# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_afh305 _database_code_depnum_ccdc_archive 'CCDC 916892' #TrackingRef '[ONO]Fe_CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [ONOq]FeCl2 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H48 Cl2 Fe N O2' _chemical_formula_weight 641.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.1903(6) _cell_length_b 12.5783(8) _cell_length_c 27.2498(17) _cell_angle_alpha 90.00 _cell_angle_beta 96.4952(8) _cell_angle_gamma 90.00 _cell_volume 3470.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 7537 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 25.76 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1364 _exptl_absorpt_coefficient_mu 0.618 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.8775 _exptl_absorpt_correction_T_max 0.9557 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 36819 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 26.39 _reflns_number_total 7105 _reflns_number_gt 5507 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+1.5450P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7105 _refine_ls_number_parameters 468 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0802 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.40721(2) 0.65200(2) 0.162352(10) 0.01950(8) Uani 1 1 d . . . Cl2 Cl 0.55976(5) 0.53272(5) 0.15131(2) 0.03871(14) Uani 1 1 d . . . Cl1 Cl 0.48542(5) 0.81188(4) 0.18180(2) 0.03761(14) Uani 1 1 d . . . O1 O 0.34122(12) 0.68157(11) 0.09403(5) 0.0248(3) Uani 1 1 d . . . O2 O 0.37981(12) 0.60334(10) 0.23022(5) 0.0218(3) Uani 1 1 d . . . N1 N 0.19691(14) 0.66510(11) 0.16460(5) 0.0168(3) Uani 1 1 d . . . C1 C 0.13032(17) 0.69646(14) 0.12097(6) 0.0173(4) Uani 1 1 d . . . C2 C 0.21851(17) 0.70836(14) 0.08342(6) 0.0184(4) Uani 1 1 d . . . C3 C 0.16920(17) 0.74937(15) 0.03597(7) 0.0206(4) Uani 1 1 d . . . C4 C 0.03656(17) 0.77123(15) 0.02823(7) 0.0210(4) Uani 1 1 d . . . H4A H 0.0028 0.7997 -0.0029 0.025 Uiso 1 1 calc R . . C5 C -0.05426(17) 0.75419(15) 0.06366(7) 0.0196(4) Uani 1 1 d . A . C6 C -0.00608(17) 0.71689(14) 0.10910(7) 0.0191(4) Uani 1 1 d . . . H6A H -0.0649 0.7044 0.1331 0.023 Uiso 1 1 calc R . . C7 C 0.26300(18) 0.76975(17) -0.00317(7) 0.0262(4) Uani 1 1 d . . . C8 C 0.36769(19) 0.85141(18) 0.01708(8) 0.0328(5) Uani 1 1 d . . . H8A H 0.3241 0.9179 0.0247 0.049 Uiso 1 1 calc R . . H8B H 0.4282 0.8649 -0.0077 0.049 Uiso 1 1 calc R . . H8C H 0.4175 0.8234 0.0472 0.049 Uiso 1 1 calc R . . C9 C 0.3291(2) 0.66576(19) -0.01664(8) 0.0359(5) Uani 1 1 d . . . H9A H 0.3798 0.6361 0.0129 0.054 Uiso 1 1 calc R . . H9B H 0.3884 0.6800 -0.0418 0.054 Uiso 1 1 calc R . . H9C H 0.2612 0.6148 -0.0296 0.054 Uiso 1 1 calc R . . C10 C 0.1887(2) 0.8164(2) -0.05036(7) 0.0346(5) Uani 1 1 d . . . H10A H 0.1445 0.8823 -0.0424 0.052 Uiso 1 1 calc R . . H10B H 0.1227 0.7651 -0.0647 0.052 Uiso 1 1 calc R . . H10C H 0.2514 0.8315 -0.0742 0.052 Uiso 1 1 calc R . . C11 C -0.20184(18) 0.77829(16) 0.05134(7) 0.0252(4) Uani 1 1 d . . . C12 C -0.2452(3) 0.8589(3) 0.08850(11) 0.0382(8) Uani 0.773(4) 1 d P A 1 H12A H -0.2346 0.8276 0.1216 0.057 Uiso 0.773(4) 1 calc PR A 1 H12B H -0.3381 0.8777 0.0793 0.057 Uiso 0.773(4) 1 calc PR A 1 H12C H -0.1906 0.9230 0.0883 0.057 Uiso 0.773(4) 1 calc PR A 1 C13 C -0.2358(3) 0.8260(3) -0.00058(10) 0.0371(8) Uani 0.773(4) 1 d P A 1 H13A H -0.2152 0.7742 -0.0255 0.056 Uiso 0.773(4) 1 calc PR A 1 H13B H -0.1837 0.8907 -0.0036 0.056 Uiso 0.773(4) 1 calc PR A 1 H13C H -0.3301 0.8435 -0.0057 0.056 Uiso 0.773(4) 1 calc PR A 1 C14 C -0.2803(3) 0.6752(2) 0.05403(12) 0.0399(9) Uani 0.773(4) 1 d P A 1 H14A H -0.2629 0.6448 0.0872 0.060 Uiso 0.773(4) 1 calc PR A 1 H14B H -0.2534 0.6244 0.0298 0.060 Uiso 0.773(4) 1 calc PR A 1 H14C H -0.3749 0.6903 0.0468 0.060 Uiso 0.773(4) 1 calc PR A 1 C13B C -0.2564(10) 0.7141(10) 0.0076(4) 0.052(4) Uani 0.227(4) 1 d P A 2 H13D H -0.2055 0.7284 -0.0201 0.079 Uiso 0.227(4) 1 calc PR A 2 H13E H -0.3491 0.7334 -0.0017 0.079 Uiso 0.227(4) 1 calc PR A 2 H13F H -0.2505 0.6383 0.0159 0.079 Uiso 0.227(4) 1 calc PR A 2 C12B C -0.2105(10) 0.8984(9) 0.0385(5) 0.047(3) Uani 0.227(4) 1 d P A 2 H12D H -0.1629 0.9123 0.0098 0.071 Uiso 0.227(4) 1 calc PR A 2 H12E H -0.1708 0.9399 0.0668 0.071 Uiso 0.227(4) 1 calc PR A 2 H12F H -0.3033 0.9189 0.0307 0.071 Uiso 0.227(4) 1 calc PR A 2 C14B C -0.2790(9) 0.7599(13) 0.0949(4) 0.062(5) Uani 0.227(4) 1 d P A 2 H14D H -0.2759 0.6843 0.1037 0.093 Uiso 0.227(4) 1 calc PR A 2 H14E H -0.3710 0.7816 0.0862 0.093 Uiso 0.227(4) 1 calc PR A 2 H14F H -0.2399 0.8018 0.1232 0.093 Uiso 0.227(4) 1 calc PR A 2 C15 C 0.15719(17) 0.64991(14) 0.20897(6) 0.0180(4) Uani 1 1 d . . . C16 C 0.26594(17) 0.61033(14) 0.24453(6) 0.0178(4) Uani 1 1 d . . . C17 C 0.24003(17) 0.57991(14) 0.29358(6) 0.0184(4) Uani 1 1 d . . . C18 C 0.11455(18) 0.59513(15) 0.30463(7) 0.0205(4) Uani 1 1 d . . . H18A H 0.0950 0.5731 0.3363 0.025 Uiso 1 1 calc R . . C19 C 0.00863(17) 0.64213(15) 0.27204(7) 0.0201(4) Uani 1 1 d . . . C20 C 0.03097(17) 0.66809(14) 0.22538(7) 0.0200(4) Uani 1 1 d . . . H20A H -0.0379 0.6986 0.2035 0.024 Uiso 1 1 calc R . . C21 C 0.35118(18) 0.53431(15) 0.32988(7) 0.0207(4) Uani 1 1 d . . . C22 C 0.45804(19) 0.61981(16) 0.34200(7) 0.0255(4) Uani 1 1 d . . . H22A H 0.4919 0.6429 0.3115 0.038 Uiso 1 1 calc R . . H22B H 0.5305 0.5902 0.3646 0.038 Uiso 1 1 calc R . . H22C H 0.4197 0.6808 0.3576 0.038 Uiso 1 1 calc R . . C23 C 0.4121(2) 0.43616(16) 0.30771(7) 0.0281(4) Uani 1 1 d . . . H23A H 0.4511 0.4568 0.2778 0.042 Uiso 1 1 calc R . . H23B H 0.3433 0.3827 0.2993 0.042 Uiso 1 1 calc R . . H23C H 0.4809 0.4064 0.3319 0.042 Uiso 1 1 calc R . . C24 C 0.3002(2) 0.50074(17) 0.37841(7) 0.0291(5) Uani 1 1 d . . . H24A H 0.2305 0.4474 0.3716 0.044 Uiso 1 1 calc R . . H24B H 0.2646 0.5629 0.3940 0.044 Uiso 1 1 calc R . . H24C H 0.3730 0.4704 0.4006 0.044 Uiso 1 1 calc R . . C25 C -0.12363(18) 0.66091(16) 0.29190(7) 0.0245(4) Uani 1 1 d . . . C26 C -0.2233(2) 0.7149(2) 0.25371(8) 0.0385(6) Uani 1 1 d . . . H26A H -0.1882 0.7837 0.2445 0.058 Uiso 1 1 calc R . . H26B H -0.3065 0.7259 0.2678 0.058 Uiso 1 1 calc R . . H26C H -0.2391 0.6697 0.2243 0.058 Uiso 1 1 calc R . . C27 C -0.1804(2) 0.55373(18) 0.30597(10) 0.0433(6) Uani 1 1 d . . . H27A H -0.1955 0.5086 0.2765 0.065 Uiso 1 1 calc R . . H27B H -0.2642 0.5653 0.3196 0.065 Uiso 1 1 calc R . . H27C H -0.1177 0.5187 0.3307 0.065 Uiso 1 1 calc R . . C28 C -0.1021(2) 0.73244(18) 0.33754(7) 0.0399(6) Uani 1 1 d . . . H28A H -0.0655 0.8008 0.3284 0.060 Uiso 1 1 calc R . . H28B H -0.0404 0.6980 0.3628 0.060 Uiso 1 1 calc R . . H28C H -0.1867 0.7443 0.3506 0.060 Uiso 1 1 calc R . . C29 C 0.0110(2) 0.4034(2) 0.18628(10) 0.0396(11) Uani 0.645(5) 1 d PR B 1 H29A H -0.0574 0.4032 0.2072 0.048 Uiso 0.645(5) 1 calc PR B 1 C30 C -0.0173(6) 0.4303(8) 0.1384(5) 0.0358(17) Uani 0.645(5) 1 d P B 1 H30A H -0.1056 0.4473 0.1259 0.043 Uiso 0.645(5) 1 calc PR B 1 C31 C 0.0849(8) 0.4335(8) 0.1059(4) 0.0361(19) Uani 0.645(5) 1 d P B 1 C32 C 0.2103(5) 0.4069(4) 0.1259(2) 0.0419(13) Uani 0.645(5) 1 d P B 1 H32A H 0.2795 0.4084 0.1053 0.050 Uiso 0.645(5) 1 calc PR B 1 C33 C 0.2407(14) 0.3776(9) 0.1758(3) 0.0368(19) Uani 0.645(5) 1 d P B 1 H33A H 0.3282 0.3594 0.1889 0.044 Uiso 0.645(5) 1 calc PR B 1 C34 C 0.1377(5) 0.3762(3) 0.2054(2) 0.0388(11) Uani 0.645(5) 1 d P B 1 H34A H 0.1549 0.3562 0.2391 0.047 Uiso 0.645(5) 1 calc PR B 1 C35 C 0.0543(5) 0.4659(3) 0.05286(16) 0.0566(14) Uani 0.645(5) 1 d P B 1 H35A H 0.1351 0.4628 0.0365 0.085 Uiso 0.645(5) 1 calc PR B 1 H35B H 0.0195 0.5386 0.0512 0.085 Uiso 0.645(5) 1 calc PR B 1 H35C H -0.0117 0.4174 0.0362 0.085 Uiso 0.645(5) 1 calc PR B 1 C29B C 0.254(3) 0.3912(17) 0.1598(6) 0.041(4) Uani 0.355(5) 1 d P B 2 H29B H 0.3297 0.3744 0.1820 0.049 Uiso 0.355(5) 1 calc PR B 2 C30B C 0.1384(10) 0.3958(6) 0.1785(4) 0.041(2) Uani 0.355(5) 1 d P B 2 H30B H 0.1295 0.3807 0.2122 0.049 Uiso 0.355(5) 1 calc PR B 2 C31B C 0.0283(10) 0.4258(16) 0.1432(10) 0.036(3) Uani 0.355(5) 1 d P B 2 C32B C 0.0408(15) 0.4415(16) 0.0977(8) 0.037(4) Uani 0.355(5) 1 d P B 2 H32B H -0.0350 0.4581 0.0755 0.045 Uiso 0.355(5) 1 calc PR B 2 C33B C 0.1640(9) 0.4348(6) 0.0801(3) 0.053(2) Uani 0.355(5) 1 d P B 2 H33B H 0.1732 0.4483 0.0464 0.063 Uiso 0.355(5) 1 calc PR B 2 C34B C 0.2719(10) 0.4080(7) 0.1129(4) 0.049(2) Uani 0.355(5) 1 d P B 2 H34B H 0.3571 0.4017 0.1023 0.058 Uiso 0.355(5) 1 calc PR B 2 C35B C -0.1062(8) 0.4309(6) 0.1639(3) 0.060(3) Uani 0.355(5) 1 d P B 2 H35D H -0.0941 0.4138 0.1993 0.090 Uiso 0.355(5) 1 calc PR B 2 H35E H -0.1669 0.3795 0.1465 0.090 Uiso 0.355(5) 1 calc PR B 2 H35F H -0.1430 0.5026 0.1593 0.090 Uiso 0.355(5) 1 calc PR B 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 0.01463(13) 0.02377(15) 0.02008(14) 0.00411(12) 0.00186(10) 0.00159(11) Cl2 0.0372(3) 0.0410(3) 0.0402(3) 0.0100(3) 0.0144(2) 0.0197(2) Cl1 0.0307(3) 0.0266(3) 0.0526(4) 0.0063(2) -0.0082(2) -0.0059(2) O1 0.0173(6) 0.0378(8) 0.0197(7) 0.0044(6) 0.0036(5) 0.0050(6) O2 0.0179(7) 0.0266(7) 0.0207(7) 0.0047(6) 0.0020(5) 0.0021(5) N1 0.0162(7) 0.0158(8) 0.0183(8) 0.0006(6) 0.0012(6) -0.0008(6) C1 0.0184(9) 0.0166(9) 0.0166(9) -0.0007(7) 0.0006(7) -0.0015(7) C2 0.0172(9) 0.0207(10) 0.0174(9) -0.0011(8) 0.0018(7) -0.0011(7) C3 0.0208(9) 0.0241(10) 0.0170(9) 0.0001(8) 0.0024(7) -0.0011(8) C4 0.0216(9) 0.0247(10) 0.0163(9) 0.0013(8) 0.0001(7) -0.0009(8) C5 0.0162(9) 0.0214(10) 0.0211(9) -0.0013(8) 0.0010(7) -0.0018(7) C6 0.0174(9) 0.0209(10) 0.0194(9) -0.0019(8) 0.0035(7) -0.0017(7) C7 0.0200(10) 0.0415(12) 0.0175(10) 0.0047(9) 0.0037(7) 0.0042(9) C8 0.0209(10) 0.0472(14) 0.0307(11) 0.0103(10) 0.0048(8) -0.0028(10) C9 0.0320(12) 0.0528(15) 0.0239(11) -0.0019(10) 0.0075(9) 0.0073(10) C10 0.0260(11) 0.0591(16) 0.0192(10) 0.0099(10) 0.0051(8) 0.0030(10) C11 0.0170(9) 0.0349(12) 0.0231(10) 0.0034(9) 0.0000(8) 0.0004(8) C12 0.0220(14) 0.057(2) 0.0350(17) -0.0041(15) 0.0007(12) 0.0135(14) C13 0.0200(14) 0.058(2) 0.0316(16) 0.0121(15) -0.0027(11) 0.0052(13) C14 0.0180(14) 0.049(2) 0.051(2) 0.0088(15) -0.0020(12) -0.0077(13) C13B 0.023(5) 0.066(9) 0.064(8) -0.008(7) -0.018(5) 0.002(5) C12B 0.025(5) 0.050(7) 0.067(8) 0.016(6) 0.004(5) 0.013(5) C14B 0.015(5) 0.123(14) 0.048(7) 0.048(8) 0.010(4) 0.023(6) C15 0.0193(9) 0.0159(9) 0.0186(9) 0.0001(8) 0.0015(7) -0.0007(7) C16 0.0193(9) 0.0146(9) 0.0190(9) -0.0005(7) -0.0005(7) -0.0004(7) C17 0.0225(9) 0.0138(9) 0.0185(9) 0.0010(7) 0.0003(7) -0.0012(7) C18 0.0243(10) 0.0198(10) 0.0175(9) 0.0018(8) 0.0029(7) -0.0027(8) C19 0.0208(9) 0.0187(10) 0.0212(9) -0.0010(8) 0.0043(7) -0.0006(7) C20 0.0170(9) 0.0211(10) 0.0213(9) 0.0002(8) 0.0003(7) 0.0025(7) C21 0.0221(9) 0.0208(10) 0.0187(9) 0.0025(8) 0.0000(7) -0.0003(8) C22 0.0249(10) 0.0272(11) 0.0230(10) 0.0016(8) -0.0032(8) -0.0007(8) C23 0.0310(11) 0.0248(11) 0.0274(11) 0.0038(9) -0.0014(9) 0.0061(9) C24 0.0287(11) 0.0361(12) 0.0218(11) 0.0091(9) -0.0007(8) 0.0017(9) C25 0.0222(10) 0.0265(11) 0.0261(10) 0.0030(9) 0.0084(8) 0.0030(8) C26 0.0251(11) 0.0585(16) 0.0336(12) 0.0081(11) 0.0103(9) 0.0153(10) C27 0.0264(12) 0.0366(13) 0.0708(17) 0.0087(12) 0.0224(11) 0.0011(10) C28 0.0400(13) 0.0500(15) 0.0322(13) -0.0067(11) 0.0146(10) 0.0070(11) C29 0.047(3) 0.0255(19) 0.050(3) -0.0103(17) 0.019(2) -0.0124(17) C30 0.020(4) 0.026(2) 0.062(4) -0.015(2) 0.010(5) -0.008(4) C31 0.044(6) 0.025(3) 0.039(4) -0.011(3) 0.006(4) -0.009(4) C32 0.044(4) 0.030(2) 0.055(4) -0.016(2) 0.021(3) -0.013(2) C33 0.043(4) 0.024(3) 0.042(5) -0.004(4) -0.004(4) -0.005(2) C34 0.057(3) 0.021(2) 0.038(3) -0.0040(19) 0.005(2) -0.0074(17) C35 0.084(4) 0.040(2) 0.044(3) -0.012(2) 0.001(2) -0.014(2) C29B 0.051(8) 0.032(7) 0.037(10) -0.003(7) -0.007(8) 0.009(6) C30B 0.061(6) 0.019(4) 0.040(5) -0.005(4) -0.002(5) -0.014(4) C31B 0.005(6) 0.027(4) 0.077(9) -0.016(4) 0.008(8) -0.006(6) C32B 0.027(8) 0.027(5) 0.054(10) -0.005(5) -0.010(5) 0.000(6) C33B 0.075(6) 0.038(4) 0.045(5) -0.020(4) 0.009(5) -0.013(4) C34B 0.036(5) 0.037(5) 0.073(7) -0.022(4) 0.007(5) -0.007(4) C35B 0.039(5) 0.044(5) 0.098(7) -0.020(4) 0.013(5) -0.015(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 O1 1.9427(13) . ? Fe1 O2 1.9973(12) . ? Fe1 N1 2.1571(14) . ? Fe1 Cl2 2.2054(6) . ? Fe1 Cl1 2.2057(6) . ? O1 C2 1.296(2) . ? O2 C16 1.268(2) . ? N1 C15 1.332(2) . ? N1 C1 1.359(2) . ? C1 C6 1.415(2) . ? C1 C2 1.444(2) . ? C2 C3 1.429(2) . ? C3 C4 1.372(2) . ? C3 C7 1.532(2) . ? C4 C5 1.427(2) . ? C5 C6 1.363(3) . ? C5 C11 1.534(2) . ? C7 C10 1.533(3) . ? C7 C9 1.535(3) . ? C7 C8 1.538(3) . ? C11 C13B 1.495(11) . ? C11 C14B 1.515(10) . ? C11 C14 1.530(3) . ? C11 C12 1.533(3) . ? C11 C13 1.540(3) . ? C11 C12B 1.551(11) . ? C15 C20 1.427(2) . ? C15 C16 1.474(2) . ? C16 C17 1.443(2) . ? C17 C18 1.360(3) . ? C17 C21 1.529(2) . ? C18 C19 1.444(3) . ? C19 C20 1.357(2) . ? C19 C25 1.527(2) . ? C21 C24 1.534(3) . ? C21 C23 1.536(3) . ? C21 C22 1.540(3) . ? C25 C26 1.529(3) . ? C25 C28 1.530(3) . ? C25 C27 1.533(3) . ? C29 C30 1.348(13) . ? C29 C34 1.379(5) . ? C30 C31 1.441(14) . ? C31 C32 1.373(9) . ? C31 C35 1.501(11) . ? C32 C33 1.410(10) . ? C33 C34 1.392(12) . ? C29B C34B 1.329(16) . ? C29B C30B 1.33(3) . ? C30B C31B 1.44(2) . ? C31B C32B 1.27(3) . ? C31B C35B 1.542(16) . ? C32B C33B 1.40(2) . ? C33B C34B 1.378(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O2 151.23(5) . . ? O1 Fe1 N1 77.01(5) . . ? O2 Fe1 N1 75.74(5) . . ? O1 Fe1 Cl2 99.93(4) . . ? O2 Fe1 Cl2 95.30(4) . . ? N1 Fe1 Cl2 140.69(4) . . ? O1 Fe1 Cl1 97.59(5) . . ? O2 Fe1 Cl1 98.14(4) . . ? N1 Fe1 Cl1 104.87(4) . . ? Cl2 Fe1 Cl1 114.32(2) . . ? C2 O1 Fe1 118.97(11) . . ? C16 O2 Fe1 119.47(11) . . ? C15 N1 C1 131.54(15) . . ? C15 N1 Fe1 114.82(11) . . ? C1 N1 Fe1 113.37(11) . . ? N1 C1 C6 129.29(16) . . ? N1 C1 C2 111.15(15) . . ? C6 C1 C2 119.56(16) . . ? O1 C2 C3 121.83(16) . . ? O1 C2 C1 118.50(16) . . ? C3 C2 C1 119.67(16) . . ? C4 C3 C2 116.80(16) . . ? C4 C3 C7 122.73(16) . . ? C2 C3 C7 120.45(15) . . ? C3 C4 C5 124.67(17) . . ? C6 C5 C4 118.15(16) . . ? C6 C5 C11 120.70(16) . . ? C4 C5 C11 121.14(16) . . ? C5 C6 C1 120.94(17) . . ? C3 C7 C10 111.10(15) . . ? C3 C7 C9 110.43(17) . . ? C10 C7 C9 108.29(17) . . ? C3 C7 C8 108.92(16) . . ? C10 C7 C8 107.59(17) . . ? C9 C7 C8 110.48(16) . . ? C13B C11 C14B 111.3(8) . . ? C13B C11 C14 55.3(5) . . ? C14B C11 C14 60.8(6) . . ? C13B C11 C12 140.8(4) . . ? C14B C11 C12 50.9(6) . . ? C14 C11 C12 109.8(2) . . ? C13B C11 C5 109.6(4) . . ? C14B C11 C5 112.4(4) . . ? C14 C11 C5 109.07(18) . . ? C12 C11 C5 109.57(17) . . ? C13B C11 C13 56.8(5) . . ? C14B C11 C13 134.2(4) . . ? C14 C11 C13 108.1(2) . . ? C12 C11 C13 107.3(2) . . ? C5 C11 C13 113.02(17) . . ? C13B C11 C12B 109.9(7) . . ? C14B C11 C12B 107.7(7) . . ? C14 C11 C12B 145.1(4) . . ? C12 C11 C12B 59.4(5) . . ? C5 C11 C12B 105.7(4) . . ? C13 C11 C12B 54.0(5) . . ? N1 C15 C20 129.70(16) . . ? N1 C15 C16 111.24(15) . . ? C20 C15 C16 119.05(16) . . ? O2 C16 C17 122.41(16) . . ? O2 C16 C15 117.86(15) . . ? C17 C16 C15 119.72(15) . . ? C18 C17 C16 116.29(16) . . ? C18 C17 C21 123.77(16) . . ? C16 C17 C21 119.93(15) . . ? C17 C18 C19 125.26(17) . . ? C20 C19 C18 118.81(16) . . ? C20 C19 C25 122.93(16) . . ? C18 C19 C25 118.26(16) . . ? C19 C20 C15 120.52(17) . . ? C17 C21 C24 111.26(15) . . ? C17 C21 C23 110.49(15) . . ? C24 C21 C23 108.02(16) . . ? C17 C21 C22 109.33(15) . . ? C24 C21 C22 107.92(15) . . ? C23 C21 C22 109.76(15) . . ? C19 C25 C26 111.88(16) . . ? C19 C25 C28 109.16(16) . . ? C26 C25 C28 108.37(17) . . ? C19 C25 C27 109.01(16) . . ? C26 C25 C27 108.69(18) . . ? C28 C25 C27 109.71(18) . . ? C30 C29 C34 121.1(4) . . ? C29 C30 C31 120.7(6) . . ? C32 C31 C30 117.0(8) . . ? C32 C31 C35 122.1(8) . . ? C30 C31 C35 120.9(7) . . ? C31 C32 C33 122.6(9) . . ? C34 C33 C32 117.6(11) . . ? C29 C34 C33 120.9(6) . . ? C34B C29B C30B 125.8(19) . . ? C29B C30B C31B 114.1(15) . . ? C32B C31B C30B 122.2(14) . . ? C32B C31B C35B 122.7(14) . . ? C30B C31B C35B 115(2) . . ? C31B C32B C33B 121.2(11) . . ? C34B C33B C32B 118.3(11) . . ? C29B C34B C33B 118.4(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Fe1 O1 C2 28.3(2) . . . . ? N1 Fe1 O1 C2 9.24(13) . . . . ? Cl2 Fe1 O1 C2 149.21(13) . . . . ? Cl1 Fe1 O1 C2 -94.36(13) . . . . ? O1 Fe1 O2 C16 -25.1(2) . . . . ? N1 Fe1 O2 C16 -5.92(13) . . . . ? Cl2 Fe1 O2 C16 -147.02(13) . . . . ? Cl1 Fe1 O2 C16 97.44(13) . . . . ? O1 Fe1 N1 C15 179.15(13) . . . . ? O2 Fe1 N1 C15 8.48(12) . . . . ? Cl2 Fe1 N1 C15 89.28(13) . . . . ? Cl1 Fe1 N1 C15 -86.32(12) . . . . ? O1 Fe1 N1 C1 -6.17(12) . . . . ? O2 Fe1 N1 C1 -176.84(13) . . . . ? Cl2 Fe1 N1 C1 -96.03(13) . . . . ? Cl1 Fe1 N1 C1 88.37(12) . . . . ? C15 N1 C1 C6 -4.1(3) . . . . ? Fe1 N1 C1 C6 -177.64(15) . . . . ? C15 N1 C1 C2 176.15(18) . . . . ? Fe1 N1 C1 C2 2.60(18) . . . . ? Fe1 O1 C2 C3 168.62(13) . . . . ? Fe1 O1 C2 C1 -11.1(2) . . . . ? N1 C1 C2 O1 4.9(2) . . . . ? C6 C1 C2 O1 -174.87(16) . . . . ? N1 C1 C2 C3 -174.83(16) . . . . ? C6 C1 C2 C3 5.4(3) . . . . ? O1 C2 C3 C4 177.55(17) . . . . ? C1 C2 C3 C4 -2.7(3) . . . . ? O1 C2 C3 C7 -3.9(3) . . . . ? C1 C2 C3 C7 175.80(17) . . . . ? C2 C3 C4 C5 -1.1(3) . . . . ? C7 C3 C4 C5 -179.60(18) . . . . ? C3 C4 C5 C6 2.3(3) . . . . ? C3 C4 C5 C11 -178.41(18) . . . . ? C4 C5 C6 C1 0.5(3) . . . . ? C11 C5 C6 C1 -178.77(17) . . . . ? N1 C1 C6 C5 176.01(18) . . . . ? C2 C1 C6 C5 -4.3(3) . . . . ? C4 C3 C7 C10 0.0(3) . . . . ? C2 C3 C7 C10 -178.45(18) . . . . ? C4 C3 C7 C9 -120.2(2) . . . . ? C2 C3 C7 C9 61.4(2) . . . . ? C4 C3 C7 C8 118.3(2) . . . . ? C2 C3 C7 C8 -60.1(2) . . . . ? C6 C5 C11 C13B -122.2(6) . . . . ? C4 C5 C11 C13B 58.6(6) . . . . ? C6 C5 C11 C14B 2.2(7) . . . . ? C4 C5 C11 C14B -177.1(7) . . . . ? C6 C5 C11 C14 -63.3(3) . . . . ? C4 C5 C11 C14 117.5(2) . . . . ? C6 C5 C11 C12 56.9(3) . . . . ? C4 C5 C11 C12 -122.4(2) . . . . ? C6 C5 C11 C13 176.5(2) . . . . ? C4 C5 C11 C13 -2.8(3) . . . . ? C6 C5 C11 C12B 119.5(5) . . . . ? C4 C5 C11 C12B -59.8(5) . . . . ? C1 N1 C15 C20 -4.1(3) . . . . ? Fe1 N1 C15 C20 169.43(16) . . . . ? C1 N1 C15 C16 177.22(17) . . . . ? Fe1 N1 C15 C16 -9.30(19) . . . . ? Fe1 O2 C16 C17 -177.95(13) . . . . ? Fe1 O2 C16 C15 2.8(2) . . . . ? N1 C15 C16 O2 4.7(2) . . . . ? C20 C15 C16 O2 -174.15(16) . . . . ? N1 C15 C16 C17 -174.52(16) . . . . ? C20 C15 C16 C17 6.6(3) . . . . ? O2 C16 C17 C18 177.68(17) . . . . ? C15 C16 C17 C18 -3.1(3) . . . . ? O2 C16 C17 C21 -1.8(3) . . . . ? C15 C16 C17 C21 177.37(16) . . . . ? C16 C17 C18 C19 -2.3(3) . . . . ? C21 C17 C18 C19 177.21(17) . . . . ? C17 C18 C19 C20 4.3(3) . . . . ? C17 C18 C19 C25 -175.42(18) . . . . ? C18 C19 C20 C15 -0.4(3) . . . . ? C25 C19 C20 C15 179.23(17) . . . . ? N1 C15 C20 C19 176.64(18) . . . . ? C16 C15 C20 C19 -4.7(3) . . . . ? C18 C17 C21 C24 4.2(3) . . . . ? C16 C17 C21 C24 -176.29(16) . . . . ? C18 C17 C21 C23 124.21(19) . . . . ? C16 C17 C21 C23 -56.3(2) . . . . ? C18 C17 C21 C22 -114.88(19) . . . . ? C16 C17 C21 C22 64.6(2) . . . . ? C20 C19 C25 C26 -1.9(3) . . . . ? C18 C19 C25 C26 177.79(18) . . . . ? C20 C19 C25 C28 -121.8(2) . . . . ? C18 C19 C25 C28 57.9(2) . . . . ? C20 C19 C25 C27 118.4(2) . . . . ? C18 C19 C25 C27 -62.0(2) . . . . ? C34 C29 C30 C31 -1.3(11) . . . . ? C29 C30 C31 C32 0.8(14) . . . . ? C29 C30 C31 C35 -178.5(7) . . . . ? C30 C31 C32 C33 -0.1(13) . . . . ? C35 C31 C32 C33 179.2(8) . . . . ? C31 C32 C33 C34 -0.1(13) . . . . ? C30 C29 C34 C33 1.2(9) . . . . ? C32 C33 C34 C29 -0.5(12) . . . . ? C34B C29B C30B C31B -2(3) . . . . ? C29B C30B C31B C32B 3(3) . . . . ? C29B C30B C31B C35B 179.6(14) . . . . ? C30B C31B C32B C33B -3(3) . . . . ? C35B C31B C32B C33B -179.1(14) . . . . ? C31B C32B C33B C34B 2(2) . . . . ? C30B C29B C34B C33B 1(3) . . . . ? C32B C33B C34B C29B -0.8(18) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.331 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.049 data_afh317 _database_code_depnum_ccdc_archive 'CCDC 916893' #TrackingRef '[ONO]Fe_CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [ONOq]Fe[N(SiMe3)2]2 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H76 Fe N3 O2 Si4' _chemical_formula_weight 799.25 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' Si Si 0.0817 0.0704 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.9269(7) _cell_length_b 17.5744(10) _cell_length_c 24.1583(13) _cell_angle_alpha 90.00 _cell_angle_beta 111.5826(6) _cell_angle_gamma 90.00 _cell_volume 4708.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.127 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1740 _exptl_absorpt_coefficient_mu 0.455 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8060 _exptl_absorpt_correction_T_max 0.9491 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11228 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 28.29 _reflns_number_total 11228 _reflns_number_gt 9967 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+0.9098P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11228 _refine_ls_number_parameters 756 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0737 _refine_ls_wR_factor_gt 0.0705 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.123407(18) 0.209567(11) 0.333562(9) 0.01355(5) Uani 1 1 d . . . Si1 Si 0.02871(4) 0.08976(2) 0.40153(2) 0.02114(9) Uani 1 1 d . . . Si2 Si 0.24284(4) 0.18321(3) 0.474975(18) 0.02135(9) Uani 1 1 d . . . Si3 Si 0.07997(4) 0.38121(2) 0.353013(19) 0.01805(9) Uani 1 1 d . . . Si4 Si 0.26211(4) 0.34561(2) 0.29624(2) 0.02053(9) Uani 1 1 d . . . O1 O 0.26878(9) 0.14728(6) 0.33388(4) 0.0180(2) Uani 1 1 d . . . O2 O -0.06391(9) 0.22023(6) 0.29231(4) 0.0164(2) Uani 1 1 d . . . N1 N 0.07831(11) 0.17107(7) 0.24176(5) 0.0146(2) Uani 1 1 d . . . N2 N 0.12954(11) 0.16306(7) 0.40714(5) 0.0171(2) Uani 1 1 d . . . N3 N 0.16655(11) 0.31573(7) 0.33173(5) 0.0162(2) Uani 1 1 d . . . C1 C 0.26749(13) 0.11734(8) 0.28557(6) 0.0153(3) Uani 1 1 d . . . C2 C 0.36349(13) 0.06834(8) 0.28360(6) 0.0158(3) Uani 1 1 d . . . C3 C 0.36071(13) 0.04874(8) 0.22821(7) 0.0169(3) Uani 1 1 d . . . C4 C 0.26385(13) 0.06640(8) 0.17326(6) 0.0156(3) Uani 1 1 d . . . C5 C 0.16725(14) 0.10547(8) 0.17546(7) 0.0173(3) Uani 1 1 d . . . C6 C 0.16602(13) 0.13338(8) 0.23074(6) 0.0152(3) Uani 1 1 d . . . C7 C 0.45489(13) 0.03536(9) 0.34103(6) 0.0181(3) Uani 1 1 d . . . C8 C 0.54628(15) -0.01688(10) 0.32866(8) 0.0236(3) Uani 1 1 d . . . C9 C 0.52701(15) 0.09755(10) 0.38443(7) 0.0220(3) Uani 1 1 d . . . C10 C 0.38261(16) -0.01224(10) 0.37009(8) 0.0246(3) Uani 1 1 d . . . C11 C 0.27174(14) 0.03728(9) 0.11498(6) 0.0184(3) Uani 1 1 d . . . C12 C 0.15257(17) 0.04873(11) 0.06222(7) 0.0277(4) Uani 1 1 d . . . C13 C 0.30215(17) -0.04791(10) 0.11985(8) 0.0258(4) Uani 1 1 d . . . C14 C 0.37142(18) 0.08104(11) 0.10281(8) 0.0291(4) Uani 1 1 d . . . C15 C -0.10832(13) 0.21724(8) 0.23554(6) 0.0151(3) Uani 1 1 d . . . C16 C -0.23474(13) 0.23166(8) 0.20055(6) 0.0164(3) Uani 1 1 d . . . C17 C -0.26764(14) 0.23114(9) 0.14008(7) 0.0187(3) Uani 1 1 d . . . C18 C -0.18826(14) 0.21750(8) 0.10876(6) 0.0186(3) Uani 1 1 d . . . C19 C -0.07151(14) 0.20022(9) 0.14066(7) 0.0180(3) Uani 1 1 d . . . C20 C -0.02932(13) 0.19559(8) 0.20411(6) 0.0157(3) Uani 1 1 d . . . C21 C -0.32824(13) 0.24124(9) 0.22980(7) 0.0197(3) Uani 1 1 d . . . C22 C -0.33644(16) 0.16536(11) 0.25977(9) 0.0288(4) Uani 1 1 d . . . C23 C -0.45374(14) 0.25977(11) 0.18397(8) 0.0253(3) Uani 1 1 d . . . C24 C -0.29392(16) 0.30536(11) 0.27595(8) 0.0291(4) Uani 1 1 d . . . C25 C -0.24126(15) 0.22059(10) 0.04058(7) 0.0243(3) Uani 1 1 d . . . C26 C -0.34008(17) 0.15964(13) 0.01801(8) 0.0339(4) Uani 1 1 d . . . C27 C -0.14598(17) 0.20391(13) 0.01370(8) 0.0324(4) Uani 1 1 d . . . C28 C -0.2954(2) 0.29918(13) 0.02004(9) 0.0398(5) Uani 1 1 d . . . C29 C 0.0964(2) 0.00854(11) 0.45370(10) 0.0372(4) Uani 1 1 d . . . C30 C -0.10546(17) 0.12416(11) 0.41675(8) 0.0278(4) Uani 1 1 d . . . C31 C -0.0209(2) 0.04427(11) 0.32650(9) 0.0327(4) Uani 1 1 d . . . C32 C 0.18152(18) 0.19730(13) 0.53576(8) 0.0313(4) Uani 1 1 d . . . C33 C 0.36112(19) 0.10747(14) 0.50181(9) 0.0362(4) Uani 1 1 d . . . C34 C 0.33087(17) 0.27029(12) 0.47331(8) 0.0314(4) Uani 1 1 d . . . C35 C 0.16582(19) 0.46462(11) 0.39775(9) 0.0312(4) Uani 1 1 d . . . C36 C 0.00969(15) 0.33782(9) 0.40323(7) 0.0197(3) Uani 1 1 d . . . C37 C -0.03916(17) 0.42218(10) 0.28550(8) 0.0280(4) Uani 1 1 d . . . C38 C 0.1951(2) 0.33198(12) 0.21337(9) 0.0362(5) Uani 1 1 d . . . C39 C 0.4115(2) 0.29657(14) 0.32500(14) 0.0432(5) Uani 1 1 d . . . C40 C 0.30199(18) 0.44935(10) 0.30567(9) 0.0297(4) Uani 1 1 d . . . H3A H 0.4255(16) 0.0195(10) 0.2249(7) 0.018(4) Uiso 1 1 d . . . H5A H 0.1025(17) 0.1143(10) 0.1428(8) 0.023(5) Uiso 1 1 d . . . H8A H 0.5046(17) -0.0575(10) 0.3027(8) 0.020(4) Uiso 1 1 d . . . H8B H 0.5979(19) -0.0385(12) 0.3658(9) 0.034(5) Uiso 1 1 d . . . H8C H 0.5961(18) 0.0100(11) 0.3123(8) 0.026(5) Uiso 1 1 d . . . H9A H 0.5695(17) 0.1262(11) 0.3665(8) 0.026(5) Uiso 1 1 d . . . H9B H 0.5828(18) 0.0755(11) 0.4190(9) 0.029(5) Uiso 1 1 d . . . H9C H 0.4755(17) 0.1330(11) 0.3941(8) 0.022(5) Uiso 1 1 d . . . H10A H 0.3411(18) -0.0527(12) 0.3448(9) 0.031(5) Uiso 1 1 d . . . H10B H 0.3242(17) 0.0183(11) 0.3765(8) 0.024(5) Uiso 1 1 d . . . H10C H 0.4350(18) -0.0354(11) 0.4068(9) 0.029(5) Uiso 1 1 d . . . H12A H 0.1370(19) 0.1037(13) 0.0561(9) 0.038(6) Uiso 1 1 d . . . H12B H 0.0873(19) 0.0229(12) 0.0688(9) 0.033(5) Uiso 1 1 d . . . H12C H 0.1604(18) 0.0286(11) 0.0288(9) 0.032(5) Uiso 1 1 d . . . H13A H 0.2459(18) -0.0752(11) 0.1306(9) 0.029(5) Uiso 1 1 d . . . H13B H 0.3847(19) -0.0593(11) 0.1504(9) 0.030(5) Uiso 1 1 d . . . H13C H 0.3048(19) -0.0661(12) 0.0827(9) 0.035(5) Uiso 1 1 d . . . H14A H 0.352(2) 0.1329(14) 0.0989(10) 0.050(7) Uiso 1 1 d . . . H14B H 0.3812(19) 0.0606(12) 0.0672(10) 0.038(6) Uiso 1 1 d . . . H14C H 0.4496(19) 0.0724(11) 0.1349(9) 0.033(5) Uiso 1 1 d . . . H17A H -0.3464(16) 0.2392(9) 0.1171(8) 0.015(4) Uiso 1 1 d . . . H19A H -0.0170(17) 0.1942(10) 0.1218(8) 0.023(5) Uiso 1 1 d . . . H22A H -0.365(2) 0.1283(13) 0.2309(10) 0.043(6) Uiso 1 1 d . . . H22B H -0.390(2) 0.1720(13) 0.2814(10) 0.045(6) Uiso 1 1 d . . . H22C H -0.2630(19) 0.1529(11) 0.2894(9) 0.026(5) Uiso 1 1 d . . . H23A H -0.4533(18) 0.3059(12) 0.1641(9) 0.029(5) Uiso 1 1 d . . . H23B H -0.5102(18) 0.2628(11) 0.2063(9) 0.030(5) Uiso 1 1 d . . . H23C H -0.4838(17) 0.2207(11) 0.1552(8) 0.023(5) Uiso 1 1 d . . . H24A H -0.2974(18) 0.3519(12) 0.2580(9) 0.029(5) Uiso 1 1 d . . . H24B H -0.218(2) 0.2966(11) 0.3067(9) 0.032(5) Uiso 1 1 d . . . H24C H -0.356(2) 0.3057(12) 0.2947(9) 0.037(6) Uiso 1 1 d . . . H26A H -0.304(2) 0.1073(14) 0.0303(10) 0.049(7) Uiso 1 1 d . . . H26B H -0.373(2) 0.1629(13) -0.0250(11) 0.048(6) Uiso 1 1 d . . . H26C H -0.4024(19) 0.1676(12) 0.0337(9) 0.035(6) Uiso 1 1 d . . . H27A H -0.084(2) 0.2388(13) 0.0281(10) 0.042(6) Uiso 1 1 d . . . H27B H -0.181(2) 0.2045(12) -0.0286(10) 0.038(6) Uiso 1 1 d . . . H27C H -0.1134(19) 0.1521(12) 0.0246(9) 0.034(5) Uiso 1 1 d . . . H28A H -0.234(2) 0.3374(12) 0.0341(9) 0.033(6) Uiso 1 1 d . . . H28B H -0.365(2) 0.3116(12) 0.0363(9) 0.038(6) Uiso 1 1 d . . . H28C H -0.323(2) 0.3033(14) -0.0211(12) 0.055(7) Uiso 1 1 d . . . H29A H 0.163(2) -0.0142(13) 0.4439(10) 0.045(6) Uiso 1 1 d . . . H29B H 0.040(3) -0.0276(17) 0.4496(13) 0.074(9) Uiso 1 1 d . . . H29C H 0.120(2) 0.0215(13) 0.4936(11) 0.049(7) Uiso 1 1 d . . . H30A H -0.1431(19) 0.1679(12) 0.3917(9) 0.033(5) Uiso 1 1 d . . . H30B H -0.085(2) 0.1353(13) 0.4568(11) 0.048(6) Uiso 1 1 d . . . H30C H -0.161(2) 0.0910(13) 0.4077(10) 0.041(6) Uiso 1 1 d . . . H31A H 0.051(2) 0.0251(14) 0.3215(11) 0.053(7) Uiso 1 1 d . . . H31B H -0.065(2) 0.0746(13) 0.2931(11) 0.047(6) Uiso 1 1 d . . . H31C H -0.070(2) 0.0007(16) 0.3257(11) 0.064(8) Uiso 1 1 d . . . H32A H 0.128(2) 0.2380(13) 0.5280(10) 0.044(6) Uiso 1 1 d . . . H32B H 0.249(2) 0.2093(12) 0.5730(10) 0.045(6) Uiso 1 1 d . . . H32C H 0.142(2) 0.1553(12) 0.5412(9) 0.034(6) Uiso 1 1 d . . . H33A H 0.399(2) 0.0981(14) 0.4751(12) 0.061(8) Uiso 1 1 d . . . H33B H 0.336(2) 0.0596(16) 0.5087(12) 0.062(8) Uiso 1 1 d . . . H33C H 0.423(2) 0.1268(14) 0.5377(11) 0.055(7) Uiso 1 1 d . . . H34A H 0.371(2) 0.2651(12) 0.4452(10) 0.039(6) Uiso 1 1 d . . . H34B H 0.391(2) 0.2773(12) 0.5135(10) 0.045(6) Uiso 1 1 d . . . H34C H 0.288(2) 0.3131(13) 0.4650(10) 0.043(6) Uiso 1 1 d . . . H35A H 0.240(2) 0.4522(12) 0.4260(10) 0.040(6) Uiso 1 1 d . . . H35B H 0.119(2) 0.4880(13) 0.4165(10) 0.047(6) Uiso 1 1 d . . . H35C H 0.180(2) 0.5026(13) 0.3742(10) 0.045(6) Uiso 1 1 d . . . H36A H -0.0365(19) 0.2922(12) 0.3877(9) 0.029(5) Uiso 1 1 d . . . H36B H -0.0412(19) 0.3737(12) 0.4081(9) 0.035(5) Uiso 1 1 d . . . H36C H 0.0658(18) 0.3271(10) 0.4414(8) 0.024(5) Uiso 1 1 d . . . H37A H -0.090(2) 0.3818(13) 0.2574(10) 0.040(6) Uiso 1 1 d . . . H37B H -0.003(2) 0.4539(13) 0.2655(10) 0.047(7) Uiso 1 1 d . . . H37C H -0.096(2) 0.4536(14) 0.2931(10) 0.051(7) Uiso 1 1 d . . . H38A H 0.194(2) 0.2816(13) 0.2000(10) 0.041(6) Uiso 1 1 d . . . H38B H 0.246(2) 0.3600(14) 0.1978(11) 0.054(7) Uiso 1 1 d . . . H38C H 0.115(2) 0.3469(15) 0.1982(11) 0.059(8) Uiso 1 1 d . . . H39A H 0.443(3) 0.297(2) 0.3632(16) 0.097(13) Uiso 1 1 d . . . H39B H 0.465(2) 0.3215(14) 0.3096(11) 0.054(7) Uiso 1 1 d . . . H39C H 0.406(3) 0.251(2) 0.3129(15) 0.091(12) Uiso 1 1 d . . . H40A H 0.3425(19) 0.4635(12) 0.3473(10) 0.038(6) Uiso 1 1 d . . . H40B H 0.233(2) 0.4820(13) 0.2891(10) 0.048(6) Uiso 1 1 d . . . H40C H 0.355(2) 0.4562(14) 0.2850(11) 0.056(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01340(10) 0.01572(10) 0.01188(9) 0.00055(8) 0.00507(8) 0.00087(8) Si1 0.0277(2) 0.0180(2) 0.0212(2) 0.00257(16) 0.01310(18) -0.00010(17) Si2 0.0188(2) 0.0312(2) 0.01367(19) 0.00422(16) 0.00552(17) 0.00480(18) Si3 0.0198(2) 0.01651(19) 0.0205(2) -0.00035(16) 0.01055(17) 0.00044(16) Si4 0.0214(2) 0.0205(2) 0.0247(2) 0.00105(17) 0.01427(18) -0.00188(17) O1 0.0164(5) 0.0225(5) 0.0143(5) -0.0007(4) 0.0049(4) 0.0039(4) O2 0.0147(5) 0.0204(5) 0.0142(5) -0.0011(4) 0.0053(4) 0.0003(4) N1 0.0134(6) 0.0153(6) 0.0150(6) 0.0004(5) 0.0052(5) 0.0004(4) N2 0.0186(6) 0.0189(6) 0.0145(6) 0.0039(5) 0.0071(5) 0.0027(5) N3 0.0161(6) 0.0164(6) 0.0173(6) 0.0004(5) 0.0075(5) -0.0004(5) C1 0.0148(7) 0.0171(7) 0.0144(6) 0.0009(5) 0.0057(6) 0.0003(5) C2 0.0135(7) 0.0165(7) 0.0162(7) 0.0007(5) 0.0042(5) 0.0023(5) C3 0.0162(7) 0.0170(7) 0.0188(7) 0.0004(6) 0.0078(6) 0.0030(6) C4 0.0174(7) 0.0165(7) 0.0135(6) 0.0002(5) 0.0063(6) 0.0000(5) C5 0.0162(7) 0.0202(7) 0.0135(7) 0.0013(6) 0.0030(6) 0.0015(6) C6 0.0143(7) 0.0150(6) 0.0157(6) 0.0010(5) 0.0050(6) 0.0006(5) C7 0.0139(7) 0.0235(7) 0.0156(7) 0.0017(6) 0.0037(6) 0.0051(6) C8 0.0186(8) 0.0282(8) 0.0215(8) 0.0025(7) 0.0044(7) 0.0099(7) C9 0.0170(7) 0.0296(9) 0.0158(7) -0.0005(6) 0.0018(6) 0.0030(7) C10 0.0234(8) 0.0278(9) 0.0227(8) 0.0081(7) 0.0085(7) 0.0061(7) C11 0.0200(7) 0.0215(7) 0.0145(7) -0.0018(6) 0.0074(6) 0.0013(6) C12 0.0282(9) 0.0378(10) 0.0142(7) -0.0042(7) 0.0044(7) 0.0071(8) C13 0.0313(9) 0.0231(8) 0.0228(8) -0.0045(7) 0.0098(7) 0.0037(7) C14 0.0338(10) 0.0334(10) 0.0260(9) -0.0023(8) 0.0179(8) -0.0064(8) C15 0.0150(7) 0.0142(7) 0.0167(7) -0.0003(5) 0.0066(6) -0.0004(5) C16 0.0129(7) 0.0163(7) 0.0194(7) -0.0014(5) 0.0053(6) 0.0011(5) C17 0.0135(7) 0.0205(7) 0.0199(7) -0.0011(6) 0.0038(6) 0.0013(6) C18 0.0207(7) 0.0189(7) 0.0159(7) 0.0017(6) 0.0065(6) 0.0028(6) C19 0.0178(7) 0.0209(7) 0.0171(7) 0.0004(6) 0.0087(6) 0.0023(6) C20 0.0151(7) 0.0154(7) 0.0167(7) 0.0001(5) 0.0060(6) 0.0013(5) C21 0.0140(7) 0.0243(7) 0.0217(7) -0.0036(6) 0.0077(6) -0.0002(6) C22 0.0205(8) 0.0393(10) 0.0289(9) 0.0055(8) 0.0118(7) -0.0021(7) C23 0.0143(7) 0.0310(9) 0.0296(9) -0.0044(7) 0.0070(7) 0.0022(6) C24 0.0182(8) 0.0389(10) 0.0314(9) -0.0144(8) 0.0105(7) -0.0005(7) C25 0.0219(8) 0.0337(9) 0.0152(7) 0.0035(6) 0.0043(6) 0.0087(7) C26 0.0244(9) 0.0525(12) 0.0208(8) -0.0083(8) 0.0036(7) 0.0059(8) C27 0.0281(9) 0.0528(12) 0.0163(8) 0.0056(8) 0.0081(7) 0.0089(9) C28 0.0478(12) 0.0421(12) 0.0266(10) 0.0149(9) 0.0105(9) 0.0195(10) C29 0.0480(12) 0.0271(9) 0.0409(11) 0.0142(8) 0.0215(10) 0.0038(9) C30 0.0261(9) 0.0318(9) 0.0288(9) -0.0001(8) 0.0140(8) -0.0040(7) C31 0.0490(12) 0.0219(8) 0.0306(9) -0.0059(7) 0.0189(9) -0.0088(8) C32 0.0312(10) 0.0457(12) 0.0177(8) -0.0002(8) 0.0098(7) 0.0029(9) C33 0.0303(10) 0.0503(12) 0.0253(9) 0.0095(8) 0.0070(8) 0.0168(9) C34 0.0227(9) 0.0442(11) 0.0219(8) 0.0002(8) 0.0019(7) -0.0067(8) C35 0.0380(11) 0.0260(9) 0.0364(10) -0.0098(8) 0.0217(9) -0.0077(8) C36 0.0217(8) 0.0201(8) 0.0204(8) -0.0006(6) 0.0112(6) 0.0015(6) C37 0.0284(9) 0.0256(8) 0.0333(9) 0.0103(7) 0.0152(8) 0.0084(7) C38 0.0567(14) 0.0329(10) 0.0284(9) -0.0037(8) 0.0265(10) -0.0147(9) C39 0.0281(10) 0.0429(13) 0.0703(17) 0.0142(12) 0.0319(11) 0.0051(9) C40 0.0342(10) 0.0262(9) 0.0360(10) -0.0017(8) 0.0215(9) -0.0083(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.9331(12) . ? Fe1 N3 1.9402(12) . ? Fe1 O1 2.0480(10) . ? Fe1 O2 2.0932(10) . ? Fe1 N1 2.1881(12) . ? Si1 N2 1.7332(13) . ? Si1 C31 1.8670(19) . ? Si1 C30 1.8693(18) . ? Si1 C29 1.8786(19) . ? Si2 N2 1.7343(13) . ? Si2 C34 1.865(2) . ? Si2 C33 1.873(2) . ? Si2 C32 1.8823(18) . ? Si3 N3 1.7453(13) . ? Si3 C37 1.8688(18) . ? Si3 C36 1.8719(16) . ? Si3 C35 1.8843(18) . ? Si4 N3 1.7403(13) . ? Si4 C39 1.868(2) . ? Si4 C40 1.8767(18) . ? Si4 C38 1.878(2) . ? O1 C1 1.2752(17) . ? O2 C15 1.2765(17) . ? N1 C20 1.3423(18) . ? N1 C6 1.3449(19) . ? C1 C2 1.4474(19) . ? C1 C6 1.4558(19) . ? C2 C3 1.370(2) . ? C2 C7 1.528(2) . ? C3 C4 1.437(2) . ? C4 C5 1.359(2) . ? C4 C11 1.5333(19) . ? C5 C6 1.428(2) . ? C7 C8 1.536(2) . ? C7 C9 1.540(2) . ? C7 C10 1.543(2) . ? C11 C14 1.533(2) . ? C11 C12 1.534(2) . ? C11 C13 1.535(2) . ? C15 C16 1.454(2) . ? C15 C20 1.461(2) . ? C16 C17 1.366(2) . ? C16 C21 1.533(2) . ? C17 C18 1.433(2) . ? C18 C19 1.355(2) . ? C18 C25 1.533(2) . ? C19 C20 1.429(2) . ? C21 C24 1.531(2) . ? C21 C23 1.534(2) . ? C21 C22 1.538(2) . ? C25 C28 1.528(2) . ? C25 C27 1.530(2) . ? C25 C26 1.536(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N3 120.46(5) . . ? N2 Fe1 O1 91.43(5) . . ? N3 Fe1 O1 106.42(5) . . ? N2 Fe1 O2 98.54(5) . . ? N3 Fe1 O2 98.55(5) . . ? O1 Fe1 O2 143.46(4) . . ? N2 Fe1 N1 135.50(5) . . ? N3 Fe1 N1 104.04(5) . . ? O1 Fe1 N1 74.38(4) . . ? O2 Fe1 N1 73.96(4) . . ? N2 Si1 C31 110.93(8) . . ? N2 Si1 C30 111.34(8) . . ? C31 Si1 C30 109.93(10) . . ? N2 Si1 C29 113.45(9) . . ? C31 Si1 C29 103.32(10) . . ? C30 Si1 C29 107.53(9) . . ? N2 Si2 C34 113.35(7) . . ? N2 Si2 C33 114.06(9) . . ? C34 Si2 C33 103.43(10) . . ? N2 Si2 C32 111.89(8) . . ? C34 Si2 C32 107.00(10) . . ? C33 Si2 C32 106.42(9) . . ? N3 Si3 C37 109.83(7) . . ? N3 Si3 C36 112.14(7) . . ? C37 Si3 C36 110.16(8) . . ? N3 Si3 C35 115.24(8) . . ? C37 Si3 C35 106.21(9) . . ? C36 Si3 C35 102.92(8) . . ? N3 Si4 C39 112.67(9) . . ? N3 Si4 C40 114.59(7) . . ? C39 Si4 C40 103.80(11) . . ? N3 Si4 C38 112.82(8) . . ? C39 Si4 C38 108.12(12) . . ? C40 Si4 C38 104.05(9) . . ? C1 O1 Fe1 119.47(9) . . ? C15 O2 Fe1 117.15(9) . . ? C20 N1 C6 130.06(13) . . ? C20 N1 Fe1 113.87(9) . . ? C6 N1 Fe1 115.71(9) . . ? Si1 N2 Si2 120.17(7) . . ? Si1 N2 Fe1 116.86(7) . . ? Si2 N2 Fe1 122.37(7) . . ? Si4 N3 Si3 120.78(7) . . ? Si4 N3 Fe1 121.92(7) . . ? Si3 N3 Fe1 115.90(7) . . ? O1 C1 C2 122.16(13) . . ? O1 C1 C6 118.62(13) . . ? C2 C1 C6 119.22(13) . . ? C3 C2 C1 116.51(13) . . ? C3 C2 C7 122.96(13) . . ? C1 C2 C7 120.29(12) . . ? C2 C3 C4 124.77(13) . . ? C5 C4 C3 118.56(13) . . ? C5 C4 C11 122.95(13) . . ? C3 C4 C11 118.44(13) . . ? C4 C5 C6 120.71(14) . . ? N1 C6 C5 129.10(13) . . ? N1 C6 C1 111.22(12) . . ? C5 C6 C1 119.57(13) . . ? C2 C7 C8 111.73(12) . . ? C2 C7 C9 112.48(13) . . ? C8 C7 C9 107.34(13) . . ? C2 C7 C10 106.69(12) . . ? C8 C7 C10 108.64(13) . . ? C9 C7 C10 109.91(13) . . ? C14 C11 C4 108.82(13) . . ? C14 C11 C12 108.78(14) . . ? C4 C11 C12 111.60(13) . . ? C14 C11 C13 109.03(14) . . ? C4 C11 C13 110.35(12) . . ? C12 C11 C13 108.20(14) . . ? O2 C15 C16 123.31(13) . . ? O2 C15 C20 118.48(13) . . ? C16 C15 C20 118.18(12) . . ? C17 C16 C15 116.68(13) . . ? C17 C16 C21 121.47(13) . . ? C15 C16 C21 121.71(12) . . ? C16 C17 C18 125.45(14) . . ? C19 C18 C17 118.54(13) . . ? C19 C18 C25 123.39(14) . . ? C17 C18 C25 118.03(13) . . ? C18 C19 C20 120.36(14) . . ? N1 C20 C19 128.07(14) . . ? N1 C20 C15 111.73(12) . . ? C19 C20 C15 120.17(13) . . ? C24 C21 C16 111.80(13) . . ? C24 C21 C23 107.33(13) . . ? C16 C21 C23 111.88(13) . . ? C24 C21 C22 109.99(14) . . ? C16 C21 C22 107.74(13) . . ? C23 C21 C22 108.05(14) . . ? C28 C25 C27 109.05(16) . . ? C28 C25 C18 109.81(14) . . ? C27 C25 C18 111.85(13) . . ? C28 C25 C26 109.72(16) . . ? C27 C25 C26 107.95(15) . . ? C18 C25 C26 108.42(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Fe1 O1 C1 137.18(11) . . . . ? N3 Fe1 O1 C1 -100.41(11) . . . . ? O2 Fe1 O1 C1 30.74(14) . . . . ? N1 Fe1 O1 C1 -0.03(10) . . . . ? N2 Fe1 O2 C15 -150.13(10) . . . . ? N3 Fe1 O2 C15 87.13(10) . . . . ? O1 Fe1 O2 C15 -45.96(13) . . . . ? N1 Fe1 O2 C15 -15.11(10) . . . . ? N2 Fe1 N1 C20 105.68(11) . . . . ? N3 Fe1 N1 C20 -75.20(11) . . . . ? O1 Fe1 N1 C20 -178.65(11) . . . . ? O2 Fe1 N1 C20 19.83(10) . . . . ? N2 Fe1 N1 C6 -80.44(12) . . . . ? N3 Fe1 N1 C6 98.67(10) . . . . ? O1 Fe1 N1 C6 -4.78(10) . . . . ? O2 Fe1 N1 C6 -166.30(11) . . . . ? C31 Si1 N2 Si2 -147.88(10) . . . . ? C30 Si1 N2 Si2 89.36(10) . . . . ? C29 Si1 N2 Si2 -32.11(12) . . . . ? C31 Si1 N2 Fe1 23.47(11) . . . . ? C30 Si1 N2 Fe1 -99.29(9) . . . . ? C29 Si1 N2 Fe1 139.24(9) . . . . ? C34 Si2 N2 Si1 -173.80(9) . . . . ? C33 Si2 N2 Si1 68.18(11) . . . . ? C32 Si2 N2 Si1 -52.69(11) . . . . ? C34 Si2 N2 Fe1 15.34(12) . . . . ? C33 Si2 N2 Fe1 -102.68(10) . . . . ? C32 Si2 N2 Fe1 136.45(10) . . . . ? N3 Fe1 N2 Si1 150.02(7) . . . . ? O1 Fe1 N2 Si1 -99.94(7) . . . . ? O2 Fe1 N2 Si1 44.79(8) . . . . ? N1 Fe1 N2 Si1 -30.98(11) . . . . ? N3 Fe1 N2 Si2 -38.84(10) . . . . ? O1 Fe1 N2 Si2 71.21(8) . . . . ? O2 Fe1 N2 Si2 -144.06(7) . . . . ? N1 Fe1 N2 Si2 140.17(7) . . . . ? C39 Si4 N3 Si3 137.47(12) . . . . ? C40 Si4 N3 Si3 19.09(12) . . . . ? C38 Si4 N3 Si3 -99.74(11) . . . . ? C39 Si4 N3 Fe1 -56.59(13) . . . . ? C40 Si4 N3 Fe1 -174.98(9) . . . . ? C38 Si4 N3 Fe1 66.19(11) . . . . ? C37 Si3 N3 Si4 68.64(10) . . . . ? C36 Si3 N3 Si4 -168.53(8) . . . . ? C35 Si3 N3 Si4 -51.24(11) . . . . ? C37 Si3 N3 Fe1 -98.11(9) . . . . ? C36 Si3 N3 Fe1 24.73(10) . . . . ? C35 Si3 N3 Fe1 142.02(9) . . . . ? N2 Fe1 N3 Si4 133.37(7) . . . . ? O1 Fe1 N3 Si4 31.63(9) . . . . ? O2 Fe1 N3 Si4 -121.41(8) . . . . ? N1 Fe1 N3 Si4 -45.92(9) . . . . ? N2 Fe1 N3 Si3 -60.05(9) . . . . ? O1 Fe1 N3 Si3 -161.79(6) . . . . ? O2 Fe1 N3 Si3 45.17(7) . . . . ? N1 Fe1 N3 Si3 120.66(7) . . . . ? Fe1 O1 C1 C2 -175.58(10) . . . . ? Fe1 O1 C1 C6 4.60(17) . . . . ? O1 C1 C2 C3 -170.75(14) . . . . ? C6 C1 C2 C3 9.1(2) . . . . ? O1 C1 C2 C7 14.7(2) . . . . ? C6 C1 C2 C7 -165.53(13) . . . . ? C1 C2 C3 C4 -7.0(2) . . . . ? C7 C2 C3 C4 167.43(14) . . . . ? C2 C3 C4 C5 0.1(2) . . . . ? C2 C3 C4 C11 -177.26(14) . . . . ? C3 C4 C5 C6 4.7(2) . . . . ? C11 C4 C5 C6 -178.06(13) . . . . ? C20 N1 C6 C5 -3.1(3) . . . . ? Fe1 N1 C6 C5 -175.79(12) . . . . ? C20 N1 C6 C1 -179.26(14) . . . . ? Fe1 N1 C6 C1 8.07(15) . . . . ? C4 C5 C6 N1 -178.14(14) . . . . ? C4 C5 C6 C1 -2.3(2) . . . . ? O1 C1 C6 N1 -8.42(19) . . . . ? C2 C1 C6 N1 171.75(13) . . . . ? O1 C1 C6 C5 175.02(13) . . . . ? C2 C1 C6 C5 -4.8(2) . . . . ? C3 C2 C7 C8 4.0(2) . . . . ? C1 C2 C7 C8 178.21(14) . . . . ? C3 C2 C7 C9 124.79(16) . . . . ? C1 C2 C7 C9 -60.98(18) . . . . ? C3 C2 C7 C10 -114.62(16) . . . . ? C1 C2 C7 C10 59.61(18) . . . . ? C5 C4 C11 C14 112.75(17) . . . . ? C3 C4 C11 C14 -69.99(17) . . . . ? C5 C4 C11 C12 -7.3(2) . . . . ? C3 C4 C11 C12 169.96(14) . . . . ? C5 C4 C11 C13 -127.65(16) . . . . ? C3 C4 C11 C13 49.61(18) . . . . ? Fe1 O2 C15 C16 -173.36(10) . . . . ? Fe1 O2 C15 C20 8.92(17) . . . . ? O2 C15 C16 C17 175.97(13) . . . . ? C20 C15 C16 C17 -6.3(2) . . . . ? O2 C15 C16 C21 -8.3(2) . . . . ? C20 C15 C16 C21 169.40(13) . . . . ? C15 C16 C17 C18 0.1(2) . . . . ? C21 C16 C17 C18 -175.59(14) . . . . ? C16 C17 C18 C19 3.1(2) . . . . ? C16 C17 C18 C25 -178.93(14) . . . . ? C17 C18 C19 C20 0.2(2) . . . . ? C25 C18 C19 C20 -177.63(14) . . . . ? C6 N1 C20 C19 -12.3(3) . . . . ? Fe1 N1 C20 C19 160.43(13) . . . . ? C6 N1 C20 C15 166.02(14) . . . . ? Fe1 N1 C20 C15 -21.20(15) . . . . ? C18 C19 C20 N1 171.78(15) . . . . ? C18 C19 C20 C15 -6.5(2) . . . . ? O2 C15 C20 N1 8.88(19) . . . . ? C16 C15 C20 N1 -168.96(12) . . . . ? O2 C15 C20 C19 -172.61(13) . . . . ? C16 C15 C20 C19 9.6(2) . . . . ? C17 C16 C21 C24 -127.70(16) . . . . ? C15 C16 C21 C24 56.80(19) . . . . ? C17 C16 C21 C23 -7.3(2) . . . . ? C15 C16 C21 C23 177.22(13) . . . . ? C17 C16 C21 C22 111.34(16) . . . . ? C15 C16 C21 C22 -64.17(18) . . . . ? C19 C18 C25 C28 -122.66(18) . . . . ? C17 C18 C25 C28 59.5(2) . . . . ? C19 C18 C25 C27 -1.4(2) . . . . ? C17 C18 C25 C27 -179.29(16) . . . . ? C19 C18 C25 C26 117.47(17) . . . . ? C17 C18 C25 C26 -60.37(19) . . . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.453 _refine_diff_density_min -0.240 _refine_diff_density_rms 0.051 data_afh333 _database_code_depnum_ccdc_archive 'CCDC 916894' #TrackingRef '[ONO]Fe_CIF.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; {[ONO]Fe(ortho-C6O2Cl4)}2 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75.50 H98 Cl8 Fe2 N2 O8' _chemical_formula_weight 1556.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.8709(8) _cell_length_b 15.7470(8) _cell_length_c 17.9214(10) _cell_angle_alpha 94.0663(7) _cell_angle_beta 111.4278(7) _cell_angle_gamma 95.5142(7) _cell_volume 3863.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 9975 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 26.37 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1634 _exptl_absorpt_coefficient_mu 0.706 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8682 _exptl_absorpt_correction_T_max 0.9424 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 42365 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 26.40 _reflns_number_total 15780 _reflns_number_gt 11327 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. There were 1.5 molecules of pentane solvent present per formula-unit. One solvent molecule was located about an inversion center and disordered. The disordered solvent was included using partial site-occupancy factors and equivalent positional and thermal parameters (EXYZ, EADP). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+0.6266P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15780 _refine_ls_number_parameters 893 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.0999 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.71150(2) 0.66770(2) 0.79276(2) 0.01624(9) Uani 1 1 d . . . Fe2 Fe 0.72806(2) 0.83465(2) 0.69460(2) 0.01687(9) Uani 1 1 d . . . Cl1 Cl 0.61456(5) 0.51163(4) 0.64491(4) 0.02479(14) Uani 1 1 d . . . Cl2 Cl 0.61426(5) 0.43523(4) 0.47877(4) 0.02954(16) Uani 1 1 d . . . Cl3 Cl 0.65078(6) 0.55944(4) 0.36100(4) 0.03501(17) Uani 1 1 d . . . Cl4 Cl 0.70692(5) 0.75775(4) 0.41809(4) 0.02882(15) Uani 1 1 d . . . Cl5 Cl 0.81020(5) 0.99396(4) 0.84687(4) 0.03189(16) Uani 1 1 d . . . Cl6 Cl 0.91512(5) 1.05138(4) 1.03133(4) 0.03088(16) Uani 1 1 d . . . Cl7 Cl 0.94104(5) 0.91548(4) 1.15316(4) 0.03384(17) Uani 1 1 d . . . Cl8 Cl 0.85521(5) 0.72261(4) 1.08936(4) 0.02694(15) Uani 1 1 d . . . O1 O 0.81709(11) 0.60306(10) 0.77986(10) 0.0189(4) Uani 1 1 d . . . O2 O 0.57603(11) 0.66407(10) 0.78914(10) 0.0185(4) Uani 1 1 d . . . O3 O 0.87329(11) 0.84870(10) 0.72157(10) 0.0195(4) Uani 1 1 d . . . O4 O 0.60466(11) 0.88507(10) 0.67576(10) 0.0199(4) Uani 1 1 d . . . O5 O 0.68077(11) 0.70367(10) 0.68116(9) 0.0170(4) Uani 1 1 d . . . O6 O 0.74914(11) 0.80090(10) 0.80658(9) 0.0175(4) Uani 1 1 d . . . O7 O 0.77379(12) 0.69076(10) 0.90988(10) 0.0211(4) Uani 1 1 d . . . O8 O 0.70981(12) 0.80377(10) 0.58222(10) 0.0203(4) Uani 1 1 d . . . N1 N 0.68185(14) 0.54276(12) 0.82708(11) 0.0162(4) Uani 1 1 d . . . N2 N 0.76140(14) 0.96388(12) 0.67098(12) 0.0174(4) Uani 1 1 d . . . C1 C 0.75784(17) 0.49794(15) 0.84453(14) 0.0172(5) Uani 1 1 d . . . C2 C 0.82688(17) 0.53119(15) 0.80976(14) 0.0178(5) Uani 1 1 d . . . C3 C 0.90138(17) 0.47950(15) 0.80746(14) 0.0183(5) Uani 1 1 d . . . C4 C 0.91211(17) 0.41144(15) 0.85117(15) 0.0211(5) Uani 1 1 d . . . H4A H 0.9625 0.3783 0.8520 0.025 Uiso 1 1 calc R . . C5 C 0.85347(17) 0.38524(15) 0.89636(15) 0.0191(5) Uani 1 1 d . . . C6 C 0.77648(17) 0.42748(15) 0.89090(14) 0.0186(5) Uani 1 1 d . . . H6A H 0.7349 0.4100 0.9181 0.022 Uiso 1 1 calc R . . C7 C 0.96258(18) 0.50163(16) 0.75723(15) 0.0224(6) Uani 1 1 d . . . C8 C 0.8946(2) 0.50687(19) 0.66948(16) 0.0325(7) Uani 1 1 d . . . H8A H 0.8536 0.4516 0.6471 0.049 Uiso 1 1 calc R . . H8B H 0.9337 0.5204 0.6372 0.049 Uiso 1 1 calc R . . H8C H 0.8532 0.5519 0.6684 0.049 Uiso 1 1 calc R . . C9 C 1.02746(19) 0.58767(17) 0.79137(17) 0.0305(6) Uani 1 1 d . . . H9A H 1.0723 0.5841 0.8466 0.046 Uiso 1 1 calc R . . H9B H 0.9867 0.6330 0.7917 0.046 Uiso 1 1 calc R . . H9C H 1.0649 0.6011 0.7577 0.046 Uiso 1 1 calc R . . C10 C 1.0283(2) 0.43311(18) 0.75559(19) 0.0371(7) Uani 1 1 d . . . H10A H 0.9886 0.3768 0.7363 0.056 Uiso 1 1 calc R . . H10B H 1.0763 0.4319 0.8101 0.056 Uiso 1 1 calc R . . H10C H 1.0622 0.4468 0.7193 0.056 Uiso 1 1 calc R . . C11 C 0.88086(18) 0.31130(16) 0.94765(15) 0.0227(6) Uani 1 1 d . . . C12 C 0.98294(19) 0.33788(18) 1.01248(16) 0.0291(6) Uani 1 1 d . . . H12A H 0.9829 0.3900 1.0458 0.044 Uiso 1 1 calc R . . H12B H 1.0299 0.3491 0.9865 0.044 Uiso 1 1 calc R . . H12C H 1.0012 0.2915 1.0466 0.044 Uiso 1 1 calc R . . C13 C 0.8797(2) 0.23046(16) 0.89368(16) 0.0297(6) Uani 1 1 d . . . H13A H 0.8133 0.2123 0.8545 0.045 Uiso 1 1 calc R . . H13B H 0.9017 0.1843 0.9272 0.045 Uiso 1 1 calc R . . H13C H 0.9234 0.2433 0.8650 0.045 Uiso 1 1 calc R . . C14 C 0.80939(19) 0.29034(17) 0.98925(17) 0.0299(6) Uani 1 1 d . . . H14A H 0.7437 0.2736 0.9484 0.045 Uiso 1 1 calc R . . H14B H 0.8096 0.3411 1.0243 0.045 Uiso 1 1 calc R . . H14C H 0.8291 0.2429 1.0217 0.045 Uiso 1 1 calc R . . C15 C 0.59580(17) 0.52787(15) 0.83515(14) 0.0164(5) Uani 1 1 d . . . C16 C 0.53943(16) 0.59918(15) 0.81279(14) 0.0163(5) Uani 1 1 d . . . C17 C 0.44503(17) 0.59419(15) 0.81832(14) 0.0186(5) Uani 1 1 d . . . C18 C 0.41247(18) 0.52023(16) 0.84118(15) 0.0212(5) Uani 1 1 d . . . H18A H 0.3502 0.5165 0.8450 0.025 Uiso 1 1 calc R . . C19 C 0.46483(17) 0.44758(15) 0.85995(14) 0.0184(5) Uani 1 1 d . . . C20 C 0.55480(17) 0.45246(15) 0.85682(14) 0.0179(5) Uani 1 1 d . . . H20A H 0.5909 0.4053 0.8692 0.021 Uiso 1 1 calc R . . C21 C 0.38592(19) 0.66916(17) 0.79819(17) 0.0266(6) Uani 1 1 d . . . C22 C 0.36473(19) 0.68502(17) 0.71035(16) 0.0307(6) Uani 1 1 d . . . H22A H 0.3316 0.6321 0.6747 0.046 Uiso 1 1 calc R . . H22B H 0.4261 0.7025 0.7037 0.046 Uiso 1 1 calc R . . H22C H 0.3229 0.7306 0.6965 0.046 Uiso 1 1 calc R . . C23 C 0.2884(2) 0.6504(2) 0.8087(2) 0.0487(9) Uani 1 1 d . . . H23A H 0.2496 0.6003 0.7713 0.073 Uiso 1 1 calc R . . H23B H 0.2530 0.7003 0.7972 0.073 Uiso 1 1 calc R . . H23C H 0.3004 0.6386 0.8642 0.073 Uiso 1 1 calc R . . C24 C 0.4428(2) 0.75044(17) 0.85574(17) 0.0348(7) Uani 1 1 d . . . H24A H 0.5040 0.7660 0.8481 0.052 Uiso 1 1 calc R . . H24B H 0.4570 0.7391 0.9117 0.052 Uiso 1 1 calc R . . H24C H 0.4035 0.7979 0.8439 0.052 Uiso 1 1 calc R . . C25 C 0.41655(18) 0.36862(16) 0.88254(15) 0.0218(5) Uani 1 1 d . . . C26 C 0.32332(19) 0.33101(17) 0.81047(16) 0.0298(6) Uani 1 1 d . . . H26A H 0.2791 0.3747 0.7960 0.045 Uiso 1 1 calc R . . H26B H 0.2912 0.2813 0.8251 0.045 Uiso 1 1 calc R . . H26C H 0.3403 0.3131 0.7643 0.045 Uiso 1 1 calc R . . C27 C 0.3905(2) 0.39443(17) 0.95529(16) 0.0296(6) Uani 1 1 d . . . H27A H 0.4499 0.4191 1.0009 0.044 Uiso 1 1 calc R . . H27B H 0.3602 0.3436 0.9700 0.044 Uiso 1 1 calc R . . H27C H 0.3449 0.4371 0.9416 0.044 Uiso 1 1 calc R . . C28 C 0.4838(2) 0.29931(16) 0.90414(17) 0.0299(6) Uani 1 1 d . . . H28A H 0.5441 0.3226 0.9495 0.045 Uiso 1 1 calc R . . H28B H 0.4993 0.2805 0.8574 0.045 Uiso 1 1 calc R . . H28C H 0.4512 0.2503 0.9194 0.045 Uiso 1 1 calc R . . C29 C 0.84969(17) 0.98060(15) 0.66712(14) 0.0177(5) Uani 1 1 d . . . C30 C 0.90767(17) 0.91049(15) 0.69338(14) 0.0174(5) Uani 1 1 d . . . C31 C 1.00202(17) 0.91521(15) 0.68788(14) 0.0196(5) Uani 1 1 d . . . C32 C 1.03488(18) 0.98890(15) 0.66448(14) 0.0206(5) Uani 1 1 d . . . H32A H 1.0990 0.9941 0.6644 0.025 Uiso 1 1 calc R . . C33 C 0.97937(18) 1.05957(15) 0.63990(14) 0.0202(5) Uani 1 1 d . . . C34 C 0.88766(18) 1.05289(15) 0.63958(15) 0.0210(5) Uani 1 1 d . . . H34A H 0.8484 1.0970 0.6208 0.025 Uiso 1 1 calc R . . C35 C 1.06030(18) 0.83915(16) 0.70659(16) 0.0236(6) Uani 1 1 d . . . C36 C 1.08687(19) 0.82485(17) 0.79537(15) 0.0269(6) Uani 1 1 d . . . H36A H 1.1261 0.8766 0.8298 0.040 Uiso 1 1 calc R . . H36B H 1.1244 0.7762 0.8070 0.040 Uiso 1 1 calc R . . H36C H 1.0271 0.8126 0.8061 0.040 Uiso 1 1 calc R . . C37 C 0.9987(2) 0.75814(16) 0.65105(16) 0.0294(6) Uani 1 1 d . . . H37A H 0.9781 0.7697 0.5946 0.044 Uiso 1 1 calc R . . H37B H 0.9411 0.7429 0.6640 0.044 Uiso 1 1 calc R . . H37C H 1.0378 0.7105 0.6593 0.044 Uiso 1 1 calc R . . C38 C 1.1548(2) 0.85502(19) 0.69107(18) 0.0344(7) Uani 1 1 d . . . H38A H 1.1969 0.9043 0.7278 0.052 Uiso 1 1 calc R . . H38B H 1.1395 0.8670 0.6351 0.052 Uiso 1 1 calc R . . H38C H 1.1884 0.8040 0.7003 0.052 Uiso 1 1 calc R . . C39 C 1.02650(19) 1.13707(16) 0.61443(16) 0.0252(6) Uani 1 1 d . . . C40 C 0.9568(2) 1.20388(18) 0.5876(2) 0.0498(9) Uani 1 1 d . . . H40A H 0.8983 1.1780 0.5417 0.075 Uiso 1 1 calc R . . H40B H 0.9890 1.2525 0.5715 0.075 Uiso 1 1 calc R . . H40C H 0.9383 1.2240 0.6323 0.075 Uiso 1 1 calc R . . C41 C 1.0551(2) 1.10970(18) 0.54404(17) 0.0345(7) Uani 1 1 d . . . H41A H 0.9965 1.0867 0.4971 0.052 Uiso 1 1 calc R . . H41B H 1.0984 1.0653 0.5588 0.052 Uiso 1 1 calc R . . H41C H 1.0890 1.1594 0.5308 0.052 Uiso 1 1 calc R . . C42 C 1.1178(2) 1.1778(2) 0.68532(18) 0.0463(9) Uani 1 1 d . . . H42A H 1.1630 1.1352 0.7024 0.070 Uiso 1 1 calc R . . H42B H 1.0998 1.1980 0.7303 0.070 Uiso 1 1 calc R . . H42C H 1.1494 1.2265 0.6688 0.070 Uiso 1 1 calc R . . C43 C 0.69036(17) 1.01330(15) 0.66192(14) 0.0177(5) Uani 1 1 d . . . C44 C 0.60208(17) 0.96382(15) 0.66149(14) 0.0178(5) Uani 1 1 d . . . C45 C 0.51569(17) 1.00583(15) 0.64542(15) 0.0194(5) Uani 1 1 d . . . C46 C 0.52614(18) 1.09163(15) 0.63971(15) 0.0217(5) Uani 1 1 d . . . H46A H 0.4694 1.1195 0.6275 0.026 Uiso 1 1 calc R . . C47 C 0.61583(18) 1.14370(15) 0.65065(15) 0.0201(5) Uani 1 1 d . . . C48 C 0.69563(18) 1.10396(15) 0.66037(15) 0.0199(5) Uani 1 1 d . . . H48A H 0.7554 1.1367 0.6662 0.024 Uiso 1 1 calc R . . C49 C 0.41873(18) 0.95501(16) 0.63736(16) 0.0247(6) Uani 1 1 d . . . C50 C 0.4292(2) 0.92293(18) 0.71849(17) 0.0326(7) Uani 1 1 d . . . H50A H 0.4447 0.9722 0.7597 0.049 Uiso 1 1 calc R . . H50B H 0.4816 0.8867 0.7341 0.049 Uiso 1 1 calc R . . H50C H 0.3678 0.8894 0.7135 0.049 Uiso 1 1 calc R . . C51 C 0.33579(19) 1.01053(18) 0.6137(2) 0.0400(8) Uani 1 1 d . . . H51A H 0.3491 1.0576 0.6566 0.060 Uiso 1 1 calc R . . H51B H 0.2743 0.9753 0.6058 0.060 Uiso 1 1 calc R . . H51C H 0.3309 1.0343 0.5634 0.060 Uiso 1 1 calc R . . C52 C 0.3912(2) 0.87834(18) 0.57211(17) 0.0353(7) Uani 1 1 d . . . H52A H 0.3868 0.8989 0.5207 0.053 Uiso 1 1 calc R . . H52B H 0.3281 0.8475 0.5662 0.053 Uiso 1 1 calc R . . H52C H 0.4411 0.8396 0.5877 0.053 Uiso 1 1 calc R . . C53 C 0.61657(18) 1.24062(15) 0.65170(16) 0.0226(6) Uani 1 1 d . . . C54 C 0.5435(2) 1.26102(17) 0.57109(16) 0.0300(6) Uani 1 1 d . . . H54A H 0.4802 1.2269 0.5591 0.045 Uiso 1 1 calc R . . H54B H 0.5672 1.2470 0.5280 0.045 Uiso 1 1 calc R . . H54C H 0.5364 1.3222 0.5747 0.045 Uiso 1 1 calc R . . C55 C 0.5865(2) 1.27498(17) 0.72030(17) 0.0312(6) Uani 1 1 d . . . H55A H 0.6322 1.2614 0.7719 0.047 Uiso 1 1 calc R . . H55B H 0.5206 1.2481 0.7114 0.047 Uiso 1 1 calc R . . H55C H 0.5874 1.3374 0.7214 0.047 Uiso 1 1 calc R . . C56 C 0.71735(19) 1.28706(16) 0.66481(18) 0.0315(7) Uani 1 1 d . . . H56A H 0.7641 1.2770 0.7174 0.047 Uiso 1 1 calc R . . H56B H 0.7141 1.3488 0.6634 0.047 Uiso 1 1 calc R . . H56C H 0.7383 1.2651 0.6221 0.047 Uiso 1 1 calc R . . C57 C 0.67147(16) 0.66473(15) 0.60856(14) 0.0172(5) Uani 1 1 d . . . C58 C 0.64543(17) 0.57799(15) 0.58293(15) 0.0194(5) Uani 1 1 d . . . C59 C 0.64124(18) 0.54479(15) 0.50755(15) 0.0218(6) Uani 1 1 d . . . C60 C 0.66069(18) 0.59950(16) 0.45627(15) 0.0224(6) Uani 1 1 d . . . C61 C 0.68512(18) 0.68721(16) 0.48106(15) 0.0205(5) Uani 1 1 d . . . C62 C 0.69037(17) 0.72119(15) 0.55666(15) 0.0180(5) Uani 1 1 d . . . C63 C 0.79344(17) 0.83361(15) 0.88503(15) 0.0187(5) Uani 1 1 d . . . C64 C 0.82609(18) 0.91877(15) 0.91423(15) 0.0210(5) Uani 1 1 d . . . C65 C 0.87181(18) 0.94467(15) 0.99698(15) 0.0225(6) Uani 1 1 d . . . C66 C 0.88329(18) 0.88464(16) 1.05106(15) 0.0236(6) Uani 1 1 d . . . C67 C 0.84839(18) 0.79823(16) 1.02253(15) 0.0204(5) Uani 1 1 d . . . C68 C 0.80523(17) 0.77168(15) 0.94007(15) 0.0177(5) Uani 1 1 d . . . C69 C 0.6803(3) 0.9315(2) 1.1432(2) 0.0591(10) Uani 1 1 d . . . H69A H 0.6680 0.8760 1.1616 0.089 Uiso 1 1 calc R . . H69B H 0.6514 0.9748 1.1658 0.089 Uiso 1 1 calc R . . H69C H 0.7507 0.9486 1.1612 0.089 Uiso 1 1 calc R . . C70 C 0.6353(2) 0.9237(2) 1.0522(2) 0.0466(8) Uani 1 1 d . . . H70A H 0.5651 0.9020 1.0343 0.056 Uiso 1 1 calc R . . H70B H 0.6662 0.8811 1.0298 0.056 Uiso 1 1 calc R . . C71 C 0.6464(2) 1.0084(2) 1.0185(2) 0.0447(8) Uani 1 1 d . . . H71A H 0.6162 1.0511 1.0417 0.054 Uiso 1 1 calc R . . H71B H 0.7167 1.0296 1.0361 0.054 Uiso 1 1 calc R . . C72 C 0.6011(2) 1.0026(2) 0.9278(2) 0.0480(9) Uani 1 1 d . . . H72A H 0.5306 0.9823 0.9101 0.058 Uiso 1 1 calc R . . H72B H 0.6305 0.9593 0.9045 0.058 Uiso 1 1 calc R . . C73 C 0.6141(3) 1.0883(2) 0.8945(2) 0.0620(11) Uani 1 1 d . . . H73A H 0.5838 1.0801 0.8354 0.093 Uiso 1 1 calc R . . H73B H 0.6838 1.1086 0.9111 0.093 Uiso 1 1 calc R . . H73C H 0.5831 1.1310 0.9157 0.093 Uiso 1 1 calc R . . C74 C 0.0144(3) 0.5468(3) 0.4990(2) 0.0855(17) Uani 1 1 d . . . H74A H -0.0198 0.5817 0.5255 0.103 Uiso 1 1 calc R A 1 H74B H -0.0057 0.5593 0.4422 0.103 Uiso 1 1 calc R A 1 C75 C 0.1237(3) 0.5714(4) 0.5416(3) 0.1022(19) Uani 0.50 1 d P B 1 H75A H 0.1408 0.5726 0.6005 0.123 Uiso 0.50 1 calc PR B 1 H75B H 0.1573 0.5269 0.5248 0.123 Uiso 0.50 1 calc PR B 1 C76 C 0.1562(6) 0.6480(5) 0.5260(4) 0.061(2) Uani 0.50 1 d P B 1 H76A H 0.2271 0.6595 0.5539 0.092 Uiso 0.50 1 calc PR B 1 H76B H 0.1258 0.6930 0.5450 0.092 Uiso 0.50 1 calc PR B 1 H76C H 0.1393 0.6475 0.4677 0.092 Uiso 0.50 1 calc PR B 1 C77 C 0.1237(3) 0.5714(4) 0.5416(3) 0.1022(19) Uani 0.50 1 d P B 2 H77A H 0.1392 0.6341 0.5491 0.153 Uiso 0.50 1 calc PR B 2 H77B H 0.1570 0.5466 0.5089 0.153 Uiso 0.50 1 calc PR B 2 H77C H 0.1454 0.5495 0.5943 0.153 Uiso 0.50 1 calc PR B 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 0.01737(18) 0.01261(17) 0.02091(19) 0.00522(14) 0.00907(15) 0.00211(14) Fe2 0.01797(18) 0.01215(17) 0.02247(19) 0.00588(14) 0.00893(15) 0.00296(14) Cl1 0.0341(4) 0.0170(3) 0.0239(3) 0.0056(2) 0.0121(3) -0.0010(3) Cl2 0.0436(4) 0.0165(3) 0.0283(4) 0.0009(3) 0.0145(3) 0.0000(3) Cl3 0.0576(5) 0.0262(4) 0.0256(4) 0.0009(3) 0.0221(3) 0.0011(3) Cl4 0.0389(4) 0.0245(3) 0.0286(4) 0.0083(3) 0.0194(3) -0.0009(3) Cl5 0.0494(4) 0.0177(3) 0.0276(4) 0.0059(3) 0.0134(3) 0.0016(3) Cl6 0.0420(4) 0.0188(3) 0.0309(4) -0.0023(3) 0.0149(3) -0.0024(3) Cl7 0.0452(4) 0.0315(4) 0.0210(3) -0.0011(3) 0.0110(3) -0.0039(3) Cl8 0.0315(4) 0.0265(3) 0.0244(3) 0.0086(3) 0.0118(3) 0.0019(3) O1 0.0187(9) 0.0161(9) 0.0262(10) 0.0073(7) 0.0122(8) 0.0039(7) O2 0.0165(9) 0.0156(9) 0.0260(9) 0.0072(7) 0.0101(7) 0.0026(7) O3 0.0170(9) 0.0172(9) 0.0269(10) 0.0082(7) 0.0102(8) 0.0027(7) O4 0.0175(9) 0.0152(9) 0.0300(10) 0.0077(7) 0.0108(8) 0.0049(7) O5 0.0207(9) 0.0124(8) 0.0193(9) 0.0048(7) 0.0083(7) 0.0035(7) O6 0.0200(9) 0.0129(8) 0.0205(9) 0.0034(7) 0.0086(7) 0.0017(7) O7 0.0253(10) 0.0161(9) 0.0219(9) 0.0041(7) 0.0084(8) 0.0031(7) O8 0.0254(9) 0.0147(9) 0.0224(9) 0.0043(7) 0.0106(8) 0.0013(7) N1 0.0181(10) 0.0130(10) 0.0193(11) 0.0032(8) 0.0090(9) 0.0023(8) N2 0.0169(10) 0.0148(10) 0.0220(11) 0.0041(8) 0.0084(9) 0.0029(8) C1 0.0161(12) 0.0157(12) 0.0198(13) 0.0018(10) 0.0070(10) 0.0009(10) C2 0.0172(12) 0.0162(12) 0.0189(13) 0.0030(10) 0.0058(10) 0.0007(10) C3 0.0180(12) 0.0142(12) 0.0225(13) 0.0010(10) 0.0077(11) 0.0016(10) C4 0.0194(13) 0.0176(13) 0.0262(14) 0.0020(10) 0.0079(11) 0.0055(10) C5 0.0183(13) 0.0147(12) 0.0220(13) 0.0028(10) 0.0058(11) -0.0007(10) C6 0.0185(13) 0.0165(12) 0.0215(13) 0.0054(10) 0.0086(11) -0.0003(10) C7 0.0232(14) 0.0223(14) 0.0286(14) 0.0069(11) 0.0161(12) 0.0066(11) C8 0.0325(16) 0.0415(17) 0.0293(16) 0.0066(13) 0.0176(13) 0.0065(13) C9 0.0248(14) 0.0329(16) 0.0407(17) 0.0086(13) 0.0204(13) 0.0003(12) C10 0.0412(18) 0.0359(17) 0.054(2) 0.0181(15) 0.0347(16) 0.0198(14) C11 0.0220(13) 0.0206(13) 0.0266(14) 0.0090(11) 0.0086(11) 0.0053(11) C12 0.0261(15) 0.0357(16) 0.0257(15) 0.0100(12) 0.0072(12) 0.0109(12) C13 0.0331(16) 0.0204(14) 0.0358(16) 0.0128(12) 0.0104(13) 0.0072(12) C14 0.0284(15) 0.0283(15) 0.0379(17) 0.0195(13) 0.0143(13) 0.0070(12) C15 0.0172(12) 0.0161(12) 0.0169(12) 0.0006(9) 0.0080(10) 0.0017(10) C16 0.0154(12) 0.0160(12) 0.0174(12) 0.0017(10) 0.0066(10) 0.0010(10) C17 0.0179(12) 0.0169(12) 0.0223(13) 0.0026(10) 0.0086(11) 0.0039(10) C18 0.0173(13) 0.0240(14) 0.0254(14) 0.0038(11) 0.0113(11) 0.0035(10) C19 0.0188(13) 0.0188(13) 0.0190(13) 0.0032(10) 0.0093(10) 0.0002(10) C20 0.0193(13) 0.0145(12) 0.0206(13) 0.0048(10) 0.0077(10) 0.0029(10) C21 0.0241(14) 0.0233(14) 0.0418(17) 0.0128(12) 0.0200(13) 0.0095(11) C22 0.0251(15) 0.0267(15) 0.0395(17) 0.0112(13) 0.0082(13) 0.0103(12) C23 0.0373(18) 0.0399(19) 0.092(3) 0.0328(18) 0.0419(19) 0.0229(15) C24 0.0519(19) 0.0257(15) 0.0377(17) 0.0086(13) 0.0258(15) 0.0165(14) C25 0.0231(13) 0.0191(13) 0.0246(14) 0.0048(10) 0.0118(11) -0.0038(10) C26 0.0293(15) 0.0281(15) 0.0290(15) 0.0036(12) 0.0102(13) -0.0088(12) C27 0.0324(16) 0.0275(15) 0.0315(15) 0.0072(12) 0.0166(13) -0.0051(12) C28 0.0328(16) 0.0215(14) 0.0404(17) 0.0140(12) 0.0184(13) 0.0000(12) C29 0.0190(13) 0.0139(12) 0.0204(13) 0.0009(10) 0.0080(10) 0.0014(10) C30 0.0191(13) 0.0151(12) 0.0186(13) 0.0001(10) 0.0085(10) 0.0013(10) C31 0.0201(13) 0.0214(13) 0.0167(13) 0.0012(10) 0.0062(10) 0.0043(10) C32 0.0192(13) 0.0231(14) 0.0220(13) 0.0025(10) 0.0112(11) 0.0012(10) C33 0.0232(13) 0.0180(13) 0.0212(13) 0.0025(10) 0.0106(11) 0.0014(10) C34 0.0254(14) 0.0140(12) 0.0246(14) 0.0044(10) 0.0100(11) 0.0036(10) C35 0.0218(14) 0.0246(14) 0.0284(15) 0.0064(11) 0.0121(12) 0.0080(11) C36 0.0249(14) 0.0266(15) 0.0319(15) 0.0096(12) 0.0113(12) 0.0097(11) C37 0.0370(16) 0.0215(14) 0.0321(16) 0.0030(12) 0.0139(13) 0.0116(12) C38 0.0279(15) 0.0379(17) 0.0484(19) 0.0175(14) 0.0219(14) 0.0164(13) C39 0.0288(15) 0.0183(13) 0.0316(15) 0.0043(11) 0.0159(12) -0.0020(11) C40 0.055(2) 0.0212(16) 0.092(3) 0.0247(17) 0.046(2) 0.0059(14) C41 0.0426(18) 0.0300(16) 0.0337(17) 0.0080(13) 0.0189(14) -0.0039(13) C42 0.053(2) 0.0451(19) 0.0338(18) 0.0036(15) 0.0169(16) -0.0275(16) C43 0.0198(13) 0.0145(12) 0.0208(13) 0.0055(10) 0.0088(11) 0.0043(10) C44 0.0209(13) 0.0144(12) 0.0208(13) 0.0047(10) 0.0100(11) 0.0039(10) C45 0.0173(13) 0.0193(13) 0.0235(13) 0.0072(10) 0.0085(11) 0.0039(10) C46 0.0221(13) 0.0204(13) 0.0254(14) 0.0058(11) 0.0103(11) 0.0077(11) C47 0.0237(13) 0.0160(12) 0.0217(13) 0.0067(10) 0.0086(11) 0.0043(10) C48 0.0194(13) 0.0160(12) 0.0266(14) 0.0048(10) 0.0113(11) 0.0005(10) C49 0.0183(13) 0.0202(13) 0.0382(16) 0.0095(12) 0.0121(12) 0.0046(10) C50 0.0321(16) 0.0281(15) 0.0474(18) 0.0100(13) 0.0255(14) 0.0032(12) C51 0.0213(15) 0.0291(16) 0.072(2) 0.0199(15) 0.0175(15) 0.0068(12) C52 0.0262(15) 0.0341(17) 0.0363(17) 0.0022(13) 0.0028(13) -0.0032(13) C53 0.0232(14) 0.0142(13) 0.0322(15) 0.0035(11) 0.0119(12) 0.0044(10) C54 0.0352(16) 0.0201(14) 0.0391(17) 0.0124(12) 0.0159(13) 0.0101(12) C55 0.0352(16) 0.0227(14) 0.0372(17) 0.0012(12) 0.0153(14) 0.0051(12) C56 0.0310(16) 0.0150(13) 0.0499(19) 0.0058(12) 0.0163(14) 0.0030(11) C57 0.0133(12) 0.0189(12) 0.0197(13) 0.0048(10) 0.0053(10) 0.0053(10) C58 0.0198(13) 0.0165(12) 0.0233(13) 0.0088(10) 0.0086(11) 0.0032(10) C59 0.0260(14) 0.0144(12) 0.0243(14) 0.0021(10) 0.0089(11) 0.0015(10) C60 0.0253(14) 0.0224(14) 0.0211(13) 0.0016(11) 0.0106(11) 0.0037(11) C61 0.0215(13) 0.0206(13) 0.0236(14) 0.0098(11) 0.0120(11) 0.0034(10) C62 0.0156(12) 0.0136(12) 0.0251(13) 0.0030(10) 0.0074(10) 0.0037(10) C63 0.0158(12) 0.0190(13) 0.0232(13) 0.0032(10) 0.0093(11) 0.0027(10) C64 0.0233(13) 0.0160(13) 0.0269(14) 0.0068(10) 0.0118(11) 0.0044(10) C65 0.0264(14) 0.0165(13) 0.0266(14) -0.0006(11) 0.0134(12) 0.0012(11) C66 0.0225(14) 0.0258(14) 0.0223(14) -0.0006(11) 0.0091(11) 0.0019(11) C67 0.0206(13) 0.0210(13) 0.0249(14) 0.0083(11) 0.0132(11) 0.0040(10) C68 0.0157(12) 0.0158(12) 0.0249(13) 0.0037(10) 0.0106(10) 0.0045(10) C69 0.049(2) 0.053(2) 0.067(3) 0.0014(19) 0.0126(19) 0.0114(18) C70 0.0336(18) 0.043(2) 0.059(2) 0.0016(16) 0.0120(16) 0.0075(15) C71 0.0335(17) 0.0365(18) 0.065(2) -0.0034(16) 0.0212(17) 0.0029(14) C72 0.0403(19) 0.0394(19) 0.068(2) 0.0060(17) 0.0258(18) 0.0014(15) C73 0.061(2) 0.042(2) 0.088(3) 0.007(2) 0.036(2) -0.0021(18) C74 0.050(3) 0.162(5) 0.039(2) -0.010(3) 0.0199(19) -0.009(3) C75 0.063(3) 0.175(6) 0.049(3) 0.016(3) 0.005(2) -0.015(3) C76 0.078(6) 0.059(5) 0.044(4) 0.002(4) 0.019(4) 0.014(4) C77 0.063(3) 0.175(6) 0.049(3) 0.016(3) 0.005(2) -0.015(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 O7 1.9499(17) . ? Fe1 O2 1.9868(16) . ? Fe1 O5 2.0180(16) . ? Fe1 O1 2.0235(16) . ? Fe1 O6 2.0912(16) . ? Fe1 N1 2.1557(19) . ? Fe2 O8 1.9500(17) . ? Fe2 O4 1.9942(16) . ? Fe2 O3 2.0192(16) . ? Fe2 O6 2.0328(16) . ? Fe2 O5 2.0819(16) . ? Fe2 N2 2.1557(19) . ? Cl1 C58 1.727(2) . ? Cl2 C59 1.730(2) . ? Cl3 C60 1.726(2) . ? Cl4 C61 1.729(2) . ? Cl5 C64 1.721(2) . ? Cl6 C65 1.724(2) . ? Cl7 C66 1.723(3) . ? Cl8 C67 1.732(2) . ? O1 C2 1.284(3) . ? O2 C16 1.282(3) . ? O3 C30 1.275(3) . ? O4 C44 1.285(3) . ? O5 C57 1.352(3) . ? O6 C63 1.353(3) . ? O7 C68 1.318(3) . ? O8 C62 1.316(3) . ? N1 C15 1.340(3) . ? N1 C1 1.341(3) . ? N2 C43 1.341(3) . ? N2 C29 1.342(3) . ? C1 C6 1.421(3) . ? C1 C2 1.458(3) . ? C2 C3 1.447(3) . ? C3 C4 1.360(3) . ? C3 C7 1.530(3) . ? C4 C5 1.443(3) . ? C5 C6 1.355(3) . ? C5 C11 1.528(3) . ? C7 C10 1.530(3) . ? C7 C9 1.530(4) . ? C7 C8 1.541(4) . ? C11 C14 1.530(3) . ? C11 C12 1.533(3) . ? C11 C13 1.538(4) . ? C15 C20 1.425(3) . ? C15 C16 1.457(3) . ? C16 C17 1.438(3) . ? C17 C18 1.365(3) . ? C17 C21 1.525(3) . ? C18 C19 1.436(3) . ? C19 C20 1.355(3) . ? C19 C25 1.529(3) . ? C21 C23 1.532(4) . ? C21 C22 1.532(4) . ? C21 C24 1.544(4) . ? C25 C28 1.526(4) . ? C25 C27 1.529(3) . ? C25 C26 1.538(3) . ? C29 C34 1.421(3) . ? C29 C30 1.464(3) . ? C30 C31 1.437(3) . ? C31 C32 1.368(3) . ? C31 C35 1.530(3) . ? C32 C33 1.447(3) . ? C33 C34 1.356(3) . ? C33 C39 1.529(3) . ? C35 C38 1.530(3) . ? C35 C36 1.532(3) . ? C35 C37 1.545(4) . ? C39 C41 1.520(4) . ? C39 C42 1.525(4) . ? C39 C40 1.527(4) . ? C43 C48 1.425(3) . ? C43 C44 1.458(3) . ? C44 C45 1.446(3) . ? C45 C46 1.360(3) . ? C45 C49 1.533(3) . ? C46 C47 1.437(3) . ? C47 C48 1.355(3) . ? C47 C53 1.524(3) . ? C49 C51 1.531(3) . ? C49 C52 1.532(4) . ? C49 C50 1.532(4) . ? C53 C56 1.531(3) . ? C53 C54 1.535(3) . ? C53 C55 1.536(4) . ? C57 C58 1.381(3) . ? C57 C62 1.412(3) . ? C58 C59 1.391(3) . ? C59 C60 1.389(3) . ? C60 C61 1.391(3) . ? C61 C62 1.393(3) . ? C63 C64 1.378(3) . ? C63 C68 1.413(3) . ? C64 C65 1.397(3) . ? C65 C66 1.379(3) . ? C66 C67 1.398(3) . ? C67 C68 1.392(3) . ? C69 C70 1.510(5) . ? C70 C71 1.522(4) . ? C71 C72 1.507(4) . ? C72 C73 1.539(4) . ? C74 C74 1.502(9) 2_566 ? C74 C75 1.518(6) . ? C75 C76 1.342(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 O7 Fe1 O2 95.49(7) . . ? O7 Fe1 O5 151.43(7) . . ? O2 Fe1 O5 95.19(7) . . ? O7 Fe1 O1 94.84(7) . . ? O2 Fe1 O1 148.20(7) . . ? O5 Fe1 O1 89.83(6) . . ? O7 Fe1 O6 79.23(6) . . ? O2 Fe1 O6 98.98(6) . . ? O5 Fe1 O6 72.97(6) . . ? O1 Fe1 O6 112.48(6) . . ? O7 Fe1 N1 79.50(7) . . ? O2 Fe1 N1 76.32(7) . . ? O5 Fe1 N1 128.85(7) . . ? O1 Fe1 N1 76.15(7) . . ? O6 Fe1 N1 157.65(7) . . ? O8 Fe2 O4 98.21(7) . . ? O8 Fe2 O3 88.19(7) . . ? O4 Fe2 O3 150.59(7) . . ? O8 Fe2 O6 150.34(7) . . ? O4 Fe2 O6 97.57(7) . . ? O3 Fe2 O6 90.26(6) . . ? O8 Fe2 O5 79.38(6) . . ? O4 Fe2 O5 101.95(6) . . ? O3 Fe2 O5 107.44(6) . . ? O6 Fe2 O5 72.87(6) . . ? O8 Fe2 N2 84.50(7) . . ? O4 Fe2 N2 76.28(7) . . ? O3 Fe2 N2 75.81(7) . . ? O6 Fe2 N2 123.71(7) . . ? O5 Fe2 N2 163.38(7) . . ? C2 O1 Fe1 116.67(15) . . ? C16 O2 Fe1 118.69(14) . . ? C30 O3 Fe2 116.41(15) . . ? C44 O4 Fe2 118.70(15) . . ? C57 O5 Fe1 135.51(14) . . ? C57 O5 Fe2 112.11(14) . . ? Fe1 O5 Fe2 107.37(7) . . ? C63 O6 Fe2 140.02(15) . . ? C63 O6 Fe1 112.25(14) . . ? Fe2 O6 Fe1 106.46(7) . . ? C68 O7 Fe1 116.73(15) . . ? C62 O8 Fe2 116.04(15) . . ? C15 N1 C1 131.8(2) . . ? C15 N1 Fe1 114.63(15) . . ? C1 N1 Fe1 113.16(15) . . ? C43 N2 C29 131.2(2) . . ? C43 N2 Fe2 114.76(15) . . ? C29 N2 Fe2 114.08(15) . . ? N1 C1 C6 128.5(2) . . ? N1 C1 C2 111.2(2) . . ? C6 C1 C2 120.3(2) . . ? O1 C2 C3 122.7(2) . . ? O1 C2 C1 119.1(2) . . ? C3 C2 C1 118.1(2) . . ? C4 C3 C2 116.3(2) . . ? C4 C3 C7 123.2(2) . . ? C2 C3 C7 120.5(2) . . ? C3 C4 C5 125.6(2) . . ? C6 C5 C4 118.1(2) . . ? C6 C5 C11 123.3(2) . . ? C4 C5 C11 118.6(2) . . ? C5 C6 C1 120.1(2) . . ? C10 C7 C9 108.0(2) . . ? C10 C7 C3 111.7(2) . . ? C9 C7 C3 110.9(2) . . ? C10 C7 C8 107.6(2) . . ? C9 C7 C8 109.2(2) . . ? C3 C7 C8 109.4(2) . . ? C5 C11 C14 111.6(2) . . ? C5 C11 C12 108.4(2) . . ? C14 C11 C12 108.7(2) . . ? C5 C11 C13 109.6(2) . . ? C14 C11 C13 108.3(2) . . ? C12 C11 C13 110.3(2) . . ? N1 C15 C20 128.4(2) . . ? N1 C15 C16 111.3(2) . . ? C20 C15 C16 120.1(2) . . ? O2 C16 C17 122.5(2) . . ? O2 C16 C15 118.7(2) . . ? C17 C16 C15 118.8(2) . . ? C18 C17 C16 116.9(2) . . ? C18 C17 C21 123.1(2) . . ? C16 C17 C21 119.9(2) . . ? C17 C18 C19 125.2(2) . . ? C20 C19 C18 118.3(2) . . ? C20 C19 C25 123.2(2) . . ? C18 C19 C25 118.5(2) . . ? C19 C20 C15 120.5(2) . . ? C17 C21 C23 111.1(2) . . ? C17 C21 C22 109.7(2) . . ? C23 C21 C22 108.2(2) . . ? C17 C21 C24 109.8(2) . . ? C23 C21 C24 107.6(2) . . ? C22 C21 C24 110.3(2) . . ? C28 C25 C19 111.6(2) . . ? C28 C25 C27 108.4(2) . . ? C19 C25 C27 109.6(2) . . ? C28 C25 C26 108.5(2) . . ? C19 C25 C26 109.2(2) . . ? C27 C25 C26 109.5(2) . . ? N2 C29 C34 128.4(2) . . ? N2 C29 C30 111.1(2) . . ? C34 C29 C30 120.5(2) . . ? O3 C30 C31 122.7(2) . . ? O3 C30 C29 118.8(2) . . ? C31 C30 C29 118.5(2) . . ? C32 C31 C30 117.1(2) . . ? C32 C31 C35 122.9(2) . . ? C30 C31 C35 120.0(2) . . ? C31 C32 C33 124.9(2) . . ? C34 C33 C32 118.1(2) . . ? C34 C33 C39 123.5(2) . . ? C32 C33 C39 118.4(2) . . ? C33 C34 C29 120.6(2) . . ? C38 C35 C31 111.3(2) . . ? C38 C35 C36 108.2(2) . . ? C31 C35 C36 109.9(2) . . ? C38 C35 C37 107.9(2) . . ? C31 C35 C37 109.1(2) . . ? C36 C35 C37 110.4(2) . . ? C41 C39 C42 108.8(2) . . ? C41 C39 C40 107.5(2) . . ? C42 C39 C40 109.3(2) . . ? C41 C39 C33 110.6(2) . . ? C42 C39 C33 109.2(2) . . ? C40 C39 C33 111.5(2) . . ? N2 C43 C48 128.3(2) . . ? N2 C43 C44 111.3(2) . . ? C48 C43 C44 120.1(2) . . ? O4 C44 C45 123.0(2) . . ? O4 C44 C43 118.6(2) . . ? C45 C44 C43 118.4(2) . . ? C46 C45 C44 116.6(2) . . ? C46 C45 C49 122.8(2) . . ? C44 C45 C49 120.6(2) . . ? C45 C46 C47 125.5(2) . . ? C48 C47 C46 118.2(2) . . ? C48 C47 C53 123.5(2) . . ? C46 C47 C53 118.4(2) . . ? C47 C48 C43 120.3(2) . . ? C51 C49 C52 107.8(2) . . ? C51 C49 C50 108.6(2) . . ? C52 C49 C50 109.6(2) . . ? C51 C49 C45 111.6(2) . . ? C52 C49 C45 110.2(2) . . ? C50 C49 C45 109.0(2) . . ? C47 C53 C56 112.1(2) . . ? C47 C53 C54 109.5(2) . . ? C56 C53 C54 108.6(2) . . ? C47 C53 C55 109.3(2) . . ? C56 C53 C55 108.3(2) . . ? C54 C53 C55 109.0(2) . . ? O5 C57 C58 125.9(2) . . ? O5 C57 C62 114.2(2) . . ? C58 C57 C62 119.9(2) . . ? C57 C58 C59 120.7(2) . . ? C57 C58 Cl1 118.83(19) . . ? C59 C58 Cl1 120.39(19) . . ? C60 C59 C58 119.9(2) . . ? C60 C59 Cl2 120.18(19) . . ? C58 C59 Cl2 119.90(19) . . ? C59 C60 C61 119.7(2) . . ? C59 C60 Cl3 120.23(19) . . ? C61 C60 Cl3 120.08(19) . . ? C60 C61 C62 121.0(2) . . ? C60 C61 Cl4 121.08(19) . . ? C62 C61 Cl4 117.89(19) . . ? O8 C62 C61 123.7(2) . . ? O8 C62 C57 117.6(2) . . ? C61 C62 C57 118.8(2) . . ? O6 C63 C64 126.5(2) . . ? O6 C63 C68 114.3(2) . . ? C64 C63 C68 119.2(2) . . ? C63 C64 C65 121.2(2) . . ? C63 C64 Cl5 118.91(19) . . ? C65 C64 Cl5 119.88(19) . . ? C66 C65 C64 119.9(2) . . ? C66 C65 Cl6 120.1(2) . . ? C64 C65 Cl6 120.00(19) . . ? C65 C66 C67 119.6(2) . . ? C65 C66 Cl7 120.4(2) . . ? C67 C66 Cl7 120.0(2) . . ? C68 C67 C66 120.7(2) . . ? C68 C67 Cl8 118.77(19) . . ? C66 C67 Cl8 120.47(19) . . ? O7 C68 C67 123.2(2) . . ? O7 C68 C63 117.5(2) . . ? C67 C68 C63 119.3(2) . . ? C69 C70 C71 113.0(3) . . ? C72 C71 C70 114.1(3) . . ? C71 C72 C73 113.5(3) . . ? C74 C74 C75 111.0(5) 2_566 . ? C76 C75 C74 113.3(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Fe1 O1 C2 66.17(17) . . . . ? O2 Fe1 O1 C2 -42.4(2) . . . . ? O5 Fe1 O1 C2 -142.05(16) . . . . ? O6 Fe1 O1 C2 146.50(15) . . . . ? N1 Fe1 O1 C2 -11.76(16) . . . . ? O7 Fe1 O2 C16 -72.55(17) . . . . ? O5 Fe1 O2 C16 133.99(16) . . . . ? O1 Fe1 O2 C16 35.9(2) . . . . ? O6 Fe1 O2 C16 -152.47(16) . . . . ? N1 Fe1 O2 C16 5.23(16) . . . . ? O8 Fe2 O3 C30 67.06(16) . . . . ? O4 Fe2 O3 C30 -36.5(2) . . . . ? O6 Fe2 O3 C30 -142.56(16) . . . . ? O5 Fe2 O3 C30 145.34(16) . . . . ? N2 Fe2 O3 C30 -17.72(16) . . . . ? O8 Fe2 O4 C44 -83.69(17) . . . . ? O3 Fe2 O4 C44 17.3(3) . . . . ? O6 Fe2 O4 C44 121.51(17) . . . . ? O5 Fe2 O4 C44 -164.49(16) . . . . ? N2 Fe2 O4 C44 -1.44(17) . . . . ? O7 Fe1 O5 C57 142.4(2) . . . . ? O2 Fe1 O5 C57 -106.0(2) . . . . ? O1 Fe1 O5 C57 42.6(2) . . . . ? O6 Fe1 O5 C57 156.2(2) . . . . ? N1 Fe1 O5 C57 -29.4(2) . . . . ? O7 Fe1 O5 Fe2 -9.39(18) . . . . ? O2 Fe1 O5 Fe2 102.20(7) . . . . ? O1 Fe1 O5 Fe2 -109.24(7) . . . . ? O6 Fe1 O5 Fe2 4.39(6) . . . . ? N1 Fe1 O5 Fe2 178.80(7) . . . . ? O8 Fe2 O5 C57 5.86(14) . . . . ? O4 Fe2 O5 C57 102.10(14) . . . . ? O3 Fe2 O5 C57 -78.83(15) . . . . ? O6 Fe2 O5 C57 -163.56(15) . . . . ? N2 Fe2 O5 C57 20.1(3) . . . . ? O8 Fe2 O5 Fe1 164.90(8) . . . . ? O4 Fe2 O5 Fe1 -98.85(8) . . . . ? O3 Fe2 O5 Fe1 80.22(8) . . . . ? O6 Fe2 O5 Fe1 -4.52(7) . . . . ? N2 Fe2 O5 Fe1 179.1(2) . . . . ? O8 Fe2 O6 C63 148.2(2) . . . . ? O4 Fe2 O6 C63 -90.2(2) . . . . ? O3 Fe2 O6 C63 61.4(2) . . . . ? O5 Fe2 O6 C63 169.6(2) . . . . ? N2 Fe2 O6 C63 -11.6(2) . . . . ? O8 Fe2 O6 Fe1 -17.06(17) . . . . ? O4 Fe2 O6 Fe1 104.57(7) . . . . ? O3 Fe2 O6 Fe1 -103.86(7) . . . . ? O5 Fe2 O6 Fe1 4.34(6) . . . . ? N2 Fe2 O6 Fe1 -176.91(7) . . . . ? O7 Fe1 O6 C63 -0.96(14) . . . . ? O2 Fe1 O6 C63 92.98(15) . . . . ? O5 Fe1 O6 C63 -174.30(16) . . . . ? O1 Fe1 O6 C63 -91.77(15) . . . . ? N1 Fe1 O6 C63 17.2(3) . . . . ? O7 Fe1 O6 Fe2 168.87(8) . . . . ? O2 Fe1 O6 Fe2 -97.19(8) . . . . ? O5 Fe1 O6 Fe2 -4.47(7) . . . . ? O1 Fe1 O6 Fe2 78.06(8) . . . . ? N1 Fe1 O6 Fe2 -172.98(15) . . . . ? O2 Fe1 O7 C68 -96.67(16) . . . . ? O5 Fe1 O7 C68 14.8(2) . . . . ? O1 Fe1 O7 C68 113.44(16) . . . . ? O6 Fe1 O7 C68 1.45(15) . . . . ? N1 Fe1 O7 C68 -171.64(17) . . . . ? O4 Fe2 O8 C62 -108.44(16) . . . . ? O3 Fe2 O8 C62 100.39(16) . . . . ? O6 Fe2 O8 C62 13.0(2) . . . . ? O5 Fe2 O8 C62 -7.74(15) . . . . ? N2 Fe2 O8 C62 176.30(16) . . . . ? O7 Fe1 N1 C15 93.35(17) . . . . ? O2 Fe1 N1 C15 -5.01(16) . . . . ? O5 Fe1 N1 C15 -90.62(17) . . . . ? O1 Fe1 N1 C15 -168.94(17) . . . . ? O6 Fe1 N1 C15 75.2(2) . . . . ? O7 Fe1 N1 C1 -80.08(16) . . . . ? O2 Fe1 N1 C1 -178.43(17) . . . . ? O5 Fe1 N1 C1 95.95(17) . . . . ? O1 Fe1 N1 C1 17.63(16) . . . . ? O6 Fe1 N1 C1 -98.2(2) . . . . ? O8 Fe2 N2 C43 104.37(17) . . . . ? O4 Fe2 N2 C43 4.52(16) . . . . ? O3 Fe2 N2 C43 -166.11(18) . . . . ? O6 Fe2 N2 C43 -85.49(18) . . . . ? O5 Fe2 N2 C43 90.4(3) . . . . ? O8 Fe2 N2 C29 -75.01(17) . . . . ? O4 Fe2 N2 C29 -174.86(18) . . . . ? O3 Fe2 N2 C29 14.51(16) . . . . ? O6 Fe2 N2 C29 95.13(17) . . . . ? O5 Fe2 N2 C29 -89.0(3) . . . . ? C15 N1 C1 C6 -12.6(4) . . . . ? Fe1 N1 C1 C6 159.4(2) . . . . ? C15 N1 C1 C2 168.2(2) . . . . ? Fe1 N1 C1 C2 -19.8(2) . . . . ? Fe1 O1 C2 C3 -177.86(17) . . . . ? Fe1 O1 C2 C1 4.9(3) . . . . ? N1 C1 C2 O1 10.7(3) . . . . ? C6 C1 C2 O1 -168.5(2) . . . . ? N1 C1 C2 C3 -166.7(2) . . . . ? C6 C1 C2 C3 14.1(3) . . . . ? O1 C2 C3 C4 171.0(2) . . . . ? C1 C2 C3 C4 -11.7(3) . . . . ? O1 C2 C3 C7 -9.6(4) . . . . ? C1 C2 C3 C7 167.7(2) . . . . ? C2 C3 C4 C5 2.5(4) . . . . ? C7 C3 C4 C5 -176.9(2) . . . . ? C3 C4 C5 C6 5.0(4) . . . . ? C3 C4 C5 C11 -175.2(2) . . . . ? C4 C5 C6 C1 -2.8(3) . . . . ? C11 C5 C6 C1 177.4(2) . . . . ? N1 C1 C6 C5 174.3(2) . . . . ? C2 C1 C6 C5 -6.6(3) . . . . ? C4 C3 C7 C10 5.9(3) . . . . ? C2 C3 C7 C10 -173.4(2) . . . . ? C4 C3 C7 C9 -114.5(3) . . . . ? C2 C3 C7 C9 66.1(3) . . . . ? C4 C3 C7 C8 125.0(3) . . . . ? C2 C3 C7 C8 -54.3(3) . . . . ? C6 C5 C11 C14 1.5(3) . . . . ? C4 C5 C11 C14 -178.3(2) . . . . ? C6 C5 C11 C12 -118.1(3) . . . . ? C4 C5 C11 C12 62.1(3) . . . . ? C6 C5 C11 C13 121.5(3) . . . . ? C4 C5 C11 C13 -58.3(3) . . . . ? C1 N1 C15 C20 -8.2(4) . . . . ? Fe1 N1 C15 C20 179.88(19) . . . . ? C1 N1 C15 C16 175.9(2) . . . . ? Fe1 N1 C15 C16 4.0(2) . . . . ? Fe1 O2 C16 C17 174.97(17) . . . . ? Fe1 O2 C16 C15 -4.9(3) . . . . ? N1 C15 C16 O2 0.2(3) . . . . ? C20 C15 C16 O2 -176.0(2) . . . . ? N1 C15 C16 C17 -179.6(2) . . . . ? C20 C15 C16 C17 4.1(3) . . . . ? O2 C16 C17 C18 177.4(2) . . . . ? C15 C16 C17 C18 -2.8(3) . . . . ? O2 C16 C17 C21 -2.0(4) . . . . ? C15 C16 C17 C21 177.8(2) . . . . ? C16 C17 C18 C19 0.0(4) . . . . ? C21 C17 C18 C19 179.3(2) . . . . ? C17 C18 C19 C20 1.6(4) . . . . ? C17 C18 C19 C25 -178.5(2) . . . . ? C18 C19 C20 C15 -0.2(4) . . . . ? C25 C19 C20 C15 179.9(2) . . . . ? N1 C15 C20 C19 -178.1(2) . . . . ? C16 C15 C20 C19 -2.6(3) . . . . ? C18 C17 C21 C23 1.0(4) . . . . ? C16 C17 C21 C23 -179.6(2) . . . . ? C18 C17 C21 C22 -118.6(3) . . . . ? C16 C17 C21 C22 60.7(3) . . . . ? C18 C17 C21 C24 120.0(3) . . . . ? C16 C17 C21 C24 -60.7(3) . . . . ? C20 C19 C25 C28 2.4(3) . . . . ? C18 C19 C25 C28 -177.5(2) . . . . ? C20 C19 C25 C27 122.6(3) . . . . ? C18 C19 C25 C27 -57.4(3) . . . . ? C20 C19 C25 C26 -117.5(3) . . . . ? C18 C19 C25 C26 62.6(3) . . . . ? C43 N2 C29 C34 -10.9(4) . . . . ? Fe2 N2 C29 C34 168.4(2) . . . . ? C43 N2 C29 C30 171.3(2) . . . . ? Fe2 N2 C29 C30 -9.5(2) . . . . ? Fe2 O3 C30 C31 -162.45(18) . . . . ? Fe2 O3 C30 C29 18.9(3) . . . . ? N2 C29 C30 O3 -5.5(3) . . . . ? C34 C29 C30 O3 176.5(2) . . . . ? N2 C29 C30 C31 175.9(2) . . . . ? C34 C29 C30 C31 -2.2(3) . . . . ? O3 C30 C31 C32 -173.3(2) . . . . ? C29 C30 C31 C32 5.3(3) . . . . ? O3 C30 C31 C35 7.6(4) . . . . ? C29 C30 C31 C35 -173.8(2) . . . . ? C30 C31 C32 C33 -4.3(4) . . . . ? C35 C31 C32 C33 174.7(2) . . . . ? C31 C32 C33 C34 -0.2(4) . . . . ? C31 C32 C33 C39 -179.2(2) . . . . ? C32 C33 C34 C29 3.6(4) . . . . ? C39 C33 C34 C29 -177.4(2) . . . . ? N2 C29 C34 C33 179.9(2) . . . . ? C30 C29 C34 C33 -2.4(4) . . . . ? C32 C31 C35 C38 -3.2(3) . . . . ? C30 C31 C35 C38 175.8(2) . . . . ? C32 C31 C35 C36 116.7(3) . . . . ? C30 C31 C35 C36 -64.3(3) . . . . ? C32 C31 C35 C37 -122.1(3) . . . . ? C30 C31 C35 C37 56.9(3) . . . . ? C34 C33 C39 C41 -120.6(3) . . . . ? C32 C33 C39 C41 58.4(3) . . . . ? C34 C33 C39 C42 119.8(3) . . . . ? C32 C33 C39 C42 -61.2(3) . . . . ? C34 C33 C39 C40 -1.1(4) . . . . ? C32 C33 C39 C40 177.9(2) . . . . ? C29 N2 C43 C48 -13.1(4) . . . . ? Fe2 N2 C43 C48 167.6(2) . . . . ? C29 N2 C43 C44 172.9(2) . . . . ? Fe2 N2 C43 C44 -6.4(2) . . . . ? Fe2 O4 C44 C45 178.69(17) . . . . ? Fe2 O4 C44 C43 -1.6(3) . . . . ? N2 C43 C44 O4 5.5(3) . . . . ? C48 C43 C44 O4 -169.1(2) . . . . ? N2 C43 C44 C45 -174.9(2) . . . . ? C48 C43 C44 C45 10.6(3) . . . . ? O4 C44 C45 C46 173.3(2) . . . . ? C43 C44 C45 C46 -6.3(3) . . . . ? O4 C44 C45 C49 -5.4(4) . . . . ? C43 C44 C45 C49 175.0(2) . . . . ? C44 C45 C46 C47 -2.0(4) . . . . ? C49 C45 C46 C47 176.7(2) . . . . ? C45 C46 C47 C48 6.3(4) . . . . ? C45 C46 C47 C53 -173.0(2) . . . . ? C46 C47 C48 C43 -1.8(4) . . . . ? C53 C47 C48 C43 177.5(2) . . . . ? N2 C43 C48 C47 -179.9(2) . . . . ? C44 C43 C48 C47 -6.4(4) . . . . ? C46 C45 C49 C51 6.0(4) . . . . ? C44 C45 C49 C51 -175.4(2) . . . . ? C46 C45 C49 C52 125.7(3) . . . . ? C44 C45 C49 C52 -55.7(3) . . . . ? C46 C45 C49 C50 -113.9(3) . . . . ? C44 C45 C49 C50 64.7(3) . . . . ? C48 C47 C53 C56 0.1(4) . . . . ? C46 C47 C53 C56 179.3(2) . . . . ? C48 C47 C53 C54 120.7(3) . . . . ? C46 C47 C53 C54 -60.1(3) . . . . ? C48 C47 C53 C55 -120.1(3) . . . . ? C46 C47 C53 C55 59.2(3) . . . . ? Fe1 O5 C57 C58 26.3(3) . . . . ? Fe2 O5 C57 C58 177.19(19) . . . . ? Fe1 O5 C57 C62 -154.11(16) . . . . ? Fe2 O5 C57 C62 -3.3(2) . . . . ? O5 C57 C58 C59 -177.9(2) . . . . ? C62 C57 C58 C59 2.5(4) . . . . ? O5 C57 C58 Cl1 4.0(3) . . . . ? C62 C57 C58 Cl1 -175.55(18) . . . . ? C57 C58 C59 C60 -1.8(4) . . . . ? Cl1 C58 C59 C60 176.23(19) . . . . ? C57 C58 C59 Cl2 176.83(19) . . . . ? Cl1 C58 C59 Cl2 -5.1(3) . . . . ? C58 C59 C60 C61 0.6(4) . . . . ? Cl2 C59 C60 C61 -178.10(19) . . . . ? C58 C59 C60 Cl3 -177.34(19) . . . . ? Cl2 C59 C60 Cl3 4.0(3) . . . . ? C59 C60 C61 C62 0.0(4) . . . . ? Cl3 C60 C61 C62 177.87(19) . . . . ? C59 C60 C61 Cl4 -178.39(19) . . . . ? Cl3 C60 C61 Cl4 -0.5(3) . . . . ? Fe2 O8 C62 C61 -173.16(18) . . . . ? Fe2 O8 C62 C57 8.5(3) . . . . ? C60 C61 C62 O8 -177.6(2) . . . . ? Cl4 C61 C62 O8 0.8(3) . . . . ? C60 C61 C62 C57 0.7(4) . . . . ? Cl4 C61 C62 C57 179.13(17) . . . . ? O5 C57 C62 O8 -3.1(3) . . . . ? C58 C57 C62 O8 176.4(2) . . . . ? O5 C57 C62 C61 178.4(2) . . . . ? C58 C57 C62 C61 -2.0(3) . . . . ? Fe2 O6 C63 C64 16.0(4) . . . . ? Fe1 O6 C63 C64 -179.3(2) . . . . ? Fe2 O6 C63 C68 -164.35(17) . . . . ? Fe1 O6 C63 C68 0.4(2) . . . . ? O6 C63 C64 C65 -179.4(2) . . . . ? C68 C63 C64 C65 1.0(4) . . . . ? O6 C63 C64 Cl5 0.4(3) . . . . ? C68 C63 C64 Cl5 -179.25(18) . . . . ? C63 C64 C65 C66 -1.2(4) . . . . ? Cl5 C64 C65 C66 179.0(2) . . . . ? C63 C64 C65 Cl6 178.02(19) . . . . ? Cl5 C64 C65 Cl6 -1.7(3) . . . . ? C64 C65 C66 C67 -0.4(4) . . . . ? Cl6 C65 C66 C67 -179.64(19) . . . . ? C64 C65 C66 Cl7 179.09(19) . . . . ? Cl6 C65 C66 Cl7 -0.1(3) . . . . ? C65 C66 C67 C68 2.2(4) . . . . ? Cl7 C66 C67 C68 -177.26(19) . . . . ? C65 C66 C67 Cl8 -176.04(19) . . . . ? Cl7 C66 C67 Cl8 4.5(3) . . . . ? Fe1 O7 C68 C67 177.95(18) . . . . ? Fe1 O7 C68 C63 -1.7(3) . . . . ? C66 C67 C68 O7 177.9(2) . . . . ? Cl8 C67 C68 O7 -3.8(3) . . . . ? C66 C67 C68 C63 -2.4(4) . . . . ? Cl8 C67 C68 C63 175.87(18) . . . . ? O6 C63 C68 O7 0.8(3) . . . . ? C64 C63 C68 O7 -179.5(2) . . . . ? O6 C63 C68 C67 -178.9(2) . . . . ? C64 C63 C68 C67 0.8(3) . . . . ? C69 C70 C71 C72 -179.4(3) . . . . ? C70 C71 C72 C73 -179.2(3) . . . . ? C74 C74 C75 C76 165.6(6) 2_566 . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.567 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.063 _iucr_refine_instructions_details ; TITL afh333 in P-1 CELL 0.71073 14.8709 15.7470 17.9214 94.0663 111.4278 95.5142 ZERR 2.00 0.0008 0.0008 0.0010 0.0007 0.0007 0.0007 LATT 1 SFAC C H N O CL FE UNIT 151 196 4 16 16 4 TEMP -130.000 SIZE 0.085 0.161 0.206 rem Janice Wong 60s sphere ccd2 rem APEX2 2011.4-1, SAINT 7.68a, SADABS 2008/1, SHELXTL 2008/4 EXYZ C75 C77 EADP C75 C77 OMIT 0 1 0 OMIT -1 1 1 L.S. 12 ACTA 51 CONF WGHT 0.047800 0.626600 FVAR 0.05958 FE1 6 0.711497 0.667705 0.792761 11.00000 0.01737 0.01261 = 0.02091 0.00522 0.00907 0.00211 FE2 6 0.728060 0.834654 0.694596 11.00000 0.01797 0.01215 = 0.02247 0.00588 0.00893 0.00296 CL1 5 0.614558 0.511628 0.644909 11.00000 0.03412 0.01696 = 0.02393 0.00557 0.01212 -0.00103 CL2 5 0.614257 0.435230 0.478767 11.00000 0.04364 0.01649 = 0.02827 0.00095 0.01445 0.00004 CL3 5 0.650783 0.559443 0.360997 11.00000 0.05759 0.02616 = 0.02559 0.00087 0.02207 0.00108 CL4 5 0.706918 0.757752 0.418095 11.00000 0.03886 0.02451 = 0.02860 0.00826 0.01937 -0.00086 CL5 5 0.810197 0.993962 0.846867 11.00000 0.04943 0.01769 = 0.02756 0.00586 0.01339 0.00156 CL6 5 0.915118 1.051379 1.031327 11.00000 0.04201 0.01875 = 0.03085 -0.00232 0.01494 -0.00235 CL7 5 0.941043 0.915483 1.153161 11.00000 0.04525 0.03153 = 0.02097 -0.00109 0.01095 -0.00391 CL8 5 0.855214 0.722612 1.089357 11.00000 0.03154 0.02653 = 0.02436 0.00863 0.01179 0.00194 O1 4 0.817088 0.603055 0.779857 11.00000 0.01870 0.01607 = 0.02622 0.00731 0.01215 0.00388 O2 4 0.576029 0.664074 0.789136 11.00000 0.01654 0.01559 = 0.02602 0.00724 0.01013 0.00258 O3 4 0.873288 0.848705 0.721572 11.00000 0.01702 0.01724 = 0.02689 0.00815 0.01016 0.00273 O4 4 0.604662 0.885066 0.675760 11.00000 0.01754 0.01518 = 0.03000 0.00767 0.01076 0.00492 O5 4 0.680765 0.703668 0.681157 11.00000 0.02073 0.01243 = 0.01925 0.00479 0.00828 0.00347 O6 4 0.749137 0.800900 0.806582 11.00000 0.02002 0.01294 = 0.02045 0.00338 0.00858 0.00166 O7 4 0.773785 0.690758 0.909882 11.00000 0.02535 0.01605 = 0.02190 0.00411 0.00845 0.00312 O8 4 0.709805 0.803766 0.582219 11.00000 0.02540 0.01468 = 0.02239 0.00426 0.01061 0.00126 N1 3 0.681849 0.542758 0.827081 11.00000 0.01805 0.01304 = 0.01933 0.00325 0.00895 0.00227 N2 3 0.761401 0.963878 0.670982 11.00000 0.01690 0.01477 = 0.02200 0.00405 0.00841 0.00288 C1 1 0.757840 0.497944 0.844530 11.00000 0.01611 0.01568 = 0.01983 0.00184 0.00697 0.00089 C2 1 0.826876 0.531187 0.809765 11.00000 0.01718 0.01620 = 0.01893 0.00304 0.00576 0.00067 C3 1 0.901379 0.479501 0.807458 11.00000 0.01803 0.01419 = 0.02251 0.00096 0.00775 0.00160 C4 1 0.912115 0.411436 0.851168 11.00000 0.01944 0.01763 = 0.02623 0.00200 0.00793 0.00552 AFIX 43 H4A 2 0.962534 0.378305 0.852023 11.00000 -1.20000 AFIX 0 C5 1 0.853466 0.385241 0.896357 11.00000 0.01835 0.01474 = 0.02204 0.00279 0.00579 -0.00073 C6 1 0.776483 0.427476 0.890904 11.00000 0.01854 0.01653 = 0.02147 0.00543 0.00857 -0.00035 AFIX 43 H6A 2 0.734914 0.409964 0.918112 11.00000 -1.20000 AFIX 0 C7 1 0.962575 0.501628 0.757225 11.00000 0.02323 0.02229 = 0.02856 0.00687 0.01611 0.00660 C8 1 0.894567 0.506869 0.669478 11.00000 0.03249 0.04152 = 0.02935 0.00656 0.01762 0.00645 AFIX 137 H8A 2 0.853563 0.451588 0.647059 11.00000 -1.50000 H8B 2 0.933729 0.520420 0.637155 11.00000 -1.50000 H8C 2 0.853160 0.551932 0.668421 11.00000 -1.50000 AFIX 0 C9 1 1.027459 0.587670 0.791372 11.00000 0.02478 0.03294 = 0.04074 0.00859 0.02040 0.00027 AFIX 137 H9A 2 1.072298 0.584055 0.846594 11.00000 -1.50000 H9B 2 0.986725 0.632950 0.791699 11.00000 -1.50000 H9C 2 1.064913 0.601114 0.757694 11.00000 -1.50000 AFIX 0 C10 1 1.028346 0.433114 0.755592 11.00000 0.04119 0.03594 = 0.05375 0.01808 0.03468 0.01982 AFIX 137 H10A 2 0.988644 0.376831 0.736321 11.00000 -1.50000 H10B 2 1.076349 0.431872 0.810112 11.00000 -1.50000 H10C 2 1.062174 0.446754 0.719298 11.00000 -1.50000 AFIX 0 C11 1 0.880855 0.311300 0.947647 11.00000 0.02203 0.02058 = 0.02660 0.00902 0.00858 0.00530 C12 1 0.982938 0.337884 1.012484 11.00000 0.02613 0.03566 = 0.02574 0.00996 0.00723 0.01089 AFIX 137 H12A 2 0.982937 0.390029 1.045757 11.00000 -1.50000 H12B 2 1.029910 0.349080 0.986543 11.00000 -1.50000 H12C 2 1.001225 0.291537 1.046602 11.00000 -1.50000 AFIX 0 C13 1 0.879718 0.230461 0.893682 11.00000 0.03309 0.02036 = 0.03581 0.01282 0.01042 0.00716 AFIX 137 H13A 2 0.813325 0.212306 0.854494 11.00000 -1.50000 H13B 2 0.901712 0.184269 0.927167 11.00000 -1.50000 H13C 2 0.923393 0.243297 0.864998 11.00000 -1.50000 AFIX 0 C14 1 0.809389 0.290341 0.989254 11.00000 0.02836 0.02833 = 0.03788 0.01954 0.01433 0.00696 AFIX 137 H14A 2 0.743702 0.273599 0.948393 11.00000 -1.50000 H14B 2 0.809563 0.341067 1.024329 11.00000 -1.50000 H14C 2 0.829125 0.242931 1.021689 11.00000 -1.50000 AFIX 0 C15 1 0.595801 0.527867 0.835146 11.00000 0.01724 0.01606 = 0.01689 0.00057 0.00805 0.00174 C16 1 0.539426 0.599185 0.812795 11.00000 0.01545 0.01604 = 0.01743 0.00169 0.00659 0.00097 C17 1 0.445033 0.594187 0.818320 11.00000 0.01787 0.01688 = 0.02231 0.00257 0.00864 0.00386 C18 1 0.412469 0.520227 0.841179 11.00000 0.01729 0.02404 = 0.02537 0.00378 0.01127 0.00347 AFIX 43 H18A 2 0.350173 0.516507 0.844978 11.00000 -1.20000 AFIX 0 C19 1 0.464825 0.447581 0.859946 11.00000 0.01883 0.01880 = 0.01899 0.00319 0.00926 0.00020 C20 1 0.554802 0.452460 0.856820 11.00000 0.01932 0.01449 = 0.02059 0.00478 0.00774 0.00289 AFIX 43 H20A 2 0.590866 0.405251 0.869172 11.00000 -1.20000 AFIX 0 C21 1 0.385920 0.669164 0.798192 11.00000 0.02407 0.02330 = 0.04175 0.01280 0.01995 0.00946 C22 1 0.364730 0.685021 0.710348 11.00000 0.02509 0.02668 = 0.03946 0.01118 0.00818 0.01028 AFIX 137 H22A 2 0.331592 0.632117 0.674713 11.00000 -1.50000 H22B 2 0.426129 0.702535 0.703656 11.00000 -1.50000 H22C 2 0.322919 0.730551 0.696497 11.00000 -1.50000 AFIX 0 C23 1 0.288446 0.650393 0.808660 11.00000 0.03732 0.03990 = 0.09180 0.03280 0.04195 0.02290 AFIX 137 H23A 2 0.249554 0.600290 0.771252 11.00000 -1.50000 H23B 2 0.252996 0.700274 0.797204 11.00000 -1.50000 H23C 2 0.300447 0.638609 0.864218 11.00000 -1.50000 AFIX 0 C24 1 0.442820 0.750445 0.855737 11.00000 0.05185 0.02569 = 0.03766 0.00858 0.02577 0.01650 AFIX 137 H24A 2 0.504047 0.765982 0.848112 11.00000 -1.50000 H24B 2 0.457015 0.739057 0.911692 11.00000 -1.50000 H24C 2 0.403505 0.797876 0.843926 11.00000 -1.50000 AFIX 0 C25 1 0.416552 0.368622 0.882541 11.00000 0.02309 0.01914 = 0.02456 0.00483 0.01183 -0.00380 C26 1 0.323324 0.331006 0.810471 11.00000 0.02927 0.02805 = 0.02899 0.00361 0.01016 -0.00875 AFIX 137 H26A 2 0.279149 0.374723 0.796042 11.00000 -1.50000 H26B 2 0.291169 0.281267 0.825147 11.00000 -1.50000 H26C 2 0.340265 0.313062 0.764313 11.00000 -1.50000 AFIX 0 C27 1 0.390536 0.394431 0.955292 11.00000 0.03236 0.02748 = 0.03148 0.00717 0.01659 -0.00513 AFIX 137 H27A 2 0.449852 0.419130 1.000947 11.00000 -1.50000 H27B 2 0.360161 0.343637 0.969981 11.00000 -1.50000 H27C 2 0.344921 0.437066 0.941573 11.00000 -1.50000 AFIX 0 C28 1 0.483791 0.299309 0.904136 11.00000 0.03280 0.02147 = 0.04038 0.01397 0.01839 -0.00004 AFIX 137 H28A 2 0.544055 0.322595 0.949479 11.00000 -1.50000 H28B 2 0.499307 0.280542 0.857428 11.00000 -1.50000 H28C 2 0.451202 0.250271 0.919372 11.00000 -1.50000 AFIX 0 C29 1 0.849690 0.980598 0.667119 11.00000 0.01902 0.01392 = 0.02040 0.00085 0.00803 0.00138 C30 1 0.907669 0.910489 0.693376 11.00000 0.01915 0.01513 = 0.01862 0.00015 0.00852 0.00125 C31 1 1.002015 0.915207 0.687881 11.00000 0.02012 0.02144 = 0.01674 0.00125 0.00625 0.00431 C32 1 1.034884 0.988897 0.664483 11.00000 0.01924 0.02315 = 0.02201 0.00248 0.01117 0.00122 AFIX 43 H32A 2 1.099006 0.994076 0.664362 11.00000 -1.20000 AFIX 0 C33 1 0.979375 1.059566 0.639898 11.00000 0.02322 0.01798 = 0.02118 0.00249 0.01058 0.00141 C34 1 0.887661 1.052891 0.639584 11.00000 0.02538 0.01403 = 0.02458 0.00442 0.01005 0.00359 AFIX 43 H34A 2 0.848437 1.096952 0.620782 11.00000 -1.20000 AFIX 0 C35 1 1.060304 0.839148 0.706586 11.00000 0.02178 0.02458 = 0.02843 0.00637 0.01212 0.00801 C36 1 1.086872 0.824852 0.795371 11.00000 0.02493 0.02662 = 0.03194 0.00958 0.01127 0.00965 AFIX 137 H36A 2 1.126100 0.876636 0.829818 11.00000 -1.50000 H36B 2 1.124360 0.776222 0.806981 11.00000 -1.50000 H36C 2 1.027150 0.812554 0.806109 11.00000 -1.50000 AFIX 0 C37 1 0.998687 0.758140 0.651051 11.00000 0.03695 0.02151 = 0.03210 0.00300 0.01390 0.01161 AFIX 137 H37A 2 0.978116 0.769708 0.594618 11.00000 -1.50000 H37B 2 0.941069 0.742857 0.664044 11.00000 -1.50000 H37C 2 1.037786 0.710464 0.659260 11.00000 -1.50000 AFIX 0 C38 1 1.154765 0.855023 0.691071 11.00000 0.02786 0.03793 = 0.04839 0.01754 0.02186 0.01639 AFIX 137 H38A 2 1.196868 0.904283 0.727820 11.00000 -1.50000 H38B 2 1.139503 0.867000 0.635146 11.00000 -1.50000 H38C 2 1.188428 0.803954 0.700307 11.00000 -1.50000 AFIX 0 C39 1 1.026500 1.137069 0.614430 11.00000 0.02884 0.01828 = 0.03156 0.00430 0.01586 -0.00197 C40 1 0.956772 1.203885 0.587564 11.00000 0.05508 0.02124 = 0.09184 0.02466 0.04586 0.00589 AFIX 137 H40A 2 0.898314 1.177994 0.541666 11.00000 -1.50000 H40B 2 0.988971 1.252525 0.571495 11.00000 -1.50000 H40C 2 0.938273 1.224025 0.632284 11.00000 -1.50000 AFIX 0 C41 1 1.055130 1.109698 0.544037 11.00000 0.04263 0.03000 = 0.03373 0.00800 0.01885 -0.00390 AFIX 137 H41A 2 0.996472 1.086692 0.497058 11.00000 -1.50000 H41B 2 1.098395 1.065331 0.558843 11.00000 -1.50000 H41C 2 1.088986 1.159418 0.530813 11.00000 -1.50000 AFIX 0 C42 1 1.117842 1.177834 0.685319 11.00000 0.05332 0.04514 = 0.03378 0.00364 0.01693 -0.02753 AFIX 137 H42A 2 1.162954 1.135185 0.702377 11.00000 -1.50000 H42B 2 1.099836 1.197981 0.730314 11.00000 -1.50000 H42C 2 1.149417 1.226523 0.668808 11.00000 -1.50000 AFIX 0 C43 1 0.690357 1.013300 0.661923 11.00000 0.01976 0.01453 = 0.02082 0.00549 0.00884 0.00434 C44 1 0.602084 0.963819 0.661491 11.00000 0.02092 0.01442 = 0.02083 0.00472 0.01004 0.00388 C45 1 0.515692 1.005834 0.645424 11.00000 0.01734 0.01927 = 0.02350 0.00724 0.00850 0.00388 C46 1 0.526144 1.091633 0.639715 11.00000 0.02213 0.02037 = 0.02538 0.00585 0.01034 0.00765 AFIX 43 H46A 2 0.469373 1.119475 0.627465 11.00000 -1.20000 AFIX 0 C47 1 0.615833 1.143701 0.650653 11.00000 0.02367 0.01601 = 0.02169 0.00667 0.00863 0.00425 C48 1 0.695628 1.103961 0.660374 11.00000 0.01940 0.01598 = 0.02660 0.00484 0.01129 0.00055 AFIX 43 H48A 2 0.755359 1.136705 0.666182 11.00000 -1.20000 AFIX 0 C49 1 0.418727 0.955011 0.637360 11.00000 0.01829 0.02018 = 0.03819 0.00950 0.01211 0.00459 C50 1 0.429150 0.922929 0.718492 11.00000 0.03213 0.02811 = 0.04741 0.01001 0.02551 0.00325 AFIX 137 H50A 2 0.444709 0.972164 0.759742 11.00000 -1.50000 H50B 2 0.481597 0.886716 0.734093 11.00000 -1.50000 H50C 2 0.367811 0.889389 0.713529 11.00000 -1.50000 AFIX 0 C51 1 0.335794 1.010530 0.613665 11.00000 0.02132 0.02907 = 0.07231 0.01990 0.01747 0.00677 AFIX 137 H51A 2 0.349097 1.057571 0.656631 11.00000 -1.50000 H51B 2 0.274319 0.975296 0.605764 11.00000 -1.50000 H51C 2 0.330866 1.034270 0.563431 11.00000 -1.50000 AFIX 0 C52 1 0.391186 0.878342 0.572111 11.00000 0.02618 0.03415 = 0.03628 0.00216 0.00283 -0.00321 AFIX 137 H52A 2 0.386798 0.898907 0.520703 11.00000 -1.50000 H52B 2 0.328080 0.847492 0.566207 11.00000 -1.50000 H52C 2 0.441064 0.839587 0.587690 11.00000 -1.50000 AFIX 0 C53 1 0.616565 1.240622 0.651695 11.00000 0.02323 0.01420 = 0.03221 0.00348 0.01194 0.00444 C54 1 0.543484 1.261022 0.571094 11.00000 0.03523 0.02011 = 0.03910 0.01238 0.01591 0.01014 AFIX 137 H54A 2 0.480163 1.226881 0.559108 11.00000 -1.50000 H54B 2 0.567226 1.246960 0.527992 11.00000 -1.50000 H54C 2 0.536411 1.322247 0.574729 11.00000 -1.50000 AFIX 0 C55 1 0.586472 1.274980 0.720301 11.00000 0.03523 0.02271 = 0.03722 0.00124 0.01530 0.00514 AFIX 137 H55A 2 0.632216 1.261412 0.771922 11.00000 -1.50000 H55B 2 0.520611 1.248077 0.711365 11.00000 -1.50000 H55C 2 0.587387 1.337373 0.721392 11.00000 -1.50000 AFIX 0 C56 1 0.717354 1.287057 0.664807 11.00000 0.03098 0.01500 = 0.04988 0.00580 0.01631 0.00296 AFIX 137 H56A 2 0.764137 1.276967 0.717376 11.00000 -1.50000 H56B 2 0.714141 1.348818 0.663364 11.00000 -1.50000 H56C 2 0.738300 1.265110 0.622074 11.00000 -1.50000 AFIX 0 C57 1 0.671469 0.664731 0.608563 11.00000 0.01333 0.01887 = 0.01970 0.00478 0.00531 0.00535 C58 1 0.645434 0.577990 0.582934 11.00000 0.01984 0.01652 = 0.02335 0.00881 0.00864 0.00315 C59 1 0.641237 0.544789 0.507555 11.00000 0.02605 0.01444 = 0.02432 0.00212 0.00889 0.00147 C60 1 0.660693 0.599497 0.456272 11.00000 0.02530 0.02239 = 0.02109 0.00161 0.01059 0.00367 C61 1 0.685123 0.687209 0.481060 11.00000 0.02148 0.02058 = 0.02361 0.00981 0.01200 0.00340 C62 1 0.690369 0.721192 0.556664 11.00000 0.01560 0.01363 = 0.02505 0.00298 0.00745 0.00371 C63 1 0.793444 0.833610 0.885025 11.00000 0.01575 0.01903 = 0.02321 0.00320 0.00935 0.00267 C64 1 0.826087 0.918772 0.914234 11.00000 0.02330 0.01599 = 0.02689 0.00683 0.01180 0.00438 C65 1 0.871809 0.944666 0.996978 11.00000 0.02643 0.01654 = 0.02658 -0.00064 0.01336 0.00120 C66 1 0.883286 0.884644 1.051059 11.00000 0.02252 0.02579 = 0.02233 -0.00059 0.00913 0.00187 C67 1 0.848387 0.798228 1.022528 11.00000 0.02058 0.02101 = 0.02492 0.00835 0.01323 0.00395 C68 1 0.805228 0.771682 0.940067 11.00000 0.01571 0.01582 = 0.02488 0.00366 0.01062 0.00447 C69 1 0.680291 0.931463 1.143188 11.00000 0.04921 0.05324 = 0.06702 0.00136 0.01265 0.01141 AFIX 137 H69A 2 0.667974 0.875954 1.161575 11.00000 -1.50000 H69B 2 0.651384 0.974817 1.165846 11.00000 -1.50000 H69C 2 0.750717 0.948646 1.161188 11.00000 -1.50000 AFIX 0 C70 1 0.635285 0.923716 1.052179 11.00000 0.03357 0.04256 = 0.05903 0.00156 0.01204 0.00754 AFIX 23 H70A 2 0.565101 0.902048 1.034295 11.00000 -1.20000 H70B 2 0.666240 0.881089 1.029762 11.00000 -1.20000 AFIX 0 C71 1 0.646383 1.008405 1.018470 11.00000 0.03351 0.03648 = 0.06479 -0.00345 0.02117 0.00290 AFIX 23 H71A 2 0.616238 1.051103 1.041656 11.00000 -1.20000 H71B 2 0.716651 1.029638 1.036124 11.00000 -1.20000 AFIX 0 C72 1 0.601077 1.002563 0.927793 11.00000 0.04028 0.03936 = 0.06826 0.00595 0.02580 0.00138 AFIX 23 H72A 2 0.530576 0.982271 0.910074 11.00000 -1.20000 H72B 2 0.630528 0.959349 0.904479 11.00000 -1.20000 AFIX 0 C73 1 0.614114 1.088336 0.894471 11.00000 0.06109 0.04162 = 0.08823 0.00741 0.03594 -0.00206 AFIX 137 H73A 2 0.583808 1.080095 0.835429 11.00000 -1.50000 H73B 2 0.683753 1.108550 0.911067 11.00000 -1.50000 H73C 2 0.583085 1.130998 0.915691 11.00000 -1.50000 AFIX 0 C74 1 0.014394 0.546813 0.498987 11.00000 0.04997 0.16189 = 0.03923 -0.00973 0.01991 -0.00871 AFIX 23 H74A 2 -0.019786 0.581701 0.525548 11.00000 -1.20000 H74B 2 -0.005657 0.559281 0.442229 11.00000 -1.20000 AFIX 0 part 1 C75 1 0.123689 0.571430 0.541592 10.50000 0.06285 0.17459 = 0.04938 0.01647 0.00494 -0.01531 AFIX 23 H75A 2 0.140827 0.572594 0.600515 10.50000 -1.20000 H75B 2 0.157301 0.526863 0.524814 10.50000 -1.20000 AFIX 0 C76 1 0.156160 0.648018 0.526001 10.50000 0.07774 0.05937 = 0.04386 0.00205 0.01851 0.01380 AFIX 137 H76A 2 0.227089 0.659538 0.553874 10.50000 -1.50000 H76B 2 0.125780 0.692953 0.545002 10.50000 -1.50000 H76C 2 0.139328 0.647505 0.467739 10.50000 -1.50000 AFIX 0 part 2 C77 1 0.123689 0.571430 0.541592 10.50000 0.06285 0.17459 = 0.04938 0.01647 0.00494 -0.01531 AFIX 137 H77A 2 0.139186 0.634117 0.549135 10.50000 -1.50000 H77B 2 0.157019 0.546570 0.508852 10.50000 -1.50000 H77C 2 0.145409 0.549494 0.594290 10.50000 -1.50000 HKLF 4 REM afh333 in P-1 REM R1 = 0.0401 for 11327 Fo > 4sig(Fo) and 0.0676 for all 15780 data REM 893 parameters refined using 0 restraints END WGHT 0.0478 0.6266 REM Highest difference peak 0.567, deepest hole -0.317, 1-sigma level 0.063 Q1 1 0.5433 0.4475 0.4528 11.00000 0.05 0.57 Q2 1 0.6719 0.6473 0.7383 11.00000 0.05 0.44 Q3 1 0.7527 0.8593 0.7491 11.00000 0.05 0.40 Q4 1 0.7445 0.6916 0.8541 11.00000 0.05 0.38 Q5 1 0.7017 0.8129 0.6287 11.00000 0.05 0.36 Q6 1 0.7166 0.5107 0.8311 11.00000 0.05 0.36 Q7 1 0.7886 0.5133 0.8289 11.00000 0.05 0.35 Q8 1 0.6881 1.0568 0.6515 11.00000 0.05 0.34 Q9 1 0.5786 0.5704 0.8365 11.00000 0.05 0.34 Q10 1 0.6968 0.6922 0.5888 11.00000 0.05 0.34 Q11 1 0.7992 0.8633 0.6784 11.00000 0.05 0.33 Q12 1 0.8986 0.9024 1.0955 11.00000 0.05 0.33 Q13 1 0.5528 0.5207 0.6162 11.00000 0.05 0.33 Q14 1 0.9193 0.3181 0.9784 11.00000 0.05 0.33 Q15 1 0.9364 0.5126 0.7196 11.00000 0.05 0.33 Q16 1 0.3830 0.3397 0.8556 11.00000 0.05 0.33 Q17 1 0.9944 0.5415 0.7693 11.00000 0.05 0.32 Q18 1 0.4400 0.4022 0.8711 11.00000 0.05 0.32 Q19 1 0.4005 0.3940 0.9109 11.00000 0.05 0.32 Q20 1 0.6884 0.6846 0.6461 11.00000 0.05 0.31 ; data_afh334 _database_code_depnum_ccdc_archive 'CCDC 916895' #TrackingRef '[ONO]Fe_CIF.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; [ONOq]Fe(ortho-C6O2Cl4)(py) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H55 Cl4 Fe N2 O5' _chemical_formula_weight 877.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.6068(11) _cell_length_b 24.431(2) _cell_length_c 16.6177(14) _cell_angle_alpha 90.00 _cell_angle_beta 111.8027(9) _cell_angle_gamma 90.00 _cell_volume 4752.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 88(2) _cell_measurement_reflns_used 9938 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 26.14 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1844 _exptl_absorpt_coefficient_mu 0.584 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7938 _exptl_absorpt_correction_T_max 0.8942 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 88(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 46245 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8703 _reflns_number_gt 6367 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. There was one molecule of diethylether solvent present. The solvent was disordered and included using multiple components, partial site-occupancy-factors, equivalent isotropic thermal parameters and restrained distances. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+13.9490P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8703 _refine_ls_number_parameters 498 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0916 _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.1709 _refine_ls_wR_factor_gt 0.1486 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.08676(4) 0.19989(2) 0.14476(4) 0.02715(17) Uani 1 1 d . . . Cl1 Cl 0.16660(13) 0.09340(6) 0.41529(9) 0.0624(4) Uani 1 1 d . . . Cl2 Cl -0.03649(13) 0.01265(6) 0.39607(9) 0.0566(4) Uani 1 1 d . . . Cl3 Cl -0.24910(9) 0.00884(5) 0.22248(9) 0.0437(3) Uani 1 1 d . . . Cl4 Cl -0.25503(8) 0.08420(4) 0.06696(8) 0.0370(3) Uani 1 1 d . . . O1 O 0.0530(2) 0.26756(11) 0.2057(2) 0.0318(7) Uani 1 1 d . . . O2 O 0.1861(2) 0.15960(10) 0.09419(18) 0.0275(6) Uani 1 1 d . . . O3 O 0.1285(2) 0.15791(11) 0.25315(19) 0.0326(7) Uani 1 1 d . . . O4 O -0.0490(2) 0.15504(11) 0.11056(18) 0.0274(6) Uani 1 1 d . . . N1 N 0.2431(3) 0.24660(13) 0.1873(2) 0.0280(7) Uani 1 1 d . . . N2 N 0.0012(3) 0.24473(14) 0.0260(2) 0.0330(8) Uani 1 1 d . . . C1 C 0.2390(3) 0.29547(16) 0.2216(3) 0.0282(9) Uani 1 1 d . . . C2 C 0.1296(3) 0.30420(16) 0.2314(3) 0.0285(9) Uani 1 1 d . . . C3 C 0.1146(3) 0.35409(16) 0.2736(3) 0.0306(9) Uani 1 1 d . . . C4 C 0.2027(3) 0.39037(17) 0.2983(3) 0.0302(9) Uani 1 1 d . . . H4A H 0.1949 0.4223 0.3283 0.036 Uiso 1 1 calc R . . C5 C 0.3071(3) 0.38416(16) 0.2824(3) 0.0289(9) Uani 1 1 d . . . C6 C 0.3230(3) 0.33745(16) 0.2451(3) 0.0283(9) Uani 1 1 d . . . H6A H 0.3914 0.3326 0.2343 0.034 Uiso 1 1 calc R . . C7 C 0.0042(3) 0.36296(18) 0.2907(3) 0.0375(11) Uani 1 1 d . . . C8 C -0.0029(4) 0.3194(2) 0.3543(3) 0.0460(12) Uani 1 1 d . . . H8A H -0.0089 0.2831 0.3278 0.069 Uiso 1 1 calc R . . H8B H -0.0703 0.3261 0.3689 0.069 Uiso 1 1 calc R . . H8C H 0.0660 0.3210 0.4072 0.069 Uiso 1 1 calc R . . C9 C -0.1006(4) 0.3609(2) 0.2051(4) 0.0494(13) Uani 1 1 d . . . H9A H -0.1057 0.3246 0.1787 0.074 Uiso 1 1 calc R . . H9B H -0.0929 0.3888 0.1653 0.074 Uiso 1 1 calc R . . H9C H -0.1701 0.3679 0.2169 0.074 Uiso 1 1 calc R . . C10 C 0.0038(4) 0.41989(19) 0.3309(3) 0.0426(12) Uani 1 1 d . . . H10A H 0.0704 0.4232 0.3851 0.064 Uiso 1 1 calc R . . H10B H -0.0662 0.4243 0.3429 0.064 Uiso 1 1 calc R . . H10C H 0.0071 0.4483 0.2903 0.064 Uiso 1 1 calc R . . C11 C 0.3949(3) 0.43037(16) 0.3102(3) 0.0332(10) Uani 1 1 d . . . C12 C 0.4392(4) 0.43555(19) 0.4092(3) 0.0394(11) Uani 1 1 d . . . H12A H 0.3751 0.4432 0.4274 0.059 Uiso 1 1 calc R . . H12B H 0.4947 0.4655 0.4278 0.059 Uiso 1 1 calc R . . H12C H 0.4760 0.4012 0.4356 0.059 Uiso 1 1 calc R . . C13 C 0.3397(4) 0.48450(18) 0.2677(4) 0.0432(12) Uani 1 1 d . . . H13A H 0.2731 0.4923 0.2828 0.065 Uiso 1 1 calc R . . H13B H 0.3156 0.4814 0.2046 0.065 Uiso 1 1 calc R . . H13C H 0.3953 0.5143 0.2887 0.065 Uiso 1 1 calc R . . C14 C 0.4959(4) 0.41883(18) 0.2825(3) 0.0379(11) Uani 1 1 d . . . H14A H 0.5333 0.3847 0.3092 0.057 Uiso 1 1 calc R . . H14B H 0.5508 0.4490 0.3013 0.057 Uiso 1 1 calc R . . H14C H 0.4683 0.4154 0.2193 0.057 Uiso 1 1 calc R . . C15 C 0.3311(3) 0.22077(16) 0.1750(3) 0.0298(9) Uani 1 1 d . . . C16 C 0.2927(3) 0.17206(15) 0.1221(3) 0.0268(9) Uani 1 1 d . . . C17 C 0.3752(3) 0.13990(15) 0.1019(3) 0.0269(9) Uani 1 1 d . . . C18 C 0.4863(3) 0.15698(16) 0.1357(3) 0.0339(10) Uani 1 1 d . . . H18A H 0.5408 0.1365 0.1213 0.041 Uiso 1 1 calc R . . C19 C 0.5267(3) 0.20344(18) 0.1914(4) 0.0431(12) Uani 1 1 d . . . C20 C 0.4493(3) 0.23391(18) 0.2111(3) 0.0412(12) Uani 1 1 d . . . H20A H 0.4745 0.2642 0.2494 0.049 Uiso 1 1 calc R . . C21 C 0.3379(3) 0.08976(15) 0.0440(3) 0.0275(9) Uani 1 1 d . . . C22 C 0.2780(4) 0.04828(16) 0.0827(3) 0.0393(11) Uani 1 1 d . . . H22A H 0.3303 0.0374 0.1406 0.059 Uiso 1 1 calc R . . H22B H 0.2560 0.0159 0.0453 0.059 Uiso 1 1 calc R . . H22C H 0.2096 0.0651 0.0867 0.059 Uiso 1 1 calc R . . C23 C 0.4396(3) 0.06026(17) 0.0338(3) 0.0354(10) Uani 1 1 d . . . H23A H 0.4779 0.0851 0.0069 0.053 Uiso 1 1 calc R . . H23B H 0.4123 0.0279 -0.0029 0.053 Uiso 1 1 calc R . . H23C H 0.4936 0.0490 0.0909 0.053 Uiso 1 1 calc R . . C24 C 0.2552(4) 0.1073(2) -0.0460(3) 0.0404(11) Uani 1 1 d . . . H24A H 0.2921 0.1347 -0.0699 0.061 Uiso 1 1 calc R . . H24B H 0.1863 0.1230 -0.0412 0.061 Uiso 1 1 calc R . . H24C H 0.2344 0.0753 -0.0843 0.061 Uiso 1 1 calc R . . C25 C 0.6553(4) 0.2151(2) 0.2286(5) 0.0645(19) Uani 1 1 d . . . C26 C 0.7193(4) 0.1653(2) 0.2797(4) 0.069(2) Uani 1 1 d . . . H26A H 0.6924 0.1574 0.3267 0.104 Uiso 1 1 calc R . . H26B H 0.8014 0.1731 0.3041 0.104 Uiso 1 1 calc R . . H26C H 0.7050 0.1336 0.2409 0.104 Uiso 1 1 calc R . . C27 C 0.6950(5) 0.2270(2) 0.1535(5) 0.078(2) Uani 1 1 d . . . H27A H 0.6540 0.2590 0.1211 0.117 Uiso 1 1 calc R . . H27B H 0.6790 0.1953 0.1149 0.117 Uiso 1 1 calc R . . H27C H 0.7773 0.2345 0.1767 0.117 Uiso 1 1 calc R . . C28 C 0.6828(4) 0.2655(3) 0.2888(6) 0.103(3) Uani 1 1 d . . . H28A H 0.6467 0.2980 0.2553 0.155 Uiso 1 1 calc R . . H28B H 0.7657 0.2708 0.3144 0.155 Uiso 1 1 calc R . . H28C H 0.6533 0.2597 0.3350 0.155 Uiso 1 1 calc R . . C29 C 0.0457(3) 0.12374(16) 0.2516(3) 0.0301(9) Uani 1 1 d . . . C30 C 0.0478(4) 0.09076(19) 0.3197(3) 0.0378(10) Uani 1 1 d . . . C31 C -0.0432(4) 0.05468(18) 0.3107(3) 0.0378(10) Uani 1 1 d . . . C32 C -0.1358(3) 0.05228(17) 0.2333(3) 0.0327(10) Uani 1 1 d . . . C33 C -0.1388(3) 0.08544(16) 0.1649(3) 0.0283(9) Uani 1 1 d . . . C34 C -0.0506(3) 0.12151(15) 0.1731(3) 0.0262(9) Uani 1 1 d . . . C35 C -0.1143(3) 0.24461(18) -0.0114(3) 0.0383(11) Uani 1 1 d . . . H35A H -0.1560 0.2201 0.0101 0.046 Uiso 1 1 calc R . . C36 C -0.1740(4) 0.2788(2) -0.0797(3) 0.0443(12) Uani 1 1 d . . . H36A H -0.2552 0.2781 -0.1036 0.053 Uiso 1 1 calc R . . C37 C -0.1157(4) 0.3134(2) -0.1123(4) 0.0536(14) Uani 1 1 d . . . H37A H -0.1553 0.3377 -0.1584 0.064 Uiso 1 1 calc R . . C38 C 0.0031(5) 0.3126(3) -0.0771(4) 0.0692(19) Uani 1 1 d . . . H38A H 0.0462 0.3355 -0.0998 0.083 Uiso 1 1 calc R . . C39 C 0.0572(4) 0.2779(2) -0.0083(3) 0.0496(13) Uani 1 1 d . . . H39A H 0.1383 0.2776 0.0157 0.060 Uiso 1 1 calc R . . C40 C 0.6506(13) 0.0741(7) 0.5392(12) 0.1131(17) Uiso 0.50 1 d PD A 1 H40A H 0.6214 0.0380 0.5155 0.170 Uiso 0.50 1 calc PR A 1 H40B H 0.5951 0.1023 0.5085 0.170 Uiso 0.50 1 calc PR A 1 H40C H 0.6629 0.0751 0.6010 0.170 Uiso 0.50 1 calc PR A 1 C41 C 0.7645(14) 0.0849(5) 0.5278(14) 0.1131(17) Uiso 0.50 1 d PD A 1 H41A H 0.8284 0.0705 0.5786 0.136 Uiso 0.50 1 calc PR A 1 H41B H 0.7649 0.0655 0.4756 0.136 Uiso 0.50 1 calc PR A 1 O5 O 0.7814(10) 0.1450(5) 0.5186(9) 0.1131(17) Uiso 0.50 1 d PD A 1 C42 C 0.8916(12) 0.1455(6) 0.5041(13) 0.1131(17) Uiso 0.50 1 d PD A 1 H42A H 0.8852 0.1269 0.4495 0.136 Uiso 0.50 1 calc PR A 1 H42B H 0.9552 0.1294 0.5533 0.136 Uiso 0.50 1 calc PR A 1 C43 C 0.9031(16) 0.2080(6) 0.4987(12) 0.1131(17) Uiso 0.50 1 d PD A 1 H43A H 0.9768 0.2168 0.4946 0.170 Uiso 0.50 1 calc PR A 1 H43B H 0.8987 0.2251 0.5507 0.170 Uiso 0.50 1 calc PR A 1 H43C H 0.8411 0.2219 0.4473 0.170 Uiso 0.50 1 calc PR A 1 C44 C 0.4834(14) 0.0388(8) 0.3378(11) 0.1131(17) Uiso 0.50 1 d PD B 2 H44A H 0.4473 0.0093 0.2968 0.170 Uiso 0.50 1 calc PR B 2 H44B H 0.4925 0.0711 0.3060 0.170 Uiso 0.50 1 calc PR B 2 H44C H 0.4353 0.0481 0.3706 0.170 Uiso 0.50 1 calc PR B 2 C45 C 0.5973(14) 0.0205(7) 0.3987(11) 0.1131(17) Uiso 0.50 1 d PD B 2 H45A H 0.5892 -0.0065 0.4405 0.136 Uiso 0.50 1 calc PR B 2 H45B H 0.6413 0.0036 0.3668 0.136 Uiso 0.50 1 calc PR B 2 O6 O 0.6537(10) 0.0700(5) 0.4433(8) 0.1131(17) Uiso 0.50 1 d PD B 2 C46 C 0.7663(14) 0.0650(7) 0.4948(12) 0.1131(17) Uiso 0.50 1 d PD B 2 H46A H 0.8101 0.0482 0.4625 0.136 Uiso 0.50 1 calc PR B 2 H46B H 0.7757 0.0423 0.5463 0.136 Uiso 0.50 1 calc PR B 2 C47 C 0.8047(17) 0.1219(7) 0.5205(14) 0.1131(17) Uiso 0.50 1 d PD B 2 H47A H 0.8836 0.1262 0.5240 0.170 Uiso 0.50 1 calc PR B 2 H47B H 0.8008 0.1297 0.5772 0.170 Uiso 0.50 1 calc PR B 2 H47C H 0.7550 0.1473 0.4773 0.170 Uiso 0.50 1 calc PR B 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 0.0125(3) 0.0244(3) 0.0428(4) -0.0063(3) 0.0083(2) -0.0031(2) Cl1 0.0607(8) 0.0648(9) 0.0417(7) 0.0045(6) -0.0041(6) -0.0241(7) Cl2 0.0698(9) 0.0544(8) 0.0500(8) 0.0030(6) 0.0274(7) -0.0170(7) Cl3 0.0319(6) 0.0362(6) 0.0719(8) -0.0066(5) 0.0297(6) -0.0101(5) Cl4 0.0157(4) 0.0344(6) 0.0556(7) -0.0093(5) 0.0073(4) -0.0059(4) O1 0.0167(13) 0.0270(15) 0.0516(19) -0.0080(13) 0.0126(13) -0.0038(11) O2 0.0136(13) 0.0228(14) 0.0449(17) -0.0063(12) 0.0094(12) -0.0019(10) O3 0.0208(14) 0.0315(15) 0.0407(17) -0.0059(13) 0.0060(13) -0.0080(12) O4 0.0128(12) 0.0274(14) 0.0391(17) -0.0078(13) 0.0060(12) -0.0027(10) N1 0.0173(16) 0.0237(17) 0.042(2) -0.0070(15) 0.0097(15) -0.0021(13) N2 0.0190(16) 0.0276(18) 0.049(2) -0.0069(16) 0.0086(16) 0.0000(14) C1 0.0173(19) 0.027(2) 0.041(2) -0.0048(18) 0.0111(17) -0.0015(15) C2 0.0161(18) 0.027(2) 0.040(2) -0.0047(18) 0.0084(17) -0.0010(16) C3 0.0181(19) 0.029(2) 0.043(3) -0.0054(18) 0.0086(18) 0.0024(16) C4 0.021(2) 0.026(2) 0.042(3) -0.0072(18) 0.0102(18) -0.0001(16) C5 0.0184(19) 0.029(2) 0.038(2) -0.0066(18) 0.0098(17) -0.0017(16) C6 0.0170(18) 0.025(2) 0.043(2) -0.0036(18) 0.0103(17) 0.0000(15) C7 0.020(2) 0.036(2) 0.059(3) -0.015(2) 0.017(2) -0.0028(18) C8 0.031(2) 0.049(3) 0.070(4) -0.016(3) 0.031(2) -0.010(2) C9 0.022(2) 0.044(3) 0.075(4) -0.021(3) 0.010(2) 0.002(2) C10 0.024(2) 0.041(3) 0.068(3) -0.019(2) 0.023(2) -0.0023(19) C11 0.022(2) 0.023(2) 0.056(3) -0.0092(19) 0.017(2) -0.0054(16) C12 0.026(2) 0.040(3) 0.054(3) -0.018(2) 0.015(2) -0.0103(19) C13 0.036(3) 0.030(2) 0.069(3) -0.006(2) 0.025(2) -0.0041(19) C14 0.025(2) 0.030(2) 0.059(3) -0.010(2) 0.016(2) -0.0098(18) C15 0.0159(18) 0.025(2) 0.049(3) -0.0092(18) 0.0127(18) -0.0015(15) C16 0.0151(18) 0.022(2) 0.041(2) -0.0041(17) 0.0076(17) -0.0034(15) C17 0.0182(18) 0.0196(19) 0.043(2) -0.0022(17) 0.0113(17) -0.0010(15) C18 0.021(2) 0.025(2) 0.058(3) -0.011(2) 0.018(2) -0.0025(16) C19 0.018(2) 0.033(2) 0.076(4) -0.022(2) 0.015(2) -0.0067(18) C20 0.021(2) 0.030(2) 0.071(3) -0.020(2) 0.015(2) -0.0050(17) C21 0.0199(19) 0.0212(19) 0.043(2) -0.0041(17) 0.0133(18) -0.0021(15) C22 0.028(2) 0.019(2) 0.075(3) -0.004(2) 0.023(2) -0.0043(17) C23 0.025(2) 0.026(2) 0.056(3) -0.010(2) 0.015(2) 0.0010(17) C24 0.027(2) 0.047(3) 0.045(3) -0.006(2) 0.009(2) 0.008(2) C25 0.017(2) 0.054(3) 0.120(5) -0.051(3) 0.023(3) -0.012(2) C26 0.016(2) 0.078(4) 0.102(5) -0.050(4) 0.008(3) 0.001(2) C27 0.039(3) 0.050(3) 0.165(7) -0.036(4) 0.061(4) -0.020(3) C28 0.019(2) 0.084(5) 0.199(8) -0.097(5) 0.031(4) -0.021(3) C29 0.021(2) 0.027(2) 0.042(3) -0.0071(18) 0.0116(18) -0.0031(16) C30 0.036(2) 0.037(2) 0.036(3) -0.007(2) 0.008(2) -0.0068(19) C31 0.044(3) 0.033(2) 0.042(3) -0.005(2) 0.023(2) -0.005(2) C32 0.025(2) 0.028(2) 0.051(3) -0.010(2) 0.021(2) -0.0064(17) C33 0.0162(18) 0.027(2) 0.042(2) -0.0110(18) 0.0111(17) -0.0012(15) C34 0.0203(19) 0.0209(19) 0.039(2) -0.0080(17) 0.0133(17) 0.0007(15) C35 0.020(2) 0.031(2) 0.057(3) -0.002(2) 0.006(2) 0.0013(17) C36 0.023(2) 0.044(3) 0.056(3) -0.004(2) 0.002(2) 0.002(2) C37 0.033(3) 0.059(3) 0.055(3) 0.011(3) 0.001(2) 0.003(2) C38 0.035(3) 0.099(5) 0.063(4) 0.029(3) 0.006(3) -0.015(3) C39 0.024(2) 0.064(3) 0.051(3) 0.013(3) 0.004(2) -0.004(2) _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 O4 1.932(3) . ? Fe1 O3 1.967(3) . ? Fe1 O2 2.006(3) . ? Fe1 O1 2.064(3) . ? Fe1 N1 2.156(3) . ? Fe1 N2 2.163(4) . ? Cl1 C30 1.733(5) . ? Cl2 C31 1.728(5) . ? Cl3 C32 1.734(4) . ? Cl4 C33 1.740(4) . ? O1 C2 1.268(5) . ? O2 C16 1.285(4) . ? O3 C29 1.328(5) . ? O4 C34 1.329(5) . ? N1 C1 1.332(5) . ? N1 C15 1.356(5) . ? N2 C39 1.333(6) . ? N2 C35 1.355(5) . ? C1 C6 1.421(5) . ? C1 C2 1.464(5) . ? C2 C3 1.453(6) . ? C3 C4 1.360(6) . ? C3 C7 1.536(5) . ? C4 C5 1.444(5) . ? C5 C6 1.349(6) . ? C5 C11 1.527(5) . ? C7 C8 1.526(7) . ? C7 C9 1.541(6) . ? C7 C10 1.544(6) . ? C11 C14 1.533(6) . ? C11 C12 1.534(7) . ? C11 C13 1.538(6) . ? C15 C20 1.422(5) . ? C15 C16 1.452(5) . ? C16 C17 1.440(5) . ? C17 C18 1.366(5) . ? C17 C21 1.521(5) . ? C18 C19 1.433(6) . ? C19 C20 1.360(6) . ? C19 C25 1.533(6) . ? C21 C24 1.532(6) . ? C21 C23 1.534(5) . ? C21 C22 1.540(6) . ? C25 C26 1.530(9) . ? C25 C27 1.534(9) . ? C25 C28 1.542(7) . ? C29 C30 1.382(6) . ? C29 C34 1.415(6) . ? C30 C31 1.410(6) . ? C31 C32 1.380(6) . ? C32 C33 1.385(6) . ? C33 C34 1.385(5) . ? C35 C36 1.386(7) . ? C36 C37 1.357(7) . ? C37 C38 1.391(7) . ? C38 C39 1.383(7) . ? C40 C41 1.539(2) . ? C41 O5 1.498(2) . ? O5 C42 1.497(2) . ? C42 C43 1.539(2) . ? C44 C45 1.485(15) . ? C45 O6 1.459(14) . ? O6 C46 1.365(15) . ? C46 C47 1.480(16) . ? 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 O4 Fe1 O3 83.11(12) . . ? O4 Fe1 O2 102.78(11) . . ? O3 Fe1 O2 97.56(12) . . ? O4 Fe1 O1 106.09(11) . . ? O3 Fe1 O1 90.11(12) . . ? O2 Fe1 O1 150.81(10) . . ? O4 Fe1 N1 177.05(13) . . ? O3 Fe1 N1 94.28(12) . . ? O2 Fe1 N1 76.15(11) . . ? O1 Fe1 N1 75.22(11) . . ? O4 Fe1 N2 86.10(12) . . ? O3 Fe1 N2 166.64(12) . . ? O2 Fe1 N2 92.48(12) . . ? O1 Fe1 N2 85.33(13) . . ? N1 Fe1 N2 96.68(13) . . ? C2 O1 Fe1 117.4(2) . . ? C16 O2 Fe1 117.7(2) . . ? C29 O3 Fe1 111.6(3) . . ? C34 O4 Fe1 112.9(2) . . ? C1 N1 C15 130.2(3) . . ? C1 N1 Fe1 116.0(2) . . ? C15 N1 Fe1 113.8(2) . . ? C39 N2 C35 117.1(4) . . ? C39 N2 Fe1 122.3(3) . . ? C35 N2 Fe1 120.2(3) . . ? N1 C1 C6 128.4(4) . . ? N1 C1 C2 111.5(3) . . ? C6 C1 C2 120.1(3) . . ? O1 C2 C3 122.3(3) . . ? O1 C2 C1 119.4(3) . . ? C3 C2 C1 118.2(3) . . ? C4 C3 C2 117.0(4) . . ? C4 C3 C7 123.2(4) . . ? C2 C3 C7 119.8(3) . . ? C3 C4 C5 125.1(4) . . ? C6 C5 C4 118.3(4) . . ? C6 C5 C11 123.3(4) . . ? C4 C5 C11 118.3(3) . . ? C5 C6 C1 120.9(4) . . ? C8 C7 C3 108.7(4) . . ? C8 C7 C9 111.5(4) . . ? C3 C7 C9 110.5(4) . . ? C8 C7 C10 108.5(4) . . ? C3 C7 C10 110.8(3) . . ? C9 C7 C10 106.9(4) . . ? C5 C11 C14 111.3(3) . . ? C5 C11 C12 108.7(4) . . ? C14 C11 C12 109.0(4) . . ? C5 C11 C13 110.1(3) . . ? C14 C11 C13 107.7(4) . . ? C12 C11 C13 110.1(4) . . ? N1 C15 C20 128.3(4) . . ? N1 C15 C16 111.4(3) . . ? C20 C15 C16 120.2(3) . . ? O2 C16 C17 122.4(3) . . ? O2 C16 C15 118.8(3) . . ? C17 C16 C15 118.8(3) . . ? C18 C17 C16 117.2(4) . . ? C18 C17 C21 122.4(3) . . ? C16 C17 C21 120.5(3) . . ? C17 C18 C19 124.9(4) . . ? C20 C19 C18 118.3(4) . . ? C20 C19 C25 123.1(4) . . ? C18 C19 C25 118.5(4) . . ? C19 C20 C15 120.5(4) . . ? C17 C21 C24 109.3(3) . . ? C17 C21 C23 111.9(3) . . ? C24 C21 C23 108.5(4) . . ? C17 C21 C22 110.5(3) . . ? C24 C21 C22 109.2(4) . . ? C23 C21 C22 107.2(3) . . ? C26 C25 C19 109.6(5) . . ? C26 C25 C27 109.7(4) . . ? C19 C25 C27 108.9(5) . . ? C26 C25 C28 109.2(6) . . ? C19 C25 C28 111.0(4) . . ? C27 C25 C28 108.3(5) . . ? O3 C29 C30 125.1(4) . . ? O3 C29 C34 116.2(4) . . ? C30 C29 C34 118.8(4) . . ? C29 C30 C31 120.7(4) . . ? C29 C30 Cl1 118.4(3) . . ? C31 C30 Cl1 120.9(4) . . ? C32 C31 C30 119.9(4) . . ? C32 C31 Cl2 120.4(3) . . ? C30 C31 Cl2 119.6(4) . . ? C31 C32 C33 119.7(4) . . ? C31 C32 Cl3 120.1(4) . . ? C33 C32 Cl3 120.2(3) . . ? C32 C33 C34 121.1(4) . . ? C32 C33 Cl4 120.9(3) . . ? C34 C33 Cl4 118.0(3) . . ? O4 C34 C33 124.0(4) . . ? O4 C34 C29 116.1(3) . . ? C33 C34 C29 119.8(4) . . ? N2 C35 C36 122.6(4) . . ? C37 C36 C35 119.5(4) . . ? C36 C37 C38 118.8(5) . . ? C39 C38 C37 118.6(5) . . ? N2 C39 C38 123.3(4) . . ? O5 C41 C40 110.8(12) . . ? C42 O5 C41 101.6(10) . . ? O5 C42 C43 97.6(11) . . ? O6 C45 C44 105.1(13) . . ? C46 O6 C45 116.2(13) . . ? O6 C46 C47 104.4(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Fe1 O1 C2 -177.6(3) . . . . ? O3 Fe1 O1 C2 99.6(3) . . . . ? O2 Fe1 O1 C2 -6.3(4) . . . . ? N1 Fe1 O1 C2 5.2(3) . . . . ? N2 Fe1 O1 C2 -93.0(3) . . . . ? O4 Fe1 O2 C16 -164.4(3) . . . . ? O3 Fe1 O2 C16 -79.8(3) . . . . ? O1 Fe1 O2 C16 24.2(4) . . . . ? N1 Fe1 O2 C16 12.8(3) . . . . ? N2 Fe1 O2 C16 109.1(3) . . . . ? O4 Fe1 O3 C29 -3.2(3) . . . . ? O2 Fe1 O3 C29 -105.2(3) . . . . ? O1 Fe1 O3 C29 103.0(3) . . . . ? N1 Fe1 O3 C29 178.2(3) . . . . ? N2 Fe1 O3 C29 33.1(7) . . . . ? O3 Fe1 O4 C34 2.2(2) . . . . ? O2 Fe1 O4 C34 98.4(2) . . . . ? O1 Fe1 O4 C34 -85.9(2) . . . . ? N1 Fe1 O4 C34 30(3) . . . . ? N2 Fe1 O4 C34 -169.9(2) . . . . ? O4 Fe1 N1 C1 -123(2) . . . . ? O3 Fe1 N1 C1 -95.3(3) . . . . ? O2 Fe1 N1 C1 167.9(3) . . . . ? O1 Fe1 N1 C1 -6.3(3) . . . . ? N2 Fe1 N1 C1 77.0(3) . . . . ? O4 Fe1 N1 C15 57(3) . . . . ? O3 Fe1 N1 C15 84.4(3) . . . . ? O2 Fe1 N1 C15 -12.4(3) . . . . ? O1 Fe1 N1 C15 173.3(3) . . . . ? N2 Fe1 N1 C15 -103.3(3) . . . . ? O4 Fe1 N2 C39 -163.2(4) . . . . ? O3 Fe1 N2 C39 160.7(5) . . . . ? O2 Fe1 N2 C39 -60.5(4) . . . . ? O1 Fe1 N2 C39 90.3(4) . . . . ? N1 Fe1 N2 C39 15.8(4) . . . . ? O4 Fe1 N2 C35 24.2(3) . . . . ? O3 Fe1 N2 C35 -11.9(7) . . . . ? O2 Fe1 N2 C35 126.8(3) . . . . ? O1 Fe1 N2 C35 -82.3(3) . . . . ? N1 Fe1 N2 C35 -156.8(3) . . . . ? C15 N1 C1 C6 8.8(8) . . . . ? Fe1 N1 C1 C6 -171.6(4) . . . . ? C15 N1 C1 C2 -173.3(4) . . . . ? Fe1 N1 C1 C2 6.3(5) . . . . ? Fe1 O1 C2 C3 178.8(3) . . . . ? Fe1 O1 C2 C1 -3.6(5) . . . . ? N1 C1 C2 O1 -2.0(6) . . . . ? C6 C1 C2 O1 176.1(4) . . . . ? N1 C1 C2 C3 175.7(4) . . . . ? C6 C1 C2 C3 -6.2(6) . . . . ? O1 C2 C3 C4 180.0(4) . . . . ? C1 C2 C3 C4 2.4(6) . . . . ? O1 C2 C3 C7 1.8(7) . . . . ? C1 C2 C3 C7 -175.9(4) . . . . ? C2 C3 C4 C5 2.9(7) . . . . ? C7 C3 C4 C5 -179.0(4) . . . . ? C3 C4 C5 C6 -4.4(7) . . . . ? C3 C4 C5 C11 176.7(4) . . . . ? C4 C5 C6 C1 0.2(6) . . . . ? C11 C5 C6 C1 179.1(4) . . . . ? N1 C1 C6 C5 -177.4(4) . . . . ? C2 C1 C6 C5 4.9(6) . . . . ? C4 C3 C7 C8 -113.9(5) . . . . ? C2 C3 C7 C8 64.2(5) . . . . ? C4 C3 C7 C9 123.5(5) . . . . ? C2 C3 C7 C9 -58.4(5) . . . . ? C4 C3 C7 C10 5.2(6) . . . . ? C2 C3 C7 C10 -176.7(4) . . . . ? C6 C5 C11 C14 5.3(6) . . . . ? C4 C5 C11 C14 -175.8(4) . . . . ? C6 C5 C11 C12 -114.7(5) . . . . ? C4 C5 C11 C12 64.2(5) . . . . ? C6 C5 C11 C13 124.7(5) . . . . ? C4 C5 C11 C13 -56.4(5) . . . . ? C1 N1 C15 C20 14.2(8) . . . . ? Fe1 N1 C15 C20 -165.4(4) . . . . ? C1 N1 C15 C16 -170.2(4) . . . . ? Fe1 N1 C15 C16 10.2(5) . . . . ? Fe1 O2 C16 C17 169.2(3) . . . . ? Fe1 O2 C16 C15 -11.7(5) . . . . ? N1 C15 C16 O2 0.3(6) . . . . ? C20 C15 C16 O2 176.3(4) . . . . ? N1 C15 C16 C17 179.4(4) . . . . ? C20 C15 C16 C17 -4.6(6) . . . . ? O2 C16 C17 C18 -179.6(4) . . . . ? C15 C16 C17 C18 1.3(6) . . . . ? O2 C16 C17 C21 1.4(6) . . . . ? C15 C16 C17 C21 -177.7(4) . . . . ? C16 C17 C18 C19 1.7(7) . . . . ? C21 C17 C18 C19 -179.3(4) . . . . ? C17 C18 C19 C20 -1.5(8) . . . . ? C17 C18 C19 C25 176.2(5) . . . . ? C18 C19 C20 C15 -2.0(8) . . . . ? C25 C19 C20 C15 -179.6(5) . . . . ? N1 C15 C20 C19 -179.8(5) . . . . ? C16 C15 C20 C19 5.0(7) . . . . ? C18 C17 C21 C24 -117.0(4) . . . . ? C16 C17 C21 C24 62.0(5) . . . . ? C18 C17 C21 C23 3.3(6) . . . . ? C16 C17 C21 C23 -177.7(4) . . . . ? C18 C17 C21 C22 122.8(4) . . . . ? C16 C17 C21 C22 -58.2(5) . . . . ? C20 C19 C25 C26 120.0(6) . . . . ? C18 C19 C25 C26 -57.5(7) . . . . ? C20 C19 C25 C27 -119.9(6) . . . . ? C18 C19 C25 C27 62.5(6) . . . . ? C20 C19 C25 C28 -0.8(9) . . . . ? C18 C19 C25 C28 -178.3(6) . . . . ? Fe1 O3 C29 C30 -176.8(3) . . . . ? Fe1 O3 C29 C34 3.6(4) . . . . ? O3 C29 C30 C31 -178.2(4) . . . . ? C34 C29 C30 C31 1.4(6) . . . . ? O3 C29 C30 Cl1 -0.1(6) . . . . ? C34 C29 C30 Cl1 179.5(3) . . . . ? C29 C30 C31 C32 -0.3(7) . . . . ? Cl1 C30 C31 C32 -178.4(3) . . . . ? C29 C30 C31 Cl2 178.3(3) . . . . ? Cl1 C30 C31 Cl2 0.2(6) . . . . ? C30 C31 C32 C33 -0.1(6) . . . . ? Cl2 C31 C32 C33 -178.7(3) . . . . ? C30 C31 C32 Cl3 -178.8(3) . . . . ? Cl2 C31 C32 Cl3 2.6(5) . . . . ? C31 C32 C33 C34 -0.6(6) . . . . ? Cl3 C32 C33 C34 178.2(3) . . . . ? C31 C32 C33 Cl4 -179.1(3) . . . . ? Cl3 C32 C33 Cl4 -0.3(5) . . . . ? Fe1 O4 C34 C33 179.6(3) . . . . ? Fe1 O4 C34 C29 -0.8(4) . . . . ? C32 C33 C34 O4 -178.8(4) . . . . ? Cl4 C33 C34 O4 -0.3(5) . . . . ? C32 C33 C34 C29 1.6(6) . . . . ? Cl4 C33 C34 C29 -179.8(3) . . . . ? O3 C29 C34 O4 -1.9(5) . . . . ? C30 C29 C34 O4 178.4(4) . . . . ? O3 C29 C34 C33 177.6(3) . . . . ? C30 C29 C34 C33 -2.0(6) . . . . ? C39 N2 C35 C36 -2.9(7) . . . . ? Fe1 N2 C35 C36 170.1(4) . . . . ? N2 C35 C36 C37 1.2(8) . . . . ? C35 C36 C37 C38 1.3(8) . . . . ? C36 C37 C38 C39 -2.0(10) . . . . ? C35 N2 C39 C38 2.1(8) . . . . ? Fe1 N2 C39 C38 -170.7(5) . . . . ? C37 C38 C39 N2 0.3(10) . . . . ? C40 C41 O5 C42 -177.3(15) . . . . ? C41 O5 C42 C43 -178.2(15) . . . . ? C44 C45 O6 C46 -171.6(16) . . . . ? C45 O6 C46 C47 171.9(16) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.890 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.079 _iucr_refine_instructions_details ; TITL afh334 in P2(1)/n CELL 0.71073 12.6068 24.4311 16.6177 90.000 111.8027 90.000 ZERR 4.00 0.0011 0.0021 0.0014 0.000 0.0009 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O CL FE UNIT 172 220 8 20 16 4 TEMP -185.000 SIZE 0.196 0.237 0.415 rem APEX2 2011.4-1, SAINT 7.68a, SADABS 2008/1, SHELXTL 2008/4 rem Janice Wong 25s sphere 0.50 scan width ccd1 eadp c40 > c47 dfix 1.54 0.002 c40 c41 c42 c43 dfix 1.50 0.002 c41 o5 c42 o5 OMIT 2 0 0 SHEL 100 0.83 L.S. 12 acta 51 conf FMAP 2 PLAN 10 WGHT 0.061700 13.948999 FVAR 0.08467 FE1 6 0.086757 0.199893 0.144763 11.00000 0.01253 0.02442 = 0.04278 -0.00631 0.00828 -0.00311 CL1 5 0.166603 0.093398 0.415288 11.00000 0.06071 0.06479 = 0.04170 0.00448 -0.00408 -0.02407 CL2 5 -0.036489 0.012648 0.396074 11.00000 0.06981 0.05439 = 0.04998 0.00298 0.02742 -0.01696 CL3 5 -0.249102 0.008840 0.222479 11.00000 0.03191 0.03622 = 0.07191 -0.00658 0.02968 -0.01011 CL4 5 -0.255033 0.084197 0.066958 11.00000 0.01574 0.03436 = 0.05562 -0.00928 0.00727 -0.00589 O1 4 0.053023 0.267560 0.205719 11.00000 0.01674 0.02699 = 0.05157 -0.00801 0.01264 -0.00378 O2 4 0.186078 0.159601 0.094192 11.00000 0.01362 0.02284 = 0.04494 -0.00634 0.00943 -0.00191 O3 4 0.128467 0.157912 0.253151 11.00000 0.02084 0.03148 = 0.04073 -0.00590 0.00598 -0.00797 O4 4 -0.049042 0.155043 0.110559 11.00000 0.01279 0.02735 = 0.03906 -0.00783 0.00603 -0.00269 N1 3 0.243072 0.246601 0.187328 11.00000 0.01731 0.02367 = 0.04189 -0.00696 0.00967 -0.00212 N2 3 0.001246 0.244735 0.025966 11.00000 0.01904 0.02761 = 0.04877 -0.00690 0.00859 -0.00005 C1 1 0.239003 0.295469 0.221585 11.00000 0.01734 0.02665 = 0.04082 -0.00476 0.01115 -0.00153 C2 1 0.129589 0.304198 0.231413 11.00000 0.01609 0.02748 = 0.04015 -0.00471 0.00837 -0.00101 C3 1 0.114554 0.354094 0.273586 11.00000 0.01806 0.02867 = 0.04278 -0.00538 0.00861 0.00242 C4 1 0.202690 0.390371 0.298283 11.00000 0.02093 0.02625 = 0.04216 -0.00716 0.01017 -0.00015 AFIX 43 H4A 2 0.194920 0.422276 0.328311 11.00000 -1.20000 AFIX 0 C5 1 0.307130 0.384163 0.282414 11.00000 0.01836 0.02916 = 0.03840 -0.00656 0.00980 -0.00166 C6 1 0.323044 0.337454 0.245055 11.00000 0.01697 0.02469 = 0.04253 -0.00363 0.01034 0.00000 AFIX 43 H6A 2 0.391362 0.332564 0.234291 11.00000 -1.20000 AFIX 0 C7 1 0.004158 0.362962 0.290681 11.00000 0.02036 0.03586 = 0.05853 -0.01493 0.01721 -0.00283 C8 1 -0.002893 0.319396 0.354326 11.00000 0.03057 0.04899 = 0.06962 -0.01634 0.03146 -0.00978 AFIX 137 H8A 2 -0.008942 0.283132 0.327777 11.00000 -1.50000 H8B 2 -0.070280 0.326125 0.368909 11.00000 -1.50000 H8C 2 0.066015 0.320955 0.407160 11.00000 -1.50000 AFIX 0 C9 1 -0.100647 0.360892 0.205116 11.00000 0.02186 0.04431 = 0.07539 -0.02061 0.01045 0.00178 AFIX 137 H9A 2 -0.105663 0.324636 0.178721 11.00000 -1.50000 H9B 2 -0.092872 0.388820 0.165331 11.00000 -1.50000 H9C 2 -0.170060 0.367905 0.216880 11.00000 -1.50000 AFIX 0 C10 1 0.003834 0.419885 0.330912 11.00000 0.02403 0.04138 = 0.06778 -0.01890 0.02332 -0.00229 AFIX 137 H10A 2 0.070411 0.423205 0.385096 11.00000 -1.50000 H10B 2 -0.066191 0.424252 0.342866 11.00000 -1.50000 H10C 2 0.007074 0.448336 0.290315 11.00000 -1.50000 AFIX 0 C11 1 0.394866 0.430370 0.310210 11.00000 0.02247 0.02304 = 0.05597 -0.00917 0.01658 -0.00542 C12 1 0.439170 0.435550 0.409206 11.00000 0.02550 0.03971 = 0.05371 -0.01821 0.01546 -0.01028 AFIX 137 H12A 2 0.375103 0.443218 0.427409 11.00000 -1.50000 H12B 2 0.494674 0.465513 0.427835 11.00000 -1.50000 H12C 2 0.476044 0.401230 0.435638 11.00000 -1.50000 AFIX 0 C13 1 0.339712 0.484496 0.267738 11.00000 0.03593 0.02964 = 0.06907 -0.00601 0.02540 -0.00415 AFIX 137 H13A 2 0.273116 0.492267 0.282840 11.00000 -1.50000 H13B 2 0.315553 0.481441 0.204645 11.00000 -1.50000 H13C 2 0.395325 0.514267 0.288668 11.00000 -1.50000 AFIX 0 C14 1 0.495930 0.418829 0.282482 11.00000 0.02529 0.02967 = 0.05914 -0.01025 0.01625 -0.00979 AFIX 137 H14A 2 0.533275 0.384662 0.309212 11.00000 -1.50000 H14B 2 0.550837 0.449028 0.301259 11.00000 -1.50000 H14C 2 0.468270 0.415421 0.219252 11.00000 -1.50000 AFIX 0 C15 1 0.331053 0.220772 0.174989 11.00000 0.01589 0.02521 = 0.04886 -0.00922 0.01270 -0.00149 C16 1 0.292652 0.172057 0.122102 11.00000 0.01511 0.02227 = 0.04053 -0.00405 0.00759 -0.00337 C17 1 0.375214 0.139903 0.101883 11.00000 0.01822 0.01962 = 0.04281 -0.00221 0.01135 -0.00103 C18 1 0.486287 0.156984 0.135739 11.00000 0.02084 0.02528 = 0.05817 -0.01050 0.01759 -0.00253 AFIX 43 H18A 2 0.540831 0.136533 0.121307 11.00000 -1.20000 AFIX 0 C19 1 0.526658 0.203444 0.191391 11.00000 0.01762 0.03308 = 0.07639 -0.02159 0.01475 -0.00668 C20 1 0.449339 0.233906 0.211139 11.00000 0.02068 0.03016 = 0.07062 -0.01960 0.01456 -0.00495 AFIX 43 H20A 2 0.474544 0.264195 0.249385 11.00000 -1.20000 AFIX 0 C21 1 0.337919 0.089759 0.043953 11.00000 0.01985 0.02118 = 0.04301 -0.00411 0.01333 -0.00210 C22 1 0.278009 0.048283 0.082664 11.00000 0.02822 0.01864 = 0.07477 -0.00430 0.02338 -0.00427 AFIX 137 H22A 2 0.330272 0.037436 0.140615 11.00000 -1.50000 H22B 2 0.256021 0.015910 0.045280 11.00000 -1.50000 H22C 2 0.209611 0.065112 0.086731 11.00000 -1.50000 AFIX 0 C23 1 0.439605 0.060264 0.033806 11.00000 0.02468 0.02603 = 0.05563 -0.01033 0.01494 0.00104 AFIX 137 H23A 2 0.477913 0.085063 0.006910 11.00000 -1.50000 H23B 2 0.412322 0.027891 -0.002922 11.00000 -1.50000 H23C 2 0.493565 0.048990 0.090944 11.00000 -1.50000 AFIX 0 C24 1 0.255211 0.107251 -0.045976 11.00000 0.02666 0.04654 = 0.04455 -0.00586 0.00906 0.00845 AFIX 137 H24A 2 0.292064 0.134675 -0.069920 11.00000 -1.50000 H24B 2 0.186264 0.122971 -0.041211 11.00000 -1.50000 H24C 2 0.234382 0.075299 -0.084341 11.00000 -1.50000 AFIX 0 C25 1 0.655334 0.215136 0.228589 11.00000 0.01743 0.05372 = 0.12018 -0.05067 0.02318 -0.01172 C26 1 0.719291 0.165347 0.279669 11.00000 0.01578 0.07797 = 0.10217 -0.05033 0.00840 0.00148 AFIX 137 H26A 2 0.692431 0.157382 0.326716 11.00000 -1.50000 H26B 2 0.801407 0.173125 0.304068 11.00000 -1.50000 H26C 2 0.704992 0.133648 0.240933 11.00000 -1.50000 AFIX 0 C27 1 0.695013 0.227041 0.153535 11.00000 0.03863 0.04975 = 0.16494 -0.03565 0.06073 -0.01996 AFIX 137 H27A 2 0.654047 0.259018 0.121135 11.00000 -1.50000 H27B 2 0.679042 0.195258 0.114859 11.00000 -1.50000 H27C 2 0.777298 0.234450 0.176669 11.00000 -1.50000 AFIX 0 C28 1 0.682772 0.265517 0.288820 11.00000 0.01853 0.08364 = 0.19933 -0.09685 0.03125 -0.02086 AFIX 137 H28A 2 0.646741 0.298047 0.255291 11.00000 -1.50000 H28B 2 0.765696 0.270844 0.314388 11.00000 -1.50000 H28C 2 0.653312 0.259667 0.335047 11.00000 -1.50000 AFIX 0 C29 1 0.045746 0.123737 0.251560 11.00000 0.02089 0.02710 = 0.04221 -0.00712 0.01164 -0.00305 C30 1 0.047777 0.090757 0.319706 11.00000 0.03583 0.03730 = 0.03605 -0.00735 0.00830 -0.00685 C31 1 -0.043218 0.054685 0.310658 11.00000 0.04411 0.03297 = 0.04227 -0.00491 0.02294 -0.00543 C32 1 -0.135807 0.052275 0.233256 11.00000 0.02514 0.02816 = 0.05096 -0.01032 0.02121 -0.00636 C33 1 -0.138764 0.085445 0.164889 11.00000 0.01621 0.02702 = 0.04205 -0.01097 0.01113 -0.00117 C34 1 -0.050574 0.121506 0.173052 11.00000 0.02033 0.02090 = 0.03913 -0.00797 0.01326 0.00068 C35 1 -0.114274 0.244613 -0.011384 11.00000 0.01994 0.03129 = 0.05693 -0.00156 0.00634 0.00127 AFIX 43 H35A 2 -0.155990 0.220104 0.010125 11.00000 -1.20000 AFIX 0 C36 1 -0.174029 0.278833 -0.079744 11.00000 0.02281 0.04403 = 0.05555 -0.00350 0.00229 0.00214 AFIX 43 H36A 2 -0.255164 0.278104 -0.103607 11.00000 -1.20000 AFIX 0 C37 1 -0.115708 0.313389 -0.112321 11.00000 0.03288 0.05944 = 0.05528 0.01095 0.00120 0.00307 AFIX 43 H37A 2 -0.155320 0.337653 -0.158370 11.00000 -1.20000 AFIX 0 C38 1 0.003082 0.312647 -0.077092 11.00000 0.03457 0.09869 = 0.06348 0.02909 0.00560 -0.01527 AFIX 43 H38A 2 0.046175 0.335541 -0.099792 11.00000 -1.20000 AFIX 0 C39 1 0.057176 0.277890 -0.008325 11.00000 0.02417 0.06447 = 0.05130 0.01345 0.00371 -0.00421 AFIX 43 H39A 2 0.138320 0.277636 0.015686 11.00000 -1.20000 AFIX 0 PART 1 C40 1 0.650639 0.074102 0.539237 10.50000 0.11307 AFIX 137 H40A 2 0.621427 0.038015 0.515526 10.50000 -1.50000 H40B 2 0.595081 0.102291 0.508452 10.50000 -1.50000 H40C 2 0.662914 0.075111 0.601013 10.50000 -1.50000 AFIX 0 C41 1 0.764510 0.084925 0.527802 10.50000 0.11307 AFIX 23 H41A 2 0.828357 0.070532 0.578638 10.50000 -1.20000 H41B 2 0.764878 0.065486 0.475634 10.50000 -1.20000 AFIX 0 O5 4 0.781359 0.144955 0.518624 10.50000 0.11307 C42 1 0.891613 0.145515 0.504067 10.50000 0.11307 AFIX 23 H42A 2 0.885168 0.126946 0.449493 10.50000 -1.20000 H42B 2 0.955206 0.129356 0.553265 10.50000 -1.20000 AFIX 0 C43 1 0.903109 0.207990 0.498680 10.50000 0.11307 AFIX 137 H43A 2 0.976825 0.216774 0.494650 10.50000 -1.50000 H43B 2 0.898675 0.225062 0.550705 10.50000 -1.50000 H43C 2 0.841147 0.221919 0.447254 10.50000 -1.50000 AFIX 0 PART 2 same c40 c41 o5 c42 c43 C44 1 0.483399 0.038809 0.337844 10.50000 0.11307 AFIX 137 H44A 2 0.447332 0.009310 0.296833 10.50000 -1.50000 H44B 2 0.492463 0.071095 0.305989 10.50000 -1.50000 H44C 2 0.435261 0.048114 0.370551 10.50000 -1.50000 AFIX 0 C45 1 0.597254 0.020486 0.398693 10.50000 0.11307 AFIX 23 H45A 2 0.589220 -0.006494 0.440518 10.50000 -1.20000 H45B 2 0.641317 0.003568 0.366756 10.50000 -1.20000 AFIX 0 O6 4 0.653659 0.070019 0.443251 10.50000 0.11307 C46 1 0.766310 0.065014 0.494833 10.50000 0.11307 AFIX 23 H46A 2 0.810080 0.048244 0.462547 10.50000 -1.20000 H46B 2 0.775742 0.042262 0.546340 10.50000 -1.20000 AFIX 0 C47 1 0.804679 0.121864 0.520502 10.50000 0.11307 AFIX 137 H47A 2 0.883563 0.126160 0.524003 10.50000 -1.50000 H47B 2 0.800831 0.129728 0.577183 10.50000 -1.50000 H47C 2 0.755041 0.147337 0.477311 10.50000 -1.50000 PART 0 HKLF 4 REM afh334 in P2(1)/n REM R1 = 0.0610 for 6367 Fo > 4sig(Fo) and 0.0916 for all 8703 data REM 498 parameters refined using 11 restraints END WGHT 0.0617 13.9497 REM Highest difference peak 0.890, deepest hole -0.698, 1-sigma level 0.079 Q1 1 0.6974 0.0909 0.4400 11.00000 0.05 0.70 Q2 1 0.5420 0.0407 0.3136 11.00000 0.05 0.61 Q3 1 0.4829 -0.0216 0.3999 11.00000 0.05 0.56 Q4 1 0.4585 0.0079 0.3808 11.00000 0.05 0.51 Q5 1 0.4400 0.0785 0.3062 11.00000 0.05 0.49 Q6 1 0.6253 0.0433 0.4599 11.00000 0.05 0.48 Q7 1 0.4905 -0.0171 0.3210 11.00000 0.05 0.48 Q8 1 0.5280 0.0820 0.5802 11.00000 0.05 0.47 Q9 1 0.8193 0.2010 0.5230 11.00000 0.05 0.45 Q10 1 0.0436 0.2047 0.0599 11.00000 0.05 0.45 ; data_afh336 _database_code_depnum_ccdc_archive 'CCDC 916896' #TrackingRef '[ONO]Fe_CIF.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; [ONOcat]Fe(py)3 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H90 Fe2 N4 O4' _chemical_formula_weight 1115.12 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.1943(10) _cell_length_b 14.2798(10) _cell_length_c 17.1104(13) _cell_angle_alpha 90.00 _cell_angle_beta 113.9953(9) _cell_angle_gamma 90.00 _cell_volume 3168.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 9522 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 26.29 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1196 _exptl_absorpt_coefficient_mu 0.505 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9022 _exptl_absorpt_correction_T_max 0.9612 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 33737 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 26.42 _reflns_number_total 6485 _reflns_number_gt 5107 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0655P)^2^+1.0602P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6485 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1125 _refine_ls_wR_factor_gt 0.1024 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.47137(2) 0.48383(2) 0.070801(17) 0.01610(10) Uani 1 1 d . . . O1 O 0.35283(11) 0.55869(10) 0.03399(9) 0.0222(3) Uani 1 1 d . . . O2 O 0.60123(11) 0.49831(10) 0.16184(9) 0.0202(3) Uani 1 1 d . . . N1 N 0.52727(13) 0.60068(11) 0.02133(10) 0.0168(3) Uani 1 1 d . . . N2 N 0.42095(14) 0.39822(12) 0.14859(11) 0.0217(4) Uani 1 1 d . . . C1 C 0.44531(15) 0.66856(14) -0.01036(12) 0.0186(4) Uani 1 1 d . . . C2 C 0.35368(16) 0.64085(14) -0.00347(13) 0.0204(4) Uani 1 1 d . . . C3 C 0.26571(16) 0.69919(16) -0.03627(13) 0.0241(5) Uani 1 1 d . . . C4 C 0.27383(18) 0.78131(16) -0.07574(14) 0.0276(5) Uani 1 1 d . . . H4A H 0.2156 0.8216 -0.0971 0.033 Uiso 1 1 calc R . . C5 C 0.36235(18) 0.80876(15) -0.08614(13) 0.0254(5) Uani 1 1 d . . . C6 C 0.44866(17) 0.75146(15) -0.05229(13) 0.0228(4) Uani 1 1 d . . . H6A H 0.5103 0.7688 -0.0577 0.027 Uiso 1 1 calc R . . C7 C 0.16647(17) 0.67055(18) -0.02640(15) 0.0308(5) Uani 1 1 d . . . C8 C 0.1910(2) 0.6592(2) 0.06928(16) 0.0393(6) Uani 1 1 d . . . H8A H 0.1284 0.6406 0.0762 0.059 Uiso 1 1 calc R . . H8B H 0.2161 0.7189 0.0987 0.059 Uiso 1 1 calc R . . H8C H 0.2441 0.6111 0.0939 0.059 Uiso 1 1 calc R . . C9 C 0.12376(19) 0.57885(19) -0.07408(17) 0.0386(6) Uani 1 1 d . . . H9A H 0.1774 0.5306 -0.0543 0.058 Uiso 1 1 calc R . . H9B H 0.1020 0.5887 -0.1356 0.058 Uiso 1 1 calc R . . H9C H 0.0645 0.5586 -0.0628 0.058 Uiso 1 1 calc R . . C10 C 0.08259(19) 0.7461(2) -0.06190(18) 0.0450(7) Uani 1 1 d . . . H10A H 0.0640 0.7541 -0.1233 0.067 Uiso 1 1 calc R . . H10B H 0.1087 0.8055 -0.0323 0.067 Uiso 1 1 calc R . . H10C H 0.0216 0.7269 -0.0528 0.067 Uiso 1 1 calc R . . C11 C 0.3616(2) 0.90037(16) -0.13281(15) 0.0327(5) Uani 1 1 d . . . C12 C 0.2671(3) 0.9030(2) -0.21807(18) 0.0605(9) Uani 1 1 d . . . H12A H 0.2701 0.8505 -0.2539 0.091 Uiso 1 1 calc R . . H12B H 0.2662 0.9621 -0.2474 0.091 Uiso 1 1 calc R . . H12C H 0.2043 0.8981 -0.2076 0.091 Uiso 1 1 calc R . . C13 C 0.4582(2) 0.91260(19) -0.1499(2) 0.0495(8) Uani 1 1 d . . . H13A H 0.5194 0.9094 -0.0957 0.074 Uiso 1 1 calc R . . H13B H 0.4560 0.9736 -0.1768 0.074 Uiso 1 1 calc R . . H13C H 0.4614 0.8627 -0.1880 0.074 Uiso 1 1 calc R . . C14 C 0.3551(2) 0.98232(18) -0.0776(2) 0.0443(7) Uani 1 1 d . . . H14A H 0.2897 0.9792 -0.0711 0.066 Uiso 1 1 calc R . . H14B H 0.3588 1.0415 -0.1053 0.066 Uiso 1 1 calc R . . H14C H 0.4127 0.9788 -0.0212 0.066 Uiso 1 1 calc R . . C15 C 0.62940(15) 0.62243(14) 0.08335(12) 0.0168(4) Uani 1 1 d . . . C16 C 0.66468(15) 0.56462(14) 0.15580(12) 0.0173(4) Uani 1 1 d . . . C17 C 0.76487(15) 0.57662(14) 0.22062(13) 0.0191(4) Uani 1 1 d . . . C18 C 0.82580(16) 0.64528(14) 0.20693(13) 0.0208(4) Uani 1 1 d . . . H18A H 0.8934 0.6544 0.2498 0.025 Uiso 1 1 calc R . . C19 C 0.79382(15) 0.70171(14) 0.13398(13) 0.0195(4) Uani 1 1 d . . . C20 C 0.69444(16) 0.68950(14) 0.07219(13) 0.0192(4) Uani 1 1 d . . . H20A H 0.6705 0.7270 0.0220 0.023 Uiso 1 1 calc R . . C21 C 0.80108(16) 0.51650(15) 0.30165(13) 0.0233(4) Uani 1 1 d . . . C22 C 0.72808(18) 0.53138(17) 0.34700(14) 0.0289(5) Uani 1 1 d . . . H22A H 0.7280 0.5977 0.3617 0.043 Uiso 1 1 calc R . . H22B H 0.7517 0.4936 0.3993 0.043 Uiso 1 1 calc R . . H22C H 0.6581 0.5123 0.3088 0.043 Uiso 1 1 calc R . . C23 C 0.90988(18) 0.54280(18) 0.36512(15) 0.0333(6) Uani 1 1 d . . . H23A H 0.9583 0.5344 0.3380 0.050 Uiso 1 1 calc R . . H23B H 0.9303 0.5025 0.4157 0.050 Uiso 1 1 calc R . . H23C H 0.9108 0.6084 0.3823 0.050 Uiso 1 1 calc R . . C24 C 0.80211(18) 0.41216(16) 0.27893(15) 0.0293(5) Uani 1 1 d . . . H24A H 0.7345 0.3946 0.2352 0.044 Uiso 1 1 calc R . . H24B H 0.8174 0.3740 0.3302 0.044 Uiso 1 1 calc R . . H24C H 0.8551 0.4016 0.2569 0.044 Uiso 1 1 calc R . . C25 C 0.86915(16) 0.77344(15) 0.12473(14) 0.0232(5) Uani 1 1 d . . . C26 C 0.96874(18) 0.72365(19) 0.13376(18) 0.0382(6) Uani 1 1 d . . . H26A H 0.9525 0.6747 0.0901 0.057 Uiso 1 1 calc R . . H26B H 1.0012 0.6954 0.1907 0.057 Uiso 1 1 calc R . . H26C H 1.0161 0.7691 0.1262 0.057 Uiso 1 1 calc R . . C27 C 0.89353(18) 0.84796(16) 0.19459(15) 0.0299(5) Uani 1 1 d . . . H27A H 0.9425 0.8934 0.1895 0.045 Uiso 1 1 calc R . . H27B H 0.9239 0.8180 0.2509 0.045 Uiso 1 1 calc R . . H27C H 0.8299 0.8802 0.1881 0.045 Uiso 1 1 calc R . . C28 C 0.82486(18) 0.82266(17) 0.03809(15) 0.0324(5) Uani 1 1 d . . . H28A H 0.8088 0.7761 -0.0076 0.049 Uiso 1 1 calc R . . H28B H 0.8756 0.8673 0.0348 0.049 Uiso 1 1 calc R . . H28C H 0.7618 0.8561 0.0314 0.049 Uiso 1 1 calc R . . C29 C 0.32047(17) 0.38936(16) 0.13114(14) 0.0258(5) Uani 1 1 d . . . H29A H 0.2716 0.4203 0.0823 0.031 Uiso 1 1 calc R . . C30 C 0.28548(19) 0.33695(17) 0.18149(16) 0.0336(6) Uani 1 1 d . . . H30A H 0.2136 0.3315 0.1671 0.040 Uiso 1 1 calc R . . C31 C 0.3557(2) 0.29245(17) 0.25295(16) 0.0347(6) Uani 1 1 d . . . H31A H 0.3331 0.2565 0.2888 0.042 Uiso 1 1 calc R . . C32 C 0.4593(2) 0.30117(17) 0.27135(16) 0.0345(6) Uani 1 1 d . . . H32A H 0.5094 0.2711 0.3200 0.041 Uiso 1 1 calc R . . C33 C 0.48915(18) 0.35439(16) 0.21783(14) 0.0279(5) Uani 1 1 d . . . H33A H 0.5606 0.3601 0.2306 0.033 Uiso 1 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 0.01457(15) 0.01915(16) 0.01641(15) 0.00085(11) 0.00818(11) 0.00000(11) O1 0.0195(7) 0.0250(8) 0.0263(8) 0.0038(6) 0.0136(6) 0.0030(6) O2 0.0178(7) 0.0230(8) 0.0182(7) 0.0028(6) 0.0058(6) -0.0037(6) N1 0.0171(8) 0.0171(8) 0.0170(8) 0.0000(7) 0.0075(7) 0.0012(7) N2 0.0253(9) 0.0209(9) 0.0234(9) -0.0013(7) 0.0147(8) -0.0021(7) C1 0.0193(10) 0.0206(10) 0.0152(9) -0.0014(8) 0.0063(8) 0.0034(8) C2 0.0217(10) 0.0229(11) 0.0175(10) 0.0008(8) 0.0090(8) 0.0044(8) C3 0.0223(11) 0.0311(12) 0.0202(10) 0.0004(9) 0.0099(9) 0.0071(9) C4 0.0285(12) 0.0284(12) 0.0241(11) 0.0029(9) 0.0087(9) 0.0126(9) C5 0.0331(12) 0.0226(11) 0.0180(10) 0.0005(8) 0.0078(9) 0.0052(9) C6 0.0253(11) 0.0223(11) 0.0210(10) -0.0007(8) 0.0097(9) -0.0005(9) C7 0.0214(11) 0.0435(14) 0.0302(12) 0.0058(11) 0.0133(10) 0.0113(10) C8 0.0330(14) 0.0571(17) 0.0369(14) 0.0065(12) 0.0236(12) 0.0162(12) C9 0.0212(12) 0.0539(17) 0.0401(14) 0.0052(12) 0.0120(11) 0.0024(11) C10 0.0259(13) 0.0604(18) 0.0522(17) 0.0136(14) 0.0195(12) 0.0192(12) C11 0.0400(14) 0.0236(12) 0.0315(13) 0.0054(10) 0.0114(11) 0.0041(10) C12 0.079(2) 0.0457(18) 0.0332(15) 0.0181(13) -0.0009(15) -0.0083(16) C13 0.071(2) 0.0296(14) 0.0640(19) 0.0187(13) 0.0439(17) 0.0111(13) C14 0.0465(16) 0.0258(13) 0.0594(18) -0.0019(12) 0.0202(14) 0.0020(12) C15 0.0149(9) 0.0194(10) 0.0176(9) -0.0046(8) 0.0083(8) 0.0003(8) C16 0.0184(10) 0.0173(10) 0.0189(10) -0.0022(8) 0.0105(8) -0.0006(8) C17 0.0194(10) 0.0206(10) 0.0189(10) -0.0019(8) 0.0094(8) 0.0019(8) C18 0.0141(9) 0.0255(11) 0.0226(10) -0.0041(9) 0.0074(8) -0.0003(8) C19 0.0185(10) 0.0204(10) 0.0230(10) -0.0039(8) 0.0119(9) -0.0015(8) C20 0.0223(11) 0.0203(10) 0.0183(10) -0.0013(8) 0.0118(8) -0.0002(8) C21 0.0197(11) 0.0280(11) 0.0202(10) 0.0022(9) 0.0060(8) 0.0008(9) C22 0.0300(12) 0.0386(14) 0.0190(11) 0.0012(9) 0.0108(9) -0.0010(10) C23 0.0242(12) 0.0408(14) 0.0270(12) 0.0075(10) 0.0022(10) -0.0032(10) C24 0.0263(12) 0.0279(12) 0.0319(12) 0.0065(10) 0.0101(10) 0.0048(9) C25 0.0184(10) 0.0262(12) 0.0283(11) -0.0020(9) 0.0129(9) -0.0050(9) C26 0.0262(13) 0.0408(15) 0.0578(17) -0.0004(13) 0.0277(12) -0.0030(11) C27 0.0276(12) 0.0301(13) 0.0328(12) -0.0033(10) 0.0132(10) -0.0090(10) C28 0.0325(13) 0.0366(14) 0.0323(13) 0.0017(11) 0.0175(11) -0.0133(10) C29 0.0246(11) 0.0305(12) 0.0266(11) -0.0001(9) 0.0148(9) -0.0025(9) C30 0.0335(13) 0.0351(13) 0.0430(14) -0.0025(11) 0.0267(12) -0.0081(11) C31 0.0487(15) 0.0295(13) 0.0384(14) 0.0010(11) 0.0304(12) -0.0087(11) C32 0.0438(15) 0.0317(13) 0.0316(13) 0.0089(10) 0.0191(11) 0.0004(11) C33 0.0289(12) 0.0284(12) 0.0283(12) 0.0036(9) 0.0136(10) -0.0014(9) _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 O1 1.8732(14) . ? Fe1 O2 1.8792(14) . ? Fe1 N1 1.9915(16) 3_665 ? Fe1 N2 2.1338(17) . ? Fe1 N1 2.1626(16) . ? O1 C2 1.339(2) . ? O2 C16 1.339(2) . ? N1 C15 1.440(2) . ? N1 C1 1.440(2) . ? N1 Fe1 1.9916(16) 3_665 ? N2 C29 1.339(3) . ? N2 C33 1.342(3) . ? C1 C6 1.395(3) . ? C1 C2 1.410(3) . ? C2 C3 1.414(3) . ? C3 C4 1.381(3) . ? C3 C7 1.541(3) . ? C4 C5 1.395(3) . ? C5 C6 1.389(3) . ? C5 C11 1.530(3) . ? C7 C9 1.532(4) . ? C7 C10 1.537(3) . ? C7 C8 1.538(3) . ? C11 C13 1.524(4) . ? C11 C12 1.529(4) . ? C11 C14 1.530(4) . ? C15 C20 1.396(3) . ? C15 C16 1.401(3) . ? C16 C17 1.414(3) . ? C17 C18 1.389(3) . ? C17 C21 1.531(3) . ? C18 C19 1.397(3) . ? C19 C20 1.387(3) . ? C19 C25 1.534(3) . ? C21 C23 1.530(3) . ? C21 C22 1.541(3) . ? C21 C24 1.541(3) . ? C25 C28 1.526(3) . ? C25 C27 1.531(3) . ? C25 C26 1.533(3) . ? C29 C30 1.377(3) . ? C30 C31 1.379(4) . ? C31 C32 1.379(3) . ? C32 C33 1.382(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O2 131.30(6) . . ? O1 Fe1 N1 112.10(7) . 3_665 ? O2 Fe1 N1 113.63(7) . 3_665 ? O1 Fe1 N2 93.06(7) . . ? O2 Fe1 N2 90.62(7) . . ? N1 Fe1 N2 105.09(7) 3_665 . ? O1 Fe1 N1 81.40(6) . . ? O2 Fe1 N1 81.21(6) . . ? N1 Fe1 N1 91.98(6) 3_665 . ? N2 Fe1 N1 162.89(6) . . ? C2 O1 Fe1 118.63(12) . . ? C16 O2 Fe1 118.52(12) . . ? C15 N1 C1 123.33(16) . . ? C15 N1 Fe1 112.53(12) . 3_665 ? C1 N1 Fe1 112.10(12) . 3_665 ? C15 N1 Fe1 107.31(12) . . ? C1 N1 Fe1 107.33(12) . . ? Fe1 N1 Fe1 88.02(6) 3_665 . ? C29 N2 C33 118.26(19) . . ? C29 N2 Fe1 120.81(15) . . ? C33 N2 Fe1 120.90(15) . . ? C6 C1 C2 120.45(19) . . ? C6 C1 N1 125.00(18) . . ? C2 C1 N1 114.28(17) . . ? O1 C2 C1 118.30(18) . . ? O1 C2 C3 121.86(19) . . ? C1 C2 C3 119.83(19) . . ? C4 C3 C2 117.3(2) . . ? C4 C3 C7 122.73(19) . . ? C2 C3 C7 119.96(19) . . ? C3 C4 C5 124.0(2) . . ? C6 C5 C4 118.0(2) . . ? C6 C5 C11 122.6(2) . . ? C4 C5 C11 119.4(2) . . ? C5 C6 C1 120.4(2) . . ? C9 C7 C10 108.3(2) . . ? C9 C7 C8 110.3(2) . . ? C10 C7 C8 107.3(2) . . ? C9 C7 C3 110.49(19) . . ? C10 C7 C3 111.5(2) . . ? C8 C7 C3 108.88(19) . . ? C13 C11 C12 108.9(2) . . ? C13 C11 C14 108.4(2) . . ? C12 C11 C14 108.7(2) . . ? C13 C11 C5 112.4(2) . . ? C12 C11 C5 109.6(2) . . ? C14 C11 C5 108.7(2) . . ? C20 C15 C16 120.44(18) . . ? C20 C15 N1 124.80(18) . . ? C16 C15 N1 114.55(17) . . ? O2 C16 C15 118.36(17) . . ? O2 C16 C17 121.23(17) . . ? C15 C16 C17 120.40(18) . . ? C18 C17 C16 116.74(18) . . ? C18 C17 C21 123.08(18) . . ? C16 C17 C21 120.17(18) . . ? C17 C18 C19 124.02(19) . . ? C20 C19 C18 117.93(19) . . ? C20 C19 C25 122.72(19) . . ? C18 C19 C25 119.35(18) . . ? C19 C20 C15 120.40(19) . . ? C23 C21 C17 112.05(18) . . ? C23 C21 C22 107.46(18) . . ? C17 C21 C22 109.38(17) . . ? C23 C21 C24 107.81(18) . . ? C17 C21 C24 110.34(17) . . ? C22 C21 C24 109.73(19) . . ? C28 C25 C27 108.14(19) . . ? C28 C25 C26 108.06(19) . . ? C27 C25 C26 109.71(19) . . ? C28 C25 C19 112.24(17) . . ? C27 C25 C19 109.22(17) . . ? C26 C25 C19 109.43(18) . . ? N2 C29 C30 122.3(2) . . ? C29 C30 C31 119.4(2) . . ? C30 C31 C32 118.7(2) . . ? C31 C32 C33 119.0(2) . . ? N2 C33 C32 122.4(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Fe1 O1 C2 71.18(16) . . . . ? N1 Fe1 O1 C2 -87.67(15) 3_665 . . . ? N2 Fe1 O1 C2 164.69(14) . . . . ? N1 Fe1 O1 C2 0.97(14) . . . . ? O1 Fe1 O2 C16 -71.97(16) . . . . ? N1 Fe1 O2 C16 86.63(14) 3_665 . . . ? N2 Fe1 O2 C16 -166.59(14) . . . . ? N1 Fe1 O2 C16 -1.68(14) . . . . ? O1 Fe1 N1 C15 134.94(12) . . . . ? O2 Fe1 N1 C15 0.60(12) . . . . ? N1 Fe1 N1 C15 -113.01(13) 3_665 . . . ? N2 Fe1 N1 C15 62.9(3) . . . . ? O1 Fe1 N1 C1 0.50(12) . . . . ? O2 Fe1 N1 C1 -133.84(12) . . . . ? N1 Fe1 N1 C1 112.55(13) 3_665 . . . ? N2 Fe1 N1 C1 -71.6(3) . . . . ? O1 Fe1 N1 Fe1 -112.05(7) . . . 3_665 ? O2 Fe1 N1 Fe1 113.61(7) . . . 3_665 ? N1 Fe1 N1 Fe1 0.0 3_665 . . 3_665 ? N2 Fe1 N1 Fe1 175.9(2) . . . 3_665 ? O1 Fe1 N2 C29 24.88(17) . . . . ? O2 Fe1 N2 C29 156.31(17) . . . . ? N1 Fe1 N2 C29 -88.98(17) 3_665 . . . ? N1 Fe1 N2 C29 95.3(3) . . . . ? O1 Fe1 N2 C33 -152.89(17) . . . . ? O2 Fe1 N2 C33 -21.47(17) . . . . ? N1 Fe1 N2 C33 93.25(17) 3_665 . . . ? N1 Fe1 N2 C33 -82.5(3) . . . . ? C15 N1 C1 C6 58.9(3) . . . . ? Fe1 N1 C1 C6 -80.8(2) 3_665 . . . ? Fe1 N1 C1 C6 -175.79(17) . . . . ? C15 N1 C1 C2 -127.12(19) . . . . ? Fe1 N1 C1 C2 93.24(17) 3_665 . . . ? Fe1 N1 C1 C2 -1.79(19) . . . . ? Fe1 O1 C2 C1 -2.4(2) . . . . ? Fe1 O1 C2 C3 177.16(15) . . . . ? C6 C1 C2 O1 177.08(18) . . . . ? N1 C1 C2 O1 2.8(3) . . . . ? C6 C1 C2 C3 -2.5(3) . . . . ? N1 C1 C2 C3 -176.79(17) . . . . ? O1 C2 C3 C4 -178.30(19) . . . . ? C1 C2 C3 C4 1.3(3) . . . . ? O1 C2 C3 C7 2.3(3) . . . . ? C1 C2 C3 C7 -178.14(19) . . . . ? C2 C3 C4 C5 1.1(3) . . . . ? C7 C3 C4 C5 -179.5(2) . . . . ? C3 C4 C5 C6 -2.2(3) . . . . ? C3 C4 C5 C11 178.6(2) . . . . ? C4 C5 C6 C1 0.9(3) . . . . ? C11 C5 C6 C1 -179.93(19) . . . . ? C2 C1 C6 C5 1.4(3) . . . . ? N1 C1 C6 C5 175.06(18) . . . . ? C4 C3 C7 C9 118.0(2) . . . . ? C2 C3 C7 C9 -62.6(3) . . . . ? C4 C3 C7 C10 -2.5(3) . . . . ? C2 C3 C7 C10 176.8(2) . . . . ? C4 C3 C7 C8 -120.8(2) . . . . ? C2 C3 C7 C8 58.6(3) . . . . ? C6 C5 C11 C13 9.1(3) . . . . ? C4 C5 C11 C13 -171.7(2) . . . . ? C6 C5 C11 C12 130.4(3) . . . . ? C4 C5 C11 C12 -50.4(3) . . . . ? C6 C5 C11 C14 -110.9(2) . . . . ? C4 C5 C11 C14 68.3(3) . . . . ? C1 N1 C15 C20 -59.4(3) . . . . ? Fe1 N1 C15 C20 80.1(2) 3_665 . . . ? Fe1 N1 C15 C20 175.22(16) . . . . ? C1 N1 C15 C16 125.80(19) . . . . ? Fe1 N1 C15 C16 -94.71(17) 3_665 . . . ? Fe1 N1 C15 C16 0.46(19) . . . . ? Fe1 O2 C16 C15 2.5(2) . . . . ? Fe1 O2 C16 C17 -177.54(14) . . . . ? C20 C15 C16 O2 -176.88(17) . . . . ? N1 C15 C16 O2 -1.9(3) . . . . ? C20 C15 C16 C17 3.2(3) . . . . ? N1 C15 C16 C17 178.21(17) . . . . ? O2 C16 C17 C18 177.93(18) . . . . ? C15 C16 C17 C18 -2.1(3) . . . . ? O2 C16 C17 C21 -2.9(3) . . . . ? C15 C16 C17 C21 176.98(18) . . . . ? C16 C17 C18 C19 -0.1(3) . . . . ? C21 C17 C18 C19 -179.15(19) . . . . ? C17 C18 C19 C20 1.2(3) . . . . ? C17 C18 C19 C25 -178.23(19) . . . . ? C18 C19 C20 C15 -0.2(3) . . . . ? C25 C19 C20 C15 179.25(18) . . . . ? C16 C15 C20 C19 -2.0(3) . . . . ? N1 C15 C20 C19 -176.47(18) . . . . ? C18 C17 C21 C23 1.2(3) . . . . ? C16 C17 C21 C23 -177.82(19) . . . . ? C18 C17 C21 C22 120.3(2) . . . . ? C16 C17 C21 C22 -58.8(2) . . . . ? C18 C17 C21 C24 -118.9(2) . . . . ? C16 C17 C21 C24 62.0(2) . . . . ? C20 C19 C25 C28 -4.5(3) . . . . ? C18 C19 C25 C28 174.94(19) . . . . ? C20 C19 C25 C27 115.4(2) . . . . ? C18 C19 C25 C27 -65.1(2) . . . . ? C20 C19 C25 C26 -124.4(2) . . . . ? C18 C19 C25 C26 55.0(3) . . . . ? C33 N2 C29 C30 -0.2(3) . . . . ? Fe1 N2 C29 C30 -178.02(17) . . . . ? N2 C29 C30 C31 0.6(4) . . . . ? C29 C30 C31 C32 -0.6(4) . . . . ? C30 C31 C32 C33 0.3(4) . . . . ? C29 N2 C33 C32 -0.2(3) . . . . ? Fe1 N2 C33 C32 177.61(18) . . . . ? C31 C32 C33 N2 0.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.708 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.062 _iucr_refine_instructions_details ; TITL afh336 in P2(1)/c CELL 0.71073 14.1943 14.2798 17.1104 90.000 113.9953 90.000 ZERR 2.00 0.0010 0.0010 0.0013 0.000 0.0009 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O FE UNIT 132 180 8 8 4 TEMP -130.000 SIZE 0.079 0.125 0.208 rem Janice Wong 60s sphere ccd2 rem APEX2 2011.4-1, SAINT 7.68a, SADABS 2008/1, SHELXTL 2008/4 CONN 5 FE1 L.S. 12 ACTA 51 CONF FMAP 2 PLAN 10 WGHT 0.065500 1.060200 FVAR 0.12454 FE1 5 0.471373 0.483828 0.070801 11.00000 0.01457 0.01915 = 0.01641 0.00085 0.00818 0.00000 O1 4 0.352833 0.558692 0.033987 11.00000 0.01948 0.02495 = 0.02629 0.00378 0.01360 0.00299 O2 4 0.601228 0.498310 0.161837 11.00000 0.01783 0.02296 = 0.01822 0.00280 0.00583 -0.00367 N1 3 0.527274 0.600683 0.021327 11.00000 0.01706 0.01708 = 0.01698 0.00001 0.00752 0.00117 N2 3 0.420946 0.398223 0.148587 11.00000 0.02535 0.02091 = 0.02345 -0.00128 0.01474 -0.00215 C1 1 0.445314 0.668556 -0.010362 11.00000 0.01931 0.02057 = 0.01519 -0.00140 0.00631 0.00345 C2 1 0.353682 0.640849 -0.003468 11.00000 0.02173 0.02290 = 0.01750 0.00080 0.00900 0.00441 C3 1 0.265714 0.699190 -0.036271 11.00000 0.02230 0.03108 = 0.02016 0.00040 0.00992 0.00714 C4 1 0.273829 0.781315 -0.075743 11.00000 0.02851 0.02841 = 0.02412 0.00294 0.00875 0.01263 AFIX 43 H4A 2 0.215550 0.821573 -0.097122 11.00000 -1.20000 AFIX 0 C5 1 0.362354 0.808763 -0.086138 11.00000 0.03309 0.02263 = 0.01804 0.00049 0.00781 0.00522 C6 1 0.448660 0.751465 -0.052286 11.00000 0.02530 0.02234 = 0.02098 -0.00068 0.00966 -0.00049 AFIX 43 H6A 2 0.510333 0.768827 -0.057710 11.00000 -1.20000 AFIX 0 C7 1 0.166469 0.670550 -0.026402 11.00000 0.02141 0.04348 = 0.03023 0.00577 0.01329 0.01133 C8 1 0.190974 0.659238 0.069282 11.00000 0.03303 0.05712 = 0.03689 0.00655 0.02358 0.01616 AFIX 137 H8A 2 0.128358 0.640558 0.076183 11.00000 -1.50000 H8B 2 0.216126 0.718885 0.098720 11.00000 -1.50000 H8C 2 0.244056 0.611060 0.093927 11.00000 -1.50000 AFIX 0 C9 1 0.123759 0.578845 -0.074078 11.00000 0.02120 0.05394 = 0.04008 0.00516 0.01201 0.00235 AFIX 137 H9A 2 0.177444 0.530586 -0.054265 11.00000 -1.50000 H9B 2 0.102021 0.588688 -0.135648 11.00000 -1.50000 H9C 2 0.064484 0.558582 -0.062829 11.00000 -1.50000 AFIX 0 C10 1 0.082595 0.746103 -0.061896 11.00000 0.02588 0.06036 = 0.05221 0.01360 0.01951 0.01920 AFIX 137 H10A 2 0.064016 0.754144 -0.123274 11.00000 -1.50000 H10B 2 0.108735 0.805470 -0.032264 11.00000 -1.50000 H10C 2 0.021552 0.726871 -0.052782 11.00000 -1.50000 AFIX 0 C11 1 0.361584 0.900371 -0.132813 11.00000 0.03999 0.02362 = 0.03146 0.00542 0.01138 0.00412 C12 1 0.267071 0.902995 -0.218070 11.00000 0.07945 0.04573 = 0.03322 0.01811 -0.00087 -0.00829 AFIX 137 H12A 2 0.270063 0.850480 -0.253864 11.00000 -1.50000 H12B 2 0.266230 0.962113 -0.247436 11.00000 -1.50000 H12C 2 0.204340 0.898073 -0.207559 11.00000 -1.50000 AFIX 0 C13 1 0.458224 0.912598 -0.149862 11.00000 0.07101 0.02958 = 0.06402 0.01866 0.04389 0.01112 AFIX 137 H13A 2 0.519367 0.909389 -0.095679 11.00000 -1.50000 H13B 2 0.456038 0.973571 -0.176836 11.00000 -1.50000 H13C 2 0.461411 0.862698 -0.188033 11.00000 -1.50000 AFIX 0 C14 1 0.355104 0.982319 -0.077641 11.00000 0.04654 0.02582 = 0.05938 -0.00193 0.02025 0.00201 AFIX 137 H14A 2 0.289742 0.979188 -0.071062 11.00000 -1.50000 H14B 2 0.358765 1.041487 -0.105292 11.00000 -1.50000 H14C 2 0.412655 0.978787 -0.021222 11.00000 -1.50000 AFIX 0 C15 1 0.629400 0.622426 0.083349 11.00000 0.01495 0.01943 = 0.01761 -0.00457 0.00833 0.00029 C16 1 0.664680 0.564621 0.155797 11.00000 0.01841 0.01732 = 0.01886 -0.00218 0.01050 -0.00062 C17 1 0.764871 0.576621 0.220617 11.00000 0.01938 0.02062 = 0.01891 -0.00190 0.00939 0.00188 C18 1 0.825798 0.645284 0.206926 11.00000 0.01408 0.02550 = 0.02262 -0.00407 0.00738 -0.00027 AFIX 43 H18A 2 0.893356 0.654447 0.249784 11.00000 -1.20000 AFIX 0 C19 1 0.793821 0.701715 0.133979 11.00000 0.01852 0.02039 = 0.02301 -0.00389 0.01186 -0.00155 C20 1 0.694445 0.689496 0.072191 11.00000 0.02233 0.02026 = 0.01832 -0.00130 0.01175 -0.00018 AFIX 43 H20A 2 0.670513 0.726988 0.021991 11.00000 -1.20000 AFIX 0 C21 1 0.801085 0.516501 0.301655 11.00000 0.01972 0.02801 = 0.02017 0.00217 0.00600 0.00083 C22 1 0.728079 0.531384 0.346998 11.00000 0.03003 0.03859 = 0.01903 0.00120 0.01084 -0.00104 AFIX 137 H22A 2 0.728023 0.597709 0.361694 11.00000 -1.50000 H22B 2 0.751715 0.493608 0.399307 11.00000 -1.50000 H22C 2 0.658072 0.512300 0.308828 11.00000 -1.50000 AFIX 0 C23 1 0.909882 0.542796 0.365121 11.00000 0.02424 0.04079 = 0.02698 0.00749 0.00217 -0.00320 AFIX 137 H23A 2 0.958274 0.534353 0.338022 11.00000 -1.50000 H23B 2 0.930295 0.502499 0.415712 11.00000 -1.50000 H23C 2 0.910760 0.608378 0.382279 11.00000 -1.50000 AFIX 0 C24 1 0.802113 0.412158 0.278927 11.00000 0.02635 0.02789 = 0.03193 0.00651 0.01007 0.00480 AFIX 137 H24A 2 0.734478 0.394586 0.235184 11.00000 -1.50000 H24B 2 0.817435 0.373964 0.330243 11.00000 -1.50000 H24C 2 0.855078 0.401587 0.256904 11.00000 -1.50000 AFIX 0 C25 1 0.869146 0.773438 0.124735 11.00000 0.01837 0.02621 = 0.02828 -0.00202 0.01294 -0.00505 C26 1 0.968741 0.723652 0.133756 11.00000 0.02621 0.04081 = 0.05782 -0.00043 0.02772 -0.00301 AFIX 137 H26A 2 0.952543 0.674669 0.090101 11.00000 -1.50000 H26B 2 1.001249 0.695351 0.190719 11.00000 -1.50000 H26C 2 1.016096 0.769112 0.126217 11.00000 -1.50000 AFIX 0 C27 1 0.893532 0.847961 0.194595 11.00000 0.02756 0.03010 = 0.03279 -0.00333 0.01315 -0.00900 AFIX 137 H27A 2 0.942470 0.893373 0.189459 11.00000 -1.50000 H27B 2 0.923883 0.817958 0.250924 11.00000 -1.50000 H27C 2 0.829850 0.880249 0.188113 11.00000 -1.50000 AFIX 0 C28 1 0.824864 0.822658 0.038086 11.00000 0.03246 0.03661 = 0.03233 0.00174 0.01747 -0.01331 AFIX 137 H28A 2 0.808806 0.776122 -0.007630 11.00000 -1.50000 H28B 2 0.875561 0.867310 0.034806 11.00000 -1.50000 H28C 2 0.761789 0.856147 0.031442 11.00000 -1.50000 AFIX 0 C29 1 0.320474 0.389364 0.131141 11.00000 0.02464 0.03047 = 0.02662 -0.00005 0.01478 -0.00247 AFIX 43 H29A 2 0.271621 0.420305 0.082333 11.00000 -1.20000 AFIX 0 C30 1 0.285481 0.336950 0.181495 11.00000 0.03350 0.03513 = 0.04297 -0.00254 0.02670 -0.00809 AFIX 43 H30A 2 0.213634 0.331514 0.167116 11.00000 -1.20000 AFIX 0 C31 1 0.355679 0.292451 0.252953 11.00000 0.04870 0.02945 = 0.03838 0.00103 0.03036 -0.00870 AFIX 43 H31A 2 0.333109 0.256494 0.288808 11.00000 -1.20000 AFIX 0 C32 1 0.459307 0.301171 0.271348 11.00000 0.04385 0.03170 = 0.03163 0.00888 0.01909 0.00040 AFIX 43 H32A 2 0.509403 0.271074 0.320034 11.00000 -1.20000 AFIX 0 C33 1 0.489147 0.354392 0.217834 11.00000 0.02889 0.02835 = 0.02831 0.00358 0.01360 -0.00138 AFIX 43 H33A 2 0.560573 0.360142 0.230559 11.00000 -1.20000 HKLF 4 REM afh336 in P2(1)/c REM R1 = 0.0413 for 5107 Fo > 4sig(Fo) and 0.0595 for all 6485 data REM 355 parameters refined using 0 restraints END WGHT 0.0655 1.0604 REM Highest difference peak 0.708, deepest hole -0.466, 1-sigma level 0.062 Q1 1 0.4835 0.5446 0.0859 11.00000 0.05 0.71 Q2 1 0.4510 0.4268 0.0382 11.00000 0.05 0.68 Q3 1 0.4908 0.4269 0.0965 11.00000 0.05 0.65 Q4 1 0.4447 0.5302 0.0269 11.00000 0.05 0.59 Q5 1 0.7836 0.5485 0.2597 11.00000 0.05 0.43 Q6 1 0.3568 0.8536 -0.1071 11.00000 0.05 0.40 Q7 1 0.8006 0.4673 0.2897 11.00000 0.05 0.37 Q8 1 0.4617 0.7170 -0.0075 11.00000 0.05 0.34 Q9 1 0.4385 0.6967 -0.0489 11.00000 0.05 0.34 Q10 1 0.6409 0.4886 0.2162 11.00000 0.05 0.32 ; data_afh343 _database_code_depnum_ccdc_archive 'CCDC 916897' #TrackingRef '[ONO]Fe_CIF.cif' _audit_creation_method SHELXTL _chemical_name_systematic ; {[ONOcat]Fe(py)}2 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H58 Fe N5 O2' _chemical_formula_weight 756.81 _chemical_absolute_configuration ad 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 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 14.0101(6) _cell_length_b 15.7187(7) _cell_length_c 19.9340(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.6912(5) _cell_angle_gamma 90.00 _cell_volume 4350.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 88(2) _cell_measurement_reflns_used 9569 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 28.17 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1620 _exptl_absorpt_coefficient_mu 0.387 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9065 _exptl_absorpt_correction_T_max 0.9757 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 88(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 47597 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 26.37 _reflns_number_total 17560 _reflns_number_gt 15850 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+1.0368P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.002(8) _refine_ls_number_reflns 17560 _refine_ls_number_parameters 981 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0426 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0877 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.54164(2) 0.800296(18) 0.588091(15) 0.01320(7) Uani 1 1 d . . . O1 O 0.62383(10) 0.83380(9) 0.52100(7) 0.0148(3) Uani 1 1 d . . . O2 O 0.43309(11) 0.76229(10) 0.63217(7) 0.0154(3) Uani 1 1 d . . . N1 N 0.44635(12) 0.78534(12) 0.50601(9) 0.0140(4) Uani 1 1 d . . . N2 N 0.64518(13) 0.81349(12) 0.67702(9) 0.0181(4) Uani 1 1 d . . . N3 N 0.59651(13) 0.66588(12) 0.58489(9) 0.0162(4) Uani 1 1 d . . . N4 N 0.50094(13) 0.93612(12) 0.60257(9) 0.0162(4) Uani 1 1 d . . . C1 C 0.58089(16) 0.82975(13) 0.45661(11) 0.0144(4) Uani 1 1 d . . . C2 C 0.62993(16) 0.85121(13) 0.40176(11) 0.0148(4) Uani 1 1 d . . . C3 C 0.57871(16) 0.84553(14) 0.33652(11) 0.0173(5) Uani 1 1 d . . . H3A H 0.6111 0.8594 0.2990 0.021 Uiso 1 1 calc R . . C4 C 0.48215(16) 0.82041(14) 0.32402(11) 0.0171(5) Uani 1 1 d . . . C5 C 0.43477(15) 0.79881(15) 0.37891(11) 0.0156(4) Uani 1 1 d . . . H5A H 0.3695 0.7808 0.3711 0.019 Uiso 1 1 calc R . . C6 C 0.48210(15) 0.80335(15) 0.44554(10) 0.0141(4) Uani 1 1 d . . . C7 C 0.73577(16) 0.88069(14) 0.41420(11) 0.0180(5) Uani 1 1 d . . . C8 C 0.77503(17) 0.90121(15) 0.34767(11) 0.0215(5) Uani 1 1 d . . . H8A H 0.7389 0.9490 0.3252 0.032 Uiso 1 1 calc R . . H8B H 0.7679 0.8512 0.3180 0.032 Uiso 1 1 calc R . . H8C H 0.8433 0.9165 0.3574 0.032 Uiso 1 1 calc R . . C9 C 0.79993(16) 0.81037(17) 0.45009(12) 0.0244(5) Uani 1 1 d . . . H9A H 0.7827 0.8014 0.4956 0.037 Uiso 1 1 calc R . . H9B H 0.8676 0.8276 0.4534 0.037 Uiso 1 1 calc R . . H9C H 0.7903 0.7574 0.4241 0.037 Uiso 1 1 calc R . . C10 C 0.74575(17) 0.96180(15) 0.45754(12) 0.0228(5) Uani 1 1 d . . . H10A H 0.7271 0.9496 0.5022 0.034 Uiso 1 1 calc R . . H10B H 0.7037 1.0062 0.4353 0.034 Uiso 1 1 calc R . . H10C H 0.8128 0.9814 0.4627 0.034 Uiso 1 1 calc R . . C11 C 0.42943(17) 0.81921(16) 0.25103(11) 0.0230(5) Uani 1 1 d . . . C12 C 0.4307(2) 0.90884(19) 0.22102(14) 0.0414(7) Uani 1 1 d . . . H12A H 0.4031 0.9492 0.2506 0.062 Uiso 1 1 calc R . . H12B H 0.3925 0.9095 0.1761 0.062 Uiso 1 1 calc R . . H12C H 0.4972 0.9252 0.2171 0.062 Uiso 1 1 calc R . . C13 C 0.4789(2) 0.7576(2) 0.20694(13) 0.0370(7) Uani 1 1 d . . . H13A H 0.4825 0.7009 0.2277 0.055 Uiso 1 1 calc R . . H13B H 0.5441 0.7780 0.2032 0.055 Uiso 1 1 calc R . . H13C H 0.4417 0.7544 0.1617 0.055 Uiso 1 1 calc R . . C14 C 0.32455(18) 0.7903(2) 0.24804(13) 0.0379(7) Uani 1 1 d . . . H14A H 0.2898 0.8298 0.2741 0.057 Uiso 1 1 calc R . . H14B H 0.3226 0.7331 0.2672 0.057 Uiso 1 1 calc R . . H14C H 0.2941 0.7896 0.2008 0.057 Uiso 1 1 calc R . . C15 C 0.35312(16) 0.74481(14) 0.58983(11) 0.0150(5) Uani 1 1 d . . . C16 C 0.26950(16) 0.71386(14) 0.61290(11) 0.0168(5) Uani 1 1 d . . . C17 C 0.18896(16) 0.69765(14) 0.56493(12) 0.0194(5) Uani 1 1 d . . . H17A H 0.1322 0.6763 0.5802 0.023 Uiso 1 1 calc R . . C18 C 0.18849(16) 0.71142(15) 0.49591(12) 0.0195(5) Uani 1 1 d . . . C19 C 0.27252(16) 0.74180(15) 0.47331(11) 0.0184(5) Uani 1 1 d . . . H19A H 0.2730 0.7518 0.4263 0.022 Uiso 1 1 calc R . . C20 C 0.35599(15) 0.75775(14) 0.51857(11) 0.0152(4) Uani 1 1 d . . . C21 C 0.26714(16) 0.69882(14) 0.68928(11) 0.0189(5) Uani 1 1 d . . . C22 C 0.16977(18) 0.66232(16) 0.70299(13) 0.0251(5) Uani 1 1 d . . . H22A H 0.1182 0.7021 0.6863 0.038 Uiso 1 1 calc R . . H22B H 0.1706 0.6539 0.7518 0.038 Uiso 1 1 calc R . . H22C H 0.1585 0.6077 0.6796 0.038 Uiso 1 1 calc R . . C23 C 0.28254(18) 0.78235(15) 0.72885(12) 0.0248(5) Uani 1 1 d . . . H23A H 0.2326 0.8233 0.7112 0.037 Uiso 1 1 calc R . . H23B H 0.3461 0.8056 0.7238 0.037 Uiso 1 1 calc R . . H23C H 0.2788 0.7716 0.7769 0.037 Uiso 1 1 calc R . . C24 C 0.34626(17) 0.63493(15) 0.71752(12) 0.0228(5) Uani 1 1 d . . . H24A H 0.3389 0.5823 0.6910 0.034 Uiso 1 1 calc R . . H24B H 0.3403 0.6224 0.7649 0.034 Uiso 1 1 calc R . . H24C H 0.4098 0.6596 0.7145 0.034 Uiso 1 1 calc R . . C25 C 0.09862(17) 0.69574(17) 0.44376(13) 0.0260(5) Uani 1 1 d . . . C26 C 0.01454(18) 0.65883(19) 0.47539(14) 0.0331(6) Uani 1 1 d . . . H26A H 0.0325 0.6028 0.4947 0.050 Uiso 1 1 calc R . . H26B H -0.0415 0.6530 0.4406 0.050 Uiso 1 1 calc R . . H26C H -0.0014 0.6969 0.5112 0.050 Uiso 1 1 calc R . . C27 C 0.12281(19) 0.6347(2) 0.38889(14) 0.0367(7) Uani 1 1 d . . . H27A H 0.1464 0.5809 0.4097 0.055 Uiso 1 1 calc R . . H27B H 0.1727 0.6600 0.3651 0.055 Uiso 1 1 calc R . . H27C H 0.0649 0.6241 0.3566 0.055 Uiso 1 1 calc R . . C28 C 0.06572(18) 0.78247(19) 0.41107(14) 0.0347(6) Uani 1 1 d . . . H28A H 0.0533 0.8226 0.4465 0.052 Uiso 1 1 calc R . . H28B H 0.0067 0.7743 0.3794 0.052 Uiso 1 1 calc R . . H28C H 0.1164 0.8052 0.3867 0.052 Uiso 1 1 calc R . . C29 C 0.73771(17) 0.83066(15) 0.67270(12) 0.0224(5) Uani 1 1 d . . . H29A H 0.7562 0.8405 0.6292 0.027 Uiso 1 1 calc R . . C30 C 0.80746(19) 0.83479(16) 0.72833(14) 0.0293(6) Uani 1 1 d . . . H30A H 0.8725 0.8474 0.7234 0.035 Uiso 1 1 calc R . . C31 C 0.7807(2) 0.82021(16) 0.79130(14) 0.0330(6) Uani 1 1 d . . . H31A H 0.8273 0.8218 0.8306 0.040 Uiso 1 1 calc R . . C32 C 0.68488(19) 0.80324(18) 0.79678(13) 0.0319(6) Uani 1 1 d . . . H32A H 0.6649 0.7940 0.8399 0.038 Uiso 1 1 calc R . . C33 C 0.61884(17) 0.79990(16) 0.73878(11) 0.0239(5) Uani 1 1 d . . . H33A H 0.5533 0.7877 0.7425 0.029 Uiso 1 1 calc R . . C34 C 0.67679(17) 0.64780(15) 0.55839(12) 0.0207(5) Uani 1 1 d . . . H34A H 0.7151 0.6936 0.5461 0.025 Uiso 1 1 calc R . . C35 C 0.70708(17) 0.56520(17) 0.54797(12) 0.0238(5) Uani 1 1 d . . . H35A H 0.7653 0.5551 0.5297 0.029 Uiso 1 1 calc R . . C36 C 0.65118(17) 0.49810(15) 0.56467(12) 0.0216(5) Uani 1 1 d . . . H36A H 0.6694 0.4410 0.5573 0.026 Uiso 1 1 calc R . . C37 C 0.56797(18) 0.51591(16) 0.59243(12) 0.0216(5) Uani 1 1 d . . . H37A H 0.5284 0.4712 0.6051 0.026 Uiso 1 1 calc R . . C38 C 0.54332(17) 0.60007(15) 0.60140(12) 0.0182(5) Uani 1 1 d . . . H38A H 0.4859 0.6118 0.6202 0.022 Uiso 1 1 calc R . . C39 C 0.54665(16) 0.99997(15) 0.57480(12) 0.0187(5) Uani 1 1 d . . . H39A H 0.5994 0.9865 0.5513 0.022 Uiso 1 1 calc R . . C40 C 0.51990(17) 1.08442(15) 0.57914(12) 0.0204(5) Uani 1 1 d . . . H40A H 0.5543 1.1277 0.5594 0.024 Uiso 1 1 calc R . . C41 C 0.44271(17) 1.10519(15) 0.61248(11) 0.0198(5) Uani 1 1 d . . . H41A H 0.4232 1.1627 0.6162 0.024 Uiso 1 1 calc R . . C42 C 0.39460(16) 1.03971(14) 0.64040(11) 0.0209(5) Uani 1 1 d . . . H42A H 0.3409 1.0516 0.6633 0.025 Uiso 1 1 calc R . . C43 C 0.42581(16) 0.95680(14) 0.63449(12) 0.0196(5) Uani 1 1 d . . . H43A H 0.3924 0.9125 0.6539 0.024 Uiso 1 1 calc R . . Fe2 Fe 0.93798(2) 0.056239(18) 0.915347(15) 0.01392(7) Uani 1 1 d . . . O3 O 0.87573(11) 0.02398(10) 0.99371(7) 0.0168(3) Uani 1 1 d . . . O4 O 1.03280(11) 0.09403(10) 0.85863(7) 0.0164(3) Uani 1 1 d . . . N5 N 1.04948(13) 0.07190(12) 0.98798(9) 0.0148(4) Uani 1 1 d . . . N6 N 0.80878(13) 0.03738(12) 0.84369(9) 0.0181(4) Uani 1 1 d . . . N7 N 0.97612(13) -0.07943(12) 0.89613(9) 0.0164(4) Uani 1 1 d . . . N8 N 0.88148(13) 0.19021(12) 0.91892(9) 0.0169(4) Uani 1 1 d . . . C44 C 0.93205(16) 0.02781(14) 1.05330(11) 0.0155(5) Uani 1 1 d . . . C45 C 0.89824(16) 0.00583(14) 1.11454(11) 0.0165(5) Uani 1 1 d . . . C46 C 0.96214(16) 0.01359(14) 1.17413(11) 0.0171(5) Uani 1 1 d . . . H46A H 0.9398 -0.0007 1.2156 0.021 Uiso 1 1 calc R . . C47 C 1.05741(15) 0.04132(14) 1.17612(11) 0.0157(4) Uani 1 1 d . . . C48 C 1.09032(15) 0.06174(16) 1.11522(11) 0.0168(4) Uani 1 1 d . . . H48A H 1.1548 0.0808 1.1157 0.020 Uiso 1 1 calc R . . C49 C 1.02993(15) 0.05477(16) 1.05275(11) 0.0159(4) Uani 1 1 d . . . C50 C 0.79385(17) -0.02569(15) 1.11428(12) 0.0209(5) Uani 1 1 d . . . C51 C 0.77340(17) -0.04762(15) 1.18584(12) 0.0227(5) Uani 1 1 d . . . H51A H 0.8179 -0.0921 1.2049 0.034 Uiso 1 1 calc R . . H51B H 0.7070 -0.0680 1.1840 0.034 Uiso 1 1 calc R . . H51C H 0.7822 0.0033 1.2144 0.034 Uiso 1 1 calc R . . C52 C 0.77651(19) -0.10645(17) 1.07095(12) 0.0289(6) Uani 1 1 d . . . H52A H 0.8231 -0.1503 1.0884 0.043 Uiso 1 1 calc R . . H52B H 0.7844 -0.0933 1.0240 0.043 Uiso 1 1 calc R . . H52C H 0.7110 -0.1273 1.0728 0.043 Uiso 1 1 calc R . . C53 C 0.72165(17) 0.04422(18) 1.08654(12) 0.0289(6) Uani 1 1 d . . . H53A H 0.6559 0.0248 1.0894 0.043 Uiso 1 1 calc R . . H53B H 0.7288 0.0560 1.0392 0.043 Uiso 1 1 calc R . . H53C H 0.7345 0.0962 1.1134 0.043 Uiso 1 1 calc R . . C54 C 1.12253(16) 0.04689(16) 1.24446(11) 0.0192(5) Uani 1 1 d . . . C55 C 1.1257(2) -0.04031(17) 1.27975(13) 0.0349(6) Uani 1 1 d . . . H55A H 1.1674 -0.0369 1.3233 0.052 Uiso 1 1 calc R . . H55B H 1.1513 -0.0830 1.2511 0.052 Uiso 1 1 calc R . . H55C H 1.0605 -0.0566 1.2874 0.052 Uiso 1 1 calc R . . C56 C 1.08231(18) 0.11251(17) 1.29003(12) 0.0281(6) Uani 1 1 d . . . H56A H 1.1248 0.1163 1.3332 0.042 Uiso 1 1 calc R . . H56B H 1.0178 0.0950 1.2984 0.042 Uiso 1 1 calc R . . H56C H 1.0786 0.1682 1.2677 0.042 Uiso 1 1 calc R . . C57 C 1.22572(17) 0.0727(2) 1.23657(12) 0.0335(7) Uani 1 1 d . . . H57A H 1.2645 0.0751 1.2812 0.050 Uiso 1 1 calc R . . H57B H 1.2253 0.1288 1.2151 0.050 Uiso 1 1 calc R . . H57C H 1.2535 0.0308 1.2083 0.050 Uiso 1 1 calc R . . C58 C 1.12049(16) 0.10787(14) 0.89200(11) 0.0147(4) Uani 1 1 d . . . C59 C 1.19867(16) 0.13535(14) 0.85877(11) 0.0164(5) Uani 1 1 d . . . C60 C 1.28745(17) 0.14590(16) 0.89734(12) 0.0221(5) Uani 1 1 d . . . H60A H 1.3398 0.1646 0.8753 0.027 Uiso 1 1 calc R . . C61 C 1.30468(17) 0.13049(17) 0.96751(12) 0.0249(5) Uani 1 1 d . . . C62 C 1.22692(17) 0.10571(16) 0.99950(12) 0.0224(5) Uani 1 1 d . . . H62A H 1.2367 0.0955 1.0469 0.027 Uiso 1 1 calc R . . C63 C 1.13458(16) 0.09539(14) 0.96391(11) 0.0160(5) Uani 1 1 d . . . C64 C 1.18310(16) 0.15138(14) 0.78168(11) 0.0171(5) Uani 1 1 d . . . C65 C 1.27502(17) 0.18550(15) 0.75737(12) 0.0218(5) Uani 1 1 d . . . H65A H 1.2642 0.1927 0.7081 0.033 Uiso 1 1 calc R . . H65B H 1.3278 0.1452 0.7696 0.033 Uiso 1 1 calc R . . H65C H 1.2918 0.2405 0.7789 0.033 Uiso 1 1 calc R . . C66 C 1.15487(17) 0.06891(15) 0.74284(11) 0.0233(5) Uani 1 1 d . . . H66A H 1.1475 0.0802 0.6941 0.035 Uiso 1 1 calc R . . H66B H 1.0938 0.0478 0.7553 0.035 Uiso 1 1 calc R . . H66C H 1.2052 0.0261 0.7543 0.035 Uiso 1 1 calc R . . C67 C 1.10363(16) 0.21797(15) 0.76324(12) 0.0206(5) Uani 1 1 d . . . H67A H 1.1013 0.2337 0.7155 0.031 Uiso 1 1 calc R . . H67B H 1.1175 0.2686 0.7916 0.031 Uiso 1 1 calc R . . H67C H 1.0414 0.1941 0.7709 0.031 Uiso 1 1 calc R . . C68 C 1.40637(19) 0.1445(2) 1.00641(13) 0.0381(7) Uani 1 1 d . . . C69 C 1.4295(3) 0.2438(2) 1.0078(2) 0.0620(10) Uani 1 1 d . . . H69A H 1.4944 0.2534 1.0316 0.093 Uiso 1 1 calc R . . H69B H 1.3825 0.2739 1.0313 0.093 Uiso 1 1 calc R . . H69C H 1.4257 0.2651 0.9613 0.093 Uiso 1 1 calc R . . C70 C 1.4151(2) 0.1166(3) 1.07844(15) 0.0492(9) Uani 1 1 d . . . H70A H 1.4000 0.0558 1.0803 0.074 Uiso 1 1 calc R . . H70B H 1.3701 0.1491 1.1020 0.074 Uiso 1 1 calc R . . H70C H 1.4811 0.1265 1.1003 0.074 Uiso 1 1 calc R . . C71 C 1.4830(2) 0.1059(3) 0.96974(16) 0.0588(11) Uani 1 1 d . . . H71A H 1.4771 0.0438 0.9699 0.088 Uiso 1 1 calc R . . H71B H 1.5467 0.1224 0.9925 0.088 Uiso 1 1 calc R . . H71C H 1.4751 0.1265 0.9229 0.088 Uiso 1 1 calc R . . C72 C 0.80589(17) 0.05112(16) 0.77707(11) 0.0235(5) Uani 1 1 d . . . H72A H 0.8639 0.0651 0.7598 0.028 Uiso 1 1 calc R . . C73 C 0.72151(18) 0.04567(18) 0.73257(13) 0.0310(6) Uani 1 1 d . . . H73A H 0.7219 0.0547 0.6855 0.037 Uiso 1 1 calc R . . C74 C 0.6367(2) 0.02694(16) 0.75757(14) 0.0331(6) Uani 1 1 d . . . H74A H 0.5777 0.0239 0.7280 0.040 Uiso 1 1 calc R . . C75 C 0.63877(18) 0.01281(17) 0.82583(14) 0.0311(6) Uani 1 1 d . . . H75A H 0.5812 -0.0002 0.8441 0.037 Uiso 1 1 calc R . . C76 C 0.72556(17) 0.01777(16) 0.86738(13) 0.0259(5) Uani 1 1 d . . . H76A H 0.7269 0.0070 0.9144 0.031 Uiso 1 1 calc R . . C77 C 1.01722(17) -0.10141(15) 0.84185(12) 0.0227(5) Uani 1 1 d . . . H77A H 1.0277 -0.0584 0.8102 0.027 Uiso 1 1 calc R . . C78 C 1.04532(17) -0.18380(15) 0.82947(12) 0.0246(5) Uani 1 1 d . . . H78A H 1.0741 -0.1968 0.7902 0.029 Uiso 1 1 calc R . . C79 C 1.03071(16) -0.24706(15) 0.87557(12) 0.0216(5) Uani 1 1 d . . . H79A H 1.0493 -0.3041 0.8685 0.026 Uiso 1 1 calc R . . C80 C 0.98859(17) -0.22537(15) 0.93193(12) 0.0213(5) Uani 1 1 d . . . H80A H 0.9776 -0.2673 0.9644 0.026 Uiso 1 1 calc R . . C81 C 0.96265(17) -0.14127(15) 0.94036(12) 0.0193(5) Uani 1 1 d . . . H81A H 0.9339 -0.1267 0.9794 0.023 Uiso 1 1 calc R . . C82 C 0.80407(17) 0.20822(16) 0.94912(12) 0.0224(5) Uani 1 1 d . . . H82A H 0.7700 0.1626 0.9662 0.027 Uiso 1 1 calc R . . C83 C 0.77179(18) 0.28955(16) 0.95653(13) 0.0264(5) Uani 1 1 d . . . H83A H 0.7162 0.2995 0.9780 0.032 Uiso 1 1 calc R . . C84 C 0.82067(18) 0.35691(17) 0.93261(12) 0.0259(5) Uani 1 1 d . . . H84A H 0.7997 0.4138 0.9375 0.031 Uiso 1 1 calc R . . C85 C 0.90098(18) 0.33966(15) 0.90137(12) 0.0218(5) Uani 1 1 d . . . H85A H 0.9364 0.3846 0.8845 0.026 Uiso 1 1 calc R . . C86 C 0.92887(17) 0.25567(16) 0.89515(12) 0.0202(5) Uani 1 1 d . . . H86A H 0.9836 0.2439 0.8732 0.024 Uiso 1 1 calc R . . C87 C 0.1438(2) 0.92366(19) 0.57515(16) 0.0414(7) Uani 1 1 d . . . H87A H 0.1861 0.9664 0.5995 0.062 Uiso 1 1 calc R . . H87B H 0.1132 0.9476 0.5322 0.062 Uiso 1 1 calc R . . H87C H 0.1819 0.8737 0.5661 0.062 Uiso 1 1 calc R . . C88 C 0.0702(3) 0.8989(2) 0.61610(17) 0.0475(8) Uani 1 1 d . . . N9 N 0.0156(3) 0.8805(2) 0.65051(18) 0.0778(10) Uani 1 1 d . . . C89 C 0.2876(2) -0.0789(2) 0.89498(18) 0.0503(9) Uani 1 1 d . . . H89A H 0.2477 -0.0287 0.9003 0.075 Uiso 1 1 calc R . . H89B H 0.3220 -0.0953 0.9391 0.075 Uiso 1 1 calc R . . H89C H 0.2464 -0.1260 0.8764 0.075 Uiso 1 1 calc R . . C90 C 0.3562(2) -0.0591(2) 0.84947(16) 0.0414(7) Uani 1 1 d . . . N10 N 0.4076(2) -0.0411(2) 0.81128(18) 0.0735(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01480(15) 0.01199(16) 0.01309(15) 0.00057(12) 0.00293(11) -0.00171(12) O1 0.0161(8) 0.0146(8) 0.0138(7) 0.0010(6) 0.0027(6) -0.0012(6) O2 0.0190(8) 0.0135(8) 0.0144(8) 0.0004(6) 0.0048(6) -0.0033(6) N1 0.0148(9) 0.0113(10) 0.0162(9) -0.0004(7) 0.0036(7) -0.0001(7) N2 0.0217(10) 0.0122(9) 0.0198(10) -0.0017(8) -0.0001(7) 0.0001(8) N3 0.0189(9) 0.0153(10) 0.0140(9) 0.0003(7) 0.0007(7) -0.0023(7) N4 0.0180(9) 0.0154(10) 0.0149(9) -0.0020(8) 0.0013(7) -0.0019(8) C1 0.0196(11) 0.0090(10) 0.0150(11) 0.0005(8) 0.0038(9) 0.0037(8) C2 0.0192(11) 0.0095(11) 0.0164(11) 0.0021(8) 0.0052(9) 0.0033(8) C3 0.0224(12) 0.0152(11) 0.0157(11) 0.0028(9) 0.0083(9) 0.0054(9) C4 0.0217(12) 0.0148(12) 0.0149(11) -0.0008(8) 0.0025(9) 0.0065(9) C5 0.0157(10) 0.0123(11) 0.0187(11) -0.0020(10) 0.0020(8) 0.0008(9) C6 0.0201(11) 0.0084(10) 0.0143(10) 0.0022(9) 0.0048(8) 0.0044(9) C7 0.0189(11) 0.0179(12) 0.0186(12) 0.0029(9) 0.0075(9) 0.0002(9) C8 0.0260(12) 0.0197(12) 0.0210(12) 0.0006(9) 0.0109(10) -0.0008(10) C9 0.0189(11) 0.0287(13) 0.0268(12) 0.0057(11) 0.0071(9) 0.0021(10) C10 0.0252(13) 0.0217(13) 0.0234(13) -0.0025(10) 0.0100(10) -0.0070(10) C11 0.0220(12) 0.0316(14) 0.0155(11) 0.0014(10) 0.0026(9) 0.0077(10) C12 0.0528(19) 0.0387(17) 0.0301(15) 0.0130(13) -0.0034(13) 0.0101(14) C13 0.0365(16) 0.0508(18) 0.0225(14) -0.0129(12) -0.0001(12) 0.0125(13) C14 0.0216(13) 0.072(2) 0.0185(13) 0.0008(14) -0.0022(10) 0.0067(14) C15 0.0156(11) 0.0101(11) 0.0195(12) -0.0027(8) 0.0032(9) 0.0001(8) C16 0.0208(12) 0.0123(11) 0.0187(12) -0.0004(9) 0.0075(9) 0.0015(9) C17 0.0165(11) 0.0165(11) 0.0267(13) -0.0014(9) 0.0086(9) -0.0016(9) C18 0.0147(11) 0.0192(12) 0.0245(12) -0.0049(9) 0.0027(9) -0.0006(9) C19 0.0177(11) 0.0217(12) 0.0157(11) -0.0016(9) 0.0021(9) 0.0020(9) C20 0.0161(11) 0.0111(11) 0.0192(11) -0.0015(9) 0.0049(9) 0.0005(8) C21 0.0215(12) 0.0177(11) 0.0189(12) 0.0000(9) 0.0074(9) -0.0050(9) C22 0.0263(13) 0.0246(13) 0.0271(13) 0.0005(10) 0.0132(10) -0.0065(10) C23 0.0333(13) 0.0242(13) 0.0188(12) -0.0030(9) 0.0108(10) -0.0045(10) C24 0.0260(13) 0.0249(13) 0.0187(12) 0.0040(10) 0.0074(10) -0.0048(10) C25 0.0170(12) 0.0330(14) 0.0273(13) -0.0001(11) 0.0000(10) -0.0011(10) C26 0.0178(12) 0.0442(17) 0.0365(15) -0.0006(12) 0.0001(11) -0.0056(11) C27 0.0241(14) 0.0522(18) 0.0320(15) -0.0157(13) -0.0032(11) -0.0056(12) C28 0.0228(13) 0.0471(18) 0.0324(15) 0.0030(12) -0.0032(11) -0.0023(12) C29 0.0213(12) 0.0184(12) 0.0272(13) -0.0034(10) 0.0019(10) -0.0027(9) C30 0.0269(14) 0.0226(13) 0.0359(15) -0.0014(11) -0.0053(11) -0.0004(10) C31 0.0383(15) 0.0226(14) 0.0326(15) -0.0002(11) -0.0160(12) 0.0001(11) C32 0.0428(15) 0.0301(14) 0.0213(13) 0.0051(11) -0.0012(11) -0.0048(13) C33 0.0294(13) 0.0229(12) 0.0184(11) 0.0000(10) -0.0004(9) -0.0043(11) C34 0.0233(12) 0.0169(12) 0.0223(12) 0.0003(10) 0.0044(10) -0.0016(9) C35 0.0210(11) 0.0223(14) 0.0290(13) 0.0009(11) 0.0073(10) 0.0037(10) C36 0.0289(13) 0.0106(11) 0.0250(13) -0.0013(9) 0.0024(10) 0.0018(9) C37 0.0250(13) 0.0168(12) 0.0230(13) 0.0011(9) 0.0034(10) -0.0052(10) C38 0.0194(12) 0.0151(12) 0.0206(12) -0.0004(9) 0.0041(9) -0.0022(9) C39 0.0201(12) 0.0200(13) 0.0172(12) 0.0000(9) 0.0067(9) -0.0033(9) C40 0.0264(13) 0.0149(12) 0.0202(12) 0.0032(9) 0.0043(10) -0.0038(9) C41 0.0245(12) 0.0156(12) 0.0188(12) -0.0002(9) 0.0009(9) 0.0008(9) C42 0.0210(11) 0.0189(12) 0.0238(12) -0.0033(9) 0.0071(9) -0.0005(9) C43 0.0207(12) 0.0194(12) 0.0195(12) 0.0009(9) 0.0049(9) -0.0037(9) Fe2 0.01642(15) 0.01277(16) 0.01276(16) 0.00063(12) 0.00270(12) -0.00037(13) O3 0.0188(8) 0.0168(8) 0.0153(8) 0.0019(6) 0.0038(6) 0.0005(6) O4 0.0170(8) 0.0172(8) 0.0148(8) 0.0009(6) 0.0017(6) -0.0016(6) N5 0.0168(9) 0.0127(10) 0.0149(9) 0.0012(7) 0.0025(7) 0.0007(7) N6 0.0187(9) 0.0135(10) 0.0217(10) -0.0028(8) 0.0014(8) 0.0010(7) N7 0.0166(9) 0.0151(10) 0.0171(10) 0.0019(7) 0.0007(7) -0.0011(7) N8 0.0199(10) 0.0154(10) 0.0152(9) 0.0007(8) 0.0015(7) -0.0012(7) C44 0.0200(11) 0.0133(11) 0.0130(11) 0.0004(8) 0.0020(9) 0.0038(8) C45 0.0213(12) 0.0113(11) 0.0183(11) 0.0010(9) 0.0081(9) 0.0038(9) C46 0.0236(12) 0.0134(11) 0.0150(11) 0.0027(9) 0.0051(9) 0.0058(9) C47 0.0197(11) 0.0129(11) 0.0145(10) -0.0003(8) 0.0027(8) 0.0069(8) C48 0.0167(11) 0.0145(11) 0.0193(11) -0.0002(10) 0.0030(8) 0.0050(10) C49 0.0229(11) 0.0101(11) 0.0156(11) 0.0003(10) 0.0056(9) 0.0038(10) C50 0.0244(12) 0.0210(12) 0.0185(12) 0.0045(9) 0.0072(10) 0.0023(10) C51 0.0236(13) 0.0235(13) 0.0228(13) 0.0042(10) 0.0099(10) 0.0008(10) C52 0.0346(14) 0.0310(14) 0.0224(13) 0.0020(11) 0.0084(11) -0.0112(11) C53 0.0212(12) 0.0408(16) 0.0260(13) 0.0125(12) 0.0077(10) 0.0080(11) C54 0.0226(11) 0.0201(12) 0.0149(11) 0.0005(9) 0.0028(9) 0.0065(10) C55 0.0499(18) 0.0289(15) 0.0231(14) 0.0061(11) -0.0059(12) 0.0084(12) C56 0.0269(13) 0.0360(15) 0.0201(12) -0.0077(11) -0.0014(10) 0.0083(11) C57 0.0223(13) 0.061(2) 0.0165(12) 0.0012(12) 0.0014(10) 0.0064(12) C58 0.0169(11) 0.0102(11) 0.0167(11) -0.0008(8) 0.0016(9) 0.0041(8) C59 0.0205(11) 0.0156(11) 0.0136(11) -0.0005(9) 0.0042(9) 0.0014(9) C60 0.0174(12) 0.0296(14) 0.0205(12) 0.0013(10) 0.0067(9) 0.0005(10) C61 0.0190(12) 0.0351(15) 0.0205(12) 0.0026(11) 0.0026(10) 0.0004(10) C62 0.0214(12) 0.0302(14) 0.0152(12) 0.0017(10) 0.0010(9) 0.0033(10) C63 0.0185(11) 0.0127(11) 0.0173(11) 0.0006(9) 0.0038(9) 0.0019(8) C64 0.0183(11) 0.0197(12) 0.0135(11) 0.0005(9) 0.0028(9) -0.0029(9) C65 0.0220(12) 0.0246(13) 0.0199(12) 0.0035(9) 0.0067(9) -0.0018(9) C66 0.0312(13) 0.0200(13) 0.0197(12) -0.0007(9) 0.0073(10) -0.0044(10) C67 0.0214(12) 0.0210(12) 0.0195(12) 0.0032(9) 0.0026(9) 0.0000(9) C68 0.0207(13) 0.071(2) 0.0219(13) 0.0019(13) 0.0006(11) 0.0019(13) C69 0.046(2) 0.063(2) 0.069(2) 0.0073(19) -0.0189(18) -0.0153(17) C70 0.0234(15) 0.085(3) 0.0365(17) -0.0021(17) -0.0040(12) -0.0056(15) C71 0.0214(15) 0.120(3) 0.0347(17) -0.0023(18) 0.0014(13) 0.0141(17) C72 0.0265(12) 0.0224(12) 0.0209(12) 0.0028(10) 0.0007(9) -0.0029(11) C73 0.0359(14) 0.0270(14) 0.0266(13) 0.0036(11) -0.0083(11) -0.0054(12) C74 0.0293(14) 0.0252(14) 0.0402(16) -0.0043(11) -0.0123(12) 0.0008(11) C75 0.0194(13) 0.0319(15) 0.0414(16) -0.0109(12) 0.0016(11) -0.0033(11) C76 0.0249(13) 0.0261(13) 0.0270(13) -0.0042(10) 0.0046(10) -0.0020(10) C77 0.0260(13) 0.0175(12) 0.0260(13) 0.0040(10) 0.0085(10) -0.0016(10) C78 0.0286(13) 0.0204(13) 0.0269(13) -0.0032(10) 0.0120(10) -0.0009(10) C79 0.0192(12) 0.0149(12) 0.0297(13) -0.0012(10) -0.0007(10) 0.0008(9) C80 0.0283(13) 0.0152(12) 0.0191(12) 0.0035(9) -0.0020(10) -0.0027(9) C81 0.0248(12) 0.0165(12) 0.0162(11) -0.0005(9) 0.0016(9) -0.0014(9) C82 0.0245(12) 0.0203(13) 0.0236(13) 0.0006(10) 0.0080(10) -0.0037(10) C83 0.0282(13) 0.0220(14) 0.0311(13) -0.0011(11) 0.0115(10) 0.0024(10) C84 0.0284(13) 0.0211(13) 0.0276(13) -0.0028(11) 0.0018(10) 0.0049(10) C85 0.0272(13) 0.0164(12) 0.0210(12) 0.0007(9) 0.0003(10) -0.0027(10) C86 0.0209(12) 0.0215(13) 0.0185(12) 0.0019(10) 0.0034(9) -0.0016(10) C87 0.0492(18) 0.0295(16) 0.0473(18) -0.0025(13) 0.0128(15) -0.0024(13) C88 0.057(2) 0.0421(18) 0.0444(18) 0.0033(15) 0.0086(16) 0.0009(16) N9 0.072(2) 0.086(3) 0.081(2) 0.023(2) 0.031(2) -0.003(2) C89 0.060(2) 0.0345(17) 0.062(2) 0.0109(15) 0.0288(18) 0.0068(15) C90 0.0370(16) 0.0438(17) 0.0455(18) -0.0185(14) 0.0138(14) -0.0075(14) N10 0.057(2) 0.092(3) 0.075(2) -0.026(2) 0.0193(18) -0.0233(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O2 1.9492(15) . ? Fe1 O1 1.9505(15) . ? Fe1 N1 1.9824(18) . ? Fe1 N2 2.1451(18) . ? Fe1 N4 2.2384(19) . ? Fe1 N3 2.2522(19) . ? O1 C1 1.344(3) . ? O2 C15 1.338(3) . ? N1 C20 1.392(3) . ? N1 C6 1.395(3) . ? N2 C29 1.338(3) . ? N2 C33 1.349(3) . ? N3 C34 1.336(3) . ? N3 C38 1.341(3) . ? N4 C43 1.341(3) . ? N4 C39 1.349(3) . ? C1 C2 1.408(3) . ? C1 C6 1.434(3) . ? C2 C3 1.402(3) . ? C2 C7 1.542(3) . ? C3 C4 1.399(3) . ? C4 C5 1.395(3) . ? C4 C11 1.541(3) . ? C5 C6 1.405(3) . ? C7 C10 1.536(3) . ? C7 C8 1.536(3) . ? C7 C9 1.539(3) . ? C11 C14 1.531(4) . ? C11 C12 1.532(4) . ? C11 C13 1.535(3) . ? C15 C16 1.402(3) . ? C15 C20 1.441(3) . ? C16 C17 1.401(3) . ? C16 C21 1.545(3) . ? C17 C18 1.392(3) . ? C18 C19 1.400(3) . ? C18 C25 1.542(3) . ? C19 C20 1.401(3) . ? C21 C23 1.532(3) . ? C21 C22 1.538(3) . ? C21 C24 1.545(3) . ? C25 C26 1.523(3) . ? C25 C27 1.527(4) . ? C25 C28 1.554(4) . ? C29 C30 1.378(3) . ? C30 C31 1.377(4) . ? C31 C32 1.387(4) . ? C32 C33 1.382(3) . ? C34 C35 1.390(3) . ? C35 C36 1.381(3) . ? C36 C37 1.384(3) . ? C37 C38 1.385(3) . ? C39 C40 1.385(3) . ? C40 C41 1.382(3) . ? C41 C42 1.387(3) . ? C42 C43 1.385(3) . ? Fe2 O4 1.9488(15) . ? Fe2 O3 1.9552(15) . ? Fe2 N5 1.9980(18) . ? Fe2 N6 2.1709(19) . ? Fe2 N7 2.2438(19) . ? Fe2 N8 2.2542(19) . ? O3 C44 1.337(3) . ? O4 C58 1.334(3) . ? N5 C49 1.382(3) . ? N5 C63 1.393(3) . ? N6 C72 1.341(3) . ? N6 C76 1.351(3) . ? N7 C77 1.337(3) . ? N7 C81 1.343(3) . ? N8 C82 1.339(3) . ? N8 C86 1.345(3) . ? C44 C45 1.410(3) . ? C44 C49 1.437(3) . ? C45 C46 1.394(3) . ? C45 C50 1.544(3) . ? C46 C47 1.400(3) . ? C47 C48 1.392(3) . ? C47 C54 1.537(3) . ? C48 C49 1.413(3) . ? C50 C51 1.531(3) . ? C50 C52 1.536(3) . ? C50 C53 1.545(3) . ? C54 C57 1.530(3) . ? C54 C56 1.531(3) . ? C54 C55 1.539(3) . ? C58 C59 1.421(3) . ? C58 C63 1.434(3) . ? C59 C60 1.382(3) . ? C59 C64 1.544(3) . ? C60 C61 1.408(3) . ? C61 C62 1.390(3) . ? C61 C68 1.544(3) . ? C62 C63 1.399(3) . ? C64 C65 1.532(3) . ? C64 C66 1.534(3) . ? C64 C67 1.537(3) . ? C68 C70 1.491(4) . ? C68 C71 1.504(4) . ? C68 C69 1.594(5) . ? C72 C73 1.382(3) . ? C73 C74 1.380(4) . ? C74 C75 1.375(4) . ? C75 C76 1.379(4) . ? C77 C78 1.385(3) . ? C78 C79 1.388(3) . ? C79 C80 1.380(3) . ? C80 C81 1.387(3) . ? C82 C83 1.371(4) . ? C83 C84 1.380(4) . ? C84 C85 1.384(3) . ? C85 C86 1.387(3) . ? C87 C88 1.452(4) . ? C88 N9 1.131(4) . ? C89 C90 1.441(4) . ? C90 N10 1.151(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 O2 Fe1 O1 163.67(6) . . ? O2 Fe1 N1 81.71(7) . . ? O1 Fe1 N1 81.97(7) . . ? O2 Fe1 N2 98.01(7) . . ? O1 Fe1 N2 98.31(7) . . ? N1 Fe1 N2 178.73(8) . . ? O2 Fe1 N4 90.38(6) . . ? O1 Fe1 N4 90.85(6) . . ? N1 Fe1 N4 93.70(7) . . ? N2 Fe1 N4 87.53(7) . . ? O2 Fe1 N3 90.87(7) . . ? O1 Fe1 N3 89.93(6) . . ? N1 Fe1 N3 93.44(7) . . ? N2 Fe1 N3 85.32(7) . . ? N4 Fe1 N3 172.85(7) . . ? C1 O1 Fe1 114.34(13) . . ? C15 O2 Fe1 114.62(13) . . ? C20 N1 C6 131.22(19) . . ? C20 N1 Fe1 114.63(14) . . ? C6 N1 Fe1 114.15(14) . . ? C29 N2 C33 118.5(2) . . ? C29 N2 Fe1 121.34(15) . . ? C33 N2 Fe1 120.11(15) . . ? C34 N3 C38 117.2(2) . . ? C34 N3 Fe1 121.30(15) . . ? C38 N3 Fe1 120.90(15) . . ? C43 N4 C39 117.4(2) . . ? C43 N4 Fe1 121.48(15) . . ? C39 N4 Fe1 120.92(15) . . ? O1 C1 C2 121.8(2) . . ? O1 C1 C6 117.41(18) . . ? C2 C1 C6 120.75(19) . . ? C3 C2 C1 117.6(2) . . ? C3 C2 C7 122.03(19) . . ? C1 C2 C7 120.39(19) . . ? C4 C3 C2 123.1(2) . . ? C5 C4 C3 118.6(2) . . ? C5 C4 C11 121.3(2) . . ? C3 C4 C11 120.09(19) . . ? C4 C5 C6 121.01(19) . . ? N1 C6 C5 128.92(19) . . ? N1 C6 C1 112.13(18) . . ? C5 C6 C1 118.95(18) . . ? C10 C7 C8 107.17(18) . . ? C10 C7 C9 109.3(2) . . ? C8 C7 C9 107.33(18) . . ? C10 C7 C2 110.68(18) . . ? C8 C7 C2 111.84(19) . . ? C9 C7 C2 110.37(18) . . ? C14 C11 C12 108.6(2) . . ? C14 C11 C13 107.2(2) . . ? C12 C11 C13 109.1(2) . . ? C14 C11 C4 112.12(19) . . ? C12 C11 C4 109.2(2) . . ? C13 C11 C4 110.63(19) . . ? O2 C15 C16 122.0(2) . . ? O2 C15 C20 117.48(19) . . ? C16 C15 C20 120.5(2) . . ? C17 C16 C15 118.1(2) . . ? C17 C16 C21 121.5(2) . . ? C15 C16 C21 120.4(2) . . ? C18 C17 C16 122.9(2) . . ? C17 C18 C19 118.6(2) . . ? C17 C18 C25 122.5(2) . . ? C19 C18 C25 118.9(2) . . ? C18 C19 C20 121.3(2) . . ? N1 C20 C19 129.9(2) . . ? N1 C20 C15 111.55(19) . . ? C19 C20 C15 118.60(19) . . ? C23 C21 C22 107.18(19) . . ? C23 C21 C24 108.9(2) . . ? C22 C21 C24 107.64(19) . . ? C23 C21 C16 110.86(18) . . ? C22 C21 C16 111.6(2) . . ? C24 C21 C16 110.46(18) . . ? C26 C25 C27 108.4(2) . . ? C26 C25 C18 112.9(2) . . ? C27 C25 C18 110.1(2) . . ? C26 C25 C28 107.8(2) . . ? C27 C25 C28 109.4(2) . . ? C18 C25 C28 108.2(2) . . ? N2 C29 C30 123.1(2) . . ? C31 C30 C29 118.4(2) . . ? C30 C31 C32 119.3(2) . . ? C33 C32 C31 119.2(2) . . ? N2 C33 C32 121.6(2) . . ? N3 C34 C35 123.2(2) . . ? C36 C35 C34 118.9(2) . . ? C35 C36 C37 118.5(2) . . ? C36 C37 C38 118.9(2) . . ? N3 C38 C37 123.3(2) . . ? N4 C39 C40 122.7(2) . . ? C41 C40 C39 119.5(2) . . ? C40 C41 C42 118.1(2) . . ? C43 C42 C41 119.2(2) . . ? N4 C43 C42 123.1(2) . . ? O4 Fe2 O3 162.59(6) . . ? O4 Fe2 N5 81.68(7) . . ? O3 Fe2 N5 80.91(7) . . ? O4 Fe2 N6 103.47(7) . . ? O3 Fe2 N6 93.92(7) . . ? N5 Fe2 N6 174.79(7) . . ? O4 Fe2 N7 89.67(6) . . ? O3 Fe2 N7 91.82(7) . . ? N5 Fe2 N7 93.44(7) . . ? N6 Fe2 N7 87.39(7) . . ? O4 Fe2 N8 90.18(7) . . ? O3 Fe2 N8 91.20(6) . . ? N5 Fe2 N8 96.07(7) . . ? N6 Fe2 N8 83.27(7) . . ? N7 Fe2 N8 170.37(7) . . ? C44 O3 Fe2 115.15(13) . . ? C58 O4 Fe2 114.46(13) . . ? C49 N5 C63 131.24(19) . . ? C49 N5 Fe2 114.81(14) . . ? C63 N5 Fe2 113.90(14) . . ? C72 N6 C76 118.0(2) . . ? C72 N6 Fe2 122.80(15) . . ? C76 N6 Fe2 118.94(16) . . ? C77 N7 C81 117.2(2) . . ? C77 N7 Fe2 121.45(15) . . ? C81 N7 Fe2 121.23(15) . . ? C82 N8 C86 117.7(2) . . ? C82 N8 Fe2 121.37(16) . . ? C86 N8 Fe2 120.77(15) . . ? O3 C44 C45 122.1(2) . . ? O3 C44 C49 117.19(19) . . ? C45 C44 C49 120.7(2) . . ? C46 C45 C44 117.7(2) . . ? C46 C45 C50 122.1(2) . . ? C44 C45 C50 120.2(2) . . ? C45 C46 C47 123.5(2) . . ? C48 C47 C46 118.2(2) . . ? C48 C47 C54 122.21(19) . . ? C46 C47 C54 119.56(19) . . ? C47 C48 C49 121.4(2) . . ? N5 C49 C48 129.7(2) . . ? N5 C49 C44 111.93(19) . . ? C48 C49 C44 118.40(19) . . ? C51 C50 C52 107.62(19) . . ? C51 C50 C45 111.4(2) . . ? C52 C50 C45 110.21(19) . . ? C51 C50 C53 107.36(18) . . ? C52 C50 C53 109.9(2) . . ? C45 C50 C53 110.33(19) . . ? C57 C54 C56 108.1(2) . . ? C57 C54 C47 112.39(18) . . ? C56 C54 C47 110.02(18) . . ? C57 C54 C55 108.3(2) . . ? C56 C54 C55 108.6(2) . . ? C47 C54 C55 109.4(2) . . ? O4 C58 C59 122.20(19) . . ? O4 C58 C63 118.06(19) . . ? C59 C58 C63 119.7(2) . . ? C60 C59 C58 118.0(2) . . ? C60 C59 C64 122.1(2) . . ? C58 C59 C64 119.91(19) . . ? C59 C60 C61 123.6(2) . . ? C62 C61 C60 117.6(2) . . ? C62 C61 C68 122.5(2) . . ? C60 C61 C68 119.9(2) . . ? C61 C62 C63 121.9(2) . . ? N5 C63 C62 129.2(2) . . ? N5 C63 C58 111.77(19) . . ? C62 C63 C58 119.0(2) . . ? C65 C64 C66 107.87(18) . . ? C65 C64 C67 107.37(18) . . ? C66 C64 C67 108.98(18) . . ? C65 C64 C59 111.05(18) . . ? C66 C64 C59 110.92(18) . . ? C67 C64 C59 110.53(18) . . ? C70 C68 C71 112.2(3) . . ? C70 C68 C61 113.2(2) . . ? C71 C68 C61 111.7(2) . . ? C70 C68 C69 106.3(3) . . ? C71 C68 C69 104.2(3) . . ? C61 C68 C69 108.6(2) . . ? N6 C72 C73 122.4(2) . . ? C74 C73 C72 119.0(2) . . ? C75 C74 C73 119.1(2) . . ? C74 C75 C76 119.0(2) . . ? N6 C76 C75 122.4(2) . . ? N7 C77 C78 123.3(2) . . ? C77 C78 C79 118.8(2) . . ? C80 C79 C78 118.6(2) . . ? C79 C80 C81 118.8(2) . . ? N7 C81 C80 123.3(2) . . ? N8 C82 C83 123.0(2) . . ? C82 C83 C84 119.5(2) . . ? C83 C84 C85 118.4(2) . . ? C84 C85 C86 118.9(2) . . ? N8 C86 C85 122.6(2) . . ? N9 C88 C87 176.9(4) . . ? N10 C90 C89 176.6(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.628 _refine_diff_density_min -0.321 _refine_diff_density_rms 0.046 _iucr_refine_instructions_details ; TITL afh343 in P2(1) CELL 0.71073 14.0101 15.7187 19.9340 90.000 97.6912 90.000 ZERR 4.00 0.0006 0.0007 0.0008 0.000 0.0005 0.000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O FE UNIT 180 232 20 8 4 TEMP -185.000 SIZE 0.064 0.245 0.259 rem Janice Wong 45s ccd1 rem APEX2 2011.4-1, SAINT 7.68a, SADABS 2008/1, SHELXTL 2008/4 SHEL 100 0.80 L.S. 16 ACTA 51 WGHT 0.046900 1.036800 FVAR 0.08096 FE1 5 0.541636 0.800296 0.588091 11.00000 0.01480 0.01199 = 0.01309 0.00057 0.00293 -0.00171 O1 4 0.623831 0.833798 0.520997 11.00000 0.01609 0.01460 = 0.01381 0.00099 0.00272 -0.00122 O2 4 0.433086 0.762287 0.632165 11.00000 0.01899 0.01353 = 0.01440 0.00038 0.00485 -0.00330 N1 3 0.446346 0.785335 0.506013 11.00000 0.01482 0.01132 = 0.01624 -0.00045 0.00359 -0.00008 N2 3 0.645179 0.813490 0.677018 11.00000 0.02169 0.01220 = 0.01976 -0.00168 -0.00005 0.00013 N3 3 0.596511 0.665880 0.584885 11.00000 0.01893 0.01528 = 0.01404 0.00034 0.00067 -0.00232 N4 3 0.500942 0.936119 0.602573 11.00000 0.01797 0.01542 = 0.01488 -0.00204 0.00128 -0.00187 C1 1 0.580891 0.829752 0.456614 11.00000 0.01961 0.00899 = 0.01499 0.00053 0.00379 0.00367 C2 1 0.629934 0.851206 0.401759 11.00000 0.01920 0.00945 = 0.01637 0.00207 0.00519 0.00330 C3 1 0.578709 0.845535 0.336516 11.00000 0.02244 0.01520 = 0.01569 0.00277 0.00825 0.00539 AFIX 43 H3A 2 0.611068 0.859398 0.299017 11.00000 -1.20000 AFIX 0 C4 1 0.482147 0.820412 0.324021 11.00000 0.02168 0.01483 = 0.01488 -0.00082 0.00249 0.00649 C5 1 0.434772 0.798815 0.378907 11.00000 0.01568 0.01226 = 0.01872 -0.00199 0.00203 0.00084 AFIX 43 H5A 2 0.369514 0.780770 0.371089 11.00000 -1.20000 AFIX 0 C6 1 0.482099 0.803347 0.445543 11.00000 0.02014 0.00844 = 0.01430 0.00218 0.00482 0.00437 C7 1 0.735773 0.880694 0.414198 11.00000 0.01893 0.01785 = 0.01858 0.00291 0.00750 0.00022 C8 1 0.775028 0.901212 0.347667 11.00000 0.02596 0.01967 = 0.02097 0.00059 0.01087 -0.00080 AFIX 137 H8A 2 0.738884 0.948965 0.325155 11.00000 -1.50000 H8B 2 0.767949 0.851243 0.318017 11.00000 -1.50000 H8C 2 0.843288 0.916515 0.357392 11.00000 -1.50000 AFIX 0 C9 1 0.799929 0.810374 0.450095 11.00000 0.01890 0.02874 = 0.02681 0.00575 0.00712 0.00209 AFIX 137 H9A 2 0.782694 0.801360 0.495615 11.00000 -1.50000 H9B 2 0.867640 0.827553 0.453425 11.00000 -1.50000 H9C 2 0.790296 0.757439 0.424097 11.00000 -1.50000 AFIX 0 C10 1 0.745753 0.961802 0.457539 11.00000 0.02518 0.02168 = 0.02338 -0.00253 0.01003 -0.00698 AFIX 137 H10A 2 0.727140 0.949584 0.502222 11.00000 -1.50000 H10B 2 0.703727 1.006222 0.435331 11.00000 -1.50000 H10C 2 0.812759 0.981350 0.462720 11.00000 -1.50000 AFIX 0 C11 1 0.429427 0.819208 0.251034 11.00000 0.02198 0.03159 = 0.01549 0.00141 0.00256 0.00773 C12 1 0.430691 0.908836 0.221016 11.00000 0.05280 0.03872 = 0.03012 0.01295 -0.00337 0.01009 AFIX 137 H12A 2 0.403142 0.949155 0.250641 11.00000 -1.50000 H12B 2 0.392520 0.909489 0.176075 11.00000 -1.50000 H12C 2 0.497221 0.925209 0.217125 11.00000 -1.50000 AFIX 0 C13 1 0.478898 0.757569 0.206941 11.00000 0.03649 0.05082 = 0.02245 -0.01287 -0.00009 0.01254 AFIX 137 H13A 2 0.482483 0.700939 0.227689 11.00000 -1.50000 H13B 2 0.544086 0.777973 0.203246 11.00000 -1.50000 H13C 2 0.441718 0.754432 0.161728 11.00000 -1.50000 AFIX 0 C14 1 0.324551 0.790331 0.248042 11.00000 0.02163 0.07220 = 0.01854 0.00084 -0.00216 0.00670 AFIX 137 H14A 2 0.289831 0.829835 0.274133 11.00000 -1.50000 H14B 2 0.322637 0.733058 0.267242 11.00000 -1.50000 H14C 2 0.294068 0.789621 0.200837 11.00000 -1.50000 AFIX 0 C15 1 0.353115 0.744813 0.589827 11.00000 0.01560 0.01008 = 0.01955 -0.00268 0.00324 0.00011 C16 1 0.269504 0.713864 0.612900 11.00000 0.02075 0.01227 = 0.01869 -0.00042 0.00755 0.00153 C17 1 0.188958 0.697646 0.564931 11.00000 0.01651 0.01646 = 0.02671 -0.00139 0.00864 -0.00160 AFIX 43 H17A 2 0.132181 0.676312 0.580191 11.00000 -1.20000 AFIX 0 C18 1 0.188487 0.711422 0.495908 11.00000 0.01474 0.01921 = 0.02450 -0.00492 0.00266 -0.00057 C19 1 0.272524 0.741797 0.473309 11.00000 0.01767 0.02169 = 0.01573 -0.00162 0.00211 0.00196 AFIX 43 H19A 2 0.272962 0.751788 0.426350 11.00000 -1.20000 AFIX 0 C20 1 0.355988 0.757753 0.518571 11.00000 0.01613 0.01108 = 0.01917 -0.00146 0.00487 0.00052 C21 1 0.267140 0.698820 0.689277 11.00000 0.02151 0.01767 = 0.01887 0.00001 0.00743 -0.00503 C22 1 0.169770 0.662324 0.702995 11.00000 0.02629 0.02462 = 0.02715 0.00050 0.01318 -0.00649 AFIX 137 H22A 2 0.118161 0.702128 0.686321 11.00000 -1.50000 H22B 2 0.170639 0.653912 0.751785 11.00000 -1.50000 H22C 2 0.158457 0.607674 0.679620 11.00000 -1.50000 AFIX 0 C23 1 0.282543 0.782353 0.728853 11.00000 0.03325 0.02425 = 0.01876 -0.00298 0.01085 -0.00454 AFIX 137 H23A 2 0.232613 0.823266 0.711243 11.00000 -1.50000 H23B 2 0.346093 0.805579 0.723772 11.00000 -1.50000 H23C 2 0.278774 0.771645 0.776859 11.00000 -1.50000 AFIX 0 C24 1 0.346264 0.634933 0.717522 11.00000 0.02603 0.02494 = 0.01869 0.00398 0.00741 -0.00484 AFIX 137 H24A 2 0.338855 0.582280 0.691010 11.00000 -1.50000 H24B 2 0.340344 0.622362 0.764941 11.00000 -1.50000 H24C 2 0.409780 0.659637 0.714532 11.00000 -1.50000 AFIX 0 C25 1 0.098618 0.695742 0.443758 11.00000 0.01702 0.03296 = 0.02726 -0.00013 -0.00002 -0.00110 C26 1 0.014541 0.658831 0.475394 11.00000 0.01778 0.04417 = 0.03647 -0.00056 0.00010 -0.00561 AFIX 137 H26A 2 0.032459 0.602836 0.494731 11.00000 -1.50000 H26B 2 -0.041512 0.653009 0.440598 11.00000 -1.50000 H26C 2 -0.001411 0.696903 0.511206 11.00000 -1.50000 AFIX 0 C27 1 0.122810 0.634694 0.388886 11.00000 0.02414 0.05221 = 0.03196 -0.01567 -0.00318 -0.00563 AFIX 137 H27A 2 0.146383 0.580881 0.409723 11.00000 -1.50000 H27B 2 0.172702 0.659962 0.365077 11.00000 -1.50000 H27C 2 0.064871 0.624058 0.356638 11.00000 -1.50000 AFIX 0 C28 1 0.065719 0.782474 0.411071 11.00000 0.02275 0.04707 = 0.03243 0.00302 -0.00318 -0.00231 AFIX 137 H28A 2 0.053301 0.822588 0.446531 11.00000 -1.50000 H28B 2 0.006674 0.774334 0.379354 11.00000 -1.50000 H28C 2 0.116435 0.805191 0.386717 11.00000 -1.50000 AFIX 0 C29 1 0.737706 0.830658 0.672698 11.00000 0.02133 0.01841 = 0.02717 -0.00337 0.00194 -0.00266 AFIX 43 H29A 2 0.756189 0.840463 0.629207 11.00000 -1.20000 AFIX 0 C30 1 0.807463 0.834792 0.728332 11.00000 0.02687 0.02264 = 0.03585 -0.00142 -0.00535 -0.00041 AFIX 43 H30A 2 0.872459 0.847399 0.723352 11.00000 -1.20000 AFIX 0 C31 1 0.780666 0.820209 0.791301 11.00000 0.03827 0.02257 = 0.03263 -0.00024 -0.01604 0.00007 AFIX 43 H31A 2 0.827268 0.821751 0.830559 11.00000 -1.20000 AFIX 0 C32 1 0.684877 0.803240 0.796784 11.00000 0.04281 0.03015 = 0.02133 0.00510 -0.00116 -0.00479 AFIX 43 H32A 2 0.664903 0.794024 0.839903 11.00000 -1.20000 AFIX 0 C33 1 0.618836 0.799898 0.738782 11.00000 0.02936 0.02294 = 0.01837 -0.00004 -0.00044 -0.00429 AFIX 43 H33A 2 0.553327 0.787739 0.742493 11.00000 -1.20000 AFIX 0 C34 1 0.676787 0.647801 0.558389 11.00000 0.02330 0.01690 = 0.02225 0.00033 0.00438 -0.00161 AFIX 43 H34A 2 0.715071 0.693638 0.546059 11.00000 -1.20000 AFIX 0 C35 1 0.707078 0.565200 0.547965 11.00000 0.02101 0.02233 = 0.02903 0.00088 0.00734 0.00365 AFIX 43 H35A 2 0.765259 0.555091 0.529658 11.00000 -1.20000 AFIX 0 C36 1 0.651175 0.498097 0.564669 11.00000 0.02895 0.01055 = 0.02498 -0.00126 0.00241 0.00181 AFIX 43 H36A 2 0.669406 0.441000 0.557281 11.00000 -1.20000 AFIX 0 C37 1 0.567966 0.515911 0.592425 11.00000 0.02498 0.01678 = 0.02304 0.00111 0.00341 -0.00515 AFIX 43 H37A 2 0.528445 0.471168 0.605101 11.00000 -1.20000 AFIX 0 C38 1 0.543320 0.600067 0.601399 11.00000 0.01940 0.01506 = 0.02061 -0.00041 0.00407 -0.00225 AFIX 43 H38A 2 0.485877 0.611778 0.620187 11.00000 -1.20000 AFIX 0 C39 1 0.546648 0.999973 0.574802 11.00000 0.02010 0.01998 = 0.01720 0.00002 0.00667 -0.00333 AFIX 43 H39A 2 0.599356 0.986478 0.551295 11.00000 -1.20000 AFIX 0 C40 1 0.519904 1.084417 0.579143 11.00000 0.02640 0.01490 = 0.02020 0.00324 0.00425 -0.00376 AFIX 43 H40A 2 0.554345 1.127716 0.559360 11.00000 -1.20000 AFIX 0 C41 1 0.442712 1.105186 0.612484 11.00000 0.02451 0.01562 = 0.01877 -0.00016 0.00092 0.00083 AFIX 43 H41A 2 0.423161 1.162678 0.616175 11.00000 -1.20000 AFIX 0 C42 1 0.394605 1.039708 0.640400 11.00000 0.02098 0.01889 = 0.02381 -0.00334 0.00709 -0.00049 AFIX 43 H42A 2 0.340866 1.051605 0.663314 11.00000 -1.20000 AFIX 0 C43 1 0.425809 0.956802 0.634485 11.00000 0.02067 0.01942 = 0.01945 0.00088 0.00488 -0.00367 AFIX 43 H43A 2 0.392427 0.912509 0.653945 11.00000 -1.20000 AFIX 0 FE2 5 0.937985 0.056239 0.915347 11.00000 0.01642 0.01277 = 0.01276 0.00063 0.00270 -0.00037 O3 4 0.875732 0.023983 0.993712 11.00000 0.01884 0.01679 = 0.01531 0.00188 0.00376 0.00051 O4 4 1.032799 0.094031 0.858630 11.00000 0.01701 0.01721 = 0.01481 0.00093 0.00172 -0.00165 N5 3 1.049480 0.071904 0.987984 11.00000 0.01676 0.01268 = 0.01494 0.00121 0.00249 0.00071 N6 3 0.808778 0.037383 0.843694 11.00000 0.01869 0.01346 = 0.02171 -0.00279 0.00138 0.00097 N7 3 0.976115 -0.079428 0.896130 11.00000 0.01656 0.01508 = 0.01706 0.00193 0.00065 -0.00107 N8 3 0.881481 0.190208 0.918918 11.00000 0.01987 0.01543 = 0.01517 0.00066 0.00147 -0.00120 C44 1 0.932051 0.027813 1.053302 11.00000 0.02002 0.01332 = 0.01301 0.00043 0.00196 0.00383 C45 1 0.898236 0.005834 1.114542 11.00000 0.02135 0.01134 = 0.01830 0.00104 0.00809 0.00385 C46 1 0.962140 0.013587 1.174133 11.00000 0.02357 0.01345 = 0.01503 0.00274 0.00506 0.00580 AFIX 43 H46A 2 0.939823 -0.000725 1.215648 11.00000 -1.20000 AFIX 0 C47 1 1.057414 0.041319 1.176115 11.00000 0.01974 0.01295 = 0.01454 -0.00025 0.00274 0.00694 C48 1 1.090316 0.061745 1.115222 11.00000 0.01668 0.01448 = 0.01931 -0.00018 0.00302 0.00504 AFIX 43 H48A 2 1.154759 0.080778 1.115687 11.00000 -1.20000 AFIX 0 C49 1 1.029928 0.054775 1.052750 11.00000 0.02294 0.01007 = 0.01556 0.00034 0.00561 0.00384 C50 1 0.793846 -0.025694 1.114285 11.00000 0.02441 0.02103 = 0.01849 0.00452 0.00717 0.00234 C51 1 0.773405 -0.047619 1.185839 11.00000 0.02365 0.02347 = 0.02276 0.00424 0.00989 0.00076 AFIX 137 H51A 2 0.817946 -0.092150 1.204910 11.00000 -1.50000 H51B 2 0.706993 -0.067990 1.183982 11.00000 -1.50000 H51C 2 0.782193 0.003252 1.214422 11.00000 -1.50000 AFIX 0 C52 1 0.776513 -0.106451 1.070949 11.00000 0.03458 0.03100 = 0.02236 0.00200 0.00837 -0.01119 AFIX 137 H52A 2 0.823056 -0.150279 1.088428 11.00000 -1.50000 H52B 2 0.784425 -0.093281 1.023957 11.00000 -1.50000 H52C 2 0.711001 -0.127304 1.072819 11.00000 -1.50000 AFIX 0 C53 1 0.721651 0.044222 1.086544 11.00000 0.02124 0.04075 = 0.02605 0.01248 0.00768 0.00803 AFIX 137 H53A 2 0.655854 0.024799 1.089420 11.00000 -1.50000 H53B 2 0.728783 0.056044 1.039201 11.00000 -1.50000 H53C 2 0.734523 0.096172 1.113415 11.00000 -1.50000 AFIX 0 C54 1 1.122532 0.046894 1.244461 11.00000 0.02262 0.02015 = 0.01485 0.00048 0.00277 0.00655 C55 1 1.125740 -0.040308 1.279750 11.00000 0.04986 0.02887 = 0.02313 0.00608 -0.00586 0.00842 AFIX 137 H55A 2 1.167382 -0.036885 1.323270 11.00000 -1.50000 H55B 2 1.151330 -0.082972 1.251053 11.00000 -1.50000 H55C 2 1.060550 -0.056610 1.287405 11.00000 -1.50000 AFIX 0 C56 1 1.082313 0.112512 1.290029 11.00000 0.02688 0.03598 = 0.02011 -0.00773 -0.00138 0.00832 AFIX 137 H56A 2 1.124800 0.116328 1.333168 11.00000 -1.50000 H56B 2 1.017807 0.095041 1.298404 11.00000 -1.50000 H56C 2 1.078584 0.168175 1.267686 11.00000 -1.50000 AFIX 0 C57 1 1.225718 0.072733 1.236570 11.00000 0.02229 0.06144 = 0.01655 0.00117 0.00143 0.00645 AFIX 137 H57A 2 1.264506 0.075103 1.281250 11.00000 -1.50000 H57B 2 1.225296 0.128828 1.215075 11.00000 -1.50000 H57C 2 1.253451 0.030822 1.208331 11.00000 -1.50000 AFIX 0 C58 1 1.120494 0.107873 0.892000 11.00000 0.01686 0.01024 = 0.01670 -0.00078 0.00158 0.00405 C59 1 1.198672 0.135352 0.858768 11.00000 0.02045 0.01565 = 0.01364 -0.00047 0.00423 0.00144 C60 1 1.287452 0.145903 0.897338 11.00000 0.01738 0.02965 = 0.02048 0.00130 0.00667 0.00049 AFIX 43 H60A 2 1.339757 0.164588 0.875295 11.00000 -1.20000 AFIX 0 C61 1 1.304682 0.130491 0.967511 11.00000 0.01905 0.03507 = 0.02054 0.00263 0.00263 0.00041 C62 1 1.226924 0.105710 0.999498 11.00000 0.02142 0.03024 = 0.01521 0.00169 0.00104 0.00332 AFIX 43 H62A 2 1.236747 0.095479 1.046890 11.00000 -1.20000 AFIX 0 C63 1 1.134585 0.095394 0.963914 11.00000 0.01853 0.01267 = 0.01728 0.00061 0.00380 0.00190 C64 1 1.183102 0.151375 0.781683 11.00000 0.01826 0.01970 = 0.01348 0.00053 0.00283 -0.00286 C65 1 1.275016 0.185504 0.757366 11.00000 0.02205 0.02465 = 0.01991 0.00345 0.00674 -0.00183 AFIX 137 H65A 2 1.264192 0.192658 0.708096 11.00000 -1.50000 H65B 2 1.327816 0.145157 0.769563 11.00000 -1.50000 H65C 2 1.291823 0.240525 0.778886 11.00000 -1.50000 AFIX 0 C66 1 1.154870 0.068907 0.742836 11.00000 0.03119 0.02003 = 0.01972 -0.00071 0.00734 -0.00442 AFIX 137 H66A 2 1.147506 0.080206 0.694068 11.00000 -1.50000 H66B 2 1.093828 0.047763 0.755297 11.00000 -1.50000 H66C 2 1.205243 0.026084 0.754332 11.00000 -1.50000 AFIX 0 C67 1 1.103626 0.217966 0.763243 11.00000 0.02137 0.02099 = 0.01948 0.00319 0.00256 0.00001 AFIX 137 H67A 2 1.101298 0.233716 0.715484 11.00000 -1.50000 H67B 2 1.117517 0.268568 0.791591 11.00000 -1.50000 H67C 2 1.041376 0.194085 0.770894 11.00000 -1.50000 AFIX 0 C68 1 1.406366 0.144462 1.006405 11.00000 0.02073 0.07107 = 0.02186 0.00192 0.00057 0.00190 C69 1 1.429465 0.243786 1.007778 11.00000 0.04615 0.06336 = 0.06933 0.00733 -0.01892 -0.01529 AFIX 137 H69A 2 1.494407 0.253449 1.031575 11.00000 -1.50000 H69B 2 1.382457 0.273894 1.031307 11.00000 -1.50000 H69C 2 1.425732 0.265082 0.961295 11.00000 -1.50000 AFIX 0 C70 1 1.415142 0.116593 1.078443 11.00000 0.02338 0.08545 = 0.03649 -0.00209 -0.00401 -0.00561 AFIX 137 H70A 2 1.400025 0.055840 1.080348 11.00000 -1.50000 H70B 2 1.370074 0.149120 1.102020 11.00000 -1.50000 H70C 2 1.481097 0.126498 1.100321 11.00000 -1.50000 AFIX 0 C71 1 1.482993 0.105940 0.969744 11.00000 0.02137 0.11973 = 0.03466 -0.00227 0.00138 0.01412 AFIX 137 H71A 2 1.477111 0.043818 0.969934 11.00000 -1.50000 H71B 2 1.546669 0.122416 0.992502 11.00000 -1.50000 H71C 2 1.475114 0.126492 0.922914 11.00000 -1.50000 AFIX 0 C72 1 0.805889 0.051119 0.777067 11.00000 0.02654 0.02243 = 0.02089 0.00283 0.00073 -0.00294 AFIX 43 H72A 2 0.863926 0.065101 0.759818 11.00000 -1.20000 AFIX 0 C73 1 0.721511 0.045671 0.732568 11.00000 0.03587 0.02699 = 0.02665 0.00361 -0.00828 -0.00537 AFIX 43 H73A 2 0.721884 0.054687 0.685479 11.00000 -1.20000 AFIX 0 C74 1 0.636731 0.026942 0.757566 11.00000 0.02929 0.02523 = 0.04022 -0.00431 -0.01227 0.00082 AFIX 43 H74A 2 0.577727 0.023850 0.728008 11.00000 -1.20000 AFIX 0 C75 1 0.638769 0.012812 0.825829 11.00000 0.01943 0.03185 = 0.04144 -0.01087 0.00160 -0.00329 AFIX 43 H75A 2 0.581227 -0.000171 0.844084 11.00000 -1.20000 AFIX 0 C76 1 0.725565 0.017765 0.867385 11.00000 0.02489 0.02607 = 0.02702 -0.00416 0.00465 -0.00205 AFIX 43 H76A 2 0.726889 0.006987 0.914393 11.00000 -1.20000 AFIX 0 C77 1 1.017217 -0.101409 0.841850 11.00000 0.02602 0.01750 = 0.02602 0.00396 0.00848 -0.00162 AFIX 43 H77A 2 1.027667 -0.058357 0.810187 11.00000 -1.20000 AFIX 0 C78 1 1.045320 -0.183799 0.829472 11.00000 0.02861 0.02041 = 0.02691 -0.00322 0.01202 -0.00088 AFIX 43 H78A 2 1.074064 -0.196751 0.790151 11.00000 -1.20000 AFIX 0 C79 1 1.030706 -0.247057 0.875575 11.00000 0.01924 0.01490 = 0.02967 -0.00122 -0.00065 0.00085 AFIX 43 H79A 2 1.049318 -0.304124 0.868481 11.00000 -1.20000 AFIX 0 C80 1 0.988586 -0.225373 0.931932 11.00000 0.02830 0.01519 = 0.01909 0.00348 -0.00202 -0.00269 AFIX 43 H80A 2 0.977553 -0.267274 0.964368 11.00000 -1.20000 AFIX 0 C81 1 0.962646 -0.141270 0.940360 11.00000 0.02484 0.01649 = 0.01624 -0.00053 0.00158 -0.00144 AFIX 43 H81A 2 0.933927 -0.126711 0.979364 11.00000 -1.20000 AFIX 0 C82 1 0.804065 0.208219 0.949122 11.00000 0.02449 0.02026 = 0.02362 0.00065 0.00801 -0.00373 AFIX 43 H82A 2 0.769981 0.162551 0.966185 11.00000 -1.20000 AFIX 0 C83 1 0.771788 0.289546 0.956530 11.00000 0.02824 0.02198 = 0.03114 -0.00106 0.01146 0.00240 AFIX 43 H83A 2 0.716198 0.299474 0.977962 11.00000 -1.20000 AFIX 0 C84 1 0.820671 0.356913 0.932613 11.00000 0.02840 0.02112 = 0.02763 -0.00277 0.00184 0.00487 AFIX 43 H84A 2 0.799680 0.413778 0.937482 11.00000 -1.20000 AFIX 0 C85 1 0.900978 0.339659 0.901374 11.00000 0.02721 0.01635 = 0.02099 0.00067 0.00029 -0.00269 AFIX 43 H85A 2 0.936400 0.384561 0.884485 11.00000 -1.20000 AFIX 0 C86 1 0.928868 0.255666 0.895146 11.00000 0.02087 0.02152 = 0.01846 0.00192 0.00345 -0.00162 AFIX 43 H86A 2 0.983594 0.243927 0.873226 11.00000 -1.20000 AFIX 0 C87 1 0.143849 0.923662 0.575150 11.00000 0.04921 0.02949 = 0.04734 -0.00255 0.01285 -0.00237 AFIX 137 H87A 2 0.186097 0.966429 0.599466 11.00000 -1.50000 H87B 2 0.113237 0.947612 0.532200 11.00000 -1.50000 H87C 2 0.181924 0.873652 0.566141 11.00000 -1.50000 AFIX 0 C88 1 0.070214 0.898915 0.616097 11.00000 0.05653 0.04206 = 0.04444 0.00325 0.00861 0.00085 N9 3 0.015592 0.880548 0.650510 11.00000 0.07170 0.08633 = 0.08106 0.02289 0.03062 -0.00327 C89 1 0.287594 -0.078860 0.894978 11.00000 0.05984 0.03454 = 0.06213 0.01094 0.02879 0.00676 AFIX 137 H89A 2 0.247722 -0.028721 0.900315 11.00000 -1.50000 H89B 2 0.321971 -0.095305 0.939144 11.00000 -1.50000 H89C 2 0.246430 -0.125962 0.876428 11.00000 -1.50000 AFIX 0 C90 1 0.356195 -0.059146 0.849466 11.00000 0.03702 0.04383 = 0.04551 -0.01851 0.01381 -0.00752 N10 3 0.407552 -0.041053 0.811278 11.00000 0.05694 0.09196 = 0.07453 -0.02610 0.01934 -0.02327 HKLF 4 REM afh343 in P2(1) REM R1 = 0.0354 for 15850 Fo > 4sig(Fo) and 0.0426 for all 17560 data REM 981 parameters refined using 1 restraints END WGHT 0.0469 1.0369 REM Highest difference peak 0.628, deepest hole -0.321, 1-sigma level 0.046 Q1 1 1.4277 0.0201 1.0318 11.00000 0.05 0.63 Q2 1 0.3709 -0.0827 0.9776 11.00000 0.05 0.52 Q3 1 1.4030 0.1826 1.0650 11.00000 0.05 0.42 Q4 1 0.4473 -0.1293 0.8744 11.00000 0.05 0.42 Q5 1 0.4436 -0.1299 0.9540 11.00000 0.05 0.35 Q6 1 0.5318 0.8077 0.4479 11.00000 0.05 0.24 Q7 1 1.4135 0.0892 1.0139 11.00000 0.05 0.24 Q8 1 0.2734 0.7034 0.6500 11.00000 0.05 0.22 Q9 1 0.0415 0.9818 0.6227 11.00000 0.05 0.22 Q10 1 -0.0015 0.9488 0.5284 11.00000 0.05 0.21 Q11 1 0.6026 0.8546 0.4287 11.00000 0.05 0.21 Q12 1 0.0550 0.9815 0.5416 11.00000 0.05 0.21 Q13 1 1.1341 0.0603 1.1181 11.00000 0.05 0.21 Q14 1 0.9822 0.0462 1.0552 11.00000 0.05 0.20 Q15 1 0.3705 -0.1080 0.8793 11.00000 0.05 0.20 Q16 1 0.4565 0.8078 0.2897 11.00000 0.05 0.20 Q17 1 1.4677 0.1687 0.9598 11.00000 0.05 0.20 Q18 1 0.4581 0.7806 0.4771 11.00000 0.05 0.20 Q19 1 0.0533 0.8402 0.4640 11.00000 0.05 0.20 Q20 1 0.2982 0.6688 0.7000 11.00000 0.05 0.19 ; #===end