# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1820 #B006775J #The first unambiguous determination of a nitrosyl-to-nitrite #conversion in an iron nitrosyl porphyrin. #==================== data_general _publ_contact_author ; Prof. George Richter-Addo Department of Chemistry University of Oklahoma 620 Parrington Oval Norman, OK 73019 USA ; _publ_contact_author_email gbrichteraddo@chemdept.chem.ou.edu _publ_contact_author_fax 1(405)3254811 _publ_contact_author_phone 1(405) _publ_requested_journal 'Journal name' loop_ _publ_author_name _publ_author_address 'Lin Cheng' ; Department of Chemistry University of Oklahoma 620 Parrington Oval Norman, OK 73019 USA ; 'George Richter-Addo' ; Department of Chemistry University of Oklahoma 620 Parrington Oval Norman, OK 73019 USA ; _publ_section_title ; article title here <----- ; #==================== data_n99039 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H64 Fe N9 O5' _chemical_formula_sum 'C64 H64 Fe N9 O5' _chemical_formula_weight 1095.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.7905(14) _cell_length_b 17.6238(13) _cell_length_c 20.2731(16) _cell_angle_alpha 90.00 _cell_angle_beta 111.519(2) _cell_angle_gamma 90.00 _cell_volume 5913.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used 7030 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2308 _exptl_absorpt_coefficient_mu 0.311 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.735 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 158(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART/P4' _diffrn_measurement_method 'phi scan frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 198 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.19 _diffrn_reflns_number 25127 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_sigmaI/netI 0.0871 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 22.50 _reflns_number_total 7705 _reflns_number_gt 4338 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1196P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7705 _refine_ls_number_parameters 803 _refine_ls_number_restraints 771 _refine_ls_R_factor_all 0.1313 _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.2134 _refine_ls_wR_factor_gt 0.1841 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.139 _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 0.71742(5) 0.25652(5) 0.40028(5) 0.0432(3) Uani 1 1 d . . . O1 O 0.7735(8) 0.2066(9) 0.5368(7) 0.111(4) Uani 0.521(11) 1 d P A 1 N5 N 0.746(3) 0.246(2) 0.487(3) 0.049(4) Uani 0.521(11) 1 d PU A 1 O1' O 0.7188(9) 0.2505(9) 0.5361(7) 0.111(4) Uani 0.48 1 d P A 2 N5' N 0.748(4) 0.261(2) 0.492(3) 0.049(4) Uani 0.48 1 d PU A 2 N1 N 0.8041(3) 0.1902(3) 0.3904(3) 0.0417(13) Uani 1 1 d . A . N2 N 0.6454(3) 0.1665(3) 0.3849(3) 0.0385(13) Uani 1 1 d . A . N3 N 0.6200(3) 0.3228(3) 0.3793(3) 0.0397(13) Uani 1 1 d . A . N4 N 0.7798(3) 0.3469(3) 0.3883(3) 0.0401(13) Uani 1 1 d . A . C1 C 0.8814(4) 0.2119(4) 0.3964(3) 0.0418(17) Uani 1 1 d . . . C2 C 0.9296(4) 0.1468(4) 0.3977(4) 0.0545(19) Uani 1 1 d . A . H2 H 0.9847 0.1466 0.4025 0.065 Uiso 1 1 calc R . . C3 C 0.8828(4) 0.0868(4) 0.3910(4) 0.057(2) Uani 1 1 d . . . H3 H 0.8984 0.0355 0.3893 0.068 Uiso 1 1 calc R A . C4 C 0.8039(4) 0.1122(4) 0.3868(4) 0.0428(17) Uani 1 1 d . A . C5 C 0.7413(4) 0.0648(4) 0.3840(3) 0.0436(17) Uani 1 1 d . . . C6 C 0.6678(4) 0.0911(4) 0.3847(3) 0.0425(17) Uani 1 1 d . A . C7 C 0.6035(4) 0.0423(4) 0.3853(4) 0.0522(19) Uani 1 1 d . . . H7 H 0.6042 -0.0116 0.3867 0.063 Uiso 1 1 calc R A . C8 C 0.5420(4) 0.0876(4) 0.3834(4) 0.054(2) Uani 1 1 d . A . H8 H 0.4906 0.0717 0.3824 0.065 Uiso 1 1 calc R . . C9 C 0.5683(4) 0.1640(3) 0.3834(3) 0.0413(17) Uani 1 1 d . . . C10 C 0.5186(4) 0.2262(4) 0.3793(3) 0.0415(16) Uani 1 1 d . A . C11 C 0.5450(4) 0.3011(4) 0.3775(3) 0.0402(16) Uani 1 1 d . . . C12 C 0.4949(4) 0.3666(4) 0.3720(4) 0.0510(18) Uani 1 1 d . A . H12 H 0.4407 0.3667 0.3699 0.061 Uiso 1 1 calc R . . C13 C 0.5394(4) 0.4275(4) 0.3704(4) 0.0540(19) Uani 1 1 d . . . H13 H 0.5224 0.4789 0.3671 0.065 Uiso 1 1 calc R A . C14 C 0.6168(4) 0.4010(4) 0.3745(3) 0.0427(17) Uani 1 1 d . A . C15 C 0.6805(4) 0.4486(3) 0.3766(3) 0.0429(17) Uani 1 1 d . . . C16 C 0.7560(4) 0.4235(4) 0.3837(3) 0.0418(17) Uani 1 1 d . A . C17 C 0.8227(4) 0.4711(4) 0.3883(4) 0.0544(19) Uani 1 1 d . . . H17 H 0.8225 0.5249 0.3863 0.065 Uiso 1 1 calc R A . C18 C 0.8852(4) 0.4262(4) 0.3957(4) 0.0552(19) Uani 1 1 d . A . H18 H 0.9377 0.4427 0.4003 0.066 Uiso 1 1 calc R . . C19 C 0.8605(4) 0.3487(4) 0.3957(3) 0.0419(17) Uani 1 1 d . . . C20 C 0.9081(4) 0.2861(4) 0.4003(3) 0.0405(16) Uani 1 1 d . A . C21 C 0.7522(4) -0.0187(4) 0.3780(4) 0.0480(18) Uani 1 1 d . A . C22 C 0.7876(4) -0.0636(4) 0.4382(4) 0.0524(19) Uani 1 1 d . . . C23 C 0.7985(4) -0.1412(4) 0.4308(5) 0.061(2) Uani 1 1 d . A . H23 H 0.8229 -0.1718 0.4717 0.073 Uiso 1 1 calc R . . C24 C 0.7742(5) -0.1729(4) 0.3651(5) 0.064(2) Uani 1 1 d . . . H24 H 0.7821 -0.2257 0.3606 0.077 Uiso 1 1 calc R A . C25 C 0.7382(5) -0.1297(4) 0.3047(5) 0.070(2) Uani 1 1 d . A . H25 H 0.7210 -0.1527 0.2592 0.083 Uiso 1 1 calc R . . C26 C 0.7273(4) -0.0520(4) 0.3113(4) 0.062(2) Uani 1 1 d . . . H26 H 0.7029 -0.0219 0.2701 0.074 Uiso 1 1 calc R A . N27 N 0.8126(4) -0.0261(3) 0.5045(3) 0.0634(17) Uani 1 1 d . A . H27N H 0.8007 0.0347 0.4966 0.076 Uiso 1 1 d R . . C28 C 0.8559(4) -0.0525(4) 0.5695(4) 0.060(2) Uani 1 1 d D . . O29 O 0.8779(3) -0.1194(3) 0.5811(3) 0.0781(17) Uani 1 1 d . A . C30 C 0.8792(3) 0.0043(4) 0.6296(4) 0.082(2) Uani 1 1 d DU A . C31 C 0.9329(6) 0.0652(5) 0.6176(6) 0.095(3) Uani 0.718(8) 1 d PDU A 1 H31A H 0.9791 0.0415 0.6104 0.142 Uiso 0.718(8) 1 d PR A 1 H31B H 0.9524 0.0986 0.6592 0.142 Uiso 0.718(8) 1 d PR A 1 H31C H 0.9020 0.0951 0.5756 0.142 Uiso 0.718(8) 1 d PR A 1 C32 C 0.8037(5) 0.0390(6) 0.6352(5) 0.087(3) Uani 0.718(8) 1 d PDU A 1 H32A H 0.7840 0.0799 0.6002 0.131 Uiso 0.718(8) 1 d PR A 1 H32B H 0.8164 0.0596 0.6829 0.131 Uiso 0.718(8) 1 d PR A 1 H32C H 0.7619 -0.0001 0.6260 0.131 Uiso 0.718(8) 1 d PR A 1 C33 C 0.9256(7) -0.0366(6) 0.6991(4) 0.097(3) Uani 0.718(8) 1 d PDU A 1 H33A H 0.8897 -0.0728 0.7096 0.146 Uiso 0.718(8) 1 d PR A 1 H33B H 0.9453 0.0005 0.7376 0.146 Uiso 0.718(8) 1 d PR A 1 H33C H 0.9716 -0.0639 0.6947 0.146 Uiso 0.718(8) 1 d PR A 1 C31' C 0.9699(5) 0.0197(12) 0.6562(10) 0.090(4) Uani 0.282(8) 1 d PDU A 2 H31D H 0.9992 -0.0246 0.6824 0.135 Uiso 0.282(8) 1 d PR A 2 H31E H 0.9825 0.0641 0.6876 0.135 Uiso 0.282(8) 1 d PR A 2 H31F H 0.9861 0.0295 0.6158 0.135 Uiso 0.282(8) 1 d PR A 2 C32' C 0.8354(13) 0.0793(6) 0.6041(8) 0.092(4) Uani 0.282(8) 1 d PDU A 2 H32D H 0.8589 0.1052 0.5735 0.138 Uiso 0.282(8) 1 d PR A 2 H32E H 0.8411 0.1115 0.6451 0.138 Uiso 0.282(8) 1 d PR A 2 H32F H 0.7780 0.0695 0.5774 0.138 Uiso 0.282(8) 1 d PR A 2 C33' C 0.8577(14) -0.0252(10) 0.6908(7) 0.092(4) Uani 0.282(8) 1 d PDU A 2 H33D H 0.7988 -0.0287 0.6760 0.138 Uiso 0.282(8) 1 d PR A 2 H33E H 0.8786 0.0097 0.7311 0.138 Uiso 0.282(8) 1 d PR A 2 H33F H 0.8816 -0.0755 0.7048 0.138 Uiso 0.282(8) 1 d PR A 2 C34 C 0.4335(4) 0.2142(4) 0.3728(4) 0.0446(17) Uani 1 1 d . . . C35 C 0.4128(4) 0.1958(4) 0.4320(4) 0.0497(18) Uani 1 1 d . A . C36 C 0.3329(5) 0.1832(4) 0.4230(5) 0.065(2) Uani 1 1 d . . . H36 H 0.3188 0.1701 0.4624 0.078 Uiso 1 1 calc R A . C37 C 0.2738(4) 0.1897(4) 0.3566(5) 0.072(2) Uani 1 1 d . A . H37 H 0.2189 0.1820 0.3510 0.086 Uiso 1 1 calc R . . C38 C 0.2923(5) 0.2070(5) 0.2983(5) 0.073(2) Uani 1 1 d . . . H38 H 0.2509 0.2102 0.2526 0.087 Uiso 1 1 calc R A . C39 C 0.3718(4) 0.2197(4) 0.3071(4) 0.060(2) Uani 1 1 d . A . H39 H 0.3847 0.2326 0.2669 0.072 Uiso 1 1 calc R . . N40 N 0.4766(4) 0.1930(4) 0.4971(3) 0.0657(18) Uani 1 1 d . . . H40N H 0.5430 0.1988 0.4948 0.079 Uiso 1 1 d R A . C41 C 0.4789(4) 0.1617(4) 0.5578(4) 0.073(2) Uani 1 1 d D A . O42 O 0.4175(4) 0.1376(4) 0.5668(3) 0.099(2) Uani 1 1 d . . . C43 C 0.5587(5) 0.1618(4) 0.6193(4) 0.098(2) Uani 1 1 d DU . . C44 C 0.6274(6) 0.1807(10) 0.5932(7) 0.105(4) Uani 0.509(9) 1 d PDU A 1 H44A H 0.6239 0.1472 0.5536 0.158 Uiso 0.509(9) 1 d PR A 1 H44B H 0.6795 0.1733 0.6320 0.158 Uiso 0.509(9) 1 d PR A 1 H44C H 0.6225 0.2336 0.5774 0.158 Uiso 0.509(9) 1 d PR A 1 C45 C 0.5763(8) 0.0882(6) 0.6594(7) 0.116(4) Uani 0.509(9) 1 d PDU A 1 H45A H 0.5318 0.0760 0.6752 0.173 Uiso 0.509(9) 1 d PR A 1 H45B H 0.6266 0.0929 0.7008 0.173 Uiso 0.509(9) 1 d PR A 1 H45C H 0.5819 0.0476 0.6285 0.173 Uiso 0.509(9) 1 d PR A 1 C46 C 0.5590(8) 0.2269(7) 0.6700(6) 0.106(4) Uani 0.509(9) 1 d PDU A 1 H46A H 0.5444 0.2744 0.6433 0.158 Uiso 0.509(9) 1 d PR A 1 H46B H 0.6130 0.2316 0.7067 0.158 Uiso 0.509(9) 1 d PR A 1 H46C H 0.5197 0.2159 0.6923 0.158 Uiso 0.509(9) 1 d PR A 1 C44' C 0.6173(7) 0.1097(9) 0.6016(7) 0.108(4) Uani 0.491(9) 1 d PDU A 2 H44D H 0.5922 0.0600 0.5869 0.162 Uiso 0.491(9) 1 d PR A 2 H44E H 0.6668 0.1038 0.6436 0.162 Uiso 0.491(9) 1 d PR A 2 H44F H 0.6307 0.1321 0.5630 0.162 Uiso 0.491(9) 1 d PR A 2 C45' C 0.5451(8) 0.1257(9) 0.6831(5) 0.103(4) Uani 0.491(9) 1 d PDU A 2 H45D H 0.5144 0.1608 0.7011 0.155 Uiso 0.491(9) 1 d PR A 2 H45E H 0.5975 0.1151 0.7206 0.155 Uiso 0.491(9) 1 d PR A 2 H45F H 0.5149 0.0783 0.6683 0.155 Uiso 0.491(9) 1 d PR A 2 C46' C 0.5930(8) 0.2399(5) 0.6385(8) 0.110(4) Uani 0.491(9) 1 d PDU A 2 H46D H 0.6084 0.2601 0.6001 0.165 Uiso 0.491(9) 1 d PR A 2 H46E H 0.6408 0.2377 0.6824 0.165 Uiso 0.491(9) 1 d PR A 2 H46F H 0.5524 0.2731 0.6454 0.165 Uiso 0.491(9) 1 d PR A 2 C47 C 0.6647(4) 0.5326(4) 0.3725(4) 0.0491(18) Uani 1 1 d . A . C48 C 0.6639(4) 0.5707(4) 0.4329(4) 0.0539(19) Uani 1 1 d . . . C49 C 0.6473(4) 0.6489(4) 0.4288(5) 0.061(2) Uani 1 1 d . A . H49 H 0.6453 0.6755 0.4689 0.073 Uiso 1 1 calc R . . C50 C 0.6339(4) 0.6865(5) 0.3659(5) 0.068(2) Uani 1 1 d . . . H50 H 0.6228 0.7394 0.3633 0.082 Uiso 1 1 calc R A . C51 C 0.6361(5) 0.6501(5) 0.3077(5) 0.072(2) Uani 1 1 d . A . H51 H 0.6276 0.6775 0.2652 0.086 Uiso 1 1 calc R . . C52 C 0.6512(4) 0.5711(4) 0.3107(4) 0.061(2) Uani 1 1 d . . . H52 H 0.6519 0.5450 0.2699 0.073 Uiso 1 1 calc R A . N53 N 0.6845(4) 0.5289(3) 0.4955(3) 0.0650(18) Uani 1 1 d . A . H53N H 0.6985 0.4669 0.4894 0.078 Uiso 1 1 d R . . C54 C 0.6795(4) 0.5464(4) 0.5589(4) 0.068(2) Uani 1 1 d D . . O55 O 0.6534(4) 0.6073(3) 0.5701(3) 0.093(2) Uani 1 1 d . A . C56 C 0.7062(4) 0.4864(4) 0.6161(4) 0.097(2) Uani 1 1 d DU A . C57 C 0.7089(10) 0.5208(7) 0.6861(5) 0.113(4) Uani 0.577(10) 1 d PDU A 1 H57A H 0.7411 0.4881 0.7255 0.169 Uiso 0.577(10) 1 d PR A 1 H57B H 0.6539 0.5250 0.6858 0.169 Uiso 0.577(10) 1 d PR A 1 H57C H 0.7336 0.5713 0.6920 0.169 Uiso 0.577(10) 1 d PR A 1 C58 C 0.7903(6) 0.4581(8) 0.6259(7) 0.109(4) Uani 0.577(10) 1 d PDU A 1 H58A H 0.8281 0.5010 0.6376 0.163 Uiso 0.577(10) 1 d PR A 1 H58B H 0.7893 0.4343 0.5819 0.163 Uiso 0.577(10) 1 d PR A 1 H58C H 0.8078 0.4209 0.6644 0.163 Uiso 0.577(10) 1 d PR A 1 C59 C 0.6464(8) 0.4212(6) 0.5970(7) 0.118(4) Uani 0.577(10) 1 d PDU A 1 H59A H 0.6476 0.3959 0.6404 0.177 Uiso 0.577(10) 1 d PR A 1 H59B H 0.6610 0.3848 0.5672 0.177 Uiso 0.577(10) 1 d PR A 1 H59C H 0.5920 0.4408 0.5711 0.177 Uiso 0.577(10) 1 d PR A 1 C57' C 0.7684(10) 0.5185(8) 0.6836(6) 0.116(4) Uani 0.423(10) 1 d PDU A 2 H57D H 0.7485 0.5664 0.6956 0.174 Uiso 0.423(10) 1 d PR A 2 H57E H 0.8192 0.5275 0.6764 0.174 Uiso 0.423(10) 1 d PR A 2 H57F H 0.7777 0.4822 0.7224 0.174 Uiso 0.423(10) 1 d PR A 2 C58' C 0.7428(12) 0.4187(7) 0.5918(8) 0.106(4) Uani 0.423(10) 1 d PDU A 2 H58D H 0.7921 0.4346 0.5848 0.159 Uiso 0.423(10) 1 d PR A 2 H58E H 0.7039 0.3991 0.5471 0.159 Uiso 0.423(10) 1 d PR A 2 H58F H 0.7560 0.3788 0.6279 0.159 Uiso 0.423(10) 1 d PR A 2 C59' C 0.6338(7) 0.4580(10) 0.6322(10) 0.110(4) Uani 0.423(10) 1 d PDU A 2 H59D H 0.6521 0.4220 0.6717 0.166 Uiso 0.423(10) 1 d PR A 2 H59E H 0.5956 0.4328 0.5901 0.166 Uiso 0.423(10) 1 d PR A 2 H59F H 0.6071 0.5011 0.6450 0.166 Uiso 0.423(10) 1 d PR A 2 C60 C 0.9958(4) 0.2994(4) 0.4084(4) 0.0425(17) Uani 1 1 d . . . C61 C 1.0541(4) 0.3125(3) 0.4745(4) 0.0411(16) Uani 1 1 d . A . C62 C 1.1346(4) 0.3247(4) 0.4818(4) 0.0539(19) Uani 1 1 d . . . H62 H 1.1751 0.3338 0.5271 0.065 Uiso 1 1 calc R A . C63 C 1.1537(5) 0.3235(4) 0.4222(5) 0.065(2) Uani 1 1 d . A . H63 H 1.2080 0.3320 0.4264 0.078 Uiso 1 1 calc R . . C64 C 1.0963(5) 0.3102(5) 0.3573(5) 0.077(3) Uani 1 1 d . . . H64 H 1.1110 0.3087 0.3168 0.092 Uiso 1 1 calc R A . C65 C 1.0171(4) 0.2988(5) 0.3497(4) 0.064(2) Uani 1 1 d . A . H65 H 0.9771 0.2906 0.3040 0.077 Uiso 1 1 calc R . . N66 N 1.0297(3) 0.3109(3) 0.5332(3) 0.0521(15) Uani 1 1 d . . . H66N H 0.9597 0.2944 0.5122 0.063 Uiso 1 1 d R A . C67 C 1.0709(5) 0.3289(4) 0.6016(4) 0.0522(18) Uani 1 1 d . A . O68 O 1.1408(3) 0.3510(3) 0.6236(3) 0.0644(14) Uani 1 1 d . . . C69 C 1.0249(5) 0.3201(5) 0.6526(4) 0.069(2) Uani 1 1 d . . . C70 C 0.9369(5) 0.2997(6) 0.6157(5) 0.096(3) Uani 1 1 d . A . H70A H 0.9103 0.3382 0.5798 0.144 Uiso 1 1 d R . . H70B H 0.9106 0.2977 0.6505 0.144 Uiso 1 1 d R . . H70C H 0.9326 0.2501 0.5929 0.144 Uiso 1 1 d R . . C71 C 1.0687(6) 0.2580(5) 0.7041(5) 0.093(3) Uani 1 1 d . A . H71A H 1.1252 0.2728 0.7290 0.140 Uiso 1 1 d R . . H71B H 1.0665 0.2107 0.6780 0.140 Uiso 1 1 d R . . H71C H 1.0426 0.2503 0.7386 0.140 Uiso 1 1 d R . . C72 C 1.0301(7) 0.3952(5) 0.6912(5) 0.108(3) Uani 1 1 d . A . H72A H 1.0868 0.4106 0.7132 0.162 Uiso 1 1 d R . . H72B H 1.0070 0.3892 0.7279 0.162 Uiso 1 1 d R . . H72C H 0.9999 0.4341 0.6573 0.162 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0331(6) 0.0456(6) 0.0529(6) 0.0043(5) 0.0181(5) 0.0026(5) O1 0.101(9) 0.146(11) 0.077(6) 0.022(7) 0.023(7) 0.023(6) N5 0.047(4) 0.049(10) 0.053(6) 0.005(8) 0.020(4) -0.001(8) O1' 0.101(9) 0.146(11) 0.077(6) 0.022(7) 0.023(7) 0.023(6) N5' 0.047(4) 0.049(10) 0.053(6) 0.005(8) 0.020(4) -0.001(8) N1 0.042(3) 0.039(4) 0.045(3) 0.005(3) 0.016(3) 0.004(3) N2 0.036(3) 0.039(3) 0.046(3) 0.002(2) 0.021(3) 0.000(2) N3 0.031(3) 0.040(3) 0.050(4) -0.003(3) 0.016(3) 0.001(2) N4 0.036(3) 0.043(3) 0.043(3) 0.004(3) 0.016(3) -0.002(3) C1 0.028(4) 0.047(4) 0.053(5) 0.005(3) 0.017(3) 0.004(3) C2 0.039(4) 0.049(5) 0.080(6) 0.003(4) 0.028(4) 0.003(4) C3 0.047(5) 0.046(5) 0.084(6) 0.002(4) 0.032(4) 0.012(4) C4 0.034(4) 0.042(4) 0.058(5) 0.005(3) 0.023(4) 0.007(3) C5 0.040(4) 0.049(4) 0.041(4) 0.004(3) 0.014(3) 0.005(3) C6 0.038(4) 0.044(4) 0.048(4) 0.003(3) 0.018(3) 0.000(3) C7 0.051(5) 0.041(4) 0.069(5) 0.003(4) 0.027(4) 0.003(4) C8 0.042(4) 0.050(5) 0.080(6) 0.001(4) 0.032(4) -0.002(4) C9 0.039(4) 0.036(4) 0.050(4) 0.004(3) 0.018(3) -0.002(3) C10 0.037(4) 0.039(4) 0.050(4) 0.001(3) 0.019(3) -0.002(3) C11 0.028(4) 0.048(4) 0.045(4) -0.001(3) 0.014(3) 0.012(3) C12 0.036(4) 0.054(5) 0.064(5) -0.001(4) 0.019(4) 0.001(4) C13 0.038(4) 0.045(4) 0.080(6) 0.000(4) 0.022(4) 0.007(3) C14 0.039(4) 0.041(4) 0.048(4) -0.001(3) 0.016(3) 0.001(3) C15 0.040(4) 0.035(4) 0.052(4) 0.002(3) 0.014(3) 0.002(3) C16 0.035(4) 0.039(4) 0.051(4) 0.003(3) 0.014(3) 0.001(3) C17 0.039(4) 0.046(4) 0.079(6) 0.002(4) 0.023(4) 0.002(4) C18 0.042(4) 0.059(5) 0.064(5) 0.008(4) 0.018(4) -0.007(4) C19 0.027(4) 0.049(4) 0.050(4) 0.002(3) 0.014(3) -0.003(3) C20 0.034(4) 0.052(5) 0.040(4) 0.005(3) 0.019(3) 0.007(3) C21 0.043(4) 0.046(4) 0.057(5) 0.006(4) 0.021(4) 0.010(3) C22 0.045(4) 0.047(5) 0.067(5) -0.004(4) 0.022(4) 0.001(4) C23 0.058(5) 0.040(5) 0.087(7) 0.011(4) 0.030(5) 0.008(4) C24 0.062(5) 0.044(5) 0.084(6) -0.007(5) 0.024(5) 0.007(4) C25 0.068(6) 0.055(5) 0.082(7) -0.015(5) 0.023(5) 0.007(4) C26 0.064(5) 0.053(5) 0.067(6) 0.001(4) 0.024(5) 0.011(4) N27 0.077(5) 0.047(4) 0.061(5) 0.013(3) 0.019(4) 0.017(3) C28 0.037(4) 0.074(6) 0.068(6) 0.003(5) 0.019(4) 0.007(4) O29 0.067(4) 0.076(4) 0.089(4) 0.023(3) 0.026(3) 0.019(3) C30 0.074(4) 0.090(4) 0.084(4) -0.001(4) 0.030(3) 0.014(3) C31 0.089(5) 0.093(5) 0.097(5) -0.008(4) 0.029(4) -0.003(4) C32 0.085(5) 0.098(5) 0.085(5) -0.006(4) 0.038(4) 0.014(4) C33 0.090(5) 0.098(5) 0.091(5) -0.002(4) 0.019(4) 0.013(4) C31' 0.083(6) 0.092(6) 0.091(6) -0.006(5) 0.028(5) 0.006(5) C32' 0.087(6) 0.097(6) 0.091(6) -0.005(5) 0.031(5) 0.008(5) C33' 0.088(6) 0.099(6) 0.088(6) -0.003(5) 0.032(5) 0.008(5) C34 0.036(4) 0.038(4) 0.058(5) -0.006(3) 0.014(4) 0.002(3) C35 0.039(4) 0.047(4) 0.066(5) -0.001(4) 0.023(4) 0.001(3) C36 0.041(5) 0.075(6) 0.091(7) -0.004(5) 0.039(5) -0.006(4) C37 0.026(4) 0.074(6) 0.116(8) -0.010(5) 0.028(5) -0.005(4) C38 0.038(5) 0.087(6) 0.087(7) -0.004(5) 0.015(5) 0.002(4) C39 0.051(5) 0.067(5) 0.065(6) 0.002(4) 0.025(5) 0.000(4) N40 0.047(4) 0.096(5) 0.058(4) 0.004(4) 0.024(4) 0.000(4) C41 0.063(6) 0.085(6) 0.077(7) 0.012(5) 0.033(5) 0.013(5) O42 0.090(5) 0.114(5) 0.103(5) 0.038(4) 0.047(4) 0.003(4) C43 0.095(4) 0.115(5) 0.092(4) 0.012(4) 0.045(4) 0.017(4) C44 0.100(6) 0.113(6) 0.102(6) 0.010(5) 0.036(5) 0.012(5) C45 0.112(6) 0.114(6) 0.108(6) 0.010(5) 0.027(5) 0.010(5) C46 0.098(6) 0.113(6) 0.103(6) 0.012(5) 0.034(5) -0.003(5) C44' 0.105(6) 0.116(6) 0.103(6) 0.011(5) 0.037(5) 0.013(5) C45' 0.105(6) 0.107(6) 0.096(6) 0.003(5) 0.035(5) 0.011(5) C46' 0.104(6) 0.114(6) 0.106(6) 0.013(5) 0.031(5) -0.001(5) C47 0.031(4) 0.048(5) 0.062(5) 0.006(4) 0.010(4) 0.001(3) C48 0.032(4) 0.046(5) 0.077(6) 0.000(4) 0.012(4) 0.003(3) C49 0.036(4) 0.050(5) 0.087(6) -0.014(4) 0.012(4) 0.006(3) C50 0.045(5) 0.049(5) 0.104(8) 0.003(5) 0.018(5) 0.004(4) C51 0.061(6) 0.055(6) 0.095(7) 0.019(5) 0.022(5) 0.004(4) C52 0.048(5) 0.057(5) 0.068(6) 0.007(4) 0.011(4) 0.006(4) N53 0.071(5) 0.054(4) 0.069(5) -0.010(4) 0.024(4) 0.008(3) C54 0.054(5) 0.066(6) 0.092(7) -0.004(5) 0.035(5) 0.006(4) O55 0.101(5) 0.077(4) 0.131(6) -0.008(4) 0.080(4) 0.008(4) C56 0.102(4) 0.107(4) 0.098(4) -0.005(3) 0.055(3) 0.011(3) C57 0.113(5) 0.117(5) 0.110(5) -0.003(4) 0.042(4) 0.008(4) C58 0.109(5) 0.111(5) 0.107(5) 0.004(4) 0.040(4) 0.007(4) C59 0.120(5) 0.116(5) 0.117(5) 0.005(4) 0.042(4) -0.002(4) C57' 0.116(5) 0.117(5) 0.113(5) 0.001(4) 0.041(4) -0.002(4) C58' 0.108(5) 0.108(5) 0.104(5) 0.002(4) 0.041(4) 0.006(4) C59' 0.112(5) 0.110(5) 0.113(5) 0.003(4) 0.045(4) 0.002(4) C60 0.035(4) 0.045(4) 0.050(5) 0.003(3) 0.019(4) 0.000(3) C61 0.025(4) 0.046(4) 0.052(5) 0.004(3) 0.014(4) 0.000(3) C62 0.035(4) 0.061(5) 0.066(5) 0.001(4) 0.019(4) -0.004(3) C63 0.039(5) 0.079(6) 0.083(7) 0.003(5) 0.028(5) -0.003(4) C64 0.052(5) 0.120(8) 0.071(6) 0.004(5) 0.038(5) -0.014(5) C65 0.040(5) 0.099(6) 0.054(5) 0.002(4) 0.019(4) -0.001(4) N66 0.037(3) 0.068(4) 0.048(4) 0.002(3) 0.011(3) -0.011(3) C67 0.048(5) 0.047(5) 0.055(5) 0.000(4) 0.012(4) 0.004(4) O68 0.053(3) 0.065(3) 0.062(4) -0.002(3) 0.005(3) -0.013(3) C69 0.079(6) 0.073(6) 0.058(5) -0.003(4) 0.029(5) -0.016(5) C70 0.066(6) 0.157(9) 0.078(7) -0.009(6) 0.043(5) -0.020(6) C71 0.108(8) 0.099(7) 0.081(6) 0.022(6) 0.044(6) 0.006(6) C72 0.138(10) 0.100(8) 0.099(8) -0.034(6) 0.059(7) -0.010(7) _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 N5 1.65(5) . ? Fe1 N5' 1.74(6) . ? Fe1 N2 1.991(5) . ? Fe1 N3 2.002(5) . ? Fe1 N1 2.003(5) . ? Fe1 N4 2.007(5) . ? O1 N5 1.17(5) . ? O1' N5' 1.20(7) . ? N1 C4 1.377(8) . ? N1 C1 1.389(7) . ? N2 C9 1.362(8) . ? N2 C6 1.387(7) . ? N3 C11 1.375(7) . ? N3 C14 1.382(7) . ? N4 C19 1.387(7) . ? N4 C16 1.407(8) . ? C1 C20 1.383(9) . ? C1 C2 1.428(9) . ? C2 C3 1.321(9) . ? C3 C4 1.446(9) . ? C4 C5 1.377(9) . ? C5 C6 1.394(9) . ? C5 C21 1.494(9) . ? C6 C7 1.434(9) . ? C7 C8 1.343(9) . ? C8 C9 1.426(9) . ? C9 C10 1.390(8) . ? C10 C11 1.408(8) . ? C10 C34 1.486(9) . ? C11 C12 1.436(8) . ? C12 C13 1.340(9) . ? C13 C14 1.428(9) . ? C14 C15 1.398(8) . ? C15 C16 1.371(8) . ? C15 C47 1.504(9) . ? C16 C17 1.428(9) . ? C17 C18 1.327(9) . ? C18 C19 1.434(9) . ? C19 C20 1.373(8) . ? C20 C60 1.525(8) . ? C21 C26 1.389(9) . ? C21 C22 1.396(9) . ? C22 C23 1.397(9) . ? C22 N27 1.415(9) . ? C23 C24 1.361(10) . ? C24 C25 1.384(10) . ? C25 C26 1.396(10) . ? N27 C28 1.343(8) . ? C28 O29 1.237(8) . ? C28 C30 1.512(8) . ? C30 C31 1.515(5) . ? C30 C32 1.519(5) . ? C30 C33' 1.519(6) . ? C30 C31' 1.525(6) . ? C30 C32' 1.526(6) . ? C30 C33 1.528(5) . ? C34 C39 1.384(9) . ? C34 C35 1.417(9) . ? C35 C36 1.384(9) . ? C35 N40 1.390(9) . ? C36 C37 1.375(11) . ? C37 C38 1.373(11) . ? C38 C39 1.378(10) . ? N40 C41 1.335(9) . ? C41 O42 1.246(8) . ? C41 C43 1.508(9) . ? C43 C46' 1.498(5) . ? C43 C45 1.502(5) . ? C43 C44' 1.528(5) . ? C43 C44 1.535(6) . ? C43 C45' 1.538(5) . ? C43 C46 1.539(5) . ? C47 C52 1.366(9) . ? C47 C48 1.401(9) . ? C48 N53 1.394(9) . ? C48 C49 1.407(9) . ? C49 C50 1.378(10) . ? C50 C51 1.356(11) . ? C51 C52 1.416(10) . ? N53 C54 1.356(8) . ? C54 O55 1.223(8) . ? C54 C56 1.512(9) . ? C56 C59 1.516(5) . ? C56 C57' 1.518(6) . ? C56 C58 1.519(5) . ? C56 C59' 1.525(6) . ? C56 C58' 1.525(5) . ? C56 C57 1.527(5) . ? C60 C65 1.373(9) . ? C60 C61 1.381(9) . ? C61 C62 1.401(8) . ? C61 N66 1.410(8) . ? C62 C63 1.369(9) . ? C63 C64 1.357(10) . ? C64 C65 1.376(10) . ? N66 C67 1.347(8) . ? C67 O68 1.221(8) . ? C67 C69 1.544(10) . ? C69 C70 1.510(11) . ? C69 C71 1.517(11) . ? C69 C72 1.523(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 N5 Fe1 N5' 9(2) . . ? N5 Fe1 N2 90.4(16) . . ? N5' Fe1 N2 97.8(17) . . ? N5 Fe1 N3 101.6(18) . . ? N5' Fe1 N3 96.2(18) . . ? N2 Fe1 N3 88.5(2) . . ? N5 Fe1 N1 95.1(18) . . ? N5' Fe1 N1 100.5(18) . . ? N2 Fe1 N1 89.7(2) . . ? N3 Fe1 N1 163.3(2) . . ? N5 Fe1 N4 104.4(16) . . ? N5' Fe1 N4 97.0(17) . . ? N2 Fe1 N4 165.2(2) . . ? N3 Fe1 N4 89.2(2) . . ? N1 Fe1 N4 88.3(2) . . ? O1 N5 Fe1 149(4) . . ? O1' N5' Fe1 137(4) . . ? C4 N1 C1 105.2(5) . . ? C4 N1 Fe1 126.9(4) . . ? C1 N1 Fe1 127.2(4) . . ? C9 N2 C6 104.9(5) . . ? C9 N2 Fe1 127.9(4) . . ? C6 N2 Fe1 126.5(4) . . ? C11 N3 C14 105.1(5) . . ? C11 N3 Fe1 126.9(4) . . ? C14 N3 Fe1 127.4(4) . . ? C19 N4 C16 105.1(5) . . ? C19 N4 Fe1 127.0(4) . . ? C16 N4 Fe1 127.1(4) . . ? C20 C1 N1 125.0(6) . . ? C20 C1 C2 124.6(6) . . ? N1 C1 C2 110.4(6) . . ? C3 C2 C1 106.9(6) . . ? C2 C3 C4 108.6(6) . . ? C5 C4 N1 126.5(6) . . ? C5 C4 C3 124.6(6) . . ? N1 C4 C3 108.8(6) . . ? C4 C5 C6 123.1(6) . . ? C4 C5 C21 118.3(6) . . ? C6 C5 C21 118.6(6) . . ? N2 C6 C5 126.2(6) . . ? N2 C6 C7 110.1(5) . . ? C5 C6 C7 123.7(6) . . ? C8 C7 C6 106.7(6) . . ? C7 C8 C9 107.3(6) . . ? N2 C9 C10 126.1(6) . . ? N2 C9 C8 111.0(5) . . ? C10 C9 C8 122.9(6) . . ? C9 C10 C11 122.0(6) . . ? C9 C10 C34 119.9(6) . . ? C11 C10 C34 118.0(5) . . ? N3 C11 C10 126.1(5) . . ? N3 C11 C12 110.3(6) . . ? C10 C11 C12 123.5(6) . . ? C13 C12 C11 106.9(6) . . ? C12 C13 C14 107.6(6) . . ? N3 C14 C15 125.8(6) . . ? N3 C14 C13 110.1(5) . . ? C15 C14 C13 124.0(6) . . ? C16 C15 C14 124.2(6) . . ? C16 C15 C47 118.6(6) . . ? C14 C15 C47 117.2(6) . . ? C15 C16 N4 125.2(6) . . ? C15 C16 C17 125.2(6) . . ? N4 C16 C17 109.6(5) . . ? C18 C17 C16 107.4(6) . . ? C17 C18 C19 108.9(6) . . ? C20 C19 N4 125.2(6) . . ? C20 C19 C18 125.7(6) . . ? N4 C19 C18 109.0(6) . . ? C19 C20 C1 124.4(6) . . ? C19 C20 C60 117.7(6) . . ? C1 C20 C60 117.9(5) . . ? C26 C21 C22 119.5(7) . . ? C26 C21 C5 119.4(6) . . ? C22 C21 C5 121.1(6) . . ? C21 C22 C23 119.8(7) . . ? C21 C22 N27 116.8(6) . . ? C23 C22 N27 123.5(7) . . ? C24 C23 C22 120.1(7) . . ? C23 C24 C25 121.2(7) . . ? C24 C25 C26 119.4(8) . . ? C21 C26 C25 120.1(7) . . ? C28 N27 C22 129.6(6) . . ? O29 C28 N27 123.0(6) . . ? O29 C28 C30 120.3(6) . . ? N27 C28 C30 116.7(6) . . ? C28 C30 C31 110.2(5) . . ? C28 C30 C32 109.7(5) . . ? C31 C30 C32 110.7(5) . . ? C28 C30 C33' 110.7(5) . . ? C31 C30 C33' 137.4(8) . . ? C32 C30 C33' 65.2(8) . . ? C28 C30 C31' 110.2(5) . . ? C31 C30 C31' 44.2(9) . . ? C32 C30 C31' 138.7(8) . . ? C33' C30 C31' 108.8(5) . . ? C28 C30 C32' 110.3(5) . . ? C31 C30 C32' 66.8(9) . . ? C32 C30 C32' 47.1(8) . . ? C33' C30 C32' 108.7(5) . . ? C31' C30 C32' 108.0(5) . . ? C28 C30 C33 109.0(5) . . ? C31 C30 C33 108.9(5) . . ? C32 C30 C33 108.3(5) . . ? C33' C30 C33 45.4(8) . . ? C31' C30 C33 67.3(9) . . ? C32' C30 C33 139.2(8) . . ? C39 C34 C35 118.2(6) . . ? C39 C34 C10 119.8(6) . . ? C35 C34 C10 122.0(6) . . ? C36 C35 N40 124.2(7) . . ? C36 C35 C34 119.9(7) . . ? N40 C35 C34 115.9(6) . . ? C37 C36 C35 119.7(7) . . ? C38 C37 C36 121.5(7) . . ? C37 C38 C39 118.9(8) . . ? C38 C39 C34 121.8(7) . . ? C41 N40 C35 128.8(6) . . ? O42 C41 N40 123.0(7) . . ? O42 C41 C43 119.3(6) . . ? N40 C41 C43 117.6(6) . . ? C46' C43 C45 132.0(8) . . ? C46' C43 C41 112.7(5) . . ? C45 C43 C41 113.1(5) . . ? C46' C43 C44' 111.3(5) . . ? C45 C43 C44' 65.4(6) . . ? C41 C43 C44' 108.8(5) . . ? C46' C43 C44 65.8(6) . . ? C45 C43 C44 109.9(5) . . ? C41 C43 C44 110.0(5) . . ? C44' C43 C44 49.5(6) . . ? C46' C43 C45' 109.7(5) . . ? C45 C43 C45' 41.7(6) . . ? C41 C43 C45' 107.7(5) . . ? C44' C43 C45' 106.3(5) . . ? C44 C43 C45' 140.3(8) . . ? C46' C43 C46 40.7(6) . . ? C45 C43 C46 109.5(5) . . ? C41 C43 C46 109.0(5) . . ? C44' C43 C46 140.3(8) . . ? C44 C43 C46 105.1(5) . . ? C45' C43 C46 73.1(6) . . ? C52 C47 C48 120.6(7) . . ? C52 C47 C15 120.5(7) . . ? C48 C47 C15 118.9(6) . . ? N53 C48 C47 117.3(6) . . ? N53 C48 C49 123.4(7) . . ? C47 C48 C49 119.2(7) . . ? C50 C49 C48 119.1(8) . . ? C51 C50 C49 121.9(8) . . ? C50 C51 C52 119.6(8) . . ? C47 C52 C51 119.7(7) . . ? C54 N53 C48 131.0(6) . . ? O55 C54 N53 122.4(7) . . ? O55 C54 C56 120.4(6) . . ? N53 C54 C56 117.2(6) . . ? C54 C56 C59 109.8(5) . . ? C54 C56 C57' 110.6(5) . . ? C59 C56 C57' 136.4(8) . . ? C54 C56 C58 110.3(5) . . ? C59 C56 C58 110.5(5) . . ? C57' C56 C58 69.3(7) . . ? C54 C56 C59' 109.9(5) . . ? C59 C56 C59' 40.3(7) . . ? C57' C56 C59' 108.9(5) . . ? C58 C56 C59' 137.2(8) . . ? C54 C56 C58' 110.5(5) . . ? C59 C56 C58' 70.6(7) . . ? C57' C56 C58' 109.0(5) . . ? C58 C56 C58' 43.0(7) . . ? C59' C56 C58' 107.9(5) . . ? C54 C56 C57 109.2(5) . . ? C59 C56 C57 108.5(5) . . ? C57' C56 C57 41.5(7) . . ? C58 C56 C57 108.4(5) . . ? C59' C56 C57 70.9(7) . . ? C58' C56 C57 137.6(8) . . ? C65 C60 C61 119.6(6) . . ? C65 C60 C20 120.1(6) . . ? C61 C60 C20 120.4(5) . . ? C60 C61 C62 120.3(6) . . ? C60 C61 N66 117.5(5) . . ? C62 C61 N66 122.3(6) . . ? C63 C62 C61 118.6(7) . . ? C64 C63 C62 121.1(7) . . ? C63 C64 C65 120.6(7) . . ? C60 C65 C64 119.9(7) . . ? C67 N66 C61 130.1(6) . . ? O68 C67 N66 123.3(7) . . ? O68 C67 C69 120.4(7) . . ? N66 C67 C69 116.3(7) . . ? C70 C69 C71 110.3(7) . . ? C70 C69 C72 108.5(8) . . ? C71 C69 C72 110.8(7) . . ? C70 C69 C67 113.6(7) . . ? C71 C69 C67 105.6(7) . . ? C72 C69 C67 108.0(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5' Fe1 N5 O1 -162(34) . . . . ? N2 Fe1 N5 O1 54(9) . . . . ? N3 Fe1 N5 O1 143(8) . . . . ? N1 Fe1 N5 O1 -35(9) . . . . ? N4 Fe1 N5 O1 -125(8) . . . . ? N5 Fe1 N5' O1' -73(24) . . . . ? N2 Fe1 N5' O1' -37(5) . . . . ? N3 Fe1 N5' O1' 52(5) . . . . ? N1 Fe1 N5' O1' -128(4) . . . . ? N4 Fe1 N5' O1' 142(4) . . . . ? N5 Fe1 N1 C4 81.5(16) . . . . ? N5' Fe1 N1 C4 89.1(18) . . . . ? N2 Fe1 N1 C4 -8.8(5) . . . . ? N3 Fe1 N1 C4 -92.6(8) . . . . ? N4 Fe1 N1 C4 -174.1(5) . . . . ? N5 Fe1 N1 C1 -87.9(16) . . . . ? N5' Fe1 N1 C1 -80.4(18) . . . . ? N2 Fe1 N1 C1 -178.3(5) . . . . ? N3 Fe1 N1 C1 97.9(8) . . . . ? N4 Fe1 N1 C1 16.4(5) . . . . ? N5 Fe1 N2 C9 85.3(19) . . . . ? N5' Fe1 N2 C9 79.8(19) . . . . ? N3 Fe1 N2 C9 -16.3(5) . . . . ? N1 Fe1 N2 C9 -179.6(5) . . . . ? N4 Fe1 N2 C9 -97.5(9) . . . . ? N5 Fe1 N2 C6 -83.7(19) . . . . ? N5' Fe1 N2 C6 -89.2(19) . . . . ? N3 Fe1 N2 C6 174.7(5) . . . . ? N1 Fe1 N2 C6 11.3(5) . . . . ? N4 Fe1 N2 C6 93.4(9) . . . . ? N5 Fe1 N3 C11 -75.0(16) . . . . ? N5' Fe1 N3 C11 -82.7(17) . . . . ? N2 Fe1 N3 C11 15.1(5) . . . . ? N1 Fe1 N3 C11 99.0(8) . . . . ? N4 Fe1 N3 C11 -179.6(5) . . . . ? N5 Fe1 N3 C14 94.2(16) . . . . ? N5' Fe1 N3 C14 86.5(17) . . . . ? N2 Fe1 N3 C14 -175.7(5) . . . . ? N1 Fe1 N3 C14 -91.8(8) . . . . ? N4 Fe1 N3 C14 -10.4(5) . . . . ? N5 Fe1 N4 C19 77.4(19) . . . . ? N5' Fe1 N4 C19 83.0(19) . . . . ? N2 Fe1 N4 C19 -99.7(9) . . . . ? N3 Fe1 N4 C19 179.2(5) . . . . ? N1 Fe1 N4 C19 -17.4(5) . . . . ? N5 Fe1 N4 C16 -89.9(19) . . . . ? N5' Fe1 N4 C16 -84.4(19) . . . . ? N2 Fe1 N4 C16 93.0(9) . . . . ? N3 Fe1 N4 C16 11.8(5) . . . . ? N1 Fe1 N4 C16 175.3(5) . . . . ? C4 N1 C1 C20 178.7(6) . . . . ? Fe1 N1 C1 C20 -10.0(9) . . . . ? C4 N1 C1 C2 -1.0(7) . . . . ? Fe1 N1 C1 C2 170.3(4) . . . . ? C20 C1 C2 C3 -178.3(7) . . . . ? N1 C1 C2 C3 1.4(8) . . . . ? C1 C2 C3 C4 -1.2(8) . . . . ? C1 N1 C4 C5 176.5(6) . . . . ? Fe1 N1 C4 C5 5.2(10) . . . . ? C1 N1 C4 C3 0.2(7) . . . . ? Fe1 N1 C4 C3 -171.1(4) . . . . ? C2 C3 C4 C5 -175.8(7) . . . . ? C2 C3 C4 N1 0.7(8) . . . . ? N1 C4 C5 C6 -0.2(11) . . . . ? C3 C4 C5 C6 175.6(7) . . . . ? N1 C4 C5 C21 178.2(6) . . . . ? C3 C4 C5 C21 -6.1(10) . . . . ? C9 N2 C6 C5 178.2(6) . . . . ? Fe1 N2 C6 C5 -10.8(9) . . . . ? C9 N2 C6 C7 -1.9(7) . . . . ? Fe1 N2 C6 C7 169.1(4) . . . . ? C4 C5 C6 N2 3.1(11) . . . . ? C21 C5 C6 N2 -175.2(6) . . . . ? C4 C5 C6 C7 -176.8(6) . . . . ? C21 C5 C6 C7 4.9(10) . . . . ? N2 C6 C7 C8 2.1(8) . . . . ? C5 C6 C7 C8 -178.0(7) . . . . ? C6 C7 C8 C9 -1.4(8) . . . . ? C6 N2 C9 C10 -176.4(6) . . . . ? Fe1 N2 C9 C10 12.7(10) . . . . ? C6 N2 C9 C8 1.1(7) . . . . ? Fe1 N2 C9 C8 -169.8(4) . . . . ? C7 C8 C9 N2 0.2(8) . . . . ? C7 C8 C9 C10 177.8(6) . . . . ? N2 C9 C10 C11 -1.2(11) . . . . ? C8 C9 C10 C11 -178.4(6) . . . . ? N2 C9 C10 C34 175.6(6) . . . . ? C8 C9 C10 C34 -1.6(10) . . . . ? C14 N3 C11 C10 178.4(6) . . . . ? Fe1 N3 C11 C10 -10.5(9) . . . . ? C14 N3 C11 C12 -0.4(7) . . . . ? Fe1 N3 C11 C12 170.7(4) . . . . ? C9 C10 C11 N3 0.2(10) . . . . ? C34 C10 C11 N3 -176.7(6) . . . . ? C9 C10 C11 C12 178.8(6) . . . . ? C34 C10 C11 C12 2.0(10) . . . . ? N3 C11 C12 C13 0.1(8) . . . . ? C10 C11 C12 C13 -178.8(6) . . . . ? C11 C12 C13 C14 0.3(8) . . . . ? C11 N3 C14 C15 177.8(6) . . . . ? Fe1 N3 C14 C15 6.7(9) . . . . ? C11 N3 C14 C13 0.6(7) . . . . ? Fe1 N3 C14 C13 -170.5(4) . . . . ? C12 C13 C14 N3 -0.5(8) . . . . ? C12 C13 C14 C15 -177.8(6) . . . . ? N3 C14 C15 C16 0.1(11) . . . . ? C13 C14 C15 C16 177.0(7) . . . . ? N3 C14 C15 C47 -178.4(6) . . . . ? C13 C14 C15 C47 -1.5(10) . . . . ? C14 C15 C16 N4 1.5(11) . . . . ? C47 C15 C16 N4 180.0(6) . . . . ? C14 C15 C16 C17 -177.9(7) . . . . ? C47 C15 C16 C17 0.6(10) . . . . ? C19 N4 C16 C15 -179.4(6) . . . . ? Fe1 N4 C16 C15 -9.8(9) . . . . ? C19 N4 C16 C17 0.1(7) . . . . ? Fe1 N4 C16 C17 169.6(4) . . . . ? C15 C16 C17 C18 179.1(7) . . . . ? N4 C16 C17 C18 -0.3(8) . . . . ? C16 C17 C18 C19 0.4(8) . . . . ? C16 N4 C19 C20 -178.3(6) . . . . ? Fe1 N4 C19 C20 12.1(9) . . . . ? C16 N4 C19 C18 0.2(7) . . . . ? Fe1 N4 C19 C18 -169.4(4) . . . . ? C17 C18 C19 C20 178.1(7) . . . . ? C17 C18 C19 N4 -0.4(8) . . . . ? N4 C19 C20 C1 1.7(11) . . . . ? C18 C19 C20 C1 -176.5(6) . . . . ? N4 C19 C20 C60 -179.9(6) . . . . ? C18 C19 C20 C60 1.9(10) . . . . ? N1 C1 C20 C19 -2.8(11) . . . . ? C2 C1 C20 C19 176.8(6) . . . . ? N1 C1 C20 C60 178.7(6) . . . . ? C2 C1 C20 C60 -1.6(10) . . . . ? C4 C5 C21 C26 -92.1(8) . . . . ? C6 C5 C21 C26 86.3(8) . . . . ? C4 C5 C21 C22 87.3(8) . . . . ? C6 C5 C21 C22 -94.3(8) . . . . ? C26 C21 C22 C23 0.8(10) . . . . ? C5 C21 C22 C23 -178.6(6) . . . . ? C26 C21 C22 N27 179.2(6) . . . . ? C5 C21 C22 N27 -0.3(9) . . . . ? C21 C22 C23 C24 -0.5(10) . . . . ? N27 C22 C23 C24 -178.7(7) . . . . ? C22 C23 C24 C25 -0.3(11) . . . . ? C23 C24 C25 C26 0.6(12) . . . . ? C22 C21 C26 C25 -0.5(10) . . . . ? C5 C21 C26 C25 179.0(6) . . . . ? C24 C25 C26 C21 -0.3(11) . . . . ? C21 C22 N27 C28 -171.6(7) . . . . ? C23 C22 N27 C28 6.7(11) . . . . ? C22 N27 C28 O29 -3.8(11) . . . . ? C22 N27 C28 C30 174.6(6) . . . . ? O29 C28 C30 C31 116.2(7) . . . . ? N27 C28 C30 C31 -62.3(7) . . . . ? O29 C28 C30 C32 -121.7(7) . . . . ? N27 C28 C30 C32 59.8(7) . . . . ? O29 C28 C30 C33' -51.6(12) . . . . ? N27 C28 C30 C33' 129.9(11) . . . . ? O29 C28 C30 C31' 68.9(12) . . . . ? N27 C28 C30 C31' -109.6(11) . . . . ? O29 C28 C30 C32' -172.0(11) . . . . ? N27 C28 C30 C32' 9.5(11) . . . . ? O29 C28 C30 C33 -3.2(8) . . . . ? N27 C28 C30 C33 178.3(7) . . . . ? C9 C10 C34 C39 -99.8(8) . . . . ? C11 C10 C34 C39 77.2(8) . . . . ? C9 C10 C34 C35 79.2(8) . . . . ? C11 C10 C34 C35 -103.9(7) . . . . ? C39 C34 C35 C36 0.6(10) . . . . ? C10 C34 C35 C36 -178.3(6) . . . . ? C39 C34 C35 N40 -178.3(6) . . . . ? C10 C34 C35 N40 2.8(9) . . . . ? N40 C35 C36 C37 177.9(7) . . . . ? C34 C35 C36 C37 -0.9(11) . . . . ? C35 C36 C37 C38 1.3(12) . . . . ? C36 C37 C38 C39 -1.4(12) . . . . ? C37 C38 C39 C34 1.1(12) . . . . ? C35 C34 C39 C38 -0.7(11) . . . . ? C10 C34 C39 C38 178.2(7) . . . . ? C36 C35 N40 C41 17.5(12) . . . . ? C34 C35 N40 C41 -163.6(7) . . . . ? C35 N40 C41 O42 -9.6(13) . . . . ? C35 N40 C41 C43 175.5(6) . . . . ? O42 C41 C43 C46' -118.3(10) . . . . ? N40 C41 C43 C46' 56.8(9) . . . . ? O42 C41 C43 C45 47.1(10) . . . . ? N40 C41 C43 C45 -137.8(9) . . . . ? O42 C41 C43 C44' 117.7(9) . . . . ? N40 C41 C43 C44' -67.2(9) . . . . ? O42 C41 C43 C44 170.4(9) . . . . ? N40 C41 C43 C44 -14.5(9) . . . . ? O42 C41 C43 C45' 2.9(10) . . . . ? N40 C41 C43 C45' 178.0(9) . . . . ? O42 C41 C43 C46 -74.8(9) . . . . ? N40 C41 C43 C46 100.3(9) . . . . ? C16 C15 C47 C52 78.6(9) . . . . ? C14 C15 C47 C52 -102.9(8) . . . . ? C16 C15 C47 C48 -101.6(8) . . . . ? C14 C15 C47 C48 77.0(8) . . . . ? C52 C47 C48 N53 -175.1(6) . . . . ? C15 C47 C48 N53 5.1(9) . . . . ? C52 C47 C48 C49 1.3(10) . . . . ? C15 C47 C48 C49 -178.5(6) . . . . ? N53 C48 C49 C50 174.8(7) . . . . ? C47 C48 C49 C50 -1.4(10) . . . . ? C48 C49 C50 C51 0.2(11) . . . . ? C49 C50 C51 C52 1.1(12) . . . . ? C48 C47 C52 C51 -0.1(10) . . . . ? C15 C47 C52 C51 179.8(6) . . . . ? C50 C51 C52 C47 -1.1(11) . . . . ? C47 C48 N53 C54 -170.5(7) . . . . ? C49 C48 N53 C54 13.3(12) . . . . ? C48 N53 C54 O55 0.2(12) . . . . ? C48 N53 C54 C56 179.0(6) . . . . ? O55 C54 C56 C59 108.8(9) . . . . ? N53 C54 C56 C59 -70.0(9) . . . . ? O55 C54 C56 C57' -54.4(11) . . . . ? N53 C54 C56 C57' 126.8(10) . . . . ? O55 C54 C56 C58 -129.1(9) . . . . ? N53 C54 C56 C58 52.0(9) . . . . ? O55 C54 C56 C59' 65.9(11) . . . . ? N53 C54 C56 C59' -113.0(10) . . . . ? O55 C54 C56 C58' -175.2(11) . . . . ? N53 C54 C56 C58' 5.9(11) . . . . ? O55 C54 C56 C57 -10.1(9) . . . . ? N53 C54 C56 C57 171.0(8) . . . . ? C19 C20 C60 C65 -95.5(8) . . . . ? C1 C20 C60 C65 83.0(8) . . . . ? C19 C20 C60 C61 84.3(8) . . . . ? C1 C20 C60 C61 -97.2(8) . . . . ? C65 C60 C61 C62 -0.2(10) . . . . ? C20 C60 C61 C62 -179.9(6) . . . . ? C65 C60 C61 N66 -178.6(6) . . . . ? C20 C60 C61 N66 1.6(9) . . . . ? C60 C61 C62 C63 0.0(10) . . . . ? N66 C61 C62 C63 178.3(6) . . . . ? C61 C62 C63 C64 -0.4(11) . . . . ? C62 C63 C64 C65 1.0(13) . . . . ? C61 C60 C65 C64 0.8(11) . . . . ? C20 C60 C65 C64 -179.4(7) . . . . ? C63 C64 C65 C60 -1.2(13) . . . . ? C60 C61 N66 C67 -172.4(6) . . . . ? C62 C61 N66 C67 9.2(11) . . . . ? C61 N66 C67 O68 0.2(12) . . . . ? C61 N66 C67 C69 -179.7(6) . . . . ? O68 C67 C69 C70 174.3(7) . . . . ? N66 C67 C69 C70 -5.8(10) . . . . ? O68 C67 C69 C71 -64.7(9) . . . . ? N66 C67 C69 C71 115.2(7) . . . . ? O68 C67 C69 C72 53.8(10) . . . . ? N66 C67 C69 C72 -126.3(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.575 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.062 #===END #==================== data_n00018 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C69 H69 Fe N10 O6) (C H Cl3)' _chemical_formula_sum 'C70 H70 Cl3 Fe N10 O6' _chemical_formula_weight 1309.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 18.7122(8) _cell_length_b 19.0244(8) _cell_length_c 18.4955(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.543(2) _cell_angle_gamma 90.00 _cell_volume 6581.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 7802 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 28.68 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2740 _exptl_absorpt_coefficient_mu 0.411 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8025 _exptl_absorpt_correction_T_max 0.9918 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_method '\w scan frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 266 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.05 _diffrn_reflns_number 17387 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5792 _reflns_number_gt 4303 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1150P)^2^+13.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5792 _refine_ls_number_parameters 490 _refine_ls_number_restraints 121 _refine_ls_R_factor_all 0.0882 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.2098 _refine_ls_wR_factor_gt 0.1891 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.005 _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 0.5000 0.86040(3) 0.2500 0.0252(2) Uani 1 2 d S . . O1 O 0.44921(15) 0.72588(14) 0.22201(16) 0.0508(7) Uani 1 1 d . . . O2 O 0.18219(19) 0.63402(19) 0.1154(2) 0.0738(10) Uani 1 1 d . . . O3 O 0.3473(3) 0.6747(3) 0.5772(3) 0.1105(16) Uani 1 1 d . . . N1 N 0.40338(14) 0.85759(14) 0.29266(14) 0.0266(6) Uani 1 1 d . . . N2 N 0.45660(15) 0.86149(14) 0.15085(14) 0.0268(6) Uani 1 1 d . . . N3 N 0.5000 0.7581(2) 0.2500 0.0319(9) Uani 1 2 d S . . N4 N 0.5000 0.9707(2) 0.2500 0.0278(9) Uani 1 2 d S . . C1 C 0.49085(19) 0.86709(17) 0.08632(17) 0.0297(7) Uani 1 1 d . . . C2 C 0.4396(2) 0.86594(19) 0.02713(19) 0.0372(8) Uani 1 1 d . . . H2 H 0.4497 0.8701 -0.0228 0.045 Uiso 1 1 calc R . . C3 C 0.3750(2) 0.8579(2) 0.05553(19) 0.0376(9) Uani 1 1 d . . . H3 H 0.3307 0.8544 0.0294 0.045 Uiso 1 1 calc R . . C4 C 0.38499(18) 0.85545(17) 0.13277(18) 0.0301(7) Uani 1 1 d . . . C5 C 0.32975(18) 0.84814(17) 0.18073(19) 0.0299(8) Uani 1 1 d . . . C6 C 0.33917(18) 0.84884(17) 0.25570(19) 0.0289(7) Uani 1 1 d . . . C7 C 0.28250(19) 0.84432(19) 0.3057(2) 0.0356(8) Uani 1 1 d . . . H7 H 0.2333 0.8374 0.2937 0.043 Uiso 1 1 calc R . . C8 C 0.31098(19) 0.85158(19) 0.3724(2) 0.0361(8) Uani 1 1 d . . . H8 H 0.2859 0.8514 0.4164 0.043 Uiso 1 1 calc R . . C9 C 0.38689(18) 0.85963(17) 0.36467(18) 0.0296(7) Uani 1 1 d . . . C10 C 0.43565(19) 0.86813(17) 0.42193(18) 0.0296(7) Uani 1 1 d . . . C11 C 0.25470(19) 0.8436(2) 0.1500(2) 0.0378(9) Uani 1 1 d . . . C12 C 0.2238(2) 0.7789(2) 0.1306(2) 0.0459(10) Uani 1 1 d . . . C13 C 0.1547(2) 0.7778(3) 0.1006(3) 0.0661(14) Uani 1 1 d . . . H13 H 0.1332 0.7343 0.0870 0.079 Uiso 1 1 calc R . . C14 C 0.1177(3) 0.8394(3) 0.0908(3) 0.0822(18) Uani 1 1 d . . . H14 H 0.0707 0.8382 0.0701 0.099 Uiso 1 1 calc R . . C15 C 0.1471(3) 0.9023(3) 0.1101(4) 0.0857(19) Uani 1 1 d . . . H15 H 0.1207 0.9446 0.1034 0.103 Uiso 1 1 calc R . . C16 C 0.2158(2) 0.9040(2) 0.1395(3) 0.0608(13) Uani 1 1 d . . . H16 H 0.2365 0.9479 0.1527 0.073 Uiso 1 1 calc R . . N17 N 0.26394(18) 0.71747(18) 0.1422(2) 0.0566(10) Uani 1 1 d . . . H17 H 0.3089 0.7239 0.1557 0.068 Uiso 1 1 calc R . . C18 C 0.2427(2) 0.6491(2) 0.1356(2) 0.0490(11) Uani 1 1 d . . . C19 C 0.2985(2) 0.5931(2) 0.1537(3) 0.0626(13) Uani 1 1 d . . . C20 C 0.3204(3) 0.5982(3) 0.2362(3) 0.0881(19) Uani 1 1 d . . . H20A H 0.2781 0.5911 0.2654 0.132 Uiso 1 1 calc R . . H20B H 0.3407 0.6447 0.2464 0.132 Uiso 1 1 calc R . . H20C H 0.3560 0.5620 0.2481 0.132 Uiso 1 1 calc R . . C21 C 0.2681(4) 0.5215(3) 0.1385(7) 0.160(5) Uani 1 1 d . . . H21A H 0.2525 0.5186 0.0876 0.240 Uiso 1 1 calc R . . H21B H 0.2271 0.5133 0.1694 0.240 Uiso 1 1 calc R . . H21C H 0.3047 0.4858 0.1487 0.240 Uiso 1 1 calc R . . C22 C 0.3663(3) 0.6043(3) 0.1119(3) 0.0724(15) Uani 1 1 d . . . H22A H 0.3549 0.6031 0.0599 0.109 Uiso 1 1 calc R . . H22B H 0.4007 0.5670 0.1241 0.109 Uiso 1 1 calc R . . H22C H 0.3871 0.6501 0.1247 0.109 Uiso 1 1 calc R . . C23 C 0.40757(19) 0.87581(19) 0.49706(18) 0.0340(8) Uani 1 1 d . . . C24 C 0.3893(2) 0.8172(2) 0.5372(2) 0.0423(9) Uani 1 1 d . . . C25 C 0.3637(2) 0.8247(3) 0.6067(2) 0.0521(11) Uani 1 1 d . . . H25 H 0.3512 0.7846 0.6342 0.062 Uiso 1 1 calc R . . C26 C 0.3568(2) 0.8919(3) 0.6352(2) 0.0532(12) Uani 1 1 d . . . H26 H 0.3387 0.8975 0.6823 0.064 Uiso 1 1 calc R . . C27 C 0.3756(2) 0.9499(3) 0.5967(2) 0.0535(11) Uani 1 1 d . . . H27 H 0.3714 0.9953 0.6174 0.064 Uiso 1 1 calc R . . C28 C 0.4008(2) 0.9424(2) 0.5274(2) 0.0441(9) Uani 1 1 d . . . H28 H 0.4135 0.9828 0.5005 0.053 Uiso 1 1 calc R . . N29 N 0.4003(2) 0.75047(19) 0.50408(19) 0.0593(10) Uani 1 1 d . . . H29 H 0.4256 0.7526 0.4648 0.071 Uiso 1 1 calc R . . C30 C 0.3806(3) 0.6883(3) 0.5202(3) 0.0674(14) Uani 1 1 d . . . C31 C 0.3921(2) 0.6296(2) 0.4669(3) 0.0517(11) Uani 1 1 d . . . C32 C 0.4334(4) 0.6507(3) 0.4008(4) 0.095(2) Uani 1 1 d . . . H32A H 0.4044 0.6830 0.3709 0.143 Uiso 1 1 calc R . . H32B H 0.4445 0.6087 0.3725 0.143 Uiso 1 1 calc R . . H32C H 0.4779 0.6741 0.4162 0.143 Uiso 1 1 calc R . . C33 C 0.4353(4) 0.5712(3) 0.5039(4) 0.112(3) Uani 1 1 d . . . H33A H 0.4139 0.5596 0.5502 0.168 Uiso 1 1 calc R . . H33B H 0.4846 0.5870 0.5124 0.168 Uiso 1 1 calc R . . H33C H 0.4350 0.5294 0.4728 0.168 Uiso 1 1 calc R . . C34 C 0.3192(3) 0.6019(3) 0.4438(4) 0.0898(19) Uani 1 1 d . . . H34A H 0.2908 0.6400 0.4220 0.135 Uiso 1 1 calc R . . H34B H 0.2949 0.5836 0.4862 0.135 Uiso 1 1 calc R . . H34C H 0.3247 0.5641 0.4084 0.135 Uiso 1 1 calc R . . C35 C 0.45892(19) 1.00789(19) 0.2946(2) 0.0345(8) Uani 1 1 d . . . H35 H 0.4293 0.9830 0.3267 0.041 Uiso 1 1 calc R . . C36 C 0.4576(2) 1.0802(2) 0.2962(2) 0.0419(9) Uani 1 1 d . . . H36 H 0.4278 1.1042 0.3288 0.050 Uiso 1 1 calc R . . C37 C 0.5000 1.1172(3) 0.2500 0.0445(13) Uani 1 2 d S . . H37 H 0.5000 1.1672 0.2500 0.053 Uiso 1 2 calc SR . . Cl1S Cl 0.5000 0.538(2) 0.2500 0.126(6) Uani 0.068(3) 2 d SPDU A 1 Cl2S Cl 0.562(2) 0.401(2) 0.304(2) 0.128(4) Uani 0.068(3) 1 d PDU A 1 C1S C 0.5000 0.446(2) 0.2500 0.131(3) Uani 0.068(3) 2 d SPDU . 1 H1S H 0.5343 0.4465 0.2095 0.157 Uiso 0.0339(16) 1 calc PR A 1 Cl1T Cl 0.4582(8) 0.3437(8) 0.2052(10) 0.121(3) Uani 0.259(5) 1 d PDU . 2 Cl2T Cl 0.5663(8) 0.3744(7) 0.3085(9) 0.129(3) Uani 0.259(5) 1 d PDU . 2 Cl3T Cl 0.4992(8) 0.4849(6) 0.2311(5) 0.133(3) Uani 0.259(5) 1 d PDU . 2 C1T C 0.5307(9) 0.3991(7) 0.2244(9) 0.131(3) Uani 0.259(5) 1 d PDU . 2 H1T H 0.5673 0.3953 0.1863 0.157 Uiso 0.259(5) 1 calc PR . 2 Cl1U Cl 0.5828(8) 0.3032(9) 0.2638(10) 0.137(4) Uani 0.174(5) 1 d PDU B 3 Cl2U Cl 0.5284(8) 0.4457(9) 0.2846(8) 0.130(3) Uani 0.174(5) 1 d PDU . 3 Cl3U Cl 0.4383(9) 0.3390(13) 0.2123(16) 0.114(4) Uani 0.174(5) 1 d PDU . 3 C1U C 0.5240(11) 0.3687(11) 0.2337(18) 0.128(3) Uani 0.174(5) 1 d PDU B 3 H1U H 0.5431 0.3829 0.1859 0.154 Uiso 0.174(5) 1 calc PR B 3 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 0.0256(4) 0.0233(4) 0.0266(4) 0.000 0.0006(3) 0.000 O1 0.0513(17) 0.0339(15) 0.0667(19) -0.0042(14) -0.0073(14) -0.0061(13) O2 0.059(2) 0.070(2) 0.091(3) 0.0066(19) -0.0147(19) -0.0315(18) O3 0.125(4) 0.108(4) 0.101(3) 0.019(3) 0.037(3) -0.032(3) N1 0.0278(14) 0.0238(14) 0.0283(14) -0.0004(11) 0.0016(11) 0.0004(11) N2 0.0294(15) 0.0227(14) 0.0282(14) -0.0001(11) -0.0012(11) -0.0007(11) N3 0.033(2) 0.030(2) 0.033(2) 0.000 0.0023(18) 0.000 N4 0.026(2) 0.027(2) 0.030(2) 0.000 -0.0032(16) 0.000 C1 0.039(2) 0.0236(17) 0.0262(16) 0.0003(13) 0.0011(14) 0.0004(14) C2 0.043(2) 0.041(2) 0.0276(18) 0.0010(15) -0.0019(15) -0.0005(17) C3 0.037(2) 0.042(2) 0.0329(19) -0.0007(16) -0.0057(15) -0.0015(16) C4 0.0303(18) 0.0267(18) 0.0331(18) -0.0019(14) -0.0034(14) -0.0003(14) C5 0.0264(17) 0.0246(18) 0.0385(19) -0.0001(14) -0.0033(14) 0.0000(13) C6 0.0261(17) 0.0235(17) 0.0369(18) -0.0008(14) -0.0011(14) -0.0010(13) C7 0.0268(18) 0.035(2) 0.045(2) 0.0007(16) 0.0023(15) -0.0021(15) C8 0.0314(19) 0.036(2) 0.041(2) 0.0009(16) 0.0091(16) -0.0008(15) C9 0.0340(18) 0.0217(16) 0.0334(18) -0.0011(14) 0.0054(14) -0.0010(14) C10 0.0361(19) 0.0238(17) 0.0290(17) -0.0001(13) 0.0031(14) 0.0003(14) C11 0.0305(19) 0.044(2) 0.039(2) 0.0045(17) -0.0030(16) 0.0007(16) C12 0.034(2) 0.054(3) 0.049(2) -0.0096(19) -0.0083(17) -0.0019(18) C13 0.045(3) 0.074(3) 0.078(3) -0.009(3) -0.023(2) -0.005(2) C14 0.041(3) 0.102(5) 0.102(4) 0.020(4) -0.033(3) -0.005(3) C15 0.048(3) 0.071(4) 0.137(5) 0.036(4) -0.025(3) 0.009(3) C16 0.039(2) 0.046(3) 0.096(4) 0.017(2) -0.011(2) 0.003(2) N17 0.0336(18) 0.041(2) 0.094(3) -0.022(2) -0.0103(18) -0.0066(15) C18 0.042(2) 0.050(3) 0.055(2) -0.015(2) 0.0110(19) -0.0172(19) C19 0.049(3) 0.039(2) 0.102(4) -0.018(2) 0.017(3) -0.010(2) C20 0.088(4) 0.089(4) 0.089(4) 0.019(3) 0.030(3) 0.018(3) C21 0.081(5) 0.050(4) 0.350(15) -0.049(6) 0.005(7) -0.020(3) C22 0.062(3) 0.069(3) 0.088(4) -0.020(3) 0.023(3) -0.003(3) C23 0.0337(19) 0.039(2) 0.0293(18) -0.0052(15) 0.0020(14) 0.0013(16) C24 0.049(2) 0.045(2) 0.0334(19) -0.0001(17) 0.0063(17) -0.0030(18) C25 0.053(3) 0.069(3) 0.035(2) 0.002(2) 0.0052(18) -0.010(2) C26 0.035(2) 0.090(4) 0.035(2) -0.019(2) 0.0040(17) 0.001(2) C27 0.049(3) 0.062(3) 0.049(2) -0.027(2) 0.001(2) 0.005(2) C28 0.049(2) 0.039(2) 0.045(2) -0.0096(18) 0.0019(18) 0.0012(18) N29 0.094(3) 0.045(2) 0.0402(19) 0.0055(16) 0.0218(19) -0.009(2) C30 0.083(4) 0.060(3) 0.060(3) 0.005(2) 0.012(3) -0.006(3) C31 0.049(2) 0.035(2) 0.071(3) 0.002(2) 0.002(2) -0.0055(18) C32 0.105(5) 0.061(4) 0.122(5) -0.034(3) 0.049(4) -0.018(3) C33 0.107(5) 0.066(4) 0.158(7) -0.012(4) -0.077(5) 0.014(4) C34 0.051(3) 0.096(5) 0.122(5) -0.006(4) -0.005(3) -0.004(3) C35 0.0335(19) 0.0296(19) 0.0405(19) -0.0024(15) 0.0005(15) 0.0015(15) C36 0.042(2) 0.031(2) 0.053(2) -0.0080(18) -0.0032(18) 0.0055(17) C37 0.045(3) 0.028(3) 0.059(4) 0.000 -0.011(3) 0.000 Cl1S 0.102(10) 0.164(13) 0.108(11) 0.000 -0.023(10) 0.000 Cl2S 0.109(6) 0.168(9) 0.106(6) 0.002(6) -0.010(6) -0.007(6) C1S 0.111(5) 0.169(8) 0.111(5) 0.000 -0.010(5) 0.000 Cl1T 0.110(6) 0.163(7) 0.090(4) -0.006(4) 0.004(5) -0.006(5) Cl2T 0.108(4) 0.168(8) 0.109(4) 0.003(4) -0.004(4) -0.012(4) Cl3T 0.111(4) 0.173(7) 0.115(5) 0.007(3) -0.016(5) 0.000(3) C1T 0.112(5) 0.169(8) 0.110(5) 0.002(3) -0.008(5) -0.003(3) Cl1U 0.108(8) 0.153(10) 0.150(9) 0.035(7) -0.002(7) -0.044(7) Cl2U 0.110(4) 0.167(7) 0.113(4) 0.002(3) -0.012(4) -0.008(3) Cl3U 0.100(7) 0.158(8) 0.084(5) -0.007(5) 0.009(6) -0.013(6) C1U 0.111(5) 0.167(7) 0.106(4) 0.000(3) -0.004(4) -0.005(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 N3 1.946(4) . ? Fe1 N2 1.986(3) . ? Fe1 N2 1.986(3) 6_656 ? Fe1 N1 1.993(3) 6_656 ? Fe1 N1 1.993(3) . ? Fe1 N4 2.099(4) . ? O1 N3 1.233(3) . ? O2 C18 1.217(5) . ? O3 C30 1.265(6) . ? N1 C9 1.376(4) . ? N1 C6 1.376(4) . ? N2 C1 1.374(4) . ? N2 C4 1.377(4) . ? N3 O1 1.233(3) 6_656 ? N4 C35 1.344(4) 6_656 ? N4 C35 1.344(4) . ? C1 C10 1.388(5) 6_656 ? C1 C2 1.436(5) . ? C2 C3 1.341(5) . ? C3 C4 1.437(5) . ? C4 C5 1.387(5) . ? C5 C6 1.393(5) . ? C5 C11 1.503(5) . ? C6 C7 1.428(5) . ? C7 C8 1.339(5) . ? C8 C9 1.440(5) . ? C9 C10 1.389(5) . ? C10 C1 1.388(5) 6_656 ? C10 C23 1.506(5) . ? C11 C16 1.371(6) . ? C11 C12 1.402(6) . ? C12 C13 1.394(6) . ? C12 N17 1.403(5) . ? C13 C14 1.372(8) . ? C14 C15 1.360(8) . ? C15 C16 1.384(7) . ? N17 C18 1.364(5) . ? C18 C19 1.522(7) . ? C19 C21 1.501(7) . ? C19 C22 1.519(7) . ? C19 C20 1.571(8) . ? C23 C24 1.388(5) . ? C23 C28 1.393(5) . ? C24 C25 1.390(5) . ? C24 N29 1.427(5) . ? C25 C26 1.390(7) . ? C26 C27 1.364(7) . ? C27 C28 1.385(6) . ? N29 C30 1.276(6) . ? C30 C31 1.510(7) . ? C31 C34 1.512(7) . ? C31 C32 1.518(7) . ? C31 C33 1.525(7) . ? C35 C36 1.375(5) . ? C36 C37 1.376(5) . ? C37 C36 1.376(5) 6_656 ? Cl1S C1S 1.747(8) . ? Cl2S C1S 1.747(6) . ? C1S Cl2S 1.747(6) 6_656 ? Cl1T C1T 1.68(2) 6_656 ? Cl1T C1T 1.747(8) . ? Cl2T C1T 1.740(8) . ? Cl2T C1T 1.96(2) 6_656 ? Cl3T C1T 1.741(8) . ? Cl3T C1T 1.918(15) 6_656 ? Cl1U C1U 1.743(8) . ? Cl2U C1U 1.743(8) . ? Cl2U C1U 1.791(19) 6_656 ? Cl3U C1U 1.33(3) 6_656 ? Cl3U C1U 1.736(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Fe1 N2 90.60(8) . . ? N3 Fe1 N2 90.60(8) . 6_656 ? N2 Fe1 N2 178.80(16) . 6_656 ? N3 Fe1 N1 88.46(8) . 6_656 ? N2 Fe1 N1 89.28(11) . 6_656 ? N2 Fe1 N1 90.75(11) 6_656 6_656 ? N3 Fe1 N1 88.46(8) . . ? N2 Fe1 N1 90.75(11) . . ? N2 Fe1 N1 89.28(11) 6_656 . ? N1 Fe1 N1 176.93(15) 6_656 . ? N3 Fe1 N4 180.000(1) . . ? N2 Fe1 N4 89.40(8) . . ? N2 Fe1 N4 89.40(8) 6_656 . ? N1 Fe1 N4 91.54(8) 6_656 . ? N1 Fe1 N4 91.54(8) . . ? C9 N1 C6 105.6(3) . . ? C9 N1 Fe1 127.7(2) . . ? C6 N1 Fe1 126.6(2) . . ? C1 N2 C4 105.6(3) . . ? C1 N2 Fe1 127.9(2) . . ? C4 N2 Fe1 126.5(2) . . ? O1 N3 O1 120.4(4) . 6_656 ? O1 N3 Fe1 119.8(2) . . ? O1 N3 Fe1 119.8(2) 6_656 . ? C35 N4 C35 116.6(4) 6_656 . ? C35 N4 Fe1 121.7(2) 6_656 . ? C35 N4 Fe1 121.7(2) . . ? N2 C1 C10 125.7(3) . 6_656 ? N2 C1 C2 110.1(3) . . ? C10 C1 C2 124.0(3) 6_656 . ? C3 C2 C1 107.1(3) . . ? C2 C3 C4 107.3(3) . . ? N2 C4 C5 126.2(3) . . ? N2 C4 C3 109.8(3) . . ? C5 C4 C3 124.0(3) . . ? C4 C5 C6 124.0(3) . . ? C4 C5 C11 118.0(3) . . ? C6 C5 C11 117.9(3) . . ? N1 C6 C5 125.5(3) . . ? N1 C6 C7 109.8(3) . . ? C5 C6 C7 124.6(3) . . ? C8 C7 C6 107.8(3) . . ? C7 C8 C9 106.8(3) . . ? N1 C9 C10 125.6(3) . . ? N1 C9 C8 109.9(3) . . ? C10 C9 C8 124.5(3) . . ? C1 C10 C9 123.2(3) 6_656 . ? C1 C10 C23 118.3(3) 6_656 . ? C9 C10 C23 118.5(3) . . ? C16 C11 C12 119.1(4) . . ? C16 C11 C5 119.5(4) . . ? C12 C11 C5 121.4(3) . . ? C13 C12 C11 119.2(4) . . ? C13 C12 N17 122.4(4) . . ? C11 C12 N17 118.5(3) . . ? C14 C13 C12 119.9(5) . . ? C15 C14 C13 121.2(5) . . ? C14 C15 C16 119.3(5) . . ? C11 C16 C15 121.4(5) . . ? C18 N17 C12 128.8(4) . . ? O2 C18 N17 121.2(4) . . ? O2 C18 C19 121.9(4) . . ? N17 C18 C19 116.8(4) . . ? C21 C19 C22 110.5(5) . . ? C21 C19 C18 109.9(5) . . ? C22 C19 C18 111.5(4) . . ? C21 C19 C20 109.0(6) . . ? C22 C19 C20 106.6(4) . . ? C18 C19 C20 109.3(4) . . ? C24 C23 C28 119.2(3) . . ? C24 C23 C10 120.9(3) . . ? C28 C23 C10 119.9(3) . . ? C23 C24 C25 120.5(4) . . ? C23 C24 N29 116.4(3) . . ? C25 C24 N29 123.1(4) . . ? C24 C25 C26 118.8(4) . . ? C27 C26 C25 121.2(4) . . ? C26 C27 C28 119.9(4) . . ? C27 C28 C23 120.2(4) . . ? C30 N29 C24 132.7(4) . . ? O3 C30 N29 122.4(5) . . ? O3 C30 C31 118.3(5) . . ? N29 C30 C31 119.1(4) . . ? C30 C31 C34 107.3(4) . . ? C30 C31 C32 114.5(4) . . ? C34 C31 C32 109.9(5) . . ? C30 C31 C33 109.2(5) . . ? C34 C31 C33 109.6(4) . . ? C32 C31 C33 106.3(5) . . ? N4 C35 C36 123.3(4) . . ? C35 C36 C37 119.3(4) . . ? C36 C37 C36 118.3(5) . 6_656 ? Cl1S C1S Cl2S 120.0(3) . 6_656 ? Cl1S C1S Cl2S 120.0(3) . . ? Cl2S C1S Cl2S 119.9(6) 6_656 . ? C1T Cl1T C1T 52.1(15) 6_656 . ? C1T Cl2T C1T 47.7(13) . 6_656 ? C1T Cl3T C1T 48.3(13) . 6_656 ? Cl2T C1T Cl3T 108.1(8) . . ? Cl2T C1T Cl1T 107.2(8) . . ? Cl3T C1T Cl1T 108.6(8) . . ? C1U Cl2U C1U 36(2) . 6_656 ? C1U Cl3U C1U 39(3) 6_656 . ? Cl3U C1U Cl2U 115.3(11) . . ? Cl3U C1U Cl1U 114.3(11) . . ? Cl2U C1U Cl1U 114.1(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Fe1 N1 C9 93.2(3) . . . . ? N2 Fe1 N1 C9 -176.2(3) . . . . ? N2 Fe1 N1 C9 2.6(3) 6_656 . . . ? N1 Fe1 N1 C9 93.2(3) 6_656 . . . ? N4 Fe1 N1 C9 -86.8(3) . . . . ? N3 Fe1 N1 C6 -82.5(3) . . . . ? N2 Fe1 N1 C6 8.1(3) . . . . ? N2 Fe1 N1 C6 -173.1(3) 6_656 . . . ? N1 Fe1 N1 C6 -82.5(3) 6_656 . . . ? N4 Fe1 N1 C6 97.5(3) . . . . ? N3 Fe1 N2 C1 -95.2(3) . . . . ? N2 Fe1 N2 C1 84.8(3) 6_656 . . . ? N1 Fe1 N2 C1 -6.7(3) 6_656 . . . ? N1 Fe1 N2 C1 176.4(3) . . . . ? N4 Fe1 N2 C1 84.8(3) . . . . ? N3 Fe1 N2 C4 83.6(3) . . . . ? N2 Fe1 N2 C4 -96.4(3) 6_656 . . . ? N1 Fe1 N2 C4 172.1(3) 6_656 . . . ? N1 Fe1 N2 C4 -4.9(3) . . . . ? N4 Fe1 N2 C4 -96.4(3) . . . . ? N2 Fe1 N3 O1 -38.48(18) . . . . ? N2 Fe1 N3 O1 141.52(18) 6_656 . . . ? N1 Fe1 N3 O1 -127.75(18) 6_656 . . . ? N1 Fe1 N3 O1 52.25(18) . . . . ? N4 Fe1 N3 O1 -151(100) . . . . ? N2 Fe1 N3 O1 141.52(18) . . . 6_656 ? N2 Fe1 N3 O1 -38.48(18) 6_656 . . 6_656 ? N1 Fe1 N3 O1 52.25(18) 6_656 . . 6_656 ? N1 Fe1 N3 O1 -127.75(18) . . . 6_656 ? N4 Fe1 N3 O1 29(100) . . . 6_656 ? N3 Fe1 N4 C35 46(100) . . . 6_656 ? N2 Fe1 N4 C35 -66.4(2) . . . 6_656 ? N2 Fe1 N4 C35 113.6(2) 6_656 . . 6_656 ? N1 Fe1 N4 C35 22.9(2) 6_656 . . 6_656 ? N1 Fe1 N4 C35 -157.1(2) . . . 6_656 ? N3 Fe1 N4 C35 -134(100) . . . . ? N2 Fe1 N4 C35 113.6(2) . . . . ? N2 Fe1 N4 C35 -66.4(2) 6_656 . . . ? N1 Fe1 N4 C35 -157.1(2) 6_656 . . . ? N1 Fe1 N4 C35 22.9(2) . . . . ? C4 N2 C1 C10 -174.1(3) . . . 6_656 ? Fe1 N2 C1 C10 4.9(5) . . . 6_656 ? C4 N2 C1 C2 1.2(4) . . . . ? Fe1 N2 C1 C2 -179.9(2) . . . . ? N2 C1 C2 C3 -1.6(4) . . . . ? C10 C1 C2 C3 173.8(3) 6_656 . . . ? C1 C2 C3 C4 1.2(4) . . . . ? C1 N2 C4 C5 179.7(3) . . . . ? Fe1 N2 C4 C5 0.7(5) . . . . ? C1 N2 C4 C3 -0.4(4) . . . . ? Fe1 N2 C4 C3 -179.4(2) . . . . ? C2 C3 C4 N2 -0.6(4) . . . . ? C2 C3 C4 C5 179.4(3) . . . . ? N2 C4 C5 C6 2.8(5) . . . . ? C3 C4 C5 C6 -177.1(3) . . . . ? N2 C4 C5 C11 178.9(3) . . . . ? C3 C4 C5 C11 -1.0(5) . . . . ? C9 N1 C6 C5 175.9(3) . . . . ? Fe1 N1 C6 C5 -7.6(5) . . . . ? C9 N1 C6 C7 -0.9(4) . . . . ? Fe1 N1 C6 C7 175.6(2) . . . . ? C4 C5 C6 N1 0.8(5) . . . . ? C11 C5 C6 N1 -175.3(3) . . . . ? C4 C5 C6 C7 177.3(3) . . . . ? C11 C5 C6 C7 1.1(5) . . . . ? N1 C6 C7 C8 1.2(4) . . . . ? C5 C6 C7 C8 -175.7(3) . . . . ? C6 C7 C8 C9 -0.9(4) . . . . ? C6 N1 C9 C10 -179.7(3) . . . . ? Fe1 N1 C9 C10 3.9(5) . . . . ? C6 N1 C9 C8 0.3(4) . . . . ? Fe1 N1 C9 C8 -176.1(2) . . . . ? C7 C8 C9 N1 0.4(4) . . . . ? C7 C8 C9 C10 -179.6(3) . . . . ? N1 C9 C10 C1 -8.2(5) . . . 6_656 ? C8 C9 C10 C1 171.8(3) . . . 6_656 ? N1 C9 C10 C23 174.5(3) . . . . ? C8 C9 C10 C23 -5.6(5) . . . . ? C4 C5 C11 C16 -89.7(5) . . . . ? C6 C5 C11 C16 86.7(5) . . . . ? C4 C5 C11 C12 89.1(4) . . . . ? C6 C5 C11 C12 -94.5(4) . . . . ? C16 C11 C12 C13 0.5(6) . . . . ? C5 C11 C12 C13 -178.3(4) . . . . ? C16 C11 C12 N17 -179.5(4) . . . . ? C5 C11 C12 N17 1.7(6) . . . . ? C11 C12 C13 C14 -0.3(7) . . . . ? N17 C12 C13 C14 179.7(5) . . . . ? C12 C13 C14 C15 -0.3(9) . . . . ? C13 C14 C15 C16 0.6(10) . . . . ? C12 C11 C16 C15 -0.2(7) . . . . ? C5 C11 C16 C15 178.7(5) . . . . ? C14 C15 C16 C11 -0.4(9) . . . . ? C13 C12 N17 C18 -8.2(7) . . . . ? C11 C12 N17 C18 171.8(4) . . . . ? C12 N17 C18 O2 2.0(7) . . . . ? C12 N17 C18 C19 -178.6(4) . . . . ? O2 C18 C19 C21 3.4(8) . . . . ? N17 C18 C19 C21 -176.0(6) . . . . ? O2 C18 C19 C22 126.2(5) . . . . ? N17 C18 C19 C22 -53.2(6) . . . . ? O2 C18 C19 C20 -116.2(5) . . . . ? N17 C18 C19 C20 64.4(5) . . . . ? C1 C10 C23 C24 -94.8(4) 6_656 . . . ? C9 C10 C23 C24 82.6(4) . . . . ? C1 C10 C23 C28 84.2(4) 6_656 . . . ? C9 C10 C23 C28 -98.3(4) . . . . ? C28 C23 C24 C25 0.6(6) . . . . ? C10 C23 C24 C25 179.7(4) . . . . ? C28 C23 C24 N29 -177.5(4) . . . . ? C10 C23 C24 N29 1.5(6) . . . . ? C23 C24 C25 C26 0.1(6) . . . . ? N29 C24 C25 C26 178.1(4) . . . . ? C24 C25 C26 C27 -1.0(6) . . . . ? C25 C26 C27 C28 1.2(6) . . . . ? C26 C27 C28 C23 -0.5(6) . . . . ? C24 C23 C28 C27 -0.4(6) . . . . ? C10 C23 C28 C27 -179.5(4) . . . . ? C23 C24 N29 C30 -168.4(5) . . . . ? C25 C24 N29 C30 13.5(8) . . . . ? C24 N29 C30 O3 -4.2(10) . . . . ? C24 N29 C30 C31 170.9(5) . . . . ? O3 C30 C31 C34 58.6(7) . . . . ? N29 C30 C31 C34 -116.8(6) . . . . ? O3 C30 C31 C32 -179.2(6) . . . . ? N29 C30 C31 C32 5.4(8) . . . . ? O3 C30 C31 C33 -60.2(7) . . . . ? N29 C30 C31 C33 124.5(6) . . . . ? C35 N4 C35 C36 -0.1(3) 6_656 . . . ? Fe1 N4 C35 C36 179.9(3) . . . . ? N4 C35 C36 C37 0.2(5) . . . . ? C35 C36 C37 C36 -0.1(2) . . . 6_656 ? C1T Cl2T C1T Cl3T 64.2(9) 6_656 . . . ? C1T Cl2T C1T Cl1T -52.7(10) 6_656 . . . ? C1T Cl3T C1T Cl2T -65.3(11) 6_656 . . . ? C1T Cl3T C1T Cl1T 50.7(11) 6_656 . . . ? C1T Cl1T C1T Cl2T 60.0(11) 6_656 . . . ? C1T Cl1T C1T Cl3T -56.6(9) 6_656 . . . ? C1U Cl3U C1U Cl2U -38.5(17) 6_656 . . . ? C1U Cl3U C1U Cl1U 97(3) 6_656 . . . ? C1U Cl2U C1U Cl3U 29.7(14) 6_656 . . . ? C1U Cl2U C1U Cl1U -105(4) 6_656 . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.823 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.097 #===END data_gr934c _publ_requested_journal 'test' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C74 H74 Fe N11 O6' _chemical_formula_weight 1269.29 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.560(2) _cell_length_b 19.035(3) _cell_length_c 18.543(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.707(10) _cell_angle_gamma 90.00 _cell_volume 6550.5(17) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 4.76 _cell_measurement_theta_max 13.66 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method ? _exptl_crystal_F_000 2676 _exptl_absorpt_coefficient_mu 0.293 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2461 _exptl_absorpt_correction_T_max 0.2644 _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 1 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.6 _diffrn_reflns_number 5324 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0768 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 3 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 24.00 _reflns_number_total 5137 _reflns_number_observed 3403 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 7 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0845P)^2^+15.5233P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5130 _refine_ls_number_parameters 418 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1117 _refine_ls_R_factor_obs 0.0687 _refine_ls_wR_factor_all 0.2019 _refine_ls_wR_factor_obs 0.1638 _refine_ls_goodness_of_fit_all 1.041 _refine_ls_goodness_of_fit_obs 1.099 _refine_ls_restrained_S_all 1.085 _refine_ls_restrained_S_obs 1.097 _refine_ls_shift/esd_max 0.010 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.5000 0.63718(4) 0.7500 0.0256(2) Uani 1 d S . O1 O 0.5510(2) 0.7709(2) 0.7773(2) 0.0607(10) Uani 1 d . . O2 O 0.1791(2) 0.8580(2) 0.6104(2) 0.0612(10) Uani 1 d . . O3 O 0.6465(2) 0.8297(2) 0.4238(2) 0.0664(10) Uani 1 d . . N1 N 0.4028(2) 0.6390(2) 0.7949(2) 0.0267(7) Uani 1 d . . N2 N 0.4554(2) 0.6359(2) 0.6518(2) 0.0268(7) Uani 1 d . . N3 N 0.5000 0.7407(3) 0.7500 0.0355(12) Uani 1 d S . N4 N 0.5000 0.5256(2) 0.7500 0.0274(10) Uani 1 d S . N5 N 0.2617(2) 0.7763(2) 0.6386(2) 0.0491(10) Uani 1 d . . H5 H 0.3077(2) 0.7708(2) 0.6493(2) 0.059 Uiso 1 calc R . N6 N 0.6004(2) 0.7504(2) 0.4997(2) 0.0420(9) Uani 1 d . . H6 H 0.5779(2) 0.7471(2) 0.5410(2) 0.050 Uiso 1 calc R . C1 C 0.3866(2) 0.6377(2) 0.8669(2) 0.0284(8) Uani 1 d . . C2 C 0.3108(2) 0.6449(2) 0.8762(2) 0.0343(9) Uani 1 d . . H2A H 0.2862(2) 0.6449(2) 0.9208(2) 0.041 Uiso 1 calc R . C3 C 0.2805(2) 0.6517(2) 0.8105(2) 0.0342(10) Uani 1 d . . H3A H 0.2307(2) 0.6586(2) 0.8000(2) 0.041 Uiso 1 calc R . C4 C 0.3378(2) 0.6467(2) 0.7589(2) 0.0274(9) Uani 1 d . . C5 C 0.3278(2) 0.6478(2) 0.6847(2) 0.0284(9) Uani 1 d . . C6 C 0.3826(2) 0.6413(2) 0.6356(2) 0.0275(8) Uani 1 d . . C7 C 0.3724(2) 0.6388(2) 0.5589(2) 0.0336(9) Uani 1 d . . H7A H 0.3275(2) 0.6413(2) 0.5339(2) 0.040 Uiso 1 calc R . C8 C 0.4372(2) 0.6324(2) 0.5286(2) 0.0349(9) Uani 1 d . . H8A H 0.4469(2) 0.6292(2) 0.4785(2) 0.042 Uiso 1 calc R . C9 C 0.4896(2) 0.6312(2) 0.5868(2) 0.0303(9) Uani 1 d . . C10 C 0.5633(2) 0.6303(2) 0.5766(2) 0.0294(9) Uani 1 d . . C11 C 0.2514(2) 0.6506(2) 0.6560(2) 0.0313(9) Uani 1 d . . C12 C 0.2206(2) 0.7140(2) 0.6329(2) 0.0413(11) Uani 1 d . . C13 C 0.1503(2) 0.7133(3) 0.6053(3) 0.0525(13) Uani 1 d . . H13A H 0.1291(2) 0.7557(3) 0.5882(3) 0.063 Uiso 1 calc R . C14 C 0.1117(2) 0.6522(3) 0.6028(3) 0.0562(14) Uani 1 d . . H14A H 0.0638(2) 0.6528(3) 0.5844(3) 0.067 Uiso 1 calc R . C15 C 0.1408(2) 0.5901(3) 0.6264(3) 0.0556(14) Uani 1 d . . H15A H 0.1134(2) 0.5480(3) 0.6251(3) 0.067 Uiso 1 calc R . C16 C 0.2107(2) 0.5901(2) 0.6521(3) 0.0470(12) Uani 1 d . . H16A H 0.2316(2) 0.5470(2) 0.6677(3) 0.056 Uiso 1 calc R . C17 C 0.2394(2) 0.8434(2) 0.6297(2) 0.0441(12) Uani 1 d . . C18 C 0.2965(2) 0.9003(2) 0.6441(3) 0.0521(13) Uani 1 d D . C19 C 0.3640(3) 0.8864(3) 0.6030(3) 0.064(2) Uani 1 d . . H19A H 0.3852(11) 0.8418(10) 0.6190(14) 0.096 Uiso 1 calc R . H19B H 0.3984(8) 0.9246(10) 0.6118(16) 0.096 Uiso 1 calc R . H19C H 0.3525(4) 0.8838(19) 0.5514(3) 0.096 Uiso 1 calc R . C20 C 0.2654(6) 0.9738(4) 0.6337(7) 0.096(4) Uani 0.70 d PDU 1 H20A H 0.2234(25) 0.9797(14) 0.6646(30) 0.144 Uiso 0.70 calc PR 1 H20B H 0.2508(38) 0.9801(14) 0.5831(11) 0.144 Uiso 0.70 calc PR 1 H20C H 0.3020(14) 1.0089(4) 0.6466(40) 0.144 Uiso 0.70 calc PR 1 C20A C 0.2674(14) 0.9589(9) 0.5904(15) 0.103(11) Uani 0.30 d PDU 2 H20D H 0.2611(95) 0.9386(26) 0.5421(26) 0.154 Uiso 0.30 calc PR 2 H20E H 0.3021(49) 0.9976(46) 0.5884(79) 0.154 Uiso 0.30 calc PR 2 H20F H 0.2210(50) 0.9766(69) 0.6074(55) 0.154 Uiso 0.30 calc PR 2 C21 C 0.3156(3) 0.9004(4) 0.7252(3) 0.088(2) Uani 1 d . . H21A H 0.3334(23) 0.8539(8) 0.7394(6) 0.132 Uiso 1 calc R . H21B H 0.2726(7) 0.9118(24) 0.7530(3) 0.132 Uiso 1 calc R . H21C H 0.3530(18) 0.9357(17) 0.7349(5) 0.132 Uiso 1 calc R . C22 C 0.5914(2) 0.6255(2) 0.5015(2) 0.0310(9) Uani 1 d . . C23 C 0.6092(2) 0.6865(2) 0.4634(2) 0.0337(10) Uani 1 d . . C24 C 0.6353(2) 0.6810(2) 0.3935(2) 0.0415(11) Uani 1 d . . H24A H 0.6480(2) 0.7221(2) 0.3675(2) 0.050 Uiso 1 calc R . C25 C 0.6427(2) 0.6154(2) 0.3622(2) 0.0425(11) Uani 1 d . . H25A H 0.6602(2) 0.6118(2) 0.3144(2) 0.051 Uiso 1 calc R . C26 C 0.6249(2) 0.5553(2) 0.3993(2) 0.0451(12) Uani 1 d . . H26A H 0.6304(2) 0.5105(2) 0.3775(2) 0.054 Uiso 1 calc R . C27 C 0.5993(2) 0.5608(2) 0.4683(2) 0.0402(11) Uani 1 d . . H27A H 0.5867(2) 0.5193(2) 0.4937(2) 0.048 Uiso 1 calc R . C28 C 0.6203(2) 0.8156(2) 0.4821(2) 0.0388(10) Uani 1 d . . C29 C 0.6095(2) 0.8726(2) 0.5390(2) 0.0412(11) Uani 1 d . . C30 C 0.6834(3) 0.9007(3) 0.5579(4) 0.078(2) Uani 1 d . . H30A H 0.7138(7) 0.8623(5) 0.5761(21) 0.117 Uiso 1 calc R . H30B H 0.6792(4) 0.9370(16) 0.5951(16) 0.117 Uiso 1 calc R . H30C H 0.7052(9) 0.9210(20) 0.5147(6) 0.117 Uiso 1 calc R . C31 C 0.5617(3) 0.9296(3) 0.5085(3) 0.072(2) Uani 1 d . . H31A H 0.5848(10) 0.9510(14) 0.4667(13) 0.108 Uiso 1 calc R . H31B H 0.5539(18) 0.9656(11) 0.5454(8) 0.108 Uiso 1 calc R . H31C H 0.5152(8) 0.9094(5) 0.4938(20) 0.108 Uiso 1 calc R . C32 C 0.5727(3) 0.8466(3) 0.6073(3) 0.074(2) Uani 1 d . . H32A H 0.6034(10) 0.8118(16) 0.6314(12) 0.111 Uiso 1 calc R . H32B H 0.5263(10) 0.8251(19) 0.5944(4) 0.111 Uiso 1 calc R . H32C H 0.5647(20) 0.8864(4) 0.6398(10) 0.111 Uiso 1 calc R . C33 C 0.4592(2) 0.4889(2) 0.7957(2) 0.0334(10) Uani 1 d . . H33A H 0.4300(2) 0.5139(2) 0.8287(2) 0.040 Uiso 1 calc R . C34 C 0.4579(2) 0.4164(2) 0.7971(2) 0.0410(11) Uani 1 d . . H34A H 0.4282(2) 0.3922(2) 0.8302(2) 0.049 Uiso 1 calc R . C35 C 0.5000 0.3800(3) 0.7500 0.042(2) Uani 1 d S . H35A H 0.5000 0.3301(3) 0.7500 0.050 Uiso 1 calc SR . C36 C 0.5256(4) 0.9716(4) 0.2746(5) 0.120(3) Uiso 1 d . . C37 C 0.5546(4) 0.9097(4) 0.2995(4) 0.086(2) Uiso 1 d . . C38 C 0.5303(4) 0.8465(4) 0.2775(4) 0.096(2) Uiso 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 0.0270(4) 0.0230(4) 0.0269(4) 0.000 0.0003(3) 0.000 O1 0.075(2) 0.042(2) 0.065(2) -0.003(2) -0.001(2) -0.006(2) O2 0.044(2) 0.060(2) 0.079(2) -0.005(2) -0.016(2) 0.017(2) O3 0.089(3) 0.053(2) 0.058(2) 0.006(2) 0.026(2) -0.016(2) N1 0.0276(15) 0.0235(15) 0.029(2) -0.0022(14) 0.0006(13) 0.0016(13) N2 0.030(2) 0.0216(14) 0.029(2) 0.0005(14) 0.0016(13) -0.0001(13) N3 0.038(3) 0.042(3) 0.027(2) 0.000 -0.002(2) 0.000 N4 0.028(2) 0.023(2) 0.031(2) 0.000 -0.004(2) 0.000 N5 0.027(2) 0.034(2) 0.085(3) 0.013(2) -0.012(2) 0.002(2) N6 0.061(2) 0.035(2) 0.030(2) 0.005(2) 0.016(2) 0.001(2) C1 0.033(2) 0.021(2) 0.031(2) 0.006(2) 0.001(2) 0.000(2) C2 0.032(2) 0.034(2) 0.037(2) -0.001(2) 0.005(2) 0.001(2) C3 0.026(2) 0.036(2) 0.041(2) -0.002(2) 0.002(2) 0.002(2) C4 0.027(2) 0.019(2) 0.036(2) 0.001(2) 0.002(2) -0.0020(15) C5 0.033(2) 0.020(2) 0.032(2) 0.001(2) 0.000(2) -0.001(2) C6 0.027(2) 0.023(2) 0.032(2) 0.000(2) 0.000(2) -0.002(2) C7 0.033(2) 0.036(2) 0.032(2) -0.005(2) -0.004(2) -0.001(2) C8 0.044(2) 0.032(2) 0.029(2) -0.004(2) 0.003(2) 0.001(2) C9 0.038(2) 0.022(2) 0.031(2) -0.003(2) -0.002(2) 0.002(2) C10 0.038(2) 0.018(2) 0.033(2) -0.001(2) 0.000(2) 0.001(2) C11 0.030(2) 0.035(2) 0.028(2) -0.007(2) -0.001(2) -0.003(2) C12 0.031(2) 0.049(3) 0.044(2) 0.003(2) -0.004(2) -0.001(2) C13 0.032(2) 0.065(3) 0.061(3) 0.003(3) -0.011(2) 0.000(2) C14 0.036(2) 0.075(4) 0.057(3) -0.017(3) -0.013(2) -0.004(2) C15 0.043(3) 0.056(3) 0.068(3) -0.023(3) -0.003(2) -0.012(2) C16 0.040(2) 0.037(2) 0.064(3) -0.011(2) -0.003(2) -0.006(2) C17 0.040(2) 0.051(3) 0.041(2) 0.006(2) 0.004(2) 0.015(2) C18 0.042(2) 0.037(2) 0.078(3) 0.010(2) 0.004(2) 0.004(2) C19 0.057(3) 0.072(4) 0.063(3) 0.002(3) 0.016(3) -0.012(3) C20 0.080(6) 0.030(4) 0.177(11) -0.009(5) -0.029(7) 0.012(4) C20A 0.080(15) 0.014(9) 0.213(31) 0.035(14) -0.020(18) -0.011(9) C21 0.095(4) 0.099(5) 0.070(4) -0.031(3) 0.030(3) -0.044(4) C22 0.030(2) 0.034(2) 0.028(2) -0.005(2) -0.002(2) 0.002(2) C23 0.037(2) 0.034(2) 0.031(2) -0.001(2) 0.005(2) 0.000(2) C24 0.040(2) 0.055(3) 0.030(2) 0.002(2) 0.004(2) 0.000(2) C25 0.036(2) 0.064(3) 0.028(2) -0.010(2) 0.002(2) 0.007(2) C26 0.039(2) 0.048(3) 0.048(3) -0.022(2) 0.000(2) 0.005(2) C27 0.039(2) 0.035(2) 0.046(3) -0.012(2) 0.001(2) -0.004(2) C28 0.035(2) 0.043(2) 0.038(2) 0.010(2) 0.003(2) -0.006(2) C29 0.043(2) 0.036(2) 0.044(2) 0.002(2) -0.008(2) -0.003(2) C30 0.046(3) 0.076(4) 0.113(5) -0.035(4) -0.011(3) 0.000(3) C31 0.073(4) 0.062(3) 0.081(4) -0.014(3) -0.026(3) 0.017(3) C32 0.100(4) 0.055(3) 0.068(4) -0.018(3) 0.026(3) -0.007(3) C33 0.035(2) 0.028(2) 0.038(2) 0.000(2) 0.002(2) -0.003(2) C34 0.040(2) 0.035(2) 0.048(3) 0.009(2) -0.002(2) -0.007(2) C35 0.041(3) 0.023(3) 0.062(4) 0.000 -0.015(3) 0.000 _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 N3 1.971(5) . ? Fe1 N2 1.991(3) 2_656 ? Fe1 N2 1.991(3) . ? Fe1 N1 1.996(3) . ? Fe1 N1 1.996(3) 2_656 ? Fe1 N4 2.124(4) . ? O1 N3 1.212(4) . ? O2 C17 1.202(5) . ? O3 C28 1.220(5) . ? N1 C1 1.373(5) . ? N1 C4 1.379(4) . ? N2 C9 1.372(5) . ? N2 C6 1.384(4) . ? N3 O1 1.212(4) 2_656 ? N4 C33 1.340(4) . ? N4 C33 1.340(4) 2_656 ? N5 C17 1.351(5) . ? N5 C12 1.414(5) . ? N6 C28 1.337(5) . ? N6 C23 1.401(5) . ? C1 C10 1.398(5) 2_656 ? C1 C2 1.426(5) . ? C2 C3 1.341(5) . ? C3 C4 1.444(5) . ? C4 C5 1.386(5) . ? C5 C6 1.381(5) . ? C5 C11 1.509(5) . ? C6 C7 1.433(5) . ? C7 C8 1.339(5) . ? C8 C9 1.442(5) . ? C9 C10 1.384(5) . ? C10 C1 1.398(5) 2_656 ? C10 C22 1.497(5) . ? C11 C16 1.380(6) . ? C11 C12 1.400(6) . ? C12 C13 1.395(6) . ? C13 C14 1.366(7) . ? C14 C15 1.369(7) . ? C15 C16 1.376(6) . ? C17 C18 1.538(6) . ? C18 C19 1.497(7) . ? C18 C20 1.526(9) . ? C18 C21 1.541(8) . ? C18 C20A 1.59(2) . ? C22 C27 1.385(5) . ? C22 C23 1.401(5) . ? C23 C24 1.393(6) . ? C24 C25 1.385(6) . ? C25 C26 1.378(6) . ? C26 C27 1.373(6) . ? C28 C29 1.528(6) . ? C29 C31 1.508(6) . ? C29 C30 1.510(6) . ? C29 C32 1.527(7) . ? C33 C34 1.380(6) . ? C34 C35 1.368(5) . ? C35 C34 1.368(5) 2_656 ? C36 C36 1.31(2) 2_655 ? C36 C37 1.373(10) . ? C37 C38 1.347(9) . ? C38 C38 1.509(14) 2_655 ? 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 N3 Fe1 N2 90.70(9) . 2_656 ? N3 Fe1 N2 90.70(9) . . ? N2 Fe1 N2 178.6(2) 2_656 . ? N3 Fe1 N1 89.02(9) . . ? N2 Fe1 N1 89.20(12) 2_656 . ? N2 Fe1 N1 90.83(12) . . ? N3 Fe1 N1 89.02(9) . 2_656 ? N2 Fe1 N1 90.82(12) 2_656 2_656 ? N2 Fe1 N1 89.20(12) . 2_656 ? N1 Fe1 N1 178.0(2) . 2_656 ? N3 Fe1 N4 180.000(1) . . ? N2 Fe1 N4 89.30(9) 2_656 . ? N2 Fe1 N4 89.30(9) . . ? N1 Fe1 N4 90.98(9) . . ? N1 Fe1 N4 90.98(9) 2_656 . ? C1 N1 C4 105.7(3) . . ? C1 N1 Fe1 128.0(2) . . ? C4 N1 Fe1 126.1(2) . . ? C9 N2 C6 105.9(3) . . ? C9 N2 Fe1 127.8(2) . . ? C6 N2 Fe1 126.2(2) . . ? O1 N3 O1 123.4(5) 2_656 . ? O1 N3 Fe1 118.3(3) 2_656 . ? O1 N3 Fe1 118.3(3) . . ? C33 N4 C33 117.2(5) . 2_656 ? C33 N4 Fe1 121.4(2) . . ? C33 N4 Fe1 121.4(2) 2_656 . ? C17 N5 C12 128.2(4) . . ? C28 N6 C23 131.0(4) . . ? N1 C1 C10 125.3(3) . 2_656 ? N1 C1 C2 110.1(3) . . ? C10 C1 C2 124.5(3) 2_656 . ? C3 C2 C1 107.7(3) . . ? C2 C3 C4 106.9(3) . . ? N1 C4 C5 126.0(3) . . ? N1 C4 C3 109.5(3) . . ? C5 C4 C3 124.5(3) . . ? C6 C5 C4 124.3(3) . . ? C6 C5 C11 117.9(3) . . ? C4 C5 C11 117.7(3) . . ? C5 C6 N2 126.1(3) . . ? C5 C6 C7 124.7(3) . . ? N2 C6 C7 109.3(3) . . ? C8 C7 C6 108.1(3) . . ? C7 C8 C9 106.8(3) . . ? N2 C9 C10 126.1(3) . . ? N2 C9 C8 109.9(3) . . ? C10 C9 C8 123.9(3) . . ? C9 C10 C1 123.1(3) . 2_656 ? C9 C10 C22 118.9(3) . . ? C1 C10 C22 117.8(3) 2_656 . ? C16 C11 C12 118.9(4) . . ? C16 C11 C5 120.0(3) . . ? C12 C11 C5 121.2(3) . . ? C13 C12 C11 118.8(4) . . ? C13 C12 N5 122.4(4) . . ? C11 C12 N5 118.8(3) . . ? C14 C13 C12 120.5(5) . . ? C13 C14 C15 121.3(4) . . ? C14 C15 C16 118.6(4) . . ? C15 C16 C11 122.0(4) . . ? O2 C17 N5 122.6(4) . . ? O2 C17 C18 121.7(4) . . ? N5 C17 C18 115.8(4) . . ? C19 C18 C20 114.5(6) . . ? C19 C18 C17 111.5(4) . . ? C20 C18 C17 111.4(5) . . ? C19 C18 C21 108.2(4) . . ? C20 C18 C21 101.8(6) . . ? C17 C18 C21 108.7(4) . . ? C19 C18 C20A 94.9(11) . . ? C17 C18 C20A 99.1(9) . . ? C21 C18 C20A 133.2(10) . . ? C27 C22 C23 119.1(4) . . ? C27 C22 C10 120.6(4) . . ? C23 C22 C10 120.3(3) . . ? C24 C23 C22 119.5(4) . . ? C24 C23 N6 123.7(4) . . ? C22 C23 N6 116.7(3) . . ? C25 C24 C23 119.7(4) . . ? C26 C25 C24 120.9(4) . . ? C27 C26 C25 119.3(4) . . ? C26 C27 C22 121.4(4) . . ? O3 C28 N6 122.3(4) . . ? O3 C28 C29 120.9(4) . . ? N6 C28 C29 116.8(4) . . ? C31 C29 C30 111.1(4) . . ? C31 C29 C32 106.0(4) . . ? C30 C29 C32 109.7(4) . . ? C31 C29 C28 109.5(4) . . ? C30 C29 C28 106.6(4) . . ? C32 C29 C28 114.0(4) . . ? N4 C33 C34 122.9(4) . . ? C35 C34 C33 119.0(4) . . ? C34 C35 C34 119.0(5) . 2_656 ? C36 C36 C37 120.9(4) 2_655 . ? C38 C37 C36 122.4(7) . . ? C37 C38 C38 116.7(4) . 2_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Fe1 N1 C1 -92.1(3) . . . . ? N2 Fe1 N1 C1 -1.4(3) 2_656 . . . ? N2 Fe1 N1 C1 177.2(3) . . . . ? N1 Fe1 N1 C1 -92.1(3) 2_656 . . . ? N4 Fe1 N1 C1 87.9(3) . . . . ? N3 Fe1 N1 C4 83.2(3) . . . . ? N2 Fe1 N1 C4 173.9(3) 2_656 . . . ? N2 Fe1 N1 C4 -7.5(3) . . . . ? N1 Fe1 N1 C4 83.2(3) 2_656 . . . ? N4 Fe1 N1 C4 -96.8(3) . . . . ? N3 Fe1 N2 C9 94.2(3) . . . . ? N2 Fe1 N2 C9 -85.8(3) 2_656 . . . ? N1 Fe1 N2 C9 -176.8(3) . . . . ? N1 Fe1 N2 C9 5.1(3) 2_656 . . . ? N4 Fe1 N2 C9 -85.8(3) . . . . ? N3 Fe1 N2 C6 -84.2(3) . . . . ? N2 Fe1 N2 C6 95.8(3) 2_656 . . . ? N1 Fe1 N2 C6 4.8(3) . . . . ? N1 Fe1 N2 C6 -173.2(3) 2_656 . . . ? N4 Fe1 N2 C6 95.8(3) . . . . ? N2 Fe1 N3 O1 -142.1(2) 2_656 . . 2_656 ? N2 Fe1 N3 O1 37.9(2) . . . 2_656 ? N1 Fe1 N3 O1 -53.0(2) . . . 2_656 ? N1 Fe1 N3 O1 127.0(2) 2_656 . . 2_656 ? N4 Fe1 N3 O1 151.7(1000) . . . 2_656 ? N2 Fe1 N3 O1 37.9(2) 2_656 . . . ? N2 Fe1 N3 O1 -142.1(2) . . . . ? N1 Fe1 N3 O1 127.1(2) . . . . ? N1 Fe1 N3 O1 -52.9(2) 2_656 . . . ? N4 Fe1 N3 O1 -28.3(1000) . . . . ? N3 Fe1 N4 C33 132.1(1000) . . . . ? N2 Fe1 N4 C33 66.0(2) 2_656 . . . ? N2 Fe1 N4 C33 -114.0(2) . . . . ? N1 Fe1 N4 C33 -23.2(2) . . . . ? N1 Fe1 N4 C33 156.8(2) 2_656 . . . ? N3 Fe1 N4 C33 -47.9(1000) . . . 2_656 ? N2 Fe1 N4 C33 -114.0(2) 2_656 . . 2_656 ? N2 Fe1 N4 C33 66.0(2) . . . 2_656 ? N1 Fe1 N4 C33 156.8(2) . . . 2_656 ? N1 Fe1 N4 C33 -23.2(2) 2_656 . . 2_656 ? C4 N1 C1 C10 179.8(3) . . . 2_656 ? Fe1 N1 C1 C10 -4.2(5) . . . 2_656 ? C4 N1 C1 C2 -0.3(4) . . . . ? Fe1 N1 C1 C2 175.7(2) . . . . ? N1 C1 C2 C3 -0.9(4) . . . . ? C10 C1 C2 C3 179.0(4) 2_656 . . . ? C1 C2 C3 C4 1.7(4) . . . . ? C1 N1 C4 C5 -177.3(3) . . . . ? Fe1 N1 C4 C5 6.6(5) . . . . ? C1 N1 C4 C3 1.3(4) . . . . ? Fe1 N1 C4 C3 -174.8(2) . . . . ? C2 C3 C4 N1 -1.9(4) . . . . ? C2 C3 C4 C5 176.7(3) . . . . ? N1 C4 C5 C6 -0.1(6) . . . . ? C3 C4 C5 C6 -178.5(3) . . . . ? N1 C4 C5 C11 175.0(3) . . . . ? C3 C4 C5 C11 -3.4(5) . . . . ? C4 C5 C6 N2 -3.0(6) . . . . ? C11 C5 C6 N2 -178.1(3) . . . . ? C4 C5 C6 C7 176.7(4) . . . . ? C11 C5 C6 C7 1.6(5) . . . . ? C9 N2 C6 C5 -179.4(4) . . . . ? Fe1 N2 C6 C5 -0.7(5) . . . . ? C9 N2 C6 C7 0.8(4) . . . . ? Fe1 N2 C6 C7 179.5(2) . . . . ? C5 C6 C7 C8 180.0(4) . . . . ? N2 C6 C7 C8 -0.3(4) . . . . ? C6 C7 C8 C9 -0.4(4) . . . . ? C6 N2 C9 C10 174.8(4) . . . . ? Fe1 N2 C9 C10 -3.8(5) . . . . ? C6 N2 C9 C8 -1.1(4) . . . . ? Fe1 N2 C9 C8 -179.7(2) . . . . ? C7 C8 C9 N2 0.9(4) . . . . ? C7 C8 C9 C10 -175.1(4) . . . . ? N2 C9 C10 C1 -3.2(6) . . . 2_656 ? C8 C9 C10 C1 172.1(4) . . . 2_656 ? N2 C9 C10 C22 -179.6(3) . . . . ? C8 C9 C10 C22 -4.2(5) . . . . ? C6 C5 C11 C16 94.9(5) . . . . ? C4 C5 C11 C16 -80.5(5) . . . . ? C6 C5 C11 C12 -85.0(5) . . . . ? C4 C5 C11 C12 99.6(4) . . . . ? C16 C11 C12 C13 -1.3(6) . . . . ? C5 C11 C12 C13 178.6(4) . . . . ? C16 C11 C12 N5 178.4(4) . . . . ? C5 C11 C12 N5 -1.7(6) . . . . ? C17 N5 C12 C13 10.4(7) . . . . ? C17 N5 C12 C11 -169.3(4) . . . . ? C11 C12 C13 C14 1.7(7) . . . . ? N5 C12 C13 C14 -178.0(4) . . . . ? C12 C13 C14 C15 -0.6(8) . . . . ? C13 C14 C15 C16 -0.9(8) . . . . ? C14 C15 C16 C11 1.3(7) . . . . ? C12 C11 C16 C15 -0.2(7) . . . . ? C5 C11 C16 C15 179.9(4) . . . . ? C12 N5 C17 O2 -5.1(8) . . . . ? C12 N5 C17 C18 176.4(4) . . . . ? O2 C17 C18 C19 -127.0(5) . . . . ? N5 C17 C18 C19 51.5(6) . . . . ? O2 C17 C18 C20 2.3(8) . . . . ? N5 C17 C18 C20 -179.1(6) . . . . ? O2 C17 C18 C21 113.7(5) . . . . ? N5 C17 C18 C21 -67.7(5) . . . . ? O2 C17 C18 C20A -28.1(12) . . . . ? N5 C17 C18 C20A 150.4(11) . . . . ? C9 C10 C22 C27 -85.1(5) . . . . ? C1 C10 C22 C27 98.4(4) 2_656 . . . ? C9 C10 C22 C23 94.0(4) . . . . ? C1 C10 C22 C23 -82.5(4) 2_656 . . . ? C27 C22 C23 C24 -0.9(6) . . . . ? C10 C22 C23 C24 180.0(3) . . . . ? C27 C22 C23 N6 -179.8(4) . . . . ? C10 C22 C23 N6 1.1(5) . . . . ? C28 N6 C23 C24 -8.0(7) . . . . ? C28 N6 C23 C22 170.8(4) . . . . ? C22 C23 C24 C25 0.7(6) . . . . ? N6 C23 C24 C25 179.5(4) . . . . ? C23 C24 C25 C26 -0.4(6) . . . . ? C24 C25 C26 C27 0.3(6) . . . . ? C25 C26 C27 C22 -0.6(6) . . . . ? C23 C22 C27 C26 0.9(6) . . . . ? C10 C22 C27 C26 180.0(4) . . . . ? C23 N6 C28 O3 6.3(7) . . . . ? C23 N6 C28 C29 -173.1(4) . . . . ? O3 C28 C29 C31 58.5(6) . . . . ? N6 C28 C29 C31 -122.0(4) . . . . ? O3 C28 C29 C30 -61.7(6) . . . . ? N6 C28 C29 C30 117.7(5) . . . . ? O3 C28 C29 C32 177.1(4) . . . . ? N6 C28 C29 C32 -3.5(6) . . . . ? C33 N4 C33 C34 -0.1(3) 2_656 . . . ? Fe1 N4 C33 C34 179.9(3) . . . . ? N4 C33 C34 C35 0.2(6) . . . . ? C33 C34 C35 C34 -0.1(3) . . . 2_656 ? C36 C36 C37 C38 -3.1(16) 2_655 . . . ? C36 C37 C38 C38 1.2(13) . . . 2_655 ? _refine_diff_density_max 1.065 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.070 #===END data_gr854d _publ_requested_journal 'test' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C70 H71 Cl2 Fe N10 O6' _chemical_formula_weight 1275.12 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.583(3) _cell_length_b 19.081(3) _cell_length_c 18.267(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.113(10) _cell_angle_gamma 90.00 _cell_volume 6475.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 42 _cell_measurement_theta_min 4.09 _cell_measurement_theta_max 13.73 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method ? _exptl_crystal_F_000 2676 _exptl_absorpt_coefficient_mu 0.376 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4015 _exptl_absorpt_correction_T_max 0.4382 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 1 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.8 _diffrn_reflns_number 5251 _diffrn_reflns_av_R_equivalents 0.0724 _diffrn_reflns_av_sigmaI/netI 0.1471 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 24.01 _reflns_number_total 5076 _reflns_number_observed 2543 _reflns_observed_criterion >2sigma(I) _publ_section_references ; North, A.T.C., Phillips, D.C & mathews, F.S. (1968), Acta Cryst. A24, 351-359. ; _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0741P)^2^+6.4837P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5075 _refine_ls_number_parameters 443 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1760 _refine_ls_R_factor_obs 0.0810 _refine_ls_wR_factor_all 0.2286 _refine_ls_wR_factor_obs 0.1676 _refine_ls_goodness_of_fit_all 1.030 _refine_ls_goodness_of_fit_obs 1.148 _refine_ls_restrained_S_all 1.068 _refine_ls_restrained_S_obs 1.147 _refine_ls_shift/esd_max -0.047 _refine_ls_shift/esd_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.5000 0.64038(6) 0.7500 0.0298(3) Uani 1 d S . O1 O 0.5497(3) 0.7742(3) 0.7778(3) 0.073(2) Uani 1 d . . O2 O 0.1832(3) 0.8674(3) 0.6178(3) 0.079(2) Uani 1 d . . O3A O 0.6556(5) 0.8210(6) 0.4207(6) 0.074(3) Uani 0.50 d P 1 O3B O 0.6161(7) 0.8289(6) 0.4012(6) 0.073(4) Uani 0.50 d P 2 N1 N 0.4025(2) 0.6416(2) 0.7941(2) 0.0286(10) Uani 1 d . . N2 N 0.4557(2) 0.6382(2) 0.6502(2) 0.0288(10) Uani 1 d . . N3 N 0.5000 0.7410(3) 0.7500 0.036(2) Uani 1 d S . N4 N 0.5000 0.5291(4) 0.7500 0.041(2) Uani 1 d S . N5 N 0.2630(3) 0.7820(3) 0.6455(3) 0.0497(14) Uani 1 d . . H5 H 0.3081(3) 0.7750(3) 0.6592(3) 0.060 Uiso 1 calc R . N6 N 0.6005(3) 0.7498(3) 0.4931(3) 0.0547(15) Uani 1 d . . H6 H 0.5809(3) 0.7476(3) 0.5365(3) 0.066 Uiso 1 calc R . C1 C 0.3858(3) 0.6393(3) 0.8673(3) 0.0309(12) Uani 1 d . . C2 C 0.3106(3) 0.6476(3) 0.8763(3) 0.0404(14) Uani 1 d . . H2A H 0.2859(3) 0.6482(3) 0.9214(3) 0.048 Uiso 1 calc R . C3 C 0.2811(3) 0.6546(3) 0.8091(3) 0.0375(14) Uani 1 d . . H3A H 0.2315(3) 0.6614(3) 0.7978(3) 0.045 Uiso 1 calc R . C4 C 0.3372(3) 0.6500(3) 0.7579(3) 0.0328(13) Uani 1 d . . C5 C 0.3279(3) 0.6515(3) 0.6826(3) 0.0324(13) Uani 1 d . . C6 C 0.3834(3) 0.6443(3) 0.6324(3) 0.0299(12) Uani 1 d . . C7 C 0.3723(3) 0.6413(3) 0.5545(3) 0.0392(13) Uani 1 d . . H7A H 0.3275(3) 0.6441(3) 0.5288(3) 0.047 Uiso 1 calc R . C8 C 0.4378(3) 0.6338(3) 0.5246(3) 0.0355(13) Uani 1 d . . H8A H 0.4476(3) 0.6302(3) 0.4739(3) 0.043 Uiso 1 calc R . C9 C 0.4903(3) 0.6324(3) 0.5843(3) 0.0305(12) Uani 1 d . . C10 C 0.5634(3) 0.6321(3) 0.5753(3) 0.0327(13) Uani 1 d . . C11 C 0.2519(3) 0.6568(3) 0.6519(3) 0.0320(13) Uani 1 d . . C12 C 0.2216(3) 0.7216(3) 0.6340(3) 0.041(2) Uani 1 d . . C13 C 0.1513(3) 0.7229(4) 0.6064(4) 0.056(2) Uani 1 d . . H13A H 0.1300(3) 0.7666(4) 0.5938(4) 0.068 Uiso 1 calc R . C14 C 0.1125(4) 0.6628(4) 0.5972(4) 0.065(2) Uani 1 d . . H14A H 0.0647(4) 0.6652(4) 0.5780(4) 0.078 Uiso 1 calc R . C15 C 0.1414(3) 0.5997(4) 0.6153(4) 0.065(2) Uani 1 d . . H15A H 0.1137(3) 0.5582(4) 0.6092(4) 0.078 Uiso 1 calc R . C16 C 0.2119(3) 0.5956(3) 0.6427(4) 0.052(2) Uani 1 d . . H16A H 0.2324(3) 0.5515(3) 0.6550(4) 0.062 Uiso 1 calc R . C17 C 0.2428(3) 0.8500(3) 0.6383(3) 0.048(2) Uani 1 d . . C18 C 0.3008(3) 0.9047(3) 0.6550(4) 0.053(2) Uani 1 d . . C19 C 0.3660(4) 0.8941(4) 0.6097(4) 0.074(2) Uani 1 d . . H19A H 0.3921(18) 0.8524(18) 0.6270(21) 0.112 Uiso 1 calc R . H19B H 0.3973(16) 0.9352(14) 0.6141(26) 0.112 Uiso 1 calc R . H19C H 0.3513(4) 0.8876(31) 0.5584(6) 0.112 Uiso 1 calc R . C20A C 0.2694(6) 0.9792(5) 0.6539(7) 0.065(4) Uani 0.65 d P 1 H20A H 0.2521(37) 0.9905(15) 0.6043(12) 0.098 Uiso 0.65 calc PR 1 H20B H 0.3069(12) 1.0128(7) 0.6688(39) 0.098 Uiso 0.65 calc PR 1 H20C H 0.2294(26) 0.9819(12) 0.6878(31) 0.098 Uiso 0.65 calc PR 1 C20B C 0.2681(19) 0.9700(19) 0.6133(18) 0.123(13) Uiso 0.35 d P 2 H20D H 0.2594(118) 0.9579(42) 0.5618(34) 0.184 Uiso 0.35 calc PR 2 H20E H 0.3020(58) 1.0093(41) 0.6166(109) 0.184 Uiso 0.35 calc PR 2 H20F H 0.2226(66) 0.9834(78) 0.6356(83) 0.184 Uiso 0.35 calc PR 2 C21 C 0.3234(4) 0.9001(5) 0.7351(4) 0.083(3) Uani 1 d . . H21A H 0.3461(28) 0.8546(13) 0.7447(8) 0.125 Uiso 1 calc R . H21B H 0.2810(6) 0.9052(31) 0.7657(4) 0.125 Uiso 1 calc R . H21C H 0.3578(24) 0.9377(19) 0.7467(9) 0.125 Uiso 1 calc R . C22 C 0.5924(3) 0.6249(3) 0.4991(3) 0.0311(13) Uani 1 d . . C23 C 0.6101(3) 0.6840(3) 0.4588(3) 0.0381(14) Uani 1 d . . C24 C 0.6366(3) 0.6763(4) 0.3876(3) 0.050(2) Uani 1 d . . H24A H 0.6490(3) 0.7165(4) 0.3599(3) 0.060 Uiso 1 calc R . C25 C 0.6445(3) 0.6109(4) 0.3585(3) 0.054(2) Uani 1 d . . H25A H 0.6626(3) 0.6059(4) 0.3105(3) 0.064 Uiso 1 calc R . C26 C 0.6264(3) 0.5515(4) 0.3981(4) 0.055(2) Uani 1 d . . H26A H 0.6320(3) 0.5063(4) 0.3772(4) 0.067 Uiso 1 calc R . C27 C 0.6002(3) 0.5583(3) 0.4681(3) 0.043(2) Uani 1 d . . H27A H 0.5875(3) 0.5178(3) 0.4952(3) 0.051 Uiso 1 calc R . C28 C 0.6158(3) 0.8133(4) 0.4714(4) 0.052(2) Uani 1 d . . C29 C 0.6064(3) 0.8722(3) 0.5285(4) 0.047(2) Uani 1 d . . C30 C 0.6803(4) 0.8986(5) 0.5481(5) 0.079(3) Uani 1 d . . H30A H 0.7051(12) 0.9122(28) 0.5035(5) 0.118 Uiso 1 calc R . H30B H 0.7076(11) 0.8614(11) 0.5732(28) 0.118 Uiso 1 calc R . H30C H 0.6765(4) 0.9392(18) 0.5806(25) 0.118 Uiso 1 calc R . C31 C 0.5638(5) 0.9300(4) 0.4921(5) 0.087(3) Uani 1 d . . H31A H 0.5861(19) 0.9426(22) 0.4457(16) 0.130 Uiso 1 calc R . H31B H 0.5630(27) 0.9711(11) 0.5243(14) 0.130 Uiso 1 calc R . H31C H 0.5144(10) 0.9140(11) 0.4825(29) 0.130 Uiso 1 calc R . C32 C 0.5670(4) 0.8487(4) 0.5967(4) 0.091(3) Uani 1 d . . H32A H 0.5570(31) 0.8895(6) 0.6274(17) 0.136 Uiso 1 calc R . H32B H 0.5971(15) 0.8154(26) 0.6243(19) 0.136 Uiso 1 calc R . H32C H 0.5216(17) 0.8261(30) 0.5821(4) 0.136 Uiso 1 calc R . C34 C 0.4599(3) 0.4905(3) 0.7957(3) 0.042(2) Uani 1 d . . H34A H 0.4305(3) 0.5155(3) 0.8287(3) 0.050 Uiso 1 calc R . C35 C 0.4570(4) 0.4184(4) 0.7993(4) 0.055(2) Uani 1 d . . H35A H 0.4275(4) 0.3950(4) 0.8335(4) 0.065 Uiso 1 calc R . C36 C 0.5000 0.3810(6) 0.7500 0.065(3) Uani 1 d S . H36A H 0.5000 0.3312(6) 0.7500 0.079 Uiso 1 calc SR . C37 C 0.5129(9) 0.8839(6) 0.2686(9) 0.089(6) Uani 0.50 d PD . H37A H 0.5625(79) 0.8695(84) 0.2434(83) 0.090 Uiso 0.50 d P . H37B H 0.5110(77) 0.8617(81) 0.3306(81) 0.090 Uiso 0.50 d P . Cl1 Cl 0.4479(3) 0.8476(4) 0.2117(3) 0.132(2) Uani 0.50 d PD . Cl2 Cl 0.5087(4) 0.9738(3) 0.2701(4) 0.117(3) Uani 0.50 d PD . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0319(5) 0.0311(6) 0.0261(5) 0.000 -0.0045(4) 0.000 O1 0.075(3) 0.054(3) 0.089(4) -0.008(3) -0.009(3) -0.018(3) O2 0.065(3) 0.064(3) 0.108(4) -0.012(3) -0.023(3) 0.031(3) O3A 0.070(6) 0.088(8) 0.065(6) 0.023(6) 0.033(5) -0.035(6) O3B 0.112(9) 0.064(7) 0.044(6) 0.025(5) 0.012(6) 0.015(7) N1 0.036(2) 0.020(2) 0.030(2) 0.001(2) -0.002(2) 0.006(2) N2 0.036(2) 0.023(2) 0.027(2) 0.000(2) -0.005(2) 0.000(2) N3 0.040(4) 0.029(4) 0.038(4) 0.000 -0.003(3) 0.000 N4 0.034(3) 0.053(5) 0.037(4) 0.000 -0.002(3) 0.000 N5 0.031(2) 0.043(3) 0.074(4) 0.013(3) -0.018(2) 0.007(2) N6 0.088(4) 0.044(3) 0.033(3) 0.004(2) 0.020(3) 0.004(3) C1 0.036(3) 0.025(3) 0.032(3) -0.001(3) 0.003(2) 0.000(3) C2 0.045(3) 0.041(3) 0.036(3) -0.002(3) 0.008(2) 0.000(3) C3 0.032(3) 0.037(3) 0.044(3) -0.003(3) 0.003(2) 0.002(2) C4 0.028(2) 0.024(3) 0.046(3) 0.000(3) 0.000(2) 0.000(2) C5 0.034(3) 0.028(3) 0.034(3) 0.000(2) -0.009(2) 0.002(2) C6 0.035(2) 0.028(3) 0.026(3) -0.002(2) -0.006(2) 0.001(2) C7 0.036(3) 0.041(3) 0.040(3) -0.001(3) -0.013(2) 0.001(3) C8 0.046(3) 0.037(3) 0.023(2) -0.001(3) -0.005(2) 0.005(3) C9 0.041(3) 0.020(3) 0.030(3) 0.000(2) -0.005(2) 0.001(2) C10 0.042(3) 0.024(3) 0.032(3) -0.004(2) -0.002(2) 0.000(2) C11 0.032(3) 0.034(3) 0.030(3) -0.003(2) -0.004(2) 0.006(2) C12 0.036(3) 0.042(3) 0.046(3) 0.005(3) -0.006(3) 0.001(3) C13 0.046(4) 0.052(4) 0.070(5) 0.007(4) -0.017(3) 0.008(3) C14 0.041(3) 0.079(6) 0.074(5) -0.014(4) -0.019(3) 0.005(4) C15 0.042(4) 0.066(5) 0.086(5) -0.042(4) -0.013(3) -0.012(3) C16 0.042(3) 0.041(4) 0.071(4) -0.011(3) -0.011(3) 0.002(3) C17 0.043(3) 0.051(4) 0.050(3) 0.007(3) 0.003(3) 0.015(3) C18 0.052(4) 0.038(4) 0.070(4) 0.012(3) 0.004(3) 0.002(3) C19 0.068(4) 0.070(5) 0.087(5) 0.008(4) 0.024(4) -0.003(4) C20A 0.076(7) 0.026(5) 0.095(9) -0.014(6) 0.007(7) 0.002(5) C21 0.067(5) 0.100(7) 0.083(6) -0.011(5) 0.009(4) -0.023(5) C22 0.036(3) 0.031(3) 0.026(3) -0.003(2) -0.006(2) 0.005(2) C23 0.039(3) 0.039(3) 0.036(3) -0.006(3) 0.002(2) 0.011(3) C24 0.046(3) 0.061(4) 0.042(3) 0.007(3) 0.001(3) -0.006(3) C25 0.045(3) 0.078(5) 0.037(3) -0.023(3) -0.006(3) 0.010(3) C26 0.043(3) 0.066(5) 0.057(4) -0.023(4) -0.001(3) 0.008(3) C27 0.050(3) 0.043(4) 0.034(3) -0.007(3) -0.001(3) -0.004(3) C28 0.058(4) 0.043(4) 0.055(4) 0.003(3) 0.017(3) -0.010(3) C29 0.041(3) 0.037(4) 0.063(4) 0.001(3) 0.002(3) -0.001(3) C30 0.043(4) 0.088(6) 0.105(6) -0.023(5) -0.002(4) 0.003(4) C31 0.103(6) 0.044(5) 0.111(7) -0.009(5) -0.046(5) 0.002(4) C32 0.105(6) 0.074(6) 0.095(5) -0.049(4) 0.049(5) -0.018(5) C34 0.045(3) 0.033(3) 0.048(3) 0.002(3) -0.001(3) -0.001(3) C35 0.055(4) 0.049(4) 0.059(4) 0.005(3) -0.005(3) -0.009(3) C36 0.073(6) 0.047(6) 0.075(7) 0.000 -0.027(6) 0.000 C37 0.074(13) 0.114(14) 0.079(16) 0.030(10) -0.004(10) 0.022(11) Cl1 0.108(3) 0.202(7) 0.085(3) -0.042(4) 0.013(3) -0.063(4) Cl2 0.110(4) 0.114(4) 0.129(7) 0.005(4) -0.001(4) -0.024(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N3 1.920(7) . ? Fe1 N2 1.987(4) 2_656 ? Fe1 N2 1.987(4) . ? Fe1 N1 1.997(4) . ? Fe1 N1 1.997(4) 2_656 ? Fe1 N4 2.123(7) . ? O1 N3 1.223(6) . ? O2 C17 1.210(7) . ? O3A C28 1.205(11) . ? O3B C28 1.316(12) . ? N1 C1 1.378(6) . ? N1 C4 1.381(6) . ? N2 C9 1.380(6) . ? N2 C6 1.381(6) . ? N3 O1 1.223(6) 2_656 ? N4 C34 1.349(7) . ? N4 C34 1.349(7) 2_656 ? N5 C17 1.355(8) . ? N5 C12 1.401(8) . ? N6 C28 1.308(8) . ? N6 C23 1.417(8) . ? C1 C10 1.404(7) 2_656 ? C1 C2 1.420(7) . ? C2 C3 1.342(8) . ? C3 C4 1.416(7) . ? C4 C5 1.383(7) . ? C5 C6 1.400(7) . ? C5 C11 1.513(7) . ? C6 C7 1.435(7) . ? C7 C8 1.350(7) . ? C8 C9 1.449(7) . ? C9 C10 1.371(7) . ? C10 C1 1.404(7) 2_656 ? C10 C22 1.509(7) . ? C11 C16 1.392(8) . ? C11 C12 1.395(8) . ? C12 C13 1.390(8) . ? C13 C14 1.364(10) . ? C14 C15 1.357(10) . ? C15 C16 1.394(9) . ? C17 C18 1.527(9) . ? C18 C19 1.493(9) . ? C18 C21 1.516(10) . ? C18 C20A 1.538(12) . ? C18 C20B 1.58(4) . ? C22 C23 1.390(8) . ? C22 C27 1.399(8) . ? C23 C24 1.406(8) . ? C24 C25 1.366(9) . ? C25 C26 1.389(10) . ? C26 C27 1.383(8) . ? C28 C29 1.546(9) . ? C29 C30 1.499(9) . ? C29 C31 1.506(10) . ? C29 C32 1.524(9) . ? C34 C35 1.378(9) . ? C35 C36 1.410(8) . ? C36 C35 1.410(8) 2_656 ? C37 C37 0.82(3) 2_655 ? C37 Cl1 1.06(2) 2_655 ? C37 Cl2 1.717(12) . ? C37 Cl1 1.724(13) . ? C37 Cl2 1.895(14) 2_655 ? Cl1 C37 1.06(2) 2_655 ? Cl1 Cl1 2.367(12) 2_655 ? Cl2 Cl2 0.796(13) 2_655 ? Cl2 C37 1.895(14) 2_655 ? 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 N3 Fe1 N2 91.19(13) . 2_656 ? N3 Fe1 N2 91.19(13) . . ? N2 Fe1 N2 177.6(3) 2_656 . ? N3 Fe1 N1 89.34(13) . . ? N2 Fe1 N1 89.58(15) 2_656 . ? N2 Fe1 N1 90.4(2) . . ? N3 Fe1 N1 89.34(13) . 2_656 ? N2 Fe1 N1 90.4(2) 2_656 2_656 ? N2 Fe1 N1 89.58(15) . 2_656 ? N1 Fe1 N1 178.7(3) . 2_656 ? N3 Fe1 N4 180.000(2) . . ? N2 Fe1 N4 88.81(13) 2_656 . ? N2 Fe1 N4 88.81(13) . . ? N1 Fe1 N4 90.66(13) . . ? N1 Fe1 N4 90.66(13) 2_656 . ? C1 N1 C4 104.9(4) . . ? C1 N1 Fe1 127.9(3) . . ? C4 N1 Fe1 127.1(3) . . ? C9 N2 C6 105.6(4) . . ? C9 N2 Fe1 127.6(3) . . ? C6 N2 Fe1 126.7(3) . . ? O1 N3 O1 117.5(7) . 2_656 ? O1 N3 Fe1 121.2(4) . . ? O1 N3 Fe1 121.2(4) 2_656 . ? C34 N4 C34 113.7(7) . 2_656 ? C34 N4 Fe1 123.1(4) . . ? C34 N4 Fe1 123.1(4) 2_656 . ? C17 N5 C12 128.6(5) . . ? C28 N6 C23 131.1(5) . . ? N1 C1 C10 124.6(4) . 2_656 ? N1 C1 C2 110.5(4) . . ? C10 C1 C2 124.9(4) 2_656 . ? C3 C2 C1 106.8(4) . . ? C2 C3 C4 107.8(5) . . ? N1 C4 C5 124.8(4) . . ? N1 C4 C3 110.0(5) . . ? C5 C4 C3 125.1(5) . . ? C4 C5 C6 124.8(5) . . ? C4 C5 C11 117.9(4) . . ? C6 C5 C11 117.2(4) . . ? N2 C6 C5 125.4(4) . . ? N2 C6 C7 110.5(4) . . ? C5 C6 C7 124.1(5) . . ? C8 C7 C6 107.0(5) . . ? C7 C8 C9 107.3(4) . . ? C10 C9 N2 125.8(5) . . ? C10 C9 C8 124.3(4) . . ? N2 C9 C8 109.6(4) . . ? C9 C10 C1 124.2(4) . 2_656 ? C9 C10 C22 118.9(5) . . ? C1 C10 C22 116.9(4) 2_656 . ? C16 C11 C12 120.2(5) . . ? C16 C11 C5 118.8(5) . . ? C12 C11 C5 121.0(5) . . ? C13 C12 C11 118.3(6) . . ? C13 C12 N5 123.2(6) . . ? C11 C12 N5 118.5(5) . . ? C14 C13 C12 121.3(7) . . ? C15 C14 C13 120.7(6) . . ? C14 C15 C16 120.1(7) . . ? C11 C16 C15 119.5(6) . . ? O2 C17 N5 122.9(6) . . ? O2 C17 C18 120.9(6) . . ? N5 C17 C18 116.2(5) . . ? C19 C18 C21 108.3(6) . . ? C19 C18 C17 112.0(6) . . ? C21 C18 C17 109.5(6) . . ? C19 C18 C20A 115.4(7) . . ? C21 C18 C20A 99.4(7) . . ? C17 C18 C20A 111.3(7) . . ? C19 C18 C20B 98.5(13) . . ? C21 C18 C20B 127.5(14) . . ? C17 C18 C20B 100.3(14) . . ? C23 C22 C27 119.7(5) . . ? C23 C22 C10 120.5(5) . . ? C27 C22 C10 119.8(5) . . ? C22 C23 C24 119.8(6) . . ? C22 C23 N6 116.9(5) . . ? C24 C23 N6 123.4(6) . . ? C25 C24 C23 119.8(6) . . ? C24 C25 C26 120.9(6) . . ? C27 C26 C25 119.8(6) . . ? C26 C27 C22 120.0(6) . . ? O3A C28 N6 119.0(8) . . ? N6 C28 O3B 120.6(8) . . ? O3A C28 C29 120.6(8) . . ? N6 C28 C29 116.2(5) . . ? O3B C28 C29 119.8(7) . . ? C30 C29 C31 109.4(6) . . ? C30 C29 C32 110.9(6) . . ? C31 C29 C32 108.6(6) . . ? C30 C29 C28 106.9(5) . . ? C31 C29 C28 107.4(6) . . ? C32 C29 C28 113.5(5) . . ? N4 C34 C35 126.7(6) . . ? C34 C35 C36 116.8(7) . . ? C35 C36 C35 119.2(10) . 2_656 ? C37 C37 Cl1 131.6(19) 2_655 2_655 ? C37 C37 Cl2 89.2(5) 2_655 . ? Cl1 C37 Cl2 132.6(11) 2_655 . ? C37 C37 Cl1 27.5(11) 2_655 . ? Cl1 C37 Cl1 114.2(11) 2_655 . ? Cl2 C37 Cl1 112.3(9) . . ? C37 C37 Cl2 65.0(4) 2_655 2_655 ? Cl1 C37 Cl2 148.8(13) 2_655 2_655 ? Cl2 C37 Cl2 24.8(4) . 2_655 ? Cl1 C37 Cl2 89.9(7) . 2_655 ? C37 Cl1 C37 21.0(11) 2_655 . ? C37 Cl1 Cl1 41.6(8) 2_655 2_655 ? C37 Cl1 Cl1 24.2(5) . 2_655 ? Cl2 Cl2 C37 90.2(5) 2_655 . ? Cl2 Cl2 C37 65.0(4) 2_655 2_655 ? C37 Cl2 C37 25.8(8) . 2_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Fe1 N1 C1 -92.8(4) . . . . ? N2 Fe1 N1 C1 -1.6(5) 2_656 . . . ? N2 Fe1 N1 C1 176.0(5) . . . . ? N1 Fe1 N1 C1 -92.8(4) 2_656 . . . ? N4 Fe1 N1 C1 87.2(4) . . . . ? N3 Fe1 N1 C4 82.1(4) . . . . ? N2 Fe1 N1 C4 173.3(4) 2_656 . . . ? N2 Fe1 N1 C4 -9.1(4) . . . . ? N1 Fe1 N1 C4 82.1(4) 2_656 . . . ? N4 Fe1 N1 C4 -97.9(4) . . . . ? N3 Fe1 N2 C9 94.9(4) . . . . ? N2 Fe1 N2 C9 -85.1(4) 2_656 . . . ? N1 Fe1 N2 C9 -175.7(4) . . . . ? N1 Fe1 N2 C9 5.6(4) 2_656 . . . ? N4 Fe1 N2 C9 -85.1(4) . . . . ? N3 Fe1 N2 C6 -83.1(4) . . . . ? N2 Fe1 N2 C6 96.9(4) 2_656 . . . ? N1 Fe1 N2 C6 6.2(5) . . . . ? N1 Fe1 N2 C6 -172.4(5) 2_656 . . . ? N4 Fe1 N2 C6 96.9(4) . . . . ? N2 Fe1 N3 O1 37.5(3) 2_656 . . . ? N2 Fe1 N3 O1 -142.5(3) . . . . ? N1 Fe1 N3 O1 127.1(3) . . . . ? N1 Fe1 N3 O1 -52.9(3) 2_656 . . . ? N4 Fe1 N3 O1 150.9(1000) . . . . ? N2 Fe1 N3 O1 -142.5(3) 2_656 . . 2_656 ? N2 Fe1 N3 O1 37.5(3) . . . 2_656 ? N1 Fe1 N3 O1 -52.9(3) . . . 2_656 ? N1 Fe1 N3 O1 127.1(3) 2_656 . . 2_656 ? N4 Fe1 N3 O1 -29.1(1000) . . . 2_656 ? N3 Fe1 N4 C34 -47.6(1000) . . . . ? N2 Fe1 N4 C34 65.8(3) 2_656 . . . ? N2 Fe1 N4 C34 -114.2(3) . . . . ? N1 Fe1 N4 C34 -23.8(3) . . . . ? N1 Fe1 N4 C34 156.2(3) 2_656 . . . ? N3 Fe1 N4 C34 132.4(1000) . . . 2_656 ? N2 Fe1 N4 C34 -114.2(3) 2_656 . . 2_656 ? N2 Fe1 N4 C34 65.8(3) . . . 2_656 ? N1 Fe1 N4 C34 156.2(3) . . . 2_656 ? N1 Fe1 N4 C34 -23.8(3) 2_656 . . 2_656 ? C4 N1 C1 C10 -179.2(5) . . . 2_656 ? Fe1 N1 C1 C10 -3.4(8) . . . 2_656 ? C4 N1 C1 C2 -1.0(6) . . . . ? Fe1 N1 C1 C2 174.7(4) . . . . ? N1 C1 C2 C3 0.3(7) . . . . ? C10 C1 C2 C3 178.4(5) 2_656 . . . ? C1 C2 C3 C4 0.5(7) . . . . ? C1 N1 C4 C5 -176.6(5) . . . . ? Fe1 N1 C4 C5 7.6(8) . . . . ? C1 N1 C4 C3 1.4(6) . . . . ? Fe1 N1 C4 C3 -174.4(4) . . . . ? C2 C3 C4 N1 -1.2(7) . . . . ? C2 C3 C4 C5 176.8(5) . . . . ? N1 C4 C5 C6 0.3(9) . . . . ? C3 C4 C5 C6 -177.4(5) . . . . ? N1 C4 C5 C11 176.3(5) . . . . ? C3 C4 C5 C11 -1.4(8) . . . . ? C9 N2 C6 C5 -179.9(5) . . . . ? Fe1 N2 C6 C5 -1.6(8) . . . . ? C9 N2 C6 C7 0.8(6) . . . . ? Fe1 N2 C6 C7 179.1(4) . . . . ? C4 C5 C6 N2 -3.4(9) . . . . ? C11 C5 C6 N2 -179.5(5) . . . . ? C4 C5 C6 C7 175.7(6) . . . . ? C11 C5 C6 C7 -0.3(8) . . . . ? N2 C6 C7 C8 -0.3(7) . . . . ? C5 C6 C7 C8 -179.6(5) . . . . ? C6 C7 C8 C9 -0.2(6) . . . . ? C6 N2 C9 C10 173.3(5) . . . . ? Fe1 N2 C9 C10 -5.0(8) . . . . ? C6 N2 C9 C8 -0.9(6) . . . . ? Fe1 N2 C9 C8 -179.3(4) . . . . ? C7 C8 C9 C10 -173.6(5) . . . . ? C7 C8 C9 N2 0.8(6) . . . . ? N2 C9 C10 C1 -1.6(9) . . . 2_656 ? C8 C9 C10 C1 171.9(5) . . . 2_656 ? N2 C9 C10 C22 179.7(5) . . . . ? C8 C9 C10 C22 -6.9(8) . . . . ? C4 C5 C11 C16 -85.1(7) . . . . ? C6 C5 C11 C16 91.2(7) . . . . ? C4 C5 C11 C12 93.9(6) . . . . ? C6 C5 C11 C12 -89.8(7) . . . . ? C16 C11 C12 C13 -0.6(9) . . . . ? C5 C11 C12 C13 -179.6(5) . . . . ? C16 C11 C12 N5 178.6(5) . . . . ? C5 C11 C12 N5 -0.4(8) . . . . ? C17 N5 C12 C13 5.6(10) . . . . ? C17 N5 C12 C11 -173.6(6) . . . . ? C11 C12 C13 C14 0.3(10) . . . . ? N5 C12 C13 C14 -178.9(6) . . . . ? C12 C13 C14 C15 0.4(11) . . . . ? C13 C14 C15 C16 -0.8(11) . . . . ? C12 C11 C16 C15 0.2(9) . . . . ? C5 C11 C16 C15 179.3(6) . . . . ? C14 C15 C16 C11 0.5(11) . . . . ? C12 N5 C17 O2 -2.3(10) . . . . ? C12 N5 C17 C18 179.9(6) . . . . ? O2 C17 C18 C19 -122.0(7) . . . . ? N5 C17 C18 C19 55.9(8) . . . . ? O2 C17 C18 C21 117.8(7) . . . . ? N5 C17 C18 C21 -64.3(7) . . . . ? O2 C17 C18 C20A 8.9(10) . . . . ? N5 C17 C18 C20A -173.3(7) . . . . ? O2 C17 C18 C20B -18.3(14) . . . . ? N5 C17 C18 C20B 159.5(13) . . . . ? C9 C10 C22 C23 94.6(6) . . . . ? C1 C10 C22 C23 -84.3(7) 2_656 . . . ? C9 C10 C22 C27 -84.2(7) . . . . ? C1 C10 C22 C27 96.9(6) 2_656 . . . ? C27 C22 C23 C24 -0.8(8) . . . . ? C10 C22 C23 C24 -179.6(5) . . . . ? C27 C22 C23 N6 179.6(5) . . . . ? C10 C22 C23 N6 0.8(8) . . . . ? C28 N6 C23 C22 175.8(7) . . . . ? C28 N6 C23 C24 -3.8(11) . . . . ? C22 C23 C24 C25 0.2(9) . . . . ? N6 C23 C24 C25 179.8(6) . . . . ? C23 C24 C25 C26 0.3(9) . . . . ? C24 C25 C26 C27 -0.2(10) . . . . ? C25 C26 C27 C22 -0.4(9) . . . . ? C23 C22 C27 C26 0.9(8) . . . . ? C10 C22 C27 C26 179.7(5) . . . . ? C23 N6 C28 O3A -15.2(13) . . . . ? C23 N6 C28 O3B 28.6(12) . . . . ? C23 N6 C28 C29 -172.3(6) . . . . ? O3A C28 C29 C30 -45.4(10) . . . . ? N6 C28 C29 C30 111.3(7) . . . . ? O3B C28 C29 C30 -89.4(10) . . . . ? O3A C28 C29 C31 72.0(10) . . . . ? N6 C28 C29 C31 -131.3(7) . . . . ? O3B C28 C29 C31 27.9(10) . . . . ? O3A C28 C29 C32 -168.0(9) . . . . ? N6 C28 C29 C32 -11.2(9) . . . . ? O3B C28 C29 C32 148.0(9) . . . . ? C34 N4 C34 C35 0.3(5) 2_656 . . . ? Fe1 N4 C34 C35 -179.7(5) . . . . ? N4 C34 C35 C36 -0.6(9) . . . . ? C34 C35 C36 C35 0.2(4) . . . 2_656 ? C37 C37 Cl1 C37 0.000(10) 2_655 . . 2_655 ? Cl1 C37 Cl1 C37 -135.5(54) 2_655 . . 2_655 ? Cl2 C37 Cl1 C37 35.0(31) . . . 2_655 ? Cl2 C37 Cl1 C37 24.0(35) 2_655 . . 2_655 ? C37 C37 Cl1 Cl1 135.5(54) 2_655 . . 2_655 ? Cl1 C37 Cl1 Cl1 0.000(4) 2_655 . . 2_655 ? Cl2 C37 Cl1 Cl1 170.5(24) . . . 2_655 ? Cl2 C37 Cl1 Cl1 159.5(20) 2_655 . . 2_655 ? C37 C37 Cl2 Cl2 -11.6(30) 2_655 . . 2_655 ? Cl1 C37 Cl2 Cl2 141.2(23) 2_655 . . 2_655 ? Cl1 C37 Cl2 Cl2 -26.9(16) . . . 2_655 ? Cl2 C37 Cl2 Cl2 0.000(7) 2_655 . . 2_655 ? C37 C37 Cl2 C37 0.000(6) 2_655 . . 2_655 ? Cl1 C37 Cl2 C37 152.8(47) 2_655 . . 2_655 ? Cl1 C37 Cl2 C37 -15.3(18) . . . 2_655 ? Cl2 C37 Cl2 C37 11.6(30) 2_655 . . 2_655 ? _refine_diff_density_max 0.393 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.069 #===END