Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Michael Hill' _publ_contact_author_email M.S.HILL@BATH.AC.UK _publ_section_title ; Organoiron Compounds Derived From the Indium 'Carbene Analogues', [In{N(Ar)C(Me)}2CH] (Ar = Dipp = 2,6-iPr2C6H3; = Mes = 2,4,6-Me3C6H2) ; _publ_requested_category FM loop_ _publ_author_name 'Michael Hill' 'Peter B Hitchcock' 'Ruti Pongtavornpinyo' # Attachment 'msh-jan-2007.cif' data_(1)-jan305 _database_code_depnum_ccdc_archive 'CCDC 675700' _audit_creation_date 2005-01-07T15:13:45-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C36 H46 Fe I In N2 O2' _chemical_formula_sum 'C36 H46 Fe I In N2 O2' _chemical_formula_weight 836.32 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 18.4839(3) _cell_length_b 20.9025(3) _cell_length_c 20.2107(3) _cell_angle_alpha 90 _cell_angle_beta 114.284(1) _cell_angle_gamma 90 _cell_volume 7117.7(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 46569 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3360 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.955 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.5027 _exptl_absorpt_correction_T_max 0.6384 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.131742E-1 _diffrn_orient_matrix_ub_12 -0.173105E-1 _diffrn_orient_matrix_ub_13 0.497548E-1 _diffrn_orient_matrix_ub_21 0.12135E-1 _diffrn_orient_matrix_ub_22 0.442638E-1 _diffrn_orient_matrix_ub_23 0.203787E-1 _diffrn_orient_matrix_ub_31 -0.565856E-1 _diffrn_orient_matrix_ub_32 0.54624E-2 _diffrn_orient_matrix_ub_33 -0.74613E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0891 _diffrn_reflns_av_unetI/netI 0.0567 _diffrn_reflns_number 97021 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 26.02 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 13978 _reflns_number_gt 9753 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0400P)^2^+9.1989P] 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_number_reflns 13978 _refine_ls_number_parameters 779 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0967 _refine_ls_wR_factor_gt 0.0833 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.549 _refine_diff_density_min -1.169 _refine_diff_density_rms 0.119 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.31 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 In In -0.508984(18) 0.246878(14) 0.150096(16) 0.01884(8) Uani 1 1 d . . . Fe Fe -0.59638(4) 0.27161(3) 0.21461(3) 0.02420(16) Uani 1 1 d . A . I I -0.350752(18) 0.233017(16) 0.251148(18) 0.03635(10) Uani 1 1 d . A 1 O1 O -0.5984(3) 0.13598(19) 0.2459(2) 0.0667(13) Uani 1 1 d . A 1 O2 O -0.7434(2) 0.2733(2) 0.0843(2) 0.0534(11) Uani 1 1 d . A 1 N1 N -0.4913(2) 0.31357(16) 0.07454(19) 0.0205(8) Uani 1 1 d . A 1 N2 N -0.5157(2) 0.16821(16) 0.07809(18) 0.0210(8) Uani 1 1 d . A 1 C1 C -0.4619(3) 0.2932(2) 0.0289(2) 0.0233(10) Uani 1 1 d . A 1 C2 C -0.4523(3) 0.2290(2) 0.0146(2) 0.0256(10) Uani 1 1 d . A 1 H2 H -0.4209 0.2227 -0.0121 0.031 Uiso 1 1 calc R A 1 C3 C -0.4802(2) 0.1727(2) 0.0322(2) 0.0216(10) Uani 1 1 d . A 1 C4 C -0.4367(3) 0.3415(2) -0.0134(3) 0.0390(13) Uani 1 1 d . A 1 H4A H -0.4626 0.3826 -0.0143 0.059 Uiso 1 1 calc R A 1 H4B H -0.4523 0.3261 -0.0632 0.059 Uiso 1 1 calc R A 1 H4C H -0.379 0.3469 0.0099 0.059 Uiso 1 1 calc R A 1 C5 C -0.4711(3) 0.1131(2) -0.0060(3) 0.0336(12) Uani 1 1 d . A 1 H5A H -0.4241 0.0893 0.0262 0.05 Uiso 1 1 calc R A 1 H5B H -0.4649 0.1251 -0.0503 0.05 Uiso 1 1 calc R A 1 H5C H -0.5183 0.0861 -0.0188 0.05 Uiso 1 1 calc R A 1 C6 C -0.5078(3) 0.3801(2) 0.0809(2) 0.0248(11) Uani 1 1 d . A 1 C7 C -0.4473(3) 0.4220(2) 0.1249(3) 0.0287(11) Uani 1 1 d . A 1 C8 C -0.4684(3) 0.4833(2) 0.1362(3) 0.0356(12) Uani 1 1 d . A 1 H8 H -0.4285 0.5119 0.166 0.043 Uiso 1 1 calc R A 1 C9 C -0.5463(3) 0.5036(2) 0.1049(3) 0.0391(13) Uani 1 1 d . A 1 H9 H -0.5598 0.5452 0.115 0.047 Uiso 1 1 calc R A 1 C10 C -0.6041(3) 0.4637(2) 0.0592(3) 0.0346(12) Uani 1 1 d . A 1 H10 H -0.6571 0.4791 0.0366 0.042 Uiso 1 1 calc R A 1 C11 C -0.5880(3) 0.4016(2) 0.0449(3) 0.0273(11) Uani 1 1 d . A 1 C12 C -0.3591(3) 0.4039(2) 0.1589(3) 0.0327(12) Uani 1 1 d . A 1 H12 H -0.354 0.3579 0.1479 0.039 Uiso 1 1 calc R A 1 C13 C -0.3226(3) 0.4126(2) 0.2412(3) 0.0429(14) Uani 1 1 d . A 1 H13A H -0.2664 0.4007 0.261 0.064 Uiso 1 1 calc R A 1 H13B H -0.3506 0.3854 0.2625 0.064 Uiso 1 1 calc R A 1 H13C H -0.3275 0.4575 0.2529 0.064 Uiso 1 1 calc R A 1 C14 C -0.3120(3) 0.4447(3) 0.1269(3) 0.0473(15) Uani 1 1 d . A 1 H14A H -0.256 0.4321 0.1491 0.071 Uiso 1 1 calc R A 1 H14B H -0.3169 0.49 0.1369 0.071 Uiso 1 1 calc R A 1 H14C H -0.3332 0.4379 0.0743 0.071 Uiso 1 1 calc R A 1 C15 C -0.6513(3) 0.3584(2) -0.0073(3) 0.0334(12) Uani 1 1 d . A 1 H15 H -0.644 0.3149 0.0152 0.04 Uiso 1 1 calc R A 1 C16 C -0.7358(3) 0.3809(3) -0.0225(3) 0.0548(16) Uani 1 1 d . A 1 H16A H -0.7744 0.3512 -0.0563 0.082 Uiso 1 1 calc R A 1 H16B H -0.7443 0.4238 -0.0439 0.082 Uiso 1 1 calc R A 1 H16C H -0.7427 0.3821 0.0231 0.082 Uiso 1 1 calc R A 1 C17 C -0.6438(3) 0.3519(3) -0.0799(3) 0.0469(14) Uani 1 1 d . A 1 H17A H -0.6856 0.3235 -0.1121 0.07 Uiso 1 1 calc R A 1 H17B H -0.5917 0.3339 -0.0713 0.07 Uiso 1 1 calc R A 1 H17C H -0.6492 0.3941 -0.1025 0.07 Uiso 1 1 calc R A 1 C18 C -0.5514(3) 0.1085(2) 0.0852(2) 0.0251(11) Uani 1 1 d . A 1 C19 C -0.5057(3) 0.0595(2) 0.1303(3) 0.0333(12) Uani 1 1 d . A 1 C20 C -0.5444(4) 0.0037(2) 0.1360(3) 0.0457(14) Uani 1 1 d . A 1 H20 H -0.5144 -0.0301 0.1665 0.055 Uiso 1 1 calc R A 1 C21 C -0.6249(4) -0.0033(3) 0.0986(3) 0.0516(16) Uani 1 1 d . A 1 H21 H -0.6499 -0.042 0.1021 0.062 Uiso 1 1 calc R A 1 C22 C -0.6693(3) 0.0459(3) 0.0559(3) 0.0481(16) Uani 1 1 d . A 1 H22 H -0.7252 0.0409 0.0312 0.058 Uiso 1 1 calc R A 1 C23 C -0.6349(3) 0.1023(2) 0.0479(3) 0.0313(12) Uani 1 1 d . A 1 C24 C -0.4166(3) 0.0645(2) 0.1747(3) 0.0389(13) Uani 1 1 d . A 1 H24 H -0.3988 0.1073 0.165 0.047 Uiso 1 1 calc R A 1 C25 C -0.3970(4) 0.0603(3) 0.2559(3) 0.0589(17) Uani 1 1 d . A 1 H25A H -0.3395 0.0641 0.2838 0.088 Uiso 1 1 calc R A 1 H25B H -0.415 0.019 0.2665 0.088 Uiso 1 1 calc R A 1 H25C H -0.4239 0.095 0.2695 0.088 Uiso 1 1 calc R A 1 C26 C -0.3705(4) 0.0129(3) 0.1538(3) 0.0589(17) Uani 1 1 d . A 1 H26A H -0.3135 0.0181 0.1833 0.088 Uiso 1 1 calc R A 1 H26B H -0.3812 0.0173 0.1023 0.088 Uiso 1 1 calc R A 1 H26C H -0.3874 -0.0295 0.1624 0.088 Uiso 1 1 calc R A 1 C27 C -0.6841(3) 0.1551(3) -0.0009(3) 0.0377(13) Uani 1 1 d . A 1 H27 H -0.6606 0.1967 0.0225 0.045 Uiso 1 1 calc R A 1 C28 C -0.6808(3) 0.1536(3) -0.0760(3) 0.0605(18) Uani 1 1 d . A 1 H28A H -0.7128 0.1887 -0.1059 0.091 Uiso 1 1 calc R A 1 H28B H -0.7018 0.1127 -0.0999 0.091 Uiso 1 1 calc R A 1 H28C H -0.6256 0.1584 -0.0699 0.091 Uiso 1 1 calc R A 1 C29 C -0.7713(3) 0.1550(3) -0.0122(3) 0.0619(19) Uani 1 1 d . A 1 H29A H -0.799 0.1908 -0.0439 0.093 Uiso 1 1 calc R A 1 H29B H -0.7744 0.1597 0.0348 0.093 Uiso 1 1 calc R A 1 H29C H -0.7961 0.1146 -0.0348 0.093 Uiso 1 1 calc R A 1 C30 C -0.5982(3) 0.3707(2) 0.2270(3) 0.0406(14) Uani 1 1 d . A 1 H30 H -0.6218 0.4003 0.1883 0.049 Uiso 1 1 calc R A 1 C31 C -0.5190(3) 0.3491(3) 0.2551(3) 0.0426(15) Uani 1 1 d . A 1 H31 H -0.4797 0.3619 0.2389 0.051 Uiso 1 1 calc R A 1 C32 C -0.5085(3) 0.3056(3) 0.3107(3) 0.0433(14) Uani 1 1 d . A 1 H32 H -0.461 0.283 0.3385 0.052 Uiso 1 1 calc R A 1 C33 C -0.5811(4) 0.3011(3) 0.3182(3) 0.0429(14) Uani 1 1 d . A 1 H33 H -0.5906 0.2754 0.3526 0.052 Uiso 1 1 calc R A 1 C34 C -0.6361(3) 0.3406(2) 0.2667(3) 0.0399(14) Uani 1 1 d . A 1 H34 H -0.6898 0.3463 0.2594 0.048 Uiso 1 1 calc R A 1 C35 C -0.5973(3) 0.1891(3) 0.2315(3) 0.0374(13) Uani 1 1 d . A 1 C36 C -0.6836(3) 0.2701(2) 0.1347(3) 0.0315(12) Uani 1 1 d . A 1 In1B In 0.015721(18) 0.246567(14) 0.160391(16) 0.02010(8) Uani 1 1 d . . . Fe1B Fe -0.05402(4) 0.26196(3) 0.24331(4) 0.03012(17) Uani 1 1 d . B . I1B I 0.180411(18) 0.235396(16) 0.228091(18) 0.03381(9) Uani 1 1 d . B 1 O1B O -0.0529(3) 0.1255(2) 0.2667(3) 0.0773(15) Uani 1 1 d . B 1 O2B O 0.1008(3) 0.2826(3) 0.3624(2) 0.0727(14) Uani 1 1 d . B 1 N1B N 0.0053(2) 0.31219(16) 0.07335(18) 0.0185(8) Uani 1 1 d . B 1 N2B N -0.0050(2) 0.16811(16) 0.08362(18) 0.0199(8) Uani 1 1 d . B 1 C1B C 0.0367(2) 0.2937(2) 0.0274(2) 0.0205(10) Uani 1 1 d . B 1 C2B C 0.0486(2) 0.2300(2) 0.0132(2) 0.0227(10) Uani 1 1 d . B 1 H2B H 0.0793 0.2247 -0.0142 0.027 Uiso 1 1 calc R B 1 C3B C 0.0230(2) 0.1724(2) 0.0325(2) 0.0236(10) Uani 1 1 d . B 1 C4B C 0.0635(3) 0.3437(2) -0.0117(3) 0.0311(12) Uani 1 1 d . B 1 H4B1 H 0.0287 0.3812 -0.0217 0.047 Uiso 1 1 calc R B 1 H4B2 H 0.0608 0.326 -0.0576 0.047 Uiso 1 1 calc R B 1 H4B3 H 0.1182 0.3564 0.0187 0.047 Uiso 1 1 calc R B 1 C5B C 0.0267(3) 0.1139(2) -0.0096(3) 0.0321(12) Uani 1 1 d . B 1 H5B1 H 0.0796 0.0947 0.0135 0.048 Uiso 1 1 calc R B 1 H5B2 H 0.0161 0.1261 -0.0595 0.048 Uiso 1 1 calc R B 1 H5B3 H -0.0132 0.0828 -0.01 0.048 Uiso 1 1 calc R B 1 C6B C -0.0218(3) 0.3772(2) 0.0728(2) 0.0224(10) Uani 1 1 d . B 1 C7B C 0.0290(3) 0.4239(2) 0.1186(2) 0.0245(10) Uani 1 1 d . B 1 C8B C -0.0025(3) 0.4838(2) 0.1217(3) 0.0330(12) Uani 1 1 d . B 1 H8B H 0.0308 0.5156 0.1532 0.04 Uiso 1 1 calc R B 1 C9B C -0.0811(3) 0.4977(2) 0.0801(3) 0.0358(12) Uani 1 1 d . B 1 H9B H -0.1017 0.5387 0.0829 0.043 Uiso 1 1 calc R B 1 C10B C -0.1295(3) 0.4521(2) 0.0345(3) 0.0347(12) Uani 1 1 d . B 1 H10B H -0.1836 0.4623 0.0062 0.042 Uiso 1 1 calc R B 1 C11B C -0.1021(3) 0.3918(2) 0.0284(2) 0.0235(10) Uani 1 1 d . B 1 C12B C 0.1164(3) 0.4112(2) 0.1650(2) 0.0305(11) Uani 1 1 d . B 1 H12B H 0.1284 0.3665 0.1549 0.037 Uiso 1 1 calc R B 1 C13B C 0.1355(3) 0.4158(3) 0.2457(3) 0.0421(14) Uani 1 1 d . B 1 H13D H 0.1921 0.4074 0.2739 0.063 Uiso 1 1 calc R B 1 H13E H 0.1041 0.3841 0.2582 0.063 Uiso 1 1 calc R B 1 H13F H 0.1226 0.4588 0.2568 0.063 Uiso 1 1 calc R B 1 C14B C 0.1699(3) 0.4567(3) 0.1453(3) 0.0494(15) Uani 1 1 d . B 1 H14D H 0.2257 0.4473 0.176 0.074 Uiso 1 1 calc R B 1 H14E H 0.1581 0.501 0.1531 0.074 Uiso 1 1 calc R B 1 H14F H 0.1601 0.4507 0.0942 0.074 Uiso 1 1 calc R B 1 C15B C -0.1554(3) 0.3438(2) -0.0251(3) 0.0327(12) Uani 1 1 d . B 1 H15B H -0.1382 0.3002 -0.0042 0.039 Uiso 1 1 calc R B 1 C16B C -0.2435(3) 0.3508(3) -0.0410(3) 0.0489(15) Uani 1 1 d . B 1 H16D H -0.274 0.3177 -0.0756 0.073 Uiso 1 1 calc R B 1 H16E H -0.2622 0.3932 -0.0618 0.073 Uiso 1 1 calc R B 1 H16F H -0.2506 0.346 0.0042 0.073 Uiso 1 1 calc R B 1 C17B C -0.1473(3) 0.3469(3) -0.0976(3) 0.0464(14) Uani 1 1 d . B 1 H17D H -0.1824 0.3149 -0.131 0.07 Uiso 1 1 calc R B 1 H17E H -0.0922 0.338 -0.0894 0.07 Uiso 1 1 calc R B 1 H17F H -0.1623 0.3896 -0.1187 0.07 Uiso 1 1 calc R B 1 C18B C -0.0377(3) 0.1084(2) 0.0959(2) 0.0238(10) Uani 1 1 d . B 1 C19B C 0.0123(3) 0.0592(2) 0.1367(3) 0.0305(11) Uani 1 1 d . B 1 C20B C -0.0234(4) 0.0047(2) 0.1488(3) 0.0458(15) Uani 1 1 d . B 1 H20B H 0.009 -0.0298 0.1755 0.055 Uiso 1 1 calc R B 1 C21B C -0.1043(4) -0.0008(3) 0.1234(3) 0.0490(16) Uani 1 1 d . B 1 H21B H -0.1274 -0.0384 0.1327 0.059 Uiso 1 1 calc R B 1 C22B C -0.1519(3) 0.0486(3) 0.0843(3) 0.0427(14) Uani 1 1 d . B 1 H22B H -0.2079 0.0446 0.0672 0.051 Uiso 1 1 calc R B 1 C23B C -0.1207(3) 0.1038(2) 0.0695(3) 0.0293(11) Uani 1 1 d . B 1 C24B C 0.1020(3) 0.0633(2) 0.1689(3) 0.0362(12) Uani 1 1 d . B 1 H24B H 0.117 0.1046 0.1529 0.043 Uiso 1 1 calc R B 1 C25B C 0.1346(3) 0.0639(3) 0.2523(3) 0.0516(16) Uani 1 1 d . B 1 H25D H 0.1927 0.0669 0.2729 0.077 Uiso 1 1 calc R B 1 H25E H 0.1191 0.0243 0.2691 0.077 Uiso 1 1 calc R B 1 H25F H 0.113 0.1007 0.2681 0.077 Uiso 1 1 calc R B 1 C26B C 0.1402(4) 0.0087(3) 0.1441(3) 0.0544(16) Uani 1 1 d . B 1 H26D H 0.198 0.0137 0.1663 0.082 Uiso 1 1 calc R B 1 H26E H 0.121 0.0097 0.0911 0.082 Uiso 1 1 calc R B 1 H26F H 0.126 -0.0323 0.1591 0.082 Uiso 1 1 calc R B 1 C27B C -0.1743(3) 0.1573(2) 0.0245(3) 0.0350(12) Uani 1 1 d . B 1 H27B H -0.1462 0.1986 0.0434 0.042 Uiso 1 1 calc R B 1 C28B C -0.1880(3) 0.1520(3) -0.0559(3) 0.0491(15) Uani 1 1 d . B 1 H28D H -0.2224 0.1871 -0.0835 0.074 Uiso 1 1 calc R B 1 H28E H -0.2135 0.111 -0.0756 0.074 Uiso 1 1 calc R B 1 H28F H -0.137 0.1545 -0.0598 0.074 Uiso 1 1 calc R B 1 C29B C -0.2547(3) 0.1608(3) 0.0292(3) 0.0530(16) Uani 1 1 d . B 1 H29D H -0.2856 0.1964 -0.0006 0.08 Uiso 1 1 calc R B 1 H29E H -0.2464 0.1676 0.0798 0.08 Uiso 1 1 calc R B 1 H29F H -0.2835 0.1206 0.0115 0.08 Uiso 1 1 calc R B 1 C30B C -0.0993(3) 0.3423(3) 0.2751(3) 0.0479(15) Uani 1 1 d . B 1 H30B H -0.0724 0.3665 0.3181 0.057 Uiso 1 1 calc R B 1 C31B C -0.0963(3) 0.3540(3) 0.2076(3) 0.0473(15) Uani 1 1 d . B 1 H31B H -0.0667 0.3865 0.1971 0.057 Uiso 1 1 calc R B 1 C32B C -0.1461(3) 0.3075(3) 0.1581(3) 0.0510(16) Uani 1 1 d . B 1 H32B H -0.1558 0.3039 0.1083 0.061 Uiso 1 1 calc R B 1 C33B C -0.1779(3) 0.2687(3) 0.1950(3) 0.0463(15) Uani 1 1 d . B 1 H33B H -0.2135 0.2341 0.1747 0.056 Uiso 1 1 calc R B 1 C34B C -0.1480(3) 0.2896(3) 0.2688(3) 0.0432(14) Uani 1 1 d . B 1 H34B H -0.1592 0.271 0.3065 0.052 Uiso 1 1 calc R B 1 C35B C -0.0520(4) 0.1790(3) 0.2559(3) 0.0481(15) Uani 1 1 d . B 1 C36B C 0.0405(3) 0.2736(3) 0.3139(3) 0.0472(15) Uani 1 1 d . B 1 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 In 0.01803(16) 0.02057(18) 0.01799(16) -0.00073(13) 0.00747(13) -0.00112(13) Fe 0.0256(4) 0.0265(4) 0.0240(4) -0.0053(3) 0.0137(3) -0.0047(3) I 0.02130(17) 0.0380(2) 0.0372(2) 0.00170(15) -0.00069(15) -0.00116(14) O1 0.111(4) 0.031(2) 0.085(3) 0.009(2) 0.067(3) -0.004(2) O2 0.032(2) 0.088(3) 0.037(2) -0.007(2) 0.011(2) -0.002(2) N1 0.023(2) 0.018(2) 0.023(2) 0.0040(16) 0.0108(17) 0.0022(15) N2 0.023(2) 0.018(2) 0.019(2) 0.0006(15) 0.0063(17) -0.0002(15) C1 0.019(2) 0.029(3) 0.025(3) 0.004(2) 0.012(2) 0.0015(19) C2 0.026(3) 0.028(3) 0.028(3) 0.001(2) 0.016(2) 0.003(2) C3 0.018(2) 0.030(3) 0.017(2) -0.0008(19) 0.007(2) 0.0047(19) C4 0.049(3) 0.037(3) 0.043(3) 0.006(2) 0.030(3) -0.001(3) C5 0.039(3) 0.035(3) 0.034(3) -0.003(2) 0.023(3) 0.004(2) C6 0.032(3) 0.022(3) 0.025(3) 0.005(2) 0.017(2) 0.000(2) C7 0.031(3) 0.023(3) 0.031(3) 0.004(2) 0.011(2) -0.004(2) C8 0.044(3) 0.024(3) 0.035(3) -0.001(2) 0.013(3) -0.003(2) C9 0.054(4) 0.019(3) 0.050(4) 0.003(2) 0.027(3) 0.006(2) C10 0.036(3) 0.028(3) 0.044(3) 0.014(2) 0.020(3) 0.012(2) C11 0.024(3) 0.029(3) 0.031(3) 0.009(2) 0.013(2) 0.003(2) C12 0.032(3) 0.024(3) 0.039(3) 0.000(2) 0.012(3) -0.007(2) C13 0.038(3) 0.035(3) 0.048(4) -0.001(3) 0.009(3) -0.008(2) C14 0.037(3) 0.049(4) 0.059(4) 0.009(3) 0.023(3) -0.008(3) C15 0.026(3) 0.031(3) 0.036(3) 0.003(2) 0.006(2) 0.001(2) C16 0.024(3) 0.057(4) 0.074(5) 0.011(3) 0.011(3) 0.003(3) C17 0.037(3) 0.058(4) 0.035(3) -0.004(3) 0.005(3) 0.002(3) C18 0.032(3) 0.023(3) 0.024(3) -0.008(2) 0.016(2) -0.008(2) C19 0.045(3) 0.021(3) 0.035(3) -0.005(2) 0.018(3) -0.002(2) C20 0.064(4) 0.026(3) 0.046(4) -0.001(2) 0.022(3) -0.008(3) C21 0.074(5) 0.038(4) 0.052(4) -0.010(3) 0.035(4) -0.024(3) C22 0.042(4) 0.062(4) 0.044(4) -0.024(3) 0.021(3) -0.026(3) C23 0.032(3) 0.037(3) 0.030(3) -0.011(2) 0.018(2) -0.011(2) C24 0.039(3) 0.031(3) 0.038(3) 0.009(2) 0.007(3) 0.006(2) C25 0.069(5) 0.044(4) 0.046(4) 0.012(3) 0.005(3) -0.001(3) C26 0.057(4) 0.038(4) 0.071(5) 0.014(3) 0.016(4) 0.014(3) C27 0.020(3) 0.051(3) 0.039(3) -0.014(3) 0.009(2) -0.008(2) C28 0.041(4) 0.092(5) 0.033(3) 0.005(3) 0.000(3) 0.023(3) C29 0.023(3) 0.074(5) 0.075(5) -0.031(4) 0.006(3) -0.010(3) C30 0.059(4) 0.023(3) 0.038(3) -0.008(2) 0.018(3) 0.000(3) C31 0.047(4) 0.045(3) 0.047(4) -0.031(3) 0.032(3) -0.027(3) C32 0.038(3) 0.055(4) 0.028(3) -0.016(3) 0.005(3) 0.002(3) C33 0.068(4) 0.042(3) 0.027(3) -0.013(3) 0.029(3) -0.010(3) C34 0.040(3) 0.038(3) 0.053(4) -0.024(3) 0.031(3) -0.010(3) C35 0.049(4) 0.038(3) 0.035(3) -0.005(2) 0.028(3) -0.004(3) C36 0.026(3) 0.040(3) 0.038(3) -0.009(2) 0.022(3) -0.002(2) In1B 0.02195(17) 0.02041(18) 0.01886(17) 0.00031(13) 0.00934(14) -0.00108(13) Fe1B 0.0359(4) 0.0317(4) 0.0299(4) 0.0008(3) 0.0207(3) -0.0002(3) I1B 0.02163(17) 0.0367(2) 0.03249(19) 0.00419(14) 0.00036(14) -0.00100(13) O1B 0.122(4) 0.041(3) 0.093(4) 0.015(3) 0.068(3) 0.004(3) O2B 0.044(3) 0.137(4) 0.027(2) -0.012(3) 0.005(2) -0.006(3) N1B 0.020(2) 0.018(2) 0.018(2) 0.0008(15) 0.0077(17) -0.0006(15) N2B 0.0176(19) 0.020(2) 0.019(2) 0.0013(15) 0.0048(17) 0.0008(15) C1B 0.012(2) 0.027(3) 0.019(2) 0.0017(19) 0.0024(19) -0.0001(18) C2B 0.018(2) 0.032(3) 0.017(2) -0.001(2) 0.0061(19) -0.0009(19) C3B 0.014(2) 0.027(3) 0.026(3) 0.000(2) 0.005(2) 0.0062(19) C4B 0.035(3) 0.032(3) 0.031(3) 0.004(2) 0.018(2) -0.003(2) C5B 0.038(3) 0.031(3) 0.031(3) -0.003(2) 0.018(3) 0.004(2) C6B 0.028(3) 0.019(2) 0.024(3) 0.0068(19) 0.015(2) 0.0024(19) C7B 0.026(3) 0.023(3) 0.022(3) 0.001(2) 0.007(2) -0.004(2) C8B 0.046(3) 0.018(3) 0.031(3) -0.001(2) 0.012(3) 0.000(2) C9B 0.041(3) 0.026(3) 0.037(3) 0.008(2) 0.014(3) 0.013(2) C10B 0.034(3) 0.030(3) 0.039(3) 0.011(2) 0.014(3) 0.010(2) C11B 0.021(2) 0.024(3) 0.023(3) 0.005(2) 0.008(2) -0.0001(19) C12B 0.028(3) 0.028(3) 0.028(3) -0.002(2) 0.004(2) -0.005(2) C13B 0.044(3) 0.042(3) 0.028(3) -0.006(2) 0.002(3) -0.004(3) C14B 0.038(3) 0.048(4) 0.056(4) 0.003(3) 0.013(3) -0.013(3) C15B 0.027(3) 0.031(3) 0.029(3) 0.006(2) 0.000(2) 0.006(2) C16B 0.024(3) 0.064(4) 0.050(4) -0.001(3) 0.006(3) -0.004(3) C17B 0.033(3) 0.059(4) 0.033(3) -0.008(3) -0.002(3) 0.001(3) C18B 0.026(3) 0.022(3) 0.020(3) -0.0050(19) 0.007(2) -0.005(2) C19B 0.041(3) 0.022(3) 0.026(3) 0.002(2) 0.011(2) 0.001(2) C20B 0.067(4) 0.025(3) 0.036(3) 0.005(2) 0.012(3) -0.006(3) C21B 0.069(4) 0.034(3) 0.045(4) -0.003(3) 0.024(3) -0.025(3) C22B 0.043(3) 0.040(3) 0.050(4) -0.013(3) 0.024(3) -0.020(3) C23B 0.030(3) 0.027(3) 0.031(3) -0.007(2) 0.013(2) -0.009(2) C24B 0.036(3) 0.028(3) 0.033(3) 0.005(2) 0.002(3) 0.005(2) C25B 0.056(4) 0.036(3) 0.045(4) 0.009(3) 0.004(3) 0.007(3) C26B 0.056(4) 0.035(3) 0.063(4) 0.003(3) 0.015(3) 0.015(3) C27B 0.021(3) 0.037(3) 0.041(3) -0.005(2) 0.006(2) -0.004(2) C28B 0.032(3) 0.068(4) 0.040(4) 0.011(3) 0.008(3) 0.009(3) C29B 0.022(3) 0.078(5) 0.056(4) -0.015(3) 0.014(3) -0.002(3) C30B 0.050(4) 0.045(4) 0.055(4) -0.017(3) 0.028(3) 0.002(3) C31B 0.052(4) 0.037(3) 0.067(4) 0.010(3) 0.039(4) 0.013(3) C32B 0.044(4) 0.074(5) 0.039(3) 0.008(3) 0.021(3) 0.027(3) C33B 0.025(3) 0.056(4) 0.057(4) -0.015(3) 0.016(3) -0.004(3) C34B 0.042(3) 0.050(4) 0.048(4) -0.003(3) 0.030(3) 0.001(3) C35B 0.065(4) 0.044(4) 0.048(4) 0.003(3) 0.036(3) 0.000(3) C36B 0.040(3) 0.079(4) 0.030(3) -0.005(3) 0.022(3) 0.002(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 In N2 2.165(3) . ? In N1 2.190(3) . ? In Fe 2.5118(7) . ? In I 2.8100(4) . ? Fe C36 1.751(5) . ? Fe C35 1.759(6) . ? Fe C32 2.078(5) . ? Fe C33 2.087(5) . ? Fe C34 2.088(5) . ? Fe C30 2.089(5) . ? Fe C31 2.091(5) . ? O1 C35 1.150(6) . ? O2 C36 1.157(6) . ? N1 C1 1.319(5) . ? N1 C6 1.442(5) . ? N2 C3 1.341(5) . ? N2 C18 1.446(5) . ? C1 C2 1.400(6) . ? C1 C4 1.515(6) . ? C2 C3 1.388(6) . ? C3 C5 1.511(6) . ? C6 C7 1.409(6) . ? C6 C11 1.428(6) . ? C7 C8 1.386(6) . ? C7 C12 1.534(7) . ? C8 C9 1.379(7) . ? C9 C10 1.370(7) . ? C10 C11 1.388(7) . ? C11 C15 1.512(6) . ? C12 C13 1.528(7) . ? C12 C14 1.537(6) . ? C15 C17 1.535(7) . ? C15 C16 1.536(7) . ? C18 C19 1.400(7) . ? C18 C23 1.418(6) . ? C19 C20 1.398(7) . ? C19 C24 1.522(7) . ? C20 C21 1.371(8) . ? C21 C22 1.376(8) . ? C22 C23 1.379(7) . ? C23 C27 1.510(7) . ? C24 C25 1.531(7) . ? C24 C26 1.537(7) . ? C27 C29 1.531(7) . ? C27 C28 1.544(7) . ? C30 C31 1.409(7) . ? C30 C34 1.412(7) . ? C31 C32 1.396(7) . ? C32 C33 1.415(7) . ? C33 C34 1.389(7) . ? In1B N1B 2.176(3) . ? In1B N2B 2.181(3) . ? In1B Fe1B 2.5200(7) . ? In1B I1B 2.7870(4) . ? Fe1B C35B 1.751(6) . ? Fe1B C36B 1.759(6) . ? Fe1B C34B 2.086(5) . ? Fe1B C32B 2.088(5) . ? Fe1B C31B 2.089(5) . ? Fe1B C33B 2.092(5) . ? Fe1B C30B 2.092(5) . ? O1B C35B 1.140(6) . ? O2B C36B 1.157(6) . ? N1B C1B 1.339(5) . ? N1B C6B 1.448(5) . ? N2B C3B 1.336(5) . ? N2B C18B 1.452(5) . ? C1B C2B 1.398(6) . ? C1B C4B 1.512(6) . ? C2B C3B 1.405(6) . ? C3B C5B 1.507(6) . ? C6B C7B 1.405(6) . ? C6B C11B 1.416(6) . ? C7B C8B 1.394(6) . ? C7B C12B 1.521(6) . ? C8B C9B 1.377(7) . ? C9B C10B 1.371(7) . ? C10B C11B 1.384(6) . ? C11B C15B 1.507(6) . ? C12B C13B 1.523(6) . ? C12B C14B 1.538(6) . ? C15B C16B 1.531(7) . ? C15B C17B 1.534(7) . ? C18B C19B 1.401(6) . ? C18B C23B 1.406(6) . ? C19B C20B 1.389(7) . ? C19B C24B 1.513(7) . ? C20B C21B 1.371(8) . ? C21B C22B 1.375(8) . ? C22B C23B 1.376(7) . ? C23B C27B 1.522(7) . ? C24B C26B 1.531(7) . ? C24B C25B 1.539(7) . ? C27B C29B 1.530(6) . ? C27B C28B 1.543(7) . ? C30B C34B 1.396(7) . ? C30B C31B 1.409(8) . ? C31B C32B 1.426(8) . ? C32B C33B 1.387(8) . ? C33B C34B 1.429(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 In N1 89.90(13) . . ? N2 In Fe 129.34(9) . . ? N1 In Fe 122.93(9) . . ? N2 In I 99.49(9) . . ? N1 In I 99.38(9) . . ? Fe In I 110.08(2) . . ? C36 Fe C35 94.7(2) . . ? C36 Fe C32 159.6(2) . . ? C35 Fe C32 102.7(2) . . ? C36 Fe C33 128.6(2) . . ? C35 Fe C33 95.9(2) . . ? C32 Fe C33 39.7(2) . . ? C36 Fe C34 95.5(2) . . ? C35 Fe C34 123.0(2) . . ? C32 Fe C34 66.1(2) . . ? C33 Fe C34 38.9(2) . . ? C36 Fe C30 94.3(2) . . ? C35 Fe C30 161.3(2) . . ? C32 Fe C30 66.1(2) . . ? C33 Fe C30 65.8(2) . . ? C34 Fe C30 39.53(19) . . ? C36 Fe C31 126.6(2) . . ? C35 Fe C31 138.0(2) . . ? C32 Fe C31 39.1(2) . . ? C33 Fe C31 65.8(2) . . ? C34 Fe C31 66.0(2) . . ? C30 Fe C31 39.4(2) . . ? C36 Fe In 93.59(14) . . ? C35 Fe In 87.64(15) . . ? C32 Fe In 97.61(15) . . ? C33 Fe In 136.95(16) . . ? C34 Fe In 146.95(14) . . ? C30 Fe In 108.15(15) . . ? C31 Fe In 83.11(14) . . ? C1 N1 C6 122.5(4) . . ? C1 N1 In 120.3(3) . . ? C6 N1 In 117.0(3) . . ? C3 N2 C18 120.1(4) . . ? C3 N2 In 120.2(3) . . ? C18 N2 In 119.4(3) . . ? N1 C1 C2 125.3(4) . . ? N1 C1 C4 119.3(4) . . ? C2 C1 C4 115.4(4) . . ? C3 C2 C1 131.9(4) . . ? N2 C3 C2 125.1(4) . . ? N2 C3 C5 119.0(4) . . ? C2 C3 C5 115.9(4) . . ? C7 C6 C11 120.9(4) . . ? C7 C6 N1 120.8(4) . . ? C11 C6 N1 118.1(4) . . ? C8 C7 C6 118.2(4) . . ? C8 C7 C12 118.3(4) . . ? C6 C7 C12 123.5(4) . . ? C9 C8 C7 121.4(5) . . ? C10 C9 C8 120.0(5) . . ? C9 C10 C11 122.2(5) . . ? C10 C11 C6 117.1(4) . . ? C10 C11 C15 122.2(4) . . ? C6 C11 C15 120.7(4) . . ? C13 C12 C7 111.7(4) . . ? C13 C12 C14 108.6(4) . . ? C7 C12 C14 110.9(4) . . ? C11 C15 C17 111.8(4) . . ? C11 C15 C16 112.9(4) . . ? C17 C15 C16 108.7(4) . . ? C19 C18 C23 120.8(4) . . ? C19 C18 N2 121.2(4) . . ? C23 C18 N2 117.9(4) . . ? C20 C19 C18 118.2(5) . . ? C20 C19 C24 118.4(5) . . ? C18 C19 C24 123.4(4) . . ? C21 C20 C19 121.2(5) . . ? C20 C21 C22 120.0(5) . . ? C21 C22 C23 121.8(5) . . ? C22 C23 C18 118.0(5) . . ? C22 C23 C27 121.2(5) . . ? C18 C23 C27 120.8(4) . . ? C19 C24 C25 110.5(5) . . ? C19 C24 C26 112.2(4) . . ? C25 C24 C26 109.9(4) . . ? C23 C27 C29 114.2(5) . . ? C23 C27 C28 111.8(4) . . ? C29 C27 C28 108.6(4) . . ? C31 C30 C34 107.7(5) . . ? C31 C30 Fe 70.4(3) . . ? C34 C30 Fe 70.2(3) . . ? C32 C31 C30 108.2(5) . . ? C32 C31 Fe 69.9(3) . . ? C30 C31 Fe 70.2(3) . . ? C31 C32 C33 107.8(5) . . ? C31 C32 Fe 70.9(3) . . ? C33 C32 Fe 70.5(3) . . ? C34 C33 C32 108.3(5) . . ? C34 C33 Fe 70.6(3) . . ? C32 C33 Fe 69.8(3) . . ? C33 C34 C30 108.1(5) . . ? C33 C34 Fe 70.5(3) . . ? C30 C34 Fe 70.3(3) . . ? O1 C35 Fe 176.4(4) . . ? O2 C36 Fe 174.4(4) . . ? N1B In1B N2B 88.14(13) . . ? N1B In1B Fe1B 123.90(9) . . ? N2B In1B Fe1B 125.52(9) . . ? N1B In1B I1B 99.52(9) . . ? N2B In1B I1B 97.07(9) . . ? Fe1B In1B I1B 116.00(2) . . ? C35B Fe1B C36B 93.7(3) . . ? C35B Fe1B C34B 102.0(2) . . ? C36B Fe1B C34B 114.3(2) . . ? C35B Fe1B C32B 122.2(3) . . ? C36B Fe1B C32B 143.7(3) . . ? C34B Fe1B C32B 66.4(2) . . ? C35B Fe1B C31B 160.8(3) . . ? C36B Fe1B C31B 105.0(3) . . ? C34B Fe1B C31B 66.4(2) . . ? C32B Fe1B C31B 39.9(2) . . ? C35B Fe1B C33B 95.0(3) . . ? C36B Fe1B C33B 154.2(2) . . ? C34B Fe1B C33B 40.0(2) . . ? C32B Fe1B C33B 38.7(2) . . ? C31B Fe1B C33B 66.1(2) . . ? C35B Fe1B C30B 137.6(2) . . ? C36B Fe1B C30B 91.7(3) . . ? C34B Fe1B C30B 39.0(2) . . ? C32B Fe1B C30B 66.0(2) . . ? C31B Fe1B C30B 39.4(2) . . ? C33B Fe1B C30B 65.8(2) . . ? C35B Fe1B In1B 89.08(17) . . ? C36B Fe1B In1B 87.00(16) . . ? C34B Fe1B In1B 154.87(16) . . ? C32B Fe1B In1B 88.61(15) . . ? C31B Fe1B In1B 96.23(15) . . ? C33B Fe1B In1B 117.34(16) . . ? C30B Fe1B In1B 133.26(16) . . ? C1B N1B C6B 120.9(3) . . ? C1B N1B In1B 117.3(3) . . ? C6B N1B In1B 120.9(3) . . ? C3B N2B C18B 120.7(4) . . ? C3B N2B In1B 119.3(3) . . ? C18B N2B In1B 119.3(3) . . ? N1B C1B C2B 124.5(4) . . ? N1B C1B C4B 119.4(4) . . ? C2B C1B C4B 116.1(4) . . ? C1B C2B C3B 131.3(4) . . ? N2B C3B C2B 123.6(4) . . ? N2B C3B C5B 120.3(4) . . ? C2B C3B C5B 116.1(4) . . ? C7B C6B C11B 120.7(4) . . ? C7B C6B N1B 120.8(4) . . ? C11B C6B N1B 118.4(4) . . ? C8B C7B C6B 118.4(4) . . ? C8B C7B C12B 119.1(4) . . ? C6B C7B C12B 122.5(4) . . ? C9B C8B C7B 121.1(5) . . ? C10B C9B C8B 119.8(5) . . ? C9B C10B C11B 122.1(5) . . ? C10B C11B C6B 117.8(4) . . ? C10B C11B C15B 121.0(4) . . ? C6B C11B C15B 121.2(4) . . ? C7B C12B C13B 111.6(4) . . ? C7B C12B C14B 111.4(4) . . ? C13B C12B C14B 110.3(4) . . ? C11B C15B C16B 114.4(4) . . ? C11B C15B C17B 111.4(4) . . ? C16B C15B C17B 107.9(4) . . ? C19B C18B C23B 121.8(4) . . ? C19B C18B N2B 120.8(4) . . ? C23B C18B N2B 117.4(4) . . ? C20B C19B C18B 117.3(5) . . ? C20B C19B C24B 119.2(5) . . ? C18B C19B C24B 123.5(4) . . ? C21B C20B C19B 121.8(5) . . ? C20B C21B C22B 119.6(5) . . ? C21B C22B C23B 121.8(5) . . ? C22B C23B C18B 117.7(5) . . ? C22B C23B C27B 121.2(5) . . ? C18B C23B C27B 121.1(4) . . ? C19B C24B C26B 112.8(4) . . ? C19B C24B C25B 109.8(4) . . ? C26B C24B C25B 109.7(4) . . ? C23B C27B C29B 114.1(4) . . ? C23B C27B C28B 111.2(4) . . ? C29B C27B C28B 109.0(4) . . ? C34B C30B C31B 109.2(5) . . ? C34B C30B Fe1B 70.3(3) . . ? C31B C30B Fe1B 70.2(3) . . ? C30B C31B C32B 106.9(5) . . ? C30B C31B Fe1B 70.4(3) . . ? C32B C31B Fe1B 70.0(3) . . ? C33B C32B C31B 108.3(5) . . ? C33B C32B Fe1B 70.8(3) . . ? C31B C32B Fe1B 70.1(3) . . ? C32B C33B C34B 108.4(5) . . ? C32B C33B Fe1B 70.5(3) . . ? C34B C33B Fe1B 69.8(3) . . ? C30B C34B C33B 107.1(5) . . ? C30B C34B Fe1B 70.7(3) . . ? C33B C34B Fe1B 70.2(3) . . ? O1B C35B Fe1B 176.0(5) . . ? O2B C36B Fe1B 176.5(5) . . ? #===END data_(2)-mar1805 _database_code_depnum_ccdc_archive 'CCDC 675701' _audit_creation_date 2005-03-18T15:43:47-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H34 Fe I In N2 O2' _chemical_formula_sum 'C30 H34 Fe I In N2 O2' _chemical_formula_weight 752.16 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3068(3) _cell_length_b 9.7660(3) _cell_length_c 17.5106(5) _cell_angle_alpha 77.283(2) _cell_angle_beta 76.552(2) _cell_angle_gamma 83.664(2) _cell_volume 1506.99(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 16886 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.299 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.5851 _exptl_absorpt_correction_T_max 0.6877 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.976429E-1 _diffrn_orient_matrix_ub_12 0.445339E-1 _diffrn_orient_matrix_ub_13 0.233124E-1 _diffrn_orient_matrix_ub_21 0.521013E-1 _diffrn_orient_matrix_ub_22 0.668487E-1 _diffrn_orient_matrix_ub_23 0.183861E-1 _diffrn_orient_matrix_ub_31 0.20559E-2 _diffrn_orient_matrix_ub_32 0.678965E-1 _diffrn_orient_matrix_ub_33 -0.520745E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_unetI/netI 0.038 _diffrn_reflns_number 20676 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 26.16 _diffrn_reflns_theta_full 26.16 _diffrn_measured_fraction_theta_full 0.959 _diffrn_measured_fraction_theta_max 0.959 _reflns_number_total 5783 _reflns_number_gt 5118 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0134P)^2^+1.9791P] 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_number_reflns 5783 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0602 _refine_ls_wR_factor_gt 0.0577 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.733 _refine_diff_density_min -0.923 _refine_diff_density_rms 0.081 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.31 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Fe Fe 0.29346(4) 0.07827(5) 0.33457(3) 0.02738(11) Uani 1 1 d . . . In In 0.47353(2) 0.26802(2) 0.284845(12) 0.02375(6) Uani 1 1 d . A 1 I I 0.64315(3) 0.27211(3) 0.396178(14) 0.04466(8) Uani 1 1 d . A 1 O1 O 0.5562(3) -0.1089(3) 0.3397(2) 0.0737(10) Uani 1 1 d . A 1 O2 O 0.2814(3) 0.0669(3) 0.17233(16) 0.0624(8) Uani 1 1 d . A 1 N1 N 0.4075(3) 0.4895(2) 0.25230(14) 0.0259(5) Uani 1 1 d . A 1 N2 N 0.6411(2) 0.2902(3) 0.17438(14) 0.0261(5) Uani 1 1 d . A 1 C1 C 0.5037(3) 0.5804(3) 0.20634(17) 0.0296(7) Uani 1 1 d . A 1 C2 C 0.6457(3) 0.5418(3) 0.16427(18) 0.0327(7) Uani 1 1 d . A 1 H2 H 0.713 0.6144 0.1475 0.039 Uiso 1 1 calc R A 1 C3 C 0.7023(3) 0.4139(3) 0.14359(18) 0.0300(7) Uani 1 1 d . A 1 C4 C 0.4577(4) 0.7363(3) 0.1939(2) 0.0423(8) Uani 1 1 d . A 1 H4A H 0.3859 0.7578 0.1592 0.063 Uiso 1 1 calc R A 1 H4B H 0.5449 0.7906 0.1686 0.063 Uiso 1 1 calc R A 1 H4C H 0.4124 0.7613 0.2458 0.063 Uiso 1 1 calc R A 1 C5 C 0.8426(3) 0.4176(4) 0.0781(2) 0.0422(8) Uani 1 1 d . A 1 H5A H 0.9154 0.3444 0.0958 0.063 Uiso 1 1 calc R A 1 H5B H 0.8837 0.5099 0.0669 0.063 Uiso 1 1 calc R A 1 H5C H 0.8191 0.401 0.0293 0.063 Uiso 1 1 calc R A 1 C6 C 0.2575(3) 0.5380(3) 0.28444(18) 0.0280(6) Uani 1 1 d . A 1 C7 C 0.2226(4) 0.5798(3) 0.35795(19) 0.0328(7) Uani 1 1 d . A 1 C8 C 0.0754(4) 0.6180(3) 0.3886(2) 0.0419(8) Uani 1 1 d . A 1 H8 H 0.0501 0.6465 0.4388 0.05 Uiso 1 1 calc R A 1 C9 C -0.0347(4) 0.6157(4) 0.3483(2) 0.0470(9) Uani 1 1 d . A 1 C10 C 0.0031(4) 0.5741(4) 0.2752(2) 0.0465(9) Uani 1 1 d . A 1 H10 H -0.0723 0.5722 0.247 0.056 Uiso 1 1 calc R A 1 C11 C 0.1492(4) 0.5346(4) 0.2418(2) 0.0367(8) Uani 1 1 d . A 1 C12 C 0.3389(4) 0.5839(4) 0.4041(2) 0.0434(8) Uani 1 1 d . A 1 H12A H 0.3846 0.489 0.4181 0.065 Uiso 1 1 calc R A 1 H12B H 0.2931 0.6184 0.4533 0.065 Uiso 1 1 calc R A 1 H12C H 0.4147 0.6469 0.3712 0.065 Uiso 1 1 calc R A 1 C13 C -0.1951(4) 0.6587(5) 0.3824(3) 0.0713(14) Uani 1 1 d . A 1 H13A H -0.2567 0.6503 0.3454 0.107 Uiso 0.5 1 calc PR A 1 H13B H -0.2023 0.7563 0.3892 0.107 Uiso 0.5 1 calc PR A 1 H13C H -0.2295 0.5971 0.4344 0.107 Uiso 0.5 1 calc PR A 1 H13D H -0.2023 0.6855 0.434 0.107 Uiso 0.5 1 calc PR A 1 H13E H -0.2567 0.5795 0.3902 0.107 Uiso 0.5 1 calc PR A 1 H13F H -0.2295 0.7387 0.345 0.107 Uiso 0.5 1 calc PR A 1 C14 C 0.1873(4) 0.4889(5) 0.1626(2) 0.0552(11) Uani 1 1 d . A 1 H14A H 0.0999 0.5042 0.1388 0.083 Uiso 1 1 calc R A 1 H14B H 0.2196 0.3888 0.1708 0.083 Uiso 1 1 calc R A 1 H14C H 0.2672 0.5438 0.1265 0.083 Uiso 1 1 calc R A 1 C15 C 0.6913(3) 0.1748(3) 0.13386(17) 0.0268(6) Uani 1 1 d . A 1 C16 C 0.7937(3) 0.0701(3) 0.16030(18) 0.0315(7) Uani 1 1 d . A 1 C17 C 0.8401(3) -0.0381(3) 0.11823(19) 0.0352(7) Uani 1 1 d . A 1 H17 H 0.9088 -0.11 0.1366 0.042 Uiso 1 1 calc R A 1 C18 C 0.7902(3) -0.0449(3) 0.05068(19) 0.0327(7) Uani 1 1 d . A 1 C19 C 0.6866(3) 0.0600(4) 0.02651(18) 0.0347(7) Uani 1 1 d . A 1 H19 H 0.6497 0.0569 -0.0193 0.042 Uiso 1 1 calc R A 1 C20 C 0.6357(3) 0.1683(3) 0.06671(17) 0.0287(7) Uani 1 1 d . A 1 C21 C 0.8609(4) 0.0753(4) 0.2301(2) 0.0426(8) Uani 1 1 d . A 1 H21A H 0.9409 0.0015 0.2339 0.064 Uiso 1 1 calc R A 1 H21B H 0.7847 0.0602 0.2798 0.064 Uiso 1 1 calc R A 1 H21C H 0.9008 0.1674 0.222 0.064 Uiso 1 1 calc R A 1 C22 C 0.8490(4) -0.1589(4) 0.0040(2) 0.0431(8) Uani 1 1 d . A 1 H22A H 0.801 -0.1465 -0.0416 0.065 Uiso 0.5 1 calc PR A 1 H22B H 0.828 -0.251 0.0388 0.065 Uiso 0.5 1 calc PR A 1 H22C H 0.9561 -0.1535 -0.0158 0.065 Uiso 0.5 1 calc PR A 1 H22D H 0.9225 -0.2208 0.0292 0.065 Uiso 0.5 1 calc PR A 1 H22E H 0.8954 -0.1164 -0.0512 0.065 Uiso 0.5 1 calc PR A 1 H22F H 0.7673 -0.2138 0.0034 0.065 Uiso 0.5 1 calc PR A 1 C23 C 0.5251(4) 0.2812(4) 0.03767(19) 0.0408(8) Uani 1 1 d . A 1 H23A H 0.4978 0.2601 -0.0091 0.061 Uiso 1 1 calc R A 1 H23B H 0.5692 0.3725 0.0227 0.061 Uiso 1 1 calc R A 1 H23C H 0.4366 0.2843 0.0805 0.061 Uiso 1 1 calc R A 1 C24 C 0.4535(4) -0.0326(4) 0.3362(2) 0.0417(8) Uani 1 1 d . A 1 C25 C 0.2888(4) 0.0740(4) 0.2363(2) 0.0403(8) Uani 1 1 d . A 1 C26 C 0.1673(3) -0.0320(4) 0.44038(19) 0.0361(8) Uani 1 1 d . A 1 H26 H 0.1831 -0.1293 0.4618 0.043 Uiso 1 1 calc R A 1 C27 C 0.2322(4) 0.0790(4) 0.45729(19) 0.0389(8) Uani 1 1 d . A 1 H27 H 0.2999 0.0701 0.4914 0.047 Uiso 1 1 calc R A 1 C28 C 0.1775(4) 0.2055(4) 0.4139(2) 0.0478(10) Uani 1 1 d . A 1 H28 H 0.2011 0.2975 0.4143 0.057 Uiso 1 1 calc R A 1 C29 C 0.0823(4) 0.1721(4) 0.3700(2) 0.0502(10) Uani 1 1 d . A 1 H29 H 0.0314 0.2374 0.3351 0.06 Uiso 1 1 calc R A 1 C30 C 0.0757(3) 0.0255(4) 0.3868(2) 0.0434(9) Uani 1 1 d . A 1 H30 H 0.0189 -0.0258 0.3655 0.052 Uiso 1 1 calc R A 1 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 Fe 0.0231(2) 0.0270(2) 0.0294(2) -0.00146(18) -0.00400(17) -0.00239(17) In 0.02297(11) 0.02442(11) 0.02244(11) -0.00321(8) -0.00330(8) -0.00192(8) I 0.05076(14) 0.05090(16) 0.04021(14) -0.01322(11) -0.02632(11) 0.00698(11) O1 0.0391(15) 0.0405(16) 0.134(3) -0.0065(17) -0.0201(17) 0.0116(13) O2 0.0714(19) 0.082(2) 0.0393(16) -0.0158(15) -0.0135(13) -0.0190(16) N1 0.0267(12) 0.0245(13) 0.0243(12) -0.0032(10) -0.0035(10) 0.0003(10) N2 0.0235(12) 0.0294(14) 0.0242(12) -0.0059(11) -0.0026(10) -0.0012(10) C1 0.0392(17) 0.0259(16) 0.0237(15) -0.0050(13) -0.0051(13) -0.0055(13) C2 0.0320(16) 0.0318(18) 0.0305(16) -0.0029(14) 0.0018(13) -0.0112(13) C3 0.0243(15) 0.0368(18) 0.0268(16) -0.0056(14) -0.0009(12) -0.0048(13) C4 0.055(2) 0.0272(18) 0.0367(19) -0.0035(15) 0.0043(16) -0.0040(15) C5 0.0322(17) 0.044(2) 0.045(2) -0.0122(17) 0.0081(15) -0.0089(15) C6 0.0311(15) 0.0202(15) 0.0293(16) -0.0017(13) -0.0048(12) 0.0018(12) C7 0.0414(18) 0.0187(15) 0.0335(17) -0.0044(13) -0.0016(14) 0.0026(13) C8 0.049(2) 0.0261(17) 0.042(2) -0.0094(15) 0.0076(16) 0.0009(15) C9 0.0365(19) 0.0264(18) 0.066(3) -0.0043(18) 0.0041(18) 0.0062(14) C10 0.0323(18) 0.041(2) 0.064(3) -0.0036(19) -0.0155(17) 0.0065(15) C11 0.0368(17) 0.0351(18) 0.0375(18) -0.0037(15) -0.0117(14) 0.0023(14) C12 0.059(2) 0.040(2) 0.0327(18) -0.0156(16) -0.0082(16) -0.0002(17) C13 0.041(2) 0.055(3) 0.102(4) -0.016(3) 0.010(2) 0.0108(19) C14 0.047(2) 0.079(3) 0.046(2) -0.018(2) -0.0245(18) 0.009(2) C15 0.0219(14) 0.0304(16) 0.0249(15) -0.0047(13) 0.0017(11) -0.0035(12) C16 0.0229(15) 0.0367(18) 0.0324(17) -0.0074(14) -0.0015(12) -0.0002(13) C17 0.0252(15) 0.0353(18) 0.0394(18) -0.0039(15) -0.0005(13) 0.0014(13) C18 0.0304(16) 0.0317(18) 0.0330(17) -0.0089(14) 0.0053(13) -0.0106(13) C19 0.0357(17) 0.0408(19) 0.0256(16) -0.0061(14) -0.0002(13) -0.0091(14) C20 0.0278(15) 0.0312(17) 0.0250(15) -0.0061(13) -0.0005(12) -0.0034(13) C21 0.0342(18) 0.053(2) 0.046(2) -0.0171(18) -0.0182(15) 0.0094(16) C22 0.048(2) 0.036(2) 0.041(2) -0.0128(16) 0.0059(16) -0.0054(16) C23 0.0418(19) 0.049(2) 0.0297(17) -0.0051(16) -0.0111(14) 0.0060(16) C24 0.0367(18) 0.0267(17) 0.060(2) -0.0040(16) -0.0108(16) -0.0032(15) C25 0.0360(18) 0.043(2) 0.043(2) -0.0065(17) -0.0071(15) -0.0108(15) C26 0.0360(17) 0.0347(18) 0.0311(17) 0.0019(14) -0.0005(14) -0.0064(14) C27 0.0405(18) 0.043(2) 0.0315(17) -0.0065(15) -0.0030(14) -0.0080(15) C28 0.051(2) 0.034(2) 0.044(2) -0.0078(17) 0.0202(17) -0.0032(16) C29 0.0270(17) 0.057(2) 0.046(2) 0.0115(19) 0.0050(15) 0.0115(16) C30 0.0269(16) 0.063(2) 0.0360(18) -0.0007(17) -0.0015(14) -0.0137(16) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Fe C25 1.742(4) . ? Fe C24 1.744(3) . ? Fe C26 2.088(3) . ? Fe C30 2.090(3) . ? Fe C29 2.091(3) . ? Fe C27 2.092(3) . ? Fe C28 2.098(4) . ? Fe In 2.5094(4) . ? In N2 2.169(2) . ? In N1 2.170(2) . ? In I 2.7882(3) . ? O1 C24 1.150(4) . ? O2 C25 1.155(4) . ? N1 C1 1.328(4) . ? N1 C6 1.448(4) . ? N2 C3 1.341(4) . ? N2 C15 1.439(4) . ? C1 C2 1.411(4) . ? C1 C4 1.518(4) . ? C2 C3 1.391(5) . ? C2 H2 0.95 . ? C3 C5 1.523(4) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 C7 1.392(4) . ? C6 C11 1.394(4) . ? C7 C8 1.392(5) . ? C7 C12 1.503(5) . ? C8 C9 1.377(5) . ? C8 H8 0.95 . ? C9 C10 1.385(5) . ? C9 C13 1.522(5) . ? C10 C11 1.398(5) . ? C10 H10 0.95 . ? C11 C14 1.502(5) . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C13 H13D 0.98 . ? C13 H13E 0.98 . ? C13 H13F 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C16 1.397(4) . ? C15 C20 1.406(4) . ? C16 C17 1.392(5) . ? C16 C21 1.510(4) . ? C17 C18 1.384(5) . ? C17 H17 0.95 . ? C18 C19 1.392(5) . ? C18 C22 1.506(5) . ? C19 C20 1.378(4) . ? C19 H19 0.95 . ? C20 C23 1.510(4) . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C22 H22D 0.98 . ? C22 H22E 0.98 . ? C22 H22F 0.98 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C26 C30 1.398(5) . ? C26 C27 1.413(5) . ? C26 H26 0.95 . ? C27 C28 1.411(5) . ? C27 H27 0.95 . ? C28 C29 1.405(6) . ? C28 H28 0.95 . ? C29 C30 1.402(5) . ? C29 H29 0.95 . ? C30 H30 0.95 . ? 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 C25 Fe C24 94.87(17) . . ? C25 Fe C26 128.01(14) . . ? C24 Fe C26 96.00(15) . . ? C25 Fe C30 97.33(14) . . ? C24 Fe C30 127.01(15) . . ? C26 Fe C30 39.10(12) . . ? C25 Fe C29 99.29(16) . . ? C24 Fe C29 161.39(15) . . ? C26 Fe C29 65.72(13) . . ? C30 Fe C29 39.18(15) . . ? C25 Fe C27 163.13(14) . . ? C24 Fe C27 97.82(16) . . ? C26 Fe C27 39.51(13) . . ? C30 Fe C27 66.10(14) . . ? C29 Fe C27 66.14(14) . . ? C25 Fe C28 132.34(16) . . ? C24 Fe C28 131.57(17) . . ? C26 Fe C28 65.72(13) . . ? C30 Fe C28 65.64(15) . . ? C29 Fe C28 39.18(16) . . ? C27 Fe C28 39.36(14) . . ? C25 Fe In 90.32(11) . . ? C24 Fe In 83.47(11) . . ? C26 Fe In 141.39(10) . . ? C30 Fe In 147.38(11) . . ? C29 Fe In 108.34(11) . . ? C27 Fe In 102.10(9) . . ? C28 Fe In 85.83(10) . . ? N2 In N1 88.89(9) . . ? N2 In Fe 125.44(7) . . ? N1 In Fe 123.49(6) . . ? N2 In I 101.29(6) . . ? N1 In I 101.29(6) . . ? Fe In I 111.639(13) . . ? C1 N1 C6 120.3(2) . . ? C1 N1 In 121.0(2) . . ? C6 N1 In 118.70(17) . . ? C3 N2 C15 118.8(2) . . ? C3 N2 In 119.3(2) . . ? C15 N2 In 121.96(17) . . ? N1 C1 C2 124.3(3) . . ? N1 C1 C4 118.9(3) . . ? C2 C1 C4 116.7(3) . . ? C3 C2 C1 130.0(3) . . ? C3 C2 H2 115 . . ? C1 C2 H2 115 . . ? N2 C3 C2 125.5(3) . . ? N2 C3 C5 118.0(3) . . ? C2 C3 C5 116.4(3) . . ? C7 C6 C11 121.5(3) . . ? C7 C6 N1 120.2(3) . . ? C11 C6 N1 118.2(3) . . ? C6 C7 C8 118.2(3) . . ? C6 C7 C12 121.8(3) . . ? C8 C7 C12 120.0(3) . . ? C9 C8 C7 121.9(3) . . ? C9 C8 H8 119 . . ? C7 C8 H8 119 . . ? C8 C9 C10 118.7(3) . . ? C8 C9 C13 121.3(4) . . ? C10 C9 C13 120.0(4) . . ? C9 C10 C11 121.7(3) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C6 C11 C10 118.0(3) . . ? C6 C11 C14 121.3(3) . . ? C10 C11 C14 120.7(3) . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C13 H13D 109.5 . . ? H13A C13 H13D 141.1 . . ? H13B C13 H13D 56.3 . . ? H13C C13 H13D 56.3 . . ? C9 C13 H13E 109.5 . . ? H13A C13 H13E 56.3 . . ? H13B C13 H13E 141.1 . . ? H13C C13 H13E 56.3 . . ? H13D C13 H13E 109.5 . . ? C9 C13 H13F 109.5 . . ? H13A C13 H13F 56.3 . . ? H13B C13 H13F 56.3 . . ? H13C C13 H13F 141.1 . . ? H13D C13 H13F 109.5 . . ? H13E C13 H13F 109.5 . . ? C16 C15 C20 119.9(3) . . ? C16 C15 N2 121.0(3) . . ? C20 C15 N2 119.1(3) . . ? C17 C16 C15 118.7(3) . . ? C17 C16 C21 119.4(3) . . ? C15 C16 C21 121.9(3) . . ? C18 C17 C16 122.6(3) . . ? C18 C17 H17 118.7 . . ? C16 C17 H17 118.7 . . ? C17 C18 C19 117.3(3) . . ? C17 C18 C22 121.2(3) . . ? C19 C18 C22 121.4(3) . . ? C20 C19 C18 122.3(3) . . ? C20 C19 H19 118.9 . . ? C18 C19 H19 118.9 . . ? C19 C20 C15 119.2(3) . . ? C19 C20 C23 120.5(3) . . ? C15 C20 C23 120.2(3) . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C22 H22D 109.5 . . ? H22A C22 H22D 141.1 . . ? H22B C22 H22D 56.3 . . ? H22C C22 H22D 56.3 . . ? C18 C22 H22E 109.5 . . ? H22A C22 H22E 56.3 . . ? H22B C22 H22E 141.1 . . ? H22C C22 H22E 56.3 . . ? H22D C22 H22E 109.5 . . ? C18 C22 H22F 109.5 . . ? H22A C22 H22F 56.3 . . ? H22B C22 H22F 56.3 . . ? H22C C22 H22F 141.1 . . ? H22D C22 H22F 109.5 . . ? H22E C22 H22F 109.5 . . ? O1 C24 Fe 177.5(3) . . ? O2 C25 Fe 177.1(3) . . ? C30 C26 C27 108.5(3) . . ? C30 C26 Fe 70.54(18) . . ? C27 C26 Fe 70.40(18) . . ? C30 C26 H26 125.8 . . ? C27 C26 H26 125.8 . . ? Fe C26 H26 124.9 . . ? C28 C27 C26 107.1(3) . . ? C28 C27 Fe 70.5(2) . . ? C26 C27 Fe 70.09(19) . . ? C28 C27 H27 126.5 . . ? C26 C27 H27 126.5 . . ? Fe C27 H27 124.5 . . ? C29 C28 C27 108.3(3) . . ? C29 C28 Fe 70.1(2) . . ? C27 C28 Fe 70.1(2) . . ? C29 C28 H28 125.9 . . ? C27 C28 H28 125.9 . . ? Fe C28 H28 125.5 . . ? C30 C29 C28 108.0(3) . . ? C30 C29 Fe 70.4(2) . . ? C28 C29 Fe 70.7(2) . . ? C30 C29 H29 126 . . ? C28 C29 H29 126 . . ? Fe C29 H29 124.5 . . ? C26 C30 C29 108.2(3) . . ? C26 C30 Fe 70.36(18) . . ? C29 C30 Fe 70.43(19) . . ? C26 C30 H30 125.9 . . ? C29 C30 H30 125.9 . . ? Fe C30 H30 124.9 . . ? #===END data_(3)-dec904 _database_code_depnum_ccdc_archive 'CCDC 675702' _audit_creation_date 2004-12-06T11:58:41-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_moiety 'C20 H28 Fe2 I2 In2 O6 Si2, 2(C36 H46 Fe I In N2 O2)' _chemical_formula_sum 'C92 H120 Fe4 I4 In4 N4 O10 Si2' _chemical_formula_weight 2688.38 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0644(3) _cell_length_b 17.2204(6) _cell_length_c 17.4463(5) _cell_angle_alpha 67.993(2) _cell_angle_beta 89.321(2) _cell_angle_gamma 89.682(1) _cell_volume 2524.64(14) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 46700 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.733 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.755 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.6658 _exptl_absorpt_correction_T_max 0.78 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.109017 _diffrn_orient_matrix_ub_12 -0.95174E-2 _diffrn_orient_matrix_ub_13 0.33677E-2 _diffrn_orient_matrix_ub_21 -0.62974E-2 _diffrn_orient_matrix_ub_22 0.283008E-1 _diffrn_orient_matrix_ub_23 -0.614597E-1 _diffrn_orient_matrix_ub_31 0.157591E-1 _diffrn_orient_matrix_ub_32 -0.550592E-1 _diffrn_orient_matrix_ub_33 -0.58208E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_unetI/netI 0.0594 _diffrn_reflns_number 42278 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.4 _diffrn_reflns_theta_max 26.73 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.966 _diffrn_measured_fraction_theta_max 0.966 _reflns_number_total 10369 _reflns_number_gt 7969 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0132P)^2^+23.5871P] 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_number_reflns 10369 _refine_ls_number_parameters 543 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1094 _refine_ls_wR_factor_gt 0.1004 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.254 _refine_diff_density_min -1.47 _refine_diff_density_rms 0.156 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.31 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 In In 0.38363(5) 0.63662(3) 0.13590(3) 0.01530(11) Uani 1 1 d . . . Fe Fe 0.20784(9) 0.55144(6) 0.08602(5) 0.0168(2) Uani 1 1 d . A . Fe1B Fe 0.00665(14) 0.20949(7) 0.31768(7) 0.0410(3) Uani 1 1 d . . . I I 0.68343(5) 0.61132(3) 0.10904(3) 0.02676(12) Uani 1 1 d . A 1 O1 O 0.3968(6) 0.5841(4) -0.0578(3) 0.0436(14) Uani 1 1 d . A 1 O2 O 0.0315(6) 0.6999(3) 0.0018(3) 0.0367(13) Uani 1 1 d . A 1 N1 N 0.4061(5) 0.6284(3) 0.2631(3) 0.0181(11) Uani 1 1 d . A 1 N2 N 0.3937(6) 0.7737(3) 0.0964(3) 0.0204(12) Uani 1 1 d . A 1 C1 C 0.4870(7) 0.6852(4) 0.2792(4) 0.0220(14) Uani 1 1 d . A 1 C2 C 0.5289(7) 0.7619(4) 0.2197(4) 0.0243(15) Uani 1 1 d . A 1 H2 H 0.6053 0.7894 0.2366 0.029 Uiso 1 1 calc R A 1 C3 C 0.4783(7) 0.8058(4) 0.1394(4) 0.0222(14) Uani 1 1 d . A 1 C4 C 0.5349(8) 0.6673(5) 0.3668(4) 0.0312(17) Uani 1 1 d . A 1 H4A H 0.4683 0.626 0.4054 0.047 Uiso 1 1 calc R A 1 H4B H 0.5317 0.7192 0.3777 0.047 Uiso 1 1 calc R A 1 H4C H 0.6358 0.6451 0.3742 0.047 Uiso 1 1 calc R A 1 C5 C 0.5206(8) 0.8980(4) 0.1019(5) 0.0324(17) Uani 1 1 d . A 1 H5A H 0.5982 0.906 0.0601 0.049 Uiso 1 1 calc R A 1 H5B H 0.5568 0.9158 0.1454 0.049 Uiso 1 1 calc R A 1 H5C H 0.434 0.9314 0.0761 0.049 Uiso 1 1 calc R A 1 C6 C 0.3440(7) 0.5572(4) 0.3298(4) 0.0190(14) Uani 1 1 d . A 1 C7 C 0.1980(7) 0.5612(4) 0.3549(4) 0.0223(14) Uani 1 1 d . A 1 C8 C 0.1337(8) 0.4899(5) 0.4122(4) 0.0288(16) Uani 1 1 d . A 1 H8 H 0.0344 0.492 0.4293 0.035 Uiso 1 1 calc R A 1 C9 C 0.2120(8) 0.4159(5) 0.4448(4) 0.0316(17) Uani 1 1 d . A 1 H9 H 0.1658 0.3672 0.4832 0.038 Uiso 1 1 calc R A 1 C10 C 0.3564(8) 0.4127(4) 0.4216(4) 0.0266(16) Uani 1 1 d . A 1 H10 H 0.4099 0.3618 0.4451 0.032 Uiso 1 1 calc R A 1 C11 C 0.4264(7) 0.4829(4) 0.3642(4) 0.0215(14) Uani 1 1 d . A 1 C12 C 0.1100(7) 0.6434(5) 0.3220(4) 0.0283(16) Uani 1 1 d . A 1 H12 H 0.1571 0.6803 0.2688 0.034 Uiso 1 1 calc R A 1 C13 C -0.0507(9) 0.6327(6) 0.3052(7) 0.061(3) Uani 1 1 d . A 1 H13A H -0.0989 0.6877 0.2838 0.091 Uiso 1 1 calc R A 1 H13B H -0.0999 0.5971 0.3566 0.091 Uiso 1 1 calc R A 1 H13C H -0.0573 0.6065 0.2642 0.091 Uiso 1 1 calc R A 1 C14 C 0.1191(11) 0.6879(6) 0.3826(6) 0.060(3) Uani 1 1 d . A 1 H14A H 0.2228 0.6952 0.3936 0.091 Uiso 1 1 calc R A 1 H14B H 0.0687 0.6544 0.4344 0.091 Uiso 1 1 calc R A 1 H14C H 0.0715 0.7429 0.3586 0.091 Uiso 1 1 calc R A 1 C15 C 0.5868(7) 0.4753(4) 0.3419(4) 0.0243(15) Uani 1 1 d . A 1 H15 H 0.621 0.5316 0.3029 0.029 Uiso 1 1 calc R A 1 C16 C 0.6064(8) 0.4125(5) 0.2987(4) 0.0320(17) Uani 1 1 d . A 1 H16A H 0.7109 0.4095 0.2849 0.048 Uiso 1 1 calc R A 1 H16B H 0.5483 0.4311 0.2479 0.048 Uiso 1 1 calc R A 1 H16C H 0.5725 0.3571 0.3357 0.048 Uiso 1 1 calc R A 1 C17 C 0.6837(8) 0.4486(5) 0.4192(5) 0.0348(18) Uani 1 1 d . A 1 H17A H 0.7867 0.4446 0.4033 0.052 Uiso 1 1 calc R A 1 H17B H 0.6508 0.394 0.4586 0.052 Uiso 1 1 calc R A 1 H17C H 0.6755 0.4902 0.4449 0.052 Uiso 1 1 calc R A 1 C18 C 0.3273(7) 0.8299(4) 0.0208(4) 0.0218(14) Uani 1 1 d . A 1 C19 C 0.4069(8) 0.8559(4) -0.0544(4) 0.0270(16) Uani 1 1 d . A 1 C20 C 0.3387(9) 0.9122(5) -0.1253(5) 0.0352(18) Uani 1 1 d . A 1 H20 H 0.3899 0.9302 -0.1768 0.042 Uiso 1 1 calc R A 1 C21 C 0.1987(9) 0.9420(5) -0.1214(5) 0.0379(19) Uani 1 1 d . A 1 H21 H 0.1553 0.9817 -0.1696 0.045 Uiso 1 1 calc R A 1 C22 C 0.1216(8) 0.9140(5) -0.0477(5) 0.0361(18) Uani 1 1 d . A 1 H22 H 0.0242 0.9342 -0.0464 0.043 Uiso 1 1 calc R A 1 C23 C 0.1809(7) 0.8574(4) 0.0249(4) 0.0269(16) Uani 1 1 d . A 1 C24 C 0.5637(9) 0.8263(5) -0.0627(5) 0.0368(19) Uani 1 1 d . A 1 H24 H 0.598 0.7901 -0.0062 0.044 Uiso 1 1 calc R A 1 C25 C 0.5640(11) 0.7735(6) -0.1160(6) 0.058(3) Uani 1 1 d . A 1 H25A H 0.6648 0.7547 -0.1207 0.087 Uiso 1 1 calc R A 1 H25B H 0.5274 0.8071 -0.1712 0.087 Uiso 1 1 calc R A 1 H25C H 0.5001 0.7246 -0.0904 0.087 Uiso 1 1 calc R A 1 C26 C 0.6727(9) 0.8982(5) -0.0986(6) 0.050(2) Uani 1 1 d . A 1 H26A H 0.7709 0.8756 -0.1022 0.074 Uiso 1 1 calc R A 1 H26B H 0.6763 0.9304 -0.0628 0.074 Uiso 1 1 calc R A 1 H26C H 0.641 0.9347 -0.154 0.074 Uiso 1 1 calc R A 1 C27 C 0.0938(8) 0.8267(5) 0.1045(5) 0.0304(17) Uani 1 1 d . A 1 H27 H 0.1196 0.7664 0.1345 0.036 Uiso 1 1 calc R A 1 C28 C -0.0740(8) 0.8317(5) 0.0912(5) 0.041(2) Uani 1 1 d . A 1 H28A H -0.1249 0.8106 0.145 0.062 Uiso 1 1 calc R A 1 H28B H -0.1013 0.7976 0.0595 0.062 Uiso 1 1 calc R A 1 H28C H -0.1027 0.8901 0.0608 0.062 Uiso 1 1 calc R A 1 C29 C 0.1312(9) 0.8727(5) 0.1605(5) 0.042(2) Uani 1 1 d . A 1 H29A H 0.0719 0.8503 0.2113 0.063 Uiso 1 1 calc R A 1 H29B H 0.1099 0.9325 0.1321 0.063 Uiso 1 1 calc R A 1 H29C H 0.2362 0.8652 0.1742 0.063 Uiso 1 1 calc R A 1 C30 C 0.2073(8) 0.4586(4) 0.2076(4) 0.0261(16) Uani 1 1 d . A 1 H30 H 0.2549 0.4621 0.2544 0.031 Uiso 1 1 calc R A 1 C31 C 0.0633(8) 0.4837(4) 0.1832(4) 0.0287(16) Uani 1 1 d . A 1 H31 H -0.0033 0.5084 0.2099 0.034 Uiso 1 1 calc R A 1 C32 C 0.0327(7) 0.4664(4) 0.1119(4) 0.0256(16) Uani 1 1 d . A 1 H32 H -0.0575 0.477 0.0826 0.031 Uiso 1 1 calc R A 1 C33 C 0.1610(8) 0.4306(4) 0.0924(4) 0.0285(16) Uani 1 1 d . A 1 H33 H 0.172 0.4122 0.0477 0.034 Uiso 1 1 calc R A 1 C34 C 0.2703(7) 0.4270(4) 0.1506(4) 0.0243(15) Uani 1 1 d . A 1 H34 H 0.3683 0.4069 0.1514 0.029 Uiso 1 1 calc R A 1 C35 C 0.3260(8) 0.5725(4) 0.0002(5) 0.0275(16) Uani 1 1 d . A 1 C36 C 0.1031(7) 0.6430(4) 0.0372(4) 0.0243(15) Uani 1 1 d . A 1 I1B I 0.21143(7) 0.13001(4) 0.57603(4) 0.05224(17) Uani 1 1 d . B 1 In1B In 0.05238(6) 0.09955(3) 0.45640(3) 0.03193(14) Uani 1 1 d . . 1 Si1B Si 0.2664(3) -0.05322(15) 0.42500(15) 0.0426(6) Uani 1 1 d . C 1 O1B O -0.0600(7) 0.3235(4) 0.4007(5) 0.0643(19) Uani 1 1 d . . 1 O2B O 0.3196(8) 0.2491(4) 0.3067(5) 0.073(2) Uani 1 1 d . . 1 O3B O 0.1229(6) -0.0241(3) 0.4684(3) 0.0350(12) Uani 1 1 d . . 1 C1B C -0.0327(9) 0.2777(5) 0.3682(6) 0.045(2) Uani 1 1 d . . 1 C2B C 0.1968(11) 0.2319(5) 0.3116(5) 0.050(2) Uani 1 1 d . . 1 C3B C -0.0125(15) 0.2199(10) 0.1964(6) 0.085(4) Uani 1 1 d . . 1 H3B H 0.0596 0.2456 0.1548 0.103 Uiso 1 1 calc R . 1 C4B C -0.1298(13) 0.2596(7) 0.2152(6) 0.066(3) Uani 1 1 d . . 1 H4B1 H -0.1538 0.3172 0.1883 0.08 Uiso 1 1 calc R . 1 C5B C -0.2078(13) 0.2021(9) 0.2796(7) 0.073(3) Uani 1 1 d . . 1 H5B1 H -0.294 0.2128 0.3056 0.088 Uiso 1 1 calc R . 1 C6B C -0.137(2) 0.1254(8) 0.2994(7) 0.099(6) Uani 1 1 d . . 1 H6B H -0.166 0.0739 0.3412 0.119 Uiso 1 1 calc R . 1 C7B C -0.015(2) 0.1375(9) 0.2471(10) 0.105(6) Uani 1 1 d . . 1 H7B H 0.0537 0.0959 0.2467 0.127 Uiso 1 1 calc R . 1 C8B C 0.4044(10) 0.0315(6) 0.3938(7) 0.067(3) Uani 1 1 d . C 1 H8B1 H 0.3598 0.0831 0.3551 0.101 Uiso 1 1 calc R C 1 H8B2 H 0.4885 0.0157 0.367 0.101 Uiso 1 1 calc R C 1 H8B3 H 0.4381 0.0409 0.4428 0.101 Uiso 1 1 calc R C 1 C9B C 0.3419(11) -0.1533(6) 0.4981(7) 0.070(3) Uani 1 1 d . C 1 H9B1 H 0.2648 -0.1962 0.5133 0.106 Uiso 1 1 calc R C 1 H9B2 H 0.3761 -0.1456 0.5479 0.106 Uiso 1 1 calc R C 1 H9B3 H 0.4248 -0.171 0.4719 0.106 Uiso 1 1 calc R C 1 C10B C 0.2095(14) -0.0716(8) 0.3314(7) 0.082(4) Uani 1 1 d . C 1 H10A H 0.1357 -0.1164 0.3467 0.123 Uiso 1 1 calc R C 1 H10B H 0.2957 -0.0881 0.3065 0.123 Uiso 1 1 calc R C 1 H10C H 0.1671 -0.0201 0.2914 0.123 Uiso 1 1 calc R C 1 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 In 0.0131(2) 0.0154(2) 0.0175(2) -0.00628(18) -0.00018(17) -0.00120(17) Fe 0.0165(4) 0.0170(5) 0.0166(5) -0.0059(4) -0.0007(4) -0.0023(4) I 0.0157(2) 0.0332(3) 0.0321(3) -0.0132(2) 0.00371(18) 0.00379(18) O1 0.051(4) 0.048(4) 0.036(3) -0.021(3) 0.024(3) -0.019(3) O2 0.032(3) 0.030(3) 0.041(3) -0.004(3) -0.010(2) 0.006(2) N1 0.014(3) 0.022(3) 0.021(3) -0.010(2) 0.001(2) -0.002(2) N2 0.017(3) 0.015(3) 0.027(3) -0.005(2) -0.001(2) 0.000(2) C1 0.011(3) 0.031(4) 0.026(4) -0.015(3) 0.000(3) 0.005(3) C2 0.016(3) 0.025(4) 0.037(4) -0.016(3) -0.003(3) -0.002(3) C3 0.014(3) 0.019(3) 0.035(4) -0.011(3) 0.002(3) 0.000(3) C4 0.031(4) 0.040(5) 0.028(4) -0.019(4) -0.006(3) -0.003(3) C5 0.037(4) 0.022(4) 0.039(4) -0.012(3) 0.000(3) -0.006(3) C6 0.017(3) 0.023(4) 0.020(3) -0.011(3) -0.004(3) -0.002(3) C7 0.018(3) 0.031(4) 0.019(3) -0.011(3) 0.001(3) 0.002(3) C8 0.020(3) 0.042(5) 0.022(4) -0.009(3) 0.001(3) -0.003(3) C9 0.035(4) 0.032(4) 0.022(4) -0.003(3) -0.002(3) -0.011(3) C10 0.029(4) 0.025(4) 0.025(4) -0.008(3) -0.010(3) 0.002(3) C11 0.021(3) 0.029(4) 0.015(3) -0.009(3) -0.007(3) 0.003(3) C12 0.020(3) 0.034(4) 0.024(4) -0.005(3) 0.009(3) 0.003(3) C13 0.030(5) 0.058(6) 0.108(9) -0.045(6) -0.025(5) 0.018(4) C14 0.062(6) 0.053(6) 0.073(7) -0.031(6) -0.018(5) 0.022(5) C15 0.020(3) 0.023(4) 0.025(4) -0.003(3) -0.005(3) 0.002(3) C16 0.029(4) 0.037(4) 0.029(4) -0.012(3) 0.000(3) 0.007(3) C17 0.026(4) 0.041(5) 0.036(4) -0.013(4) -0.011(3) 0.005(3) C18 0.029(4) 0.013(3) 0.024(4) -0.007(3) -0.003(3) -0.001(3) C19 0.036(4) 0.018(4) 0.028(4) -0.009(3) 0.000(3) -0.003(3) C20 0.053(5) 0.025(4) 0.024(4) -0.004(3) -0.001(3) -0.007(4) C21 0.044(5) 0.025(4) 0.038(5) -0.003(3) -0.018(4) -0.002(4) C22 0.030(4) 0.031(4) 0.041(5) -0.006(4) -0.009(3) 0.000(3) C23 0.024(4) 0.018(4) 0.039(4) -0.011(3) -0.004(3) 0.000(3) C24 0.042(5) 0.025(4) 0.038(5) -0.006(3) 0.013(4) 0.000(3) C25 0.070(7) 0.044(6) 0.065(6) -0.027(5) 0.027(5) -0.010(5) C26 0.035(5) 0.043(5) 0.056(6) -0.002(4) 0.010(4) -0.003(4) C27 0.025(4) 0.022(4) 0.039(4) -0.006(3) -0.002(3) 0.005(3) C28 0.032(4) 0.037(5) 0.055(5) -0.017(4) -0.001(4) 0.004(4) C29 0.032(4) 0.051(5) 0.043(5) -0.019(4) -0.004(4) 0.008(4) C30 0.037(4) 0.017(3) 0.018(3) 0.001(3) -0.004(3) -0.012(3) C31 0.031(4) 0.019(4) 0.029(4) -0.001(3) 0.013(3) -0.003(3) C32 0.023(4) 0.025(4) 0.022(4) -0.001(3) -0.008(3) -0.006(3) C33 0.045(4) 0.015(4) 0.026(4) -0.009(3) 0.002(3) -0.006(3) C34 0.025(4) 0.014(3) 0.027(4) -0.001(3) 0.000(3) 0.000(3) C35 0.031(4) 0.022(4) 0.033(4) -0.015(3) 0.000(3) -0.006(3) C36 0.023(4) 0.029(4) 0.026(4) -0.015(3) 0.001(3) -0.014(3) I1B 0.0514(4) 0.0542(4) 0.0595(4) -0.0305(3) -0.0112(3) -0.0053(3) In1B 0.0372(3) 0.0248(3) 0.0313(3) -0.0077(2) 0.0006(2) -0.0029(2) Fe1B 0.0550(8) 0.0284(6) 0.0337(6) -0.0048(5) -0.0012(6) -0.0029(5) Si1B 0.0416(13) 0.0357(13) 0.0503(15) -0.0162(11) 0.0108(11) -0.0015(10) O1B 0.056(4) 0.052(4) 0.100(6) -0.044(4) -0.020(4) 0.017(3) O2B 0.056(5) 0.055(4) 0.087(6) -0.001(4) 0.013(4) -0.011(4) O3B 0.041(3) 0.027(3) 0.035(3) -0.009(2) 0.005(2) -0.005(2) C1B 0.039(5) 0.035(5) 0.057(6) -0.013(4) -0.016(4) 0.006(4) C2B 0.064(6) 0.027(5) 0.044(5) 0.003(4) 0.012(5) -0.006(4) C3B 0.088(9) 0.134(13) 0.031(6) -0.027(7) -0.003(6) 0.011(9) C4B 0.083(8) 0.050(6) 0.047(6) 0.004(5) -0.027(6) 0.000(6) C5B 0.065(7) 0.099(10) 0.056(7) -0.027(7) -0.006(5) -0.020(7) C6B 0.175(15) 0.060(8) 0.039(7) 0.009(6) -0.041(8) -0.065(9) C7B 0.180(17) 0.077(10) 0.085(10) -0.059(9) -0.071(11) 0.050(10) C8B 0.048(6) 0.050(6) 0.095(8) -0.016(6) 0.026(6) -0.004(5) C9B 0.061(7) 0.050(6) 0.087(8) -0.011(6) 0.019(6) 0.007(5) C10B 0.097(9) 0.087(9) 0.077(8) -0.049(7) 0.018(7) -0.002(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 In N1 2.182(5) . ? In N2 2.200(5) . ? In Fe 2.5423(9) . ? In I 2.8114(6) . ? Fe C35 1.756(7) . ? Fe C36 1.764(8) . ? Fe C33 2.087(7) . ? Fe C34 2.092(6) . ? Fe C32 2.093(6) . ? Fe C31 2.105(7) . ? Fe C30 2.125(6) . ? O1 C35 1.143(8) . ? O2 C36 1.145(8) . ? N1 C1 1.339(8) . ? N1 C6 1.447(8) . ? N2 C3 1.336(8) . ? N2 C18 1.447(8) . ? C1 C2 1.391(9) . ? C1 C4 1.511(9) . ? C2 C3 1.402(9) . ? C3 C5 1.522(9) . ? C6 C7 1.398(9) . ? C6 C11 1.408(9) . ? C7 C8 1.385(9) . ? C7 C12 1.536(9) . ? C8 C9 1.381(10) . ? C9 C10 1.373(10) . ? C10 C11 1.397(9) . ? C11 C15 1.518(9) . ? C12 C13 1.515(10) . ? C12 C14 1.524(11) . ? C15 C17 1.536(9) . ? C15 C16 1.541(10) . ? C18 C19 1.409(9) . ? C18 C23 1.416(9) . ? C19 C20 1.401(10) . ? C19 C24 1.531(10) . ? C20 C21 1.376(11) . ? C21 C22 1.376(11) . ? C22 C23 1.389(10) . ? C23 C27 1.503(10) . ? C24 C26 1.522(10) . ? C24 C25 1.526(11) . ? C27 C29 1.513(11) . ? C27 C28 1.538(10) . ? C30 C31 1.393(10) . ? C30 C34 1.414(10) . ? C31 C32 1.412(10) . ? C32 C33 1.410(10) . ? C33 C34 1.412(10) . ? I1B In1B 2.7585(8) . ? In1B O3B 2.152(5) 2_556 ? In1B O3B 2.153(5) . ? Fe1B C1B 1.746(10) . ? Fe1B C2B 1.762(10) . ? Fe1B C7B 2.060(11) . ? Fe1B C3B 2.064(10) . ? Fe1B C6B 2.065(10) . ? Fe1B C5B 2.082(11) . ? Fe1B C4B 2.087(9) . ? Fe1B In1B 2.4889(12) . ? Si1B O3B 1.665(6) . ? Si1B C8B 1.844(9) . ? Si1B C9B 1.851(10) . ? Si1B C10B 1.856(11) . ? O1B C1B 1.155(10) . ? O2B C2B 1.147(11) . ? C3B C4B 1.361(16) . ? C3B C7B 1.362(18) . ? C4B C5B 1.378(14) . ? C5B C6B 1.390(18) . ? C6B C7B 1.39(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 In N2 88.1(2) . . ? N1 In Fe 126.05(13) . . ? N2 In Fe 127.56(14) . . ? N1 In I 96.51(13) . . ? N2 In I 96.94(13) . . ? Fe In I 114.12(3) . . ? C35 Fe C36 92.9(3) . . ? C35 Fe C33 93.1(3) . . ? C36 Fe C33 127.4(3) . . ? C35 Fe C34 98.0(3) . . ? C36 Fe C34 163.1(3) . . ? C33 Fe C34 39.5(3) . . ? C35 Fe C32 123.0(3) . . ? C36 Fe C32 97.0(3) . . ? C33 Fe C32 39.4(3) . . ? C34 Fe C32 66.2(3) . . ? C35 Fe C31 158.7(3) . . ? C36 Fe C31 100.5(3) . . ? C33 Fe C31 65.7(3) . . ? C34 Fe C31 65.6(3) . . ? C32 Fe C31 39.3(3) . . ? C35 Fe C30 133.3(3) . . ? C36 Fe C30 133.4(3) . . ? C33 Fe C30 65.5(3) . . ? C34 Fe C30 39.2(3) . . ? C32 Fe C30 65.5(2) . . ? C31 Fe C30 38.5(3) . . ? C35 Fe In 87.1(2) . . ? C36 Fe In 88.9(2) . . ? C33 Fe In 143.6(2) . . ? C34 Fe In 104.45(19) . . ? C32 Fe In 148.69(19) . . ? C31 Fe In 109.4(2) . . ? C30 Fe In 88.27(18) . . ? C1 N1 C6 120.6(5) . . ? C1 N1 In 119.8(4) . . ? C6 N1 In 119.4(4) . . ? C3 N2 C18 118.8(5) . . ? C3 N2 In 118.1(4) . . ? C18 N2 In 122.7(4) . . ? N1 C1 C2 123.9(6) . . ? N1 C1 C4 119.3(6) . . ? C2 C1 C4 116.8(6) . . ? C1 C2 C3 131.3(6) . . ? N2 C3 C2 125.2(6) . . ? N2 C3 C5 119.4(6) . . ? C2 C3 C5 115.4(6) . . ? C7 C6 C11 120.6(6) . . ? C7 C6 N1 119.2(6) . . ? C11 C6 N1 120.0(5) . . ? C8 C7 C6 119.0(6) . . ? C8 C7 C12 119.7(6) . . ? C6 C7 C12 121.2(6) . . ? C9 C8 C7 120.9(6) . . ? C10 C9 C8 120.0(7) . . ? C9 C10 C11 121.3(7) . . ? C10 C11 C6 118.1(6) . . ? C10 C11 C15 118.6(6) . . ? C6 C11 C15 123.2(6) . . ? C13 C12 C14 109.1(7) . . ? C13 C12 C7 114.3(6) . . ? C14 C12 C7 109.9(6) . . ? C11 C15 C17 110.8(6) . . ? C11 C15 C16 111.7(5) . . ? C17 C15 C16 109.5(6) . . ? C19 C18 C23 121.4(6) . . ? C19 C18 N2 120.4(6) . . ? C23 C18 N2 118.2(6) . . ? C20 C19 C18 118.0(7) . . ? C20 C19 C24 118.4(7) . . ? C18 C19 C24 123.5(6) . . ? C21 C20 C19 121.1(7) . . ? C22 C21 C20 119.9(7) . . ? C21 C22 C23 122.4(7) . . ? C22 C23 C18 117.1(7) . . ? C22 C23 C27 121.5(6) . . ? C18 C23 C27 121.3(6) . . ? C26 C24 C25 109.4(7) . . ? C26 C24 C19 113.0(6) . . ? C25 C24 C19 110.2(7) . . ? C23 C27 C29 112.8(6) . . ? C23 C27 C28 113.1(6) . . ? C29 C27 C28 108.5(6) . . ? C31 C30 C34 108.1(6) . . ? C31 C30 Fe 70.0(4) . . ? C34 C30 Fe 69.2(4) . . ? C30 C31 C32 108.7(6) . . ? C30 C31 Fe 71.5(4) . . ? C32 C31 Fe 69.9(4) . . ? C33 C32 C31 107.3(6) . . ? C33 C32 Fe 70.1(4) . . ? C31 C32 Fe 70.8(4) . . ? C32 C33 C34 108.3(6) . . ? C32 C33 Fe 70.5(4) . . ? C34 C33 Fe 70.4(4) . . ? C33 C34 C30 107.6(6) . . ? C33 C34 Fe 70.1(4) . . ? C30 C34 Fe 71.7(4) . . ? O1 C35 Fe 175.9(6) . . ? O2 C36 Fe 175.0(6) . . ? O3B In1B O3B 78.8(2) 2_556 . ? O3B In1B Fe1B 122.04(14) 2_556 . ? O3B In1B Fe1B 120.64(14) . . ? O3B In1B I1B 99.96(14) 2_556 . ? O3B In1B I1B 103.39(14) . . ? Fe1B In1B I1B 122.50(4) . . ? C1B Fe1B C2B 92.7(4) . . ? C1B Fe1B C7B 161.9(5) . . ? C2B Fe1B C7B 103.7(6) . . ? C1B Fe1B C3B 133.0(5) . . ? C2B Fe1B C3B 95.7(5) . . ? C7B Fe1B C3B 38.6(5) . . ? C1B Fe1B C6B 126.7(7) . . ? C2B Fe1B C6B 139.7(7) . . ? C7B Fe1B C6B 39.3(6) . . ? C3B Fe1B C6B 65.0(5) . . ? C1B Fe1B C5B 96.4(5) . . ? C2B Fe1B C5B 159.6(4) . . ? C7B Fe1B C5B 65.6(6) . . ? C3B Fe1B C5B 64.9(5) . . ? C6B Fe1B C5B 39.2(5) . . ? C1B Fe1B C4B 100.1(4) . . ? C2B Fe1B C4B 121.7(4) . . ? C7B Fe1B C4B 64.7(5) . . ? C3B Fe1B C4B 38.3(4) . . ? C6B Fe1B C4B 64.8(4) . . ? C5B Fe1B C4B 38.6(4) . . ? C1B Fe1B In1B 87.3(3) . . ? C2B Fe1B In1B 87.6(3) . . ? C7B Fe1B In1B 101.0(4) . . ? C3B Fe1B In1B 139.1(4) . . ? C6B Fe1B In1B 86.5(3) . . ? C5B Fe1B In1B 111.0(3) . . ? C4B Fe1B In1B 149.0(3) . . ? O3B Si1B C8B 108.6(4) . . ? O3B Si1B C9B 109.7(4) . . ? C8B Si1B C9B 112.3(5) . . ? O3B Si1B C10B 110.9(4) . . ? C8B Si1B C10B 108.3(5) . . ? C9B Si1B C10B 107.0(6) . . ? Si1B O3B In1B 129.0(3) . 2_556 ? Si1B O3B In1B 129.6(3) . . ? In1B O3B In1B 101.2(2) 2_556 . ? O1B C1B Fe1B 179.0(8) . . ? O2B C2B Fe1B 177.9(8) . . ? C4B C3B C7B 109.0(13) . . ? C4B C3B Fe1B 71.8(6) . . ? C7B C3B Fe1B 70.6(6) . . ? C3B C4B C5B 108.5(11) . . ? C3B C4B Fe1B 69.9(6) . . ? C5B C4B Fe1B 70.5(6) . . ? C4B C5B C6B 107.0(12) . . ? C4B C5B Fe1B 70.9(6) . . ? C6B C5B Fe1B 69.7(7) . . ? C7B C6B C5B 107.8(10) . . ? C7B C6B Fe1B 70.2(7) . . ? C5B C6B Fe1B 71.1(6) . . ? C3B C7B C6B 107.6(13) . . ? C3B C7B Fe1B 70.9(7) . . ? C6B C7B Fe1B 70.5(7) . . ? #===END data_(4)-jun2505 _database_code_depnum_ccdc_archive 'CCDC 675703' _audit_creation_date 2005-06-27T11:32:04-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C29 H43 N2, C32 H12 B F24' _chemical_formula_sum 'C61 H55 B F24 N2' _chemical_formula_weight 1282.88 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 17.4446(9) _cell_length_b 18.3705(14) _cell_length_c 19.2043(14) _cell_angle_alpha 90 _cell_angle_beta 98.741(5) _cell_angle_gamma 90 _cell_volume 6082.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 43449 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 24.108 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2624 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.133 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.568973E-1 _diffrn_orient_matrix_ub_12 -0.10541E-1 _diffrn_orient_matrix_ub_13 0.83727E-2 _diffrn_orient_matrix_ub_21 -0.8943E-3 _diffrn_orient_matrix_ub_22 -0.70264E-2 _diffrn_orient_matrix_ub_23 -0.517533E-1 _diffrn_orient_matrix_ub_31 0.112101E-1 _diffrn_orient_matrix_ub_32 0.529405E-1 _diffrn_orient_matrix_ub_33 -0.52017E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1385 _diffrn_reflns_av_unetI/netI 0.0974 _diffrn_reflns_number 19000 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 24.15 _diffrn_reflns_theta_full 24.15 _diffrn_measured_fraction_theta_full 0.979 _diffrn_measured_fraction_theta_max 0.979 _reflns_number_total 4760 _reflns_number_gt 2878 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Weak and limited diffraction. H on N refined; other H atoms in riding mode. 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^)+(0.0631P)^2^+19.5493P] 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_number_reflns 4760 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1413 _refine_ls_R_factor_gt 0.0803 _refine_ls_wR_factor_ref 0.2016 _refine_ls_wR_factor_gt 0.1686 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.458 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.058 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' 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 N N -0.0286(2) 0.1657(2) 0.1261(2) 0.0414(10) Uani 1 1 d . . . H1X H -0.033(3) 0.189(2) 0.083(3) 0.055(15) Uiso 1 1 d . . . C1 C -0.0083(3) 0.2053(2) 0.1843(2) 0.0391(11) Uani 1 1 d . . . C2 C 0 0.1728(3) 0.25 0.0362(15) Uani 1 2 d S . . H2 H 0 0.1211 0.25 0.043 Uiso 1 2 calc SR . . C3 C 0.0087(3) 0.2836(2) 0.1697(3) 0.0567(14) Uani 1 1 d . . . H3A H 0.0213 0.288 0.1219 0.085 Uiso 1 1 calc R . . H3B H 0.0528 0.3003 0.2037 0.085 Uiso 1 1 calc R . . H3C H -0.0369 0.3134 0.1741 0.085 Uiso 1 1 calc R . . C4 C -0.0580(3) 0.0914(2) 0.1245(2) 0.0414(12) Uani 1 1 d . . . C5 C -0.1377(3) 0.0819(3) 0.1172(2) 0.0471(12) Uani 1 1 d . . . C6 C -0.1644(3) 0.0103(3) 0.1167(3) 0.0571(14) Uani 1 1 d . . . H6 H -0.2186 0.0011 0.1115 0.069 Uiso 1 1 calc R . . C7 C -0.1131(4) -0.0471(3) 0.1237(3) 0.0652(16) Uani 1 1 d . . . H7 H -0.1323 -0.0955 0.124 0.078 Uiso 1 1 calc R . . C8 C -0.0353(4) -0.0355(3) 0.1302(3) 0.0635(16) Uani 1 1 d . . . H8 H -0.001 -0.076 0.1359 0.076 Uiso 1 1 calc R . . C9 C -0.0049(3) 0.0344(3) 0.1286(2) 0.0488(13) Uani 1 1 d . . . C10 C -0.1957(3) 0.1440(3) 0.1071(3) 0.0596(15) Uani 1 1 d . . . H10 H -0.1661 0.1903 0.1177 0.072 Uiso 1 1 calc R . . C11 C -0.2551(4) 0.1395(3) 0.1569(4) 0.0825(19) Uani 1 1 d . . . H11A H -0.2907 0.1809 0.1486 0.124 Uiso 1 1 calc R . . H11B H -0.2285 0.1407 0.2056 0.124 Uiso 1 1 calc R . . H11C H -0.2844 0.094 0.1486 0.124 Uiso 1 1 calc R . . C12 C -0.2346(4) 0.1475(4) 0.0303(3) 0.091(2) Uani 1 1 d . . . H12A H -0.2713 0.1883 0.0242 0.137 Uiso 1 1 calc R . . H12B H -0.2624 0.1019 0.0176 0.137 Uiso 1 1 calc R . . H12C H -0.195 0.1547 -0.0003 0.137 Uiso 1 1 calc R . . C13 C 0.0812(3) 0.0460(3) 0.1299(3) 0.0604(14) Uani 1 1 d . . . H13 H 0.0906 0.0995 0.1275 0.072 Uiso 1 1 calc R . . C14 C 0.1083(4) 0.0106(4) 0.0660(3) 0.0816(19) Uani 1 1 d . . . H14A H 0.164 0.0191 0.0677 0.122 Uiso 1 1 calc R . . H14B H 0.08 0.032 0.0228 0.122 Uiso 1 1 calc R . . H14C H 0.0982 -0.0418 0.0664 0.122 Uiso 1 1 calc R . . C15 C 0.1286(4) 0.0174(4) 0.1970(3) 0.098(2) Uani 1 1 d . . . H15A H 0.1838 0.0265 0.1959 0.148 Uiso 1 1 calc R . . H15B H 0.1199 -0.0351 0.2009 0.148 Uiso 1 1 calc R . . H15C H 0.1129 0.0422 0.2377 0.148 Uiso 1 1 calc R . . B B 0.5 0.0703(4) 0.25 0.0339(17) Uani 1 2 d S . 1 C16 C 0.4383(3) 0.0153(2) 0.2800(2) 0.0367(11) Uani 1 1 d . A 1 C17 C 0.4368(3) 0.0029(2) 0.3512(2) 0.0379(11) Uani 1 1 d . A 1 H17 H 0.4713 0.0296 0.3849 0.045 Uiso 1 1 calc R A 1 C18 C 0.3862(3) -0.0477(2) 0.3753(2) 0.0391(11) Uani 1 1 d . A 1 C19 C 0.3369(3) -0.0884(2) 0.3275(3) 0.0426(12) Uani 1 1 d . A 1 H19 H 0.303 -0.123 0.3435 0.051 Uiso 1 1 calc R A 1 C20 C 0.3372(3) -0.0785(2) 0.2563(2) 0.0393(11) Uani 1 1 d . A 1 C21 C 0.3875(3) -0.0284(2) 0.2336(2) 0.0402(11) Uani 1 1 d . A 1 H21 H 0.3878 -0.0234 0.1844 0.048 Uiso 1 1 calc R A 1 C22 C 0.3896(3) -0.0586(3) 0.4525(3) 0.0484(13) Uani 1 1 d . A 1 C23 C 0.2890(3) -0.1257(3) 0.2051(3) 0.0591(14) Uani 1 1 d . A 1 C24 C 0.5416(3) 0.1253(2) 0.3114(2) 0.0346(11) Uani 1 1 d . B 1 C25 C 0.4954(3) 0.1690(2) 0.3480(2) 0.0383(11) Uani 1 1 d . B 1 H25 H 0.4407 0.1625 0.3393 0.046 Uiso 1 1 calc R B 1 C26 C 0.5260(3) 0.2211(2) 0.3964(2) 0.0378(11) Uani 1 1 d . B 1 C27 C 0.6046(3) 0.2333(2) 0.4097(2) 0.0433(12) Uani 1 1 d . B 1 H27 H 0.6256 0.269 0.4429 0.052 Uiso 1 1 calc R B 1 C28 C 0.6526(3) 0.1923(2) 0.3737(2) 0.0391(11) Uani 1 1 d . B 1 C29 C 0.6214(3) 0.1393(2) 0.3263(2) 0.0388(11) Uani 1 1 d . B 1 H29 H 0.6556 0.1114 0.3029 0.047 Uiso 1 1 calc R B 1 C30 C 0.4723(3) 0.2638(3) 0.4339(3) 0.0480(13) Uani 1 1 d . B 1 C31 C 0.7374(3) 0.2035(3) 0.3877(3) 0.0533(13) Uani 1 1 d . B 1 F1 F 0.3970(2) 0.00217(17) 0.48933(16) 0.0877(12) Uani 1 1 d . A 1 F2 F 0.3273(2) -0.0912(2) 0.46902(17) 0.0911(12) Uani 1 1 d . A 1 F3 F 0.4502(2) -0.0985(2) 0.48007(17) 0.0944(12) Uani 1 1 d . A 1 F4 F 0.2684(2) -0.09631(18) 0.14267(18) 0.0868(11) Uani 1 1 d . A 1 F5 F 0.2230(2) -0.14658(18) 0.22625(19) 0.0862(11) Uani 1 1 d . A 1 F6 F 0.3244(2) -0.18873(17) 0.1948(2) 0.1002(14) Uani 1 1 d . A 1 F7 F 0.4149(2) 0.29494(17) 0.39074(16) 0.0784(10) Uani 1 1 d . B 1 F8 F 0.50689(19) 0.31741(16) 0.47384(16) 0.0719(9) Uani 1 1 d . B 1 F9 F 0.4381(2) 0.22285(15) 0.47794(17) 0.0731(10) Uani 1 1 d . B 1 F10 F 0.7588(2) 0.26855(18) 0.4152(2) 0.0902(12) Uani 1 1 d . B 1 F11 F 0.7722(2) 0.1985(2) 0.33165(19) 0.1088(14) Uani 1 1 d . B 1 F12 F 0.7753(2) 0.1575(2) 0.4346(2) 0.1009(13) Uani 1 1 d . B 1 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 N 0.050(3) 0.046(2) 0.028(2) 0.0046(19) 0.0047(18) -0.0099(19) C1 0.039(3) 0.042(3) 0.037(3) 0.000(2) 0.009(2) -0.005(2) C2 0.040(4) 0.031(3) 0.036(4) 0 0.003(3) 0 C3 0.074(4) 0.045(3) 0.050(3) 0.004(2) 0.004(3) -0.020(3) C4 0.055(3) 0.042(3) 0.028(3) -0.002(2) 0.010(2) -0.010(3) C5 0.050(3) 0.052(3) 0.043(3) -0.013(2) 0.016(2) -0.012(3) C6 0.060(4) 0.053(3) 0.061(4) -0.011(3) 0.018(3) -0.011(3) C7 0.085(5) 0.045(3) 0.070(4) -0.017(3) 0.023(3) -0.017(3) C8 0.081(5) 0.043(3) 0.070(4) -0.011(3) 0.021(3) 0.001(3) C9 0.052(3) 0.053(3) 0.041(3) -0.005(2) 0.007(2) 0.000(3) C10 0.054(3) 0.051(3) 0.076(4) -0.011(3) 0.017(3) -0.009(3) C11 0.077(5) 0.091(5) 0.087(5) -0.004(4) 0.038(4) 0.017(4) C12 0.095(5) 0.099(5) 0.081(5) 0.017(4) 0.014(4) 0.020(4) C13 0.062(4) 0.057(3) 0.060(4) -0.005(3) 0.004(3) 0.001(3) C14 0.074(4) 0.115(5) 0.061(4) -0.010(4) 0.026(3) -0.009(4) C15 0.097(5) 0.135(6) 0.062(4) -0.025(4) 0.010(4) 0.041(5) B 0.037(4) 0.033(4) 0.033(4) 0 0.007(3) 0 C16 0.047(3) 0.029(2) 0.033(3) 0.0011(19) 0.004(2) 0.004(2) C17 0.043(3) 0.031(2) 0.039(3) 0.001(2) 0.002(2) 0.004(2) C18 0.045(3) 0.030(2) 0.043(3) 0.008(2) 0.008(2) 0.007(2) C19 0.046(3) 0.027(2) 0.054(3) 0.008(2) 0.007(2) 0.003(2) C20 0.040(3) 0.028(2) 0.048(3) -0.002(2) 0.001(2) 0.003(2) C21 0.051(3) 0.034(2) 0.034(3) -0.001(2) 0.002(2) 0.009(2) C22 0.054(3) 0.042(3) 0.049(3) 0.013(3) 0.008(3) -0.001(3) C23 0.064(4) 0.046(3) 0.065(4) -0.005(3) 0.001(3) -0.003(3) C24 0.044(3) 0.031(2) 0.030(2) 0.0044(19) 0.007(2) 0.000(2) C25 0.049(3) 0.033(2) 0.033(3) 0.004(2) 0.007(2) -0.001(2) C26 0.048(3) 0.039(3) 0.027(2) 0.000(2) 0.008(2) -0.004(2) C27 0.069(4) 0.033(3) 0.029(3) -0.0029(19) 0.011(2) -0.006(2) C28 0.043(3) 0.040(3) 0.034(3) 0.004(2) 0.007(2) -0.008(2) C29 0.052(3) 0.034(2) 0.033(3) 0.002(2) 0.013(2) 0.003(2) C30 0.057(3) 0.043(3) 0.044(3) -0.007(2) 0.008(3) 0.000(3) C31 0.062(4) 0.047(3) 0.052(3) -0.011(3) 0.012(3) -0.011(3) F1 0.154(4) 0.067(2) 0.0483(19) -0.0044(17) 0.035(2) -0.016(2) F2 0.093(3) 0.122(3) 0.061(2) 0.020(2) 0.0223(19) -0.045(2) F3 0.106(3) 0.121(3) 0.056(2) 0.037(2) 0.0140(19) 0.046(2) F4 0.108(3) 0.086(2) 0.058(2) -0.0049(18) -0.014(2) -0.031(2) F5 0.073(2) 0.088(2) 0.096(3) -0.010(2) 0.008(2) -0.0351(19) F6 0.084(3) 0.061(2) 0.145(4) -0.053(2) -0.017(2) 0.0086(18) F7 0.095(3) 0.077(2) 0.062(2) -0.0105(17) 0.0050(19) 0.0415(19) F8 0.089(2) 0.066(2) 0.065(2) -0.0334(16) 0.0250(18) -0.0066(17) F9 0.091(2) 0.0583(19) 0.082(2) 0.0028(16) 0.054(2) 0.0066(16) F10 0.076(2) 0.076(2) 0.120(3) -0.032(2) 0.019(2) -0.0307(18) F11 0.075(3) 0.188(4) 0.070(2) -0.044(3) 0.033(2) -0.044(3) F12 0.063(2) 0.102(3) 0.132(3) 0.041(3) -0.003(2) -0.011(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N C1 1.334(5) . ? N C4 1.457(6) . ? N H1X 0.92(5) . ? C1 C2 1.383(5) . ? C1 C3 1.504(6) . ? C2 C1 1.383(5) 2 ? C2 H2 0.95 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 C5 1.387(7) . ? C4 C9 1.393(7) . ? C5 C6 1.393(6) . ? C5 C10 1.518(7) . ? C6 C7 1.377(7) . ? C6 H6 0.95 . ? C7 C8 1.362(8) . ? C7 H7 0.95 . ? C8 C9 1.391(7) . ? C8 H8 0.95 . ? C9 C13 1.513(7) . ? C10 C11 1.515(7) . ? C10 C12 1.528(8) . ? C10 H10 1 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 C15 1.516(8) . ? C13 C14 1.526(7) . ? C13 H13 1 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? B C24 1.636(6) 2_655 ? B C24 1.636(6) . ? B C16 1.642(6) . ? B C16 1.642(6) 2_655 ? C16 C17 1.391(6) . ? C16 C21 1.409(6) . ? C17 C18 1.408(6) . ? C17 H17 0.95 . ? C18 C19 1.379(6) . ? C18 C22 1.489(6) . ? C19 C20 1.382(6) . ? C19 H19 0.95 . ? C20 C21 1.387(6) . ? C20 C23 1.474(7) . ? C21 H21 0.95 . ? C22 F1 1.317(5) . ? C22 F2 1.321(6) . ? C22 F3 1.328(6) . ? C23 F4 1.314(6) . ? C23 F5 1.335(6) . ? C23 F6 1.342(6) . ? C24 C25 1.400(6) . ? C24 C29 1.403(6) . ? C25 C26 1.384(6) . ? C25 H25 0.95 . ? C26 C27 1.374(7) . ? C26 C30 1.487(6) . ? C27 C28 1.386(6) . ? C27 H27 0.95 . ? C28 C29 1.386(6) . ? C28 C31 1.477(7) . ? C29 H29 0.95 . ? C30 F7 1.329(6) . ? C30 F8 1.336(5) . ? C30 F9 1.338(5) . ? C31 F11 1.317(6) . ? C31 F12 1.334(6) . ? C31 F10 1.337(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N C4 125.1(4) . . ? C1 N H1X 118(3) . . ? C4 N H1X 116(3) . . ? N C1 C2 120.5(4) . . ? N C1 C3 113.5(4) . . ? C2 C1 C3 125.9(4) . . ? C1 C2 C1 128.9(6) . 2 ? C1 C2 H2 115.5 . . ? C1 C2 H2 115.5 2 . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C9 124.0(4) . . ? C5 C4 N 117.7(4) . . ? C9 C4 N 118.3(4) . . ? C4 C5 C6 116.7(5) . . ? C4 C5 C10 123.8(4) . . ? C6 C5 C10 119.5(5) . . ? C7 C6 C5 120.7(5) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C8 C7 C6 120.9(5) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 121.4(5) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C8 C9 C4 116.3(5) . . ? C8 C9 C13 120.6(5) . . ? C4 C9 C13 123.1(4) . . ? C11 C10 C5 112.6(5) . . ? C11 C10 C12 111.5(5) . . ? C5 C10 C12 110.2(4) . . ? C11 C10 H10 107.4 . . ? C5 C10 H10 107.4 . . ? C12 C10 H10 107.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C15 112.2(5) . . ? C9 C13 C14 110.8(4) . . ? C15 C13 C14 110.0(5) . . ? C9 C13 H13 107.9 . . ? C15 C13 H13 107.9 . . ? C14 C13 H13 107.9 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C24 B C24 103.7(5) 2_655 . ? C24 B C16 113.0(2) 2_655 . ? C24 B C16 111.7(2) . . ? C24 B C16 111.7(2) 2_655 2_655 ? C24 B C16 113.0(2) . 2_655 ? C16 B C16 104.1(5) . 2_655 ? C17 C16 C21 115.2(4) . . ? C17 C16 B 123.8(3) . . ? C21 C16 B 120.7(3) . . ? C16 C17 C18 122.5(4) . . ? C16 C17 H17 118.7 . . ? C18 C17 H17 118.7 . . ? C19 C18 C17 119.9(4) . . ? C19 C18 C22 121.1(4) . . ? C17 C18 C22 118.9(4) . . ? C18 C19 C20 119.5(4) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? C19 C20 C21 119.7(4) . . ? C19 C20 C23 119.7(4) . . ? C21 C20 C23 120.3(5) . . ? C20 C21 C16 123.1(4) . . ? C20 C21 H21 118.4 . . ? C16 C21 H21 118.4 . . ? F1 C22 F2 105.8(4) . . ? F1 C22 F3 104.3(4) . . ? F2 C22 F3 106.7(4) . . ? F1 C22 C18 114.0(4) . . ? F2 C22 C18 113.0(4) . . ? F3 C22 C18 112.3(4) . . ? F4 C23 F5 105.5(5) . . ? F4 C23 F6 106.8(5) . . ? F5 C23 F6 103.6(4) . . ? F4 C23 C20 114.6(4) . . ? F5 C23 C20 113.4(5) . . ? F6 C23 C20 112.1(5) . . ? C25 C24 C29 114.9(4) . . ? C25 C24 B 119.4(4) . . ? C29 C24 B 125.3(3) . . ? C26 C25 C24 122.8(5) . . ? C26 C25 H25 118.6 . . ? C24 C25 H25 118.6 . . ? C27 C26 C25 120.6(4) . . ? C27 C26 C30 120.5(4) . . ? C25 C26 C30 118.9(4) . . ? C26 C27 C28 118.7(4) . . ? C26 C27 H27 120.6 . . ? C28 C27 H27 120.6 . . ? C29 C28 C27 120.1(4) . . ? C29 C28 C31 120.0(4) . . ? C27 C28 C31 119.9(4) . . ? C28 C29 C24 122.8(4) . . ? C28 C29 H29 118.6 . . ? C24 C29 H29 118.6 . . ? F7 C30 F8 105.8(4) . . ? F7 C30 F9 105.6(4) . . ? F8 C30 F9 104.9(4) . . ? F7 C30 C26 113.3(4) . . ? F8 C30 C26 113.9(4) . . ? F9 C30 C26 112.6(4) . . ? F11 C31 F12 105.4(5) . . ? F11 C31 F10 104.4(4) . . ? F12 C31 F10 102.6(4) . . ? F11 C31 C28 114.6(4) . . ? F12 C31 C28 114.5(4) . . ? F10 C31 C28 114.1(4) . . ? #===END data_(5)-jun1207 _database_code_depnum_ccdc_archive 'CCDC 675704' _audit_creation_date 2007-06-19T10:16:14-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H12 B F24, C23 H31 Fe N2 O' _chemical_formula_sum 'C55 H43 B F24 Fe N2 O' _chemical_formula_weight 1270.57 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3806(3) _cell_length_b 14.5771(3) _cell_length_c 17.6709(4) _cell_angle_alpha 70.248(2) _cell_angle_beta 70.292(1) _cell_angle_gamma 81.935(1) _cell_volume 2824.43(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25566 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1284 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.387 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8372 _exptl_absorpt_correction_T_max 0.9638 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.857165E-1 _diffrn_orient_matrix_ub_12 -0.00333 _diffrn_orient_matrix_ub_13 -0.221553E-1 _diffrn_orient_matrix_ub_21 0.33291E-2 _diffrn_orient_matrix_ub_22 -0.30556E-1 _diffrn_orient_matrix_ub_23 0.590926E-1 _diffrn_orient_matrix_ub_31 -0.30416E-2 _diffrn_orient_matrix_ub_32 -0.661269E-1 _diffrn_orient_matrix_ub_33 -0.44368E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_unetI/netI 0.036 _diffrn_reflns_number 34257 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 26.2 _diffrn_reflns_theta_full 26.2 _diffrn_measured_fraction_theta_full 0.974 _diffrn_measured_fraction_theta_max 0.974 _reflns_number_total 11051 _reflns_number_gt 8701 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The H atom on N2 was refined. The six disordered CF3 groups were included with SADI geometry restraints. 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^)+(0.0731P)^2^+2.6637P] 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_number_reflns 11051 _refine_ls_number_parameters 935 _refine_ls_number_restraints 1722 _refine_ls_R_factor_all 0.075 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1567 _refine_ls_wR_factor_gt 0.1421 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.227 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.317 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.053 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Fe Fe 0.75092(4) 0.60842(4) 0.34508(3) 0.04150(16) Uani 1 1 d . . . O O 0.9067(2) 0.6144(2) 0.43524(18) 0.0622(7) Uani 1 1 d . . . N1 N 0.8040(2) 0.73409(19) 0.25354(17) 0.0352(6) Uani 1 1 d . . . N2 N 0.8568(3) 0.5418(2) 0.2702(2) 0.0478(7) Uani 1 1 d . . . H2X H 0.837(4) 0.490(4) 0.274(3) 0.078(16) Uiso 1 1 d . . . C1 C 0.9060(3) 0.7484(3) 0.2015(2) 0.0400(7) Uani 1 1 d . . . C2 C 0.9954(3) 0.6658(3) 0.2040(2) 0.0481(9) Uani 1 1 d . . . H2A H 1.0589 0.6835 0.15 0.058 Uiso 1 1 calc R . . H2B H 1.0273 0.66 0.2498 0.058 Uiso 1 1 calc R . . C3 C 0.9545(3) 0.5688(3) 0.2173(2) 0.0472(9) Uani 1 1 d . . . C4 C 0.9491(3) 0.8449(3) 0.1375(2) 0.0500(9) Uani 1 1 d . . . H4A H 0.8881 0.8951 0.1433 0.075 Uiso 1 1 calc R . . H4B H 0.9716 0.8395 0.0804 0.075 Uiso 1 1 calc R . . H4C H 1.0156 0.8627 0.1471 0.075 Uiso 1 1 calc R . . C5 C 1.0338(4) 0.5035(3) 0.1705(3) 0.0659(12) Uani 1 1 d . . . H5A H 0.9941 0.4442 0.1824 0.099 Uiso 1 1 calc R . . H5B H 1.1023 0.4861 0.189 0.099 Uiso 1 1 calc R . . H5C H 1.0566 0.538 0.1095 0.099 Uiso 1 1 calc R . . C6 C 0.7233(3) 0.8181(2) 0.2522(2) 0.0382(7) Uani 1 1 d . . . C7 C 0.6517(3) 0.8378(2) 0.2014(2) 0.0399(7) Uani 1 1 d . . . C8 C 0.5682(3) 0.9129(2) 0.2087(2) 0.0467(8) Uani 1 1 d . . . H8 H 0.5185 0.9289 0.175 0.056 Uiso 1 1 calc R . . C9 C 0.5575(3) 0.9637(3) 0.2640(3) 0.0533(10) Uani 1 1 d . . . H9 H 0.4981 1.0122 0.2699 0.064 Uiso 1 1 calc R . . C10 C 0.6321(3) 0.9450(3) 0.3109(3) 0.0534(9) Uani 1 1 d . . . H10 H 0.6247 0.9823 0.3474 0.064 Uiso 1 1 calc R . . C11 C 0.7180(3) 0.8724(3) 0.3056(2) 0.0459(8) Uani 1 1 d . . . C12 C 0.6654(3) 0.7870(3) 0.1359(3) 0.0495(9) Uani 1 1 d . . . H12 H 0.7187 0.7292 0.1462 0.059 Uiso 1 1 calc R . . C13 C 0.5515(4) 0.7508(4) 0.1420(4) 0.0831(15) Uani 1 1 d . . . H13A H 0.4994 0.8067 0.1286 0.125 Uiso 1 1 calc R . . H13B H 0.5166 0.708 0.1995 0.125 Uiso 1 1 calc R . . H13C H 0.5656 0.7145 0.1017 0.125 Uiso 1 1 calc R . . C14 C 0.7181(4) 0.8541(4) 0.0477(3) 0.0676(12) Uani 1 1 d . . . H14A H 0.7294 0.8193 0.0067 0.101 Uiso 1 1 calc R . . H14B H 0.7923 0.8754 0.0431 0.101 Uiso 1 1 calc R . . H14C H 0.6669 0.9111 0.0359 0.101 Uiso 1 1 calc R . . C15 C 0.8044(4) 0.8599(3) 0.3533(3) 0.0604(11) Uani 1 1 d . . . H15 H 0.8598 0.8059 0.341 0.072 Uiso 1 1 calc R . . C16 C 0.8725(4) 0.9528(4) 0.3212(4) 0.0795(14) Uani 1 1 d . . . H16A H 0.9064 0.9709 0.2596 0.119 Uiso 1 1 calc R . . H16B H 0.9337 0.9411 0.3473 0.119 Uiso 1 1 calc R . . H16C H 0.8211 1.0058 0.3363 0.119 Uiso 1 1 calc R . . C17 C 0.7473(5) 0.8315(4) 0.4492(3) 0.0790(14) Uani 1 1 d . . . H17A H 0.6916 0.8828 0.463 0.119 Uiso 1 1 calc R . . H17B H 0.806 0.8234 0.477 0.119 Uiso 1 1 calc R . . H17C H 0.7078 0.77 0.4689 0.119 Uiso 1 1 calc R . . C18 C 0.6480(4) 0.4880(4) 0.4123(4) 0.0800(15) Uani 1 1 d . . . H18 H 0.677 0.4228 0.4193 0.096 Uiso 1 1 calc R . . C19 C 0.6058(4) 0.5441(4) 0.3483(3) 0.0748(13) Uani 1 1 d . . . H19 H 0.6 0.5244 0.3038 0.09 Uiso 1 1 calc R . . C20 C 0.5734(3) 0.6337(4) 0.3596(4) 0.0848(19) Uani 1 1 d . . . H20 H 0.5408 0.6866 0.3245 0.102 Uiso 1 1 calc R . . C21 C 0.5964(5) 0.6338(5) 0.4313(5) 0.098(2) Uani 1 1 d . . . H21 H 0.5839 0.6865 0.4539 0.117 Uiso 1 1 calc R . . C22 C 0.6421(5) 0.5401(6) 0.4638(3) 0.096(2) Uani 1 1 d . . . H22 H 0.6647 0.5175 0.5135 0.115 Uiso 1 1 calc R . . C23 C 0.8491(3) 0.6141(3) 0.3967(2) 0.0476(8) Uani 1 1 d . . . B B 1.3054(3) 0.2415(2) 0.2199(2) 0.0264(6) Uani 1 1 d . . . C24 C 1.2691(2) 0.29486(19) 0.13395(17) 0.0267(6) Uani 1 1 d . . . C25 C 1.1626(2) 0.2786(2) 0.12953(19) 0.0300(6) Uani 1 1 d . . . H25 H 1.1133 0.2326 0.1761 0.036 Uiso 1 1 calc R . . C26 C 1.1268(3) 0.3276(2) 0.0593(2) 0.0341(7) Uani 1 1 d . A . C27 C 1.1942(3) 0.3973(2) -0.0090(2) 0.0373(7) Uani 1 1 d . . . H27 H 1.1698 0.431 -0.057 0.045 Uiso 1 1 calc R . . C28 C 1.2984(3) 0.4165(2) -0.00510(19) 0.0349(7) Uani 1 1 d . B . C29 C 1.3352(2) 0.3659(2) 0.06425(18) 0.0302(6) Uani 1 1 d . . . H29 H 1.4078 0.3799 0.0644 0.036 Uiso 1 1 calc R . . C30 C 1.0148(3) 0.3049(3) 0.0561(2) 0.0493(9) Uani 1 1 d D . . C31 C 1.3718(3) 0.4945(3) -0.0759(2) 0.0525(9) Uani 1 1 d D . . C32 C 1.4450(2) 0.23647(19) 0.20122(17) 0.0271(6) Uani 1 1 d . . . C33 C 1.4951(3) 0.2481(2) 0.25745(19) 0.0314(6) Uani 1 1 d . . . H33 H 1.4477 0.2665 0.3052 0.038 Uiso 1 1 calc R . . C34 C 1.6127(3) 0.2336(2) 0.2453(2) 0.0357(7) Uani 1 1 d . C . C35 C 1.6841(3) 0.2061(2) 0.1775(2) 0.0388(7) Uani 1 1 d . . . H35 H 1.7641 0.1956 0.1696 0.047 Uiso 1 1 calc R . . C36 C 1.6367(3) 0.1940(2) 0.1208(2) 0.0362(7) Uani 1 1 d . D . C37 C 1.5195(2) 0.2092(2) 0.13269(19) 0.0301(6) Uani 1 1 d . . . H37 H 1.4893 0.2008 0.0928 0.036 Uiso 1 1 calc R . . C38 C 1.6619(3) 0.2494(3) 0.3067(2) 0.0514(9) Uani 1 1 d D . . C39 C 1.7139(3) 0.1664(3) 0.0462(3) 0.0561(10) Uani 1 1 d D . . C40 C 1.2381(2) 0.3087(2) 0.28055(17) 0.0271(6) Uani 1 1 d . . . C41 C 1.1300(2) 0.2869(2) 0.34043(18) 0.0316(6) Uani 1 1 d . . . H41 H 1.0974 0.2266 0.3517 0.038 Uiso 1 1 calc R . . C42 C 1.0687(2) 0.3509(2) 0.38417(19) 0.0338(7) Uani 1 1 d . E . C43 C 1.1132(3) 0.4387(2) 0.37121(19) 0.0355(7) Uani 1 1 d . . . H43 H 1.0716 0.4817 0.4019 0.043 Uiso 1 1 calc R . . C44 C 1.2205(3) 0.4621(2) 0.31190(19) 0.0326(6) Uani 1 1 d . F . C45 C 1.2808(2) 0.3986(2) 0.26768(18) 0.0296(6) Uani 1 1 d . . . H45 H 1.3538 0.4168 0.2271 0.036 Uiso 1 1 calc R . . C46 C 0.9514(3) 0.3230(3) 0.4450(2) 0.0461(8) Uani 1 1 d D . . C47 C 1.2715(3) 0.5570(2) 0.2944(2) 0.0440(8) Uani 1 1 d D . . C48 C 1.2702(2) 0.1266(2) 0.26253(18) 0.0286(6) Uani 1 1 d . . . C49 C 1.2536(3) 0.0705(2) 0.2176(2) 0.0337(6) Uani 1 1 d . . . H49 H 1.2551 0.1014 0.1605 0.04 Uiso 1 1 calc R . . C50 C 1.2347(3) -0.0292(2) 0.2531(2) 0.0393(7) Uani 1 1 d . G . C51 C 1.2368(3) -0.0782(2) 0.3344(2) 0.0437(8) Uani 1 1 d . . . H51 H 1.225 -0.1464 0.3585 0.052 Uiso 1 1 calc R . . C52 C 1.2567(3) -0.0251(2) 0.3799(2) 0.0408(7) Uani 1 1 d . H . C53 C 1.2704(3) 0.0755(2) 0.34525(19) 0.0346(7) Uani 1 1 d . . . H53 H 1.2802 0.1105 0.379 0.042 Uiso 1 1 calc R . . C54 C 1.2154(4) -0.0845(3) 0.2013(3) 0.0587(10) Uani 1 1 d D . . C55 C 1.2652(4) -0.0761(3) 0.4666(3) 0.0606(11) Uani 1 1 d D . . F1 F 1.0257(11) 0.2972(10) -0.0191(6) 0.071(3) Uani 0.55(5) 1 d PD A 1 F2 F 0.9359(13) 0.3744(12) 0.0656(11) 0.088(4) Uani 0.55(5) 1 d PD A 1 F3 F 0.9735(13) 0.2243(11) 0.1117(11) 0.110(6) Uani 0.55(5) 1 d PD A 1 F4 F 1.4812(12) 0.4673(18) -0.0973(17) 0.079(5) Uani 0.49(7) 1 d PD B 1 F5 F 1.370(2) 0.5745(14) -0.0553(17) 0.083(5) Uani 0.49(7) 1 d PD B 1 F6 F 1.342(2) 0.524(2) -0.1454(12) 0.104(7) Uani 0.49(7) 1 d PD B 1 F7 F 1.5870(4) 0.2593(11) 0.3775(5) 0.106(4) Uani 0.662(16) 1 d PD C 1 F8 F 1.7211(9) 0.3330(5) 0.2730(5) 0.090(3) Uani 0.662(16) 1 d PD C 1 F9 F 1.7385(7) 0.1852(4) 0.3282(5) 0.080(3) Uani 0.662(16) 1 d PD C 1 F10 F 1.7960(3) 0.1012(3) 0.0642(2) 0.1087(12) Uani 1 1 d D D 1 F11 F 1.6613(2) 0.1249(3) 0.0141(2) 0.1042(12) Uani 1 1 d D D 1 F12 F 1.7705(3) 0.2397(3) -0.0138(2) 0.1306(16) Uani 1 1 d D D 1 F13 F 0.95178(19) 0.23802(18) 0.50399(15) 0.0745(8) Uani 1 1 d D E 1 F14 F 0.87942(17) 0.31565(18) 0.40510(15) 0.0619(6) Uani 1 1 d D E 1 F15 F 0.90119(18) 0.38857(19) 0.48470(15) 0.0678(7) Uani 1 1 d D E 1 F16 F 1.2228(18) 0.6038(13) 0.3484(12) 0.125(6) Uani 0.50(3) 1 d PD F 1 F17 F 1.3795(10) 0.5429(10) 0.2935(13) 0.094(4) Uani 0.50(3) 1 d PD F 1 F18 F 1.2779(14) 0.6171(9) 0.2189(7) 0.084(4) Uani 0.50(3) 1 d PD F 1 F19 F 1.1483(10) -0.0341(10) 0.1554(8) 0.065(3) Uani 0.56(2) 1 d PD G 1 F20 F 1.3181(7) -0.0794(11) 0.1336(7) 0.099(4) Uani 0.56(2) 1 d PD G 1 F21 F 1.189(2) -0.1700(6) 0.2348(9) 0.167(8) Uani 0.56(2) 1 d PD G 1 F22 F 1.3022(17) -0.1684(7) 0.4780(10) 0.059(4) Uani 0.50(6) 1 d PD H 1 F23 F 1.327(3) -0.0310(13) 0.4881(14) 0.125(8) Uani 0.50(6) 1 d PD H 1 F24 F 1.1592(15) -0.0784(17) 0.5200(16) 0.105(6) Uani 0.50(6) 1 d PD H 1 F1A F 1.010(2) 0.3172(18) -0.0203(7) 0.097(6) Uani 0.45(5) 1 d PD A 2 F2A F 0.9290(12) 0.3582(16) 0.090(2) 0.118(7) Uani 0.45(5) 1 d PD A 2 F3A F 0.9843(15) 0.2131(7) 0.0991(10) 0.067(4) Uani 0.45(5) 1 d PD A 2 F4A F 1.4821(11) 0.480(2) -0.0858(14) 0.069(4) Uani 0.51(7) 1 d PD B 2 F5A F 1.344(3) 0.5796(12) -0.0638(19) 0.111(7) Uani 0.51(7) 1 d PD B 2 F6A F 1.360(2) 0.503(3) -0.1499(9) 0.089(5) Uani 0.51(7) 1 d PD B 2 F7A F 1.624(2) 0.1791(12) 0.3782(8) 0.116(9) Uani 0.338(16) 1 d PD C 2 F8A F 1.633(2) 0.3284(9) 0.3195(13) 0.105(8) Uani 0.338(16) 1 d PD C 2 F9A F 1.7728(8) 0.237(3) 0.2817(14) 0.171(13) Uani 0.338(16) 1 d PD C 2 F16A F 1.1944(8) 0.6183(8) 0.3253(9) 0.071(3) Uani 0.50(3) 1 d PD F 2 F17A F 1.3544(15) 0.5516(10) 0.3250(15) 0.118(6) Uani 0.50(3) 1 d PD F 2 F18A F 1.3093(17) 0.6045(10) 0.2138(5) 0.105(6) Uani 0.50(3) 1 d PD F 2 F19A F 1.1795(17) -0.0365(12) 0.1388(11) 0.082(5) Uani 0.44(2) 1 d PD G 2 F20A F 1.3016(6) -0.1443(12) 0.1784(12) 0.091(5) Uani 0.44(2) 1 d PD G 2 F21A F 1.1310(7) -0.1531(6) 0.2534(6) 0.058(3) Uani 0.44(2) 1 d PD G 2 F22A F 1.2846(19) -0.1703(8) 0.4807(12) 0.084(6) Uani 0.50(6) 1 d PD H 2 F23A F 1.3532(12) -0.0431(11) 0.4789(10) 0.066(4) Uani 0.50(6) 1 d PD H 2 F24A F 1.1746(11) -0.0682(15) 0.5308(11) 0.071(3) Uani 0.50(6) 1 d PD H 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0395(3) 0.0409(3) 0.0421(3) -0.0138(2) -0.0120(2) 0.0059(2) O 0.0640(17) 0.084(2) 0.0496(16) -0.0306(15) -0.0297(14) 0.0182(15) N1 0.0343(14) 0.0391(14) 0.0370(15) -0.0188(11) -0.0134(11) 0.0076(11) N2 0.058(2) 0.0410(17) 0.053(2) -0.0203(14) -0.0285(16) 0.0138(15) C1 0.0328(16) 0.0479(19) 0.048(2) -0.0256(16) -0.0147(15) 0.0041(14) C2 0.0320(17) 0.071(2) 0.045(2) -0.0276(18) -0.0132(15) 0.0151(16) C3 0.053(2) 0.058(2) 0.0389(19) -0.0237(17) -0.0265(17) 0.0259(17) C4 0.0412(19) 0.058(2) 0.049(2) -0.0195(18) -0.0068(16) -0.0090(16) C5 0.076(3) 0.077(3) 0.051(2) -0.037(2) -0.029(2) 0.041(2) C6 0.0354(16) 0.0329(16) 0.0433(19) -0.0143(14) -0.0085(14) 0.0056(13) C7 0.0391(17) 0.0305(16) 0.046(2) -0.0099(14) -0.0121(14) 0.0029(13) C8 0.0427(18) 0.0359(18) 0.054(2) -0.0099(15) -0.0139(16) 0.0075(14) C9 0.048(2) 0.0372(19) 0.058(2) -0.0126(17) -0.0047(18) 0.0143(15) C10 0.061(2) 0.042(2) 0.052(2) -0.0232(17) -0.0073(18) 0.0083(17) C11 0.0471(19) 0.0425(19) 0.050(2) -0.0233(16) -0.0118(16) 0.0052(15) C12 0.054(2) 0.044(2) 0.063(2) -0.0250(18) -0.0332(19) 0.0154(16) C13 0.080(3) 0.085(3) 0.115(4) -0.050(3) -0.049(3) -0.004(3) C14 0.080(3) 0.076(3) 0.053(3) -0.030(2) -0.026(2) 0.015(2) C15 0.064(2) 0.064(3) 0.073(3) -0.046(2) -0.028(2) 0.016(2) C16 0.073(3) 0.092(4) 0.102(4) -0.063(3) -0.031(3) 0.001(3) C17 0.108(4) 0.083(3) 0.067(3) -0.044(3) -0.041(3) 0.018(3) C18 0.058(3) 0.053(3) 0.108(4) -0.005(3) -0.020(3) -0.005(2) C19 0.049(2) 0.099(4) 0.084(3) -0.035(3) -0.019(2) -0.014(2) C20 0.031(2) 0.064(3) 0.106(4) 0.020(3) -0.001(2) 0.0013(19) C21 0.059(3) 0.112(5) 0.115(5) -0.075(4) 0.035(3) -0.035(3) C22 0.067(3) 0.142(6) 0.051(3) 0.011(3) -0.011(2) -0.042(4) C23 0.048(2) 0.054(2) 0.0373(19) -0.0188(16) -0.0113(16) 0.0137(16) B 0.0272(15) 0.0254(15) 0.0248(16) -0.0049(12) -0.0087(12) -0.0007(12) C24 0.0299(14) 0.0251(14) 0.0247(14) -0.0080(11) -0.0088(11) 0.0020(11) C25 0.0280(14) 0.0286(14) 0.0305(16) -0.0066(12) -0.0085(12) 0.0000(11) C26 0.0332(15) 0.0347(16) 0.0381(17) -0.0113(13) -0.0172(13) 0.0028(12) C27 0.0478(18) 0.0321(16) 0.0342(17) -0.0063(13) -0.0223(14) 0.0052(13) C28 0.0437(17) 0.0273(15) 0.0302(16) -0.0025(12) -0.0134(13) -0.0011(12) C29 0.0310(14) 0.0278(14) 0.0289(15) -0.0053(12) -0.0085(12) -0.0026(11) C30 0.0412(19) 0.054(2) 0.056(2) -0.0106(19) -0.0267(18) 0.0007(17) C31 0.064(3) 0.044(2) 0.041(2) 0.0035(16) -0.0189(19) -0.0103(18) C32 0.0290(14) 0.0238(13) 0.0250(14) -0.0024(11) -0.0091(11) -0.0016(11) C33 0.0348(15) 0.0289(15) 0.0284(15) -0.0043(12) -0.0129(12) 0.0014(12) C34 0.0367(16) 0.0305(15) 0.0409(18) -0.0056(13) -0.0198(14) 0.0009(12) C35 0.0287(15) 0.0333(16) 0.052(2) -0.0079(14) -0.0153(14) 0.0013(12) C36 0.0307(15) 0.0322(16) 0.0419(18) -0.0125(13) -0.0060(13) 0.0002(12) C37 0.0311(15) 0.0279(14) 0.0314(16) -0.0090(12) -0.0101(12) -0.0006(11) C38 0.054(2) 0.055(2) 0.054(2) -0.0130(19) -0.0348(19) 0.0037(18) C39 0.0371(19) 0.068(3) 0.062(3) -0.034(2) -0.0023(18) 0.0010(18) C40 0.0265(13) 0.0296(14) 0.0222(14) -0.0033(11) -0.0088(11) -0.0002(11) C41 0.0302(15) 0.0322(15) 0.0288(15) -0.0033(12) -0.0108(12) -0.0017(12) C42 0.0280(15) 0.0413(17) 0.0260(15) -0.0054(12) -0.0070(12) 0.0025(12) C43 0.0346(16) 0.0405(17) 0.0295(16) -0.0128(13) -0.0089(13) 0.0071(13) C44 0.0333(15) 0.0347(16) 0.0294(16) -0.0093(12) -0.0109(12) 0.0014(12) C45 0.0269(14) 0.0318(15) 0.0273(15) -0.0072(12) -0.0069(11) -0.0007(11) C46 0.0333(17) 0.052(2) 0.0395(19) -0.0070(16) -0.0038(14) 0.0027(15) C47 0.0452(19) 0.0406(19) 0.048(2) -0.0212(16) -0.0086(16) -0.0020(15) C48 0.0263(14) 0.0303(15) 0.0268(15) -0.0065(11) -0.0080(11) -0.0006(11) C49 0.0376(16) 0.0328(16) 0.0313(16) -0.0091(12) -0.0135(13) 0.0018(12) C50 0.0459(18) 0.0356(17) 0.0424(19) -0.0155(14) -0.0180(15) -0.0008(14) C51 0.058(2) 0.0300(16) 0.043(2) -0.0071(14) -0.0179(16) -0.0070(14) C52 0.054(2) 0.0320(16) 0.0330(17) -0.0035(13) -0.0148(15) -0.0061(14) C53 0.0449(17) 0.0295(15) 0.0297(16) -0.0065(12) -0.0132(13) -0.0045(13) C54 0.076(3) 0.052(2) 0.063(3) -0.029(2) -0.033(2) 0.005(2) C55 0.106(4) 0.036(2) 0.039(2) -0.0018(17) -0.027(2) -0.014(2) F1 0.063(4) 0.099(5) 0.094(7) -0.065(7) -0.049(4) 0.014(5) F2 0.060(6) 0.110(7) 0.135(7) -0.074(5) -0.067(5) 0.053(5) F3 0.059(6) 0.140(12) 0.105(7) 0.047(7) -0.057(5) -0.058(7) F4 0.066(8) 0.069(6) 0.065(8) -0.002(5) 0.016(6) -0.020(5) F5 0.121(10) 0.045(7) 0.079(7) -0.003(5) -0.030(8) -0.037(5) F6 0.132(12) 0.104(10) 0.063(10) 0.052(7) -0.066(10) -0.069(9) F7 0.060(3) 0.219(13) 0.078(4) -0.091(6) -0.033(3) 0.011(4) F8 0.133(7) 0.071(4) 0.096(5) -0.008(3) -0.079(5) -0.033(4) F9 0.106(6) 0.067(3) 0.105(5) -0.036(3) -0.088(5) 0.040(3) F10 0.0752(19) 0.138(3) 0.120(3) -0.079(2) -0.0242(18) 0.0569(19) F11 0.0647(17) 0.179(3) 0.102(2) -0.110(3) -0.0055(16) 0.0055(19) F12 0.145(3) 0.100(2) 0.079(2) -0.0337(19) 0.065(2) -0.027(2) F13 0.0448(12) 0.0751(16) 0.0539(14) 0.0196(12) 0.0063(10) 0.0003(11) F14 0.0335(10) 0.0808(16) 0.0625(14) -0.0137(12) -0.0091(10) -0.0108(10) F15 0.0427(12) 0.0869(17) 0.0592(15) -0.0326(13) 0.0107(10) 0.0023(11) F16 0.143(11) 0.119(10) 0.104(8) -0.094(8) 0.064(7) -0.078(8) F17 0.056(4) 0.062(5) 0.195(11) -0.064(6) -0.052(6) -0.009(3) F18 0.123(7) 0.041(4) 0.092(8) 0.019(5) -0.071(7) -0.025(4) F19 0.072(4) 0.069(5) 0.081(7) -0.029(4) -0.050(4) -0.009(3) F20 0.117(5) 0.122(8) 0.117(7) -0.094(6) -0.071(5) 0.042(5) F21 0.40(3) 0.026(3) 0.135(11) -0.014(5) -0.165(15) -0.022(10) F22 0.102(7) 0.030(5) 0.051(6) -0.009(5) -0.040(5) 0.014(5) F23 0.30(2) 0.036(5) 0.083(8) 0.006(5) -0.132(12) -0.023(8) F24 0.190(15) 0.075(6) 0.036(6) -0.008(5) -0.024(7) -0.013(7) F1A 0.098(10) 0.129(10) 0.063(7) 0.026(7) -0.061(7) -0.055(8) F2A 0.032(5) 0.141(12) 0.234(19) -0.125(13) -0.048(8) 0.016(6) F3A 0.061(6) 0.045(6) 0.106(9) -0.017(6) -0.046(6) -0.011(4) F4A 0.063(7) 0.074(8) 0.047(5) 0.022(5) -0.020(6) -0.034(5) F5A 0.136(13) 0.026(5) 0.113(14) 0.005(5) 0.012(8) -0.013(6) F6A 0.116(8) 0.108(11) 0.025(5) 0.015(6) -0.019(5) -0.042(7) F7A 0.20(2) 0.108(11) 0.069(8) 0.014(7) -0.101(12) -0.053(11) F8A 0.20(2) 0.064(7) 0.119(15) -0.060(9) -0.130(16) 0.050(10) F9A 0.048(6) 0.38(4) 0.151(18) -0.14(2) -0.053(9) -0.002(13) F16A 0.057(4) 0.044(4) 0.119(7) -0.051(4) -0.016(5) 0.005(3) F17A 0.131(11) 0.052(5) 0.237(15) -0.042(7) -0.148(12) 0.013(5) F18A 0.164(11) 0.062(6) 0.059(6) -0.034(5) 0.041(7) -0.057(6) F19A 0.162(14) 0.049(6) 0.050(5) -0.002(4) -0.053(8) -0.034(7) F20A 0.055(4) 0.106(10) 0.159(12) -0.110(10) -0.033(5) 0.023(5) F21A 0.080(6) 0.044(5) 0.062(4) -0.016(3) -0.027(3) -0.028(3) F22A 0.139(11) 0.046(7) 0.069(8) 0.024(6) -0.060(7) -0.042(8) F23A 0.093(10) 0.053(6) 0.063(5) 0.008(4) -0.053(5) -0.025(4) F24A 0.095(8) 0.086(8) 0.024(4) -0.016(4) -0.013(4) 0.005(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Fe C23 1.774(4) . ? Fe N2 1.938(3) . ? Fe N1 2.006(3) . ? Fe C22 2.066(5) . ? Fe C18 2.076(5) . ? Fe C21 2.082(5) . ? Fe C19 2.116(4) . ? Fe C20 2.118(4) . ? O C23 1.141(4) . ? N1 C1 1.283(4) . ? N1 C6 1.466(4) . ? N2 C3 1.269(5) . ? N2 H2X 0.80(5) . ? C1 C4 1.506(5) . ? C1 C2 1.517(5) . ? C2 C3 1.486(6) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 C5 1.509(5) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 C7 1.402(5) . ? C6 C11 1.405(5) . ? C7 C8 1.404(5) . ? C7 C12 1.527(5) . ? C8 C9 1.376(6) . ? C8 H8 0.95 . ? C9 C10 1.381(6) . ? C9 H9 0.95 . ? C10 C11 1.394(5) . ? C10 H10 0.95 . ? C11 C15 1.528(5) . ? C12 C14 1.508(6) . ? C12 C13 1.532(6) . ? C12 H12 1 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C17 1.530(7) . ? C15 C16 1.532(7) . ? C15 H15 1 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 C22 1.348(9) . ? C18 C19 1.370(7) . ? C18 H18 0.95 . ? C19 C20 1.373(8) . ? C19 H19 0.95 . ? C20 C21 1.390(9) . ? C20 H20 0.95 . ? C21 C22 1.410(9) . ? C21 H21 0.95 . ? C22 H22 0.95 . ? B C40 1.637(4) . ? B C24 1.637(4) . ? B C48 1.641(4) . ? B C32 1.642(4) . ? C24 C29 1.398(4) . ? C24 C25 1.405(4) . ? C25 C26 1.388(4) . ? C25 H25 0.95 . ? C26 C27 1.384(5) . ? C26 C30 1.494(4) . ? C27 C28 1.386(5) . ? C27 H27 0.95 . ? C28 C29 1.388(4) . ? C28 C31 1.498(5) . ? C29 H29 0.95 . ? C30 F3 1.288(9) . ? C30 F2A 1.317(11) . ? C30 F2 1.318(9) . ? C30 F1A 1.319(11) . ? C30 F3A 1.331(10) . ? C30 F1 1.331(8) . ? C31 F5A 1.309(11) . ? C31 F4A 1.313(11) . ? C31 F6 1.314(12) . ? C31 F4 1.319(12) . ? C31 F6A 1.330(11) . ? C31 F5 1.330(11) . ? C32 C37 1.394(4) . ? C32 C33 1.400(4) . ? C33 C34 1.394(4) . ? C33 H33 0.95 . ? C34 C35 1.375(5) . ? C34 C38 1.501(5) . ? C35 C36 1.387(5) . ? C35 H35 0.95 . ? C36 C37 1.391(4) . ? C36 C39 1.488(5) . ? C37 H37 0.95 . ? C38 F8A 1.229(8) . ? C38 F9 1.293(5) . ? C38 F9A 1.300(10) . ? C38 F7A 1.314(9) . ? C38 F7 1.322(6) . ? C38 F8 1.357(6) . ? C39 F12 1.304(5) . ? C39 F11 1.305(5) . ? C39 F10 1.334(5) . ? C40 C41 1.396(4) . ? C40 C45 1.399(4) . ? C41 C42 1.393(4) . ? C41 H41 0.95 . ? C42 C43 1.381(5) . ? C42 C46 1.499(4) . ? C43 C44 1.388(4) . ? C43 H43 0.95 . ? C44 C45 1.389(4) . ? C44 C47 1.494(4) . ? C45 H45 0.95 . ? C46 F13 1.322(4) . ? C46 F15 1.336(4) . ? C46 F14 1.343(4) . ? C47 F17A 1.293(9) . ? C47 F16 1.295(9) . ? C47 F18A 1.305(9) . ? C47 F18 1.308(9) . ? C47 F17 1.319(9) . ? C47 F16A 1.321(8) . ? C48 C49 1.393(4) . ? C48 C53 1.399(4) . ? C49 C50 1.393(4) . ? C49 H49 0.95 . ? C50 C51 1.379(5) . ? C50 C54 1.499(5) . ? C51 C52 1.384(5) . ? C51 H51 0.95 . ? C52 C53 1.395(4) . ? C52 C55 1.492(5) . ? C53 H53 0.95 . ? C54 F21 1.223(9) . ? C54 F19A 1.277(12) . ? C54 F20A 1.322(8) . ? C54 F19 1.330(9) . ? C54 F21A 1.401(8) . ? C54 F20 1.412(9) . ? C55 F23 1.294(11) . ? C55 F22A 1.312(11) . ? C55 F24A 1.324(11) . ? C55 F22 1.330(9) . ? C55 F24 1.330(11) . ? C55 F23A 1.357(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23 Fe N2 95.36(15) . . ? C23 Fe N1 92.36(15) . . ? N2 Fe N1 87.42(13) . . ? C23 Fe C22 86.8(2) . . ? N2 Fe C22 124.9(3) . . ? N1 Fe C22 147.6(3) . . ? C23 Fe C18 111.3(2) . . ? N2 Fe C18 92.8(2) . . ? N1 Fe C18 156.19(18) . . ? C22 Fe C18 38.0(2) . . ? C23 Fe C21 100.5(2) . . ? N2 Fe C21 156.30(19) . . ? N1 Fe C21 109.3(2) . . ? C22 Fe C21 39.7(3) . . ? C18 Fe C21 65.0(2) . . ? C23 Fe C19 148.7(2) . . ? N2 Fe C19 93.06(18) . . ? N1 Fe C19 118.08(17) . . ? C22 Fe C19 63.9(2) . . ? C18 Fe C19 38.1(2) . . ? C21 Fe C19 64.5(2) . . ? C23 Fe C20 138.6(2) . . ? N2 Fe C20 125.2(2) . . ? N1 Fe C20 96.79(14) . . ? C22 Fe C20 64.6(2) . . ? C18 Fe C20 63.86(19) . . ? C21 Fe C20 38.6(2) . . ? C19 Fe C20 37.8(2) . . ? C1 N1 C6 117.9(3) . . ? C1 N1 Fe 124.8(2) . . ? C6 N1 Fe 117.0(2) . . ? C3 N2 Fe 128.3(3) . . ? C3 N2 H2X 116(4) . . ? Fe N2 H2X 116(4) . . ? N1 C1 C4 125.0(3) . . ? N1 C1 C2 120.1(3) . . ? C4 C1 C2 114.8(3) . . ? C3 C2 C1 115.9(3) . . ? C3 C2 H2A 108.3 . . ? C1 C2 H2A 108.3 . . ? C3 C2 H2B 108.3 . . ? C1 C2 H2B 108.3 . . ? H2A C2 H2B 107.4 . . ? N2 C3 C2 119.3(3) . . ? N2 C3 C5 122.3(4) . . ? C2 C3 C5 118.3(4) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 123.0(3) . . ? C7 C6 N1 119.2(3) . . ? C11 C6 N1 117.7(3) . . ? C6 C7 C8 117.0(3) . . ? C6 C7 C12 123.5(3) . . ? C8 C7 C12 119.3(3) . . ? C9 C8 C7 120.9(3) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 120.7(3) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C9 C10 C11 121.2(4) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C6 117.0(3) . . ? C10 C11 C15 119.2(3) . . ? C6 C11 C15 123.6(3) . . ? C14 C12 C7 110.6(3) . . ? C14 C12 C13 109.4(4) . . ? C7 C12 C13 112.6(3) . . ? C14 C12 H12 108 . . ? C7 C12 H12 108 . . ? C13 C12 H12 108 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C17 112.4(4) . . ? C11 C15 C16 110.4(4) . . ? C17 C15 C16 110.7(4) . . ? C11 C15 H15 107.7 . . ? C17 C15 H15 107.7 . . ? C16 C15 H15 107.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C22 C18 C19 109.2(5) . . ? C22 C18 Fe 70.6(3) . . ? C19 C18 Fe 72.5(3) . . ? C22 C18 H18 125.4 . . ? C19 C18 H18 125.4 . . ? Fe C18 H18 123.1 . . ? C18 C19 C20 108.0(5) . . ? C18 C19 Fe 69.4(3) . . ? C20 C19 Fe 71.2(3) . . ? C18 C19 H19 126 . . ? C20 C19 H19 126 . . ? Fe C19 H19 125.1 . . ? C19 C20 C21 108.4(5) . . ? C19 C20 Fe 71.0(2) . . ? C21 C20 Fe 69.3(3) . . ? C19 C20 H20 125.8 . . ? C21 C20 H20 125.8 . . ? Fe C20 H20 125.5 . . ? C20 C21 C22 106.1(5) . . ? C20 C21 Fe 72.1(3) . . ? C22 C21 Fe 69.5(3) . . ? C20 C21 H21 127 . . ? C22 C21 H21 127 . . ? Fe C21 H21 123.2 . . ? C18 C22 C21 108.3(5) . . ? C18 C22 Fe 71.4(3) . . ? C21 C22 Fe 70.8(3) . . ? C18 C22 H22 125.9 . . ? C21 C22 H22 125.9 . . ? Fe C22 H22 123.6 . . ? O C23 Fe 175.1(4) . . ? C40 B C24 102.9(2) . . ? C40 B C48 113.3(2) . . ? C24 B C48 112.4(2) . . ? C40 B C32 112.7(2) . . ? C24 B C32 112.4(2) . . ? C48 B C32 103.4(2) . . ? C29 C24 C25 115.6(3) . . ? C29 C24 B 123.0(2) . . ? C25 C24 B 121.1(2) . . ? C26 C25 C24 122.2(3) . . ? C26 C25 H25 118.9 . . ? C24 C25 H25 118.9 . . ? C27 C26 C25 121.0(3) . . ? C27 C26 C30 118.8(3) . . ? C25 C26 C30 120.2(3) . . ? C26 C27 C28 117.9(3) . . ? C26 C27 H27 121.1 . . ? C28 C27 H27 121.1 . . ? C27 C28 C29 121.1(3) . . ? C27 C28 C31 119.7(3) . . ? C29 C28 C31 119.2(3) . . ? C28 C29 C24 122.2(3) . . ? C28 C29 H29 118.9 . . ? C24 C29 H29 118.9 . . ? F3 C30 F2 107.9(9) . . ? F2A C30 F1A 106.0(9) . . ? F2A C30 F3A 104.7(10) . . ? F2 C30 F3A 117.8(12) . . ? F1A C30 F3A 104.2(8) . . ? F3 C30 F1 106.8(9) . . ? F2 C30 F1 104.9(7) . . ? F3 C30 C26 113.2(6) . . ? F2A C30 C26 112.2(8) . . ? F2 C30 C26 112.7(8) . . ? F1A C30 C26 115.2(9) . . ? F3A C30 C26 113.5(8) . . ? F1 C30 C26 111.0(6) . . ? F5A C31 F4A 106.5(12) . . ? F6 C31 F4 106.7(11) . . ? F5A C31 F6A 107.1(11) . . ? F4A C31 F6A 106.0(10) . . ? F6 C31 F5 105.6(11) . . ? F4 C31 F5 104.2(11) . . ? F5A C31 C28 111.0(12) . . ? F4A C31 C28 114.1(9) . . ? F6 C31 C28 114.4(11) . . ? F4 C31 C28 112.5(11) . . ? F6A C31 C28 111.7(11) . . ? F5 C31 C28 112.6(13) . . ? C37 C32 C33 116.1(3) . . ? C37 C32 B 121.1(2) . . ? C33 C32 B 122.4(3) . . ? C34 C33 C32 121.8(3) . . ? C34 C33 H33 119.1 . . ? C32 C33 H33 119.1 . . ? C35 C34 C33 120.9(3) . . ? C35 C34 C38 119.7(3) . . ? C33 C34 C38 119.4(3) . . ? C34 C35 C36 118.5(3) . . ? C34 C35 H35 120.8 . . ? C36 C35 H35 120.8 . . ? C35 C36 C37 120.6(3) . . ? C35 C36 C39 118.8(3) . . ? C37 C36 C39 120.7(3) . . ? C36 C37 C32 122.2(3) . . ? C36 C37 H37 118.9 . . ? C32 C37 H37 118.9 . . ? F8A C38 F9A 111.8(10) . . ? F8A C38 F7A 109.0(9) . . ? F9A C38 F7A 105.8(9) . . ? F9 C38 F7 106.7(5) . . ? F9 C38 F8 101.8(5) . . ? F7 C38 F8 103.2(5) . . ? F8A C38 C34 113.6(5) . . ? F9 C38 C34 115.5(4) . . ? F9A C38 C34 109.6(7) . . ? F7A C38 C34 106.4(5) . . ? F7 C38 C34 116.2(3) . . ? F8 C38 C34 111.8(4) . . ? F12 C39 F11 108.8(4) . . ? F12 C39 F10 103.8(4) . . ? F11 C39 F10 103.8(4) . . ? F12 C39 C36 113.0(3) . . ? F11 C39 C36 113.6(3) . . ? F10 C39 C36 113.1(4) . . ? C41 C40 C45 115.8(3) . . ? C41 C40 B 123.0(3) . . ? C45 C40 B 120.8(2) . . ? C42 C41 C40 121.9(3) . . ? C42 C41 H41 119.1 . . ? C40 C41 H41 119.1 . . ? C43 C42 C41 121.3(3) . . ? C43 C42 C46 120.5(3) . . ? C41 C42 C46 118.2(3) . . ? C42 C43 C44 117.9(3) . . ? C42 C43 H43 121.1 . . ? C44 C43 H43 121.1 . . ? C43 C44 C45 120.6(3) . . ? C43 C44 C47 120.0(3) . . ? C45 C44 C47 119.4(3) . . ? C44 C45 C40 122.5(3) . . ? C44 C45 H45 118.7 . . ? C40 C45 H45 118.7 . . ? F13 C46 F15 107.2(3) . . ? F13 C46 F14 106.7(3) . . ? F15 C46 F14 105.1(3) . . ? F13 C46 C42 112.8(3) . . ? F15 C46 C42 113.2(3) . . ? F14 C46 C42 111.3(3) . . ? F17A C47 F18A 107.0(9) . . ? F16 C47 F18 107.8(9) . . ? F16 C47 F17 105.4(9) . . ? F18 C47 F17 103.6(8) . . ? F17A C47 F16A 105.4(9) . . ? F18A C47 F16A 103.3(7) . . ? F17A C47 C44 115.5(7) . . ? F16 C47 C44 116.1(7) . . ? F18A C47 C44 112.8(7) . . ? F18 C47 C44 112.8(6) . . ? F17 C47 C44 110.1(6) . . ? F16A C47 C44 111.8(6) . . ? C49 C48 C53 115.5(3) . . ? C49 C48 B 123.7(3) . . ? C53 C48 B 120.3(3) . . ? C48 C49 C50 122.5(3) . . ? C48 C49 H49 118.8 . . ? C50 C49 H49 118.8 . . ? C51 C50 C49 121.0(3) . . ? C51 C50 C54 119.5(3) . . ? C49 C50 C54 119.5(3) . . ? C50 C51 C52 117.9(3) . . ? C50 C51 H51 121 . . ? C52 C51 H51 121 . . ? C51 C52 C53 120.8(3) . . ? C51 C52 C55 119.6(3) . . ? C53 C52 C55 119.6(3) . . ? C52 C53 C48 122.3(3) . . ? C52 C53 H53 118.9 . . ? C48 C53 H53 118.9 . . ? F19A C54 F20A 110.3(10) . . ? F21 C54 F19 111.7(9) . . ? F19A C54 F21A 104.5(9) . . ? F20A C54 F21A 99.3(7) . . ? F21 C54 F20 108.2(8) . . ? F19 C54 F20 97.3(7) . . ? F21 C54 C50 119.3(6) . . ? F19A C54 C50 117.8(10) . . ? F20A C54 C50 114.2(5) . . ? F19 C54 C50 111.6(8) . . ? F21A C54 C50 108.7(5) . . ? F20 C54 C50 106.2(5) . . ? F22A C55 F24A 104.8(10) . . ? F23 C55 F22 109.6(10) . . ? F23 C55 F24 107.3(9) . . ? F22 C55 F24 106.3(9) . . ? F22A C55 F23A 105.9(9) . . ? F24A C55 F23A 104.5(9) . . ? F23 C55 C52 113.1(8) . . ? F22A C55 C52 112.3(9) . . ? F24A C55 C52 116.7(9) . . ? F22 C55 C52 113.3(7) . . ? F24 C55 C52 106.7(13) . . ? F23A C55 C52 111.7(7) . . ? #===END data_(6)-may2107 _database_code_depnum_ccdc_archive 'CCDC 675705' _audit_creation_date 2007-05-23T15:09:52-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C35 H46 Fe N2 O, C32 H12 B F24' _chemical_formula_sum 'C67 H58 B F24 Fe N2 O' _chemical_formula_weight 1429.81 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.7562(1) _cell_length_b 18.5982(2) _cell_length_c 35.9837(5) _cell_angle_alpha 90 _cell_angle_beta 90.882(1) _cell_angle_gamma 90 _cell_volume 6528.39(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 43909 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2916 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.344 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8414 _exptl_absorpt_correction_T_max 0.9899 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.999544E-1 _diffrn_orient_matrix_ub_12 -0.21797E-2 _diffrn_orient_matrix_ub_13 0.56471E-2 _diffrn_orient_matrix_ub_21 0.129476E-1 _diffrn_orient_matrix_ub_22 0.380192E-1 _diffrn_orient_matrix_ub_23 0.193892E-1 _diffrn_orient_matrix_ub_31 -0.187081E-1 _diffrn_orient_matrix_ub_32 0.379586E-1 _diffrn_orient_matrix_ub_33 -0.190959E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_unetI/netI 0.0597 _diffrn_reflns_number 47302 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 3.4 _diffrn_reflns_theta_max 26.02 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.975 _diffrn_measured_fraction_theta_max 0.975 _reflns_number_total 12517 _reflns_number_gt 8695 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; For the two disordered CF3 groups the F atoms were left isotropic. 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^)+(0.0946P)^2^+15.9606P] 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_number_reflns 12517 _refine_ls_number_parameters 871 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1132 _refine_ls_R_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.2095 _refine_ls_wR_factor_gt 0.1842 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.452 _refine_diff_density_min -0.809 _refine_diff_density_rms 0.085 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Fe Fe 0.48456(5) 0.77238(3) 0.861486(15) 0.02561(17) Uani 1 1 d . . . F4 F 0.6777(3) 0.42581(17) 0.82219(11) 0.0708(10) Uani 1 1 d . . . F5 F 0.8266(3) 0.50720(16) 0.81626(11) 0.0746(11) Uani 1 1 d . . . F6 F 0.7753(4) 0.46750(19) 0.86916(9) 0.0841(12) Uani 1 1 d . . . F10 F 1.3831(4) 0.05626(17) 0.98215(9) 0.0684(9) Uani 1 1 d . . . F11 F 1.5378(3) 0.04462(17) 0.94210(10) 0.0705(10) Uani 1 1 d . . . F12 F 1.3384(4) 0.00449(16) 0.93035(12) 0.0884(13) Uani 1 1 d . . . F13 F 0.5438(3) 0.12090(15) 0.84941(8) 0.0516(7) Uani 1 1 d . . . F14 F 0.5815(3) 0.00896(16) 0.85807(9) 0.0570(8) Uani 1 1 d . . . F15 F 0.5742(3) 0.05145(17) 0.80290(8) 0.0561(8) Uani 1 1 d . . . F16 F 1.0477(5) -0.0683(2) 0.79777(15) 0.1208(19) Uani 1 1 d . . . F17 F 1.1162(5) 0.0196(2) 0.76894(11) 0.1122(17) Uani 1 1 d . . . F18 F 1.2113(4) -0.0094(3) 0.81840(12) 0.1145(19) Uani 1 1 d . . . F19 F 0.8195(5) 0.06108(17) 0.99042(10) 0.0930(14) Uani 1 1 d . . . F20 F 0.8393(3) 0.12287(18) 1.04046(8) 0.0636(9) Uani 1 1 d . . . F21 F 0.6588(3) 0.12874(19) 1.00848(9) 0.0686(9) Uani 1 1 d . . . F22 F 0.9539(5) 0.37675(18) 1.03540(9) 0.0842(12) Uani 1 1 d . . . F23 F 0.8178(3) 0.41903(17) 0.99484(12) 0.0806(11) Uani 1 1 d . . . F24 F 1.0318(4) 0.41969(17) 0.98555(10) 0.0753(11) Uani 1 1 d . . . O O 0.6228(3) 0.87257(17) 0.81235(9) 0.0447(8) Uani 1 1 d . . . N1 N 0.4731(3) 0.69250(17) 0.82318(9) 0.0266(7) Uani 1 1 d . . . N2 N 0.6582(3) 0.72810(17) 0.88243(9) 0.0245(7) Uani 1 1 d . . . C1 C 0.5791(4) 0.6649(2) 0.80792(11) 0.0267(8) Uani 1 1 d . . . C2 C 0.7202(4) 0.6856(2) 0.82144(11) 0.0292(9) Uani 1 1 d . . . H2 H 0.7923 0.6935 0.8045 0.035 Uiso 1 1 calc R . . C3 C 0.7436(4) 0.6934(2) 0.86260(11) 0.0254(8) Uani 1 1 d . . . C4 C 0.5768(4) 0.6162(2) 0.77468(12) 0.0387(10) Uani 1 1 d . . . H4A H 0.4821 0.6016 0.7691 0.058 Uiso 1 1 calc R . . H4B H 0.6325 0.5735 0.78 0.058 Uiso 1 1 calc R . . H4C H 0.6141 0.6417 0.7533 0.058 Uiso 1 1 calc R . . C5 C 0.8748(4) 0.6599(2) 0.87681(12) 0.0355(10) Uani 1 1 d . . . H5A H 0.8925 0.6756 0.9024 0.053 Uiso 1 1 calc R . . H5B H 0.9508 0.6749 0.8611 0.053 Uiso 1 1 calc R . . H5C H 0.8664 0.6074 0.8761 0.053 Uiso 1 1 calc R . . C6 C 0.3396(4) 0.6740(2) 0.80667(12) 0.0321(9) Uani 1 1 d . . . C7 C 0.2941(4) 0.7132(2) 0.77535(12) 0.0374(10) Uani 1 1 d . . . C8 C 0.1639(5) 0.6959(3) 0.76059(14) 0.0507(13) Uani 1 1 d . . . H8 H 0.1293 0.7219 0.7397 0.061 Uiso 1 1 calc R . . C9 C 0.0856(5) 0.6421(3) 0.77584(16) 0.0564(15) Uani 1 1 d . . . H9 H -0.0025 0.6315 0.7656 0.068 Uiso 1 1 calc R . . C10 C 0.1348(5) 0.6039(3) 0.80562(15) 0.0492(13) Uani 1 1 d . . . H10 H 0.0805 0.5661 0.8153 0.059 Uiso 1 1 calc R . . C11 C 0.2624(4) 0.6185(2) 0.82252(13) 0.0369(10) Uani 1 1 d . . . C12 C 0.3781(5) 0.7701(2) 0.75599(12) 0.0400(11) Uani 1 1 d . . . H12 H 0.4718 0.7697 0.7676 0.048 Uiso 1 1 calc R . . C13 C 0.3183(6) 0.8458(3) 0.76142(14) 0.0553(14) Uani 1 1 d . . . H13A H 0.2251 0.8476 0.7509 0.083 Uiso 1 1 calc R . . H13B H 0.3758 0.8811 0.7488 0.083 Uiso 1 1 calc R . . H13C H 0.3159 0.857 0.788 0.083 Uiso 1 1 calc R . . C14 C 0.3940(6) 0.7543(3) 0.71467(14) 0.0536(13) Uani 1 1 d . . . H14A H 0.4315 0.7059 0.7115 0.08 Uiso 1 1 calc R . . H14B H 0.4564 0.7896 0.7038 0.08 Uiso 1 1 calc R . . H14C H 0.3043 0.7574 0.7021 0.08 Uiso 1 1 calc R . . C15 C 0.3157(4) 0.5724(3) 0.85397(14) 0.0426(11) Uani 1 1 d . . . H15 H 0.3833 0.6018 0.8686 0.051 Uiso 1 1 calc R . . C16 C 0.2035(5) 0.5475(3) 0.88083(16) 0.0557(13) Uani 1 1 d . . . H16A H 0.1518 0.5893 0.8895 0.083 Uiso 1 1 calc R . . H16B H 0.2462 0.5231 0.9022 0.083 Uiso 1 1 calc R . . H16C H 0.1412 0.5142 0.8679 0.083 Uiso 1 1 calc R . . C17 C 0.3905(7) 0.5063(3) 0.8398(2) 0.0718(18) Uani 1 1 d . . . H17A H 0.3268 0.4765 0.8251 0.108 Uiso 1 1 calc R . . H17B H 0.4262 0.4784 0.8609 0.108 Uiso 1 1 calc R . . H17C H 0.4667 0.5213 0.8241 0.108 Uiso 1 1 calc R . . C18 C 0.6935(4) 0.7372(2) 0.92184(11) 0.0275(9) Uani 1 1 d . . . C19 C 0.7587(4) 0.8015(2) 0.93289(11) 0.0310(9) Uani 1 1 d . . . C20 C 0.7891(4) 0.8098(2) 0.97069(12) 0.0355(10) Uani 1 1 d . . . H20 H 0.8325 0.8526 0.9791 0.043 Uiso 1 1 calc R . . C21 C 0.7574(5) 0.7571(3) 0.99607(12) 0.0381(10) Uani 1 1 d . . . H21 H 0.779 0.764 1.0217 0.046 Uiso 1 1 calc R . . C22 C 0.6946(5) 0.6945(3) 0.98454(12) 0.0386(10) Uani 1 1 d . . . H22 H 0.6736 0.6586 1.0023 0.046 Uiso 1 1 calc R . . C23 C 0.6612(4) 0.6831(2) 0.94700(11) 0.0326(9) Uani 1 1 d . . . C24 C 0.7988(4) 0.8604(2) 0.90565(12) 0.0349(10) Uani 1 1 d . . . H24 H 0.7256 0.8623 0.8859 0.042 Uiso 1 1 calc R . . C25 C 0.9341(5) 0.8446(3) 0.88626(15) 0.0511(13) Uani 1 1 d . . . H25A H 1.0069 0.8375 0.905 0.077 Uiso 1 1 calc R . . H25B H 0.9578 0.8852 0.8702 0.077 Uiso 1 1 calc R . . H25C H 0.9242 0.801 0.8712 0.077 Uiso 1 1 calc R . . C26 C 0.8074(5) 0.9350(2) 0.92303(15) 0.0482(12) Uani 1 1 d . . . H26A H 0.7222 0.9453 0.9361 0.072 Uiso 1 1 calc R . . H26B H 0.8209 0.9709 0.9035 0.072 Uiso 1 1 calc R . . H26C H 0.8847 0.9367 0.9407 0.072 Uiso 1 1 calc R . . C27 C 0.5960(5) 0.6113(3) 0.93610(13) 0.0437(11) Uani 1 1 d . . . H27 H 0.5783 0.6118 0.9087 0.052 Uiso 1 1 calc R . . C28 C 0.4595(6) 0.5989(3) 0.95532(17) 0.0630(15) Uani 1 1 d . . . H28A H 0.4732 0.6019 0.9823 0.095 Uiso 1 1 calc R . . H28B H 0.4241 0.5512 0.9487 0.095 Uiso 1 1 calc R . . H28C H 0.3936 0.6357 0.9473 0.095 Uiso 1 1 calc R . . C29 C 0.6918(6) 0.5482(3) 0.94500(15) 0.0545(13) Uani 1 1 d . . . H29A H 0.7813 0.5569 0.9339 0.082 Uiso 1 1 calc R . . H29B H 0.6524 0.5038 0.9348 0.082 Uiso 1 1 calc R . . H29C H 0.703 0.5435 0.972 0.082 Uiso 1 1 calc R . . C30 C 0.5721(4) 0.8306(2) 0.83103(11) 0.0305(9) Uani 1 1 d . . . C31 C 0.2758(4) 0.7995(3) 0.86094(13) 0.0431(12) Uani 1 1 d . . . H31 H 0.2168 0.7936 0.8399 0.052 Uiso 1 1 calc R . . C32 C 0.3553(4) 0.8603(3) 0.86936(13) 0.0414(11) Uani 1 1 d . . . H32 H 0.358 0.9033 0.8551 0.05 Uiso 1 1 calc R . . C33 C 0.4311(4) 0.8471(3) 0.90249(13) 0.0411(11) Uani 1 1 d . . . H33 H 0.4954 0.8786 0.914 0.049 Uiso 1 1 calc R . . C34 C 0.3928(4) 0.7783(3) 0.91512(12) 0.0376(10) Uani 1 1 d . . . H34 H 0.4252 0.756 0.9373 0.045 Uiso 1 1 calc R . . C35 C 0.2997(4) 0.7482(3) 0.88979(13) 0.0408(11) Uani 1 1 d . . . H35 H 0.2595 0.7019 0.8914 0.049 Uiso 1 1 calc R . . C36 C 1.0146(4) 0.2832(2) 0.85729(10) 0.0243(8) Uani 1 1 d . . . C37 C 1.1018(4) 0.2855(2) 0.82670(11) 0.0310(9) Uani 1 1 d . . . H37 H 1.1699 0.2494 0.8243 0.037 Uiso 1 1 calc R . . C38 C 1.0922(4) 0.3385(2) 0.79988(11) 0.0342(10) Uani 1 1 d . A . C39 C 0.9952(4) 0.3929(2) 0.80224(11) 0.0314(9) Uani 1 1 d . . . H39 H 0.9899 0.43 0.7841 0.038 Uiso 1 1 calc R . . C40 C 0.9067(4) 0.3914(2) 0.83180(11) 0.0260(8) Uani 1 1 d . . . C41 C 0.9156(4) 0.3376(2) 0.85869(10) 0.0241(8) Uani 1 1 d . . . H41 H 0.8527 0.3379 0.8786 0.029 Uiso 1 1 calc R . . C42 C 1.1849(5) 0.3374(3) 0.76680(14) 0.0489(13) Uani 1 1 d . . . C43 C 0.7982(4) 0.4469(2) 0.83490(12) 0.0329(9) Uani 1 1 d . . . C44 C 1.1892(4) 0.2049(2) 0.89956(10) 0.0245(8) Uani 1 1 d . . . C45 C 1.2847(4) 0.2603(2) 0.90010(11) 0.0280(9) Uani 1 1 d . . . H45 H 1.2591 0.3057 0.8901 0.034 Uiso 1 1 calc R . . C46 C 1.4175(4) 0.2516(2) 0.91488(12) 0.0319(9) Uani 1 1 d . B . C47 C 1.4580(4) 0.1863(2) 0.92937(12) 0.0347(10) Uani 1 1 d . . . H47 H 1.5481 0.18 0.9392 0.042 Uiso 1 1 calc R . . C48 C 1.3653(4) 0.1300(2) 0.92937(11) 0.0306(9) Uani 1 1 d . . . C49 C 1.2333(4) 0.1396(2) 0.91507(11) 0.0280(9) Uani 1 1 d . . . H49 H 1.1707 0.1005 0.9158 0.034 Uiso 1 1 calc R . . C50 C 1.5134(5) 0.3137(3) 0.91476(15) 0.0506(13) Uani 1 1 d . . . C51 C 1.4050(5) 0.0595(2) 0.94617(14) 0.0443(11) Uani 1 1 d . . . C52 C 0.9651(4) 0.1477(2) 0.86438(10) 0.0260(8) Uani 1 1 d . . . C53 C 0.8239(4) 0.1352(2) 0.86116(10) 0.0272(8) Uani 1 1 d . . . H53 H 0.7629 0.1657 0.8741 0.033 Uiso 1 1 calc R . . C54 C 0.7696(4) 0.0794(2) 0.83955(11) 0.0308(9) Uani 1 1 d . . . C55 C 0.8557(5) 0.0336(2) 0.82030(12) 0.0352(10) Uani 1 1 d . . . H55 H 0.8194 -0.0047 0.8057 0.042 Uiso 1 1 calc R . . C56 C 0.9954(4) 0.0450(2) 0.82287(11) 0.0339(9) Uani 1 1 d . . . C57 C 1.0490(4) 0.1011(2) 0.84459(11) 0.0291(9) Uani 1 1 d . . . H57 H 1.1455 0.1076 0.8459 0.035 Uiso 1 1 calc R . . C58 C 0.6188(5) 0.0659(2) 0.83776(12) 0.0379(10) Uani 1 1 d . . . C59 C 1.0919(5) -0.0019(3) 0.80239(13) 0.0425(11) Uani 1 1 d . . . C60 C 0.9534(4) 0.2312(2) 0.92676(10) 0.0238(8) Uani 1 1 d . . . C61 C 0.8968(4) 0.1756(2) 0.94740(11) 0.0273(8) Uani 1 1 d . . . H61 H 0.8876 0.1295 0.9363 0.033 Uiso 1 1 calc R . . C62 C 0.8532(4) 0.1849(2) 0.98376(11) 0.0303(9) Uani 1 1 d . . . C63 C 0.8631(4) 0.2518(2) 1.00072(12) 0.0336(9) Uani 1 1 d . . . H63 H 0.8326 0.2587 1.0254 0.04 Uiso 1 1 calc R . . C64 C 0.9187(4) 0.3083(2) 0.98078(11) 0.0293(9) Uani 1 1 d . . . C65 C 0.9635(4) 0.2982(2) 0.94472(11) 0.0270(8) Uani 1 1 d . . . H65 H 1.0021 0.3376 0.9318 0.032 Uiso 1 1 calc R . . C66 C 0.7951(5) 0.1236(3) 1.00516(13) 0.0398(10) Uani 1 1 d . . . C67 C 0.9312(5) 0.3809(2) 0.99881(13) 0.0407(11) Uani 1 1 d . . . B B 1.0280(4) 0.2171(2) 0.88702(12) 0.0247(9) Uani 1 1 d . . . F1 F 1.3023(7) 0.3088(4) 0.7736(2) 0.082(2) Uiso 0.584(9) 1 d P A 1 F2 F 1.2186(5) 0.4065(3) 0.75600(15) 0.0535(18) Uiso 0.584(9) 1 d P A 1 F3 F 1.1200(5) 0.3118(4) 0.73617(15) 0.0534(16) Uiso 0.584(9) 1 d P A 1 F7 F 1.5400(8) 0.3374(4) 0.87965(19) 0.069(2) Uiso 0.555(12) 1 d P B 1 F8 F 1.6350(7) 0.3007(4) 0.9284(2) 0.070(2) Uiso 0.555(12) 1 d P B 1 F9 F 1.4562(6) 0.3753(3) 0.9297(2) 0.0511(18) Uiso 0.555(12) 1 d P B 1 F1A F 1.2557(7) 0.2722(4) 0.7634(2) 0.050(2) Uiso 0.416(9) 1 d P A 2 F2A F 1.2877(12) 0.3784(6) 0.7702(3) 0.092(4) Uiso 0.416(9) 1 d P A 2 F3A F 1.1290(11) 0.3480(8) 0.7355(3) 0.093(4) Uiso 0.416(9) 1 d P A 2 F7A F 1.5963(12) 0.3089(6) 0.8854(3) 0.087(3) Uiso 0.445(12) 1 d P B 2 F8A F 1.6016(7) 0.3144(4) 0.9458(2) 0.050(2) Uiso 0.445(12) 1 d P B 2 F9A F 1.4587(9) 0.3754(5) 0.9116(4) 0.076(3) Uiso 0.445(12) 1 d P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0238(3) 0.0302(3) 0.0229(3) -0.0044(2) -0.0005(2) 0.0078(2) F4 0.0333(15) 0.0581(19) 0.121(3) -0.0223(19) -0.0116(16) 0.0146(14) F5 0.070(2) 0.0428(17) 0.112(3) 0.0360(18) 0.025(2) 0.0191(15) F6 0.136(3) 0.076(2) 0.0395(18) -0.0132(16) -0.0023(19) 0.066(2) F10 0.095(2) 0.0569(19) 0.053(2) 0.0244(16) 0.0103(17) 0.0270(17) F11 0.062(2) 0.066(2) 0.083(2) 0.0140(18) 0.0019(17) 0.0402(17) F12 0.113(3) 0.0298(15) 0.121(3) -0.0025(18) -0.060(3) 0.0144(17) F13 0.0343(14) 0.0541(17) 0.0664(19) -0.0116(15) -0.0003(13) 0.0003(12) F14 0.0526(17) 0.0547(17) 0.064(2) 0.0177(15) -0.0042(14) -0.0178(14) F15 0.0457(16) 0.084(2) 0.0382(16) -0.0102(15) -0.0166(12) -0.0071(15) F16 0.119(3) 0.059(2) 0.186(5) -0.062(3) 0.074(3) -0.007(2) F17 0.151(4) 0.123(3) 0.064(2) 0.022(2) 0.053(3) 0.086(3) F18 0.094(3) 0.146(4) 0.102(3) -0.082(3) -0.049(2) 0.084(3) F19 0.169(4) 0.0376(17) 0.075(2) 0.0018(16) 0.067(3) -0.013(2) F20 0.076(2) 0.075(2) 0.0394(17) 0.0210(15) -0.0081(15) -0.0191(17) F21 0.0499(18) 0.090(2) 0.066(2) 0.0171(18) 0.0046(15) -0.0243(17) F22 0.154(4) 0.060(2) 0.0379(18) -0.0221(16) -0.013(2) 0.000(2) F23 0.067(2) 0.0469(18) 0.128(3) -0.0307(19) -0.016(2) 0.0240(16) F24 0.090(2) 0.0528(19) 0.084(2) -0.0345(17) 0.031(2) -0.0302(17) O 0.060(2) 0.0397(18) 0.0351(18) 0.0043(15) 0.0068(15) -0.0010(16) N1 0.0253(16) 0.0301(17) 0.0244(17) -0.0025(14) -0.0026(13) 0.0076(14) N2 0.0257(16) 0.0272(17) 0.0204(16) -0.0021(14) -0.0019(13) 0.0034(13) C1 0.029(2) 0.029(2) 0.023(2) -0.0027(17) -0.0009(16) 0.0077(16) C2 0.0232(19) 0.045(2) 0.020(2) -0.0068(18) 0.0031(15) 0.0038(17) C3 0.0216(18) 0.030(2) 0.025(2) -0.0013(17) -0.0021(15) 0.0035(16) C4 0.037(2) 0.045(3) 0.034(2) -0.012(2) -0.0061(19) 0.011(2) C5 0.028(2) 0.047(3) 0.032(2) -0.004(2) -0.0032(17) 0.0126(19) C6 0.0232(19) 0.037(2) 0.036(2) -0.0129(19) -0.0032(17) 0.0084(17) C7 0.032(2) 0.045(3) 0.035(2) -0.013(2) -0.0043(18) 0.0143(19) C8 0.036(3) 0.071(4) 0.044(3) -0.017(3) -0.016(2) 0.017(3) C9 0.030(2) 0.082(4) 0.057(3) -0.023(3) -0.015(2) 0.000(3) C10 0.031(2) 0.059(3) 0.058(3) -0.021(3) -0.002(2) -0.002(2) C11 0.027(2) 0.043(2) 0.042(3) -0.014(2) -0.0024(18) 0.0049(18) C12 0.044(3) 0.046(3) 0.030(2) -0.003(2) -0.0098(19) 0.018(2) C13 0.074(4) 0.053(3) 0.039(3) -0.004(2) -0.012(3) 0.023(3) C14 0.064(3) 0.062(3) 0.035(3) -0.005(2) -0.005(2) 0.013(3) C15 0.030(2) 0.045(3) 0.054(3) 0.000(2) 0.004(2) -0.0005(19) C16 0.042(3) 0.062(3) 0.063(4) 0.005(3) 0.002(2) -0.004(2) C17 0.074(4) 0.048(3) 0.094(5) 0.006(3) 0.022(4) 0.024(3) C18 0.027(2) 0.035(2) 0.021(2) -0.0039(17) -0.0020(15) 0.0097(17) C19 0.027(2) 0.038(2) 0.028(2) -0.0057(18) -0.0014(17) 0.0089(17) C20 0.035(2) 0.043(2) 0.028(2) -0.011(2) -0.0077(18) 0.0107(19) C21 0.044(3) 0.051(3) 0.019(2) -0.007(2) -0.0055(18) 0.014(2) C22 0.044(3) 0.049(3) 0.022(2) 0.003(2) 0.0003(18) 0.013(2) C23 0.033(2) 0.039(2) 0.026(2) 0.0007(19) -0.0006(17) 0.0067(18) C24 0.036(2) 0.039(2) 0.030(2) -0.0011(19) -0.0066(18) 0.0017(19) C25 0.049(3) 0.050(3) 0.054(3) -0.009(2) 0.015(2) -0.005(2) C26 0.053(3) 0.037(3) 0.055(3) -0.003(2) -0.008(2) 0.005(2) C27 0.058(3) 0.045(3) 0.028(2) 0.005(2) -0.005(2) -0.008(2) C28 0.058(3) 0.063(4) 0.068(4) 0.019(3) 0.000(3) -0.010(3) C29 0.073(4) 0.042(3) 0.049(3) -0.003(2) 0.002(3) 0.001(3) C30 0.033(2) 0.033(2) 0.025(2) -0.0096(19) -0.0032(17) 0.0086(18) C31 0.025(2) 0.063(3) 0.042(3) -0.015(2) 0.0003(19) 0.016(2) C32 0.036(2) 0.042(3) 0.046(3) -0.004(2) 0.005(2) 0.021(2) C33 0.032(2) 0.051(3) 0.041(3) -0.018(2) 0.0044(19) 0.012(2) C34 0.035(2) 0.053(3) 0.025(2) -0.002(2) 0.0106(18) 0.018(2) C35 0.033(2) 0.043(3) 0.046(3) -0.009(2) 0.014(2) 0.0050(19) C36 0.0236(19) 0.028(2) 0.021(2) -0.0040(16) -0.0028(15) 0.0015(15) C37 0.029(2) 0.040(2) 0.024(2) 0.0003(18) 0.0025(16) 0.0088(17) C38 0.033(2) 0.048(3) 0.022(2) 0.0026(19) 0.0008(17) 0.0048(19) C39 0.033(2) 0.033(2) 0.028(2) 0.0073(18) -0.0043(17) 0.0013(18) C40 0.0251(19) 0.0254(19) 0.027(2) -0.0018(17) -0.0029(16) 0.0003(15) C41 0.0255(19) 0.0251(19) 0.022(2) -0.0039(16) -0.0006(15) -0.0007(15) C42 0.034(2) 0.073(4) 0.040(3) 0.019(3) -0.002(2) 0.011(2) C43 0.042(2) 0.027(2) 0.030(2) 0.0017(18) -0.0013(18) 0.0049(18) C44 0.0273(19) 0.027(2) 0.0190(19) -0.0003(16) 0.0048(15) 0.0043(16) C45 0.029(2) 0.029(2) 0.026(2) 0.0040(17) -0.0001(16) 0.0040(16) C46 0.028(2) 0.038(2) 0.030(2) 0.0030(18) -0.0005(17) 0.0012(17) C47 0.025(2) 0.047(3) 0.032(2) 0.002(2) -0.0005(17) 0.0097(19) C48 0.036(2) 0.033(2) 0.023(2) -0.0010(17) 0.0013(17) 0.0093(18) C49 0.032(2) 0.028(2) 0.024(2) -0.0021(17) 0.0000(16) 0.0051(17) C50 0.026(2) 0.071(4) 0.054(3) 0.022(3) -0.005(2) -0.003(2) C51 0.050(3) 0.037(3) 0.045(3) -0.002(2) -0.009(2) 0.017(2) C52 0.032(2) 0.027(2) 0.0185(19) -0.0004(16) -0.0013(15) 0.0065(16) C53 0.035(2) 0.027(2) 0.019(2) -0.0001(16) 0.0005(16) 0.0042(17) C54 0.038(2) 0.031(2) 0.023(2) 0.0034(17) -0.0060(17) -0.0002(18) C55 0.048(3) 0.029(2) 0.028(2) -0.0034(18) -0.0058(19) 0.0007(19) C56 0.044(2) 0.031(2) 0.026(2) -0.0043(18) -0.0036(18) 0.0092(19) C57 0.032(2) 0.033(2) 0.022(2) -0.0016(17) -0.0008(16) 0.0007(17) C58 0.043(2) 0.039(2) 0.031(2) -0.002(2) -0.0070(19) -0.005(2) C59 0.051(3) 0.041(3) 0.034(3) -0.013(2) -0.006(2) 0.011(2) C60 0.0222(18) 0.027(2) 0.022(2) -0.0015(16) -0.0036(15) 0.0021(15) C61 0.0264(19) 0.028(2) 0.027(2) -0.0046(17) -0.0027(16) 0.0016(16) C62 0.029(2) 0.036(2) 0.026(2) 0.0031(18) 0.0002(16) -0.0008(17) C63 0.034(2) 0.043(2) 0.024(2) -0.0054(19) 0.0026(17) 0.0045(19) C64 0.028(2) 0.032(2) 0.028(2) -0.0071(18) -0.0031(16) 0.0028(17) C65 0.0255(19) 0.028(2) 0.027(2) -0.0032(17) -0.0016(16) 0.0003(16) C66 0.044(3) 0.044(3) 0.031(2) -0.001(2) 0.0063(19) -0.003(2) C67 0.050(3) 0.039(3) 0.033(3) -0.009(2) 0.001(2) 0.003(2) B 0.026(2) 0.023(2) 0.024(2) -0.0017(18) -0.0024(17) 0.0032(17) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Fe C30 1.770(5) . ? Fe N2 2.019(3) . ? Fe N1 2.029(3) . ? Fe C32 2.086(4) . ? Fe C31 2.098(4) . ? Fe C33 2.099(4) . ? Fe C35 2.132(4) . ? Fe C34 2.143(4) . ? F4 C43 1.315(5) . ? F5 C43 1.337(5) . ? F6 C43 1.313(5) . ? F10 C51 1.317(6) . ? F11 C51 1.335(6) . ? F12 C51 1.334(6) . ? F13 C58 1.330(5) . ? F14 C58 1.339(5) . ? F15 C58 1.348(5) . ? F16 C59 1.318(6) . ? F17 C59 1.294(6) . ? F18 C59 1.299(6) . ? F19 C66 1.301(5) . ? F20 C66 1.335(5) . ? F21 C66 1.341(5) . ? F22 C67 1.334(5) . ? F23 C67 1.320(5) . ? F24 C67 1.314(6) . ? O C30 1.147(5) . ? N1 C1 1.286(5) . ? N1 C6 1.464(5) . ? N2 C3 1.279(5) . ? N2 C18 1.464(5) . ? C1 C4 1.500(6) . ? C1 C2 1.503(5) . ? C2 C3 1.502(5) . ? C2 H2 0.95 . ? C3 C5 1.506(5) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 C11 1.405(6) . ? C6 C7 1.409(6) . ? C7 C8 1.406(6) . ? C7 C12 1.514(7) . ? C8 C9 1.379(8) . ? C8 H8 0.95 . ? C9 C10 1.366(8) . ? C9 H9 0.95 . ? C10 C11 1.403(6) . ? C10 H10 0.95 . ? C11 C15 1.505(7) . ? C12 C14 1.526(6) . ? C12 C13 1.538(6) . ? C12 H12 1 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C17 1.523(7) . ? C15 C16 1.543(7) . ? C15 H15 1 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 C23 1.393(6) . ? C18 C19 1.409(6) . ? C19 C20 1.396(6) . ? C19 C24 1.526(6) . ? C20 C21 1.378(7) . ? C20 H20 0.95 . ? C21 C22 1.376(7) . ? C21 H21 0.95 . ? C22 C23 1.401(6) . ? C22 H22 0.95 . ? C23 C27 1.527(6) . ? C24 C26 1.522(6) . ? C24 C25 1.531(6) . ? C24 H24 1 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C28 1.527(7) . ? C27 C29 1.531(7) . ? C27 H27 1 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C31 C32 1.401(7) . ? C31 C35 1.426(7) . ? C31 H31 0.95 . ? C32 C33 1.414(7) . ? C32 H32 0.95 . ? C33 C34 1.410(7) . ? C33 H33 0.95 . ? C34 C35 1.393(7) . ? C34 H34 0.95 . ? C35 H35 0.95 . ? C36 C41 1.400(5) . ? C36 C37 1.402(5) . ? C36 B 1.634(6) . ? C37 C38 1.381(6) . ? C37 H37 0.95 . ? C38 C39 1.389(6) . ? C38 C42 1.506(6) . ? C39 C40 1.380(6) . ? C39 H39 0.95 . ? C40 C41 1.393(5) . ? C40 C43 1.485(5) . ? C41 H41 0.95 . ? C42 F3A 1.259(12) . ? C42 F2A 1.265(11) . ? C42 F1 1.283(8) . ? C42 F3 1.349(8) . ? C42 F2 1.385(8) . ? C42 F1A 1.401(9) . ? C44 C45 1.389(6) . ? C44 C49 1.402(5) . ? C44 B 1.645(6) . ? C45 C46 1.403(5) . ? C45 H45 0.95 . ? C46 C47 1.377(6) . ? C46 C50 1.486(7) . ? C47 C48 1.383(6) . ? C47 H47 0.95 . ? C48 C49 1.392(6) . ? C48 C51 1.493(6) . ? C49 H49 0.95 . ? C50 F9A 1.268(10) . ? C50 F8 1.300(8) . ? C50 F7A 1.343(11) . ? C50 F7 1.367(8) . ? C50 F9 1.386(8) . ? C50 F8A 1.398(9) . ? C52 C57 1.395(5) . ? C52 C53 1.401(5) . ? C52 B 1.640(6) . ? C53 C54 1.395(6) . ? C53 H53 0.95 . ? C54 C55 1.389(6) . ? C54 C58 1.494(6) . ? C55 C56 1.380(6) . ? C55 H55 0.95 . ? C56 C57 1.400(6) . ? C56 C59 1.488(6) . ? C57 H57 0.95 . ? C60 C61 1.393(6) . ? C60 C65 1.405(5) . ? C60 B 1.636(6) . ? C61 C62 1.393(6) . ? C61 H61 0.95 . ? C62 C63 1.389(6) . ? C62 C66 1.493(6) . ? C63 C64 1.387(6) . ? C63 H63 0.95 . ? C64 C65 1.388(6) . ? C64 C67 1.503(6) . ? C65 H65 0.95 . ? 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 C30 Fe N2 94.04(16) . . ? C30 Fe N1 92.83(16) . . ? N2 Fe N1 89.54(12) . . ? C30 Fe C32 84.44(19) . . ? N2 Fe C32 140.73(16) . . ? N1 Fe C32 129.72(16) . . ? C30 Fe C31 108.95(19) . . ? N2 Fe C31 155.56(17) . . ? N1 Fe C31 97.27(16) . . ? C32 Fe C31 39.12(19) . . ? C30 Fe C33 99.09(19) . . ? N2 Fe C33 102.94(15) . . ? N1 Fe C33 161.99(16) . . ? C32 Fe C33 39.50(18) . . ? C31 Fe C33 66.13(18) . . ? C30 Fe C35 147.61(19) . . ? N2 Fe C35 116.53(16) . . ? N1 Fe C35 97.60(16) . . ? C32 Fe C35 65.35(19) . . ? C31 Fe C35 39.40(19) . . ? C33 Fe C35 65.31(19) . . ? C30 Fe C34 137.62(18) . . ? N2 Fe C34 92.56(15) . . ? N1 Fe C34 129.07(17) . . ? C32 Fe C34 64.89(18) . . ? C31 Fe C34 64.97(18) . . ? C33 Fe C34 38.82(19) . . ? C35 Fe C34 38.04(18) . . ? C1 N1 C6 116.7(3) . . ? C1 N1 Fe 123.1(3) . . ? C6 N1 Fe 119.1(2) . . ? C3 N2 C18 116.9(3) . . ? C3 N2 Fe 123.2(3) . . ? C18 N2 Fe 119.9(2) . . ? N1 C1 C4 125.4(4) . . ? N1 C1 C2 119.9(3) . . ? C4 C1 C2 114.6(3) . . ? C3 C2 C1 117.9(3) . . ? C3 C2 H2 121 . . ? C1 C2 H2 121 . . ? N2 C3 C2 120.6(3) . . ? N2 C3 C5 125.2(4) . . ? C2 C3 C5 114.2(3) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 122.7(4) . . ? C11 C6 N1 119.2(4) . . ? C7 C6 N1 118.1(4) . . ? C6 C7 C8 117.1(5) . . ? C6 C7 C12 124.3(4) . . ? C8 C7 C12 118.6(4) . . ? C9 C8 C7 121.2(5) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C10 C9 C8 119.9(4) . . ? C10 C9 H9 120 . . ? C8 C9 H9 120 . . ? C9 C10 C11 122.6(5) . . ? C9 C10 H10 118.7 . . ? C11 C10 H10 118.7 . . ? C10 C11 C6 116.3(4) . . ? C10 C11 C15 120.7(4) . . ? C6 C11 C15 122.8(4) . . ? C7 C12 C14 112.2(4) . . ? C7 C12 C13 111.8(4) . . ? C14 C12 C13 110.1(4) . . ? C7 C12 H12 107.5 . . ? C14 C12 H12 107.5 . . ? C13 C12 H12 107.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C17 111.7(4) . . ? C11 C15 C16 113.7(4) . . ? C17 C15 C16 108.4(4) . . ? C11 C15 H15 107.6 . . ? C17 C15 H15 107.6 . . ? C16 C15 H15 107.6 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 122.4(4) . . ? C23 C18 N2 119.6(4) . . ? C19 C18 N2 118.0(3) . . ? C20 C19 C18 117.2(4) . . ? C20 C19 C24 119.6(4) . . ? C18 C19 C24 123.2(4) . . ? C21 C20 C19 121.4(4) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C22 C21 C20 120.3(4) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 121.0(4) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C18 C23 C22 117.7(4) . . ? C18 C23 C27 124.2(4) . . ? C22 C23 C27 118.1(4) . . ? C26 C24 C19 113.8(4) . . ? C26 C24 C25 108.7(4) . . ? C19 C24 C25 112.7(4) . . ? C26 C24 H24 107.1 . . ? C19 C24 H24 107.1 . . ? C25 C24 H24 107.1 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C23 112.2(4) . . ? C28 C27 C29 108.9(4) . . ? C23 C27 C29 111.4(4) . . ? C28 C27 H27 108 . . ? C23 C27 H27 108 . . ? C29 C27 H27 108 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O C30 Fe 174.7(4) . . ? C32 C31 C35 107.3(4) . . ? C32 C31 Fe 70.0(2) . . ? C35 C31 Fe 71.6(2) . . ? C32 C31 H31 126.3 . . ? C35 C31 H31 126.3 . . ? Fe C31 H31 123.7 . . ? C31 C32 C33 108.8(4) . . ? C31 C32 Fe 70.9(2) . . ? C33 C32 Fe 70.7(2) . . ? C31 C32 H32 125.6 . . ? C33 C32 H32 125.6 . . ? Fe C32 H32 124.4 . . ? C34 C33 C32 106.9(4) . . ? C34 C33 Fe 72.3(2) . . ? C32 C33 Fe 69.8(2) . . ? C34 C33 H33 126.5 . . ? C32 C33 H33 126.5 . . ? Fe C33 H33 123.1 . . ? C35 C34 C33 109.1(4) . . ? C35 C34 Fe 70.6(2) . . ? C33 C34 Fe 68.9(2) . . ? C35 C34 H34 125.5 . . ? C33 C34 H34 125.5 . . ? Fe C34 H34 126.6 . . ? C34 C35 C31 107.8(4) . . ? C34 C35 Fe 71.4(2) . . ? C31 C35 Fe 69.0(2) . . ? C34 C35 H35 126.1 . . ? C31 C35 H35 126.1 . . ? Fe C35 H35 125.1 . . ? C41 C36 C37 115.7(4) . . ? C41 C36 B 124.7(3) . . ? C37 C36 B 119.6(3) . . ? C38 C37 C36 122.4(4) . . ? C38 C37 H37 118.8 . . ? C36 C37 H37 118.8 . . ? C37 C38 C39 121.0(4) . . ? C37 C38 C42 120.5(4) . . ? C39 C38 C42 118.5(4) . . ? C40 C39 C38 117.8(4) . . ? C40 C39 H39 121.1 . . ? C38 C39 H39 121.1 . . ? C39 C40 C41 121.2(4) . . ? C39 C40 C43 119.9(4) . . ? C41 C40 C43 119.0(3) . . ? C40 C41 C36 122.0(3) . . ? C40 C41 H41 119 . . ? C36 C41 H41 119 . . ? F3A C42 F2A 108.8(9) . . ? F1 C42 F3 114.6(6) . . ? F1 C42 F2 102.9(5) . . ? F3 C42 F2 102.0(5) . . ? F3A C42 F1A 105.4(8) . . ? F2A C42 F1A 98.0(6) . . ? F3A C42 C38 116.6(6) . . ? F2A C42 C38 113.6(6) . . ? F1 C42 C38 113.6(5) . . ? F3 C42 C38 111.8(4) . . ? F2 C42 C38 110.9(5) . . ? F1A C42 C38 112.6(5) . . ? F6 C43 F4 104.5(4) . . ? F6 C43 F5 105.5(4) . . ? F4 C43 F5 105.5(4) . . ? F6 C43 C40 113.9(3) . . ? F4 C43 C40 113.6(3) . . ? F5 C43 C40 113.1(4) . . ? C45 C44 C49 115.9(3) . . ? C45 C44 B 122.6(3) . . ? C49 C44 B 121.0(3) . . ? C44 C45 C46 122.4(4) . . ? C44 C45 H45 118.8 . . ? C46 C45 H45 118.8 . . ? C47 C46 C45 120.2(4) . . ? C47 C46 C50 120.7(4) . . ? C45 C46 C50 119.1(4) . . ? C46 C47 C48 119.0(4) . . ? C46 C47 H47 120.5 . . ? C48 C47 H47 120.5 . . ? C47 C48 C49 120.3(4) . . ? C47 C48 C51 120.0(4) . . ? C49 C48 C51 119.7(4) . . ? C48 C49 C44 122.3(4) . . ? C48 C49 H49 118.8 . . ? C44 C49 H49 118.8 . . ? F9A C50 F7A 104.4(7) . . ? F8 C50 F7 102.9(5) . . ? F8 C50 F9 112.2(6) . . ? F7 C50 F9 100.2(5) . . ? F9A C50 F8A 108.4(7) . . ? F7A C50 F8A 104.9(6) . . ? F9A C50 C46 116.0(5) . . ? F8 C50 C46 115.1(5) . . ? F7A C50 C46 109.7(6) . . ? F7 C50 C46 112.5(5) . . ? F9 C50 C46 112.6(4) . . ? F8A C50 C46 112.5(5) . . ? F10 C51 F11 105.7(4) . . ? F10 C51 F12 107.4(5) . . ? F11 C51 F12 105.2(4) . . ? F10 C51 C48 113.1(4) . . ? F11 C51 C48 112.5(4) . . ? F12 C51 C48 112.3(4) . . ? C57 C52 C53 116.0(4) . . ? C57 C52 B 121.6(3) . . ? C53 C52 B 122.2(3) . . ? C54 C53 C52 122.3(4) . . ? C54 C53 H53 118.9 . . ? C52 C53 H53 118.9 . . ? C55 C54 C53 120.4(4) . . ? C55 C54 C58 118.6(4) . . ? C53 C54 C58 121.0(4) . . ? C56 C55 C54 118.4(4) . . ? C56 C55 H55 120.8 . . ? C54 C55 H55 120.8 . . ? C55 C56 C57 120.8(4) . . ? C55 C56 C59 120.5(4) . . ? C57 C56 C59 118.7(4) . . ? C52 C57 C56 122.1(4) . . ? C52 C57 H57 119 . . ? C56 C57 H57 119 . . ? F13 C58 F14 106.3(4) . . ? F13 C58 F15 106.0(4) . . ? F14 C58 F15 105.3(4) . . ? F13 C58 C54 113.7(4) . . ? F14 C58 C54 112.7(4) . . ? F15 C58 C54 112.1(4) . . ? F17 C59 F18 105.7(5) . . ? F17 C59 F16 103.7(5) . . ? F18 C59 F16 104.2(5) . . ? F17 C59 C56 113.9(4) . . ? F18 C59 C56 114.4(4) . . ? F16 C59 C56 113.8(4) . . ? C61 C60 C65 116.0(3) . . ? C61 C60 B 122.1(3) . . ? C65 C60 B 121.0(3) . . ? C60 C61 C62 122.5(4) . . ? C60 C61 H61 118.7 . . ? C62 C61 H61 118.7 . . ? C63 C62 C61 120.3(4) . . ? C63 C62 C66 118.8(4) . . ? C61 C62 C66 120.9(4) . . ? C62 C63 C64 118.4(4) . . ? C62 C63 H63 120.8 . . ? C64 C63 H63 120.8 . . ? C65 C64 C63 120.8(4) . . ? C65 C64 C67 120.0(4) . . ? C63 C64 C67 119.2(4) . . ? C64 C65 C60 121.9(4) . . ? C64 C65 H65 119 . . ? C60 C65 H65 119 . . ? F19 C66 F20 108.7(4) . . ? F19 C66 F21 106.8(4) . . ? F20 C66 F21 102.8(4) . . ? F19 C66 C62 113.5(4) . . ? F20 C66 C62 112.2(4) . . ? F21 C66 C62 112.1(4) . . ? F24 C67 F23 107.2(4) . . ? F24 C67 F22 106.0(4) . . ? F23 C67 F22 105.3(4) . . ? F24 C67 C64 113.1(4) . . ? F23 C67 C64 112.0(4) . . ? F22 C67 C64 112.7(4) . . ? C36 B C60 114.8(3) . . ? C36 B C52 103.9(3) . . ? C60 B C52 113.1(3) . . ? C36 B C44 110.5(3) . . ? C60 B C44 102.6(3) . . ? C52 B C44 112.1(3) . . ? #===END