# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Mei Wang' _publ_contact_author_email SYMBUENO@DLUT.EDU.CN _publ_section_title ; Structures, protonation, and electrochemical properties of diiron dithiolate complexes containing pyridyl-phosphine ligands ; loop_ _publ_author_name 'Mei Wang' 'Lin Chen' 'Ping Li' 'Jihong Liu' 'Licheng Sun' 'Zhenbo Zhao' # Attachment 'Revised-Dalton-B814336F-cif.cif' # Copyright The Royal Society of Chemistry, 2006 # CCDC Number: 643385 data_3a _database_code_depnum_ccdc_archive 'CCDC 643385' _audit_creation_date 'Oct 31 18:25:00 2006' _audit_creation_method SHELXL-97 _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP97 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Bruker, 1997)' #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 635.24 _chemical_formula_analytical ? _chemical_formula_sum 'C26 H22 Fe2 N O5 P S2' _chemical_formula_moiety 'C26 H22 Fe2 N O5 P S2' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 9.0353(13) _cell_length_b 12.3801(18) _cell_length_c 12.7353(19) _cell_angle_alpha 97.723(2) _cell_angle_beta 108.443(2) _cell_angle_gamma 91.284(2) _cell_volume 1335.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3915 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 26.95 #------------------------------------------------------------------------------ _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 1.340 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5426 _exptl_absorpt_correction_T_max 0.9737 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7773 _diffrn_reflns_av_R_equivalents 0.0109 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 26.97 _reflns_number_total 5618 _reflns_number_gt 4709 _reflns_threshold_expression >2sigma(I) _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 26.97 _diffrn_measured_fraction_theta_full 0.965 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.52998(4) 0.55297(3) 0.79882(3) 0.03778(9) Uani 1 1 d . . . Fe2 Fe 0.56639(3) 0.76226(2) 0.83448(2) 0.03373(9) Uani 1 1 d . . . S1 S 0.64981(7) 0.65368(5) 0.96744(5) 0.04077(14) Uani 1 1 d . . . S2 S 0.69093(6) 0.65249(5) 0.73958(5) 0.03882(13) Uani 1 1 d . . . P1 P 0.44924(6) 0.83036(4) 0.67707(4) 0.03335(12) Uani 1 1 d . . . N1 N 0.8557(3) 0.89456(19) 0.70702(19) 0.0560(5) Uani 1 1 d . . . O1 O 0.6720(3) 0.35027(18) 0.8576(2) 0.0903(8) Uani 1 1 d . . . O2 O 0.2383(2) 0.5380(2) 0.8516(2) 0.0780(6) Uani 1 1 d . . . O3 O 0.3622(3) 0.46018(19) 0.56632(18) 0.0793(6) Uani 1 1 d . . . O4 O 0.3051(3) 0.81233(19) 0.91661(19) 0.0751(6) Uani 1 1 d . . . O5 O 0.7717(2) 0.95539(16) 0.95463(16) 0.0662(5) Uani 1 1 d . . . C1 C 0.6172(3) 0.4289(2) 0.8333(2) 0.0531(6) Uani 1 1 d . . . C2 C 0.3538(3) 0.5443(2) 0.8335(2) 0.0498(6) Uani 1 1 d . . . C3 C 0.4260(3) 0.4997(2) 0.6557(2) 0.0515(6) Uani 1 1 d . . . C4 C 0.4067(3) 0.7931(2) 0.8836(2) 0.0460(6) Uani 1 1 d . . . C5 C 0.6919(3) 0.8806(2) 0.90341(19) 0.0439(5) Uani 1 1 d . . . C6 C 0.8618(3) 0.6409(2) 1.0089(2) 0.0524(6) Uani 1 1 d . . . H6A H 0.9073 0.6744 1.0864 0.063 Uiso 1 1 calc R . . H6B H 0.8801 0.5638 1.0056 0.063 Uiso 1 1 calc R . . C7 C 0.9479(3) 0.6899(2) 0.9416(2) 0.0598(7) Uani 1 1 d . . . H7A H 0.9353 0.7679 0.9482 0.072 Uiso 1 1 calc R . . H7B H 1.0585 0.6800 0.9738 0.072 Uiso 1 1 calc R . . C8 C 0.8961(3) 0.6431(2) 0.8199(2) 0.0531(6) Uani 1 1 d . . . H8A H 0.9180 0.5665 0.8139 0.064 Uiso 1 1 calc R . . H8B H 0.9599 0.6795 0.7848 0.064 Uiso 1 1 calc R . . C9 C 0.5796(3) 0.86171(19) 0.59654(18) 0.0415(5) Uani 1 1 d . . . H9A H 0.6171 0.7942 0.5694 0.050 Uiso 1 1 calc R . . H9B H 0.5202 0.8939 0.5320 0.050 Uiso 1 1 calc R . . C10 C 0.7175(3) 0.93891(19) 0.66567(19) 0.0413(5) Uani 1 1 d . . . C11 C 0.7007(3) 1.0481(2) 0.6860(2) 0.0491(6) Uani 1 1 d . . . H11A H 0.6051 1.0768 0.6547 0.059 Uiso 1 1 calc R . . C12 C 0.8287(4) 1.1151(2) 0.7539(3) 0.0669(8) Uani 1 1 d . . . H12A H 0.8194 1.1898 0.7694 0.080 Uiso 1 1 calc R . . C13 C 0.9687(4) 1.0722(3) 0.7982(3) 0.0654(8) Uani 1 1 d . . . H13A H 1.0552 1.1165 0.8449 0.078 Uiso 1 1 calc R . . C14 C 0.9786(3) 0.9633(3) 0.7725(3) 0.0646(8) Uani 1 1 d . . . H14A H 1.0746 0.9344 0.8014 0.078 Uiso 1 1 calc R . . C15 C 0.3591(2) 0.96076(17) 0.68915(18) 0.0367(5) Uani 1 1 d . . . C16 C 0.2545(3) 0.9937(2) 0.5940(2) 0.0461(5) Uani 1 1 d . . . H16A H 0.2194 0.9450 0.5275 0.055 Uiso 1 1 calc R . . C17 C 0.2029(3) 1.0978(2) 0.5977(2) 0.0580(7) Uani 1 1 d . . . H17A H 0.1327 1.1187 0.5340 0.070 Uiso 1 1 calc R . . C18 C 0.2553(4) 1.1705(2) 0.6954(2) 0.0608(7) Uani 1 1 d . . . H18A H 0.2225 1.2412 0.6973 0.073 Uiso 1 1 calc R . . C19 C 0.3558(3) 1.1391(2) 0.7901(2) 0.0567(7) Uani 1 1 d . . . H19A H 0.3897 1.1882 0.8563 0.068 Uiso 1 1 calc R . . C20 C 0.4073(3) 1.03446(19) 0.7877(2) 0.0467(6) Uani 1 1 d . . . H20A H 0.4744 1.0135 0.8525 0.056 Uiso 1 1 calc R . . C21 C 0.2888(3) 0.74417(18) 0.57332(18) 0.0398(5) Uani 1 1 d . . . C22 C 0.1540(3) 0.7252(2) 0.5993(2) 0.0531(6) Uani 1 1 d . . . H22A H 0.1480 0.7567 0.6683 0.064 Uiso 1 1 calc R . . C23 C 0.0279(3) 0.6605(2) 0.5249(3) 0.0655(8) Uani 1 1 d . . . H23A H -0.0619 0.6485 0.5437 0.079 Uiso 1 1 calc R . . C24 C 0.0363(4) 0.6139(2) 0.4230(3) 0.0699(9) Uani 1 1 d . . . H24A H -0.0482 0.5705 0.3724 0.084 Uiso 1 1 calc R . . C25 C 0.1681(4) 0.6313(3) 0.3959(3) 0.0734(9) Uani 1 1 d . . . H25A H 0.1733 0.5990 0.3270 0.088 Uiso 1 1 calc R . . C26 C 0.2952(3) 0.6968(2) 0.4700(2) 0.0575(7) Uani 1 1 d . . . H26A H 0.3842 0.7088 0.4503 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.03359(17) 0.03602(17) 0.04290(18) 0.00646(13) 0.01066(14) 0.00637(13) Fe2 0.03435(17) 0.03498(16) 0.03201(16) 0.00520(12) 0.01037(13) 0.00938(12) S1 0.0432(3) 0.0434(3) 0.0363(3) 0.0098(2) 0.0114(2) 0.0127(2) S2 0.0362(3) 0.0411(3) 0.0407(3) 0.0028(2) 0.0155(2) 0.0073(2) P1 0.0332(3) 0.0346(3) 0.0308(3) 0.0037(2) 0.0086(2) 0.0045(2) N1 0.0447(12) 0.0583(13) 0.0646(14) 0.0078(11) 0.0176(11) 0.0056(10) O1 0.0940(17) 0.0539(13) 0.1150(19) 0.0226(13) 0.0167(15) 0.0326(12) O2 0.0487(12) 0.0977(17) 0.1016(17) 0.0303(14) 0.0374(12) 0.0109(11) O3 0.0792(15) 0.0790(15) 0.0573(13) -0.0115(11) 0.0003(11) -0.0084(12) O4 0.0733(14) 0.0920(16) 0.0853(15) 0.0301(12) 0.0519(12) 0.0412(12) O5 0.0670(13) 0.0526(11) 0.0587(11) -0.0029(9) -0.0032(10) -0.0028(10) C1 0.0470(14) 0.0460(14) 0.0634(16) 0.0059(12) 0.0142(12) 0.0090(11) C2 0.0421(14) 0.0522(14) 0.0551(15) 0.0145(12) 0.0127(12) 0.0096(11) C3 0.0473(14) 0.0453(13) 0.0581(16) 0.0050(12) 0.0126(12) 0.0012(11) C4 0.0517(14) 0.0487(13) 0.0429(13) 0.0159(10) 0.0182(11) 0.0195(11) C5 0.0463(13) 0.0449(13) 0.0368(12) 0.0068(10) 0.0071(10) 0.0111(11) C6 0.0416(13) 0.0545(15) 0.0504(14) 0.0089(12) -0.0012(11) 0.0109(11) C7 0.0369(13) 0.0651(17) 0.0693(18) 0.0089(14) 0.0060(12) 0.0077(12) C8 0.0340(12) 0.0605(16) 0.0652(17) 0.0044(13) 0.0182(12) 0.0099(11) C9 0.0414(12) 0.0481(13) 0.0359(11) 0.0069(10) 0.0134(10) 0.0024(10) C10 0.0406(12) 0.0472(13) 0.0391(12) 0.0102(10) 0.0153(10) 0.0016(10) C11 0.0498(14) 0.0458(13) 0.0564(15) 0.0187(11) 0.0187(12) 0.0080(11) C12 0.083(2) 0.0474(15) 0.075(2) 0.0098(14) 0.0324(17) 0.0025(15) C13 0.0550(17) 0.0647(18) 0.0694(19) -0.0024(15) 0.0161(14) -0.0119(14) C14 0.0394(14) 0.075(2) 0.0739(19) 0.0067(16) 0.0120(13) 0.0050(13) C15 0.0362(11) 0.0361(11) 0.0388(11) 0.0080(9) 0.0122(9) 0.0056(9) C16 0.0504(14) 0.0470(13) 0.0406(12) 0.0105(10) 0.0120(11) 0.0101(11) C17 0.0655(17) 0.0570(16) 0.0555(16) 0.0243(13) 0.0171(13) 0.0241(13) C18 0.0730(19) 0.0443(14) 0.0717(19) 0.0174(13) 0.0280(15) 0.0218(13) C19 0.0678(17) 0.0427(13) 0.0572(16) -0.0012(12) 0.0198(14) 0.0110(12) C20 0.0493(14) 0.0427(13) 0.0439(13) 0.0039(10) 0.0095(11) 0.0105(11) C21 0.0399(12) 0.0343(11) 0.0386(11) 0.0053(9) 0.0035(10) 0.0033(9) C22 0.0481(14) 0.0526(15) 0.0537(15) 0.0032(12) 0.0118(12) -0.0033(12) C23 0.0453(15) 0.0612(18) 0.078(2) 0.0089(15) 0.0047(14) -0.0099(13) C24 0.0642(19) 0.0507(16) 0.0683(19) 0.0045(14) -0.0131(16) -0.0123(14) C25 0.087(2) 0.0647(19) 0.0507(16) -0.0126(14) 0.0070(16) -0.0144(17) C26 0.0600(17) 0.0570(16) 0.0484(15) -0.0066(12) 0.0143(13) -0.0055(13) #------------------------------------------------------------------------------ _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^)+(0.0384P)^2^+0.5833P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5618 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0804 _refine_ls_wR_factor_gt 0.0750 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.586 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.053 #------------------------------------------------------------------------------ _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C2 1.786(3) . ? Fe1 C1 1.786(3) . ? Fe1 C3 1.790(3) . ? Fe1 S2 2.2507(7) . ? Fe1 S1 2.2555(7) . ? Fe1 Fe2 2.5650(6) . ? Fe2 C4 1.775(2) . ? Fe2 C5 1.776(3) . ? Fe2 P1 2.2365(6) . ? Fe2 S2 2.2497(6) . ? Fe2 S1 2.2565(6) . ? S1 C6 1.835(2) . ? S2 C8 1.827(2) . ? P1 C21 1.824(2) . ? P1 C15 1.834(2) . ? P1 C9 1.855(2) . ? N1 C10 1.353(3) . ? N1 C14 1.354(4) . ? O1 C1 1.137(3) . ? O2 C2 1.141(3) . ? O3 C3 1.136(3) . ? O4 C4 1.141(3) . ? O5 C5 1.146(3) . ? C6 C7 1.499(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.499(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.506(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.362(3) . ? C11 C12 1.380(4) . ? C11 H11A 0.9300 . ? C12 C13 1.364(4) . ? C12 H12A 0.9300 . ? C13 C14 1.355(4) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C20 1.388(3) . ? C15 C16 1.398(3) . ? C16 C17 1.380(3) . ? C16 H16A 0.9300 . ? C17 C18 1.376(4) . ? C17 H17A 0.9300 . ? C18 C19 1.370(4) . ? C18 H18A 0.9300 . ? C19 C20 1.385(3) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C22 1.382(4) . ? C21 C26 1.386(3) . ? C22 C23 1.382(4) . ? C22 H22A 0.9300 . ? C23 C24 1.373(5) . ? C23 H23A 0.9300 . ? C24 C25 1.361(5) . ? C24 H24A 0.9300 . ? C25 C26 1.391(4) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Fe1 C1 103.43(12) . . ? C2 Fe1 C3 90.67(12) . . ? C1 Fe1 C3 95.37(12) . . ? C2 Fe1 S2 147.73(8) . . ? C1 Fe1 S2 108.75(9) . . ? C3 Fe1 S2 88.69(9) . . ? C2 Fe1 S1 89.65(9) . . ? C1 Fe1 S1 95.99(9) . . ? C3 Fe1 S1 168.24(9) . . ? S2 Fe1 S1 84.78(3) . . ? C2 Fe1 Fe2 95.90(8) . . ? C1 Fe1 Fe2 145.47(9) . . ? C3 Fe1 Fe2 112.91(8) . . ? S2 Fe1 Fe2 55.236(17) . . ? S1 Fe1 Fe2 55.375(17) . . ? C4 Fe2 C5 98.78(12) . . ? C4 Fe2 P1 90.60(7) . . ? C5 Fe2 P1 95.81(7) . . ? C4 Fe2 S2 152.75(9) . . ? C5 Fe2 S2 108.39(8) . . ? P1 Fe2 S2 88.72(2) . . ? C4 Fe2 S1 89.17(7) . . ? C5 Fe2 S1 98.78(7) . . ? P1 Fe2 S1 165.27(3) . . ? S2 Fe2 S1 84.78(2) . . ? C4 Fe2 Fe1 99.88(8) . . ? C5 Fe2 Fe1 147.53(7) . . ? P1 Fe2 Fe1 110.28(2) . . ? S2 Fe2 Fe1 55.272(19) . . ? S1 Fe2 Fe1 55.337(19) . . ? C6 S1 Fe1 110.29(9) . . ? C6 S1 Fe2 112.58(9) . . ? Fe1 S1 Fe2 69.29(2) . . ? C8 S2 Fe2 112.62(9) . . ? C8 S2 Fe1 111.76(10) . . ? Fe2 S2 Fe1 69.49(2) . . ? C21 P1 C15 101.62(10) . . ? C21 P1 C9 103.37(11) . . ? C15 P1 C9 100.71(10) . . ? C21 P1 Fe2 115.97(7) . . ? C15 P1 Fe2 117.92(7) . . ? C9 P1 Fe2 114.92(8) . . ? C10 N1 C14 117.1(2) . . ? O1 C1 Fe1 178.4(3) . . ? O2 C2 Fe1 177.6(3) . . ? O3 C3 Fe1 176.2(2) . . ? O4 C4 Fe2 179.0(2) . . ? O5 C5 Fe2 175.3(2) . . ? C7 C6 S1 116.95(18) . . ? C7 C6 H6A 108.1 . . ? S1 C6 H6A 108.1 . . ? C7 C6 H6B 108.1 . . ? S1 C6 H6B 108.1 . . ? H6A C6 H6B 107.3 . . ? C8 C7 C6 114.8(2) . . ? C8 C7 H7A 108.6 . . ? C6 C7 H7A 108.6 . . ? C8 C7 H7B 108.6 . . ? C6 C7 H7B 108.6 . . ? H7A C7 H7B 107.5 . . ? C7 C8 S2 117.07(18) . . ? C7 C8 H8A 108.0 . . ? S2 C8 H8A 108.0 . . ? C7 C8 H8B 108.0 . . ? S2 C8 H8B 108.0 . . ? H8A C8 H8B 107.3 . . ? C10 C9 P1 112.35(15) . . ? C10 C9 H9A 109.1 . . ? P1 C9 H9A 109.1 . . ? C10 C9 H9B 109.1 . . ? P1 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? N1 C10 C11 122.4(2) . . ? N1 C10 C9 117.0(2) . . ? C11 C10 C9 120.5(2) . . ? C10 C11 C12 118.5(2) . . ? C10 C11 H11A 120.7 . . ? C12 C11 H11A 120.7 . . ? C13 C12 C11 120.2(3) . . ? C13 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? C14 C13 C12 118.4(3) . . ? C14 C13 H13A 120.8 . . ? C12 C13 H13A 120.8 . . ? N1 C14 C13 123.4(3) . . ? N1 C14 H14A 118.3 . . ? C13 C14 H14A 118.3 . . ? C20 C15 C16 118.4(2) . . ? C20 C15 P1 121.34(16) . . ? C16 C15 P1 119.74(17) . . ? C17 C16 C15 120.7(2) . . ? C17 C16 H16A 119.7 . . ? C15 C16 H16A 119.7 . . ? C18 C17 C16 120.0(2) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C19 C18 C17 120.1(2) . . ? C19 C18 H18A 119.9 . . ? C17 C18 H18A 119.9 . . ? C18 C19 C20 120.4(3) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C19 C20 C15 120.4(2) . . ? C19 C20 H20A 119.8 . . ? C15 C20 H20A 119.8 . . ? C22 C21 C26 118.4(2) . . ? C22 C21 P1 118.19(18) . . ? C26 C21 P1 123.4(2) . . ? C23 C22 C21 121.3(3) . . ? C23 C22 H22A 119.3 . . ? C21 C22 H22A 119.3 . . ? C24 C23 C22 119.5(3) . . ? C24 C23 H23A 120.3 . . ? C22 C23 H23A 120.3 . . ? C25 C24 C23 120.1(3) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C24 C25 C26 120.8(3) . . ? C24 C25 H25A 119.6 . . ? C26 C25 H25A 119.6 . . ? C21 C26 C25 119.8(3) . . ? C21 C26 H26A 120.1 . . ? C25 C26 H26A 120.1 . . ? #===END # Copyright The Royal Society of Chemistry, 2006 # CCDC Number: 643386 data_3aH _database_code_depnum_ccdc_archive 'CCDC 643386' _audit_creation_date 'Oct 31 18:25:00 2006' _audit_creation_method SHELXL-97 _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP97 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Bruker, 1997)' #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 785.31 _chemical_formula_analytical ? _chemical_formula_sum 'C27 H23 F3 Fe2 N O8 P S3' _chemical_formula_moiety 'C26 H23 Fe2 N O5 P S2, C F3 O3 S' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 10.8040(6) _cell_length_b 10.9749(8) _cell_length_c 14.5372(9) _cell_angle_alpha 97.749(4) _cell_angle_beta 109.389(3) _cell_angle_gamma 94.117(4) _cell_volume 1598.53(18) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4299 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 24.72 #------------------------------------------------------------------------------ _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 1.219 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7112 _exptl_absorpt_correction_T_max 0.7925 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15173 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 27.63 _reflns_number_total 7369 _reflns_number_gt 5154 _reflns_threshold_expression >2sigma(I) _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.63 _diffrn_measured_fraction_theta_full 0.990 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' F F 0.0171 0.0103 '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 Fe1 Fe 0.72886(4) 0.55591(4) 0.38512(3) 0.05968(14) Uani 1 1 d . . . Fe2 Fe 0.53901(4) 0.46107(3) 0.22495(3) 0.04559(12) Uani 1 1 d . . . S1 S 0.66658(9) 0.64056(8) 0.24619(7) 0.0728(3) Uani 1 1 d . . . S2 S 0.51206(7) 0.54075(6) 0.36591(5) 0.05065(17) Uani 1 1 d . . . P1 P 0.46261(6) 0.27209(6) 0.23888(5) 0.03786(15) Uani 1 1 d . . . N1 N 0.1127(2) 0.2080(2) 0.14201(18) 0.0499(6) Uani 1 1 d . . . O1 O 0.8717(3) 0.7759(3) 0.5290(3) 0.1534(17) Uani 1 1 d . . . O2 O 0.9391(3) 0.4534(3) 0.3279(3) 0.1227(12) Uani 1 1 d . . . O3 O 0.7690(3) 0.4000(2) 0.53692(19) 0.0906(8) Uani 1 1 d . . . O4 O 0.6790(3) 0.3479(3) 0.1017(2) 0.0938(8) Uani 1 1 d . . . O5 O 0.3127(3) 0.5228(3) 0.07083(18) 0.0963(9) Uani 1 1 d . . . C1 C 0.8148(4) 0.6908(3) 0.4740(4) 0.0956(13) Uani 1 1 d . . . C2 C 0.8573(4) 0.4955(4) 0.3497(3) 0.0830(11) Uani 1 1 d . . . C3 C 0.7515(3) 0.4576(3) 0.4766(3) 0.0639(8) Uani 1 1 d . . . C4 C 0.6236(3) 0.3923(3) 0.1500(3) 0.0627(8) Uani 1 1 d . . . C5 C 0.3989(3) 0.4946(3) 0.1317(2) 0.0614(8) Uani 1 1 d . . . C6 C 0.5782(4) 0.7744(3) 0.2611(4) 0.0940(13) Uani 1 1 d . . . H6A H 0.6360 0.8485 0.2658 0.113 Uiso 1 1 calc R . . H6C H 0.5022 0.7687 0.2012 0.113 Uiso 1 1 calc R . . C7 C 0.5314(4) 0.7918(3) 0.3455(4) 0.0933(13) Uani 1 1 d . . . H7A H 0.6082 0.8097 0.4058 0.112 Uiso 1 1 calc R . . H7B H 0.4849 0.8644 0.3419 0.112 Uiso 1 1 calc R . . C8 C 0.4444(4) 0.6884(3) 0.3541(3) 0.0754(10) Uani 1 1 d . . . H8A H 0.3645 0.6748 0.2962 0.091 Uiso 1 1 calc R . . H8B H 0.4191 0.7131 0.4113 0.091 Uiso 1 1 calc R . . C9 C 0.3180(2) 0.2603(2) 0.28192(18) 0.0428(6) Uani 1 1 d . . . H9A H 0.2995 0.1756 0.2905 0.051 Uiso 1 1 calc R . . H9B H 0.3407 0.3129 0.3459 0.051 Uiso 1 1 calc R . . C10 C 0.1966(2) 0.2971(2) 0.21211(19) 0.0432(6) Uani 1 1 d . . . C11 C 0.1642(3) 0.4158(3) 0.2124(2) 0.0574(7) Uani 1 1 d . . . H11A H 0.2182 0.4800 0.2607 0.069 Uiso 1 1 calc R . . C12 C 0.0527(3) 0.4400(3) 0.1419(3) 0.0703(9) Uani 1 1 d . . . H12A H 0.0318 0.5208 0.1425 0.084 Uiso 1 1 calc R . . C13 C -0.0280(3) 0.3476(3) 0.0708(3) 0.0680(9) Uani 1 1 d . . . H13A H -0.1027 0.3644 0.0221 0.082 Uiso 1 1 calc R . . C14 C 0.0032(3) 0.2298(3) 0.0727(2) 0.0610(8) Uani 1 1 d . . . H14A H -0.0515 0.1646 0.0259 0.073 Uiso 1 1 calc R . . C15 C 0.4039(2) 0.1552(2) 0.12591(18) 0.0440(6) Uani 1 1 d . . . C16 C 0.3551(3) 0.1901(3) 0.0337(2) 0.0650(8) Uani 1 1 d . . . H16A H 0.3552 0.2736 0.0285 0.078 Uiso 1 1 calc R . . C17 C 0.3065(4) 0.1012(4) -0.0503(2) 0.0798(11) Uani 1 1 d . . . H17A H 0.2732 0.1252 -0.1119 0.096 Uiso 1 1 calc R . . C18 C 0.3067(3) -0.0224(4) -0.0438(2) 0.0730(10) Uani 1 1 d . . . H18A H 0.2741 -0.0819 -0.1009 0.088 Uiso 1 1 calc R . . C19 C 0.3548(3) -0.0576(3) 0.0465(2) 0.0684(9) Uani 1 1 d . . . H19A H 0.3552 -0.1413 0.0510 0.082 Uiso 1 1 calc R . . C20 C 0.4030(3) 0.0303(3) 0.1312(2) 0.0545(7) Uani 1 1 d . . . H20A H 0.4353 0.0053 0.1926 0.065 Uiso 1 1 calc R . . C21 C 0.5812(2) 0.1934(2) 0.32552(18) 0.0423(6) Uani 1 1 d . . . C22 C 0.5602(3) 0.1497(3) 0.4048(2) 0.0555(7) Uani 1 1 d . . . H22A H 0.4810 0.1578 0.4159 0.067 Uiso 1 1 calc R . . C23 C 0.6575(4) 0.0939(3) 0.4676(2) 0.0707(10) Uani 1 1 d . . . H23A H 0.6436 0.0657 0.5213 0.085 Uiso 1 1 calc R . . C24 C 0.7722(4) 0.0798(3) 0.4515(3) 0.0783(11) Uani 1 1 d . . . H24A H 0.8363 0.0417 0.4941 0.094 Uiso 1 1 calc R . . C25 C 0.7951(3) 0.1216(3) 0.3724(3) 0.0766(10) Uani 1 1 d . . . H25A H 0.8738 0.1111 0.3611 0.092 Uiso 1 1 calc R . . C26 C 0.6995(3) 0.1794(3) 0.3103(2) 0.0588(7) Uani 1 1 d . . . H26A H 0.7149 0.2091 0.2577 0.071 Uiso 1 1 calc R . . S3 S 1.15331(7) 0.88439(7) 0.20852(6) 0.05635(19) Uani 1 1 d . . . O6 O 1.1968(2) 0.7773(2) 0.16678(19) 0.0821(7) Uani 1 1 d . . . O7 O 1.2460(2) 0.9562(2) 0.29689(16) 0.0788(7) Uani 1 1 d . . . O8 O 1.0842(2) 0.95738(19) 0.13665(15) 0.0697(6) Uani 1 1 d . . . C27 C 1.0244(4) 0.8162(3) 0.2469(3) 0.0746(10) Uani 1 1 d . . . F1 F 0.9651(3) 0.8995(3) 0.2826(2) 0.1210(9) Uani 1 1 d . . . F2 F 1.0740(3) 0.7472(2) 0.31457(19) 0.1136(8) Uani 1 1 d . . . F3 F 0.9335(2) 0.7440(2) 0.17052(19) 0.1011(7) Uani 1 1 d . . . H1 H 0.124(3) 0.139(3) 0.146(2) 0.067(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0451(2) 0.0471(2) 0.0800(3) 0.0142(2) 0.0131(2) -0.00256(18) Fe2 0.0459(2) 0.0437(2) 0.0542(2) 0.01814(17) 0.02188(18) 0.00985(16) S1 0.0724(5) 0.0554(5) 0.1029(7) 0.0341(5) 0.0397(5) 0.0018(4) S2 0.0510(4) 0.0404(3) 0.0591(4) 0.0044(3) 0.0193(3) 0.0029(3) P1 0.0379(3) 0.0394(3) 0.0358(3) 0.0080(3) 0.0110(3) 0.0069(3) N1 0.0461(13) 0.0458(14) 0.0530(14) 0.0051(11) 0.0125(11) 0.0038(11) O1 0.105(2) 0.0730(19) 0.201(4) -0.025(2) -0.028(2) -0.0184(17) O2 0.0753(19) 0.152(3) 0.158(3) 0.037(2) 0.054(2) 0.037(2) O3 0.0962(19) 0.0808(17) 0.0735(16) 0.0235(14) 0.0004(14) -0.0038(14) O4 0.107(2) 0.101(2) 0.110(2) 0.0279(17) 0.0787(18) 0.0318(16) O5 0.1010(19) 0.123(2) 0.0744(16) 0.0527(16) 0.0205(14) 0.0537(17) C1 0.064(2) 0.059(2) 0.136(4) 0.008(2) 0.003(2) -0.0050(18) C2 0.058(2) 0.083(3) 0.107(3) 0.027(2) 0.024(2) 0.0074(19) C3 0.0554(18) 0.0544(18) 0.066(2) 0.0058(16) 0.0041(15) -0.0050(14) C4 0.0660(19) 0.0645(19) 0.073(2) 0.0261(16) 0.0380(17) 0.0141(16) C5 0.0696(19) 0.0631(19) 0.0618(19) 0.0262(16) 0.0274(16) 0.0213(16) C6 0.113(3) 0.049(2) 0.128(4) 0.038(2) 0.041(3) 0.017(2) C7 0.080(3) 0.0460(19) 0.154(4) 0.020(2) 0.037(3) 0.0156(18) C8 0.079(2) 0.0463(17) 0.103(3) 0.0010(17) 0.035(2) 0.0194(16) C9 0.0423(13) 0.0451(14) 0.0398(13) 0.0057(11) 0.0141(11) 0.0000(11) C10 0.0395(13) 0.0458(14) 0.0456(14) 0.0026(12) 0.0193(11) 0.0018(11) C11 0.0481(16) 0.0484(16) 0.0710(19) -0.0019(14) 0.0181(14) 0.0102(13) C12 0.0601(19) 0.0613(19) 0.090(2) 0.0124(18) 0.0238(18) 0.0244(16) C13 0.0465(17) 0.086(2) 0.069(2) 0.0184(18) 0.0126(15) 0.0201(16) C14 0.0423(15) 0.070(2) 0.0580(18) 0.0013(15) 0.0051(13) 0.0015(14) C15 0.0375(13) 0.0550(16) 0.0363(13) 0.0016(11) 0.0109(10) 0.0065(11) C16 0.073(2) 0.075(2) 0.0437(16) 0.0110(15) 0.0126(15) 0.0235(17) C17 0.074(2) 0.120(3) 0.0354(16) 0.0037(19) 0.0075(15) 0.019(2) C18 0.062(2) 0.093(3) 0.0502(19) -0.0214(18) 0.0164(15) 0.0013(18) C19 0.070(2) 0.0618(19) 0.064(2) -0.0124(16) 0.0221(17) -0.0033(16) C20 0.0595(17) 0.0512(16) 0.0473(15) -0.0008(13) 0.0158(13) 0.0019(13) C21 0.0441(14) 0.0330(12) 0.0394(13) 0.0022(10) 0.0021(11) 0.0058(10) C22 0.0635(18) 0.0472(15) 0.0452(15) 0.0112(12) 0.0045(13) 0.0026(13) C23 0.086(3) 0.0527(18) 0.0537(18) 0.0170(14) -0.0048(17) 0.0068(17) C24 0.083(3) 0.0493(18) 0.071(2) 0.0080(16) -0.0170(19) 0.0191(17) C25 0.0559(19) 0.066(2) 0.088(3) 0.0000(19) 0.0001(17) 0.0244(16) C26 0.0536(17) 0.0579(17) 0.0587(18) 0.0067(14) 0.0109(14) 0.0159(14) S3 0.0543(4) 0.0505(4) 0.0580(4) 0.0149(3) 0.0096(3) 0.0042(3) O6 0.0797(16) 0.0785(16) 0.0882(17) 0.0120(13) 0.0257(13) 0.0309(13) O7 0.0793(16) 0.0731(15) 0.0627(13) 0.0154(11) 0.0001(12) -0.0160(12) O8 0.0798(15) 0.0545(12) 0.0633(13) 0.0215(10) 0.0059(11) 0.0047(11) C27 0.070(2) 0.064(2) 0.088(3) 0.024(2) 0.022(2) 0.0055(18) F1 0.124(2) 0.117(2) 0.152(2) 0.0182(18) 0.0849(19) 0.0361(17) F2 0.1186(19) 0.1114(18) 0.1192(18) 0.0707(16) 0.0345(15) 0.0039(15) F3 0.0704(13) 0.0864(15) 0.1277(19) 0.0179(14) 0.0149(13) -0.0157(11) #------------------------------------------------------------------------------ _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^)+(0.0491P)^2^+0.3515P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7369 _refine_ls_number_parameters 410 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1065 _refine_ls_wR_factor_gt 0.0935 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.474 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.057 #------------------------------------------------------------------------------ _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C2 1.773(4) . ? Fe1 C3 1.789(4) . ? Fe1 C1 1.793(4) . ? Fe1 S1 2.2558(10) . ? Fe1 S2 2.2560(8) . ? Fe1 Fe2 2.5654(6) . ? Fe2 C5 1.766(3) . ? Fe2 C4 1.769(3) . ? Fe2 S2 2.2357(8) . ? Fe2 P1 2.2366(7) . ? Fe2 S1 2.2448(9) . ? S1 C6 1.835(4) . ? S2 C8 1.831(3) . ? P1 C21 1.831(2) . ? P1 C15 1.835(3) . ? P1 C9 1.869(3) . ? N1 C14 1.337(4) . ? N1 C10 1.344(3) . ? N1 H1 0.78(3) . ? O1 C1 1.131(4) . ? O2 C2 1.141(5) . ? O3 C3 1.123(4) . ? O4 C4 1.147(4) . ? O5 C5 1.147(3) . ? C6 C7 1.470(6) . ? C6 H6A 0.9700 . ? C6 H6C 0.9700 . ? C7 C8 1.466(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.488(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.373(4) . ? C11 C12 1.368(4) . ? C11 H11A 0.9300 . ? C12 C13 1.360(5) . ? C12 H12A 0.9300 . ? C13 C14 1.360(4) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C20 1.384(4) . ? C15 C16 1.385(4) . ? C16 C17 1.377(5) . ? C16 H16A 0.9300 . ? C17 C18 1.373(5) . ? C17 H17A 0.9300 . ? C18 C19 1.362(5) . ? C18 H18A 0.9300 . ? C19 C20 1.378(4) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C26 1.383(4) . ? C21 C22 1.385(4) . ? C22 C23 1.385(4) . ? C22 H22A 0.9300 . ? C23 C24 1.351(5) . ? C23 H23A 0.9300 . ? C24 C25 1.382(5) . ? C24 H24A 0.9300 . ? C25 C26 1.383(4) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? S3 O7 1.426(2) . ? S3 O6 1.430(2) . ? S3 O8 1.444(2) . ? S3 C27 1.813(4) . ? C27 F1 1.302(4) . ? C27 F2 1.319(4) . ? C27 F3 1.324(4) . ? #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Fe1 C3 90.65(17) . . ? C2 Fe1 C1 102.34(19) . . ? C3 Fe1 C1 93.57(17) . . ? C2 Fe1 S1 89.09(13) . . ? C3 Fe1 S1 166.26(10) . . ? C1 Fe1 S1 99.90(14) . . ? C2 Fe1 S2 148.18(13) . . ? C3 Fe1 S2 88.54(11) . . ? C1 Fe1 S2 109.46(14) . . ? S1 Fe1 S2 84.47(3) . . ? C2 Fe1 Fe2 96.44(13) . . ? C3 Fe1 Fe2 111.38(9) . . ? C1 Fe1 Fe2 148.53(13) . . ? S1 Fe1 Fe2 55.05(3) . . ? S2 Fe1 Fe2 54.80(2) . . ? C5 Fe2 C4 99.43(15) . . ? C5 Fe2 S2 104.02(11) . . ? C4 Fe2 S2 156.28(11) . . ? C5 Fe2 P1 99.47(11) . . ? C4 Fe2 P1 89.45(10) . . ? S2 Fe2 P1 90.22(3) . . ? C5 Fe2 S1 97.00(11) . . ? C4 Fe2 S1 88.45(11) . . ? S2 Fe2 S1 85.20(3) . . ? P1 Fe2 S1 163.51(3) . . ? C5 Fe2 Fe1 143.74(11) . . ? C4 Fe2 Fe1 102.45(11) . . ? S2 Fe2 Fe1 55.54(2) . . ? P1 Fe2 Fe1 109.23(2) . . ? S1 Fe2 Fe1 55.45(3) . . ? C6 S1 Fe2 111.56(14) . . ? C6 S1 Fe1 111.02(15) . . ? Fe2 S1 Fe1 69.50(3) . . ? C8 S2 Fe2 110.16(13) . . ? C8 S2 Fe1 112.93(12) . . ? Fe2 S2 Fe1 69.66(3) . . ? C21 P1 C15 102.10(11) . . ? C21 P1 C9 101.88(12) . . ? C15 P1 C9 101.11(11) . . ? C21 P1 Fe2 115.50(8) . . ? C15 P1 Fe2 116.77(9) . . ? C9 P1 Fe2 117.03(9) . . ? C14 N1 C10 123.6(3) . . ? C14 N1 H1 118(2) . . ? C10 N1 H1 118(2) . . ? O1 C1 Fe1 178.2(5) . . ? O2 C2 Fe1 178.0(4) . . ? O3 C3 Fe1 177.1(3) . . ? O4 C4 Fe2 179.7(4) . . ? O5 C5 Fe2 175.7(3) . . ? C7 C6 S1 118.2(3) . . ? C7 C6 H6A 107.8 . . ? S1 C6 H6A 107.8 . . ? C7 C6 H6C 107.8 . . ? S1 C6 H6C 107.8 . . ? H6A C6 H6C 107.1 . . ? C8 C7 C6 116.8(4) . . ? C8 C7 H7A 108.1 . . ? C6 C7 H7A 108.1 . . ? C8 C7 H7B 108.1 . . ? C6 C7 H7B 108.1 . . ? H7A C7 H7B 107.3 . . ? C7 C8 S2 116.6(3) . . ? C7 C8 H8A 108.1 . . ? S2 C8 H8A 108.1 . . ? C7 C8 H8B 108.1 . . ? S2 C8 H8B 108.1 . . ? H8A C8 H8B 107.3 . . ? C10 C9 P1 113.04(17) . . ? C10 C9 H9A 109.0 . . ? P1 C9 H9A 109.0 . . ? C10 C9 H9B 109.0 . . ? P1 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? N1 C10 C11 117.0(2) . . ? N1 C10 C9 117.8(2) . . ? C11 C10 C9 125.1(2) . . ? C12 C11 C10 120.2(3) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? C13 C12 C11 120.9(3) . . ? C13 C12 H12A 119.5 . . ? C11 C12 H12A 119.5 . . ? C12 C13 C14 118.4(3) . . ? C12 C13 H13A 120.8 . . ? C14 C13 H13A 120.8 . . ? N1 C14 C13 119.8(3) . . ? N1 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C20 C15 C16 118.6(3) . . ? C20 C15 P1 120.7(2) . . ? C16 C15 P1 120.7(2) . . ? C17 C16 C15 120.1(3) . . ? C17 C16 H16A 119.9 . . ? C15 C16 H16A 119.9 . . ? C18 C17 C16 120.6(3) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? C19 C18 C17 119.7(3) . . ? C19 C18 H18A 120.1 . . ? C17 C18 H18A 120.1 . . ? C18 C19 C20 120.3(3) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C19 C20 C15 120.6(3) . . ? C19 C20 H20A 119.7 . . ? C15 C20 H20A 119.7 . . ? C26 C21 C22 118.9(2) . . ? C26 C21 P1 116.9(2) . . ? C22 C21 P1 124.2(2) . . ? C21 C22 C23 119.8(3) . . ? C21 C22 H22A 120.1 . . ? C23 C22 H22A 120.1 . . ? C24 C23 C22 120.7(3) . . ? C24 C23 H23A 119.6 . . ? C22 C23 H23A 119.6 . . ? C23 C24 C25 120.6(3) . . ? C23 C24 H24A 119.7 . . ? C25 C24 H24A 119.7 . . ? C24 C25 C26 119.1(3) . . ? C24 C25 H25A 120.5 . . ? C26 C25 H25A 120.5 . . ? C25 C26 C21 120.9(3) . . ? C25 C26 H26A 119.6 . . ? C21 C26 H26A 119.6 . . ? O7 S3 O6 116.44(16) . . ? O7 S3 O8 113.96(13) . . ? O6 S3 O8 113.87(14) . . ? O7 S3 C27 104.70(17) . . ? O6 S3 C27 102.12(17) . . ? O8 S3 C27 103.55(15) . . ? F1 C27 F2 108.5(3) . . ? F1 C27 F3 107.5(3) . . ? F2 C27 F3 107.7(3) . . ? F1 C27 S3 112.4(3) . . ? F2 C27 S3 110.5(3) . . ? F3 C27 S3 110.2(3) . . ? #===END # Copyright The Royal Society of Chemistry, 2006 # CCDC Number: 643387 data_3b _database_code_depnum_ccdc_archive 'CCDC 643387' _audit_creation_date 'Oct 31 18:25:00 2006' _audit_creation_method SHELXL-97 _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP97 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Bruker, 1997)' #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 621.21 _chemical_formula_analytical ? _chemical_formula_sum 'C25 H20 Fe2 N O5 P S2' _chemical_formula_moiety 'C25 H20 Fe2 N O5 P S2' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 9.285(6) _cell_length_b 17.400(11) _cell_length_c 16.844(11) _cell_angle_alpha 90.00 _cell_angle_beta 103.196(9) _cell_angle_gamma 90.00 _cell_volume 2650(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3538 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 25.48 #------------------------------------------------------------------------------ _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 1.349 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5519 _exptl_absorpt_correction_T_max 0.8441 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16207 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 29.01 _reflns_number_total 6432 _reflns_number_gt 4305 _reflns_threshold_expression >2sigma(I) _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.25686(4) 0.00776(2) 0.88100(2) 0.04131(12) Uani 1 1 d . . . Fe2 Fe 0.09163(4) 0.07355(2) 0.76012(2) 0.03366(11) Uani 1 1 d . . . S1 S 0.13984(8) -0.05407(4) 0.76594(4) 0.04465(18) Uani 1 1 d . . . S2 S 0.02965(8) 0.05400(4) 0.88162(4) 0.04312(18) Uani 1 1 d . . . P1 P -0.11948(8) 0.10079(4) 0.66940(4) 0.03513(17) Uani 1 1 d . . . N1 N 0.0051(3) 0.20960(15) 0.59072(17) 0.0622(7) Uani 1 1 d . . . O1 O 0.2893(3) -0.11702(16) 1.00111(16) 0.0884(8) Uani 1 1 d . . . O2 O 0.5304(3) -0.01233(17) 0.82501(19) 0.0965(9) Uani 1 1 d . . . O3 O 0.3683(3) 0.13785(17) 0.98733(19) 0.1116(11) Uani 1 1 d . . . O4 O 0.2797(3) 0.07958(16) 0.64358(16) 0.0884(9) Uani 1 1 d . . . O5 O 0.1802(3) 0.23019(12) 0.80944(15) 0.0747(7) Uani 1 1 d . . . C1 C 0.2773(3) -0.06823(19) 0.9546(2) 0.0552(8) Uani 1 1 d . . . C2 C 0.4251(4) -0.00379(18) 0.8472(2) 0.0563(8) Uani 1 1 d . . . C3 C 0.3272(4) 0.0867(2) 0.9455(2) 0.0646(9) Uani 1 1 d . . . C4 C 0.2035(3) 0.07775(17) 0.68827(19) 0.0508(7) Uani 1 1 d . . . C5 C 0.1392(3) 0.16964(17) 0.78899(17) 0.0467(7) Uani 1 1 d . . . C6 C -0.0037(4) -0.11653(18) 0.7879(2) 0.0660(10) Uani 1 1 d . . . H6A H -0.0462 -0.1452 0.7387 0.079 Uiso 1 1 calc R . . H6B H 0.0433 -0.1534 0.8288 0.079 Uiso 1 1 calc R . . C7 C -0.1256(4) -0.0799(2) 0.8165(3) 0.0827(12) Uani 1 1 d . . . H7A H -0.1854 -0.0524 0.7705 0.099 Uiso 1 1 calc R . . H7B H -0.1869 -0.1208 0.8300 0.099 Uiso 1 1 calc R . . C8 C -0.0948(4) -0.0268(2) 0.8856(2) 0.0677(10) Uani 1 1 d . . . H8A H -0.0534 -0.0563 0.9344 0.081 Uiso 1 1 calc R . . H8B H -0.1884 -0.0060 0.8920 0.081 Uiso 1 1 calc R . . C9 C -0.2371(3) 0.01967(14) 0.62766(15) 0.0377(6) Uani 1 1 d . . . C10 C -0.1763(4) -0.04010(17) 0.59139(19) 0.0538(8) Uani 1 1 d . . . H10A H -0.0785 -0.0370 0.5869 0.065 Uiso 1 1 calc R . . C11 C -0.2594(4) -0.10399(19) 0.5621(2) 0.0700(10) Uani 1 1 d . . . H11A H -0.2182 -0.1430 0.5366 0.084 Uiso 1 1 calc R . . C12 C -0.4026(4) -0.1104(2) 0.5703(2) 0.0753(11) Uani 1 1 d . . . H12A H -0.4576 -0.1541 0.5515 0.090 Uiso 1 1 calc R . . C13 C -0.4644(4) -0.0523(2) 0.6061(2) 0.0746(11) Uani 1 1 d . . . H13A H -0.5612 -0.0565 0.6120 0.089 Uiso 1 1 calc R . . C14 C -0.3823(3) 0.01296(17) 0.6336(2) 0.0557(8) Uani 1 1 d . . . H14A H -0.4259 0.0529 0.6565 0.067 Uiso 1 1 calc R . . C15 C -0.2520(3) 0.16664(14) 0.70052(16) 0.0373(6) Uani 1 1 d . . . C16 C -0.2838(3) 0.15745(18) 0.77489(18) 0.0512(8) Uani 1 1 d . . . H16A H -0.2327 0.1209 0.8108 0.061 Uiso 1 1 calc R . . C17 C -0.3912(4) 0.2018(2) 0.7976(2) 0.0682(10) Uani 1 1 d . . . H17A H -0.4134 0.1936 0.8481 0.082 Uiso 1 1 calc R . . C18 C -0.4646(4) 0.25700(19) 0.7475(2) 0.0699(10) Uani 1 1 d . . . H18A H -0.5363 0.2868 0.7633 0.084 Uiso 1 1 calc R . . C19 C -0.4315(4) 0.2681(2) 0.6733(2) 0.0761(11) Uani 1 1 d . . . H19A H -0.4801 0.3063 0.6388 0.091 Uiso 1 1 calc R . . C20 C -0.3267(4) 0.22310(17) 0.6491(2) 0.0615(9) Uani 1 1 d . . . H20A H -0.3061 0.2307 0.5982 0.074 Uiso 1 1 calc R . . C21 C -0.0905(3) 0.14917(15) 0.57703(16) 0.0403(6) Uani 1 1 d . . . C22 C -0.1634(3) 0.12836(18) 0.49910(18) 0.0562(8) Uani 1 1 d . . . H22A H -0.2262 0.0860 0.4910 0.067 Uiso 1 1 calc R . . C23 C -0.1426(4) 0.1708(2) 0.4331(2) 0.0704(10) Uani 1 1 d . . . H23A H -0.1907 0.1571 0.3803 0.084 Uiso 1 1 calc R . . C24 C -0.0509(4) 0.2328(2) 0.4464(2) 0.0738(11) Uani 1 1 d . . . H24A H -0.0387 0.2629 0.4028 0.089 Uiso 1 1 calc R . . C25 C 0.0230(4) 0.25056(19) 0.5239(2) 0.0690(10) Uani 1 1 d . . . H25A H 0.0880 0.2920 0.5318 0.083 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0337(2) 0.0504(2) 0.0370(2) 0.00108(18) 0.00222(17) 0.00572(18) Fe2 0.0321(2) 0.0382(2) 0.0309(2) 0.00049(15) 0.00763(16) 0.00279(16) S1 0.0509(4) 0.0394(4) 0.0418(4) -0.0034(3) 0.0068(3) 0.0046(3) S2 0.0378(4) 0.0587(4) 0.0339(4) 0.0012(3) 0.0102(3) 0.0062(3) P1 0.0350(4) 0.0395(4) 0.0305(4) 0.0016(3) 0.0066(3) 0.0034(3) N1 0.0719(19) 0.0519(15) 0.0659(19) 0.0035(14) 0.0223(15) 0.0030(14) O1 0.0816(19) 0.105(2) 0.0748(18) 0.0429(16) 0.0104(15) 0.0138(16) O2 0.0487(15) 0.142(3) 0.106(2) 0.0030(19) 0.0342(16) 0.0093(16) O3 0.086(2) 0.110(2) 0.116(2) -0.0598(19) -0.0236(18) 0.0007(17) O4 0.0798(18) 0.122(2) 0.0807(19) 0.0246(16) 0.0536(16) 0.0257(16) O5 0.0912(19) 0.0473(13) 0.0833(18) -0.0135(12) 0.0152(14) -0.0113(13) C1 0.0418(18) 0.072(2) 0.049(2) 0.0079(17) 0.0052(15) 0.0081(16) C2 0.0407(18) 0.071(2) 0.055(2) 0.0061(16) 0.0051(16) 0.0078(16) C3 0.0445(19) 0.077(2) 0.064(2) -0.0134(19) -0.0040(17) 0.0058(17) C4 0.0481(18) 0.0603(19) 0.0468(19) 0.0089(15) 0.0165(15) 0.0111(15) C5 0.0455(17) 0.0514(18) 0.0415(17) 0.0022(13) 0.0061(14) 0.0037(14) C6 0.071(2) 0.0502(18) 0.070(2) 0.0032(16) 0.0016(19) -0.0148(18) C7 0.067(3) 0.085(3) 0.097(3) 0.011(2) 0.021(2) -0.029(2) C8 0.051(2) 0.093(3) 0.063(2) 0.009(2) 0.0217(18) -0.0167(19) C9 0.0398(16) 0.0402(14) 0.0305(15) 0.0017(11) 0.0025(12) 0.0046(12) C10 0.0507(19) 0.0559(18) 0.053(2) -0.0077(15) 0.0082(15) 0.0084(15) C11 0.083(3) 0.0538(19) 0.065(2) -0.0174(17) -0.001(2) 0.016(2) C12 0.073(3) 0.057(2) 0.085(3) -0.0156(19) -0.006(2) -0.011(2) C13 0.055(2) 0.074(2) 0.092(3) -0.015(2) 0.011(2) -0.0203(19) C14 0.0466(19) 0.0550(18) 0.064(2) -0.0084(16) 0.0092(16) -0.0018(15) C15 0.0336(14) 0.0398(14) 0.0374(16) -0.0025(12) 0.0058(12) 0.0006(12) C16 0.0468(18) 0.0677(19) 0.0377(17) 0.0064(14) 0.0067(14) 0.0173(15) C17 0.066(2) 0.098(3) 0.044(2) -0.0015(19) 0.0210(18) 0.012(2) C18 0.067(2) 0.069(2) 0.079(3) -0.008(2) 0.026(2) 0.0186(19) C19 0.082(3) 0.064(2) 0.088(3) 0.020(2) 0.031(2) 0.032(2) C20 0.072(2) 0.061(2) 0.057(2) 0.0171(16) 0.0255(18) 0.0236(17) C21 0.0433(16) 0.0419(15) 0.0373(16) 0.0056(12) 0.0126(13) 0.0081(13) C22 0.056(2) 0.069(2) 0.0399(18) 0.0091(15) 0.0048(15) -0.0041(17) C23 0.082(3) 0.093(3) 0.0355(19) 0.0115(18) 0.0123(18) 0.008(2) C24 0.090(3) 0.078(2) 0.066(3) 0.025(2) 0.043(2) 0.013(2) C25 0.079(3) 0.054(2) 0.080(3) 0.0084(19) 0.032(2) -0.0021(18) #------------------------------------------------------------------------------ _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^)+(0.0337P)^2^+0.5741P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6432 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0812 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.591 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.064 #------------------------------------------------------------------------------ _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C3 1.780(4) . ? Fe1 C2 1.791(4) . ? Fe1 C1 1.793(3) . ? Fe1 S2 2.2601(15) . ? Fe1 S1 2.2655(13) . ? Fe1 Fe2 2.5266(12) . ? Fe2 C4 1.767(3) . ? Fe2 C5 1.769(3) . ? Fe2 P1 2.2438(13) . ? Fe2 S1 2.2630(16) . ? Fe2 S2 2.2744(15) . ? S1 C6 1.822(3) . ? S2 C8 1.831(3) . ? P1 C9 1.824(3) . ? P1 C21 1.842(3) . ? P1 C15 1.843(3) . ? N1 C21 1.361(4) . ? N1 C25 1.374(4) . ? O1 C1 1.143(3) . ? O2 C2 1.134(4) . ? O3 C3 1.146(4) . ? O4 C4 1.145(4) . ? O5 C5 1.146(3) . ? C6 C7 1.473(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.463(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C14 1.380(4) . ? C9 C10 1.390(4) . ? C10 C11 1.379(4) . ? C10 H10A 0.9300 . ? C11 C12 1.372(5) . ? C11 H11A 0.9300 . ? C12 C13 1.368(5) . ? C12 H12A 0.9300 . ? C13 C14 1.387(4) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C16 1.361(4) . ? C15 C20 1.386(4) . ? C16 C17 1.382(4) . ? C16 H16A 0.9300 . ? C17 C18 1.355(4) . ? C17 H17A 0.9300 . ? C18 C19 1.367(5) . ? C18 H18A 0.9300 . ? C19 C20 1.381(4) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C22 1.381(4) . ? C22 C23 1.385(4) . ? C22 H22A 0.9300 . ? C23 C24 1.361(5) . ? C23 H23A 0.9300 . ? C24 C25 1.364(5) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Fe1 C2 93.15(16) . . ? C3 Fe1 C1 100.42(17) . . ? C2 Fe1 C1 100.04(14) . . ? C3 Fe1 S2 86.31(11) . . ? C2 Fe1 S2 157.49(11) . . ? C1 Fe1 S2 102.19(11) . . ? C3 Fe1 S1 157.81(12) . . ? C2 Fe1 S1 87.57(11) . . ? C1 Fe1 S1 101.28(12) . . ? S2 Fe1 S1 84.67(4) . . ? C3 Fe1 Fe2 102.30(12) . . ? C2 Fe1 Fe2 102.00(11) . . ? C1 Fe1 Fe2 147.19(10) . . ? S2 Fe1 Fe2 56.41(4) . . ? S1 Fe1 Fe2 56.04(4) . . ? C4 Fe2 C5 90.00(14) . . ? C4 Fe2 P1 94.79(11) . . ? C5 Fe2 P1 96.44(10) . . ? C4 Fe2 S1 85.92(10) . . ? C5 Fe2 S1 151.77(10) . . ? P1 Fe2 S1 111.73(3) . . ? C4 Fe2 S2 158.66(10) . . ? C5 Fe2 S2 89.58(10) . . ? P1 Fe2 S2 106.46(5) . . ? S1 Fe2 S2 84.40(3) . . ? C4 Fe2 Fe1 103.12(11) . . ? C5 Fe2 Fe1 98.00(10) . . ? P1 Fe2 Fe1 156.91(3) . . ? S1 Fe2 Fe1 56.13(3) . . ? S2 Fe2 Fe1 55.87(4) . . ? C6 S1 Fe2 116.59(12) . . ? C6 S1 Fe1 109.89(12) . . ? Fe2 S1 Fe1 67.82(3) . . ? C8 S2 Fe1 108.93(13) . . ? C8 S2 Fe2 116.07(12) . . ? Fe1 S2 Fe2 67.72(3) . . ? C9 P1 C21 102.60(13) . . ? C9 P1 C15 102.18(13) . . ? C21 P1 C15 101.07(12) . . ? C9 P1 Fe2 116.87(9) . . ? C21 P1 Fe2 113.48(10) . . ? C15 P1 Fe2 118.28(10) . . ? C21 N1 C25 117.2(3) . . ? O1 C1 Fe1 179.4(3) . . ? O2 C2 Fe1 178.7(3) . . ? O3 C3 Fe1 177.9(3) . . ? O4 C4 Fe2 177.8(3) . . ? O5 C5 Fe2 175.2(3) . . ? C7 C6 S1 117.4(2) . . ? C7 C6 H6A 107.9 . . ? S1 C6 H6A 107.9 . . ? C7 C6 H6B 107.9 . . ? S1 C6 H6B 107.9 . . ? H6A C6 H6B 107.2 . . ? C8 C7 C6 120.6(3) . . ? C8 C7 H7A 107.2 . . ? C6 C7 H7A 107.2 . . ? C8 C7 H7B 107.2 . . ? C6 C7 H7B 107.2 . . ? H7A C7 H7B 106.8 . . ? C7 C8 S2 117.8(3) . . ? C7 C8 H8A 107.9 . . ? S2 C8 H8A 107.9 . . ? C7 C8 H8B 107.9 . . ? S2 C8 H8B 107.9 . . ? H8A C8 H8B 107.2 . . ? C14 C9 C10 118.1(3) . . ? C14 C9 P1 123.1(2) . . ? C10 C9 P1 118.8(2) . . ? C11 C10 C9 120.7(3) . . ? C11 C10 H10A 119.7 . . ? C9 C10 H10A 119.7 . . ? C12 C11 C10 120.4(3) . . ? C12 C11 H11A 119.8 . . ? C10 C11 H11A 119.8 . . ? C13 C12 C11 119.8(3) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C12 C13 C14 119.9(3) . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C9 C14 C13 121.1(3) . . ? C9 C14 H14A 119.4 . . ? C13 C14 H14A 119.4 . . ? C16 C15 C20 118.4(3) . . ? C16 C15 P1 119.2(2) . . ? C20 C15 P1 122.3(2) . . ? C15 C16 C17 120.8(3) . . ? C15 C16 H16A 119.6 . . ? C17 C16 H16A 119.6 . . ? C18 C17 C16 121.0(3) . . ? C18 C17 H17A 119.5 . . ? C16 C17 H17A 119.5 . . ? C17 C18 C19 118.9(3) . . ? C17 C18 H18A 120.6 . . ? C19 C18 H18A 120.6 . . ? C18 C19 C20 120.7(3) . . ? C18 C19 H19A 119.6 . . ? C20 C19 H19A 119.6 . . ? C19 C20 C15 120.2(3) . . ? C19 C20 H20A 119.9 . . ? C15 C20 H20A 119.9 . . ? N1 C21 C22 121.5(3) . . ? N1 C21 P1 115.2(2) . . ? C22 C21 P1 123.3(2) . . ? C21 C22 C23 119.7(3) . . ? C21 C22 H22A 120.1 . . ? C23 C22 H22A 120.1 . . ? C24 C23 C22 119.1(3) . . ? C24 C23 H23A 120.4 . . ? C22 C23 H23A 120.4 . . ? C23 C24 C25 119.8(3) . . ? C23 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? C24 C25 N1 122.5(3) . . ? C24 C25 H25A 118.7 . . ? N1 C25 H25A 118.7 . . ? #===END # Copyright The Royal Society of Chemistry, 2006 # CCDC Number: 643388 data_3bH _database_code_depnum_ccdc_archive 'CCDC 643388' _audit_creation_date 'Oct 31 18:25:00 2006' _audit_creation_method SHELXL-97 _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP97 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Bruker, 1997)' #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 771.29 _chemical_formula_analytical ? _chemical_formula_sum 'C26 H21 F3 Fe2 N O8 P S3' _chemical_formula_moiety 'C25 H21 Fe2 N O5 P S2, C F3 O3 S' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 19.1778(6) _cell_length_b 8.7364(3) _cell_length_c 18.9530(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.071(2) _cell_angle_gamma 90.00 _cell_volume 3170.92(18) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2736 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 21.88 #------------------------------------------------------------------------------ _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 1.228 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5903 _exptl_absorpt_correction_T_max 0.8667 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14629 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7058 _reflns_number_gt 4115 _reflns_threshold_expression >2sigma(I) _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.969 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.39761(3) 0.74562(8) 0.13902(3) 0.0626(2) Uani 1 1 d . . . Fe2 Fe 0.31466(3) 0.94189(6) 0.08418(3) 0.04520(17) Uani 1 1 d . . . S1 S 0.42448(5) 0.90046(14) 0.04930(6) 0.0628(3) Uani 1 1 d . . . S2 S 0.30253(5) 0.68646(11) 0.06983(5) 0.0509(3) Uani 1 1 d . . . P1 P 0.24327(5) 1.03833(11) -0.00093(5) 0.0423(2) Uani 1 1 d . . . N1 N 0.11293(16) 1.1229(4) 0.04768(17) 0.0479(8) Uani 1 1 d . . . O1 O 0.4875(2) 0.4854(5) 0.1101(2) 0.1151(14) Uani 1 1 d . . . O2 O 0.4867(3) 0.9423(7) 0.2293(3) 0.178(3) Uani 1 1 d . . . O3 O 0.3265(3) 0.6187(7) 0.2586(2) 0.159(2) Uani 1 1 d . . . O4 O 0.3669(2) 1.2315(4) 0.1403(2) 0.1070(13) Uani 1 1 d . . . O5 O 0.21091(17) 0.9298(4) 0.19068(17) 0.0855(10) Uani 1 1 d . . . C1 C 0.4527(2) 0.5865(7) 0.1227(3) 0.0786(14) Uani 1 1 d . . . C2 C 0.4526(3) 0.8636(8) 0.1950(3) 0.105(2) Uani 1 1 d . . . C3 C 0.3542(3) 0.6692(7) 0.2124(3) 0.0992(19) Uani 1 1 d . . . C4 C 0.3463(2) 1.1182(6) 0.1177(2) 0.0658(12) Uani 1 1 d . . . C5 C 0.2513(2) 0.9340(5) 0.1479(2) 0.0559(10) Uani 1 1 d . . . C6 C 0.4302(2) 0.7907(6) -0.0315(2) 0.0753(14) Uani 1 1 d . . . H6A H 0.4502 0.8557 -0.0667 0.090 Uiso 1 1 calc R . . H6B H 0.4624 0.7064 -0.0222 0.090 Uiso 1 1 calc R . . C7 C 0.3633(2) 0.7271(5) -0.0622(2) 0.0704(13) Uani 1 1 d . . . H7A H 0.3727 0.6752 -0.1060 0.084 Uiso 1 1 calc R . . H7B H 0.3322 0.8118 -0.0741 0.084 Uiso 1 1 calc R . . C8 C 0.3259(2) 0.6175(5) -0.0163(2) 0.0628(11) Uani 1 1 d . . . H8A H 0.3551 0.5276 -0.0090 0.075 Uiso 1 1 calc R . . H8B H 0.2835 0.5849 -0.0421 0.075 Uiso 1 1 calc R . . C9 C 0.2746(2) 1.1697(4) -0.0671(2) 0.0492(9) Uani 1 1 d . . . C10 C 0.2287(2) 1.2604(5) -0.1069(2) 0.0614(11) Uani 1 1 d . . . H10A H 0.1815 1.2595 -0.0978 0.074 Uiso 1 1 calc R . . C11 C 0.2518(3) 1.3525(5) -0.1598(2) 0.0768(14) Uani 1 1 d . . . H11A H 0.2202 1.4127 -0.1865 0.092 Uiso 1 1 calc R . . C12 C 0.3203(4) 1.3552(6) -0.1730(3) 0.0880(16) Uani 1 1 d . . . H12A H 0.3359 1.4173 -0.2087 0.106 Uiso 1 1 calc R . . C13 C 0.3667(3) 1.2670(7) -0.1340(3) 0.0902(17) Uani 1 1 d . . . H13A H 0.4137 1.2693 -0.1436 0.108 Uiso 1 1 calc R . . C14 C 0.3448(2) 1.1736(5) -0.0799(2) 0.0670(12) Uani 1 1 d . . . H14A H 0.3768 1.1151 -0.0530 0.080 Uiso 1 1 calc R . . C15 C 0.18993(17) 0.9006(4) -0.05201(19) 0.0429(8) Uani 1 1 d . . . C16 C 0.15363(19) 0.7890(4) -0.0167(2) 0.0490(9) Uani 1 1 d . . . H16A H 0.1537 0.7917 0.0324 0.059 Uiso 1 1 calc R . . C17 C 0.1176(2) 0.6747(5) -0.0528(2) 0.0546(10) Uani 1 1 d . . . H17A H 0.0921 0.6034 -0.0284 0.066 Uiso 1 1 calc R . . C18 C 0.1194(2) 0.6664(5) -0.1245(2) 0.0608(11) Uani 1 1 d . . . H18A H 0.0961 0.5876 -0.1489 0.073 Uiso 1 1 calc R . . C19 C 0.1556(2) 0.7743(5) -0.1610(2) 0.0632(12) Uani 1 1 d . . . H19A H 0.1564 0.7683 -0.2100 0.076 Uiso 1 1 calc R . . C20 C 0.1907(2) 0.8915(5) -0.12506(19) 0.0528(10) Uani 1 1 d . . . H20A H 0.2148 0.9644 -0.1499 0.063 Uiso 1 1 calc R . . C21 C 0.17905(18) 1.1652(4) 0.03889(18) 0.0421(8) Uani 1 1 d . . . C22 C 0.1992(2) 1.3062(4) 0.0655(2) 0.0571(11) Uani 1 1 d . . . H22A H 0.2447 1.3400 0.0609 0.069 Uiso 1 1 calc R . . C23 C 0.1525(2) 1.3974(5) 0.0988(2) 0.0648(12) Uani 1 1 d . . . H23A H 0.1664 1.4923 0.1167 0.078 Uiso 1 1 calc R . . C24 C 0.0855(2) 1.3480(5) 0.1054(2) 0.0595(11) Uani 1 1 d . . . H24A H 0.0534 1.4091 0.1274 0.071 Uiso 1 1 calc R . . C25 C 0.0667(2) 1.2092(5) 0.0797(2) 0.0592(11) Uani 1 1 d . . . H25A H 0.0214 1.1736 0.0843 0.071 Uiso 1 1 calc R . . S3 S -0.00588(6) 1.23149(13) -0.11120(6) 0.0619(3) Uani 1 1 d . . . O6 O 0.0454(2) 1.3408(4) -0.09327(19) 0.1033(12) Uani 1 1 d . . . O7 O -0.0743(2) 1.2968(5) -0.1267(2) 0.1130(13) Uani 1 1 d . . . O8 O -0.0066(2) 1.1030(4) -0.06647(17) 0.0960(11) Uani 1 1 d . . . C26 C 0.0152(3) 1.1609(7) -0.1958(3) 0.0889(16) Uani 1 1 d . . . F1 F -0.0313(3) 1.0570(5) -0.2177(2) 0.174(2) Uani 1 1 d . . . F2 F 0.0738(3) 1.0934(7) -0.1936(2) 0.204(3) Uani 1 1 d . . . F3 F 0.0119(3) 1.2590(5) -0.24462(19) 0.1643(19) Uani 1 1 d . . . H1 H 0.098(2) 1.040(5) 0.031(2) 0.070(15) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0515(4) 0.0775(5) 0.0580(4) -0.0111(3) -0.0042(3) 0.0108(3) Fe2 0.0416(3) 0.0485(3) 0.0457(3) -0.0100(3) 0.0042(2) -0.0058(3) S1 0.0452(5) 0.0681(7) 0.0762(7) -0.0203(6) 0.0145(5) -0.0138(5) S2 0.0480(5) 0.0478(6) 0.0573(6) -0.0025(5) 0.0056(5) -0.0063(5) P1 0.0414(5) 0.0425(6) 0.0437(5) -0.0051(4) 0.0084(4) -0.0083(4) N1 0.0431(18) 0.044(2) 0.057(2) -0.0099(17) 0.0072(15) -0.0086(17) O1 0.097(3) 0.106(3) 0.142(4) -0.025(3) 0.008(3) 0.036(3) O2 0.151(4) 0.211(6) 0.162(5) -0.103(4) -0.072(4) 0.010(4) O3 0.161(4) 0.226(6) 0.094(3) 0.064(4) 0.044(3) 0.035(4) O4 0.104(3) 0.077(2) 0.138(3) -0.043(2) -0.003(2) -0.031(2) O5 0.088(2) 0.109(3) 0.0620(19) -0.0060(18) 0.0288(18) -0.003(2) C1 0.062(3) 0.094(4) 0.079(3) -0.011(3) -0.004(3) 0.005(3) C2 0.086(4) 0.135(5) 0.092(4) -0.041(4) -0.031(3) 0.019(4) C3 0.096(4) 0.134(5) 0.068(3) 0.009(4) 0.008(3) 0.036(4) C4 0.057(3) 0.068(3) 0.072(3) -0.014(3) -0.002(2) -0.009(2) C5 0.061(2) 0.063(3) 0.044(2) -0.009(2) 0.002(2) -0.001(2) C6 0.073(3) 0.079(3) 0.076(3) -0.019(3) 0.032(3) -0.005(3) C7 0.079(3) 0.076(3) 0.058(3) -0.018(2) 0.017(2) 0.004(3) C8 0.068(3) 0.056(3) 0.065(3) -0.021(2) 0.007(2) -0.002(2) C9 0.054(2) 0.046(2) 0.049(2) -0.0056(19) 0.0133(19) -0.014(2) C10 0.067(3) 0.063(3) 0.056(2) 0.003(2) 0.013(2) -0.014(2) C11 0.107(4) 0.067(3) 0.059(3) 0.011(2) 0.017(3) -0.013(3) C12 0.130(5) 0.068(3) 0.069(3) 0.009(3) 0.039(3) -0.026(4) C13 0.089(4) 0.086(4) 0.101(4) -0.001(3) 0.054(3) -0.029(3) C14 0.062(3) 0.066(3) 0.076(3) -0.002(2) 0.028(2) -0.012(2) C15 0.0387(19) 0.041(2) 0.050(2) -0.0054(17) 0.0063(16) 0.0001(17) C16 0.050(2) 0.049(2) 0.048(2) -0.0003(18) 0.0028(18) -0.0060(19) C17 0.049(2) 0.051(2) 0.064(3) -0.002(2) -0.003(2) -0.012(2) C18 0.060(3) 0.051(3) 0.069(3) -0.014(2) -0.009(2) -0.010(2) C19 0.074(3) 0.067(3) 0.047(2) -0.014(2) -0.002(2) -0.004(2) C20 0.057(2) 0.055(2) 0.047(2) -0.0049(19) 0.0107(19) -0.003(2) C21 0.044(2) 0.040(2) 0.043(2) 0.0051(17) 0.0078(16) -0.0043(17) C22 0.051(2) 0.046(2) 0.075(3) -0.009(2) 0.015(2) -0.011(2) C23 0.070(3) 0.048(3) 0.078(3) -0.014(2) 0.017(2) -0.006(2) C24 0.066(3) 0.047(2) 0.067(3) -0.003(2) 0.024(2) 0.006(2) C25 0.047(2) 0.060(3) 0.071(3) -0.004(2) 0.014(2) -0.005(2) S3 0.0789(8) 0.0503(6) 0.0575(7) 0.0009(5) 0.0119(6) -0.0157(6) O6 0.126(3) 0.079(2) 0.105(3) -0.012(2) 0.013(2) -0.056(2) O7 0.096(3) 0.128(3) 0.117(3) 0.002(2) 0.027(2) 0.034(3) O8 0.134(3) 0.073(2) 0.078(2) 0.0227(19) -0.013(2) -0.037(2) C26 0.101(4) 0.088(4) 0.077(4) -0.004(3) 0.004(3) 0.036(4) F1 0.267(6) 0.132(4) 0.114(3) -0.049(3) -0.067(3) 0.007(4) F2 0.178(4) 0.302(7) 0.134(3) -0.054(4) 0.006(3) 0.147(5) F3 0.266(5) 0.156(4) 0.077(2) 0.039(2) 0.063(3) 0.045(4) #------------------------------------------------------------------------------ _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^)+(0.0553P)^2^+0.5711P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7058 _refine_ls_number_parameters 401 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1008 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1317 _refine_ls_wR_factor_gt 0.1096 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.613 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.067 #------------------------------------------------------------------------------ _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 1.783(6) . ? Fe1 C2 1.784(6) . ? Fe1 C3 1.788(7) . ? Fe1 S2 2.2484(11) . ? Fe1 S1 2.2542(14) . ? Fe1 Fe2 2.5247(8) . ? Fe2 C5 1.759(4) . ? Fe2 C4 1.761(5) . ? Fe2 P1 2.2248(11) . ? Fe2 S2 2.2585(11) . ? Fe2 S1 2.2700(11) . ? S1 C6 1.816(4) . ? S2 C8 1.818(4) . ? P1 C15 1.823(4) . ? P1 C9 1.825(4) . ? P1 C21 1.848(4) . ? N1 C25 1.335(5) . ? N1 C21 1.340(4) . ? N1 H1 0.83(4) . ? O1 C1 1.140(5) . ? O2 C2 1.130(6) . ? O3 C3 1.139(6) . ? O4 C4 1.141(5) . ? O5 C5 1.152(4) . ? C6 C7 1.488(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.502(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.378(6) . ? C9 C14 1.382(5) . ? C10 C11 1.377(6) . ? C10 H10A 0.9300 . ? C11 C12 1.351(7) . ? C11 H11A 0.9300 . ? C12 C13 1.364(8) . ? C12 H12A 0.9300 . ? C13 C14 1.392(6) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C20 1.388(5) . ? C15 C16 1.391(5) . ? C16 C17 1.376(5) . ? C16 H16A 0.9300 . ? C17 C18 1.364(5) . ? C17 H17A 0.9300 . ? C18 C19 1.378(6) . ? C18 H18A 0.9300 . ? C19 C20 1.385(5) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C22 1.378(5) . ? C22 C23 1.377(5) . ? C22 H22A 0.9300 . ? C23 C24 1.366(5) . ? C23 H23A 0.9300 . ? C24 C25 1.349(5) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? S3 O6 1.400(3) . ? S3 O8 1.407(3) . ? S3 O7 1.446(4) . ? S3 C26 1.785(6) . ? C26 F3 1.260(6) . ? C26 F2 1.267(6) . ? C26 F1 1.323(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 C1 Fe1 C2 102.5(2) . . ? C1 Fe1 C3 98.5(3) . . ? C2 Fe1 C3 92.2(3) . . ? C1 Fe1 S2 100.90(15) . . ? C2 Fe1 S2 156.22(19) . . ? C3 Fe1 S2 88.33(19) . . ? C1 Fe1 S1 100.12(17) . . ? C2 Fe1 S1 87.2(2) . . ? C3 Fe1 S1 161.02(18) . . ? S2 Fe1 S1 84.78(4) . . ? C1 Fe1 Fe2 145.52(16) . . ? C2 Fe1 Fe2 101.1(2) . . ? C3 Fe1 Fe2 105.33(17) . . ? S2 Fe1 Fe2 56.12(3) . . ? S1 Fe1 Fe2 56.38(3) . . ? C5 Fe2 C4 91.36(19) . . ? C5 Fe2 P1 95.27(13) . . ? C4 Fe2 P1 96.70(15) . . ? C5 Fe2 S2 88.48(14) . . ? C4 Fe2 S2 159.84(15) . . ? P1 Fe2 S2 103.38(4) . . ? C5 Fe2 S1 151.52(13) . . ? C4 Fe2 S1 86.43(14) . . ? P1 Fe2 S1 113.19(4) . . ? S2 Fe2 S1 84.18(4) . . ? C5 Fe2 Fe1 97.68(13) . . ? C4 Fe2 Fe1 104.39(15) . . ? P1 Fe2 Fe1 154.88(4) . . ? S2 Fe2 Fe1 55.74(3) . . ? S1 Fe2 Fe1 55.78(4) . . ? C6 S1 Fe1 110.25(17) . . ? C6 S1 Fe2 115.42(16) . . ? Fe1 S1 Fe2 67.84(4) . . ? C8 S2 Fe1 111.60(14) . . ? C8 S2 Fe2 113.99(15) . . ? Fe1 S2 Fe2 68.14(3) . . ? C15 P1 C9 104.22(17) . . ? C15 P1 C21 104.20(16) . . ? C9 P1 C21 98.88(17) . . ? C15 P1 Fe2 116.17(12) . . ? C9 P1 Fe2 121.62(14) . . ? C21 P1 Fe2 109.20(11) . . ? C25 N1 C21 123.9(4) . . ? C25 N1 H1 116(3) . . ? C21 N1 H1 120(3) . . ? O1 C1 Fe1 177.9(5) . . ? O2 C2 Fe1 177.8(7) . . ? O3 C3 Fe1 179.0(7) . . ? O4 C4 Fe2 179.0(5) . . ? O5 C5 Fe2 178.6(4) . . ? C7 C6 S1 115.9(3) . . ? C7 C6 H6A 108.3 . . ? S1 C6 H6A 108.3 . . ? C7 C6 H6B 108.3 . . ? S1 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? C6 C7 C8 116.1(4) . . ? C6 C7 H7A 108.3 . . ? C8 C7 H7A 108.3 . . ? C6 C7 H7B 108.3 . . ? C8 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C7 C8 S2 117.2(3) . . ? C7 C8 H8A 108.0 . . ? S2 C8 H8A 108.0 . . ? C7 C8 H8B 108.0 . . ? S2 C8 H8B 108.0 . . ? H8A C8 H8B 107.2 . . ? C10 C9 C14 119.3(4) . . ? C10 C9 P1 120.9(3) . . ? C14 C9 P1 119.7(3) . . ? C11 C10 C9 120.9(4) . . ? C11 C10 H10A 119.5 . . ? C9 C10 H10A 119.5 . . ? C12 C11 C10 119.9(5) . . ? C12 C11 H11A 120.1 . . ? C10 C11 H11A 120.1 . . ? C11 C12 C13 120.1(5) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C12 C13 C14 121.1(5) . . ? C12 C13 H13A 119.4 . . ? C14 C13 H13A 119.4 . . ? C9 C14 C13 118.6(5) . . ? C9 C14 H14A 120.7 . . ? C13 C14 H14A 120.7 . . ? C20 C15 C16 118.2(3) . . ? C20 C15 P1 122.1(3) . . ? C16 C15 P1 119.2(3) . . ? C17 C16 C15 121.4(4) . . ? C17 C16 H16A 119.3 . . ? C15 C16 H16A 119.3 . . ? C18 C17 C16 119.7(4) . . ? C18 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? C17 C18 C19 120.3(4) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? C18 C19 C20 120.2(4) . . ? C18 C19 H19A 119.9 . . ? C20 C19 H19A 119.9 . . ? C19 C20 C15 120.2(4) . . ? C19 C20 H20A 119.9 . . ? C15 C20 H20A 119.9 . . ? N1 C21 C22 116.7(3) . . ? N1 C21 P1 122.8(3) . . ? C22 C21 P1 120.4(3) . . ? C23 C22 C21 120.5(4) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C24 C23 C22 119.8(4) . . ? C24 C23 H23A 120.1 . . ? C22 C23 H23A 120.1 . . ? C25 C24 C23 119.1(4) . . ? C25 C24 H24A 120.5 . . ? C23 C24 H24A 120.5 . . ? N1 C25 C24 120.0(4) . . ? N1 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? O6 S3 O8 115.3(2) . . ? O6 S3 O7 113.5(3) . . ? O8 S3 O7 113.5(2) . . ? O6 S3 C26 105.3(3) . . ? O8 S3 C26 106.0(3) . . ? O7 S3 C26 101.6(3) . . ? F3 C26 F2 110.5(6) . . ? F3 C26 F1 103.3(5) . . ? F2 C26 F1 105.7(6) . . ? F3 C26 S3 114.8(4) . . ? F2 C26 S3 112.0(4) . . ? F1 C26 S3 109.7(5) . . ? #===END # Copyright The Royal Society of Chemistry, 2006 # CCDC Number: 643389 data_4a _database_code_depnum_ccdc_archive 'CCDC 643389' _audit_creation_date 'Oct 31 18:25:00 2006' _audit_creation_method SHELXL-97 _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP97 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Bruker, 1997)' #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 683.30 _chemical_formula_analytical ? _chemical_formula_sum 'C28 H31 Fe2 N O4 P2 S2' _chemical_formula_moiety 'C28 H31 Fe2 N O4 P2 S2' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 9.6520(2) _cell_length_b 14.0097(3) _cell_length_c 11.7256(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.0120(10) _cell_angle_gamma 90.00 _cell_volume 1544.84(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8983 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 30.77 #------------------------------------------------------------------------------ _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _exptl_crystal_description cubic _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 1.211 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6430 _exptl_absorpt_correction_T_max 0.7127 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18855 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 30.00 _reflns_number_total 7618 _reflns_number_gt 6821 _reflns_threshold_expression >2sigma(I) _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.983 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.76175(3) 0.87283(2) 0.59402(2) 0.03565(7) Uani 1 1 d . . . Fe2 Fe 0.75405(3) 0.87468(2) 0.37505(2) 0.03415(7) Uani 1 1 d . . . S1 S 0.90701(6) 0.96103(4) 0.51062(5) 0.04035(12) Uani 1 1 d . B . S2 S 0.83319(7) 0.75068(4) 0.49578(5) 0.04548(13) Uani 1 1 d . B . P1 P 0.64713(6) 1.00290(4) 0.63365(5) 0.03963(12) Uani 1 1 d . . . P2 P 0.85685(6) 0.85906(4) 0.22443(4) 0.03507(11) Uani 1 1 d . . . N1 N 0.4963(3) 0.8961(3) 0.0510(2) 0.0837(9) Uani 1 1 d U . . O1 O 0.9185(3) 0.84491(16) 0.83404(15) 0.0731(6) Uani 1 1 d . . . O2 O 0.5070(3) 0.76547(19) 0.6021(3) 0.0960(8) Uani 1 1 d . . . O3 O 0.6202(2) 1.05510(15) 0.29421(19) 0.0690(6) Uani 1 1 d . . . O4 O 0.5005(3) 0.76267(19) 0.2832(2) 0.0853(7) Uani 1 1 d . . . C1 C 0.8572(3) 0.85669(18) 0.73964(18) 0.0473(5) Uani 1 1 d . . . C2 C 0.6077(3) 0.8074(2) 0.5987(2) 0.0565(6) Uani 1 1 d . . . C3 C 0.6710(2) 0.98377(18) 0.3254(2) 0.0450(5) Uani 1 1 d . . . C4 C 0.6002(3) 0.8064(2) 0.3176(2) 0.0524(6) Uani 1 1 d . . . C5 C 0.4695(3) 1.0230(3) 0.5455(3) 0.0728(9) Uani 1 1 d . . . H5A H 0.4315 1.0806 0.5705 0.109 Uiso 1 1 calc R . . H5B H 0.4095 0.9702 0.5547 0.109 Uiso 1 1 calc R . . H5C H 0.4733 1.0287 0.4647 0.109 Uiso 1 1 calc R . . C6 C 0.6174(4) 1.0046(3) 0.7808(3) 0.0845(11) Uani 1 1 d . . . H6A H 0.5680 1.0621 0.7922 0.127 Uiso 1 1 calc R . . H6B H 0.7071 1.0023 0.8363 0.127 Uiso 1 1 calc R . . H6C H 0.5612 0.9503 0.7918 0.127 Uiso 1 1 calc R . . C7 C 0.7294(4) 1.1177(2) 0.6243(3) 0.0684(8) Uani 1 1 d . . . H7A H 0.6697 1.1672 0.6435 0.103 Uiso 1 1 calc R . . H7B H 0.7418 1.1273 0.5461 0.103 Uiso 1 1 calc R . . H7C H 0.8203 1.1197 0.6783 0.103 Uiso 1 1 calc R . . C8 C 1.0884(3) 0.9149(2) 0.5436(2) 0.0596(7) Uani 1 1 d . . . H8A H 1.1225 0.9155 0.4718 0.072 Uiso 1 1 calc R A 1 H8B H 1.1476 0.9586 0.5976 0.072 Uiso 1 1 calc R A 1 C9 C 1.1101(4) 0.8180(4) 0.5939(3) 0.0773(15) Uani 0.810(8) 1 d P B 1 H9A H 1.2101 0.8022 0.6053 0.093 Uiso 0.810(8) 1 calc PR B 1 H9B H 1.0879 0.8194 0.6706 0.093 Uiso 0.810(8) 1 calc PR B 1 C9A C 1.1116(11) 0.8062(10) 0.5046(11) 0.041(4) Uani 0.190(8) 1 d P B 2 H9AA H 1.1060 0.8064 0.4210 0.050 Uiso 0.190(8) 1 calc PR B 2 H9AB H 1.2077 0.7875 0.5425 0.050 Uiso 0.190(8) 1 calc PR B 2 C10 C 1.0270(3) 0.7411(3) 0.5257(3) 0.0712(9) Uani 1 1 d . . . H10A H 1.0541 0.6815 0.5668 0.085 Uiso 1 1 calc R B 1 H10B H 1.0546 0.7369 0.4513 0.085 Uiso 1 1 calc R B 1 C11 C 1.0148(2) 0.93341(16) 0.23410(16) 0.0381(4) Uani 1 1 d . . . C12 C 0.9962(3) 1.03146(18) 0.2396(2) 0.0483(5) Uani 1 1 d . . . H12A H 0.9061 1.0564 0.2364 0.058 Uiso 1 1 calc R . . C13 C 1.1120(3) 1.0924(2) 0.2499(2) 0.0617(7) Uani 1 1 d . . . H13A H 1.0985 1.1580 0.2534 0.074 Uiso 1 1 calc R . . C14 C 1.2448(3) 1.0575(3) 0.2549(3) 0.0699(9) Uani 1 1 d . . . H14A H 1.3213 1.0989 0.2603 0.084 Uiso 1 1 calc R . . C15 C 1.2648(3) 0.9612(3) 0.2518(3) 0.0701(8) Uani 1 1 d . . . H15A H 1.3555 0.9369 0.2561 0.084 Uiso 1 1 calc R . . C16 C 1.1510(3) 0.8997(2) 0.2425(2) 0.0545(6) Uani 1 1 d . . . H16A H 1.1665 0.8342 0.2418 0.065 Uiso 1 1 calc R . . C17 C 0.9048(3) 0.74160(17) 0.17808(17) 0.0441(5) Uani 1 1 d . . . C18 C 0.9828(3) 0.7317(2) 0.0907(2) 0.0519(6) Uani 1 1 d . . . H18A H 1.0207 0.7857 0.0630 0.062 Uiso 1 1 calc R . . C19 C 1.0036(4) 0.6445(2) 0.0461(2) 0.0672(8) Uani 1 1 d . . . H19A H 1.0557 0.6393 -0.0114 0.081 Uiso 1 1 calc R . . C20 C 0.9481(4) 0.5647(2) 0.0856(3) 0.0732(9) Uani 1 1 d . . . H20A H 0.9617 0.5054 0.0542 0.088 Uiso 1 1 calc R . . C21 C 0.8721(5) 0.5714(2) 0.1718(3) 0.0800(10) Uani 1 1 d . . . H21A H 0.8342 0.5168 0.1982 0.096 Uiso 1 1 calc R . . C22 C 0.8523(4) 0.65982(19) 0.2189(2) 0.0599(7) Uani 1 1 d . . . H22A H 0.8033 0.6641 0.2785 0.072 Uiso 1 1 calc R . . C23 C 0.7504(3) 0.90367(19) 0.08158(18) 0.0461(5) Uani 1 1 d . . . H23A H 0.7296 0.9707 0.0903 0.055 Uiso 1 1 calc R . . H23B H 0.8085 0.8993 0.0242 0.055 Uiso 1 1 calc R . . C24 C 0.6122(3) 0.8521(2) 0.03419(18) 0.0572(7) Uani 1 1 d U . . C25 C 0.6093(4) 0.7682(3) -0.0266(3) 0.0840(10) Uani 1 1 d U . . H25A H 0.6927 0.7401 -0.0372 0.101 Uiso 1 1 calc R . . C26 C 0.4791(6) 0.7271(5) -0.0715(4) 0.1270(17) Uani 1 1 d U . . H26A H 0.4733 0.6695 -0.1119 0.152 Uiso 1 1 calc R . . C27 C 0.3594(5) 0.7708(5) -0.0567(4) 0.1295(18) Uani 1 1 d U . . H27A H 0.2705 0.7446 -0.0882 0.155 Uiso 1 1 calc R . . C28 C 0.3713(4) 0.8534(5) 0.0048(3) 0.1126(15) Uani 1 1 d U . . H28A H 0.2884 0.8822 0.0157 0.135 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.04539(15) 0.03253(14) 0.03245(12) 0.00128(13) 0.01598(10) 0.00139(14) Fe2 0.03947(14) 0.03376(15) 0.03091(12) 0.00295(13) 0.01146(9) -0.00102(14) S1 0.0429(3) 0.0428(3) 0.0384(2) -0.0042(2) 0.01570(19) -0.0050(2) S2 0.0660(4) 0.0351(3) 0.0380(2) 0.0017(2) 0.0174(2) 0.0103(3) P1 0.0440(3) 0.0395(3) 0.0390(2) 0.0021(2) 0.0169(2) 0.0044(2) P2 0.0446(3) 0.0331(3) 0.02865(19) 0.00198(19) 0.01076(18) -0.0006(2) N1 0.0526(13) 0.137(3) 0.0591(13) -0.0030(15) 0.0072(10) 0.0087(16) O1 0.1094(16) 0.0657(14) 0.0393(8) 0.0078(8) 0.0062(9) 0.0074(11) O2 0.0872(17) 0.0753(17) 0.140(2) -0.0094(16) 0.0557(17) -0.0297(15) O3 0.0761(13) 0.0562(12) 0.0750(13) 0.0180(10) 0.0174(10) 0.0247(10) O4 0.0710(13) 0.0894(17) 0.0899(15) 0.0084(13) 0.0061(11) -0.0413(13) C1 0.0690(15) 0.0375(12) 0.0385(10) 0.0016(9) 0.0186(9) 0.0045(10) C2 0.0663(16) 0.0441(14) 0.0661(15) -0.0070(12) 0.0294(12) -0.0065(13) C3 0.0440(12) 0.0493(14) 0.0429(11) 0.0046(10) 0.0124(9) 0.0025(10) C4 0.0567(15) 0.0511(14) 0.0500(12) 0.0067(11) 0.0134(11) -0.0100(12) C5 0.0461(14) 0.084(2) 0.087(2) -0.0093(17) 0.0119(13) 0.0149(15) C6 0.126(3) 0.086(2) 0.0563(16) 0.0088(16) 0.0503(17) 0.046(2) C7 0.0700(18) 0.0412(15) 0.103(2) -0.0090(14) 0.0396(17) 0.0010(13) C8 0.0391(12) 0.092(2) 0.0491(13) -0.0147(14) 0.0119(10) -0.0006(13) C9 0.051(2) 0.129(4) 0.051(2) 0.008(2) 0.0108(15) 0.036(2) C9A 0.027(5) 0.050(7) 0.047(7) -0.006(5) 0.010(4) 0.015(5) C10 0.071(2) 0.074(2) 0.0716(18) 0.0011(16) 0.0223(15) 0.0335(17) C11 0.0477(12) 0.0398(11) 0.0287(8) -0.0009(8) 0.0130(7) -0.0033(9) C12 0.0565(14) 0.0402(12) 0.0508(12) 0.0028(10) 0.0176(10) -0.0037(11) C13 0.083(2) 0.0510(16) 0.0525(14) 0.0002(12) 0.0173(13) -0.0198(14) C14 0.0568(17) 0.095(3) 0.0583(15) -0.0076(16) 0.0143(12) -0.0310(17) C15 0.0446(14) 0.091(2) 0.0741(18) -0.0170(17) 0.0118(12) -0.0093(15) C16 0.0480(13) 0.0612(17) 0.0539(12) -0.0087(11) 0.0108(10) 0.0008(11) C17 0.0634(14) 0.0360(11) 0.0326(9) -0.0023(8) 0.0102(9) 0.0036(10) C18 0.0686(16) 0.0500(15) 0.0390(10) -0.0066(10) 0.0163(10) 0.0024(12) C19 0.090(2) 0.069(2) 0.0439(12) -0.0141(13) 0.0194(13) 0.0125(17) C20 0.118(3) 0.0457(16) 0.0554(15) -0.0138(13) 0.0175(16) 0.0133(17) C21 0.139(3) 0.0402(15) 0.0614(17) -0.0037(13) 0.0240(19) -0.0023(18) C22 0.101(2) 0.0396(13) 0.0414(12) -0.0039(10) 0.0221(12) -0.0048(14) C23 0.0521(13) 0.0536(14) 0.0328(9) 0.0073(9) 0.0099(8) 0.0009(11) C24 0.0511(13) 0.088(2) 0.0315(9) 0.0050(11) 0.0071(8) -0.0037(13) C25 0.075(2) 0.107(3) 0.0655(17) -0.0260(18) 0.0079(14) -0.0229(19) C26 0.102(3) 0.172(4) 0.099(3) -0.050(3) 0.006(2) -0.049(3) C27 0.077(2) 0.221(5) 0.086(2) -0.033(3) 0.008(2) -0.058(3) C28 0.0579(17) 0.202(5) 0.077(2) -0.012(3) 0.0122(15) -0.004(3) #------------------------------------------------------------------------------ _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^)+(0.0405P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.016(10) _refine_ls_number_reflns 7618 _refine_ls_number_parameters 362 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0717 _refine_ls_wR_factor_gt 0.0691 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.426 _refine_diff_density_min -0.236 _refine_diff_density_rms 0.053 #------------------------------------------------------------------------------ _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C2 1.758(3) . ? Fe1 C1 1.763(2) . ? Fe1 P1 2.2342(7) . ? Fe1 S1 2.2507(6) . ? Fe1 S2 2.2558(6) . ? Fe1 Fe2 2.5519(3) . ? Fe2 C3 1.763(3) . ? Fe2 C4 1.767(3) . ? Fe2 P2 2.2227(6) . ? Fe2 S1 2.2613(6) . ? Fe2 S2 2.2623(6) . ? S1 C8 1.825(3) . ? S2 C10 1.829(3) . ? P1 C7 1.808(3) . ? P1 C6 1.812(3) . ? P1 C5 1.814(3) . ? P2 C17 1.825(2) . ? P2 C11 1.828(2) . ? P2 C23 1.865(2) . ? N1 C24 1.331(4) . ? N1 C28 1.347(5) . ? O1 C1 1.143(3) . ? O2 C2 1.144(3) . ? O3 C3 1.137(3) . ? O4 C4 1.136(3) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.476(6) . ? C8 C9A 1.619(13) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.468(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9A C10 1.285(14) . ? C9A H9AA 0.9700 . ? C9A H9AB 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C16 1.380(3) . ? C11 C12 1.389(3) . ? C12 C13 1.390(4) . ? C12 H12A 0.9300 . ? C13 C14 1.361(5) . ? C13 H13A 0.9300 . ? C14 C15 1.364(5) . ? C14 H14A 0.9300 . ? C15 C16 1.381(4) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C17 C22 1.381(4) . ? C17 C18 1.408(3) . ? C18 C19 1.363(4) . ? C18 H18A 0.9300 . ? C19 C20 1.365(5) . ? C19 H19A 0.9300 . ? C20 C21 1.380(5) . ? C20 H20A 0.9300 . ? C21 C22 1.387(4) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.509(4) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.371(5) . ? C25 C26 1.375(6) . ? C25 H25A 0.9300 . ? C26 C27 1.353(7) . ? C26 H26A 0.9300 . ? C27 C28 1.355(9) . ? C27 H27A 0.9300 . ? C28 H28A 0.9300 . ? #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Fe1 C1 99.45(13) . . ? C2 Fe1 P1 87.52(10) . . ? C1 Fe1 P1 94.49(8) . . ? C2 Fe1 S1 156.01(10) . . ? C1 Fe1 S1 104.51(9) . . ? P1 Fe1 S1 91.64(3) . . ? C2 Fe1 S2 88.76(9) . . ? C1 Fe1 S2 104.14(8) . . ? P1 Fe1 S2 161.36(2) . . ? S1 Fe1 S2 84.41(2) . . ? C2 Fe1 Fe2 101.72(9) . . ? C1 Fe1 Fe2 150.05(8) . . ? P1 Fe1 Fe2 107.301(18) . . ? S1 Fe1 Fe2 55.752(16) . . ? S2 Fe1 Fe2 55.730(16) . . ? C3 Fe2 C4 93.58(13) . . ? C3 Fe2 P2 94.26(8) . . ? C4 Fe2 P2 97.52(9) . . ? C3 Fe2 S1 86.82(8) . . ? C4 Fe2 S1 156.51(9) . . ? P2 Fe2 S1 105.88(2) . . ? C3 Fe2 S2 159.51(8) . . ? C4 Fe2 S2 87.68(9) . . ? P2 Fe2 S2 105.87(2) . . ? S1 Fe2 S2 84.02(2) . . ? C3 Fe2 Fe1 104.41(8) . . ? C4 Fe2 Fe1 102.11(8) . . ? P2 Fe2 Fe1 151.802(19) . . ? S1 Fe2 Fe1 55.362(17) . . ? S2 Fe2 Fe1 55.489(17) . . ? C8 S1 Fe1 112.05(11) . . ? C8 S1 Fe2 113.75(10) . . ? Fe1 S1 Fe2 68.885(19) . . ? C10 S2 Fe1 112.00(11) . . ? C10 S2 Fe2 111.28(12) . . ? Fe1 S2 Fe2 68.78(2) . . ? C7 P1 C6 102.25(18) . . ? C7 P1 C5 101.49(17) . . ? C6 P1 C5 102.01(17) . . ? C7 P1 Fe1 117.92(10) . . ? C6 P1 Fe1 113.63(11) . . ? C5 P1 Fe1 117.18(12) . . ? C17 P2 C11 105.56(11) . . ? C17 P2 C23 99.21(10) . . ? C11 P2 C23 98.49(10) . . ? C17 P2 Fe2 120.92(8) . . ? C11 P2 Fe2 114.19(7) . . ? C23 P2 Fe2 115.26(8) . . ? C24 N1 C28 116.2(4) . . ? O1 C1 Fe1 179.0(2) . . ? O2 C2 Fe1 179.4(3) . . ? O3 C3 Fe2 178.5(2) . . ? O4 C4 Fe2 178.4(3) . . ? P1 C5 H5A 109.5 . . ? P1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P1 C6 H6A 109.5 . . ? P1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P1 C7 H7A 109.5 . . ? P1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C9A 39.9(5) . . ? C9 C8 S1 117.0(2) . . ? C9A C8 S1 117.4(4) . . ? C9 C8 H8A 108.1 . . ? C9A C8 H8A 70.6 . . ? S1 C8 H8A 108.1 . . ? C9 C8 H8B 108.1 . . ? C9A C8 H8B 132.9 . . ? S1 C8 H8B 108.1 . . ? H8A C8 H8B 107.3 . . ? C10 C9 C8 116.5(3) . . ? C10 C9 H9A 108.2 . . ? C8 C9 H9A 108.2 . . ? C10 C9 H9B 108.2 . . ? C8 C9 H9B 108.2 . . ? H9A C9 H9B 107.3 . . ? C10 C9A C8 118.6(8) . . ? C10 C9A H9AA 107.7 . . ? C8 C9A H9AA 107.7 . . ? C10 C9A H9AB 107.7 . . ? C8 C9A H9AB 107.7 . . ? H9AA C9A H9AB 107.1 . . ? C9A C10 C9 44.8(6) . . ? C9A C10 S2 125.3(5) . . ? C9 C10 S2 117.4(2) . . ? C9A C10 H10A 126.5 . . ? C9 C10 H10A 107.9 . . ? S2 C10 H10A 107.9 . . ? C9A C10 H10B 63.6 . . ? C9 C10 H10B 107.9 . . ? S2 C10 H10B 107.9 . . ? H10A C10 H10B 107.2 . . ? C16 C11 C12 117.8(2) . . ? C16 C11 P2 125.24(19) . . ? C12 C11 P2 116.85(18) . . ? C11 C12 C13 120.1(3) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C14 C13 C12 120.9(3) . . ? C14 C13 H13A 119.5 . . ? C12 C13 H13A 119.5 . . ? C13 C14 C15 119.5(3) . . ? C13 C14 H14A 120.3 . . ? C15 C14 H14A 120.3 . . ? C14 C15 C16 120.3(3) . . ? C14 C15 H15A 119.8 . . ? C16 C15 H15A 119.8 . . ? C11 C16 C15 121.3(3) . . ? C11 C16 H16A 119.3 . . ? C15 C16 H16A 119.3 . . ? C22 C17 C18 117.9(2) . . ? C22 C17 P2 120.5(2) . . ? C18 C17 P2 121.20(19) . . ? C19 C18 C17 121.1(3) . . ? C19 C18 H18A 119.4 . . ? C17 C18 H18A 119.4 . . ? C18 C19 C20 120.1(3) . . ? C18 C19 H19A 119.9 . . ? C20 C19 H19A 119.9 . . ? C19 C20 C21 120.5(3) . . ? C19 C20 H20A 119.8 . . ? C21 C20 H20A 119.8 . . ? C20 C21 C22 119.7(3) . . ? C20 C21 H21A 120.1 . . ? C22 C21 H21A 120.1 . . ? C17 C22 C21 120.6(3) . . ? C17 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C24 C23 P2 115.64(17) . . ? C24 C23 H23A 108.4 . . ? P2 C23 H23A 108.4 . . ? C24 C23 H23B 108.4 . . ? P2 C23 H23B 108.4 . . ? H23A C23 H23B 107.4 . . ? N1 C24 C25 123.7(3) . . ? N1 C24 C23 115.2(3) . . ? C25 C24 C23 121.0(3) . . ? C24 C25 C26 117.9(4) . . ? C24 C25 H25A 121.0 . . ? C26 C25 H25A 121.0 . . ? C27 C26 C25 119.6(5) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C26 C27 C28 118.9(4) . . ? C26 C27 H27A 120.6 . . ? C28 C27 H27A 120.6 . . ? N1 C28 C27 123.7(5) . . ? N1 C28 H28A 118.1 . . ? C27 C28 H28A 118.1 . . ? #===END # Copyright The Royal Society of Chemistry, 2006 # CCDC Number: 643390 data_4b _database_code_depnum_ccdc_archive 'CCDC 643390' _audit_creation_date 'Oct 31 18:25:00 2006' _audit_creation_method SHELXL-97 _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP97 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Bruker, 1997)' #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 712.36 _chemical_formula_analytical ? _chemical_formula_sum 'C30 H36 Fe2 N O4 P2 S2' _chemical_formula_moiety 'C30 H36 Fe2 N O4 P2 S2' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 9.1648(18) _cell_length_b 12.253(2) _cell_length_c 15.845(3) _cell_angle_alpha 82.194(2) _cell_angle_beta 77.273(2) _cell_angle_gamma 73.081(2) _cell_volume 1655.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3581 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 27.21 #------------------------------------------------------------------------------ _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 738 _exptl_absorpt_coefficient_mu 1.133 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7274 _exptl_absorpt_correction_T_max 0.9561 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9005 _diffrn_reflns_av_R_equivalents 0.0166 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6349 _reflns_number_gt 5118 _reflns_threshold_expression >2sigma(I) _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.976 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.65887(4) 0.74993(3) 0.65762(2) 0.03813(11) Uani 1 1 d . . . Fe2 Fe 0.76386(3) 0.56368(3) 0.74422(2) 0.03135(10) Uani 1 1 d . . . S1 S 0.51738(7) 0.62693(5) 0.71910(4) 0.03916(15) Uani 1 1 d . . . S2 S 0.83049(7) 0.59563(5) 0.59679(4) 0.03875(15) Uani 1 1 d . . . P1 P 0.84382(9) 0.84083(6) 0.64163(5) 0.05144(19) Uani 1 1 d . . . P2 P 0.77961(6) 0.38210(5) 0.79604(4) 0.03070(14) Uani 1 1 d . . . N1 N 0.9292(3) 0.3834(2) 0.92403(16) 0.0584(6) Uani 1 1 d . . . O1 O 0.4928(3) 0.8605(2) 0.51832(16) 0.0951(8) Uani 1 1 d . . . O2 O 0.4705(3) 0.90667(19) 0.78713(16) 0.0857(8) Uani 1 1 d . . . O3 O 0.6662(3) 0.66286(19) 0.91115(14) 0.0724(6) Uani 1 1 d . . . O4 O 1.0852(2) 0.54973(19) 0.74634(15) 0.0703(6) Uani 1 1 d . . . C1 C 0.5623(3) 0.8189(2) 0.57218(19) 0.0550(7) Uani 1 1 d . . . C2 C 0.5463(3) 0.8447(2) 0.73647(19) 0.0543(7) Uani 1 1 d . . . C3 C 0.7011(3) 0.6227(2) 0.84585(18) 0.0437(6) Uani 1 1 d . . . C4 C 0.9581(3) 0.5530(2) 0.74655(17) 0.0437(6) Uani 1 1 d . . . C5 C 1.0382(3) 0.7795(3) 0.5809(3) 0.0779(10) Uani 1 1 d . . . H5A H 1.1027 0.8289 0.5804 0.117 Uiso 1 1 calc R . . H5B H 1.0321 0.7716 0.5224 0.117 Uiso 1 1 calc R . . H5C H 1.0820 0.7057 0.6079 0.117 Uiso 1 1 calc R . . C6 C 0.8825(5) 0.8689(3) 0.7431(2) 0.0923(12) Uani 1 1 d . . . H6A H 0.9627 0.9079 0.7310 0.139 Uiso 1 1 calc R . . H6B H 0.9158 0.7978 0.7764 0.139 Uiso 1 1 calc R . . H6C H 0.7896 0.9158 0.7754 0.139 Uiso 1 1 calc R . . C7 C 0.7965(4) 0.9847(3) 0.5880(3) 0.0801(11) Uani 1 1 d . . . H7A H 0.8810 1.0179 0.5836 0.120 Uiso 1 1 calc R . . H7B H 0.7041 1.0311 0.6212 0.120 Uiso 1 1 calc R . . H7C H 0.7795 0.9809 0.5310 0.120 Uiso 1 1 calc R . . C8 C 0.4823(3) 0.5476(2) 0.63920(18) 0.0513(7) Uani 1 1 d . . . H8A H 0.4136 0.5017 0.6693 0.062 Uiso 1 1 calc R . . H8B H 0.4276 0.6024 0.5988 0.062 Uiso 1 1 calc R . . C9 C 0.6228(3) 0.4701(2) 0.58769(18) 0.0517(7) Uani 1 1 d . . . H9A H 0.5887 0.4312 0.5495 0.062 Uiso 1 1 calc R . . H9B H 0.6750 0.4123 0.6274 0.062 Uiso 1 1 calc R . . C10 C 0.7376(3) 0.5305(2) 0.53406(16) 0.0493(7) Uani 1 1 d . . . H10A H 0.6845 0.5897 0.4955 0.059 Uiso 1 1 calc R . . H10B H 0.8177 0.4760 0.4982 0.059 Uiso 1 1 calc R . . C11 C 0.6085(3) 0.3318(2) 0.80008(15) 0.0357(5) Uani 1 1 d . . . C12 C 0.4664(3) 0.3935(2) 0.84470(17) 0.0437(6) Uani 1 1 d . . . H12A H 0.4618 0.4553 0.8743 0.052 Uiso 1 1 calc R . . C13 C 0.3322(3) 0.3636(3) 0.8453(2) 0.0563(8) Uani 1 1 d . . . H13A H 0.2377 0.4048 0.8757 0.068 Uiso 1 1 calc R . . C14 C 0.3379(3) 0.2742(3) 0.8015(2) 0.0738(10) Uani 1 1 d . . . H14A H 0.2472 0.2545 0.8015 0.089 Uiso 1 1 calc R . . C15 C 0.4778(4) 0.2127(3) 0.7572(3) 0.0761(10) Uani 1 1 d . . . H15A H 0.4812 0.1515 0.7273 0.091 Uiso 1 1 calc R . . C16 C 0.6130(3) 0.2408(2) 0.7567(2) 0.0534(7) Uani 1 1 d . . . H16A H 0.7072 0.1982 0.7271 0.064 Uiso 1 1 calc R . . C17 C 0.9412(2) 0.26845(19) 0.74563(15) 0.0346(5) Uani 1 1 d . . . C18 C 1.0205(3) 0.2886(2) 0.66279(17) 0.0492(7) Uani 1 1 d . . . H18A H 0.9907 0.3595 0.6327 0.059 Uiso 1 1 calc R . . C19 C 1.1438(3) 0.2038(3) 0.6244(2) 0.0657(9) Uani 1 1 d . . . H19A H 1.1957 0.2179 0.5684 0.079 Uiso 1 1 calc R . . C20 C 1.1902(3) 0.0993(3) 0.6679(2) 0.0603(8) Uani 1 1 d . . . H20A H 1.2737 0.0429 0.6418 0.072 Uiso 1 1 calc R . . C21 C 1.1133(3) 0.0781(2) 0.7503(2) 0.0550(7) Uani 1 1 d . . . H21A H 1.1445 0.0071 0.7802 0.066 Uiso 1 1 calc R . . C22 C 0.9894(3) 0.1621(2) 0.78914(18) 0.0444(6) Uani 1 1 d . . . H22A H 0.9377 0.1472 0.8451 0.053 Uiso 1 1 calc R . . C23 C 0.8055(3) 0.35470(19) 0.91036(15) 0.0347(5) Uani 1 1 d . . . C24 C 0.7095(3) 0.3100(3) 0.97609(18) 0.0554(7) Uani 1 1 d . . . H24A H 0.6256 0.2902 0.9646 0.067 Uiso 1 1 calc R . . C25 C 0.7381(4) 0.2947(3) 1.0594(2) 0.0723(9) Uani 1 1 d . . . H25A H 0.6744 0.2641 1.1046 0.087 Uiso 1 1 calc R . . C26 C 0.8602(4) 0.3249(3) 1.0744(2) 0.0706(9) Uani 1 1 d . . . H26A H 0.8804 0.3171 1.1303 0.085 Uiso 1 1 calc R . . C27 C 0.9526(4) 0.3668(3) 1.0066(2) 0.0730(10) Uani 1 1 d . . . H27A H 1.0378 0.3853 1.0177 0.088 Uiso 1 1 calc R . . C28 C 0.185(3) 1.0279(15) 1.0091(15) 0.435(18) Uani 1 1 d U . . H28A H 0.0942 1.0893 1.0261 0.653 Uiso 1 1 calc R . . H28B H 0.1857 0.9639 1.0515 0.653 Uiso 1 1 calc R . . H28C H 0.1833 1.0054 0.9537 0.653 Uiso 1 1 calc R . . C29 C 0.305(4) 1.0606(13) 1.0041(14) 0.430(17) Uani 1 1 d U . . H29A H 0.2848 1.1137 1.0481 0.516 Uiso 1 1 calc R . . H29C H 0.3257 1.1016 0.9479 0.516 Uiso 1 1 calc R . . C30 C 0.443(4) 0.9668(13) 1.0152(10) 0.414(17) Uani 1 1 d U . . H30A H 0.4585 0.9052 0.9788 0.497 Uiso 1 1 calc R . . H30B H 0.4403 0.9369 1.0752 0.497 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.03637(19) 0.0368(2) 0.0351(2) 0.00039(15) -0.00401(15) -0.00403(15) Fe2 0.02843(17) 0.03555(19) 0.03050(19) -0.00123(14) -0.00648(13) -0.00928(13) S1 0.0293(3) 0.0512(4) 0.0349(3) -0.0019(3) -0.0049(2) -0.0093(3) S2 0.0340(3) 0.0430(3) 0.0337(3) -0.0025(3) -0.0015(2) -0.0058(3) P1 0.0555(4) 0.0411(4) 0.0575(5) 0.0070(3) -0.0121(4) -0.0166(3) P2 0.0263(3) 0.0361(3) 0.0307(3) -0.0023(2) -0.0046(2) -0.0106(2) N1 0.0622(15) 0.0715(16) 0.0555(15) 0.0129(12) -0.0303(12) -0.0334(13) O1 0.0806(16) 0.116(2) 0.0665(16) 0.0167(14) -0.0318(13) 0.0107(15) O2 0.0920(17) 0.0669(15) 0.0744(16) -0.0270(13) 0.0094(14) 0.0062(13) O3 0.0852(16) 0.0791(15) 0.0514(13) -0.0275(11) -0.0136(12) -0.0095(12) O4 0.0419(11) 0.0884(16) 0.0887(17) 0.0208(13) -0.0278(11) -0.0309(11) C1 0.0462(16) 0.0582(18) 0.0472(17) 0.0022(14) -0.0042(13) 0.0005(13) C2 0.0530(17) 0.0482(16) 0.0510(17) -0.0015(14) -0.0015(14) -0.0043(13) C3 0.0427(14) 0.0430(14) 0.0463(16) -0.0048(12) -0.0117(12) -0.0102(11) C4 0.0443(15) 0.0446(15) 0.0443(15) 0.0090(11) -0.0136(12) -0.0167(12) C5 0.0513(18) 0.066(2) 0.111(3) 0.0115(19) -0.0047(19) -0.0236(16) C6 0.125(3) 0.095(3) 0.087(3) 0.002(2) -0.043(2) -0.064(3) C7 0.088(2) 0.0481(18) 0.098(3) 0.0186(18) -0.016(2) -0.0209(17) C8 0.0450(15) 0.0715(19) 0.0455(16) -0.0025(14) -0.0189(13) -0.0214(14) C9 0.0614(17) 0.0604(17) 0.0423(16) -0.0091(13) -0.0211(13) -0.0197(14) C10 0.0564(16) 0.0572(17) 0.0333(14) -0.0123(12) -0.0108(12) -0.0080(13) C11 0.0306(12) 0.0418(13) 0.0385(14) 0.0001(11) -0.0106(10) -0.0140(10) C12 0.0345(13) 0.0458(15) 0.0504(16) -0.0016(12) -0.0058(11) -0.0128(11) C13 0.0317(13) 0.0652(19) 0.070(2) 0.0031(15) -0.0055(13) -0.0161(13) C14 0.0404(16) 0.084(2) 0.111(3) -0.009(2) -0.0221(18) -0.0315(16) C15 0.059(2) 0.072(2) 0.116(3) -0.028(2) -0.024(2) -0.0300(17) C16 0.0408(14) 0.0536(17) 0.072(2) -0.0189(14) -0.0117(14) -0.0146(13) C17 0.0281(11) 0.0381(13) 0.0385(14) -0.0065(10) -0.0058(10) -0.0093(10) C18 0.0466(15) 0.0500(16) 0.0407(15) -0.0018(12) -0.0022(12) -0.0026(12) C19 0.0567(18) 0.069(2) 0.0500(18) -0.0088(15) 0.0095(15) 0.0026(15) C20 0.0462(16) 0.0560(18) 0.069(2) -0.0235(16) -0.0029(15) 0.0032(14) C21 0.0489(16) 0.0376(15) 0.075(2) -0.0075(14) -0.0158(15) -0.0020(12) C22 0.0411(14) 0.0442(15) 0.0475(16) -0.0021(12) -0.0056(12) -0.0134(11) C23 0.0344(12) 0.0373(13) 0.0330(13) -0.0013(10) -0.0074(10) -0.0108(10) C24 0.0492(16) 0.081(2) 0.0406(16) 0.0019(14) -0.0069(13) -0.0287(15) C25 0.070(2) 0.104(3) 0.0360(17) 0.0083(17) -0.0011(15) -0.026(2) C26 0.094(3) 0.081(2) 0.0397(18) -0.0051(16) -0.0279(17) -0.017(2) C27 0.087(2) 0.084(2) 0.071(2) 0.0126(18) -0.049(2) -0.043(2) C28 0.86(5) 0.186(10) 0.225(10) 0.004(9) 0.02(2) -0.199(16) C29 0.87(5) 0.185(9) 0.233(9) -0.004(9) -0.03(2) -0.204(18) C30 0.86(5) 0.174(10) 0.233(10) 0.015(10) -0.07(2) -0.222(18) #------------------------------------------------------------------------------ _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^)+(0.0423P)^2^+0.1280P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6349 _refine_ls_number_parameters 370 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0860 _refine_ls_wR_factor_gt 0.0805 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.292 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.054 #------------------------------------------------------------------------------ _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C2 1.762(3) . ? Fe1 C1 1.764(3) . ? Fe1 P1 2.2385(9) . ? Fe1 S2 2.2525(7) . ? Fe1 S1 2.2548(8) . ? Fe1 Fe2 2.5437(6) . ? Fe2 C4 1.755(3) . ? Fe2 C3 1.765(3) . ? Fe2 P2 2.2392(8) . ? Fe2 S1 2.2705(8) . ? Fe2 S2 2.2903(8) . ? S1 C8 1.829(3) . ? S2 C10 1.826(3) . ? P1 C6 1.817(4) . ? P1 C5 1.824(3) . ? P1 C7 1.824(3) . ? P2 C11 1.830(2) . ? P2 C17 1.831(2) . ? P2 C23 1.852(2) . ? N1 C23 1.348(3) . ? N1 C27 1.351(4) . ? O1 C1 1.151(3) . ? O2 C2 1.147(3) . ? O3 C3 1.147(3) . ? O4 C4 1.153(3) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.504(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.505(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C16 1.374(3) . ? C11 C12 1.391(3) . ? C12 C13 1.380(3) . ? C12 H12A 0.9300 . ? C13 C14 1.357(4) . ? C13 H13A 0.9300 . ? C14 C15 1.375(4) . ? C14 H14A 0.9300 . ? C15 C16 1.377(4) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C17 C18 1.381(3) . ? C17 C22 1.387(3) . ? C18 C19 1.383(4) . ? C18 H18A 0.9300 . ? C19 C20 1.367(4) . ? C19 H19A 0.9300 . ? C20 C21 1.370(4) . ? C20 H20A 0.9300 . ? C21 C22 1.383(3) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.371(3) . ? C24 C25 1.380(4) . ? C24 H24A 0.9300 . ? C25 C26 1.352(5) . ? C25 H25A 0.9300 . ? C26 C27 1.356(4) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 C29 1.26(4) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.47(5) . ? C29 H29A 0.9700 . ? C29 H29C 0.9700 . ? C30 C30 1.47(4) 2_677 ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Fe1 C1 96.57(13) . . ? C2 Fe1 P1 87.97(10) . . ? C1 Fe1 P1 101.33(10) . . ? C2 Fe1 S2 160.67(10) . . ? C1 Fe1 S2 102.44(9) . . ? P1 Fe1 S2 91.67(3) . . ? C2 Fe1 S1 88.00(10) . . ? C1 Fe1 S1 101.46(10) . . ? P1 Fe1 S1 157.17(3) . . ? S2 Fe1 S1 84.86(3) . . ? C2 Fe1 Fe2 104.68(9) . . ? C1 Fe1 Fe2 147.66(10) . . ? P1 Fe1 Fe2 103.48(3) . . ? S2 Fe1 Fe2 56.66(2) . . ? S1 Fe1 Fe2 56.09(2) . . ? C4 Fe2 C3 91.11(12) . . ? C4 Fe2 P2 94.12(8) . . ? C3 Fe2 P2 96.20(9) . . ? C4 Fe2 S1 163.15(8) . . ? C3 Fe2 S1 90.11(8) . . ? P2 Fe2 S1 102.46(3) . . ? C4 Fe2 S2 86.27(9) . . ? C3 Fe2 S2 147.22(9) . . ? P2 Fe2 S2 116.57(3) . . ? S1 Fe2 S2 83.64(2) . . ? C4 Fe2 Fe1 107.65(8) . . ? C3 Fe2 Fe1 95.02(8) . . ? P2 Fe2 Fe1 155.26(2) . . ? S1 Fe2 Fe1 55.508(19) . . ? S2 Fe2 Fe1 55.245(19) . . ? C8 S1 Fe1 112.52(9) . . ? C8 S1 Fe2 112.97(9) . . ? Fe1 S1 Fe2 68.40(2) . . ? C10 S2 Fe1 110.30(9) . . ? C10 S2 Fe2 114.83(9) . . ? Fe1 S2 Fe2 68.10(2) . . ? C6 P1 C5 102.67(19) . . ? C6 P1 C7 101.31(17) . . ? C5 P1 C7 101.38(16) . . ? C6 P1 Fe1 114.30(12) . . ? C5 P1 Fe1 120.20(12) . . ? C7 P1 Fe1 114.45(12) . . ? C11 P2 C17 103.72(11) . . ? C11 P2 C23 102.19(11) . . ? C17 P2 C23 100.63(11) . . ? C11 P2 Fe2 116.32(8) . . ? C17 P2 Fe2 118.67(8) . . ? C23 P2 Fe2 112.95(8) . . ? C23 N1 C27 116.2(2) . . ? O1 C1 Fe1 176.0(3) . . ? O2 C2 Fe1 178.7(3) . . ? O3 C3 Fe2 177.0(2) . . ? O4 C4 Fe2 177.5(2) . . ? P1 C5 H5A 109.5 . . ? P1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? P1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P1 C6 H6A 109.5 . . ? P1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P1 C7 H7A 109.5 . . ? P1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 S1 116.70(18) . . ? C9 C8 H8A 108.1 . . ? S1 C8 H8A 108.1 . . ? C9 C8 H8B 108.1 . . ? S1 C8 H8B 108.1 . . ? H8A C8 H8B 107.3 . . ? C8 C9 C10 114.3(2) . . ? C8 C9 H9A 108.7 . . ? C10 C9 H9A 108.7 . . ? C8 C9 H9B 108.7 . . ? C10 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C9 C10 S2 114.69(18) . . ? C9 C10 H10A 108.6 . . ? S2 C10 H10A 108.6 . . ? C9 C10 H10B 108.6 . . ? S2 C10 H10B 108.6 . . ? H10A C10 H10B 107.6 . . ? C16 C11 C12 118.9(2) . . ? C16 C11 P2 122.94(18) . . ? C12 C11 P2 118.03(18) . . ? C13 C12 C11 120.5(3) . . ? C13 C12 H12A 119.8 . . ? C11 C12 H12A 119.8 . . ? C14 C13 C12 120.1(3) . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C13 C14 C15 119.9(3) . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C14 C15 C16 120.7(3) . . ? C14 C15 H15A 119.7 . . ? C16 C15 H15A 119.7 . . ? C11 C16 C15 120.0(3) . . ? C11 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C18 C17 C22 118.4(2) . . ? C18 C17 P2 119.84(18) . . ? C22 C17 P2 121.72(18) . . ? C17 C18 C19 120.3(3) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? C20 C19 C18 120.7(3) . . ? C20 C19 H19A 119.6 . . ? C18 C19 H19A 119.6 . . ? C19 C20 C21 119.7(2) . . ? C19 C20 H20A 120.2 . . ? C21 C20 H20A 120.2 . . ? C20 C21 C22 120.1(3) . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C21 C22 C17 120.8(2) . . ? C21 C22 H22A 119.6 . . ? C17 C22 H22A 119.6 . . ? N1 C23 C24 122.2(2) . . ? N1 C23 P2 113.55(17) . . ? C24 C23 P2 124.29(19) . . ? C23 C24 C25 119.5(3) . . ? C23 C24 H24A 120.2 . . ? C25 C24 H24A 120.2 . . ? C26 C25 C24 119.0(3) . . ? C26 C25 H25A 120.5 . . ? C24 C25 H25A 120.5 . . ? C25 C26 C27 118.8(3) . . ? C25 C26 H26A 120.6 . . ? C27 C26 H26A 120.6 . . ? N1 C27 C26 124.3(3) . . ? N1 C27 H27A 117.9 . . ? C26 C27 H27A 117.9 . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C28 C29 C30 113.5(15) . . ? C28 C29 H29A 108.9 . . ? C30 C29 H29A 108.9 . . ? C28 C29 H29C 108.9 . . ? C30 C29 H29C 108.9 . . ? H29A C29 H29C 107.7 . . ? C29 C30 C30 96.9(13) . 2_677 ? C29 C30 H30A 112.4 . . ? C30 C30 H30A 112.4 2_677 . ? C29 C30 H30B 112.4 . . ? C30 C30 H30B 112.4 2_677 . ? H30A C30 H30B 109.9 . . ? #===END