 Co1 C8 68.3(2) . . ? C7 Co1 C8 40.8(2) . . ? C1 Co1 C8 176.6(2) . . ? C10 Co1 C8 68.20(15) . . ? C4 Co1 C8 112.87(14) . . ? C2 Co1 C8 136.2(2) . . ? C3 Co1 C8 110.07(15) . . ? C5 Co1 C8 142.1(2) . . ? C6 Co1 C9 68.4(2) . . ? C7 Co1 C9 68.1(2) . . ? C1 Co1 C9 137.16(14) . . ? C10 Co1 C9 40.96(14) . . ? C4 Co1 C9 141.74(14) . . ? C2 Co1 C9 110.7(2) . . ? C3 Co1 C9 112.7(2) . . ? C5 Co1 C9 177.5(2) . . ? C8 Co1 C9 40.0(2) . . ? C11 N1 C12 120.5(2) . . ? C5 C1 C2 107.9(3) . . ? C5 C1 C11 130.2(3) . . ? C2 C1 C11 121.9(3) . . ? C5 C1 Co1 69.9(2) . . ? C2 C1 Co1 69.8(2) . . ? C11 C1 Co1 127.0(2) . . ? C3 C2 C1 107.9(3) . . ? C3 C2 Co1 69.6(2) . . ? C1 C2 Co1 69.3(2) . . ? C4 C3 C2 107.7(3) . . ? C4 C3 Co1 69.6(2) . . ? C2 C3 Co1 69.6(2) . . ? C5 C4 C3 108.7(3) . . ? C5 C4 Co1 69.9(2) . . ? C3 C4 Co1 69.8(2) . . ? C4 C5 C1 107.7(3) . . ? C4 C5 Co1 69.6(2) . . ? C1 C5 Co1 69.3(2) . . ? C7 C6 C10 108.6(4) . . ? C7 C6 Co1 70.0(2) . . ? C10 C6 Co1 70.3(2) . . ? C6 C7 C8 107.9(4) . . ? C6 C7 Co1 69.4(2) . . ? C8 C7 Co1 70.5(2) . . ? C9 C8 C7 108.2(3) . . ? C9 C8 Co1 70.1(2) . . ? C7 C8 Co1 68.8(2) . . ? C8 C9 C10 107.9(3) . . ? C8 C9 Co1 69.9(2) . . ? C10 C9 Co1 68.9(2) . . ? C6 C10 C9 107.4(3) . . ? C6 C10 Co1 69.0(2) . . ? C9 C10 Co1 70.1(2) . . ? O1 C11 N1 123.1(2) . . ? O1 C11 C1 120.5(3) . . ? N1 C11 C1 116.4(2) . . ? N1 C12 C13 110.5(3) . . ? N1 C12 C14 108.9(2) . . ? C13 C12 C14 114.3(3) . . ? C19 C14 C15 118.6(3) . . ? C19 C14 C12 122.6(3) . . ? C15 C14 C12 118.9(3) . . ? C16 C15 C14 120.7(3) . . ? C17 C16 C15 119.7(3) . . ? C16 C17 C18 120.2(3) . . ? C17 C18 C19 120.3(3) . . ? C18 C19 C14 120.5(3) . . ? C20 B1 C26 112.8(2) . . ? C20 B1 C32 106.0(2) . . ? C26 B1 C32 112.7(2) . . ? C20 B1 C38 109.9(2) . . ? C26 B1 C38 103.8(2) . . ? C32 B1 C38 111.9(2) . . ? C21 C20 C25 115.1(2) . . ? C21 C20 B1 121.2(2) . . ? C25 C20 B1 123.6(2) . . ? C22 C21 C20 122.8(3) . . ? C23 C22 C21 120.0(3) . . ? C24 C23 C22 119.2(3) . . ? C23 C24 C25 120.0(3) . . ? C24 C25 C20 122.9(3) . . ? C31 C26 C27 114.5(3) . . ? C31 C26 B1 123.0(2) . . ? C27 C26 B1 122.1(3) . . ? C28 C27 C26 122.8(3) . . ? C27 C28 C29 120.8(3) . . ? C30 C29 C28 118.5(3) . . ? C29 C30 C31 119.7(3) . . ? C30 C31 C26 123.8(3) . . ? C37 C32 C33 115.2(3) . . ? C37 C32 B1 122.4(2) . . ? C33 C32 B1 122.3(2) . . ? C34 C33 C32 122.2(3) . . ? C35 C34 C33 120.7(3) . . ? C34 C35 C36 119.0(3) . . ? C35 C36 C37 119.9(3) . . ? C36 C37 C32 122.9(3) . . ? C39 C38 C43 115.4(3) . . ? C39 C38 B1 123.0(3) . . ? C43 C38 B1 121.4(3) . . ? C40 C39 C38 122.4(3) . . ? C41 C40 C39 120.8(3) . . ? C40 C41 C42 118.5(3) . . ? C43 C42 C41 120.2(3) . . ? C42 C43 C38 122.7(3) . . ? _refine_diff_density_max 0.679 _refine_diff_density_min -0.478 _refine_diff_density_rms 0.066 #===END data_6a _database_code_CSD 180592 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32 H32 Fe N2 O6' _chemical_formula_weight 596.45 _chemical_melting_point ? _chemical_compound_source ? 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Hexagonal' _symmetry_space_group_name_H-M 'P6(5)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' '-x, -y, z+1/2' 'y, -x+y, z+1/6' 'x-y, x, z+5/6' _cell_length_a 22.3320(15) _cell_length_b 22.3320(15) _cell_length_c 10.3690(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4478.4(5) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7937 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent column' _exptl_crystal_colour 'yellow brown' _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method ? _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 0.551 _exptl_absorpt_correction_type 'SADABS, G.M. Sheldrick 1994' _exptl_absorpt_correction_T_min 0.674 _exptl_absorpt_correction_T_max 0.900 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Siemens SMART CCD-Detector' _diffrn_measurement_method '\w-scan, 0.3 deg./frame' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18926 _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_av_sigmaI/netI 0.0723 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4980 _reflns_number_observed 3953 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SAINT 5' _computing_cell_refinement 'Siemens SAINT 5' _computing_data_reduction 'Siemens SAINT 5' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 6 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0880P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 4974 _refine_ls_number_parameters 372 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0742 _refine_ls_R_factor_obs 0.0532 _refine_ls_wR_factor_all 0.1567 _refine_ls_wR_factor_obs 0.1337 _refine_ls_goodness_of_fit_all 1.039 _refine_ls_goodness_of_fit_obs 1.097 _refine_ls_restrained_S_all 1.138 _refine_ls_restrained_S_obs 1.097 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.34833(4) 0.10786(4) 0.04523(7) 0.0242(2) Uani 1 d . . C1 C 0.3190(3) 0.1755(3) -0.0199(5) 0.0283(13) Uani 1 d . . H1 H 0.3353(3) 0.2031(3) -0.0955(5) 0.034 Uiso 1 calc R . C2 C 0.2606(3) 0.1085(3) -0.0115(6) 0.0359(14) Uani 1 d . . H2 H 0.2305(3) 0.0833(3) -0.0804(6) 0.043 Uiso 1 calc R . C3 C 0.2549(3) 0.0855(3) 0.1185(5) 0.0314(13) Uani 1 d . . H3 H 0.2206(3) 0.0419(3) 0.1509(5) 0.038 Uiso 1 calc R . C4 C 0.3088(3) 0.1383(3) 0.1905(5) 0.0281(12) Uani 1 d . . H4 H 0.3170(3) 0.1369(3) 0.2801(5) 0.034 Uiso 1 calc R . C5 C 0.3488(2) 0.1942(3) 0.1052(5) 0.0231(12) Uani 1 d . . O6 O 0.4235(2) 0.3147(2) 0.0763(3) 0.0258(8) Uani 1 d . . C6 C 0.4113(2) 0.2618(2) 0.1359(5) 0.0194(11) Uani 1 d . . N7 N 0.4523(2) 0.2633(2) 0.2311(4) 0.0220(9) Uani 1 d . . H7 H 0.4396(2) 0.2264(2) 0.2792(4) 0.026 Uiso 1 calc R . C8 C 0.5185(3) 0.3263(3) 0.2556(5) 0.0240(12) Uani 1 d . . H8 H 0.5103(3) 0.3660(3) 0.2680(5) 0.029 Uiso 1 calc R . O9 O 0.5663(2) 0.2972(2) 0.0718(4) 0.0340(9) Uani 1 d . . C9 C 0.5661(3) 0.3409(3) 0.1398(5) 0.0272(12) Uani 1 d . . O10 O 0.6098(2) 0.4084(2) 0.1292(4) 0.0358(10) Uani 1 d . . C11 C 0.6617(3) 0.4283(3) 0.0280(6) 0.048(2) Uani 1 d . . H11A H 0.6991(10) 0.4209(19) 0.0583(15) 0.072 Uiso 1 calc R . H11B H 0.6806(15) 0.4772(6) 0.0068(27) 0.072 Uiso 1 calc R . H11C H 0.6404(5) 0.4001(14) -0.0490(14) 0.072 Uiso 1 calc R . C12 C 0.5543(2) 0.3189(3) 0.3754(5) 0.0229(11) Uani 1 d . . H12A H 0.5523(2) 0.2736(3) 0.3718(5) 0.027 Uiso 1 calc R . H12B H 0.6036(2) 0.3554(3) 0.3735(5) 0.027 Uiso 1 calc R . C13 C 0.5229(3) 0.3239(3) 0.5025(5) 0.0256(12) Uani 1 d . . C14 C 0.5596(3) 0.3806(3) 0.5825(5) 0.0297(13) Uani 1 d . . H14 H 0.6032(3) 0.4172(3) 0.5545(5) 0.036 Uiso 1 calc R . C15 C 0.5349(3) 0.3855(3) 0.7010(6) 0.0398(15) Uani 1 d . . H15 H 0.5616(3) 0.4245(3) 0.7545(6) 0.048 Uiso 1 calc R . C16 C 0.4699(3) 0.3326(3) 0.7427(6) 0.0387(15) Uani 1 d . . H16 H 0.4521(3) 0.3355(3) 0.8243(6) 0.046 Uiso 1 calc R . C17 C 0.4326(3) 0.2767(3) 0.6635(6) 0.0377(15) Uani 1 d . . H17 H 0.3882(3) 0.2413(3) 0.6905(6) 0.045 Uiso 1 calc R . C18 C 0.4581(3) 0.2707(3) 0.5451(6) 0.0309(12) Uani 1 d . . H18 H 0.4320(3) 0.2310(3) 0.4931(6) 0.037 Uiso 1 calc R . C21 C 0.3556(3) 0.0210(3) 0.0679(5) 0.0323(13) Uani 1 d . . H21 H 0.3211(3) -0.0209(3) 0.1055(5) 0.039 Uiso 1 calc R . C22 C 0.3622(3) 0.0384(3) -0.0651(5) 0.0354(14) Uani 1 d . . H22 H 0.3331(3) 0.0098(3) -0.1324(5) 0.043 Uiso 1 calc R . C23 C 0.4205(3) 0.1065(3) -0.0801(5) 0.0333(14) Uani 1 d . . H23 H 0.4365(3) 0.1310(3) -0.1591(5) 0.040 Uiso 1 calc R . C24 C 0.4497(3) 0.1308(3) 0.0413(5) 0.0266(11) Uani 1 d . . H24 H 0.4890(3) 0.1746(3) 0.0590(5) 0.032 Uiso 1 calc R . C25 C 0.4102(3) 0.0780(3) 0.1348(5) 0.0267(12) Uani 1 d . . O26 O 0.4568(2) 0.1463(2) 0.3241(3) 0.0247(8) Uani 1 d . . C26 C 0.4190(3) 0.0885(3) 0.2778(5) 0.0239(12) Uani 1 d . . N27 N 0.3826(2) 0.0315(2) 0.3505(4) 0.0244(10) Uani 1 d . . H27 H 0.3576(2) -0.0091(2) 0.3137(4) 0.029 Uiso 1 calc R . C28 C 0.3850(3) 0.0377(3) 0.4900(5) 0.0225(11) Uani 1 d . . H28 H 0.4030(3) 0.0873(3) 0.5129(5) 0.027 Uiso 1 calc R . C29 C 0.4325(2) 0.0150(2) 0.5473(5) 0.0241(11) Uani 1 d . . O29 O 0.4445(2) -0.0272(2) 0.5031(4) 0.0362(9) Uani 1 d . . O30 O 0.4585(2) 0.0484(2) 0.6583(4) 0.0353(9) Uani 1 d . . C31 C 0.5030(3) 0.0293(3) 0.7283(6) 0.0408(15) Uani 1 d . . H31A H 0.5082(16) 0.0457(17) 0.8175(11) 0.061 Uiso 1 calc R . H31B H 0.5484(7) 0.0505(16) 0.6867(22) 0.061 Uiso 1 calc R . H31C H 0.4822(10) -0.0211(3) 0.7278(32) 0.061 Uiso 1 calc R . C32 C 0.3118(2) -0.0059(3) 0.5490(5) 0.0278(11) Uani 1 d . . H32A H 0.2874(2) -0.0512(3) 0.5047(5) 0.033 Uiso 1 calc R . H32B H 0.3162(2) -0.0146(3) 0.6412(5) 0.033 Uiso 1 calc R . C33 C 0.2690(3) 0.0294(3) 0.5375(5) 0.0277(12) Uani 1 d . . C34 C 0.2192(3) 0.0107(3) 0.4417(5) 0.0293(13) Uani 1 d . . H34 H 0.2109(3) -0.0254(3) 0.3832(5) 0.035 Uiso 1 calc R . C35 C 0.1818(3) 0.0445(3) 0.4315(5) 0.0367(14) Uani 1 d . . H35 H 0.1483(3) 0.0318(3) 0.3652(5) 0.044 Uiso 1 calc R . C36 C 0.1927(3) 0.0966(3) 0.5170(6) 0.0379(15) Uani 1 d . . H36 H 0.1667(3) 0.1195(3) 0.5105(6) 0.045 Uiso 1 calc R . C37 C 0.2421(3) 0.1147(3) 0.6118(6) 0.0401(15) Uani 1 d . . H37 H 0.2503(3) 0.1505(3) 0.6709(6) 0.048 Uiso 1 calc R . C38 C 0.2790(3) 0.0818(3) 0.6211(6) 0.0365(14) Uani 1 d . . H38 H 0.3128(3) 0.0951(3) 0.6872(6) 0.044 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0273(4) 0.0235(4) 0.0187(4) 0.0008(3) -0.0007(3) 0.0104(3) C1 0.028(3) 0.025(3) 0.033(3) 0.004(2) -0.001(2) 0.014(3) C2 0.033(3) 0.043(4) 0.030(3) -0.003(3) -0.007(3) 0.018(3) C3 0.023(3) 0.033(3) 0.035(3) 0.003(3) 0.002(3) 0.011(3) C4 0.026(3) 0.034(3) 0.027(3) 0.002(2) 0.004(2) 0.017(3) C5 0.019(3) 0.029(3) 0.025(3) 0.005(2) 0.002(2) 0.015(2) O6 0.028(2) 0.030(2) 0.022(2) 0.001(2) 0.000(2) 0.017(2) C6 0.022(3) 0.024(3) 0.016(3) 0.003(2) 0.005(2) 0.015(2) N7 0.022(2) 0.017(2) 0.025(2) 0.005(2) 0.002(2) 0.008(2) C8 0.023(3) 0.022(3) 0.026(3) 0.001(2) 0.002(2) 0.010(2) O9 0.036(2) 0.027(2) 0.039(2) -0.004(2) 0.008(2) 0.016(2) C9 0.022(3) 0.031(3) 0.028(3) 0.002(3) -0.001(2) 0.012(3) O10 0.032(2) 0.022(2) 0.041(2) 0.002(2) 0.017(2) 0.004(2) C11 0.042(4) 0.031(3) 0.054(4) 0.003(3) 0.032(3) 0.006(3) C12 0.020(2) 0.023(3) 0.022(3) 0.000(2) -0.001(2) 0.009(2) C13 0.029(3) 0.032(3) 0.023(3) 0.002(2) -0.002(2) 0.020(3) C14 0.038(3) 0.025(3) 0.026(3) 0.004(2) 0.001(2) 0.016(3) C15 0.064(4) 0.040(3) 0.027(3) -0.006(3) -0.003(3) 0.035(3) C16 0.043(4) 0.053(4) 0.024(3) 0.002(3) 0.008(3) 0.027(3) C17 0.024(3) 0.058(4) 0.029(3) 0.007(3) 0.007(2) 0.019(3) C18 0.025(3) 0.035(3) 0.026(3) 0.001(3) -0.004(3) 0.010(2) C21 0.042(3) 0.020(3) 0.031(4) -0.003(2) 0.002(3) 0.012(3) C22 0.052(4) 0.027(3) 0.025(3) -0.004(2) 0.001(3) 0.018(3) C23 0.044(3) 0.035(3) 0.025(3) 0.003(2) 0.011(3) 0.023(3) C24 0.029(3) 0.030(3) 0.023(3) 0.003(3) 0.005(3) 0.016(2) C25 0.030(3) 0.028(3) 0.021(3) 0.004(2) 0.001(2) 0.014(2) O26 0.033(2) 0.019(2) 0.021(2) 0.0003(15) -0.003(2) 0.012(2) C26 0.026(3) 0.026(3) 0.027(3) 0.005(2) 0.001(2) 0.019(3) N27 0.029(2) 0.021(2) 0.020(2) 0.001(2) 0.002(2) 0.010(2) C28 0.024(3) 0.021(3) 0.020(3) -0.003(2) 0.000(2) 0.009(2) C29 0.022(3) 0.020(3) 0.021(3) 0.005(2) 0.001(2) 0.004(2) O29 0.043(2) 0.040(2) 0.033(2) -0.006(2) -0.003(2) 0.027(2) O30 0.047(2) 0.040(2) 0.028(2) -0.008(2) -0.011(2) 0.030(2) C31 0.047(4) 0.042(4) 0.041(4) -0.004(3) -0.023(3) 0.028(3) C32 0.029(3) 0.030(3) 0.022(3) 0.005(2) 0.002(2) 0.013(2) C33 0.028(3) 0.029(3) 0.021(3) 0.006(3) 0.008(2) 0.010(2) C34 0.028(3) 0.035(3) 0.021(3) 0.003(2) 0.001(2) 0.012(3) C35 0.036(3) 0.051(4) 0.027(3) 0.006(3) -0.002(3) 0.025(3) C36 0.033(3) 0.040(3) 0.045(4) 0.013(3) 0.007(3) 0.021(3) C37 0.046(4) 0.041(4) 0.039(4) -0.007(3) -0.008(3) 0.025(3) C38 0.035(3) 0.045(4) 0.032(3) -0.012(3) -0.009(3) 0.021(3) _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 C5 2.020(5) . ? Fe1 C4 2.028(5) . ? Fe1 C25 2.033(5) . ? Fe1 C3 2.034(5) . ? Fe1 C21 2.039(5) . ? Fe1 C1 2.039(5) . ? Fe1 C2 2.052(6) . ? Fe1 C24 2.057(5) . ? Fe1 C22 2.073(5) . ? Fe1 C23 2.083(5) . ? C1 C2 1.411(8) . ? C1 C5 1.422(7) . ? C2 C3 1.425(8) . ? C3 C4 1.407(7) . ? C4 C5 1.422(7) . ? C5 C6 1.492(7) . ? O6 C6 1.238(5) . ? C6 N7 1.335(6) . ? N7 C8 1.467(6) . ? C8 C9 1.527(7) . ? C8 C12 1.531(7) . ? O9 C9 1.205(6) . ? C9 O10 1.330(6) . ? O10 C11 1.459(6) . ? C12 C13 1.523(7) . ? C13 C14 1.388(7) . ? C13 C18 1.407(7) . ? C14 C15 1.374(8) . ? C15 C16 1.405(8) . ? C16 C17 1.374(8) . ? C17 C18 1.388(8) . ? C21 C22 1.420(8) . ? C21 C25 1.426(7) . ? C22 C23 1.433(8) . ? C23 C24 1.397(8) . ? C24 C25 1.439(7) . ? C25 C26 1.498(7) . ? O26 C26 1.232(6) . ? C26 N27 1.348(6) . ? N27 C28 1.452(7) . ? C28 C29 1.507(7) . ? C28 C32 1.550(7) . ? C29 O29 1.193(6) . ? C29 O30 1.336(6) . ? O30 C31 1.455(6) . ? C32 C33 1.517(7) . ? C33 C38 1.382(7) . ? C33 C34 1.391(7) . ? C34 C35 1.381(8) . ? C35 C36 1.384(8) . ? C36 C37 1.378(8) . ? C37 C38 1.354(8) . ? 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 C5 Fe1 C4 41.1(2) . . ? C5 Fe1 C25 119.5(2) . . ? C4 Fe1 C25 104.6(2) . . ? C5 Fe1 C3 68.6(2) . . ? C4 Fe1 C3 40.5(2) . . ? C25 Fe1 C3 122.0(2) . . ? C5 Fe1 C21 155.1(2) . . ? C4 Fe1 C21 119.2(2) . . ? C25 Fe1 C21 41.0(2) . . ? C3 Fe1 C21 106.4(2) . . ? C5 Fe1 C1 41.0(2) . . ? C4 Fe1 C1 69.0(2) . . ? C25 Fe1 C1 156.5(2) . . ? C3 Fe1 C1 68.6(2) . . ? C21 Fe1 C1 161.9(2) . . ? C5 Fe1 C2 68.3(2) . . ? C4 Fe1 C2 68.5(2) . . ? C25 Fe1 C2 160.1(2) . . ? C3 Fe1 C2 40.8(2) . . ? C21 Fe1 C2 124.8(2) . . ? C1 Fe1 C2 40.4(2) . . ? C5 Fe1 C24 106.8(2) . . ? C4 Fe1 C24 122.8(2) . . ? C25 Fe1 C24 41.2(2) . . ? C3 Fe1 C24 159.2(2) . . ? C21 Fe1 C24 68.8(2) . . ? C1 Fe1 C24 122.1(2) . . ? C2 Fe1 C24 158.2(2) . . ? C5 Fe1 C22 162.4(2) . . ? C4 Fe1 C22 156.1(2) . . ? C25 Fe1 C22 68.1(2) . . ? C3 Fe1 C22 122.8(2) . . ? C21 Fe1 C22 40.4(2) . . ? C1 Fe1 C22 126.6(2) . . ? C2 Fe1 C22 110.4(2) . . ? C24 Fe1 C22 67.5(2) . . ? C5 Fe1 C23 124.8(2) . . ? C4 Fe1 C23 159.8(2) . . ? C25 Fe1 C23 67.9(2) . . ? C3 Fe1 C23 159.3(2) . . ? C21 Fe1 C23 68.1(2) . . ? C1 Fe1 C23 110.0(2) . . ? C2 Fe1 C23 124.7(2) . . ? C24 Fe1 C23 39.4(2) . . ? C22 Fe1 C23 40.3(2) . . ? C2 C1 C5 107.7(5) . . ? C2 C1 Fe1 70.3(3) . . ? C5 C1 Fe1 68.8(3) . . ? C1 C2 C3 108.0(5) . . ? C1 C2 Fe1 69.3(3) . . ? C3 C2 Fe1 68.9(3) . . ? C4 C3 C2 108.3(5) . . ? C4 C3 Fe1 69.5(3) . . ? C2 C3 Fe1 70.3(3) . . ? C3 C4 C5 107.7(5) . . ? C3 C4 Fe1 70.0(3) . . ? C5 C4 Fe1 69.1(3) . . ? C1 C5 C4 108.3(4) . . ? C1 C5 C6 123.8(5) . . ? C4 C5 C6 127.9(5) . . ? C1 C5 Fe1 70.2(3) . . ? C4 C5 Fe1 69.7(3) . . ? C6 C5 Fe1 125.9(3) . . ? O6 C6 N7 121.7(4) . . ? O6 C6 C5 120.5(4) . . ? N7 C6 C5 117.8(4) . . ? C6 N7 C8 120.1(4) . . ? N7 C8 C9 109.2(4) . . ? N7 C8 C12 111.5(4) . . ? C9 C8 C12 108.4(4) . . ? O9 C9 O10 124.9(5) . . ? O9 C9 C8 124.9(5) . . ? O10 C9 C8 110.1(4) . . ? C9 O10 C11 115.2(4) . . ? C13 C12 C8 114.2(4) . . ? C14 C13 C18 118.1(5) . . ? C14 C13 C12 120.0(5) . . ? C18 C13 C12 121.8(5) . . ? C15 C14 C13 122.0(5) . . ? C14 C15 C16 119.8(5) . . ? C17 C16 C15 118.8(5) . . ? C16 C17 C18 121.6(5) . . ? C17 C18 C13 119.7(5) . . ? C22 C21 C25 107.7(5) . . ? C22 C21 Fe1 71.1(3) . . ? C25 C21 Fe1 69.3(3) . . ? C21 C22 C23 108.1(5) . . ? C21 C22 Fe1 68.5(3) . . ? C23 C22 Fe1 70.2(3) . . ? C24 C23 C22 108.3(5) . . ? C24 C23 Fe1 69.3(3) . . ? C22 C23 Fe1 69.5(3) . . ? C23 C24 C25 108.2(5) . . ? C23 C24 Fe1 71.3(3) . . ? C25 C24 Fe1 68.5(3) . . ? C21 C25 C24 107.7(5) . . ? C21 C25 C26 127.5(5) . . ? C24 C25 C26 124.0(5) . . ? C21 C25 Fe1 69.7(3) . . ? C24 C25 Fe1 70.3(3) . . ? C26 C25 Fe1 117.3(4) . . ? O26 C26 N27 123.0(5) . . ? O26 C26 C25 121.2(5) . . ? N27 C26 C25 115.8(5) . . ? C26 N27 C28 119.5(4) . . ? N27 C28 C29 111.1(4) . . ? N27 C28 C32 110.9(4) . . ? C29 C28 C32 109.4(4) . . ? O29 C29 O30 124.4(5) . . ? O29 C29 C28 126.0(5) . . ? O30 C29 C28 109.6(4) . . ? C29 O30 C31 115.9(4) . . ? C33 C32 C28 112.5(4) . . ? C38 C33 C34 118.0(5) . . ? C38 C33 C32 120.9(5) . . ? C34 C33 C32 121.1(5) . . ? C35 C34 C33 120.1(5) . . ? C34 C35 C36 120.7(5) . . ? C37 C36 C35 118.8(5) . . ? C38 C37 C36 120.5(6) . . ? C37 C38 C33 122.0(5) . . ? _refine_diff_density_max 1.189 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.097 #===END data_7a _database_code_CSD 180593 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[C38 H42 Fe N4 O8], 0.5 CHCl3' _chemical_formula_analytical ? _chemical_formula_sum 'C38.50 H42.50 Cl1.50 Fe N4 O8' _chemical_formula_weight 798.29 _chemical_melting_point ? _chemical_compound_source ? 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' '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)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.7711(8) _cell_length_b 16.4209(10) _cell_length_c 18.2693(12) _cell_angle_alpha 90.00 _cell_angle_beta 93.44(1) _cell_angle_gamma 90.00 _cell_volume 3824.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12820 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent needle' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method ? _exptl_crystal_F_000 1668 _exptl_absorpt_coefficient_mu 0.556 _exptl_absorpt_correction_type 'DelrefAbs, Platon99 prog. suite, A.L. Spek' _exptl_absorpt_correction_T_min 0.424 _exptl_absorpt_correction_T_max 0.873 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Nonius KappaCCD' _diffrn_measurement_method '312 images a 1 deg. \w / 190 sec.' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22378 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 26.00 _reflns_number_total 14133 _reflns_number_observed 12397 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'DENZO, Nonius Collect Software' _computing_cell_refinement 'DENZO, Nonius Collect Software' _computing_data_reduction 'DENZO, Nonius Collect Software' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 37 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+2.7754P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.012(14) _refine_ls_number_reflns 14096 _refine_ls_number_parameters 986 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_obs 0.0516 _refine_ls_wR_factor_all 0.1551 _refine_ls_wR_factor_obs 0.1266 _refine_ls_goodness_of_fit_all 1.022 _refine_ls_goodness_of_fit_obs 1.030 _refine_ls_restrained_S_all 1.247 _refine_ls_restrained_S_obs 1.121 _refine_ls_shift/esd_max 0.006 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.21163(4) 0.57702(4) 0.68209(3) 0.02464(13) Uani 1 d . . O1 O 0.0728(2) 0.3799(2) 0.6193(2) 0.0299(6) Uani 1 d . . O2 O 0.1030(2) 0.4881(2) 0.45146(14) 0.0265(6) Uani 1 d . . O3 O 0.0207(2) 0.4842(2) 0.2785(2) 0.0425(8) Uani 1 d . . O4 O 0.1928(2) 0.4621(2) 0.2769(2) 0.0400(8) Uani 1 d . . O5 O 0.1409(2) 0.7660(2) 0.5719(2) 0.0291(6) Uani 1 d . . O6 O -0.0925(2) 0.6534(2) 0.54611(15) 0.0290(6) Uani 1 d . . O7 O -0.3194(2) 0.6508(2) 0.4370(2) 0.0408(8) Uani 1 d . . O8 O -0.3602(2) 0.6671(2) 0.5533(2) 0.0420(8) Uani 1 d . . N1 N -0.0198(2) 0.4863(2) 0.5703(2) 0.0257(7) Uani 1 d . . H1N H -0.0413(2) 0.5368(2) 0.5758(2) 0.031 Uiso 1 calc R . N2 N 0.0206(3) 0.3793(2) 0.4009(2) 0.0272(7) Uani 1 d . . H2N H -0.0328(3) 0.3454(2) 0.4008(2) 0.033 Uiso 1 calc R . N3 N 0.1065(2) 0.6589(2) 0.4970(2) 0.0241(7) Uani 1 d . . H3N H 0.1231(2) 0.6089(2) 0.4848(2) 0.029 Uiso 1 calc R . N4 N -0.1473(2) 0.7574(2) 0.4738(2) 0.0267(7) Uani 1 d . . H4N H -0.1334(2) 0.7910(2) 0.4381(2) 0.032 Uiso 1 calc R . N5 N 0.5858(2) 0.5774(2) 0.9898(2) 0.0259(7) Uani 1 d . . H5N H 0.5875(2) 0.5255(2) 0.9776(2) 0.031 Uiso 1 calc R . N6 N 0.3375(3) 0.6823(2) 1.0061(2) 0.0364(9) Uani 1 d . . H6N H 0.3509(3) 0.7219(2) 0.9755(2) 0.044 Uiso 1 calc R . N7 N 0.4765(3) 0.4064(2) 1.0709(2) 0.0293(8) Uani 1 d . . H7N H 0.4597(3) 0.4558(2) 1.0846(2) 0.035 Uiso 1 calc R . N8 N 0.4410(3) 0.3138(2) 0.8910(2) 0.0325(8) Uani 1 d . . H8N H 0.3890(3) 0.2815(2) 0.9016(2) 0.039 Uiso 1 calc R . C1 C 0.3475(3) 0.5413(3) 0.6373(2) 0.0281(9) Uani 1 d . . H1 H 0.3806(3) 0.4896(3) 0.6426(2) 0.034 Uiso 1 calc R . C2 C 0.2700(3) 0.5636(3) 0.5819(2) 0.0251(8) Uani 1 d . . H2 H 0.2423(3) 0.5295(3) 0.5435(2) 0.030 Uiso 1 calc R . C3 C 0.2410(3) 0.6462(2) 0.5940(2) 0.0232(8) Uani 1 d . . C4 C 0.3016(3) 0.6747(3) 0.6571(2) 0.0287(9) Uani 1 d . . H4 H 0.2986(3) 0.7276(3) 0.6778(2) 0.034 Uiso 1 calc R . C5 C 0.3668(3) 0.6104(3) 0.6833(2) 0.0304(9) Uani 1 d . . H5 H 0.4154(3) 0.6127(3) 0.7248(2) 0.036 Uiso 1 calc R . C6 C 0.0558(3) 0.5874(3) 0.6986(2) 0.0263(8) Uani 1 d . . H6 H 0.0063(3) 0.6198(3) 0.6708(2) 0.032 Uiso 1 calc R . C7 C 0.0833(3) 0.5047(3) 0.6835(2) 0.0262(8) Uani 1 d . . C8 C 0.1600(3) 0.4796(3) 0.7389(2) 0.0291(8) Uani 1 d . . H8 H 0.1921(3) 0.4275(3) 0.7429(2) 0.035 Uiso 1 calc R . C9 C 0.1800(3) 0.5464(3) 0.7870(2) 0.0322(10) Uani 1 d . . H9 H 0.2283(3) 0.5468(3) 0.8286(2) 0.039 Uiso 1 calc R . C10 C 0.1157(3) 0.6124(3) 0.7625(2) 0.0311(9) Uani 1 d . . H10 H 0.1131(3) 0.6644(3) 0.7850(2) 0.037 Uiso 1 calc R . C11 C 0.0459(3) 0.4524(2) 0.6225(2) 0.0240(8) Uani 1 d . . C12 C -0.0552(3) 0.4411(3) 0.5057(2) 0.0256(8) Uani 1 d . . H12 H -0.0691(3) 0.3839(3) 0.5213(2) 0.031 Uiso 1 calc R . C13 C -0.1559(3) 0.4749(3) 0.4712(2) 0.0360(10) Uani 1 d . . H13A H -0.2091(3) 0.4761(3) 0.5077(2) 0.054 Uiso 1 calc R . H13B H -0.1802(3) 0.4403(3) 0.4299(2) 0.054 Uiso 1 calc R . H13C H -0.1438(3) 0.5303(3) 0.4536(2) 0.054 Uiso 1 calc R . C14 C 0.0302(3) 0.4381(3) 0.4509(2) 0.0254(9) Uani 1 d . . C15 C 0.0987(3) 0.3711(3) 0.3461(2) 0.0277(9) Uani 1 d . . H15 H 0.1698(3) 0.3656(3) 0.3716(2) 0.033 Uiso 1 calc R . C16 C 0.0968(3) 0.4466(3) 0.2974(2) 0.0308(9) Uani 1 d . . C17 C 0.2022(5) 0.5288(4) 0.2263(3) 0.0573(15) Uani 1 d . . H17A H 0.2757(5) 0.5350(4) 0.2149(3) 0.086 Uiso 1 calc R . H17B H 0.1777(5) 0.5791(4) 0.2485(3) 0.086 Uiso 1 calc R . H17C H 0.1594(5) 0.5175(4) 0.1811(3) 0.086 Uiso 1 calc R . C18 C 0.0740(4) 0.2941(3) 0.3015(3) 0.0408(11) Uani 1 d . . H18A H 0.0690(4) 0.2478(3) 0.3358(3) 0.049 Uiso 1 calc R . H18B H 0.0043(4) 0.3008(3) 0.2754(3) 0.049 Uiso 1 calc R . C19 C 0.1525(4) 0.2723(3) 0.2458(3) 0.0399(11) Uani 1 d . . C20 C 0.2589(4) 0.2706(4) 0.2627(3) 0.0561(15) Uani 1 d . . H20 H 0.2848(4) 0.2842(4) 0.3109(3) 0.067 Uiso 1 calc R . C21 C 0.3289(5) 0.2495(4) 0.2111(4) 0.069(2) Uani 1 d . . H21 H 0.4022(5) 0.2503(4) 0.2233(4) 0.083 Uiso 1 calc R . C22 C 0.2915(6) 0.2273(4) 0.1418(3) 0.066(2) Uani 1 d . . H22 H 0.3395(6) 0.2145(4) 0.1058(3) 0.079 Uiso 1 calc R . C23 C 0.1862(6) 0.2235(4) 0.1243(3) 0.068(2) Uani 1 d . . H23 H 0.1610(6) 0.2045(4) 0.0774(3) 0.082 Uiso 1 calc R . C24 C 0.1159(5) 0.2475(4) 0.1753(3) 0.060(2) Uani 1 d . . H24 H 0.0427(5) 0.2471(4) 0.1625(3) 0.072 Uiso 1 calc R . C25 C 0.1582(3) 0.6947(2) 0.5543(2) 0.0233(8) Uani 1 d . . C26 C 0.0241(3) 0.7009(3) 0.4551(2) 0.0260(9) Uani 1 d . . H26 H 0.0467(3) 0.7586(3) 0.4483(2) 0.031 Uiso 1 calc R . C27 C 0.0051(3) 0.6623(3) 0.3793(2) 0.0314(9) Uani 1 d . . H27A H 0.0706(3) 0.6625(3) 0.3539(2) 0.047 Uiso 1 calc R . H27B H -0.0484(3) 0.6935(3) 0.3507(2) 0.047 Uiso 1 calc R . H27C H -0.0189(3) 0.6060(3) 0.3847(2) 0.047 Uiso 1 calc R . C28 C -0.0767(3) 0.7015(3) 0.4963(2) 0.0258(9) Uani 1 d . . C29 C -0.2462(3) 0.7632(3) 0.5077(2) 0.0255(8) Uani 1 d . . H29 H -0.2319(3) 0.7691(3) 0.5618(2) 0.031 Uiso 1 calc R . C30 C -0.3111(3) 0.6868(3) 0.4932(2) 0.0286(9) Uani 1 d . . C31 C -0.4332(4) 0.5990(4) 0.5450(4) 0.061(2) Uani 1 d . . H31A H -0.4651(4) 0.5892(4) 0.5917(4) 0.091 Uiso 1 calc R . H31B H -0.3953(4) 0.5501(4) 0.5308(4) 0.091 Uiso 1 calc R . H31C H -0.4881(4) 0.6119(4) 0.5070(4) 0.091 Uiso 1 calc R . C32 C -0.3055(3) 0.8394(3) 0.4786(2) 0.0296(9) Uani 1 d . . H32A H -0.2584(3) 0.8871(3) 0.4841(2) 0.035 Uiso 1 calc R . H32B H -0.3246(3) 0.8321(3) 0.4257(2) 0.035 Uiso 1 calc R . C33 C -0.4035(3) 0.8561(3) 0.5181(2) 0.0288(9) Uani 1 d . . C34 C -0.4994(4) 0.8245(3) 0.4911(3) 0.0398(11) Uani 1 d . . H34 H -0.5037(4) 0.7950(3) 0.4463(3) 0.048 Uiso 1 calc R . C35 C -0.5885(4) 0.8358(3) 0.5296(3) 0.0472(12) Uani 1 d . . H35 H -0.6538(4) 0.8146(3) 0.5107(3) 0.057 Uiso 1 calc R . C36 C -0.5833(4) 0.8774(3) 0.5948(3) 0.0453(12) Uani 1 d . . H36 H -0.6444(4) 0.8843(3) 0.6213(3) 0.054 Uiso 1 calc R . C37 C -0.4890(4) 0.9089(4) 0.6216(3) 0.0504(14) Uani 1 d . . H37 H -0.4848(4) 0.9374(4) 0.6669(3) 0.061 Uiso 1 calc R . C38 C -0.4000(4) 0.8992(3) 0.5828(3) 0.0390(11) Uani 1 d . . H38 H -0.3356(4) 0.9226(3) 0.6011(3) 0.047 Uiso 1 calc R . Fe2 Fe 0.74608(5) 0.48011(4) 1.14435(3) 0.02846(14) Uani 1 d . . O9 O 0.6690(2) 0.6822(2) 1.0487(2) 0.0291(6) Uani 1 d . . O10 O 0.4065(2) 0.5739(2) 1.06725(14) 0.0296(6) Uani 1 d . . O11 O 0.1249(3) 0.5726(3) 1.0165(3) 0.0644(11) Uani 1 d . . O12 O 0.1332(3) 0.6663(3) 0.9283(2) 0.0702(13) Uani 1 d . . O13 O 0.5801(2) 0.2966(2) 1.0911(2) 0.0358(7) Uani 1 d . . O14 O 0.5491(2) 0.4148(2) 0.9314(2) 0.0360(7) Uani 1 d . . O15 O 0.3919(3) 0.3487(2) 0.7067(2) 0.0442(8) Uani 1 d . . O16 O 0.3276(2) 0.2474(2) 0.7720(2) 0.0346(7) Uani 1 d . . C40 C 0.6860(4) 0.5114(3) 1.2421(2) 0.0363(10) Uani 1 d . . H40 H 0.6955(4) 0.5613(3) 1.2681(2) 0.044 Uiso 1 calc R . C41 C 0.7508(4) 0.4420(3) 1.2509(2) 0.0399(11) Uani 1 d . . H41 H 0.8119(4) 0.4373(3) 1.2830(2) 0.048 Uiso 1 calc R . C42 C 0.7086(4) 0.3805(3) 1.2033(2) 0.0374(10) Uani 1 d . . H42 H 0.7358(4) 0.3270(3) 1.1987(2) 0.045 Uiso 1 calc R . C43 C 0.6181(4) 0.4128(3) 1.1637(2) 0.0308(9) Uani 1 d . . C44 C 0.6039(3) 0.4946(3) 1.1878(2) 0.0318(9) Uani 1 d . . H44 H 0.5499(3) 0.5309(3) 1.1709(2) 0.038 Uiso 1 calc R . C45 C 0.8325(3) 0.5763(3) 1.1098(2) 0.0317(9) Uani 1 d . . H45 H 0.8406(3) 0.6278(3) 1.1332(2) 0.038 Uiso 1 calc R . C46 C 0.8979(3) 0.5078(3) 1.1224(2) 0.0351(10) Uani 1 d . . H46 H 0.9578(3) 0.5051(3) 1.1557(2) 0.042 Uiso 1 calc R . C47 C 0.8584(4) 0.4438(3) 1.0766(2) 0.0342(10) Uani 1 d . . H47 H 0.8878(4) 0.3908(3) 1.0741(2) 0.041 Uiso 1 calc R . C48 C 0.7685(3) 0.4714(3) 1.0352(2) 0.0283(9) Uani 1 d . . H48 H 0.7268(3) 0.4407(3) 1.0004(2) 0.034 Uiso 1 calc R . C49 C 0.7517(3) 0.5544(3) 1.0554(2) 0.0262(9) Uani 1 d . . C50 C 0.6661(3) 0.6099(2) 1.0317(2) 0.0236(8) Uani 1 d . . C51 C 0.4978(3) 0.6265(3) 0.9649(2) 0.0262(9) Uani 1 d . . H51 H 0.5226(3) 0.6840(3) 0.9612(2) 0.031 Uiso 1 calc R . C52 C 0.4555(4) 0.5996(3) 0.8886(2) 0.0357(10) Uani 1 d . . H52A H 0.5122(4) 0.6009(3) 0.8548(2) 0.054 Uiso 1 calc R . H52B H 0.3992(4) 0.6365(3) 0.8709(2) 0.054 Uiso 1 calc R . H52C H 0.4279(4) 0.5440(3) 0.8912(2) 0.054 Uiso 1 calc R . C53 C 0.4104(3) 0.6248(3) 1.0183(2) 0.0274(9) Uani 1 d . . C54 C 0.2382(3) 0.6834(3) 1.0398(2) 0.0301(9) Uani 1 d . . H54 H 0.2442(3) 0.6553(3) 1.0884(2) 0.036 Uiso 1 calc R . C55 C 0.1583(4) 0.6405(3) 0.9879(3) 0.0410(11) Uani 1 d . . C56 C 0.0481(6) 0.5279(5) 0.9667(5) 0.095(3) Uani 1 d . . H56A H 0.0260(6) 0.4780(5) 0.9908(5) 0.142 Uiso 1 calc R . H56B H 0.0810(6) 0.5138(5) 0.9213(5) 0.142 Uiso 1 calc R . H56C H -0.0132(6) 0.5625(5) 0.9552(5) 0.142 Uiso 1 calc R . C57 C 0.2046(4) 0.7718(3) 1.0486(3) 0.0389(11) Uani 1 d . . H57A H 0.2580(4) 0.8001(3) 1.0809(3) 0.047 Uiso 1 calc R . H57B H 0.2026(4) 0.7986(3) 1.0001(3) 0.047 Uiso 1 calc R . C58 C 0.0985(4) 0.7818(3) 1.0805(3) 0.0419(11) Uani 1 d . . C59 C 0.0059(4) 0.7749(4) 1.0370(3) 0.0442(12) Uani 1 d . . H59 H 0.0090(4) 0.7645(4) 0.9860(3) 0.053 Uiso 1 calc R . C60 C -0.0905(4) 0.7830(3) 1.0664(3) 0.0465(12) Uani 1 d . . H60 H -0.1529(4) 0.7764(3) 1.0359(3) 0.056 Uiso 1 calc R . C61 C -0.0967(4) 0.8004(4) 1.1384(3) 0.0523(14) Uani 1 d . . H61 H -0.1634(4) 0.8091(4) 1.1573(3) 0.063 Uiso 1 calc R . C62 C -0.0082(4) 0.8055(5) 1.1844(4) 0.066(2) Uani 1 d . . H62 H -0.0129(4) 0.8152(5) 1.2354(4) 0.079 Uiso 1 calc R . C63 C 0.0890(5) 0.7962(4) 1.1543(4) 0.066(2) Uani 1 d . . H63 H 0.1509(5) 0.7998(4) 1.1857(4) 0.079 Uiso 1 calc R . C64 C 0.5578(3) 0.3680(3) 1.1058(2) 0.0287(9) Uani 1 d . . C65 C 0.4159(4) 0.3674(3) 1.0108(2) 0.0323(10) Uani 1 d . . H65 H 0.4019(4) 0.3097(3) 1.0249(2) 0.039 Uiso 1 calc R . C66 C 0.3118(4) 0.4106(3) 0.9967(3) 0.0421(11) Uani 1 d . . H66A H 0.2734(4) 0.4103(3) 1.0416(3) 0.063 Uiso 1 calc R . H66B H 0.2704(4) 0.3825(3) 0.9575(3) 0.063 Uiso 1 calc R . H66C H 0.3243(4) 0.4670(3) 0.9819(3) 0.063 Uiso 1 calc R . C67 C 0.4774(3) 0.3671(3) 0.9414(2) 0.0286(9) Uani 1 d . . C68 C 0.4835(3) 0.3069(3) 0.8197(2) 0.0318(9) Uani 1 d . . H68 H 0.5294(3) 0.3552(3) 0.8122(2) 0.038 Uiso 1 calc R . C69 C 0.3975(4) 0.3054(3) 0.7592(2) 0.0310(9) Uani 1 d . . C70 C 0.2444(4) 0.2356(3) 0.7160(2) 0.0371(10) Uani 1 d . . H70A H 0.1980(4) 0.1919(3) 0.7310(2) 0.056 Uiso 1 calc R . H70B H 0.2746(4) 0.2207(3) 0.6698(2) 0.056 Uiso 1 calc R . H70C H 0.2042(4) 0.2861(3) 0.7093(2) 0.056 Uiso 1 calc R . C71 C 0.5499(4) 0.2298(3) 0.8153(2) 0.0380(11) Uani 1 d . . H71A H 0.6094(4) 0.2336(3) 0.8525(2) 0.046 Uiso 1 calc R . H71B H 0.5066(4) 0.1826(3) 0.8285(2) 0.046 Uiso 1 calc R . C72 C 0.5930(3) 0.2134(3) 0.7419(2) 0.0381(11) Uani 1 d . . C73 C 0.5574(4) 0.1476(3) 0.7006(3) 0.0453(12) Uani 1 d . . H73 H 0.5043(4) 0.1136(3) 0.7183(3) 0.054 Uiso 1 calc R . C74 C 0.5981(5) 0.1304(4) 0.6334(3) 0.0559(15) Uani 1 d . . H74 H 0.5735(5) 0.0849(4) 0.6052(3) 0.067 Uiso 1 calc R . C75 C 0.6741(5) 0.1801(5) 0.6086(3) 0.065(2) Uani 1 d . . H75 H 0.7034(5) 0.1679(5) 0.5633(3) 0.078 Uiso 1 calc R . C76 C 0.7083(4) 0.2453(5) 0.6465(4) 0.065(2) Uani 1 d . . H76 H 0.7603(4) 0.2794(5) 0.6275(4) 0.078 Uiso 1 calc R . C77 C 0.6675(4) 0.2638(4) 0.7142(3) 0.0526(14) Uani 1 d . . H77 H 0.6912(4) 0.3106(4) 0.7409(3) 0.063 Uiso 1 calc R . C80 C 0.2703(5) 0.0360(6) 0.2482(3) 0.052(2) Uani 0.60 d PD 1 H80 H 0.2721(5) 0.0969(6) 0.2482(3) 0.063 Uiso 0.60 calc PR 1 Cl1 Cl 0.3978(2) -0.0041(2) 0.26374(13) 0.0583(6) Uani 0.60 d PD 1 Cl2 Cl 0.1946(3) 0.0010(3) 0.3152(2) 0.107(2) Uani 0.60 d PD 1 Cl3 Cl 0.2221(3) -0.0013(3) 0.1613(2) 0.1030(12) Uani 0.60 d PD 1 C80X C 0.2246(12) 0.0349(17) 0.2223(6) 0.096(8) Uiso 0.40 d PD 2 H80X H 0.2269(12) 0.0924(17) 0.2045(6) 0.115 Uiso 0.40 calc PR 2 Cl1X Cl 0.2233(5) 0.0474(7) 0.3152(3) 0.190(7) Uani 0.40 d PD 2 Cl2X Cl 0.1101(6) 0.0002(8) 0.1812(5) 0.246(8) Uani 0.40 d PD 2 Cl3X Cl 0.3286(5) -0.0076(5) 0.1836(4) 0.138(3) Uani 0.40 d PD 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 0.0264(3) 0.0251(3) 0.0225(3) 0.0013(2) 0.0017(2) -0.0013(2) O1 0.035(2) 0.022(2) 0.0329(15) 0.0001(12) 0.0058(12) 0.0036(12) O2 0.0286(14) 0.022(2) 0.0290(13) 0.0014(12) 0.0012(11) -0.0037(12) O3 0.036(2) 0.055(2) 0.035(2) 0.013(2) -0.0031(13) 0.002(2) O4 0.037(2) 0.039(2) 0.044(2) 0.0093(14) 0.0082(14) -0.0064(14) O5 0.0297(15) 0.022(2) 0.036(2) -0.0012(12) 0.0044(12) 0.0015(12) O6 0.0284(14) 0.027(2) 0.0318(15) 0.0044(13) 0.0048(12) 0.0006(12) O7 0.043(2) 0.039(2) 0.040(2) -0.004(2) -0.0002(14) -0.0118(15) O8 0.037(2) 0.040(2) 0.050(2) 0.008(2) 0.0127(14) -0.0074(14) N1 0.028(2) 0.023(2) 0.026(2) -0.0010(14) 0.0015(13) -0.0025(14) N2 0.028(2) 0.026(2) 0.028(2) -0.0038(14) 0.0035(14) -0.0072(14) N3 0.022(2) 0.022(2) 0.028(2) 0.0005(14) 0.0008(13) 0.0032(13) N4 0.023(2) 0.023(2) 0.034(2) 0.0031(14) 0.0023(14) 0.0035(14) N5 0.0247(15) 0.021(2) 0.031(2) -0.002(2) -0.0006(12) -0.0015(15) N6 0.031(2) 0.033(2) 0.046(2) 0.012(2) 0.010(2) 0.002(2) N7 0.041(2) 0.023(2) 0.024(2) -0.0043(14) 0.0077(15) -0.004(2) N8 0.042(2) 0.031(2) 0.025(2) -0.0007(15) 0.0028(15) -0.015(2) C1 0.023(2) 0.031(2) 0.030(2) 0.005(2) 0.004(2) 0.001(2) C2 0.024(2) 0.024(2) 0.027(2) 0.006(2) 0.0033(15) -0.001(2) C3 0.022(2) 0.020(2) 0.028(2) 0.002(2) 0.0036(15) -0.001(2) C4 0.028(2) 0.027(2) 0.031(2) 0.001(2) 0.001(2) -0.004(2) C5 0.025(2) 0.035(2) 0.031(2) 0.004(2) 0.001(2) -0.001(2) C6 0.025(2) 0.028(2) 0.026(2) 0.002(2) 0.0048(15) 0.000(2) C7 0.030(2) 0.026(2) 0.023(2) 0.001(2) 0.006(2) 0.000(2) C8 0.031(2) 0.028(2) 0.028(2) 0.010(2) 0.005(2) 0.001(2) C9 0.036(2) 0.040(3) 0.020(2) 0.001(2) 0.002(2) -0.003(2) C10 0.035(2) 0.031(2) 0.028(2) -0.006(2) 0.009(2) -0.005(2) C11 0.028(2) 0.022(2) 0.023(2) 0.0025(15) 0.008(2) -0.002(2) C12 0.026(2) 0.023(2) 0.028(2) -0.004(2) 0.003(2) -0.004(2) C13 0.028(2) 0.043(3) 0.036(2) -0.006(2) -0.002(2) -0.007(2) C14 0.025(2) 0.025(2) 0.026(2) 0.007(2) 0.000(2) 0.001(2) C15 0.033(2) 0.025(2) 0.025(2) -0.004(2) 0.004(2) -0.004(2) C16 0.028(2) 0.041(3) 0.023(2) -0.002(2) 0.000(2) -0.005(2) C17 0.061(3) 0.061(4) 0.051(3) 0.018(3) 0.009(3) -0.015(3) C18 0.050(3) 0.039(3) 0.035(2) -0.012(2) 0.013(2) -0.014(2) C19 0.052(3) 0.033(3) 0.037(2) -0.004(2) 0.018(2) -0.007(2) C20 0.054(3) 0.056(4) 0.060(3) -0.023(3) 0.014(3) 0.000(3) C21 0.055(3) 0.053(4) 0.103(5) -0.019(4) 0.032(3) 0.009(3) C22 0.094(5) 0.054(4) 0.054(3) 0.010(3) 0.044(3) 0.016(3) C23 0.090(5) 0.076(5) 0.040(3) -0.005(3) 0.018(3) 0.019(4) C24 0.071(4) 0.069(4) 0.040(3) -0.003(3) 0.009(3) 0.004(3) C25 0.020(2) 0.023(2) 0.027(2) -0.001(2) 0.0077(15) -0.001(2) C26 0.024(2) 0.024(2) 0.030(2) 0.005(2) 0.002(2) 0.002(2) C27 0.026(2) 0.037(3) 0.031(2) -0.002(2) 0.000(2) 0.004(2) C28 0.023(2) 0.023(2) 0.032(2) 0.003(2) 0.001(2) 0.002(2) C29 0.022(2) 0.026(2) 0.029(2) -0.001(2) 0.001(2) 0.000(2) C30 0.025(2) 0.024(2) 0.037(2) 0.005(2) 0.005(2) 0.002(2) C31 0.048(3) 0.059(4) 0.076(4) 0.023(3) 0.009(3) -0.024(3) C32 0.027(2) 0.024(2) 0.038(2) 0.000(2) 0.003(2) 0.000(2) C33 0.025(2) 0.026(2) 0.036(2) -0.001(2) 0.002(2) 0.004(2) C34 0.030(2) 0.044(3) 0.045(3) -0.010(2) 0.005(2) 0.002(2) C35 0.030(2) 0.047(3) 0.065(3) -0.004(3) 0.008(2) 0.002(2) C36 0.039(3) 0.049(3) 0.049(3) 0.008(2) 0.017(2) 0.017(2) C37 0.056(3) 0.055(3) 0.041(3) -0.006(2) 0.001(2) 0.025(3) C38 0.036(2) 0.031(3) 0.049(3) -0.013(2) -0.004(2) 0.010(2) Fe2 0.0336(3) 0.0288(3) 0.0230(3) 0.0005(2) 0.0017(2) 0.0005(3) O9 0.0314(15) 0.022(2) 0.0340(15) -0.0047(12) 0.0028(12) -0.0009(12) O10 0.0325(14) 0.025(2) 0.0315(14) 0.0024(13) 0.0023(11) 0.0000(13) O11 0.056(2) 0.043(2) 0.097(3) -0.015(2) 0.030(2) -0.020(2) O12 0.070(3) 0.102(4) 0.038(2) -0.015(2) -0.001(2) -0.020(3) O13 0.042(2) 0.021(2) 0.045(2) -0.0078(13) 0.0132(14) 0.0003(13) O14 0.047(2) 0.027(2) 0.035(2) -0.0029(13) 0.0075(14) -0.0118(14) O15 0.063(2) 0.035(2) 0.035(2) 0.0138(15) -0.001(2) 0.001(2) O16 0.038(2) 0.037(2) 0.0280(15) 0.0046(13) -0.0041(13) -0.0071(14) C40 0.045(3) 0.041(3) 0.024(2) 0.000(2) 0.008(2) -0.001(2) C41 0.047(3) 0.051(3) 0.021(2) 0.007(2) -0.001(2) -0.005(2) C42 0.047(3) 0.036(3) 0.030(2) 0.009(2) 0.008(2) 0.008(2) C43 0.045(2) 0.023(2) 0.025(2) 0.003(2) 0.010(2) 0.002(2) C44 0.041(2) 0.028(2) 0.027(2) -0.002(2) 0.008(2) -0.002(2) C45 0.034(2) 0.039(2) 0.022(2) -0.002(2) 0.003(2) -0.004(2) C46 0.031(2) 0.046(3) 0.028(2) 0.003(2) -0.002(2) -0.002(2) C47 0.036(2) 0.033(3) 0.033(2) 0.000(2) 0.004(2) 0.007(2) C48 0.032(2) 0.031(2) 0.022(2) -0.004(2) 0.005(2) -0.001(2) C49 0.027(2) 0.027(2) 0.025(2) -0.002(2) 0.003(2) -0.003(2) C50 0.027(2) 0.026(2) 0.018(2) -0.0006(15) 0.0064(14) -0.001(2) C51 0.024(2) 0.024(2) 0.031(2) 0.005(2) -0.001(2) -0.002(2) C52 0.036(2) 0.039(3) 0.031(2) -0.001(2) -0.005(2) 0.002(2) C53 0.031(2) 0.023(2) 0.028(2) 0.001(2) -0.005(2) -0.003(2) C54 0.034(2) 0.026(2) 0.031(2) 0.005(2) 0.006(2) -0.002(2) C55 0.039(3) 0.037(3) 0.049(3) -0.007(2) 0.017(2) -0.003(2) C56 0.079(5) 0.087(6) 0.122(6) -0.052(5) 0.047(4) -0.054(4) C57 0.034(2) 0.028(3) 0.055(3) 0.002(2) 0.004(2) -0.005(2) C58 0.044(3) 0.029(3) 0.053(3) -0.002(2) 0.012(2) 0.000(2) C59 0.034(2) 0.055(3) 0.044(3) 0.000(2) 0.002(2) 0.005(2) C60 0.040(3) 0.050(3) 0.050(3) 0.000(2) 0.003(2) 0.005(2) C61 0.038(3) 0.065(4) 0.055(3) -0.001(3) 0.011(2) 0.010(3) C62 0.050(3) 0.088(5) 0.061(4) -0.019(3) 0.012(3) 0.013(3) C63 0.044(3) 0.083(5) 0.068(4) -0.029(3) -0.012(3) 0.010(3) C64 0.036(2) 0.022(2) 0.030(2) 0.000(2) 0.016(2) -0.005(2) C65 0.045(2) 0.021(2) 0.031(2) -0.004(2) 0.005(2) -0.007(2) C66 0.036(2) 0.039(3) 0.052(3) -0.016(2) 0.002(2) -0.008(2) C67 0.038(2) 0.023(2) 0.025(2) 0.002(2) 0.003(2) 0.001(2) C68 0.039(2) 0.033(3) 0.024(2) 0.002(2) 0.006(2) -0.009(2) C69 0.044(2) 0.020(2) 0.029(2) 0.001(2) 0.002(2) 0.004(2) C70 0.041(2) 0.038(3) 0.030(2) 0.000(2) -0.006(2) 0.003(2) C71 0.040(2) 0.049(3) 0.024(2) 0.007(2) -0.004(2) 0.003(2) C72 0.027(2) 0.056(3) 0.031(2) 0.010(2) 0.002(2) 0.011(2) C73 0.056(3) 0.042(3) 0.038(2) 0.006(2) 0.008(2) 0.011(2) C74 0.077(4) 0.047(3) 0.045(3) 0.004(3) 0.019(3) 0.017(3) C75 0.066(4) 0.082(5) 0.048(3) 0.011(3) 0.018(3) 0.036(4) C76 0.036(3) 0.097(6) 0.062(4) 0.034(4) 0.011(3) -0.001(3) C77 0.033(2) 0.078(4) 0.048(3) 0.014(3) 0.003(2) -0.012(3) C80 0.066(6) 0.045(6) 0.048(5) -0.002(4) 0.019(5) 0.000(5) Cl1 0.0385(10) 0.073(2) 0.0650(13) -0.0266(13) 0.0134(10) -0.0066(10) Cl2 0.051(2) 0.188(5) 0.087(2) 0.065(3) 0.044(2) 0.014(2) Cl3 0.105(3) 0.106(3) 0.094(2) -0.016(2) -0.033(2) 0.023(2) Cl1X 0.048(3) 0.407(19) 0.115(5) 0.137(9) 0.018(3) -0.023(6) Cl2X 0.269(12) 0.260(14) 0.227(11) -0.174(11) 0.156(10) -0.120(11) Cl3X 0.106(4) 0.138(6) 0.176(7) 0.037(6) 0.062(5) 0.044(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 Fe1 C3 2.024(4) . ? Fe1 C7 2.025(4) . ? Fe1 C2 2.029(4) . ? Fe1 C8 2.038(4) . ? Fe1 C6 2.038(4) . ? Fe1 C4 2.040(4) . ? Fe1 C9 2.045(4) . ? Fe1 C1 2.049(4) . ? Fe1 C10 2.052(4) . ? Fe1 C5 2.055(4) . ? O1 C11 1.242(5) . ? O2 C14 1.240(5) . ? O3 C16 1.186(5) . ? O4 C16 1.328(5) . ? O4 C17 1.443(6) . ? O5 C25 1.238(5) . ? O6 C28 1.230(5) . ? O7 C30 1.185(5) . ? O8 C30 1.335(5) . ? O8 C31 1.457(6) . ? N1 C11 1.351(5) . ? N1 C12 1.444(5) . ? N2 C14 1.331(5) . ? N2 C15 1.461(5) . ? N3 C25 1.341(5) . ? N3 C26 1.440(5) . ? N4 C28 1.334(5) . ? N4 C29 1.443(5) . ? N5 C50 1.353(5) . ? N5 C51 1.435(5) . ? N6 C53 1.335(6) . ? N6 C54 1.443(5) . ? N7 C64 1.341(6) . ? N7 C65 1.454(5) . ? N8 C67 1.333(5) . ? N8 C68 1.444(5) . ? C1 C2 1.420(6) . ? C1 C5 1.425(6) . ? C2 C3 1.427(6) . ? C3 C4 1.428(6) . ? C3 C25 1.477(5) . ? C4 C5 1.411(6) . ? C6 C10 1.416(6) . ? C6 C7 1.434(6) . ? C7 C8 1.427(6) . ? C7 C11 1.464(6) . ? C8 C9 1.418(6) . ? C9 C10 1.416(6) . ? C12 C13 1.504(6) . ? C12 C14 1.524(5) . ? C15 C16 1.526(6) . ? C15 C18 1.528(6) . ? C18 C19 1.513(6) . ? C19 C20 1.375(7) . ? C19 C24 1.403(7) . ? C20 C21 1.382(8) . ? C21 C22 1.374(10) . ? C22 C23 1.366(10) . ? C23 C24 1.389(8) . ? C26 C27 1.529(6) . ? C26 C28 1.531(5) . ? C29 C30 1.517(6) . ? C29 C32 1.540(6) . ? C32 C33 1.506(6) . ? C33 C38 1.376(6) . ? C33 C34 1.393(6) . ? C34 C35 1.385(7) . ? C35 C36 1.371(8) . ? C36 C37 1.373(8) . ? C37 C38 1.383(7) . ? Fe2 C43 2.021(4) . ? Fe2 C42 2.032(5) . ? Fe2 C48 2.036(4) . ? Fe2 C49 2.036(4) . ? Fe2 C44 2.039(4) . ? Fe2 C47 2.039(4) . ? Fe2 C41 2.043(4) . ? Fe2 C45 2.049(5) . ? Fe2 C40 2.051(4) . ? Fe2 C46 2.054(4) . ? O9 C50 1.226(5) . ? O10 C53 1.226(5) . ? O11 C55 1.314(6) . ? O11 C56 1.490(8) . ? O12 C55 1.193(6) . ? O13 C64 1.240(5) . ? O14 C67 1.228(5) . ? O15 C69 1.192(5) . ? O16 C69 1.337(5) . ? O16 C70 1.442(5) . ? C40 C41 1.413(7) . ? C40 C44 1.426(6) . ? C41 C42 1.418(7) . ? C42 C43 1.430(6) . ? C43 C44 1.428(6) . ? C43 C64 1.467(6) . ? C45 C46 1.412(7) . ? C45 C49 1.435(5) . ? C46 C47 1.417(6) . ? C47 C48 1.412(6) . ? C48 C49 1.431(6) . ? C49 C50 1.469(6) . ? C51 C53 1.526(6) . ? C51 C52 1.530(6) . ? C54 C55 1.524(7) . ? C54 C57 1.524(6) . ? C57 C58 1.515(7) . ? C58 C63 1.381(8) . ? C58 C59 1.390(7) . ? C59 C60 1.378(7) . ? C60 C61 1.353(8) . ? C61 C62 1.370(8) . ? C62 C63 1.396(8) . ? C65 C66 1.515(7) . ? C65 C67 1.532(6) . ? C68 C69 1.512(6) . ? C68 C71 1.529(7) . ? C71 C72 1.504(6) . ? C72 C73 1.379(7) . ? C72 C77 1.379(7) . ? C73 C74 1.392(7) . ? C74 C75 1.366(9) . ? C75 C76 1.335(10) . ? C76 C77 1.405(9) . ? C80 Cl2 1.703(6) . ? C80 Cl1 1.764(7) . ? C80 Cl3 1.777(7) . ? C80X Cl3X 1.69(2) . ? C80X Cl2X 1.702(9) . ? C80X Cl1X 1.709(9) . ? 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 C3 Fe1 C7 121.9(2) . . ? C3 Fe1 C2 41.2(2) . . ? C7 Fe1 C2 106.8(2) . . ? C3 Fe1 C8 158.0(2) . . ? C7 Fe1 C8 41.1(2) . . ? C2 Fe1 C8 121.5(2) . . ? C3 Fe1 C6 107.4(2) . . ? C7 Fe1 C6 41.3(2) . . ? C2 Fe1 C6 123.9(2) . . ? C8 Fe1 C6 69.0(2) . . ? C3 Fe1 C4 41.1(2) . . ? C7 Fe1 C4 158.5(2) . . ? C2 Fe1 C4 69.0(2) . . ? C8 Fe1 C4 159.2(2) . . ? C6 Fe1 C4 122.4(2) . . ? C3 Fe1 C9 160.0(2) . . ? C7 Fe1 C9 68.8(2) . . ? C2 Fe1 C9 157.3(2) . . ? C8 Fe1 C9 40.7(2) . . ? C6 Fe1 C9 68.4(2) . . ? C4 Fe1 C9 123.3(2) . . ? C3 Fe1 C1 69.0(2) . . ? C7 Fe1 C1 122.9(2) . . ? C2 Fe1 C1 40.8(2) . . ? C8 Fe1 C1 106.7(2) . . ? C6 Fe1 C1 160.3(2) . . ? C4 Fe1 C1 68.5(2) . . ? C9 Fe1 C1 121.6(2) . . ? C3 Fe1 C10 123.9(2) . . ? C7 Fe1 C10 68.8(2) . . ? C2 Fe1 C10 160.7(2) . . ? C8 Fe1 C10 68.4(2) . . ? C6 Fe1 C10 40.5(2) . . ? C4 Fe1 C10 107.8(2) . . ? C9 Fe1 C10 40.4(2) . . ? C1 Fe1 C10 157.5(2) . . ? C3 Fe1 C5 68.6(2) . . ? C7 Fe1 C5 159.5(2) . . ? C2 Fe1 C5 68.4(2) . . ? C8 Fe1 C5 123.0(2) . . ? C6 Fe1 C5 157.8(2) . . ? C4 Fe1 C5 40.3(2) . . ? C9 Fe1 C5 107.5(2) . . ? C1 Fe1 C5 40.6(2) . . ? C10 Fe1 C5 122.2(2) . . ? C16 O4 C17 116.1(4) . . ? C30 O8 C31 115.5(4) . . ? C11 N1 C12 121.0(4) . . ? C14 N2 C15 119.9(3) . . ? C25 N3 C26 121.0(3) . . ? C28 N4 C29 120.3(3) . . ? C50 N5 C51 120.6(4) . . ? C53 N6 C54 124.0(4) . . ? C64 N7 C65 120.9(4) . . ? C67 N8 C68 122.6(4) . . ? C2 C1 C5 107.7(4) . . ? C2 C1 Fe1 68.9(2) . . ? C5 C1 Fe1 69.9(2) . . ? C1 C2 C3 108.2(4) . . ? C1 C2 Fe1 70.4(2) . . ? C3 C2 Fe1 69.2(2) . . ? C2 C3 C4 107.6(3) . . ? C2 C3 C25 128.4(4) . . ? C4 C3 C25 123.9(4) . . ? C2 C3 Fe1 69.6(2) . . ? C4 C3 Fe1 70.1(2) . . ? C25 C3 Fe1 122.1(3) . . ? C5 C4 C3 108.1(4) . . ? C5 C4 Fe1 70.4(2) . . ? C3 C4 Fe1 68.8(2) . . ? C4 C5 C1 108.5(4) . . ? C4 C5 Fe1 69.3(2) . . ? C1 C5 Fe1 69.5(2) . . ? C10 C6 C7 107.8(4) . . ? C10 C6 Fe1 70.3(2) . . ? C7 C6 Fe1 68.9(2) . . ? C8 C7 C6 107.6(4) . . ? C8 C7 C11 123.3(4) . . ? C6 C7 C11 129.0(4) . . ? C8 C7 Fe1 69.9(2) . . ? C6 C7 Fe1 69.8(2) . . ? C11 C7 Fe1 124.1(3) . . ? C9 C8 C7 107.8(4) . . ? C9 C8 Fe1 70.0(3) . . ? C7 C8 Fe1 69.0(2) . . ? C10 C9 C8 108.5(4) . . ? C10 C9 Fe1 70.1(2) . . ? C8 C9 Fe1 69.4(2) . . ? C9 C10 C6 108.3(4) . . ? C9 C10 Fe1 69.5(2) . . ? C6 C10 Fe1 69.2(2) . . ? O1 C11 N1 121.6(4) . . ? O1 C11 C7 121.3(4) . . ? N1 C11 C7 117.1(4) . . ? N1 C12 C13 111.8(4) . . ? N1 C12 C14 110.6(3) . . ? C13 C12 C14 111.3(3) . . ? O2 C14 N2 121.6(4) . . ? O2 C14 C12 122.6(4) . . ? N2 C14 C12 115.8(3) . . ? N2 C15 C16 109.7(3) . . ? N2 C15 C18 108.3(3) . . ? C16 C15 C18 111.4(3) . . ? O3 C16 O4 125.0(4) . . ? O3 C16 C15 125.2(4) . . ? O4 C16 C15 109.8(4) . . ? C19 C18 C15 115.5(4) . . ? C20 C19 C24 118.0(5) . . ? C20 C19 C18 122.7(5) . . ? C24 C19 C18 119.2(5) . . ? C19 C20 C21 121.5(6) . . ? C22 C21 C20 119.4(6) . . ? C23 C22 C21 120.7(5) . . ? C22 C23 C24 119.8(6) . . ? C23 C24 C19 120.3(6) . . ? O5 C25 N3 122.0(4) . . ? O5 C25 C3 121.0(4) . . ? N3 C25 C3 116.9(4) . . ? N3 C26 C27 110.7(3) . . ? N3 C26 C28 110.5(3) . . ? C27 C26 C28 110.9(3) . . ? O6 C28 N4 122.2(4) . . ? O6 C28 C26 122.6(3) . . ? N4 C28 C26 115.1(3) . . ? N4 C29 C30 110.8(3) . . ? N4 C29 C32 109.3(3) . . ? C30 C29 C32 111.1(3) . . ? O7 C30 O8 124.7(4) . . ? O7 C30 C29 125.7(4) . . ? O8 C30 C29 109.7(4) . . ? C33 C32 C29 112.9(3) . . ? C38 C33 C34 118.5(4) . . ? C38 C33 C32 121.3(4) . . ? C34 C33 C32 120.1(4) . . ? C35 C34 C33 120.1(5) . . ? C36 C35 C34 120.6(5) . . ? C35 C36 C37 119.5(4) . . ? C36 C37 C38 120.2(5) . . ? C33 C38 C37 120.9(5) . . ? C43 Fe2 C42 41.3(2) . . ? C43 Fe2 C48 107.2(2) . . ? C42 Fe2 C48 121.0(2) . . ? C43 Fe2 C49 122.3(2) . . ? C42 Fe2 C49 157.8(2) . . ? C48 Fe2 C49 41.1(2) . . ? C43 Fe2 C44 41.2(2) . . ? C42 Fe2 C44 69.1(2) . . ? C48 Fe2 C44 124.8(2) . . ? C49 Fe2 C44 108.4(2) . . ? C43 Fe2 C47 123.5(2) . . ? C42 Fe2 C47 106.5(2) . . ? C48 Fe2 C47 40.5(2) . . ? C49 Fe2 C47 68.3(2) . . ? C44 Fe2 C47 161.1(2) . . ? C43 Fe2 C41 69.2(2) . . ? C42 Fe2 C41 40.7(2) . . ? C48 Fe2 C41 156.1(2) . . ? C49 Fe2 C41 160.7(2) . . ? C44 Fe2 C41 68.9(2) . . ? C47 Fe2 C41 120.5(2) . . ? C43 Fe2 C45 158.7(2) . . ? C42 Fe2 C45 158.9(2) . . ? C48 Fe2 C45 69.1(2) . . ? C49 Fe2 C45 41.14(15) . . ? C44 Fe2 C45 122.6(2) . . ? C47 Fe2 C45 68.1(2) . . ? C41 Fe2 C45 123.0(2) . . ? C43 Fe2 C40 68.7(2) . . ? C42 Fe2 C40 68.1(2) . . ? C48 Fe2 C40 162.2(2) . . ? C49 Fe2 C40 125.3(2) . . ? C44 Fe2 C40 40.8(2) . . ? C47 Fe2 C40 156.3(2) . . ? C41 Fe2 C40 40.4(2) . . ? C45 Fe2 C40 108.1(2) . . ? C43 Fe2 C46 159.7(2) . . ? C42 Fe2 C46 122.5(2) . . ? C48 Fe2 C46 68.6(2) . . ? C49 Fe2 C46 68.5(2) . . ? C44 Fe2 C46 157.4(2) . . ? C47 Fe2 C46 40.5(2) . . ? C41 Fe2 C46 106.2(2) . . ? C45 Fe2 C46 40.2(2) . . ? C40 Fe2 C46 121.4(2) . . ? C55 O11 C56 113.1(5) . . ? C69 O16 C70 116.3(3) . . ? C41 C40 C44 108.9(4) . . ? C41 C40 Fe2 69.5(3) . . ? C44 C40 Fe2 69.2(2) . . ? C40 C41 C42 107.8(4) . . ? C40 C41 Fe2 70.1(3) . . ? C42 C41 Fe2 69.2(2) . . ? C41 C42 C43 108.2(4) . . ? C41 C42 Fe2 70.0(3) . . ? C43 C42 Fe2 68.9(3) . . ? C44 C43 C42 107.8(4) . . ? C44 C43 C64 128.6(4) . . ? C42 C43 C64 123.5(4) . . ? C44 C43 Fe2 70.1(2) . . ? C42 C43 Fe2 69.7(3) . . ? C64 C43 Fe2 122.9(3) . . ? C40 C44 C43 107.2(4) . . ? C40 C44 Fe2 70.0(3) . . ? C43 C44 Fe2 68.8(2) . . ? C46 C45 C49 107.8(4) . . ? C46 C45 Fe2 70.1(3) . . ? C49 C45 Fe2 69.0(2) . . ? C45 C46 C47 108.0(4) . . ? C45 C46 Fe2 69.7(2) . . ? C47 C46 Fe2 69.2(3) . . ? C48 C47 C46 109.1(4) . . ? C48 C47 Fe2 69.6(2) . . ? C46 C47 Fe2 70.3(3) . . ? C47 C48 C49 107.3(4) . . ? C47 C48 Fe2 69.8(2) . . ? C49 C48 Fe2 69.4(2) . . ? C48 C49 C45 107.8(4) . . ? C48 C49 C50 129.4(4) . . ? C45 C49 C50 122.7(4) . . ? C48 C49 Fe2 69.4(2) . . ? C45 C49 Fe2 69.9(2) . . ? C50 C49 Fe2 123.1(3) . . ? O9 C50 N5 122.4(4) . . ? O9 C50 C49 121.0(4) . . ? N5 C50 C49 116.6(4) . . ? N5 C51 C53 112.1(3) . . ? N5 C51 C52 110.7(4) . . ? C53 C51 C52 110.2(3) . . ? O10 C53 N6 123.1(4) . . ? O10 C53 C51 122.8(4) . . ? N6 C53 C51 114.1(4) . . ? N6 C54 C55 107.5(3) . . ? N6 C54 C57 108.6(4) . . ? C55 C54 C57 108.9(4) . . ? O12 C55 O11 126.0(5) . . ? O12 C55 C54 122.5(5) . . ? O11 C55 C54 111.5(5) . . ? C58 C57 C54 114.1(4) . . ? C63 C58 C59 116.8(5) . . ? C63 C58 C57 121.8(5) . . ? C59 C58 C57 121.4(5) . . ? C60 C59 C58 121.2(5) . . ? C61 C60 C59 120.3(5) . . ? C60 C61 C62 121.1(5) . . ? C61 C62 C63 118.1(5) . . ? C58 C63 C62 122.4(5) . . ? O13 C64 N7 121.5(4) . . ? O13 C64 C43 120.8(4) . . ? N7 C64 C43 117.7(4) . . ? N7 C65 C66 110.2(4) . . ? N7 C65 C67 110.5(3) . . ? C66 C65 C67 110.4(4) . . ? O14 C67 N8 123.4(4) . . ? O14 C67 C65 123.0(4) . . ? N8 C67 C65 113.5(4) . . ? N8 C68 C69 111.4(4) . . ? N8 C68 C71 110.6(3) . . ? C69 C68 C71 109.2(4) . . ? O15 C69 O16 123.9(4) . . ? O15 C69 C68 125.8(4) . . ? O16 C69 C68 110.3(3) . . ? C72 C71 C68 115.3(4) . . ? C73 C72 C77 118.8(5) . . ? C73 C72 C71 120.1(4) . . ? C77 C72 C71 121.2(5) . . ? C72 C73 C74 120.9(5) . . ? C75 C74 C73 118.8(6) . . ? C76 C75 C74 121.6(5) . . ? C75 C76 C77 120.2(6) . . ? C72 C77 C76 119.6(6) . . ? Cl2 C80 Cl1 108.5(4) . . ? Cl2 C80 Cl3 110.2(5) . . ? Cl1 C80 Cl3 106.3(4) . . ? Cl3X C80X Cl2X 110.6(10) . . ? Cl3X C80X Cl1X 121.3(11) . . ? Cl2X C80X Cl1X 114.8(8) . . ? _refine_diff_density_max 1.128 _refine_diff_density_min -0.735 _refine_diff_density_rms 0.073 #===END