# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Young Keun Chung' _publ_contact_author_address ; Department of Chemistry Seoul National University Seoul KOREA ; _publ_contact_author_email YKCHUNG@PLAZA.SNU.AC.KR _publ_section_title ; A chiral molecular bowl containing three ferrocenes: synthesis and its efficiency in an optical resolution of 1,1'-bi-2-naphthol ; loop_ _publ_author_name 'Young Keun Chung' 'Bog Ki Hong' 'In Su Lee' 'Dong Mok Shin' data_(R)3-(R)4 _database_code_depnum_ccdc_archive 'CCDC 227311' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H90.50 Cl5.50 Fe3 N6 O5' _chemical_formula_weight 1578.61 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 15.5300(2) _cell_length_b 21.4870(2) _cell_length_c 26.6130(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8880.57(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2436 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 24.713 _exptl_crystal_description needle _exptl_crystal_colour 'deep orange' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.181 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3296 _exptl_absorpt_coefficient_mu 0.696 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Since the crystal decomposed when it was out of the mother liquor, It was placed in the fine-sealed capillary tube with mother liquor, and then measured. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15088 _diffrn_reflns_av_R_equivalents 0.1344 _diffrn_reflns_av_sigmaI/netI 0.2615 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 24.89 _reflns_number_total 9728 _reflns_number_gt 3905 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0906P)^2^+1.5481P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(4) _refine_ls_number_reflns 9728 _refine_ls_number_parameters 832 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.2539 _refine_ls_R_factor_gt 0.0960 _refine_ls_wR_factor_ref 0.2431 _refine_ls_wR_factor_gt 0.1810 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 0.86443(16) 0.62007(11) 0.08908(10) 0.0722(8) Uani 1 1 d . . . Fe2 Fe 0.89651(14) 0.83671(10) 0.31072(10) 0.0644(8) Uani 1 1 d . . . Fe3 Fe 0.53992(14) 0.64771(11) 0.27716(9) 0.0644(8) Uani 1 1 d . . . N1 N 1.0700(8) 0.6089(5) 0.1813(6) 0.060(4) Uani 1 1 d . . . N2 N 1.0050(8) 0.6816(7) 0.2666(6) 0.066(4) Uani 1 1 d . . . N3 N 0.8604(9) 0.7140(7) 0.4266(5) 0.074(4) Uani 1 1 d . . . N4 N 0.7454(9) 0.6362(6) 0.3679(5) 0.063(4) Uani 1 1 d . . . N5 N 0.5847(8) 0.4707(6) 0.2253(6) 0.059(4) Uani 1 1 d . . . N6 N 0.7402(9) 0.4934(7) 0.1693(5) 0.078(5) Uani 1 1 d . . . C1 C 0.9843(10) 0.5861(9) 0.1037(9) 0.071(6) Uani 1 1 d . . . C2 C 0.9328(10) 0.5405(9) 0.0754(7) 0.078(6) Uani 1 1 d . . . H2 H 0.9183 0.5013 0.0874 0.093 Uiso 1 1 calc R . . C3 C 0.9079(11) 0.5637(10) 0.0273(8) 0.085(6) Uani 1 1 d . . . H3 H 0.8767 0.5432 0.0025 0.103 Uiso 1 1 calc R . . C4 C 0.9431(12) 0.6283(11) 0.0258(7) 0.087(6) Uani 1 1 d . . . H4 H 0.9376 0.6560 -0.0009 0.105 Uiso 1 1 calc R . . C5 C 0.9893(11) 0.6415(10) 0.0748(9) 0.087(6) Uani 1 1 d . . . H5 H 1.0157 0.6786 0.0841 0.104 Uiso 1 1 calc R . . C6 C 0.7505(10) 0.5958(8) 0.1243(7) 0.061(5) Uani 1 1 d . . . C7 C 0.7348(10) 0.6367(9) 0.0818(8) 0.080(6) Uani 1 1 d . . . H7 H 0.6992 0.6282 0.0545 0.096 Uiso 1 1 calc R . . C8 C 0.7831(15) 0.6912(8) 0.0892(10) 0.117(9) Uani 1 1 d . . . H8 H 0.7880 0.7233 0.0659 0.141 Uiso 1 1 calc R . . C9 C 0.8243(12) 0.6907(9) 0.1381(9) 0.089(7) Uani 1 1 d . . . H9 H 0.8559 0.7224 0.1531 0.107 Uiso 1 1 calc R . . C10 C 0.8053(11) 0.6307(8) 0.1579(7) 0.069(5) Uani 1 1 d . . . H10 H 0.8256 0.6159 0.1885 0.083 Uiso 1 1 calc R . . C11 C 0.9284(12) 0.7801(9) 0.2506(7) 0.077(6) Uani 1 1 d . . . C12 C 0.8439(12) 0.7620(7) 0.2712(6) 0.066(5) Uani 1 1 d . . . H12 H 0.8291 0.7228 0.2832 0.079 Uiso 1 1 calc R . . C13 C 0.7877(11) 0.8160(8) 0.2693(7) 0.074(5) Uani 1 1 d . . . H13 H 0.7316 0.8180 0.2813 0.089 Uiso 1 1 calc R . . C14 C 0.8354(12) 0.8674(8) 0.2450(7) 0.084(6) Uani 1 1 d . . . H14 H 0.8150 0.9074 0.2390 0.101 Uiso 1 1 calc R . . C15 C 0.9174(14) 0.8442(8) 0.2326(6) 0.085(6) Uani 1 1 d . . . H15 H 0.9591 0.8666 0.2152 0.102 Uiso 1 1 calc R . . C16 C 0.9249(12) 0.8055(8) 0.3830(6) 0.061(5) Uani 1 1 d . . . C17 C 0.8613(12) 0.8522(9) 0.3841(6) 0.070(5) Uani 1 1 d . . . H17 H 0.8058 0.8475 0.3965 0.084 Uiso 1 1 calc R . . C18 C 0.8954(14) 0.9070(9) 0.3634(7) 0.082(6) Uani 1 1 d . . . H18 H 0.8668 0.9448 0.3599 0.098 Uiso 1 1 calc R . . C19 C 0.9795(13) 0.8946(9) 0.3491(7) 0.082(6) Uani 1 1 d . . . H19 H 1.0177 0.9237 0.3360 0.098 Uiso 1 1 calc R . . C20 C 0.9986(10) 0.8311(8) 0.3574(7) 0.074(6) Uani 1 1 d . . . H20 H 1.0486 0.8101 0.3481 0.089 Uiso 1 1 calc R . . C21 C 0.6473(9) 0.6873(7) 0.3101(8) 0.060(5) Uani 1 1 d . . . C22 C 0.5808(11) 0.7331(8) 0.2987(10) 0.089(7) Uani 1 1 d . . . H22 H 0.5529 0.7580 0.3222 0.107 Uiso 1 1 calc R . . C23 C 0.5657(12) 0.7337(9) 0.2466(8) 0.080(6) Uani 1 1 d . . . H23 H 0.5275 0.7599 0.2300 0.096 Uiso 1 1 calc R . . C24 C 0.6174(11) 0.6884(9) 0.2240(8) 0.085(6) Uani 1 1 d . . . H24 H 0.6187 0.6789 0.1899 0.102 Uiso 1 1 calc R . . C25 C 0.6675(9) 0.6594(8) 0.2620(7) 0.065(5) Uani 1 1 d . . . H25 H 0.7070 0.6276 0.2568 0.078 Uiso 1 1 calc R . . C26 C 0.5155(11) 0.5526(9) 0.2766(8) 0.077(5) Uani 1 1 d . . . C27 C 0.4648(10) 0.5846(8) 0.2384(7) 0.068(5) Uani 1 1 d . . . H27 H 0.4654 0.5774 0.2039 0.082 Uiso 1 1 calc R . . C28 C 0.4141(10) 0.6294(8) 0.2652(9) 0.075(5) Uani 1 1 d . . . H28 H 0.3767 0.6575 0.2500 0.090 Uiso 1 1 calc R . . C29 C 0.4284(10) 0.6253(9) 0.3185(8) 0.079(6) Uani 1 1 d . . . H29 H 0.4008 0.6478 0.3436 0.094 Uiso 1 1 calc R . . C30 C 0.4927(12) 0.5801(10) 0.3247(8) 0.094(7) Uani 1 1 d . . . H30 H 0.5174 0.5692 0.3553 0.112 Uiso 1 1 calc R . . C31 C 1.0868(11) 0.5918(8) 0.2362(7) 0.073(5) Uani 1 1 d . . . H31 H 1.0409 0.5642 0.2482 0.088 Uiso 1 1 calc R . . C32 C 1.0891(10) 0.6510(7) 0.2690(7) 0.069(5) Uani 1 1 d . . . H32 H 1.1325 0.6794 0.2553 0.083 Uiso 1 1 calc R . . C33 C 1.1117(11) 0.6376(8) 0.3244(5) 0.075(6) Uani 1 1 d . . . H33A H 1.1140 0.6765 0.3428 0.090 Uiso 1 1 calc R . . H33B H 1.0669 0.6120 0.3392 0.090 Uiso 1 1 calc R . . C34 C 1.1973(11) 0.6046(9) 0.3289(8) 0.093(7) Uani 1 1 d . . . H34A H 1.2079 0.5938 0.3638 0.112 Uiso 1 1 calc R . . H34B H 1.2432 0.6319 0.3178 0.112 Uiso 1 1 calc R . . C35 C 1.1962(11) 0.5434(9) 0.2956(8) 0.089(6) Uani 1 1 d . . . H35A H 1.1539 0.5147 0.3092 0.106 Uiso 1 1 calc R . . H35B H 1.2521 0.5234 0.2977 0.106 Uiso 1 1 calc R . . C36 C 1.1742(10) 0.5564(8) 0.2376(6) 0.068(5) Uani 1 1 d . . . H36A H 1.2191 0.5814 0.2223 0.082 Uiso 1 1 calc R . . H36B H 1.1697 0.5175 0.2193 0.082 Uiso 1 1 calc R . . C37 C 1.0152(10) 0.5764(8) 0.1576(7) 0.062(5) Uani 1 1 d . . . H37 H 0.9913 0.5431 0.1750 0.074 Uiso 1 1 calc R . . C38 C 1.0016(11) 0.7392(11) 0.2516(7) 0.079(6) Uani 1 1 d . . . H38 H 1.0531 0.7560 0.2401 0.094 Uiso 1 1 calc R . . C39 C 0.8613(10) 0.6460(8) 0.4349(7) 0.069(5) Uani 1 1 d . . . H39 H 0.9031 0.6269 0.4121 0.083 Uiso 1 1 calc R . . C40 C 0.7695(10) 0.6216(8) 0.4220(8) 0.074(6) Uani 1 1 d . . . H40 H 0.7279 0.6419 0.4443 0.088 Uiso 1 1 calc R . . C41 C 0.7661(11) 0.5499(8) 0.4314(9) 0.093(7) Uani 1 1 d . . . H41A H 0.7078 0.5355 0.4255 0.112 Uiso 1 1 calc R . . H41B H 0.8032 0.5295 0.4072 0.112 Uiso 1 1 calc R . . C42 C 0.7939(15) 0.5302(10) 0.4849(8) 0.117(9) Uani 1 1 d . . . H42A H 0.7527 0.5457 0.5093 0.140 Uiso 1 1 calc R . . H42B H 0.7948 0.4851 0.4873 0.140 Uiso 1 1 calc R . . C43 C 0.8803(15) 0.5552(9) 0.4964(8) 0.110(7) Uani 1 1 d . . . H43A H 0.9223 0.5356 0.4745 0.132 Uiso 1 1 calc R . . H43B H 0.8953 0.5448 0.5308 0.132 Uiso 1 1 calc R . . C44 C 0.8850(11) 0.6292(9) 0.4894(6) 0.085(6) Uani 1 1 d . . . H44A H 0.8453 0.6492 0.5124 0.102 Uiso 1 1 calc R . . H44B H 0.9426 0.6438 0.4969 0.102 Uiso 1 1 calc R . . C45 C 0.9158(10) 0.7384(9) 0.3956(7) 0.067(5) Uani 1 1 d . . . H45 H 0.9535 0.7110 0.3798 0.081 Uiso 1 1 calc R . . C46 C 0.6787(10) 0.6692(9) 0.3629(6) 0.063(5) Uani 1 1 d . . . H46 H 0.6485 0.6824 0.3911 0.076 Uiso 1 1 calc R . . C47 C 0.6537(10) 0.4258(7) 0.2220(7) 0.064(5) Uani 1 1 d . . . H47 H 0.6964 0.4331 0.2485 0.077 Uiso 1 1 calc R . . C48 C 0.6969(10) 0.4314(8) 0.1685(7) 0.070(5) Uani 1 1 d . . . H48 H 0.6533 0.4296 0.1419 0.084 Uiso 1 1 calc R . . C49 C 0.7645(10) 0.3824(9) 0.1608(7) 0.086(6) Uani 1 1 d . . . H49A H 0.8101 0.3879 0.1853 0.103 Uiso 1 1 calc R . . H49B H 0.7893 0.3868 0.1275 0.103 Uiso 1 1 calc R . . C50 C 0.7236(14) 0.3143(10) 0.1667(10) 0.109(8) Uani 1 1 d . . . H50A H 0.6803 0.3079 0.1409 0.131 Uiso 1 1 calc R . . H50B H 0.7682 0.2832 0.1623 0.131 Uiso 1 1 calc R . . C51 C 0.6835(12) 0.3070(8) 0.2172(12) 0.115(9) Uani 1 1 d . . . H51A H 0.7277 0.3098 0.2428 0.138 Uiso 1 1 calc R . . H51B H 0.6572 0.2661 0.2197 0.138 Uiso 1 1 calc R . . C52 C 0.6144(11) 0.3575(7) 0.2267(7) 0.086(6) Uani 1 1 d . . . H52A H 0.5904 0.3521 0.2600 0.103 Uiso 1 1 calc R . . H52B H 0.5681 0.3527 0.2025 0.103 Uiso 1 1 calc R . . C53 C 0.5839(10) 0.5038(7) 0.2654(8) 0.064(5) Uani 1 1 d . . . H53 H 0.6275 0.4977 0.2889 0.077 Uiso 1 1 calc R . . C54 C 0.7190(3) 0.52755(18) 0.13275(14) 0.076(6) Uani 1 1 d . . . H54 H 0.6817 0.5108 0.1090 0.091 Uiso 1 1 calc R . . O1 O 0.8318(3) 0.40021(18) 0.30369(14) 0.077(3) Uani 1 1 d R . . O2 O 0.8833(3) 0.22346(18) 0.35624(14) 0.079(3) Uani 1 1 d R . . C55 C 0.8574(3) 0.34862(18) 0.38708(14) 0.059(5) Uani 1 1 d R . . C56 C 0.8745(3) 0.39472(18) 0.35184(14) 0.057(5) Uani 1 1 d R . . C57 C 0.9428(3) 0.43557(18) 0.35929(14) 0.071(5) Uani 1 1 d R . . H57 H 0.9542 0.4664 0.3357 0.085 Uiso 1 1 calc R . . C58 C 0.9938(3) 0.43032(18) 0.40198(14) 0.113(9) Uani 1 1 d R . . H58 H 1.0394 0.4577 0.4070 0.135 Uiso 1 1 calc R . . C59 C 0.9766(3) 0.38422(18) 0.43723(14) 0.080(6) Uani 1 1 d R . . C60 C 0.9084(3) 0.34337(18) 0.42978(14) 0.055(5) Uani 1 1 d R . . C61 C 0.8912(3) 0.29727(18) 0.46502(14) 0.083(6) Uani 1 1 d R . . H61 H 0.8456 0.2699 0.4600 0.100 Uiso 1 1 calc R . . C62 C 0.9423(3) 0.29202(18) 0.50772(14) 0.120(8) Uani 1 1 d R . . H62 H 0.9308 0.2612 0.5313 0.144 Uiso 1 1 calc R . . C63 C 1.0105(3) 0.33287(18) 0.51517(14) 0.127(10) Uani 1 1 d R . . H63 H 1.0446 0.3294 0.5437 0.152 Uiso 1 1 calc R . . C64 C 1.0276(3) 0.37897(18) 0.47992(14) 0.129(9) Uani 1 1 d R . . H64 H 1.0733 0.4063 0.4849 0.155 Uiso 1 1 calc R . . C65 C 0.7786(3) 0.30511(18) 0.37138(14) 0.048(4) Uani 1 1 d R . . C66 C 0.7977(3) 0.24330(18) 0.36071(14) 0.072(6) Uani 1 1 d R . . C67 C 0.7315(3) 0.20050(18) 0.35418(14) 0.101(7) Uani 1 1 d R . . H67 H 0.7443 0.1591 0.3470 0.121 Uiso 1 1 calc R . . C68 C 0.6463(3) 0.21950(18) 0.35831(14) 0.076(6) Uani 1 1 d R . . H68 H 0.6020 0.1909 0.3539 0.091 Uiso 1 1 calc R . . C69 C 0.6272(3) 0.28131(18) 0.36898(14) 0.059(5) Uani 1 1 d R . . C70 C 0.6933(3) 0.32411(18) 0.37552(14) 0.065(5) Uani 1 1 d R . . C71 C 0.6742(3) 0.38591(18) 0.38619(14) 0.067(5) Uani 1 1 d R . . H71 H 0.7185 0.4145 0.3906 0.080 Uiso 1 1 calc R . . C72 C 0.5890(3) 0.40492(18) 0.39032(14) 0.092(7) Uani 1 1 d R . . H72 H 0.5762 0.4463 0.3975 0.111 Uiso 1 1 calc R . . C73 C 0.5228(3) 0.36212(18) 0.38379(14) 0.089(7) Uani 1 1 d R . . H73 H 0.4658 0.3748 0.3866 0.107 Uiso 1 1 calc R . . C74 C 0.5419(3) 0.30031(18) 0.37312(14) 0.088(6) Uani 1 1 d R . . H74 H 0.4976 0.2717 0.3687 0.106 Uiso 1 1 calc R . . O1W O 0.8791(6) 0.5971(4) 0.2981(4) 0.075(3) Uani 1 1 d . . . O2W O 0.8732(6) 0.4927(4) 0.2386(4) 0.073(3) Uani 1 1 d . . . Cl1 Cl 0.4520(6) 0.3871(4) 0.1057(3) 0.138(4) Uani 0.828(12) 1 d PD A 1 Cl2 Cl 0.4478(6) 0.5194(3) 0.0982(3) 0.131(4) Uani 0.828(12) 1 d PD A 1 Cl3 Cl 0.3372(4) 0.4539(5) 0.1718(4) 0.183(5) Uani 0.828(12) 1 d PD A 1 C1CL C 0.4345(10) 0.4565(6) 0.1399(6) 0.098(7) Uiso 0.828(12) 1 d PD A 1 H1CL H 0.4802 0.4595 0.1652 0.118 Uiso 0.828(12) 1 calc PR A 1 Cl12 Cl 0.408(6) 0.3775(15) 0.139(4) 0.30(5) Uiso 0.172(12) 1 d PD A 2 Cl22 Cl 0.364(3) 0.5154(17) 0.1192(19) 0.17(2) Uiso 0.172(12) 1 d PD A 2 C12L C 0.4345(10) 0.4565(6) 0.1399(6) 0.098(7) Uiso 0.17 1 d PD A 2 H12A H 0.4870 0.4609 0.1205 0.118 Uiso 0.172(12) 1 calc PR A 2 H12B H 0.4492 0.4663 0.1744 0.118 Uiso 0.172(12) 1 calc PR A 2 Cl4 Cl 0.8604(18) 0.2608(14) 0.0274(11) 0.43(2) Uani 0.616(16) 1 d PD B 1 Cl5 Cl 0.696(2) 0.2028(16) 0.0594(9) 0.48(2) Uani 0.616(16) 1 d PD B 1 Cl6 Cl 0.8188(19) 0.1416(19) -0.0019(11) 0.76(5) Uani 0.616(16) 1 d PD B 1 C2CL C 0.7728(18) 0.2134(15) 0.0119(13) 0.19(2) Uiso 0.616(16) 1 d PD B 1 H2CL H 0.7445 0.2298 -0.0182 0.225 Uiso 0.616(16) 1 calc PR B 1 Cl7 Cl 0.546(2) 0.2153(15) 0.0587(9) 0.254(17) Uani 0.384(16) 1 d PD B 2 Cl8 Cl 0.482(2) 0.1080(15) 0.0092(10) 0.29(2) Uani 0.384(16) 1 d PD B 2 C3CL C 0.475(6) 0.1891(18) 0.012(4) 0.31(6) Uiso 0.384(16) 1 d PD B 2 H3C1 H 0.4901 0.2071 -0.0199 0.377 Uiso 0.384(16) 1 calc PR B 2 H3C2 H 0.4164 0.2015 0.0204 0.377 Uiso 0.384(16) 1 calc PR B 2 C1S C 0.741(3) 0.8810(18) 0.1188(16) 0.278(19) Uiso 1 1 d D . . C2S C 0.725(3) 0.8644(18) 0.0646(17) 0.29(2) Uiso 1 1 d D . . O3S O 0.718(3) 0.9190(18) 0.0335(16) 0.43(2) Uiso 1 1 d D . . C4S C 0.713(4) 0.898(2) -0.0194(17) 0.43(4) Uiso 1 1 d D . . C5S C 0.706(3) 0.956(2) -0.0516(16) 0.30(2) Uiso 1 1 d 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 0.094(2) 0.0644(17) 0.0578(19) 0.0107(16) -0.0028(15) -0.0158(14) Fe2 0.0719(17) 0.0466(15) 0.0748(19) 0.0024(16) 0.0081(14) -0.0013(12) Fe3 0.0525(15) 0.0716(18) 0.0691(19) -0.0101(16) -0.0041(13) 0.0086(12) N1 0.062(9) 0.030(8) 0.087(13) -0.034(9) 0.010(8) -0.014(6) N2 0.067(10) 0.041(9) 0.089(13) -0.010(9) 0.018(8) 0.002(7) N3 0.075(11) 0.084(12) 0.064(11) 0.020(10) -0.011(9) -0.006(9) N4 0.059(10) 0.079(11) 0.050(11) 0.010(9) -0.013(8) 0.001(8) N5 0.059(9) 0.051(9) 0.068(11) -0.020(9) -0.005(8) 0.016(7) N6 0.073(11) 0.099(13) 0.062(12) 0.012(10) 0.001(8) -0.022(9) C1 0.047(12) 0.062(13) 0.104(19) 0.000(14) -0.012(11) 0.007(9) C2 0.073(13) 0.107(16) 0.052(15) -0.020(14) 0.018(10) -0.024(12) C3 0.085(14) 0.120(18) 0.051(15) -0.003(13) -0.017(11) -0.056(13) C4 0.100(15) 0.122(19) 0.040(14) 0.023(13) 0.022(11) -0.014(14) C5 0.086(14) 0.078(15) 0.097(19) -0.014(15) 0.014(12) -0.026(11) C6 0.060(12) 0.065(13) 0.057(13) 0.014(12) -0.005(10) -0.016(10) C7 0.074(13) 0.091(16) 0.075(16) 0.004(14) -0.006(10) 0.014(12) C8 0.19(2) 0.036(12) 0.13(2) 0.028(14) -0.063(19) -0.030(14) C9 0.105(16) 0.066(15) 0.10(2) -0.007(14) -0.022(13) 0.019(11) C10 0.091(14) 0.038(11) 0.078(15) 0.022(11) 0.015(11) 0.013(10) C11 0.054(12) 0.094(16) 0.084(15) -0.004(13) 0.042(11) 0.015(11) C12 0.116(16) 0.047(10) 0.035(11) 0.002(10) -0.005(11) 0.030(10) C13 0.080(13) 0.055(12) 0.088(16) 0.005(12) -0.007(11) -0.015(11) C14 0.089(15) 0.060(13) 0.103(17) 0.026(13) -0.004(12) 0.022(12) C15 0.143(19) 0.050(12) 0.062(14) 0.019(12) 0.029(12) 0.009(12) C16 0.086(15) 0.034(11) 0.063(14) -0.029(10) 0.019(10) -0.018(10) C17 0.084(13) 0.074(13) 0.052(12) -0.011(11) 0.018(10) 0.009(12) C18 0.079(16) 0.071(14) 0.096(17) 0.003(13) 0.003(12) -0.008(12) C19 0.064(15) 0.076(16) 0.105(17) -0.021(13) -0.009(12) -0.018(11) C20 0.050(11) 0.050(12) 0.123(18) -0.011(13) 0.004(11) -0.009(9) C21 0.047(10) 0.046(10) 0.086(16) 0.004(11) 0.004(11) 0.003(8) C22 0.067(13) 0.070(14) 0.13(2) -0.012(14) 0.011(13) 0.016(10) C23 0.107(17) 0.093(16) 0.041(14) 0.013(12) -0.036(12) -0.005(13) C24 0.077(14) 0.098(15) 0.080(16) -0.011(14) 0.029(13) 0.043(12) C25 0.050(11) 0.091(14) 0.052(13) -0.034(13) 0.008(9) 0.021(10) C26 0.077(14) 0.098(16) 0.055(15) 0.002(14) -0.002(12) -0.006(11) C27 0.050(11) 0.068(12) 0.087(16) -0.009(13) -0.029(11) -0.007(9) C28 0.065(12) 0.066(13) 0.094(18) -0.003(13) 0.012(11) 0.004(10) C29 0.039(11) 0.118(17) 0.079(17) -0.029(14) 0.015(10) 0.021(11) C30 0.092(17) 0.127(19) 0.061(17) -0.008(14) 0.001(12) 0.005(14) C31 0.080(14) 0.079(14) 0.060(15) 0.016(12) -0.019(10) -0.018(11) C32 0.050(11) 0.049(11) 0.107(17) -0.036(12) 0.017(10) -0.010(9) C33 0.096(14) 0.110(16) 0.019(11) -0.005(10) -0.022(9) -0.005(12) C34 0.071(14) 0.109(17) 0.100(18) -0.013(15) -0.018(11) 0.016(12) C35 0.075(13) 0.101(16) 0.090(18) 0.000(15) -0.009(11) -0.015(11) C36 0.074(13) 0.065(12) 0.066(16) 0.025(11) -0.004(10) 0.007(9) C37 0.058(13) 0.058(12) 0.069(15) -0.009(11) 0.015(10) 0.004(9) C38 0.054(13) 0.127(19) 0.055(14) -0.021(14) 0.009(9) -0.008(13) C39 0.070(13) 0.052(12) 0.086(15) 0.025(11) 0.010(10) 0.000(9) C40 0.045(11) 0.058(12) 0.118(19) -0.018(13) 0.012(11) -0.006(9) C41 0.079(14) 0.046(12) 0.15(2) -0.039(14) -0.002(13) -0.018(10) C42 0.12(2) 0.121(19) 0.11(2) 0.064(17) -0.054(16) -0.050(16) C43 0.16(2) 0.074(15) 0.096(18) 0.039(14) -0.014(16) -0.001(14) C44 0.073(13) 0.135(19) 0.048(13) 0.036(13) -0.015(9) -0.001(12) C45 0.067(13) 0.086(16) 0.049(13) -0.028(12) -0.003(10) -0.009(10) C46 0.046(11) 0.111(16) 0.032(12) -0.007(11) -0.013(9) 0.002(10) C47 0.057(11) 0.071(12) 0.066(14) 0.003(12) 0.005(10) -0.013(10) C48 0.046(11) 0.070(13) 0.093(17) 0.001(12) -0.005(10) -0.010(10) C49 0.057(12) 0.088(15) 0.113(18) -0.038(14) 0.018(10) -0.010(12) C50 0.088(17) 0.100(19) 0.14(2) -0.010(16) -0.004(15) 0.024(14) C51 0.065(14) 0.055(13) 0.23(3) 0.002(18) 0.023(16) -0.013(11) C52 0.082(13) 0.057(12) 0.118(16) -0.001(12) 0.007(12) -0.035(11) C53 0.053(11) 0.049(11) 0.090(17) 0.011(12) 0.007(11) -0.002(9) C54 0.050(12) 0.100(17) 0.076(17) -0.049(14) 0.019(11) -0.014(11) O1 0.073(8) 0.078(8) 0.078(9) 0.035(7) -0.009(7) -0.011(6) O2 0.075(8) 0.064(8) 0.097(10) -0.009(7) -0.009(7) 0.001(6) C55 0.060(11) 0.049(10) 0.068(13) 0.020(10) 0.007(9) 0.014(9) C56 0.050(11) 0.049(11) 0.071(14) -0.003(10) -0.018(10) -0.009(8) C57 0.059(13) 0.068(13) 0.086(16) -0.002(12) -0.004(10) -0.004(10) C58 0.073(15) 0.094(17) 0.17(3) -0.053(18) 0.011(16) -0.028(12) C59 0.064(14) 0.085(15) 0.090(17) -0.010(13) -0.035(11) 0.014(11) C60 0.091(13) 0.051(11) 0.025(10) -0.002(9) -0.027(9) 0.031(10) C61 0.111(15) 0.086(14) 0.053(14) 0.000(12) -0.025(12) 0.024(12) C62 0.119(19) 0.17(2) 0.076(17) 0.048(17) -0.011(14) 0.048(16) C63 0.069(16) 0.24(3) 0.070(18) -0.041(19) -0.035(13) 0.025(17) C64 0.14(2) 0.15(2) 0.10(2) 0.022(18) -0.013(16) -0.008(18) C65 0.077(12) 0.043(10) 0.025(11) 0.005(8) -0.010(8) 0.011(9) C66 0.078(14) 0.052(12) 0.088(16) 0.025(12) 0.031(11) -0.001(10) C67 0.136(19) 0.052(12) 0.115(19) 0.012(13) 0.053(16) -0.012(13) C68 0.062(12) 0.099(15) 0.065(14) -0.001(12) 0.004(10) -0.036(11) C69 0.036(10) 0.041(10) 0.099(15) 0.001(11) 0.028(9) -0.006(8) C70 0.055(12) 0.049(11) 0.090(15) 0.028(11) -0.004(10) 0.031(9) C71 0.049(11) 0.092(14) 0.060(12) 0.013(12) -0.008(9) 0.020(10) C72 0.065(14) 0.131(18) 0.081(15) -0.028(13) 0.011(11) 0.047(12) C73 0.055(13) 0.15(2) 0.059(14) -0.007(14) 0.008(9) 0.039(13) C74 0.083(14) 0.117(17) 0.065(15) -0.006(13) 0.031(11) -0.013(13) O1W 0.074(7) 0.065(7) 0.085(9) -0.019(7) 0.012(6) 0.006(6) O2W 0.076(7) 0.058(7) 0.084(9) 0.014(7) -0.004(7) -0.002(6) Cl1 0.188(9) 0.117(6) 0.109(7) -0.030(6) -0.002(6) 0.000(5) Cl2 0.162(8) 0.123(6) 0.107(6) 0.019(5) 0.011(6) -0.001(5) Cl3 0.075(5) 0.280(12) 0.194(10) -0.069(9) 0.048(5) -0.054(6) Cl4 0.45(4) 0.42(3) 0.44(4) 0.11(3) -0.29(3) 0.01(3) Cl5 0.57(5) 0.60(5) 0.26(3) 0.24(3) 0.09(3) 0.05(4) Cl6 0.50(5) 1.45(14) 0.35(4) -0.39(6) -0.12(3) 0.61(7) Cl7 0.30(3) 0.31(3) 0.16(2) 0.13(2) 0.03(2) -0.04(3) Cl8 0.46(5) 0.25(3) 0.15(2) -0.08(2) 0.10(2) -0.09(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 C8 1.98(2) . ? Fe1 C5 2.029(16) . ? Fe1 C1 2.037(15) . ? Fe1 C2 2.045(19) . ? Fe1 C7 2.053(16) . ? Fe1 C10 2.061(17) . ? Fe1 C6 2.070(16) . ? Fe1 C4 2.088(16) . ? Fe1 C9 2.095(19) . ? Fe1 C3 2.15(2) . ? Fe2 C20 2.017(17) . ? Fe2 C17 2.054(16) . ? Fe2 C18 2.061(18) . ? Fe2 C19 2.062(17) . ? Fe2 C13 2.065(17) . ? Fe2 C11 2.070(18) . ? Fe2 C16 2.084(19) . ? Fe2 C12 2.087(16) . ? Fe2 C14 2.096(17) . ? Fe2 C15 2.111(17) . ? Fe3 C28 2.019(16) . ? Fe3 C22 2.025(18) . ? Fe3 C25 2.038(14) . ? Fe3 C24 2.053(18) . ? Fe3 C23 2.058(18) . ? Fe3 C30 2.06(2) . ? Fe3 C27 2.065(15) . ? Fe3 C21 2.067(16) . ? Fe3 C26 2.078(19) . ? Fe3 C29 2.108(16) . ? N1 C37 1.267(17) . ? N1 C31 1.53(2) . ? N2 C38 1.30(2) . ? N2 C32 1.464(18) . ? N3 C45 1.303(18) . ? N3 C39 1.476(19) . ? N4 C46 1.262(17) . ? N4 C40 1.52(2) . ? N5 C53 1.284(19) . ? N5 C47 1.445(18) . ? N6 C54 1.262(15) . ? N6 C48 1.492(19) . ? C1 C5 1.42(2) . ? C1 C2 1.47(2) . ? C1 C37 1.53(2) . ? C2 C3 1.43(2) . ? C3 C4 1.49(2) . ? C4 C5 1.51(2) . ? C6 C10 1.44(2) . ? C6 C7 1.45(2) . ? C6 C54 1.562(17) . ? C7 C8 1.41(2) . ? C8 C9 1.45(3) . ? C9 C10 1.42(2) . ? C11 C38 1.44(2) . ? C11 C15 1.47(2) . ? C11 C12 1.47(2) . ? C12 C13 1.453(19) . ? C13 C14 1.48(2) . ? C14 C15 1.41(2) . ? C16 C17 1.41(2) . ? C16 C20 1.44(2) . ? C16 C45 1.49(2) . ? C17 C18 1.40(2) . ? C18 C19 1.39(2) . ? C19 C20 1.41(2) . ? C21 C25 1.45(2) . ? C21 C22 1.46(2) . ? C21 C46 1.54(2) . ? C22 C23 1.40(2) . ? C23 C24 1.40(2) . ? C24 C25 1.42(2) . ? C26 C30 1.45(2) . ? C26 C27 1.46(2) . ? C26 C53 1.52(2) . ? C27 C28 1.43(2) . ? C28 C29 1.44(2) . ? C29 C30 1.40(2) . ? C31 C32 1.54(2) . ? C31 C36 1.56(2) . ? C32 C33 1.54(2) . ? C33 C34 1.51(2) . ? C34 C35 1.59(2) . ? C35 C36 1.61(2) . ? C39 C44 1.54(2) . ? C39 C40 1.558(19) . ? C40 C41 1.56(2) . ? C41 C42 1.55(2) . ? C42 C43 1.48(2) . ? C43 C44 1.60(2) . ? C47 C48 1.58(2) . ? C47 C52 1.594(19) . ? C48 C49 1.50(2) . ? C49 C50 1.60(2) . ? C50 C51 1.49(3) . ? C51 C52 1.55(2) . ? O1 C56 1.4476 . ? O2 C66 1.4013 . ? C55 C60 1.3900 . ? C55 C56 1.3900 . ? C55 C65 1.5953 . ? C56 C57 1.3900 . ? C57 C58 1.3900 . ? C58 C59 1.3899 . ? C59 C64 1.3900 . ? C59 C60 1.3900 . ? C60 C61 1.3900 . ? C61 C62 1.3899 . ? C62 C63 1.3900 . ? C63 C64 1.3899 . ? C65 C66 1.3900 . ? C65 C70 1.3900 . ? C66 C67 1.3900 . ? C67 C68 1.3899 . ? C68 C69 1.3900 . ? C69 C74 1.3900 . ? C69 C70 1.3900 . ? C70 C71 1.3900 . ? C71 C72 1.3900 . ? C72 C73 1.3900 . ? C73 C74 1.3900 . ? Cl1 C1CL 1.767(13) . ? Cl2 C1CL 1.761(13) . ? Cl3 C1CL 1.734(12) . ? Cl4 C2CL 1.748(15) . ? Cl5 C2CL 1.751(15) . ? Cl6 C2CL 1.739(15) . ? Cl7 C3CL 1.75(2) . ? Cl8 C3CL 1.75(2) . ? C1S C2S 1.507(19) . ? C2S O3S 1.439(19) . ? O3S C4S 1.48(2) . ? C4S C5S 1.51(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 Fe1 C5 115.7(9) . . ? C8 Fe1 C1 149.1(9) . . ? C5 Fe1 C1 40.9(6) . . ? C8 Fe1 C2 167.3(9) . . ? C5 Fe1 C2 70.1(7) . . ? C1 Fe1 C2 42.3(6) . . ? C8 Fe1 C7 40.7(7) . . ? C5 Fe1 C7 151.6(9) . . ? C1 Fe1 C7 167.4(8) . . ? C2 Fe1 C7 129.6(8) . . ? C8 Fe1 C10 68.3(9) . . ? C5 Fe1 C10 124.6(8) . . ? C1 Fe1 C10 106.1(8) . . ? C2 Fe1 C10 118.8(7) . . ? C7 Fe1 C10 68.2(7) . . ? C8 Fe1 C6 69.5(8) . . ? C5 Fe1 C6 163.6(8) . . ? C1 Fe1 C6 127.2(8) . . ? C2 Fe1 C6 108.3(7) . . ? C7 Fe1 C6 41.3(6) . . ? C10 Fe1 C6 40.9(6) . . ? C8 Fe1 C4 108.0(9) . . ? C5 Fe1 C4 43.1(7) . . ? C1 Fe1 C4 69.5(8) . . ? C2 Fe1 C4 67.9(8) . . ? C7 Fe1 C4 118.9(8) . . ? C10 Fe1 C4 165.4(8) . . ? C6 Fe1 C4 152.6(8) . . ? C8 Fe1 C9 41.5(7) . . ? C5 Fe1 C9 103.7(8) . . ? C1 Fe1 C9 114.4(8) . . ? C2 Fe1 C9 150.5(8) . . ? C7 Fe1 C9 69.0(7) . . ? C10 Fe1 C9 40.1(6) . . ? C6 Fe1 C9 69.3(7) . . ? C4 Fe1 C9 127.9(9) . . ? C8 Fe1 C3 129.4(10) . . ? C5 Fe1 C3 71.6(7) . . ? C1 Fe1 C3 70.0(8) . . ? C2 Fe1 C3 39.7(6) . . ? C7 Fe1 C3 109.5(7) . . ? C10 Fe1 C3 151.8(8) . . ? C6 Fe1 C3 118.3(7) . . ? C4 Fe1 C3 41.2(6) . . ? C9 Fe1 C3 167.6(9) . . ? C20 Fe2 C17 68.5(7) . . ? C20 Fe2 C18 68.4(7) . . ? C17 Fe2 C18 39.9(6) . . ? C20 Fe2 C19 40.6(6) . . ? C17 Fe2 C19 66.3(8) . . ? C18 Fe2 C19 39.3(6) . . ? C20 Fe2 C13 163.4(7) . . ? C17 Fe2 C13 108.9(8) . . ? C18 Fe2 C13 120.9(8) . . ? C19 Fe2 C13 154.9(8) . . ? C20 Fe2 C11 104.6(8) . . ? C17 Fe2 C11 153.3(8) . . ? C18 Fe2 C11 163.4(8) . . ? C19 Fe2 C11 126.0(8) . . ? C13 Fe2 C11 69.9(7) . . ? C20 Fe2 C16 41.1(6) . . ? C17 Fe2 C16 39.8(6) . . ? C18 Fe2 C16 67.1(7) . . ? C19 Fe2 C16 66.7(7) . . ? C13 Fe2 C16 126.6(7) . . ? C11 Fe2 C16 118.2(8) . . ? C20 Fe2 C12 124.9(7) . . ? C17 Fe2 C12 120.0(7) . . ? C18 Fe2 C12 154.7(8) . . ? C19 Fe2 C12 163.5(8) . . ? C13 Fe2 C12 41.0(5) . . ? C11 Fe2 C12 41.5(6) . . ? C16 Fe2 C12 107.5(6) . . ? C20 Fe2 C14 152.6(8) . . ? C17 Fe2 C14 128.4(8) . . ? C18 Fe2 C14 109.5(8) . . ? C19 Fe2 C14 120.4(8) . . ? C13 Fe2 C14 41.6(6) . . ? C11 Fe2 C14 69.4(7) . . ? C16 Fe2 C14 165.2(8) . . ? C12 Fe2 C14 69.1(7) . . ? C20 Fe2 C15 119.3(8) . . ? C17 Fe2 C15 164.7(8) . . ? C18 Fe2 C15 127.9(7) . . ? C19 Fe2 C15 110.2(8) . . ? C13 Fe2 C15 67.4(8) . . ? C11 Fe2 C15 41.1(6) . . ? C16 Fe2 C15 154.3(8) . . ? C12 Fe2 C15 67.8(7) . . ? C14 Fe2 C15 39.1(6) . . ? C28 Fe3 C22 121.7(7) . . ? C28 Fe3 C25 159.0(8) . . ? C22 Fe3 C25 68.8(7) . . ? C28 Fe3 C24 122.8(9) . . ? C22 Fe3 C24 68.0(8) . . ? C25 Fe3 C24 40.6(6) . . ? C28 Fe3 C23 107.5(7) . . ? C22 Fe3 C23 40.2(6) . . ? C25 Fe3 C23 67.8(7) . . ? C24 Fe3 C23 39.8(6) . . ? C28 Fe3 C30 67.4(7) . . ? C22 Fe3 C30 125.3(9) . . ? C25 Fe3 C30 123.7(8) . . ? C24 Fe3 C30 158.7(8) . . ? C23 Fe3 C30 160.8(9) . . ? C28 Fe3 C27 41.1(6) . . ? C22 Fe3 C27 156.1(8) . . ? C25 Fe3 C27 122.1(7) . . ? C24 Fe3 C27 105.5(8) . . ? C23 Fe3 C27 120.2(7) . . ? C30 Fe3 C27 69.0(7) . . ? C28 Fe3 C21 158.2(8) . . ? C22 Fe3 C21 41.7(6) . . ? C25 Fe3 C21 41.3(6) . . ? C24 Fe3 C21 69.1(8) . . ? C23 Fe3 C21 68.9(7) . . ? C30 Fe3 C21 108.5(8) . . ? C27 Fe3 C21 159.7(7) . . ? C28 Fe3 C26 68.3(7) . . ? C22 Fe3 C26 161.9(9) . . ? C25 Fe3 C26 107.3(7) . . ? C24 Fe3 C26 121.4(8) . . ? C23 Fe3 C26 156.3(9) . . ? C30 Fe3 C26 41.0(7) . . ? C27 Fe3 C26 41.2(6) . . ? C21 Fe3 C26 123.7(7) . . ? C28 Fe3 C29 40.8(6) . . ? C22 Fe3 C29 108.5(7) . . ? C25 Fe3 C29 158.6(8) . . ? C24 Fe3 C29 159.8(8) . . ? C23 Fe3 C29 124.8(9) . . ? C30 Fe3 C29 39.3(6) . . ? C27 Fe3 C29 69.3(7) . . ? C21 Fe3 C29 122.4(8) . . ? C26 Fe3 C29 68.2(7) . . ? C37 N1 C31 117.2(14) . . ? C38 N2 C32 118.5(14) . . ? C45 N3 C39 119.1(15) . . ? C46 N4 C40 114.7(14) . . ? C53 N5 C47 115.3(14) . . ? C54 N6 C48 113.0(13) . . ? C5 C1 C2 108.0(17) . . ? C5 C1 C37 127.3(18) . . ? C2 C1 C37 124.2(19) . . ? C5 C1 Fe1 69.2(9) . . ? C2 C1 Fe1 69.2(9) . . ? C37 C1 Fe1 121.1(12) . . ? C3 C2 C1 112.0(18) . . ? C3 C2 Fe1 74.1(12) . . ? C1 C2 Fe1 68.6(9) . . ? C2 C3 C4 104.4(16) . . ? C2 C3 Fe1 66.2(11) . . ? C4 C3 Fe1 67.2(10) . . ? C3 C4 C5 109.0(16) . . ? C3 C4 Fe1 71.6(10) . . ? C5 C4 Fe1 66.4(9) . . ? C1 C5 C4 106.5(16) . . ? C1 C5 Fe1 69.9(9) . . ? C4 C5 Fe1 70.5(9) . . ? C10 C6 C7 105.5(14) . . ? C10 C6 C54 125.7(15) . . ? C7 C6 C54 128.8(15) . . ? C10 C6 Fe1 69.2(9) . . ? C7 C6 Fe1 68.8(9) . . ? C54 C6 Fe1 124.7(10) . . ? C8 C7 C6 107.8(17) . . ? C8 C7 Fe1 67.0(11) . . ? C6 C7 Fe1 70.0(9) . . ? C7 C8 C9 110.7(19) . . ? C7 C8 Fe1 72.3(10) . . ? C9 C8 Fe1 73.4(12) . . ? C10 C9 C8 104.4(18) . . ? C10 C9 Fe1 68.7(10) . . ? C8 C9 Fe1 65.1(12) . . ? C9 C10 C6 111.3(17) . . ? C9 C10 Fe1 71.3(11) . . ? C6 C10 Fe1 69.9(10) . . ? C38 C11 C15 132.3(18) . . ? C38 C11 C12 122.4(18) . . ? C15 C11 C12 105.4(15) . . ? C38 C11 Fe2 122.3(13) . . ? C15 C11 Fe2 70.9(10) . . ? C12 C11 Fe2 69.8(9) . . ? C13 C12 C11 108.1(15) . . ? C13 C12 Fe2 68.7(9) . . ? C11 C12 Fe2 68.6(10) . . ? C12 C13 C14 108.1(15) . . ? C12 C13 Fe2 70.3(9) . . ? C14 C13 Fe2 70.3(9) . . ? C15 C14 C13 107.0(15) . . ? C15 C14 Fe2 71.0(10) . . ? C13 C14 Fe2 68.1(10) . . ? C14 C15 C11 111.1(16) . . ? C14 C15 Fe2 69.9(10) . . ? C11 C15 Fe2 68.0(10) . . ? C17 C16 C20 107.1(16) . . ? C17 C16 C45 128.3(17) . . ? C20 C16 C45 123.6(17) . . ? C17 C16 Fe2 69.0(10) . . ? C20 C16 Fe2 67.0(10) . . ? C45 C16 Fe2 120.1(11) . . ? C18 C17 C16 109.0(16) . . ? C18 C17 Fe2 70.3(10) . . ? C16 C17 Fe2 71.2(10) . . ? C19 C18 C17 107.5(17) . . ? C19 C18 Fe2 70.4(11) . . ? C17 C18 Fe2 69.8(10) . . ? C18 C19 C20 110.0(17) . . ? C18 C19 Fe2 70.3(10) . . ? C20 C19 Fe2 68.0(10) . . ? C19 C20 C16 106.0(16) . . ? C19 C20 Fe2 71.4(10) . . ? C16 C20 Fe2 71.9(10) . . ? C25 C21 C22 104.4(17) . . ? C25 C21 C46 129.3(14) . . ? C22 C21 C46 125.9(19) . . ? C25 C21 Fe3 68.3(9) . . ? C22 C21 Fe3 67.6(9) . . ? C46 C21 Fe3 122.6(10) . . ? C23 C22 C21 109.3(18) . . ? C23 C22 Fe3 71.1(12) . . ? C21 C22 Fe3 70.7(10) . . ? C24 C23 C22 108.8(18) . . ? C24 C23 Fe3 69.9(11) . . ? C22 C23 Fe3 68.6(11) . . ? C23 C24 C25 108.3(17) . . ? C23 C24 Fe3 70.3(10) . . ? C25 C24 Fe3 69.1(10) . . ? C24 C25 C21 109.2(14) . . ? C24 C25 Fe3 70.3(9) . . ? C21 C25 Fe3 70.4(8) . . ? C30 C26 C27 107.0(17) . . ? C30 C26 C53 128.5(19) . . ? C27 C26 C53 124.4(19) . . ? C30 C26 Fe3 68.8(11) . . ? C27 C26 Fe3 68.9(10) . . ? C53 C26 Fe3 123.4(11) . . ? C28 C27 C26 105.4(17) . . ? C28 C27 Fe3 67.8(9) . . ? C26 C27 Fe3 69.9(9) . . ? C27 C28 C29 111.3(17) . . ? C27 C28 Fe3 71.2(9) . . ? C29 C28 Fe3 72.9(10) . . ? C30 C29 C28 105.5(16) . . ? C30 C29 Fe3 68.5(10) . . ? C28 C29 Fe3 66.3(10) . . ? C29 C30 C26 110.6(18) . . ? C29 C30 Fe3 72.2(12) . . ? C26 C30 Fe3 70.1(11) . . ? N1 C31 C32 110.3(14) . . ? N1 C31 C36 106.8(14) . . ? C32 C31 C36 111.7(13) . . ? N2 C32 C33 109.2(14) . . ? N2 C32 C31 109.0(13) . . ? C33 C32 C31 113.1(14) . . ? C34 C33 C32 111.4(14) . . ? C33 C34 C35 109.6(14) . . ? C34 C35 C36 113.2(15) . . ? C31 C36 C35 107.1(14) . . ? N1 C37 C1 127.1(17) . . ? N2 C38 C11 128.3(17) . . ? N3 C39 C44 112.1(15) . . ? N3 C39 C40 107.0(13) . . ? C44 C39 C40 110.3(14) . . ? N4 C40 C39 111.4(14) . . ? N4 C40 C41 110.3(15) . . ? C39 C40 C41 109.1(14) . . ? C42 C41 C40 114.1(16) . . ? C43 C42 C41 110.1(16) . . ? C42 C43 C44 112.2(16) . . ? C39 C44 C43 109.5(15) . . ? N3 C45 C16 126.6(16) . . ? N4 C46 C21 119.9(15) . . ? N5 C47 C48 108.6(14) . . ? N5 C47 C52 109.0(12) . . ? C48 C47 C52 107.7(14) . . ? N6 C48 C49 108.2(14) . . ? N6 C48 C47 104.3(14) . . ? C49 C48 C47 111.5(15) . . ? C48 C49 C50 110.5(14) . . ? C51 C50 C49 110.5(18) . . ? C50 C51 C52 111.3(19) . . ? C51 C52 C47 111.6(13) . . ? N5 C53 C26 123.5(17) . . ? N6 C54 C6 125.1(11) . . ? C60 C55 C56 120.0 . . ? C60 C55 C65 127.1 . . ? C56 C55 C65 112.8 . . ? C57 C56 C55 120.0 . . ? C57 C56 O1 115.1 . . ? C55 C56 O1 124.6 . . ? C58 C57 C56 120.0 . . ? C59 C58 C57 120.0 . . ? C58 C59 C64 120.0 . . ? C58 C59 C60 120.0 . . ? C64 C59 C60 120.0 . . ? C59 C60 C61 120.0 . . ? C59 C60 C55 120.0 . . ? C61 C60 C55 120.0 . . ? C62 C61 C60 120.0 . . ? C61 C62 C63 120.0 . . ? C64 C63 C62 120.0 . . ? C63 C64 C59 120.0 . . ? C66 C65 C70 120.0 . . ? C66 C65 C55 116.7 . . ? C70 C65 C55 122.5 . . ? C65 C66 C67 120.0 . . ? C65 C66 O2 120.7 . . ? C67 C66 O2 119.3 . . ? C68 C67 C66 120.0 . . ? C67 C68 C69 120.0 . . ? C68 C69 C74 120.0 . . ? C68 C69 C70 120.0 . . ? C74 C69 C70 120.0 . . ? C71 C70 C69 120.0 . . ? C71 C70 C65 120.0 . . ? C69 C70 C65 120.0 . . ? C72 C71 C70 120.0 . . ? C73 C72 C71 120.0 . . ? C72 C73 C74 120.0 . . ? C69 C74 C73 120.0 . . ? Cl3 C1CL Cl2 115.8(9) . . ? Cl3 C1CL Cl1 111.1(9) . . ? Cl2 C1CL Cl1 107.7(9) . . ? Cl6 C2CL Cl4 104.4(19) . . ? Cl6 C2CL Cl5 108.4(19) . . ? Cl4 C2CL Cl5 116(2) . . ? Cl7 C3CL Cl8 108(3) . . ? O3S C2S C1S 112(3) . . ? C2S O3S C4S 108(3) . . ? O3S C4S C5S 107(3) . . ? _diffrn_measured_fraction_theta_max 0.768 _diffrn_reflns_theta_full 24.89 _diffrn_measured_fraction_theta_full 0.768 _refine_diff_density_max 0.284 _refine_diff_density_min -0.272 _refine_diff_density_rms 0.066 #========================================================================END data_(R)3-(R)4' _database_code_depnum_ccdc_archive 'CCDC 227312' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H80 Cl2 Fe3 N6 O4' _chemical_formula_weight 1367.90 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 13.5860(10) _cell_length_b 20.4300(10) _cell_length_c 25.7270(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7140.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8552 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2864 _exptl_absorpt_coefficient_mu 0.727 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15803 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 27.48 _reflns_number_total 15803 _reflns_number_gt 10149 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0503P)^2^+2.4944P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.013(14) _refine_ls_number_reflns 15803 _refine_ls_number_parameters 842 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1039 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1273 _refine_ls_wR_factor_gt 0.1087 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.011 _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 0.07867(4) 0.27958(3) 0.36057(2) 0.05318(14) Uani 1 1 d . . . Fe2 Fe 0.39768(4) 0.34164(3) 0.12947(2) 0.06504(17) Uani 1 1 d . . . Fe3 Fe 0.55640(5) 0.17784(3) 0.37553(2) 0.06171(17) Uani 1 1 d . . . N1 N 0.0357(2) 0.44146(16) 0.28026(12) 0.0564(8) Uani 1 1 d . . . N2 N 0.1997(2) 0.42633(15) 0.20935(12) 0.0530(8) Uani 1 1 d . . . N3 N 0.6222(3) 0.41063(17) 0.20770(14) 0.0656(9) Uani 1 1 d . . . N4 N 0.6071(2) 0.34150(17) 0.30591(12) 0.0590(8) Uani 1 1 d . . . N5 N 0.4834(2) 0.31583(15) 0.47868(11) 0.0545(8) Uani 1 1 d . . . N6 N 0.3156(2) 0.35915(15) 0.42331(11) 0.0517(7) Uani 1 1 d . . . O1 O 0.3203(3) 0.78201(17) 0.32379(13) 0.0897(10) Uani 1 1 d . . . O2 O 0.2997(2) 0.59667(14) 0.30447(10) 0.0739(8) Uani 1 1 d . . . C1 C 0.0096(3) 0.36789(18) 0.35075(14) 0.0516(9) Uani 1 1 d . . . C2 C 0.0156(3) 0.3507(2) 0.40501(14) 0.0592(10) Uani 1 1 d . . . H2 H 0.0473 0.3746 0.4308 0.071 Uiso 1 1 calc R . . C3 C -0.0353(3) 0.2912(2) 0.41182(18) 0.0701(12) Uani 1 1 d . . . H3 H -0.0432 0.2690 0.4431 0.084 Uiso 1 1 calc R . . C4 C -0.0717(3) 0.2712(2) 0.36359(19) 0.0707(11) Uani 1 1 d . . . H4 H -0.1079 0.2333 0.3575 0.085 Uiso 1 1 calc R . . C5 C -0.0445(3) 0.3177(2) 0.32551(16) 0.0603(10) Uani 1 1 d . . . H5 H -0.0594 0.3157 0.2903 0.072 Uiso 1 1 calc R . . C6 C 0.0580(3) 0.42364(18) 0.32599(14) 0.0542(9) Uani 1 1 d . . . H6 H 0.1061 0.4465 0.3441 0.065 Uiso 1 1 calc R . . C7 C 0.0897(3) 0.49740(17) 0.25941(13) 0.0515(9) Uani 1 1 d . . . H7 H 0.1454 0.5076 0.2822 0.077 Uiso 1 1 calc R . . C8 C 0.1276(3) 0.47918(18) 0.20537(14) 0.0530(9) Uani 1 1 d . . . H8 H 0.0723 0.4647 0.1838 0.079 Uiso 1 1 calc R . . C9 C 0.1770(3) 0.53727(19) 0.17990(16) 0.0665(12) Uani 1 1 d . . . H9A H 0.2366 0.5478 0.1989 0.100 Uiso 1 1 calc R . . H9B H 0.1959 0.5254 0.1448 0.100 Uiso 1 1 calc R . . C10 C 0.1121(4) 0.5973(2) 0.17792(17) 0.0815(14) Uani 1 1 d . . . H10A H 0.0563 0.5890 0.1553 0.122 Uiso 1 1 calc R . . H10B H 0.1489 0.6338 0.1637 0.122 Uiso 1 1 calc R . . C11 C 0.0754(4) 0.61478(19) 0.23216(15) 0.0707(12) Uani 1 1 d . . . H11A H 0.1308 0.6264 0.2541 0.106 Uiso 1 1 calc R . . H11B H 0.0318 0.6523 0.2301 0.106 Uiso 1 1 calc R . . C12 C 0.0207(3) 0.5572(2) 0.25591(16) 0.0667(11) Uani 1 1 d . . . H12A H -0.0361 0.5465 0.2347 0.100 Uiso 1 1 calc R . . H12B H -0.0025 0.5688 0.2904 0.100 Uiso 1 1 calc R . . C13 C 0.1985(3) 0.38193(19) 0.17542(16) 0.0583(10) Uani 1 1 d . . . H13 H 0.1474 0.3826 0.1514 0.070 Uiso 1 1 calc R . . C14 C 0.2703(3) 0.3301(2) 0.17093(17) 0.0642(11) Uani 1 1 d . . . C15 C 0.2744(4) 0.2851(2) 0.1281(2) 0.0912(15) Uani 1 1 d . . . H15 H 0.2299 0.2827 0.1007 0.109 Uiso 1 1 calc R . . C16 C 0.3574(5) 0.2455(2) 0.1348(3) 0.1007(18) Uani 1 1 d . . . H16 H 0.3769 0.2120 0.1126 0.121 Uiso 1 1 calc R . . C17 C 0.4063(4) 0.2642(2) 0.1802(2) 0.0847(14) Uani 1 1 d . . . H17 H 0.4634 0.2454 0.1934 0.102 Uiso 1 1 calc R . . C18 C 0.3536(3) 0.3166(2) 0.20239(18) 0.0672(11) Uani 1 1 d . . . H18 H 0.3707 0.3387 0.2327 0.081 Uiso 1 1 calc R . . C19 C 0.5053(3) 0.4109(2) 0.13675(17) 0.0647(11) Uani 1 1 d . . . C20 C 0.5357(4) 0.3591(3) 0.10156(18) 0.0807(14) Uani 1 1 d . . . H20 H 0.5895 0.3316 0.1060 0.097 Uiso 1 1 calc R . . C21 C 0.4705(4) 0.3580(3) 0.06039(19) 0.0992(18) Uani 1 1 d . . . H21 H 0.4746 0.3299 0.0320 0.119 Uiso 1 1 calc R . . C22 C 0.3963(4) 0.4060(3) 0.0677(2) 0.0984(17) Uani 1 1 d . . . H22 H 0.3433 0.4145 0.0458 0.118 Uiso 1 1 calc R . . C23 C 0.4182(3) 0.4383(2) 0.11445(18) 0.0759(12) Uani 1 1 d . . . H23 H 0.3817 0.4723 0.1287 0.091 Uiso 1 1 calc R . . C24 C 0.5430(3) 0.42976(19) 0.18693(17) 0.0593(10) Uani 1 1 d . . . H24 H 0.5051 0.4591 0.2060 0.071 Uiso 1 1 calc R . . C25 C 0.6465(3) 0.4411(2) 0.25781(18) 0.0681(12) Uani 1 1 d . . . H25 H 0.5866 0.4607 0.2722 0.102 Uiso 1 1 calc R . . C26 C 0.6849(3) 0.3906(2) 0.29635(17) 0.0695(12) Uani 1 1 d . . . H26 H 0.7431 0.3689 0.2818 0.104 Uiso 1 1 calc R . . C27 C 0.7113(4) 0.4222(3) 0.34785(19) 0.0850(14) Uani 1 1 d . . . H27A H 0.7399 0.3896 0.3707 0.127 Uiso 1 1 calc R . . H27B H 0.6520 0.4388 0.3642 0.127 Uiso 1 1 calc R . . C28 C 0.7843(4) 0.4784(3) 0.3406(2) 0.1072(19) Uani 1 1 d . . . H28A H 0.7951 0.4998 0.3738 0.161 Uiso 1 1 calc R . . H28B H 0.8469 0.4609 0.3289 0.161 Uiso 1 1 calc R . . C29 C 0.7476(4) 0.5281(3) 0.3016(3) 0.1019(18) Uani 1 1 d . . . H29A H 0.7978 0.5612 0.2960 0.153 Uiso 1 1 calc R . . H29B H 0.6894 0.5496 0.3152 0.153 Uiso 1 1 calc R . . C30 C 0.7231(4) 0.4953(2) 0.2503(2) 0.0886(15) Uani 1 1 d . . . H30A H 0.7825 0.4767 0.2355 0.133 Uiso 1 1 calc R . . H30B H 0.6978 0.5276 0.2262 0.133 Uiso 1 1 calc R . . C31 C 0.6285(3) 0.2820(2) 0.29875(14) 0.0631(11) Uani 1 1 d . . . H31 H 0.6916 0.2718 0.2874 0.076 Uiso 1 1 calc R . . C32 C 0.5599(3) 0.22893(19) 0.30733(14) 0.0602(10) Uani 1 1 d . . . C33 C 0.5798(4) 0.1609(2) 0.29819(16) 0.0802(14) Uani 1 1 d . . . H33 H 0.6371 0.1441 0.2836 0.096 Uiso 1 1 calc R . . C34 C 0.4989(5) 0.1243(3) 0.3148(2) 0.0949(17) Uani 1 1 d . . . H34 H 0.4933 0.0790 0.3132 0.114 Uiso 1 1 calc R . . C35 C 0.4268(4) 0.1678(2) 0.33450(19) 0.0814(13) Uani 1 1 d . . . H35 H 0.3659 0.1560 0.3481 0.098 Uiso 1 1 calc R . . C36 C 0.4633(3) 0.2318(2) 0.32994(16) 0.0641(11) Uani 1 1 d . . . H36 H 0.4304 0.2697 0.3399 0.077 Uiso 1 1 calc R . . C37 C 0.5811(3) 0.2294(2) 0.44231(14) 0.0618(10) Uani 1 1 d . . . C38 C 0.5245(4) 0.1729(2) 0.45303(15) 0.0766(13) Uani 1 1 d . . . H38 H 0.4618 0.1723 0.4675 0.092 Uiso 1 1 calc R . . C39 C 0.5796(5) 0.1177(2) 0.43799(17) 0.0892(17) Uani 1 1 d . . . H39 H 0.5597 0.0743 0.4411 0.107 Uiso 1 1 calc R . . C40 C 0.6693(5) 0.1391(3) 0.41767(18) 0.0940(18) Uani 1 1 d . . . H40 H 0.7191 0.1125 0.4047 0.113 Uiso 1 1 calc R . . C41 C 0.6717(4) 0.2085(3) 0.42016(17) 0.0782(13) Uani 1 1 d . . . H41 H 0.7230 0.2353 0.4093 0.094 Uiso 1 1 calc R . . C42 C 0.5502(3) 0.29784(19) 0.44808(14) 0.0567(10) Uani 1 1 d . . . H42 H 0.5817 0.3295 0.4281 0.068 Uiso 1 1 calc R . . C43 C 0.4569(3) 0.38541(17) 0.47826(13) 0.0491(9) Uani 1 1 d . . . H43 H 0.4906 0.4076 0.4495 0.074 Uiso 1 1 calc R . . C44 C 0.3459(3) 0.39171(18) 0.47159(15) 0.0534(9) Uani 1 1 d . . . H44 H 0.3130 0.3706 0.5011 0.080 Uiso 1 1 calc R . . C45 C 0.3172(3) 0.4634(2) 0.47014(17) 0.0706(12) Uani 1 1 d . . . H45A H 0.2466 0.4670 0.4654 0.106 Uiso 1 1 calc R . . H45B H 0.3489 0.4842 0.4407 0.106 Uiso 1 1 calc R . . C46 C 0.3467(4) 0.4989(2) 0.5198(2) 0.0867(15) Uani 1 1 d . . . H46A H 0.3082 0.4822 0.5487 0.130 Uiso 1 1 calc R . . H46B H 0.3327 0.5452 0.5162 0.130 Uiso 1 1 calc R . . C47 C 0.4568(4) 0.4892(2) 0.53106(18) 0.0779(14) Uani 1 1 d . . . H47A H 0.4950 0.5127 0.5052 0.117 Uiso 1 1 calc R . . H47B H 0.4721 0.5076 0.5648 0.117 Uiso 1 1 calc R . . C48 C 0.4865(4) 0.4173(2) 0.53042(16) 0.0726(12) Uani 1 1 d . . . H48A H 0.4544 0.3945 0.5588 0.109 Uiso 1 1 calc R . . H48B H 0.5571 0.4136 0.5352 0.109 Uiso 1 1 calc R . . C49 C 0.2598(3) 0.31035(19) 0.42795(15) 0.0549(9) Uani 1 1 d . . . H49 H 0.2422 0.2976 0.4614 0.066 Uiso 1 1 calc R . . C50 C 0.2209(3) 0.2723(2) 0.38451(15) 0.0579(10) Uani 1 1 d . . . C51 C 0.2179(3) 0.2900(2) 0.33094(16) 0.0625(11) Uani 1 1 d . . . H51 H 0.2444 0.3276 0.3162 0.075 Uiso 1 1 calc R . . C52 C 0.1669(3) 0.2396(3) 0.30412(19) 0.0747(13) Uani 1 1 d . . . H52 H 0.1536 0.2387 0.2687 0.090 Uiso 1 1 calc R . . C53 C 0.1396(3) 0.1907(2) 0.3405(2) 0.0808(14) Uani 1 1 d . . . H53 H 0.1065 0.1520 0.3329 0.097 Uiso 1 1 calc R . . C54 C 0.1712(3) 0.2108(2) 0.3902(2) 0.0726(12) Uani 1 1 d . . . H54 H 0.1615 0.1882 0.4211 0.087 Uiso 1 1 calc R . . C55 C 0.2190(4) 0.7005(2) 0.36027(17) 0.0721(12) Uani 1 1 d . . . C56 C 0.2271(4) 0.7591(2) 0.33391(16) 0.0652(11) Uani 1 1 d . . . C57 C 0.1454(4) 0.7933(3) 0.3173(2) 0.0916(15) Uani 1 1 d . . . H57 H 0.1536 0.8333 0.3005 0.110 Uiso 1 1 calc R . . C58 C 0.0507(4) 0.7692(3) 0.3253(2) 0.0955(17) Uani 1 1 d . . . H58 H -0.0036 0.7922 0.3130 0.115 Uiso 1 1 calc R . . C59 C 0.0378(4) 0.7100(3) 0.3520(2) 0.0907(17) Uani 1 1 d . . . C60 C -0.0523(5) 0.6829(4) 0.3625(3) 0.122(2) Uani 1 1 d . . . H60 H -0.1078 0.7043 0.3499 0.147 Uiso 1 1 calc R . . C61 C -0.0662(6) 0.6268(5) 0.3903(3) 0.139(3) Uani 1 1 d . . . H61 H -0.1291 0.6109 0.3970 0.166 Uiso 1 1 calc R . . C62 C 0.0157(7) 0.5945(4) 0.4079(3) 0.134(3) Uani 1 1 d . . . H62 H 0.0070 0.5563 0.4270 0.160 Uiso 1 1 calc R . . C63 C 0.1098(5) 0.6157(3) 0.39878(19) 0.0966(18) Uani 1 1 d . . . H63 H 0.1632 0.5918 0.4110 0.116 Uiso 1 1 calc R . . C64 C 0.1252(4) 0.6753(3) 0.37013(18) 0.0847(15) Uani 1 1 d . . . C65 C 0.3087(3) 0.6648(2) 0.37825(15) 0.0693(11) Uani 1 1 d . . . C66 C 0.3479(4) 0.6147(2) 0.34862(15) 0.0651(11) Uani 1 1 d . . . C67 C 0.4367(4) 0.5833(2) 0.36268(17) 0.0739(12) Uani 1 1 d . . . H67 H 0.4634 0.5509 0.3415 0.089 Uiso 1 1 calc R . . C68 C 0.4828(4) 0.6010(3) 0.40764(19) 0.0842(15) Uani 1 1 d . . . H68 H 0.5413 0.5804 0.4168 0.101 Uiso 1 1 calc R . . C70 C 0.4906(5) 0.6675(3) 0.4882(2) 0.109(2) Uani 1 1 d . . . H70 H 0.5489 0.6474 0.4983 0.131 Uiso 1 1 calc R . . C71 C 0.4487(7) 0.7144(4) 0.5191(2) 0.123(3) Uani 1 1 d . . . H71 H 0.4788 0.7252 0.5504 0.147 Uiso 1 1 calc R . . C72 C 0.3632(7) 0.7461(4) 0.5050(2) 0.126(3) Uani 1 1 d . . . H72 H 0.3373 0.7783 0.5265 0.151 Uiso 1 1 calc R . . C73 C 0.3160(5) 0.7306(3) 0.45934(18) 0.1000(18) Uani 1 1 d . . . H73 H 0.2579 0.7518 0.4503 0.120 Uiso 1 1 calc R . . C74 C 0.3564(4) 0.6818(2) 0.42601(16) 0.0781(14) Uani 1 1 d . . . C75 C 0.4444(4) 0.6493(3) 0.44009(17) 0.0828(16) Uani 1 1 d . . . O1W O 0.4319(3) 0.40632(16) 0.33833(13) 0.0787(10) Uani 1 1 d . . . H1W H 0.478(4) 0.379(2) 0.3266(19) 0.094 Uiso 1 1 d . . . H2W H 0.405(4) 0.396(2) 0.3652(19) 0.094 Uiso 1 1 d . . . O2W O 0.3592(3) 0.48430(16) 0.26501(13) 0.0684(9) Uani 1 1 d . . . H3W H 0.376(4) 0.462(2) 0.2899(18) 0.082 Uiso 1 1 d . . . H4W H 0.321(4) 0.464(3) 0.254(2) 0.082 Uiso 1 1 d . . . C1S C 0.2754(13) 0.0007(7) 0.4740(6) 0.624(11) Uani 0.408(8) 1 d PD A 1 H1S1 H 0.2087 -0.0089 0.4851 0.749 Uiso 0.408(8) 1 calc PR A 1 H1S2 H 0.3155 -0.0385 0.4759 0.749 Uiso 0.408(8) 1 calc PR A 1 Cl1S Cl 0.2796(10) 0.0384(5) 0.4112(4) 0.261(7) Uani 0.408(8) 1 d PD A 1 Cl2S Cl 0.3244(15) 0.0630(12) 0.5062(5) 0.508(19) Uani 0.408(8) 1 d PD A 1 C2S C 0.2312(10) -0.0742(8) 0.4664(9) 0.42(3) Uani 0.592(8) 1 d PD A 2 H2S1 H 0.1774 -0.0843 0.4898 0.503 Uiso 0.592(8) 1 calc PR A 2 H2S2 H 0.2815 -0.1079 0.4681 0.503 Uiso 0.592(8) 1 calc PR A 2 Cl3S Cl 0.1922(10) -0.0571(10) 0.4024(5) 0.548(15) Uani 0.592(8) 1 d PD A 2 Cl4S Cl 0.2754(13) 0.0007(7) 0.4740(6) 0.624(11) Uani 0.59 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0460(3) 0.0540(3) 0.0596(3) 0.0008(2) -0.0017(2) -0.0067(2) Fe2 0.0611(4) 0.0640(4) 0.0699(4) -0.0123(3) 0.0053(3) 0.0103(3) Fe3 0.0746(4) 0.0516(3) 0.0589(3) -0.0014(3) -0.0036(3) 0.0159(3) N1 0.0503(19) 0.066(2) 0.0526(19) 0.0058(16) 0.0056(15) 0.0016(16) N2 0.0490(19) 0.0510(18) 0.0589(19) 0.0061(16) 0.0031(15) 0.0092(15) N3 0.053(2) 0.069(2) 0.075(2) 0.0071(19) 0.0116(18) 0.0018(18) N4 0.0440(19) 0.066(2) 0.0668(19) 0.0037(17) 0.0035(15) 0.0048(17) N5 0.061(2) 0.0557(19) 0.0467(16) 0.0018(15) -0.0007(15) 0.0018(16) N6 0.0474(19) 0.0562(19) 0.0515(17) 0.0012(15) 0.0044(14) -0.0066(15) O1 0.080(2) 0.089(2) 0.100(2) 0.0079(19) -0.0028(18) -0.0188(19) O2 0.085(2) 0.0780(19) 0.0590(16) -0.0128(15) -0.0130(15) 0.0061(17) C1 0.047(2) 0.053(2) 0.054(2) 0.0000(17) 0.0030(17) -0.0003(18) C2 0.064(3) 0.060(2) 0.054(2) -0.0005(19) 0.0062(18) -0.005(2) C3 0.069(3) 0.069(3) 0.072(3) 0.010(2) 0.019(2) -0.009(2) C4 0.048(2) 0.062(2) 0.102(3) -0.007(2) 0.007(2) -0.013(2) C5 0.044(2) 0.074(3) 0.063(2) -0.004(2) -0.0095(18) 0.002(2) C6 0.052(2) 0.053(2) 0.057(2) 0.0002(18) 0.0029(18) 0.0025(19) C7 0.051(2) 0.056(2) 0.0476(19) 0.0061(16) 0.0027(18) 0.0082(18) C8 0.053(2) 0.056(2) 0.050(2) 0.0059(18) 0.0014(17) 0.0071(18) C9 0.082(3) 0.058(2) 0.059(2) 0.017(2) 0.012(2) 0.017(2) C10 0.094(4) 0.081(3) 0.069(3) 0.022(2) 0.010(2) 0.030(3) C11 0.086(3) 0.057(2) 0.069(3) 0.0095(19) 0.001(2) 0.027(2) C12 0.062(3) 0.072(3) 0.066(3) -0.003(2) 0.005(2) 0.020(2) C13 0.050(2) 0.059(2) 0.066(2) -0.009(2) -0.0050(19) -0.001(2) C14 0.057(3) 0.050(2) 0.086(3) -0.010(2) 0.010(2) -0.005(2) C15 0.085(4) 0.076(3) 0.113(4) -0.039(3) -0.005(3) -0.008(3) C16 0.102(4) 0.060(3) 0.140(5) -0.036(3) 0.021(4) 0.000(3) C17 0.074(3) 0.056(3) 0.124(4) 0.005(3) 0.012(3) 0.017(2) C18 0.064(3) 0.055(2) 0.082(3) 0.006(2) 0.010(2) 0.009(2) C19 0.056(2) 0.066(3) 0.072(3) 0.009(2) 0.016(2) 0.007(2) C20 0.066(3) 0.100(4) 0.076(3) 0.010(3) 0.020(3) 0.018(3) C21 0.096(4) 0.144(5) 0.059(3) -0.007(3) 0.012(3) 0.017(4) C22 0.098(4) 0.124(5) 0.073(3) 0.013(3) -0.007(3) 0.020(4) C23 0.063(3) 0.074(3) 0.090(3) 0.021(2) 0.010(3) 0.011(2) C24 0.056(3) 0.046(2) 0.075(3) 0.0084(19) 0.015(2) -0.0008(19) C25 0.049(3) 0.066(3) 0.089(3) -0.001(2) 0.014(2) -0.004(2) C26 0.044(2) 0.083(3) 0.082(3) 0.004(2) 0.008(2) 0.007(2) C27 0.064(3) 0.099(4) 0.092(3) -0.007(3) -0.005(3) -0.014(3) C28 0.077(4) 0.123(5) 0.122(5) -0.018(4) -0.001(3) -0.033(4) C29 0.074(4) 0.089(4) 0.142(5) -0.006(4) 0.005(4) -0.023(3) C30 0.070(4) 0.081(3) 0.114(4) 0.000(3) 0.011(3) -0.014(3) C31 0.054(2) 0.081(3) 0.054(2) 0.002(2) 0.0022(18) 0.023(2) C32 0.072(3) 0.060(2) 0.048(2) -0.0030(18) -0.0031(19) 0.013(2) C33 0.107(4) 0.073(3) 0.061(2) -0.015(2) -0.008(3) 0.033(3) C34 0.122(5) 0.064(3) 0.099(4) -0.012(3) -0.026(4) -0.002(4) C35 0.078(3) 0.064(3) 0.102(3) 0.005(3) -0.019(3) -0.004(3) C36 0.062(3) 0.060(3) 0.070(3) 0.003(2) -0.011(2) 0.011(2) C37 0.072(3) 0.063(3) 0.051(2) -0.0015(18) -0.006(2) 0.013(2) C38 0.107(4) 0.066(3) 0.057(2) 0.007(2) 0.016(2) 0.017(3) C39 0.141(5) 0.059(3) 0.067(3) 0.014(2) -0.001(3) 0.033(3) C40 0.115(5) 0.110(4) 0.057(3) -0.004(3) -0.013(3) 0.059(4) C41 0.073(3) 0.097(4) 0.064(3) -0.010(3) -0.012(2) 0.022(3) C42 0.057(2) 0.060(2) 0.052(2) -0.0012(17) -0.0042(19) -0.002(2) C43 0.055(2) 0.046(2) 0.047(2) -0.0006(16) 0.0008(17) -0.0077(17) C44 0.051(2) 0.054(2) 0.055(2) -0.0032(18) 0.0079(17) -0.0048(18) C45 0.064(3) 0.065(3) 0.083(3) -0.004(2) 0.007(2) 0.008(2) C46 0.101(4) 0.061(3) 0.098(4) -0.019(3) 0.024(3) 0.001(3) C47 0.103(4) 0.058(3) 0.073(3) -0.020(2) -0.005(3) -0.004(3) C48 0.090(3) 0.066(3) 0.062(3) -0.007(2) -0.006(2) -0.008(2) C49 0.048(2) 0.061(2) 0.056(2) 0.0064(19) -0.0008(17) -0.002(2) C50 0.048(2) 0.058(2) 0.068(3) 0.005(2) -0.0048(18) -0.0060(19) C51 0.045(2) 0.075(3) 0.067(3) 0.003(2) 0.0037(19) -0.003(2) C52 0.059(3) 0.094(4) 0.071(3) -0.022(3) -0.008(2) 0.007(3) C53 0.056(3) 0.066(3) 0.121(4) -0.019(3) -0.015(3) 0.002(2) C54 0.061(3) 0.056(3) 0.100(3) 0.008(2) -0.014(2) -0.002(2) C55 0.087(3) 0.071(3) 0.058(2) -0.016(2) 0.013(2) -0.019(2) C56 0.066(3) 0.061(3) 0.068(3) -0.006(2) 0.001(2) -0.007(2) C57 0.096(4) 0.093(4) 0.085(3) -0.009(3) 0.010(3) 0.010(3) C58 0.076(4) 0.115(5) 0.096(4) -0.036(3) 0.008(3) -0.003(3) C59 0.081(4) 0.106(4) 0.085(3) -0.044(3) 0.029(3) -0.017(3) C60 0.092(4) 0.144(6) 0.131(5) -0.071(5) 0.048(4) -0.040(4) C61 0.107(6) 0.164(8) 0.146(6) -0.083(6) 0.058(5) -0.053(6) C62 0.155(7) 0.118(6) 0.127(6) -0.041(4) 0.068(6) -0.064(6) C63 0.113(5) 0.095(4) 0.082(3) -0.020(3) 0.036(3) -0.048(3) C64 0.100(4) 0.085(3) 0.069(3) -0.037(3) 0.029(3) -0.033(3) C65 0.086(3) 0.070(3) 0.052(2) -0.004(2) -0.006(2) -0.015(2) C66 0.081(3) 0.062(3) 0.052(2) 0.001(2) -0.005(2) -0.015(2) C67 0.090(3) 0.062(3) 0.070(3) 0.010(2) -0.009(3) -0.007(2) C68 0.097(4) 0.074(3) 0.082(3) 0.015(3) -0.031(3) -0.022(3) C70 0.145(6) 0.107(5) 0.075(3) 0.024(3) -0.037(4) -0.041(4) C71 0.198(8) 0.116(5) 0.055(3) -0.003(4) -0.020(4) -0.063(6) C72 0.196(8) 0.127(5) 0.054(3) -0.010(3) 0.005(4) -0.039(6) C73 0.140(5) 0.104(4) 0.057(3) -0.017(3) 0.007(3) -0.035(4) C74 0.112(4) 0.073(3) 0.050(2) 0.002(2) 0.000(3) -0.030(3) C75 0.116(4) 0.074(3) 0.059(3) 0.018(2) -0.026(3) -0.041(3) O1W 0.075(2) 0.080(2) 0.081(2) 0.0297(17) 0.0219(17) 0.0255(18) O2W 0.074(2) 0.059(2) 0.073(2) -0.0042(15) -0.0127(17) 0.0096(16) C1S 0.47(2) 0.66(3) 0.74(3) -0.15(3) -0.02(2) 0.07(2) Cl1S 0.365(15) 0.184(8) 0.234(9) 0.055(7) 0.050(10) 0.014(8) Cl2S 0.52(3) 0.75(4) 0.249(13) 0.035(17) -0.003(14) -0.43(3) C2S 0.123(14) 0.163(17) 0.97(9) 0.27(3) 0.26(3) 0.059(12) Cl3S 0.461(19) 0.80(4) 0.384(14) -0.212(17) 0.208(14) 0.14(2) Cl4S 0.47(2) 0.66(3) 0.74(3) -0.15(3) -0.02(2) 0.07(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 C54 2.033(4) . ? Fe1 C50 2.034(4) . ? Fe1 C2 2.038(4) . ? Fe1 C3 2.047(4) . ? Fe1 C1 2.049(4) . ? Fe1 C51 2.050(4) . ? Fe1 C4 2.051(4) . ? Fe1 C52 2.052(4) . ? Fe1 C5 2.054(4) . ? Fe1 C53 2.062(5) . ? Fe2 C23 2.032(4) . ? Fe2 C18 2.034(4) . ? Fe2 C15 2.035(5) . ? Fe2 C20 2.039(5) . ? Fe2 C19 2.044(4) . ? Fe2 C16 2.044(5) . ? Fe2 C14 2.047(4) . ? Fe2 C17 2.055(5) . ? Fe2 C21 2.061(5) . ? Fe2 C22 2.063(5) . ? Fe3 C40 2.038(5) . ? Fe3 C41 2.040(5) . ? Fe3 C32 2.042(4) . ? Fe3 C38 2.043(4) . ? Fe3 C37 2.043(4) . ? Fe3 C33 2.044(4) . ? Fe3 C36 2.047(4) . ? Fe3 C39 2.047(4) . ? Fe3 C34 2.061(5) . ? Fe3 C35 2.063(5) . ? N1 C6 1.268(4) . ? N1 C7 1.460(5) . ? N2 C13 1.259(5) . ? N2 C8 1.461(5) . ? N3 C24 1.263(5) . ? N3 C25 1.469(5) . ? N4 C31 1.264(5) . ? N4 C26 1.478(5) . ? N5 C42 1.257(5) . ? N5 C43 1.467(5) . ? N6 C49 1.257(5) . ? N6 C44 1.468(5) . ? O1 C56 1.374(5) . ? O2 C66 1.362(5) . ? C1 C5 1.419(5) . ? C1 C2 1.442(5) . ? C1 C6 1.461(5) . ? C2 C3 1.409(6) . ? C3 C4 1.397(6) . ? C4 C5 1.414(6) . ? C7 C8 1.528(5) . ? C7 C12 1.542(5) . ? C8 C9 1.513(5) . ? C9 C10 1.512(6) . ? C10 C11 1.524(6) . ? C11 C12 1.520(6) . ? C13 C14 1.445(6) . ? C14 C18 1.419(6) . ? C14 C15 1.437(6) . ? C15 C16 1.398(7) . ? C16 C17 1.397(8) . ? C17 C18 1.408(6) . ? C19 C23 1.429(6) . ? C19 C24 1.441(6) . ? C19 C20 1.452(6) . ? C20 C21 1.381(7) . ? C21 C22 1.419(7) . ? C22 C23 1.404(7) . ? C25 C26 1.524(6) . ? C25 C30 1.531(6) . ? C26 C27 1.518(6) . ? C27 C28 1.528(7) . ? C28 C29 1.512(8) . ? C29 C30 1.517(7) . ? C31 C32 1.447(6) . ? C32 C33 1.435(6) . ? C32 C36 1.437(6) . ? C33 C34 1.397(7) . ? C34 C35 1.417(7) . ? C35 C36 1.403(6) . ? C37 C38 1.414(6) . ? C37 C41 1.422(6) . ? C37 C42 1.467(5) . ? C38 C39 1.408(6) . ? C39 C40 1.396(8) . ? C40 C41 1.419(7) . ? C43 C44 1.523(5) . ? C43 C48 1.545(5) . ? C44 C45 1.516(5) . ? C45 C46 1.522(6) . ? C46 C47 1.537(7) . ? C47 C48 1.524(6) . ? C49 C50 1.461(5) . ? C50 C51 1.426(6) . ? C50 C54 1.433(6) . ? C51 C52 1.421(6) . ? C52 C53 1.419(7) . ? C53 C54 1.408(6) . ? C55 C56 1.381(6) . ? C55 C64 1.398(6) . ? C55 C65 1.494(7) . ? C56 C57 1.380(7) . ? C57 C58 1.393(8) . ? C58 C59 1.402(8) . ? C59 C60 1.370(8) . ? C59 C64 1.459(8) . ? C60 C61 1.365(10) . ? C61 C62 1.371(11) . ? C62 C63 1.369(9) . ? C63 C64 1.439(7) . ? C65 C66 1.383(6) . ? C65 C74 1.432(6) . ? C66 C67 1.413(6) . ? C67 C68 1.365(6) . ? C68 C75 1.393(7) . ? C70 C71 1.370(9) . ? C70 C75 1.435(7) . ? C71 C72 1.379(10) . ? C72 C73 1.375(8) . ? C73 C74 1.425(7) . ? C74 C75 1.415(7) . ? C1S Cl2S 1.658(12) . ? C1S Cl1S 1.791(12) . ? C2S Cl3S 1.765(14) . ? 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 C54 Fe1 C50 41.26(16) . . ? C54 Fe1 C2 122.87(18) . . ? C50 Fe1 C2 106.38(17) . . ? C54 Fe1 C3 107.86(19) . . ? C50 Fe1 C3 122.13(18) . . ? C2 Fe1 C3 40.36(16) . . ? C54 Fe1 C1 159.67(17) . . ? C50 Fe1 C1 122.49(15) . . ? C2 Fe1 C1 41.30(15) . . ? C3 Fe1 C1 68.34(16) . . ? C54 Fe1 C51 68.93(18) . . ? C50 Fe1 C51 40.86(16) . . ? C2 Fe1 C51 121.50(17) . . ? C3 Fe1 C51 157.66(18) . . ? C1 Fe1 C51 106.57(17) . . ? C54 Fe1 C4 122.93(18) . . ? C50 Fe1 C4 158.21(18) . . ? C2 Fe1 C4 67.65(17) . . ? C3 Fe1 C4 39.86(17) . . ? C1 Fe1 C4 67.81(16) . . ? C51 Fe1 C4 160.28(18) . . ? C54 Fe1 C52 68.20(19) . . ? C50 Fe1 C52 68.31(17) . . ? C2 Fe1 C52 157.88(19) . . ? C3 Fe1 C52 160.62(19) . . ? C1 Fe1 C52 122.06(18) . . ? C51 Fe1 C52 40.52(17) . . ? C4 Fe1 C52 125.08(18) . . ? C54 Fe1 C5 158.43(17) . . ? C50 Fe1 C5 159.21(16) . . ? C2 Fe1 C5 68.50(16) . . ? C3 Fe1 C5 67.84(17) . . ? C1 Fe1 C5 40.46(15) . . ? C51 Fe1 C5 123.30(17) . . ? C4 Fe1 C5 40.28(16) . . ? C52 Fe1 C5 108.42(17) . . ? C54 Fe1 C53 40.22(18) . . ? C50 Fe1 C53 68.26(17) . . ? C2 Fe1 C53 159.61(19) . . ? C3 Fe1 C53 124.5(2) . . ? C1 Fe1 C53 158.24(18) . . ? C51 Fe1 C53 68.17(19) . . ? C4 Fe1 C53 109.60(18) . . ? C52 Fe1 C53 40.34(19) . . ? C5 Fe1 C53 123.45(18) . . ? C23 Fe2 C18 117.42(19) . . ? C23 Fe2 C15 131.4(2) . . ? C18 Fe2 C15 68.4(2) . . ? C23 Fe2 C20 68.7(2) . . ? C18 Fe2 C20 129.73(19) . . ? C15 Fe2 C20 148.2(2) . . ? C23 Fe2 C19 41.05(17) . . ? C18 Fe2 C19 107.47(18) . . ? C15 Fe2 C19 169.65(18) . . ? C20 Fe2 C19 41.67(18) . . ? C23 Fe2 C16 169.7(2) . . ? C18 Fe2 C16 67.5(2) . . ? C15 Fe2 C16 40.1(2) . . ? C20 Fe2 C16 116.0(2) . . ? C19 Fe2 C16 148.3(2) . . ? C23 Fe2 C14 109.14(18) . . ? C18 Fe2 C14 40.69(17) . . ? C15 Fe2 C14 41.22(18) . . ? C20 Fe2 C14 168.88(19) . . ? C19 Fe2 C14 129.60(16) . . ? C16 Fe2 C14 68.1(2) . . ? C23 Fe2 C17 149.5(2) . . ? C18 Fe2 C17 40.27(17) . . ? C15 Fe2 C17 67.7(2) . . ? C20 Fe2 C17 107.9(2) . . ? C19 Fe2 C17 115.7(2) . . ? C16 Fe2 C17 39.9(2) . . ? C14 Fe2 C17 68.16(19) . . ? C23 Fe2 C21 67.2(2) . . ? C18 Fe2 C21 167.7(2) . . ? C15 Fe2 C21 118.1(2) . . ? C20 Fe2 C21 39.36(19) . . ? C19 Fe2 C21 67.9(2) . . ? C16 Fe2 C21 110.0(3) . . ? C14 Fe2 C21 150.9(2) . . ? C17 Fe2 C21 130.2(2) . . ? C23 Fe2 C22 40.1(2) . . ? C18 Fe2 C22 150.2(2) . . ? C15 Fe2 C22 109.9(2) . . ? C20 Fe2 C22 68.0(2) . . ? C19 Fe2 C22 68.6(2) . . ? C16 Fe2 C22 131.5(3) . . ? C14 Fe2 C22 117.9(2) . . ? C17 Fe2 C22 168.8(2) . . ? C21 Fe2 C22 40.2(2) . . ? C40 Fe3 C41 40.7(2) . . ? C40 Fe3 C32 129.6(2) . . ? C41 Fe3 C32 108.0(2) . . ? C40 Fe3 C38 67.7(2) . . ? C41 Fe3 C38 68.2(2) . . ? C32 Fe3 C38 150.30(16) . . ? C40 Fe3 C37 68.25(18) . . ? C41 Fe3 C37 40.76(17) . . ? C32 Fe3 C37 117.07(15) . . ? C38 Fe3 C37 40.48(17) . . ? C40 Fe3 C33 109.6(2) . . ? C41 Fe3 C33 118.7(2) . . ? C32 Fe3 C33 41.11(16) . . ? C38 Fe3 C33 167.1(2) . . ? C37 Fe3 C33 151.6(2) . . ? C40 Fe3 C36 168.2(2) . . ? C41 Fe3 C36 129.2(2) . . ? C32 Fe3 C36 41.14(17) . . ? C38 Fe3 C36 117.04(19) . . ? C37 Fe3 C36 107.78(17) . . ? C33 Fe3 C36 68.26(18) . . ? C40 Fe3 C39 40.0(2) . . ? C41 Fe3 C39 67.9(2) . . ? C32 Fe3 C39 167.8(2) . . ? C38 Fe3 C39 40.28(18) . . ? C37 Fe3 C39 67.93(17) . . ? C33 Fe3 C39 129.69(18) . . ? C36 Fe3 C39 150.2(2) . . ? C40 Fe3 C34 118.8(2) . . ? C41 Fe3 C34 151.7(2) . . ? C32 Fe3 C34 68.2(2) . . ? C38 Fe3 C34 129.3(2) . . ? C37 Fe3 C34 166.7(2) . . ? C33 Fe3 C34 39.8(2) . . ? C36 Fe3 C34 67.50(19) . . ? C39 Fe3 C34 109.6(2) . . ? C40 Fe3 C35 151.1(2) . . ? C41 Fe3 C35 166.8(2) . . ? C32 Fe3 C35 68.35(19) . . ? C38 Fe3 C35 108.3(2) . . ? C37 Fe3 C35 128.4(2) . . ? C33 Fe3 C35 67.5(2) . . ? C36 Fe3 C35 39.92(17) . . ? C39 Fe3 C35 118.3(2) . . ? C34 Fe3 C35 40.2(2) . . ? C6 N1 C7 116.5(3) . . ? C13 N2 C8 118.4(3) . . ? C24 N3 C25 115.6(4) . . ? C31 N4 C26 117.6(4) . . ? C42 N5 C43 117.2(3) . . ? C49 N6 C44 116.6(3) . . ? C5 C1 C2 107.3(3) . . ? C5 C1 C6 126.6(3) . . ? C2 C1 C6 125.9(3) . . ? C5 C1 Fe1 70.0(2) . . ? C2 C1 Fe1 68.9(2) . . ? C6 C1 Fe1 122.3(3) . . ? C3 C2 C1 107.6(4) . . ? C3 C2 Fe1 70.2(2) . . ? C1 C2 Fe1 69.8(2) . . ? C4 C3 C2 108.4(4) . . ? C4 C3 Fe1 70.2(2) . . ? C2 C3 Fe1 69.5(2) . . ? C3 C4 C5 109.0(4) . . ? C3 C4 Fe1 69.9(2) . . ? C5 C4 Fe1 70.0(2) . . ? C4 C5 C1 107.7(3) . . ? C4 C5 Fe1 69.7(2) . . ? C1 C5 Fe1 69.6(2) . . ? N1 C6 C1 121.4(4) . . ? N1 C7 C8 108.2(3) . . ? N1 C7 C12 109.6(3) . . ? C8 C7 C12 110.1(3) . . ? N2 C8 C9 108.2(3) . . ? N2 C8 C7 110.0(3) . . ? C9 C8 C7 110.6(3) . . ? C10 C9 C8 113.0(4) . . ? C9 C10 C11 110.5(3) . . ? C12 C11 C10 110.3(4) . . ? C11 C12 C7 109.8(3) . . ? N2 C13 C14 125.1(4) . . ? C18 C14 C15 106.4(4) . . ? C18 C14 C13 129.4(4) . . ? C15 C14 C13 123.8(4) . . ? C18 C14 Fe2 69.2(2) . . ? C15 C14 Fe2 69.0(3) . . ? C13 C14 Fe2 121.8(3) . . ? C16 C15 C14 107.8(5) . . ? C16 C15 Fe2 70.3(3) . . ? C14 C15 Fe2 69.8(2) . . ? C17 C16 C15 109.2(4) . . ? C17 C16 Fe2 70.5(3) . . ? C15 C16 Fe2 69.6(3) . . ? C16 C17 C18 107.8(5) . . ? C16 C17 Fe2 69.7(3) . . ? C18 C17 Fe2 69.1(2) . . ? C17 C18 C14 108.8(4) . . ? C17 C18 Fe2 70.6(3) . . ? C14 C18 Fe2 70.1(2) . . ? C23 C19 C24 123.3(4) . . ? C23 C19 C20 105.6(4) . . ? C24 C19 C20 130.7(4) . . ? C23 C19 Fe2 69.0(3) . . ? C24 C19 Fe2 121.4(3) . . ? C20 C19 Fe2 69.0(3) . . ? C21 C20 C19 108.0(4) . . ? C21 C20 Fe2 71.2(3) . . ? C19 C20 Fe2 69.3(2) . . ? C20 C21 C22 110.0(5) . . ? C20 C21 Fe2 69.4(3) . . ? C22 C21 Fe2 70.0(3) . . ? C23 C22 C21 106.7(5) . . ? C23 C22 Fe2 68.7(3) . . ? C21 C22 Fe2 69.8(3) . . ? C22 C23 C19 109.7(4) . . ? C22 C23 Fe2 71.2(3) . . ? C19 C23 Fe2 69.9(2) . . ? N3 C24 C19 126.8(4) . . ? N3 C25 C26 111.2(4) . . ? N3 C25 C30 110.4(4) . . ? C26 C25 C30 109.8(4) . . ? N4 C26 C27 108.3(4) . . ? N4 C26 C25 108.8(3) . . ? C27 C26 C25 111.1(4) . . ? C26 C27 C28 111.5(4) . . ? C29 C28 C27 111.8(5) . . ? C28 C29 C30 110.6(5) . . ? C29 C30 C25 111.1(4) . . ? N4 C31 C32 123.4(4) . . ? C33 C32 C36 106.2(4) . . ? C33 C32 C31 125.4(4) . . ? C36 C32 C31 128.3(4) . . ? C33 C32 Fe3 69.5(2) . . ? C36 C32 Fe3 69.6(2) . . ? C31 C32 Fe3 121.9(3) . . ? C34 C33 C32 108.7(5) . . ? C34 C33 Fe3 70.8(3) . . ? C32 C33 Fe3 69.4(2) . . ? C33 C34 C35 108.5(4) . . ? C33 C34 Fe3 69.5(3) . . ? C35 C34 Fe3 70.0(3) . . ? C36 C35 C34 108.1(5) . . ? C36 C35 Fe3 69.4(3) . . ? C34 C35 Fe3 69.8(3) . . ? C35 C36 C32 108.6(4) . . ? C35 C36 Fe3 70.7(3) . . ? C32 C36 Fe3 69.2(2) . . ? C38 C37 C41 107.6(4) . . ? C38 C37 C42 127.1(4) . . ? C41 C37 C42 125.0(4) . . ? C38 C37 Fe3 69.7(2) . . ? C41 C37 Fe3 69.5(2) . . ? C42 C37 Fe3 122.0(3) . . ? C39 C38 C37 108.2(5) . . ? C39 C38 Fe3 70.0(2) . . ? C37 C38 Fe3 69.8(2) . . ? C40 C39 C38 108.4(5) . . ? C40 C39 Fe3 69.7(3) . . ? C38 C39 Fe3 69.7(2) . . ? C39 C40 C41 108.4(5) . . ? C39 C40 Fe3 70.4(3) . . ? C41 C40 Fe3 69.7(3) . . ? C40 C41 C37 107.4(5) . . ? C40 C41 Fe3 69.6(3) . . ? C37 C41 Fe3 69.7(2) . . ? N5 C42 C37 123.3(4) . . ? N5 C43 C44 109.0(3) . . ? N5 C43 C48 109.8(3) . . ? C44 C43 C48 108.7(3) . . ? N6 C44 C45 110.2(3) . . ? N6 C44 C43 109.6(3) . . ? C45 C44 C43 109.8(3) . . ? C44 C45 C46 111.9(4) . . ? C45 C46 C47 110.7(4) . . ? C48 C47 C46 112.3(4) . . ? C47 C48 C43 110.3(4) . . ? N6 C49 C50 124.6(4) . . ? C51 C50 C54 107.9(4) . . ? C51 C50 C49 127.9(4) . . ? C54 C50 C49 124.1(4) . . ? C51 C50 Fe1 70.2(2) . . ? C54 C50 Fe1 69.4(2) . . ? C49 C50 Fe1 122.5(3) . . ? C52 C51 C50 107.4(4) . . ? C52 C51 Fe1 69.8(2) . . ? C50 C51 Fe1 68.9(2) . . ? C53 C52 C51 108.5(4) . . ? C53 C52 Fe1 70.2(3) . . ? C51 C52 Fe1 69.7(2) . . ? C54 C53 C52 108.2(4) . . ? C54 C53 Fe1 68.8(3) . . ? C52 C53 Fe1 69.5(3) . . ? C53 C54 C50 107.9(4) . . ? C53 C54 Fe1 71.0(3) . . ? C50 C54 Fe1 69.4(2) . . ? C56 C55 C64 118.7(5) . . ? C56 C55 C65 120.8(4) . . ? C64 C55 C65 120.5(4) . . ? O1 C56 C57 120.7(4) . . ? O1 C56 C55 117.5(4) . . ? C57 C56 C55 121.8(5) . . ? C56 C57 C58 121.3(5) . . ? C57 C58 C59 119.5(6) . . ? C60 C59 C58 123.8(7) . . ? C60 C59 C64 117.9(6) . . ? C58 C59 C64 118.3(5) . . ? C61 C60 C59 124.5(8) . . ? C60 C61 C62 117.7(7) . . ? C63 C62 C61 123.3(8) . . ? C62 C63 C64 119.4(7) . . ? C55 C64 C63 122.5(6) . . ? C55 C64 C59 120.4(5) . . ? C63 C64 C59 117.1(5) . . ? C66 C65 C74 118.6(5) . . ? C66 C65 C55 120.4(4) . . ? C74 C65 C55 121.1(4) . . ? O2 C66 C65 118.3(4) . . ? O2 C66 C67 120.1(4) . . ? C65 C66 C67 121.6(4) . . ? C68 C67 C66 119.2(5) . . ? C67 C68 C75 121.6(5) . . ? C71 C70 C75 120.0(7) . . ? C70 C71 C72 121.7(6) . . ? C73 C72 C71 120.7(7) . . ? C72 C73 C74 119.7(7) . . ? C75 C74 C73 120.0(5) . . ? C75 C74 C65 119.2(5) . . ? C73 C74 C65 120.8(5) . . ? C68 C75 C74 119.7(4) . . ? C68 C75 C70 122.4(6) . . ? C74 C75 C70 117.9(6) . . ? Cl2S C1S Cl1S 96.2(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W N4 0.89(5) 1.98(5) 2.848(5) 163(5) . O1W H2W N6 0.81(5) 2.06(5) 2.865(4) 168(5) . O2W H3W O1W 0.82(5) 1.84(5) 2.660(4) 170(5) . O2W H4W N2 0.71(5) 2.16(5) 2.854(5) 165(6) . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.292 _refine_diff_density_min -0.214 _refine_diff_density_rms 0.042 #========================================================================END data_(R)5 _database_code_depnum_ccdc_archive 'CCDC 227313' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H70 Cl2 Fe3 N6 O' _chemical_formula_weight 1357.86 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.8360(2) _cell_length_b 16.4830(3) _cell_length_c 34.7660(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6782.60(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13004 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 25.682 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2824 _exptl_absorpt_coefficient_mu 0.762 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25476 _diffrn_reflns_av_R_equivalents 0.0908 _diffrn_reflns_av_sigmaI/netI 0.1271 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 25.71 _reflns_number_total 12861 _reflns_number_gt 6660 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0238P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.009(12) _refine_ls_number_reflns 12861 _refine_ls_number_parameters 845 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1423 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_gt 0.0665 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.969 _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 0.50116(6) 0.81697(4) 0.127725(15) 0.05576(18) Uani 1 1 d . . . Fe2 Fe 0.23097(5) 0.46690(4) 0.205725(15) 0.05142(18) Uani 1 1 d . . . Fe3 Fe 0.39234(6) 0.42034(4) 0.017228(16) 0.0649(2) Uani 1 1 d . . . N1 N 0.5547(3) 0.6581(2) 0.20967(9) 0.0520(9) Uani 1 1 d . . . N2 N 0.4740(3) 0.5608(2) 0.26825(8) 0.0507(10) Uani 1 1 d . . . N3 N 0.5137(3) 0.3841(2) 0.15636(8) 0.0501(9) Uani 1 1 d . . . N4 N 0.5716(3) 0.2873(2) 0.09100(10) 0.0577(10) Uani 1 1 d . . . N5 N 0.6414(3) 0.5602(2) 0.04605(9) 0.0560(10) Uani 1 1 d . . . N6 N 0.7401(3) 0.7158(2) 0.06631(9) 0.0501(9) Uani 1 1 d . . . C1 C 0.4390(4) 0.7388(3) 0.16790(13) 0.0584(13) Uani 1 1 d . . . C2 C 0.3623(4) 0.8044(3) 0.16139(14) 0.0849(17) Uani 1 1 d . . . H2 H 0.3370 0.8415 0.1796 0.102 Uiso 1 1 calc R . . C3 C 0.3321(4) 0.8020(4) 0.12179(18) 0.098(2) Uani 1 1 d . . . H3 H 0.2827 0.8374 0.1095 0.118 Uiso 1 1 calc R . . C4 C 0.3892(5) 0.7375(4) 0.10457(15) 0.0895(18) Uani 1 1 d . . . H4 H 0.3846 0.7231 0.0788 0.107 Uiso 1 1 calc R . . C5 C 0.4546(4) 0.6979(3) 0.13248(13) 0.0667(13) Uani 1 1 d . . . H5 H 0.5003 0.6528 0.1284 0.080 Uiso 1 1 calc R . . C6 C 0.4999(4) 0.7227(3) 0.20393(11) 0.0534(11) Uani 1 1 d . . . H6 H 0.4980 0.7616 0.2233 0.064 Uiso 1 1 calc R . . C7 C 0.6212(3) 0.6538(2) 0.24538(10) 0.0465(11) Uani 1 1 d . . . H7 H 0.6007 0.6990 0.2623 0.070 Uiso 1 1 calc R . . C8 C 0.7456(4) 0.6590(2) 0.23534(12) 0.0469(11) Uani 1 1 d . . . C9 C 0.7841(4) 0.6299(2) 0.20010(12) 0.0592(12) Uani 1 1 d . . . H9 H 0.7331 0.6099 0.1821 0.071 Uiso 1 1 calc R . . C10 C 0.8982(5) 0.6309(3) 0.19188(13) 0.0737(14) Uani 1 1 d . . . H10 H 0.9233 0.6117 0.1682 0.088 Uiso 1 1 calc R . . C11 C 0.9740(4) 0.6592(3) 0.21770(16) 0.0737(15) Uani 1 1 d . . . H11 H 1.0505 0.6601 0.2116 0.088 Uiso 1 1 calc R . . C12 C 0.9381(5) 0.6866(3) 0.25293(15) 0.0716(14) Uani 1 1 d . . . H12 H 0.9908 0.7044 0.2709 0.086 Uiso 1 1 calc R . . C13 C 0.8251(5) 0.6880(3) 0.26195(12) 0.0638(13) Uani 1 1 d . . . H13 H 0.8014 0.7082 0.2856 0.077 Uiso 1 1 calc R . . C14 C 0.5954(4) 0.5717(2) 0.26586(10) 0.0484(11) Uani 1 1 d . . . H14 H 0.6285 0.5270 0.2510 0.073 Uiso 1 1 calc R . . C15 C 0.6451(4) 0.5720(3) 0.30617(11) 0.0482(11) Uani 1 1 d . . . C16 C 0.5940(4) 0.6151(3) 0.33507(13) 0.0626(13) Uani 1 1 d . . . H16 H 0.5264 0.6418 0.3301 0.075 Uiso 1 1 calc R . . C17 C 0.6409(5) 0.6199(3) 0.37151(15) 0.0840(17) Uani 1 1 d . . . H17 H 0.6058 0.6502 0.3906 0.101 Uiso 1 1 calc R . . C18 C 0.7395(6) 0.5794(4) 0.37919(16) 0.0971(19) Uani 1 1 d . . . H18 H 0.7717 0.5827 0.4035 0.116 Uiso 1 1 calc R . . C19 C 0.7909(5) 0.5342(4) 0.35105(18) 0.0979(18) Uani 1 1 d . . . H19 H 0.8573 0.5062 0.3563 0.118 Uiso 1 1 calc R . . C20 C 0.7422(5) 0.5306(3) 0.31432(13) 0.0760(14) Uani 1 1 d . . . H20 H 0.7765 0.4997 0.2952 0.091 Uiso 1 1 calc R . . C21 C 0.4367(4) 0.4923(3) 0.25647(10) 0.0503(12) Uani 1 1 d . . . H21 H 0.4881 0.4539 0.2477 0.060 Uiso 1 1 calc R . . C22 C 0.3173(4) 0.4723(3) 0.25626(10) 0.0503(12) Uani 1 1 d . . . C23 C 0.2251(4) 0.5264(3) 0.25725(10) 0.0551(12) Uani 1 1 d . . . H23 H 0.2301 0.5823 0.2607 0.066 Uiso 1 1 calc R . . C24 C 0.1248(4) 0.4827(3) 0.25229(11) 0.0630(13) Uani 1 1 d . . . H24 H 0.0522 0.5042 0.2518 0.076 Uiso 1 1 calc R . . C25 C 0.1534(4) 0.3999(3) 0.24809(11) 0.0646(14) Uani 1 1 d . . . H25 H 0.1032 0.3572 0.2444 0.078 Uiso 1 1 calc R . . C26 C 0.2722(4) 0.3936(3) 0.25052(10) 0.0553(12) Uani 1 1 d . . . H26 H 0.3138 0.3459 0.2487 0.066 Uiso 1 1 calc R . . C27 C 0.3203(4) 0.4298(3) 0.15865(11) 0.0529(12) Uani 1 1 d . . . C28 C 0.3340(4) 0.5149(3) 0.16385(11) 0.0591(13) Uani 1 1 d . . . H28 H 0.4019 0.5421 0.1679 0.071 Uiso 1 1 calc R . . C29 C 0.2261(5) 0.5506(3) 0.16184(11) 0.0742(15) Uani 1 1 d . . . H29 H 0.2107 0.6057 0.1639 0.089 Uiso 1 1 calc R . . C30 C 0.1456(5) 0.4891(4) 0.15626(12) 0.0757(16) Uani 1 1 d . . . H30 H 0.0679 0.4966 0.1544 0.091 Uiso 1 1 calc R . . C31 C 0.2020(4) 0.4145(4) 0.15391(11) 0.0672(14) Uani 1 1 d . . . H31 H 0.1686 0.3641 0.1500 0.081 Uiso 1 1 calc R . . C32 C 0.4093(5) 0.3685(3) 0.15935(10) 0.0517(12) Uani 1 1 d . . . H32 H 0.3879 0.3145 0.1622 0.062 Uiso 1 1 calc R . . C33 C 0.5915(3) 0.3146(3) 0.15948(10) 0.0496(11) Uani 1 1 d . . . H33 H 0.5470 0.2657 0.1646 0.074 Uiso 1 1 calc R . . C34 C 0.6733(4) 0.3273(3) 0.19265(11) 0.0480(11) Uani 1 1 d . . . C35 C 0.6867(4) 0.2652(3) 0.21937(12) 0.0580(13) Uani 1 1 d . . . H35 H 0.6432 0.2184 0.2178 0.070 Uiso 1 1 calc R . . C36 C 0.7656(5) 0.2743(3) 0.24829(13) 0.0678(14) Uani 1 1 d . . . H36 H 0.7753 0.2329 0.2662 0.081 Uiso 1 1 calc R . . C37 C 0.8295(4) 0.3429(4) 0.25100(13) 0.0739(16) Uani 1 1 d . . . H37 H 0.8820 0.3482 0.2707 0.089 Uiso 1 1 calc R . . C38 C 0.8162(4) 0.4039(3) 0.22465(14) 0.0712(15) Uani 1 1 d . . . H38 H 0.8603 0.4505 0.2262 0.085 Uiso 1 1 calc R . . C39 C 0.7369(4) 0.3959(3) 0.19565(11) 0.0602(12) Uani 1 1 d . . . H39 H 0.7270 0.4377 0.1780 0.072 Uiso 1 1 calc R . . C40 C 0.6559(4) 0.3028(2) 0.12085(10) 0.0496(11) Uani 1 1 d . . . H40 H 0.6974 0.3526 0.1146 0.074 Uiso 1 1 calc R . . C41 C 0.7386(4) 0.2329(3) 0.12454(11) 0.0539(12) Uani 1 1 d . . . C42 C 0.7049(4) 0.1532(3) 0.12079(13) 0.0757(15) Uani 1 1 d . . . H42 H 0.6313 0.1417 0.1133 0.091 Uiso 1 1 calc R . . C43 C 0.7784(7) 0.0906(4) 0.12797(18) 0.106(2) Uani 1 1 d . . . H43 H 0.7534 0.0373 0.1258 0.127 Uiso 1 1 calc R . . C44 C 0.8860(8) 0.1053(5) 0.13813(18) 0.115(3) Uani 1 1 d . . . H44 H 0.9345 0.0623 0.1433 0.138 Uiso 1 1 calc R . . C45 C 0.9242(5) 0.1832(5) 0.14086(13) 0.094(2) Uani 1 1 d . . . H45 H 0.9993 0.1937 0.1471 0.113 Uiso 1 1 calc R . . C46 C 0.8496(5) 0.2467(3) 0.13426(11) 0.0719(14) Uani 1 1 d . . . H46 H 0.8753 0.2998 0.1365 0.086 Uiso 1 1 calc R . . C47 C 0.5795(4) 0.3306(3) 0.06140(12) 0.0578(13) Uani 1 1 d . . . H47 H 0.6392 0.3671 0.0598 0.069 Uiso 1 1 calc R . . C48 C 0.4995(5) 0.3267(3) 0.02928(11) 0.0623(12) Uani 1 1 d . . . C49 C 0.3859(5) 0.3000(3) 0.02960(14) 0.0799(16) Uani 1 1 d . . . H49 H 0.3491 0.2774 0.0507 0.096 Uiso 1 1 calc R . . C50 C 0.3369(6) 0.3129(3) -0.00672(18) 0.0995(19) Uani 1 1 d . . . H50 H 0.2635 0.2999 -0.0140 0.119 Uiso 1 1 calc R . . C51 C 0.4188(6) 0.3486(4) -0.02963(15) 0.095(2) Uani 1 1 d . . . H51 H 0.4086 0.3641 -0.0551 0.114 Uiso 1 1 calc R . . C52 C 0.5198(5) 0.3581(3) -0.00866(13) 0.0790(15) Uani 1 1 d . . . H52 H 0.5869 0.3805 -0.0177 0.095 Uiso 1 1 calc R . . C53 C 0.4454(4) 0.5358(3) 0.02846(12) 0.0585(12) Uani 1 1 d . . . C54 C 0.3563(4) 0.5364(3) 0.00020(13) 0.0737(14) Uani 1 1 d . . . H54 H 0.3612 0.5563 -0.0248 0.088 Uiso 1 1 calc R . . C55 C 0.2603(5) 0.5012(3) 0.01753(16) 0.0774(14) Uani 1 1 d . . . H55 H 0.1902 0.4945 0.0059 0.093 Uiso 1 1 calc R . . C56 C 0.2879(5) 0.4774(3) 0.05571(14) 0.0761(15) Uani 1 1 d . . . H56 H 0.2399 0.4520 0.0731 0.091 Uiso 1 1 calc R . . C57 C 0.4006(4) 0.4990(3) 0.06223(12) 0.0592(13) Uani 1 1 d . . . H57 H 0.4401 0.4907 0.0850 0.071 Uiso 1 1 calc R . . C58 C 0.5616(4) 0.5611(2) 0.02155(12) 0.0599(13) Uani 1 1 d . . . H58 H 0.5790 0.5797 -0.0030 0.072 Uiso 1 1 calc R . . C59 C 0.7538(4) 0.5852(3) 0.03306(10) 0.0516(11) Uani 1 1 d . . . H59 H 0.7457 0.6156 0.0090 0.077 Uiso 1 1 calc R . . C60 C 0.8281(4) 0.5123(3) 0.02570(13) 0.0556(12) Uani 1 1 d . . . C61 C 0.8547(4) 0.4587(3) 0.05437(14) 0.0736(14) Uani 1 1 d . . . H61 H 0.8232 0.4661 0.0786 0.088 Uiso 1 1 calc R . . C62 C 0.9274(5) 0.3934(3) 0.04852(19) 0.0947(18) Uani 1 1 d . . . H62 H 0.9461 0.3589 0.0687 0.114 Uiso 1 1 calc R . . C63 C 0.9712(5) 0.3808(3) 0.0123(2) 0.0986(19) Uani 1 1 d . . . H63 H 1.0193 0.3373 0.0076 0.118 Uiso 1 1 calc R . . C64 C 0.9431(6) 0.4327(4) -0.01632(17) 0.104(2) Uani 1 1 d . . . H64 H 0.9725 0.4240 -0.0408 0.125 Uiso 1 1 calc R . . C65 C 0.8727(5) 0.4981(3) -0.01051(14) 0.0840(17) Uani 1 1 d . . . H65 H 0.8551 0.5325 -0.0308 0.101 Uiso 1 1 calc R . . C66 C 0.8075(4) 0.6413(3) 0.06329(11) 0.0466(11) Uani 1 1 d . . . H66 H 0.8075 0.6137 0.0882 0.070 Uiso 1 1 calc R . . C67 C 0.9269(4) 0.6635(2) 0.05291(11) 0.0462(11) Uani 1 1 d . . . C68 C 1.0164(4) 0.6359(3) 0.07431(11) 0.0594(12) Uani 1 1 d . . . H68 H 1.0025 0.6033 0.0956 0.071 Uiso 1 1 calc R . . C69 C 1.1261(5) 0.6554(3) 0.06508(15) 0.0785(15) Uani 1 1 d . . . H69 H 1.1855 0.6368 0.0802 0.094 Uiso 1 1 calc R . . C70 C 1.1474(5) 0.7025(3) 0.03347(17) 0.0804(16) Uani 1 1 d . . . H70 H 1.2215 0.7156 0.0271 0.097 Uiso 1 1 calc R . . C71 C 1.0620(5) 0.7299(3) 0.01145(13) 0.0704(15) Uani 1 1 d . . . H71 H 1.0773 0.7614 -0.0102 0.085 Uiso 1 1 calc R . . C72 C 0.9508(4) 0.7113(3) 0.02102(11) 0.0579(12) Uani 1 1 d . . . H72 H 0.8920 0.7310 0.0059 0.070 Uiso 1 1 calc R . . C73 C 0.7232(3) 0.7425(3) 0.10028(12) 0.0491(11) Uani 1 1 d . . . H73 H 0.7511 0.7124 0.1208 0.059 Uiso 1 1 calc R . . C74 C 0.6630(4) 0.8173(3) 0.10879(11) 0.0502(11) Uani 1 1 d . . . C75 C 0.5939(4) 0.8644(3) 0.08379(11) 0.0587(13) Uani 1 1 d . . . H75 H 0.5835 0.8552 0.0576 0.070 Uiso 1 1 calc R . . C76 C 0.5434(4) 0.9275(3) 0.10547(12) 0.0722(15) Uani 1 1 d . . . H76 H 0.4929 0.9661 0.0962 0.087 Uiso 1 1 calc R . . C77 C 0.5832(4) 0.9215(3) 0.14342(12) 0.0703(14) Uani 1 1 d . . . H77 H 0.5652 0.9566 0.1634 0.084 Uiso 1 1 calc R . . C78 C 0.6553(4) 0.8532(3) 0.14628(12) 0.0609(13) Uani 1 1 d . . . H78 H 0.6912 0.8349 0.1684 0.073 Uiso 1 1 calc R . . C1S C 0.9898(9) 0.8428(5) 0.1090(3) 0.207(5) Uani 0.775(9) 1 d PD A 1 H1S1 H 1.0388 0.7958 0.1071 0.248 Uiso 0.775(9) 1 calc PR A 1 H1S2 H 0.9188 0.8288 0.0967 0.248 Uiso 0.775(9) 1 calc PR A 1 Cl1 Cl 1.0467(4) 0.9159(3) 0.08508(6) 0.1396(18) Uani 0.775(9) 1 d PD A 1 Cl2 Cl 0.9633(4) 0.8614(4) 0.15797(11) 0.160(2) Uani 0.775(9) 1 d PD A 1 C2S C 0.9898(9) 0.8428(5) 0.1090(3) 0.207(5) Uani 0.22 1 d PD A 2 H2S1 H 0.9241 0.8106 0.1023 0.248 Uiso 0.225(9) 1 calc PR A 2 H2S2 H 1.0498 0.8248 0.0920 0.248 Uiso 0.225(9) 1 calc PR A 2 Cl12 Cl 0.961(3) 0.9316(13) 0.0953(7) 0.289(11) Uani 0.225(9) 1 d PD A 2 Cl22 Cl 1.0250(18) 0.8126(9) 0.1494(3) 0.181(6) Uani 0.225(9) 1 d PD A 2 O1W O 0.6450(3) 0.5275(2) 0.12672(10) 0.0809(12) Uani 1 1 d . . . H1W H 0.608(5) 0.494(3) 0.1340(14) 0.097 Uiso 1 1 d . . . H2W H 0.629(4) 0.532(3) 0.0981(12) 0.097 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 0.0530(4) 0.0606(4) 0.0537(3) 0.0067(3) 0.0013(3) 0.0073(4) Fe2 0.0438(4) 0.0513(4) 0.0592(4) 0.0038(3) 0.0004(3) 0.0014(4) Fe3 0.0688(5) 0.0652(5) 0.0607(4) -0.0035(4) -0.0137(3) 0.0000(4) N1 0.046(2) 0.052(3) 0.058(2) 0.006(2) 0.0009(19) 0.003(2) N2 0.045(3) 0.053(3) 0.055(2) 0.0090(19) 0.0014(17) 0.001(2) N3 0.042(3) 0.053(3) 0.0553(19) 0.0039(17) -0.0028(19) 0.004(2) N4 0.062(3) 0.053(3) 0.058(2) 0.004(2) -0.007(2) -0.001(2) N5 0.052(3) 0.063(3) 0.053(2) 0.0025(19) -0.003(2) -0.007(2) N6 0.058(3) 0.049(2) 0.044(2) -0.0013(17) 0.0019(18) 0.001(2) C1 0.046(3) 0.072(4) 0.057(3) 0.014(3) 0.006(2) 0.004(3) C2 0.059(4) 0.110(5) 0.085(4) 0.029(3) 0.020(3) 0.030(4) C3 0.047(4) 0.137(6) 0.110(5) 0.069(5) -0.006(3) 0.020(4) C4 0.073(5) 0.108(5) 0.088(4) 0.029(4) -0.020(4) -0.021(4) C5 0.053(3) 0.072(3) 0.075(3) 0.021(3) -0.004(3) -0.017(3) C6 0.045(3) 0.061(3) 0.055(3) 0.007(2) 0.013(3) 0.005(3) C7 0.044(3) 0.047(3) 0.049(2) 0.001(2) 0.000(2) 0.001(2) C8 0.044(3) 0.038(3) 0.059(3) 0.008(2) -0.002(2) -0.002(3) C9 0.056(4) 0.061(3) 0.061(3) 0.007(2) 0.003(3) 0.003(3) C10 0.061(4) 0.085(4) 0.075(3) -0.005(3) 0.015(3) -0.002(3) C11 0.044(4) 0.078(4) 0.100(4) 0.015(3) 0.015(3) -0.007(3) C12 0.058(4) 0.063(4) 0.094(4) 0.004(3) -0.011(3) -0.015(3) C13 0.061(4) 0.058(3) 0.072(3) 0.004(3) -0.004(3) -0.003(3) C14 0.045(3) 0.042(3) 0.058(3) 0.003(2) 0.005(2) 0.005(3) C15 0.051(3) 0.036(3) 0.057(3) 0.010(2) 0.000(2) 0.004(2) C16 0.064(4) 0.057(3) 0.066(3) -0.006(3) -0.004(3) 0.005(3) C17 0.097(5) 0.085(4) 0.069(4) -0.009(3) -0.001(3) -0.005(4) C18 0.092(5) 0.130(6) 0.070(4) -0.002(4) -0.014(4) -0.015(5) C19 0.063(4) 0.122(5) 0.108(4) 0.027(4) -0.020(4) 0.010(4) C20 0.077(4) 0.079(4) 0.072(3) 0.007(3) -0.004(3) 0.011(4) C21 0.052(4) 0.050(3) 0.049(3) 0.005(2) 0.001(2) 0.003(3) C22 0.047(3) 0.055(3) 0.049(2) 0.004(2) 0.003(2) -0.004(3) C23 0.058(3) 0.047(3) 0.060(3) -0.001(2) 0.011(2) 0.001(3) C24 0.045(4) 0.062(4) 0.082(3) 0.003(3) 0.010(3) -0.005(3) C25 0.055(4) 0.059(4) 0.080(3) 0.011(3) 0.009(3) -0.021(3) C26 0.051(3) 0.050(3) 0.065(3) 0.010(2) -0.005(2) -0.003(3) C27 0.048(3) 0.056(3) 0.055(3) 0.003(3) -0.002(2) 0.009(3) C28 0.061(4) 0.055(4) 0.061(3) 0.015(3) 0.008(2) 0.002(3) C29 0.078(4) 0.081(4) 0.064(3) 0.016(3) 0.007(3) 0.025(4) C30 0.049(4) 0.110(5) 0.068(3) 0.008(3) -0.005(3) 0.036(4) C31 0.044(4) 0.087(4) 0.071(3) -0.009(3) -0.007(2) -0.004(3) C32 0.060(4) 0.045(3) 0.050(3) 0.002(2) -0.003(3) 0.003(3) C33 0.038(3) 0.048(3) 0.062(3) 0.007(2) 0.006(2) -0.004(3) C34 0.044(3) 0.047(3) 0.053(3) -0.002(3) 0.005(2) 0.007(3) C35 0.051(3) 0.067(4) 0.056(3) 0.002(3) 0.003(2) 0.005(3) C36 0.062(4) 0.075(4) 0.066(3) 0.010(3) 0.005(3) 0.021(3) C37 0.062(4) 0.103(5) 0.056(3) -0.009(3) -0.014(3) 0.025(4) C38 0.062(4) 0.075(4) 0.077(3) -0.008(3) -0.010(3) -0.002(3) C39 0.063(3) 0.049(3) 0.068(3) 0.004(2) -0.010(3) 0.000(3) C40 0.047(3) 0.046(3) 0.056(3) 0.005(2) 0.000(2) -0.005(3) C41 0.053(4) 0.058(4) 0.051(3) 0.000(2) 0.008(2) 0.010(3) C42 0.061(4) 0.056(4) 0.110(4) 0.003(3) 0.025(3) 0.010(3) C43 0.103(5) 0.063(4) 0.152(5) 0.007(4) 0.046(5) 0.028(5) C44 0.121(7) 0.109(6) 0.115(5) 0.029(5) 0.034(5) 0.062(6) C45 0.070(5) 0.137(6) 0.075(3) -0.001(4) -0.002(3) 0.047(5) C46 0.073(4) 0.076(4) 0.066(3) -0.012(3) 0.003(3) 0.005(4) C47 0.057(3) 0.056(3) 0.061(3) -0.012(3) -0.007(3) 0.000(3) C48 0.069(4) 0.058(3) 0.060(3) -0.005(2) -0.007(3) -0.002(3) C49 0.094(5) 0.057(3) 0.089(4) -0.001(3) -0.024(3) -0.016(3) C50 0.104(5) 0.087(5) 0.107(5) -0.025(4) -0.052(4) -0.008(4) C51 0.122(6) 0.098(5) 0.066(4) -0.022(3) -0.032(4) 0.023(4) C52 0.081(4) 0.093(4) 0.063(3) -0.007(3) -0.001(3) 0.013(3) C53 0.055(4) 0.058(3) 0.062(3) 0.001(3) 0.005(3) -0.002(3) C54 0.074(4) 0.074(4) 0.073(3) 0.005(3) -0.018(3) 0.001(3) C55 0.053(4) 0.076(4) 0.103(4) 0.001(3) -0.013(3) -0.006(3) C56 0.073(4) 0.078(4) 0.077(4) -0.007(3) 0.005(3) -0.005(3) C57 0.058(4) 0.059(3) 0.060(3) -0.006(2) 0.001(3) -0.002(3) C58 0.068(4) 0.056(3) 0.056(3) 0.002(2) 0.005(3) 0.001(3) C59 0.052(3) 0.053(3) 0.050(2) 0.003(2) 0.000(2) -0.002(3) C60 0.058(3) 0.046(3) 0.063(3) -0.004(3) 0.008(3) -0.012(3) C61 0.081(4) 0.053(3) 0.087(4) 0.010(3) 0.014(3) 0.001(3) C62 0.091(5) 0.068(4) 0.126(5) 0.018(4) 0.022(4) 0.012(4) C63 0.082(5) 0.055(4) 0.158(6) -0.025(4) 0.022(5) 0.002(3) C64 0.137(6) 0.084(5) 0.091(4) -0.028(4) 0.022(4) 0.012(5) C65 0.102(5) 0.073(4) 0.077(4) -0.012(3) 0.017(3) 0.002(4) C66 0.049(3) 0.048(3) 0.043(2) 0.004(2) 0.001(2) 0.004(3) C67 0.052(3) 0.040(3) 0.047(3) 0.003(2) 0.003(2) -0.001(3) C68 0.052(4) 0.067(3) 0.060(3) 0.010(2) -0.003(3) -0.004(3) C69 0.066(5) 0.078(4) 0.092(4) 0.007(3) -0.006(3) 0.000(3) C70 0.048(4) 0.082(4) 0.111(4) -0.004(4) 0.019(3) -0.014(3) C71 0.087(5) 0.059(4) 0.065(3) -0.003(3) 0.016(3) -0.020(3) C72 0.055(4) 0.054(3) 0.065(3) 0.004(3) -0.002(3) 0.001(3) C73 0.040(3) 0.054(3) 0.053(3) 0.005(2) -0.001(2) -0.002(3) C74 0.049(3) 0.053(3) 0.048(3) -0.005(3) 0.008(2) 0.007(3) C75 0.075(4) 0.053(3) 0.049(3) 0.009(2) 0.003(3) 0.000(3) C76 0.097(4) 0.056(3) 0.064(3) 0.000(3) 0.011(3) 0.027(3) C77 0.100(4) 0.049(3) 0.062(3) -0.011(3) 0.007(3) -0.001(3) C78 0.070(4) 0.057(3) 0.056(3) -0.008(3) 0.003(2) -0.003(3) C1S 0.185(10) 0.135(9) 0.300(13) -0.120(9) 0.056(11) -0.071(9) Cl1 0.162(3) 0.180(3) 0.0766(16) -0.0252(16) -0.0216(15) -0.005(3) Cl2 0.130(3) 0.197(5) 0.152(3) 0.056(3) -0.022(2) -0.031(3) C2S 0.185(10) 0.135(9) 0.300(13) -0.120(9) 0.056(11) -0.071(9) Cl12 0.26(2) 0.28(2) 0.33(2) -0.108(16) -0.132(17) 0.125(18) Cl22 0.255(17) 0.171(12) 0.116(7) 0.011(7) 0.024(9) 0.061(12) O1W 0.097(3) 0.083(3) 0.0631(19) 0.007(2) -0.011(2) -0.022(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 C78 2.025(4) . ? Fe1 C74 2.025(4) . ? Fe1 C3 2.027(5) . ? Fe1 C2 2.028(5) . ? Fe1 C4 2.030(5) . ? Fe1 C75 2.036(4) . ? Fe1 C1 2.038(4) . ? Fe1 C76 2.042(4) . ? Fe1 C5 2.045(4) . ? Fe1 C77 2.051(4) . ? Fe2 C31 2.027(4) . ? Fe2 C30 2.028(4) . ? Fe2 C26 2.030(4) . ? Fe2 C22 2.035(4) . ? Fe2 C27 2.042(4) . ? Fe2 C23 2.043(4) . ? Fe2 C25 2.057(4) . ? Fe2 C29 2.057(4) . ? Fe2 C28 2.058(4) . ? Fe2 C24 2.066(4) . ? Fe3 C49 2.030(5) . ? Fe3 C52 2.034(5) . ? Fe3 C57 2.035(4) . ? Fe3 C51 2.037(5) . ? Fe3 C48 2.041(5) . ? Fe3 C53 2.041(5) . ? Fe3 C54 2.047(5) . ? Fe3 C56 2.050(5) . ? Fe3 C55 2.054(5) . ? Fe3 C50 2.064(5) . ? N1 C6 1.263(4) . ? N1 C7 1.472(4) . ? N2 C21 1.279(4) . ? N2 C14 1.451(5) . ? N3 C32 1.267(5) . ? N3 C33 1.473(5) . ? N4 C47 1.256(4) . ? N4 C40 1.462(5) . ? N5 C58 1.272(5) . ? N5 C59 1.465(5) . ? N6 C73 1.276(4) . ? N6 C66 1.467(5) . ? C1 C5 1.415(5) . ? C1 C2 1.430(6) . ? C1 C6 1.470(5) . ? C2 C3 1.423(6) . ? C3 C4 1.395(7) . ? C4 C5 1.403(6) . ? C7 C8 1.515(5) . ? C7 C14 1.559(5) . ? C8 C9 1.392(5) . ? C8 C13 1.404(6) . ? C9 C10 1.380(6) . ? C10 C11 1.352(6) . ? C11 C12 1.373(6) . ? C12 C13 1.374(6) . ? C14 C15 1.519(5) . ? C15 C20 1.366(5) . ? C15 C16 1.371(5) . ? C16 C17 1.385(6) . ? C17 C18 1.370(7) . ? C18 C19 1.372(7) . ? C19 C20 1.402(6) . ? C21 C22 1.451(6) . ? C22 C23 1.410(5) . ? C22 C26 1.417(5) . ? C23 C24 1.399(6) . ? C24 C25 1.414(6) . ? C25 C26 1.412(6) . ? C27 C28 1.425(5) . ? C27 C31 1.431(5) . ? C27 C32 1.459(6) . ? C28 C29 1.407(6) . ? C29 C30 1.405(6) . ? C30 C31 1.401(6) . ? C33 C34 1.520(5) . ? C33 C40 1.556(5) . ? C34 C39 1.363(5) . ? C34 C35 1.390(5) . ? C35 C36 1.380(6) . ? C36 C37 1.364(6) . ? C37 C38 1.369(6) . ? C38 C39 1.384(5) . ? C40 C41 1.517(5) . ? C41 C46 1.376(6) . ? C41 C42 1.379(6) . ? C42 C43 1.373(7) . ? C43 C44 1.343(8) . ? C44 C45 1.365(8) . ? C45 C46 1.388(7) . ? C47 C48 1.465(6) . ? C48 C49 1.415(6) . ? C48 C52 1.437(5) . ? C49 C50 1.406(6) . ? C50 C51 1.386(7) . ? C51 C52 1.408(7) . ? C53 C57 1.423(5) . ? C53 C54 1.441(5) . ? C53 C58 1.458(6) . ? C54 C55 1.411(6) . ? C55 C56 1.422(6) . ? C56 C57 1.400(6) . ? C59 C60 1.511(5) . ? C59 C66 1.537(5) . ? C60 C61 1.369(6) . ? C60 C65 1.385(6) . ? C61 C62 1.393(6) . ? C62 C63 1.378(6) . ? C63 C64 1.354(7) . ? C64 C65 1.377(7) . ? C66 C67 1.503(5) . ? C67 C68 1.371(5) . ? C67 C72 1.389(5) . ? C68 C69 1.377(6) . ? C69 C70 1.368(6) . ? C70 C71 1.346(6) . ? C71 C72 1.392(6) . ? C73 C74 1.455(5) . ? C74 C75 1.424(5) . ? C74 C78 1.434(5) . ? C75 C76 1.417(5) . ? C76 C77 1.405(5) . ? C77 C78 1.416(5) . ? C1S Cl1 1.612(9) . ? C1S Cl2 1.758(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C78 Fe1 C74 41.46(15) . . ? C78 Fe1 C3 163.3(3) . . ? C74 Fe1 C3 154.3(2) . . ? C78 Fe1 C2 125.2(2) . . ? C74 Fe1 C2 162.6(2) . . ? C3 Fe1 C2 41.09(18) . . ? C78 Fe1 C4 154.8(3) . . ? C74 Fe1 C4 119.4(2) . . ? C3 Fe1 C4 40.2(2) . . ? C2 Fe1 C4 68.5(2) . . ? C78 Fe1 C75 68.92(17) . . ? C74 Fe1 C75 41.03(15) . . ? C3 Fe1 C75 120.1(2) . . ? C2 Fe1 C75 155.3(2) . . ? C4 Fe1 C75 107.6(2) . . ? C78 Fe1 C1 107.06(18) . . ? C74 Fe1 C1 124.46(19) . . ? C3 Fe1 C1 68.68(18) . . ? C2 Fe1 C1 41.17(16) . . ? C4 Fe1 C1 68.15(19) . . ? C75 Fe1 C1 162.01(19) . . ? C78 Fe1 C76 68.73(19) . . ? C74 Fe1 C76 69.08(18) . . ? C3 Fe1 C76 108.2(2) . . ? C2 Fe1 C76 120.6(2) . . ? C4 Fe1 C76 125.8(2) . . ? C75 Fe1 C76 40.67(15) . . ? C1 Fe1 C76 155.86(19) . . ? C78 Fe1 C5 119.98(19) . . ? C74 Fe1 C5 106.48(19) . . ? C3 Fe1 C5 68.0(2) . . ? C2 Fe1 C5 68.71(19) . . ? C4 Fe1 C5 40.27(17) . . ? C75 Fe1 C5 125.03(18) . . ? C1 Fe1 C5 40.57(15) . . ? C76 Fe1 C5 162.36(19) . . ? C78 Fe1 C77 40.65(16) . . ? C74 Fe1 C77 68.67(19) . . ? C3 Fe1 C77 126.6(3) . . ? C2 Fe1 C77 108.4(2) . . ? C4 Fe1 C77 163.0(2) . . ? C75 Fe1 C77 67.80(17) . . ? C1 Fe1 C77 121.32(19) . . ? C76 Fe1 C77 40.14(15) . . ? C5 Fe1 C77 155.76(19) . . ? C31 Fe2 C30 40.42(17) . . ? C31 Fe2 C26 118.0(2) . . ? C30 Fe2 C26 151.3(2) . . ? C31 Fe2 C22 150.6(2) . . ? C30 Fe2 C22 167.1(2) . . ? C26 Fe2 C22 40.81(15) . . ? C31 Fe2 C27 41.19(15) . . ? C30 Fe2 C27 68.44(18) . . ? C26 Fe2 C27 108.18(18) . . ? C22 Fe2 C27 116.45(18) . . ? C31 Fe2 C23 167.9(2) . . ? C30 Fe2 C23 129.8(2) . . ? C26 Fe2 C23 67.75(17) . . ? C22 Fe2 C23 40.44(15) . . ? C27 Fe2 C23 149.8(2) . . ? C31 Fe2 C25 109.41(19) . . ? C30 Fe2 C25 118.8(2) . . ? C26 Fe2 C25 40.40(16) . . ? C22 Fe2 C25 68.24(17) . . ? C27 Fe2 C25 130.1(2) . . ? C23 Fe2 C25 67.35(17) . . ? C31 Fe2 C29 67.8(2) . . ? C30 Fe2 C29 40.23(17) . . ? C26 Fe2 C29 167.0(2) . . ? C22 Fe2 C29 128.7(2) . . ? C27 Fe2 C29 67.73(19) . . ? C23 Fe2 C29 109.11(19) . . ? C25 Fe2 C29 151.5(2) . . ? C31 Fe2 C28 68.61(18) . . ? C30 Fe2 C28 68.06(19) . . ? C26 Fe2 C28 129.0(2) . . ? C22 Fe2 C28 107.23(19) . . ? C27 Fe2 C28 40.68(15) . . ? C23 Fe2 C28 117.11(19) . . ? C25 Fe2 C28 167.9(2) . . ? C29 Fe2 C28 40.00(16) . . ? C31 Fe2 C24 130.34(19) . . ? C30 Fe2 C24 109.79(19) . . ? C26 Fe2 C24 67.66(18) . . ? C22 Fe2 C24 67.86(17) . . ? C27 Fe2 C24 168.7(2) . . ? C23 Fe2 C24 39.81(15) . . ? C25 Fe2 C24 40.10(16) . . ? C29 Fe2 C24 118.7(2) . . ? C28 Fe2 C24 150.1(2) . . ? C49 Fe3 C52 68.2(2) . . ? C49 Fe3 C57 117.49(18) . . ? C52 Fe3 C57 128.8(2) . . ? C49 Fe3 C51 67.0(2) . . ? C52 Fe3 C51 40.49(19) . . ? C57 Fe3 C51 167.8(3) . . ? C49 Fe3 C48 40.67(18) . . ? C52 Fe3 C48 41.31(16) . . ? C57 Fe3 C48 107.12(18) . . ? C51 Fe3 C48 68.28(18) . . ? C49 Fe3 C53 151.81(19) . . ? C52 Fe3 C53 109.1(2) . . ? C57 Fe3 C53 40.87(15) . . ? C51 Fe3 C53 130.3(2) . . ? C48 Fe3 C53 118.3(2) . . ? C49 Fe3 C54 165.0(2) . . ? C52 Fe3 C54 119.8(2) . . ? C57 Fe3 C54 68.70(17) . . ? C51 Fe3 C54 110.1(2) . . ? C48 Fe3 C54 153.6(2) . . ? C53 Fe3 C54 41.28(16) . . ? C49 Fe3 C56 106.7(2) . . ? C52 Fe3 C56 165.3(2) . . ? C57 Fe3 C56 40.08(16) . . ? C51 Fe3 C56 151.7(3) . . ? C48 Fe3 C56 125.98(19) . . ? C53 Fe3 C56 68.48(19) . . ? C54 Fe3 C56 68.57(19) . . ? C49 Fe3 C55 127.1(2) . . ? C52 Fe3 C55 153.3(2) . . ? C57 Fe3 C55 67.62(19) . . ? C51 Fe3 C55 119.8(2) . . ? C48 Fe3 C55 164.2(2) . . ? C53 Fe3 C55 68.19(19) . . ? C54 Fe3 C55 40.26(16) . . ? C56 Fe3 C55 40.55(17) . . ? C49 Fe3 C50 40.14(17) . . ? C52 Fe3 C50 68.0(2) . . ? C57 Fe3 C50 150.7(2) . . ? C51 Fe3 C50 39.51(19) . . ? C48 Fe3 C50 68.4(2) . . ? C53 Fe3 C50 167.1(2) . . ? C54 Fe3 C50 128.2(2) . . ? C56 Fe3 C50 117.7(3) . . ? C55 Fe3 C50 108.4(2) . . ? C6 N1 C7 116.6(4) . . ? C21 N2 C14 115.7(4) . . ? C32 N3 C33 116.5(4) . . ? C47 N4 C40 115.6(4) . . ? C58 N5 C59 117.7(3) . . ? C73 N6 C66 116.1(3) . . ? C5 C1 C2 107.8(4) . . ? C5 C1 C6 126.3(4) . . ? C2 C1 C6 125.6(5) . . ? C5 C1 Fe1 70.0(2) . . ? C2 C1 Fe1 69.0(3) . . ? C6 C1 Fe1 121.4(3) . . ? C3 C2 C1 107.0(5) . . ? C3 C2 Fe1 69.4(3) . . ? C1 C2 Fe1 69.8(3) . . ? C4 C3 C2 108.3(5) . . ? C4 C3 Fe1 70.0(3) . . ? C2 C3 Fe1 69.5(3) . . ? C3 C4 C5 109.0(5) . . ? C3 C4 Fe1 69.8(3) . . ? C5 C4 Fe1 70.4(3) . . ? C4 C5 C1 108.0(5) . . ? C4 C5 Fe1 69.3(3) . . ? C1 C5 Fe1 69.5(3) . . ? N1 C6 C1 122.6(4) . . ? N1 C7 C8 108.8(3) . . ? N1 C7 C14 108.8(3) . . ? C8 C7 C14 110.2(3) . . ? C9 C8 C13 118.5(4) . . ? C9 C8 C7 120.1(4) . . ? C13 C8 C7 121.2(4) . . ? C10 C9 C8 119.9(4) . . ? C11 C10 C9 121.0(4) . . ? C10 C11 C12 120.0(5) . . ? C11 C12 C13 120.7(5) . . ? C12 C13 C8 119.7(4) . . ? N2 C14 C15 109.3(3) . . ? N2 C14 C7 109.1(3) . . ? C15 C14 C7 110.0(3) . . ? C20 C15 C16 118.5(4) . . ? C20 C15 C14 121.0(4) . . ? C16 C15 C14 120.5(4) . . ? C15 C16 C17 121.5(5) . . ? C18 C17 C16 119.5(5) . . ? C17 C18 C19 120.2(5) . . ? C18 C19 C20 119.3(5) . . ? C15 C20 C19 120.9(5) . . ? N2 C21 C22 122.5(4) . . ? C23 C22 C26 106.9(4) . . ? C23 C22 C21 127.6(4) . . ? C26 C22 C21 125.1(5) . . ? C23 C22 Fe2 70.1(2) . . ? C26 C22 Fe2 69.4(2) . . ? C21 C22 Fe2 120.2(3) . . ? C24 C23 C22 109.2(4) . . ? C24 C23 Fe2 71.0(2) . . ? C22 C23 Fe2 69.4(2) . . ? C23 C24 C25 107.9(4) . . ? C23 C24 Fe2 69.2(2) . . ? C25 C24 Fe2 69.6(2) . . ? C26 C25 C24 107.6(4) . . ? C26 C25 Fe2 68.8(2) . . ? C24 C25 Fe2 70.3(2) . . ? C25 C26 C22 108.5(4) . . ? C25 C26 Fe2 70.8(2) . . ? C22 C26 Fe2 69.8(2) . . ? C28 C27 C31 107.4(5) . . ? C28 C27 C32 126.7(5) . . ? C31 C27 C32 125.9(5) . . ? C28 C27 Fe2 70.2(3) . . ? C31 C27 Fe2 68.8(3) . . ? C32 C27 Fe2 124.6(3) . . ? C29 C28 C27 107.5(5) . . ? C29 C28 Fe2 70.0(3) . . ? C27 C28 Fe2 69.1(3) . . ? C30 C29 C28 108.8(5) . . ? C30 C29 Fe2 68.8(3) . . ? C28 C29 Fe2 70.0(3) . . ? C31 C30 C29 108.5(5) . . ? C31 C30 Fe2 69.8(3) . . ? C29 C30 Fe2 71.0(3) . . ? C30 C31 C27 107.8(5) . . ? C30 C31 Fe2 69.8(3) . . ? C27 C31 Fe2 70.0(2) . . ? N3 C32 C27 124.2(4) . . ? N3 C33 C34 110.3(3) . . ? N3 C33 C40 109.9(3) . . ? C34 C33 C40 111.1(3) . . ? C39 C34 C35 119.7(4) . . ? C39 C34 C33 121.6(4) . . ? C35 C34 C33 118.6(4) . . ? C36 C35 C34 119.0(5) . . ? C37 C36 C35 121.0(5) . . ? C36 C37 C38 120.0(5) . . ? C37 C38 C39 119.7(5) . . ? C34 C39 C38 120.7(4) . . ? N4 C40 C41 111.6(3) . . ? N4 C40 C33 107.4(3) . . ? C41 C40 C33 109.8(3) . . ? C46 C41 C42 117.1(5) . . ? C46 C41 C40 120.8(5) . . ? C42 C41 C40 122.0(5) . . ? C43 C42 C41 121.1(5) . . ? C44 C43 C42 120.8(7) . . ? C43 C44 C45 120.2(7) . . ? C44 C45 C46 119.1(6) . . ? C41 C46 C45 121.6(5) . . ? N4 C47 C48 123.4(4) . . ? C49 C48 C52 106.1(4) . . ? C49 C48 C47 128.5(4) . . ? C52 C48 C47 125.1(5) . . ? C49 C48 Fe3 69.3(3) . . ? C52 C48 Fe3 69.1(3) . . ? C47 C48 Fe3 121.6(3) . . ? C50 C49 C48 109.8(5) . . ? C50 C49 Fe3 71.2(3) . . ? C48 C49 Fe3 70.1(3) . . ? C51 C50 C49 106.9(5) . . ? C51 C50 Fe3 69.2(3) . . ? C49 C50 Fe3 68.6(3) . . ? C50 C51 C52 110.1(5) . . ? C50 C51 Fe3 71.3(3) . . ? C52 C51 Fe3 69.7(3) . . ? C51 C52 C48 107.0(5) . . ? C51 C52 Fe3 69.9(3) . . ? C48 C52 Fe3 69.6(3) . . ? C57 C53 C54 107.0(4) . . ? C57 C53 C58 127.5(4) . . ? C54 C53 C58 125.2(4) . . ? C57 C53 Fe3 69.3(3) . . ? C54 C53 Fe3 69.6(3) . . ? C58 C53 Fe3 121.7(3) . . ? C55 C54 C53 107.2(4) . . ? C55 C54 Fe3 70.1(3) . . ? C53 C54 Fe3 69.1(3) . . ? C54 C55 C56 109.1(5) . . ? C54 C55 Fe3 69.6(3) . . ? C56 C55 Fe3 69.6(3) . . ? C57 C56 C55 107.5(4) . . ? C57 C56 Fe3 69.4(3) . . ? C55 C56 Fe3 69.9(3) . . ? C56 C57 C53 109.3(4) . . ? C56 C57 Fe3 70.5(3) . . ? C53 C57 Fe3 69.8(2) . . ? N5 C58 C53 126.0(4) . . ? N5 C59 C60 110.8(3) . . ? N5 C59 C66 109.5(3) . . ? C60 C59 C66 110.7(3) . . ? C61 C60 C65 117.7(5) . . ? C61 C60 C59 121.6(4) . . ? C65 C60 C59 120.7(5) . . ? C60 C61 C62 122.3(5) . . ? C63 C62 C61 118.9(5) . . ? C64 C63 C62 118.9(6) . . ? C63 C64 C65 122.4(5) . . ? C64 C65 C60 119.8(5) . . ? N6 C66 C67 109.0(3) . . ? N6 C66 C59 109.1(3) . . ? C67 C66 C59 111.7(3) . . ? C68 C67 C72 117.6(4) . . ? C68 C67 C66 121.0(4) . . ? C72 C67 C66 121.4(4) . . ? C67 C68 C69 121.7(4) . . ? C70 C69 C68 119.5(5) . . ? C71 C70 C69 120.6(5) . . ? C70 C71 C72 120.0(5) . . ? C67 C72 C71 120.6(4) . . ? N6 C73 C74 123.9(4) . . ? C75 C74 C78 107.1(4) . . ? C75 C74 C73 128.3(4) . . ? C78 C74 C73 124.4(4) . . ? C75 C74 Fe1 69.9(2) . . ? C78 C74 Fe1 69.3(2) . . ? C73 C74 Fe1 121.8(3) . . ? C76 C75 C74 108.5(4) . . ? C76 C75 Fe1 69.9(2) . . ? C74 C75 Fe1 69.1(2) . . ? C77 C76 C75 107.8(4) . . ? C77 C76 Fe1 70.3(3) . . ? C75 C76 Fe1 69.5(2) . . ? C76 C77 C78 108.9(4) . . ? C76 C77 Fe1 69.6(3) . . ? C78 C77 Fe1 68.7(2) . . ? C77 C78 C74 107.6(4) . . ? C77 C78 Fe1 70.7(3) . . ? C74 C78 Fe1 69.3(2) . . ? Cl1 C1S Cl2 116.3(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H2W N5 1.02(4) 1.87(4) 2.856(5) 161(4) . O1W H1W N3 0.75(5) 2.27(5) 3.010(5) 174(6) . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.71 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.202 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.045