# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Mei Wang' _publ_contact_author_address ; State Key Laboratory of Fine Chemicals Dalian University of Technology Zhongshan Road 158-46, Dalian 11601 Dalian 116012 CHINA ; _publ_contact_author_email SYMBUENO@DLUT.EDU.CN _publ_section_title ; An insight into the protonation property of a diiron azadithiolate complex pertinent to the active site of Fe-only hydrogenases ; loop_ _publ_author_name 'Mei Wang' 'Weibing Dong' 'Kun Jin' 'Guanghua Li' 'Xiaoyang Liu' ; Licheng Sun ; 'Fujiun Wang' # Attachment 'ChemCommunB513270C-(revised).cif' # Copyright The Royal Society of Chemistry, 2005 # CCDC Number: 246474 data_NO2-2P _database_code_depnum_ccdc_archive 'CCDC 246474' #------------------------------------------------------------------------------ _audit_creation_date 'Jul 10 10:01:24 2005' _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 604.17 _chemical_formula_analytical ? _chemical_formula_sum 'C18 H26 Fe2 N2 O6 P2 S2' _chemical_formula_moiety 'C18 H26 Fe2 N2 O6 P2 S2' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 13.248(3) _cell_length_b 14.676(3) _cell_length_c 15.028(3) _cell_angle_alpha 64.96(3) _cell_angle_beta 82.40(3) _cell_angle_gamma 82.83(3) _cell_volume 2616.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? #------------------------------------------------------------------------------ _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 'deep red' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.534 _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 1.425 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2813 _exptl_absorpt_correction_T_max 0.3448 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD area-detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_decay_% none _diffrn_reflns_number 25865 _reflns_number_observed 7847 _reflns_number_total 11823 _reflns_observed_criterion >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.46 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.987 #------------------------------------------------------------------------------ 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 0.68339(3) -0.17752(3) -0.27674(4) 0.03988(13) Uani 1 1 d . . . Fe3 Fe 0.15318(4) 0.25541(4) -0.18201(4) 0.04700(14) Uani 1 1 d . . . Fe2 Fe 0.54304(4) -0.29489(4) -0.24934(4) 0.04302(14) Uani 1 1 d . . . Fe4 Fe 0.20810(5) 0.41308(5) -0.32778(4) 0.05901(17) Uani 1 1 d . . . S2 S 0.62321(7) -0.29075(6) -0.12720(7) 0.0458(2) Uani 1 1 d . . . S1 S 0.51711(7) -0.12573(7) -0.30094(7) 0.0460(2) Uani 1 1 d . . . S3 S 0.04609(7) 0.39403(8) -0.25483(8) 0.0542(2) Uani 1 1 d . . . S4 S 0.25263(7) 0.36491(9) -0.17106(8) 0.0571(3) Uani 1 1 d . . . P2 P 0.60611(7) -0.45424(7) -0.21415(8) 0.0488(2) Uani 1 1 d . . . P1 P 0.72341(8) -0.07677(8) -0.43271(8) 0.0581(3) Uani 1 1 d . . . P3 P 0.05524(9) 0.16183(9) -0.21212(9) 0.0624(3) Uani 1 1 d . . . P4 P 0.20940(10) 0.58055(10) -0.40631(9) 0.0724(3) Uani 1 1 d . . . C31 C 0.0196(3) 0.3620(3) -0.0042(3) 0.0483(9) Uani 1 1 d . . . C1 C 0.7775(3) -0.2664(3) -0.2898(3) 0.0521(9) Uani 1 1 d . . . C13 C 0.5613(3) -0.0479(3) -0.1126(3) 0.0475(9) Uani 1 1 d . . . C36 C -0.0745(3) 0.3281(3) -0.0059(3) 0.0549(10) Uani 1 1 d . . . H36A H -0.1026 0.3485 -0.0655 0.066 Uiso 1 1 calc R . . C2 C 0.7525(3) -0.1025(3) -0.2438(3) 0.0510(9) Uani 1 1 d . . . C12 C 0.4490(3) -0.1029(3) -0.1955(3) 0.0568(10) Uani 1 1 d . . . H12A H 0.4214 -0.0332 -0.2196 0.068 Uiso 1 1 calc R . . H12B H 0.3918 -0.1449 -0.1696 0.068 Uiso 1 1 calc R . . C17 C 0.6558(3) 0.0101(4) -0.0237(4) 0.0662(12) Uani 1 1 d . . . H17A H 0.6897 -0.0026 0.0312 0.079 Uiso 1 1 calc R . . C20 C 0.2598(3) 0.1893(3) -0.2161(4) 0.0662(12) Uani 1 1 d . . . C32 C 0.0596(3) 0.3293(3) 0.0869(3) 0.0569(10) Uani 1 1 d . . . H32A H 0.1221 0.3501 0.0898 0.068 Uiso 1 1 calc R . . C18 C 0.6141(3) -0.0668(3) -0.0313(3) 0.0576(10) Uani 1 1 d . . . H18A H 0.6210 -0.1319 0.0178 0.069 Uiso 1 1 calc R . . C34 C -0.0841(3) 0.2352(3) 0.1674(3) 0.0511(9) Uani 1 1 d . . . C14 C 0.5577(3) 0.0500(3) -0.1881(3) 0.0569(10) Uani 1 1 d . . . H14A H 0.5261 0.0634 -0.2445 0.068 Uiso 1 1 calc R . . C3 C 0.4217(3) -0.3321(3) -0.1872(3) 0.0581(10) Uani 1 1 d . . . C15 C 0.5998(3) 0.1256(3) -0.1797(4) 0.0694(13) Uani 1 1 d . . . H15A H 0.5964 0.1904 -0.2296 0.083 Uiso 1 1 calc R . . C19 C 0.1257(3) 0.1807(3) -0.0546(3) 0.0586(10) Uani 1 1 d . . . C33 C 0.0078(3) 0.2669(3) 0.1720(3) 0.0621(11) Uani 1 1 d . . . H33A H 0.0345 0.2461 0.2324 0.075 Uiso 1 1 calc R . . C29 C 0.1806(3) 0.4335(3) -0.1010(3) 0.0653(11) Uani 1 1 d . . . H29A H 0.2049 0.4065 -0.0359 0.078 Uiso 1 1 calc R . . H29B H 0.1952 0.5039 -0.1340 0.078 Uiso 1 1 calc R . . C35 C -0.1252(3) 0.2653(3) 0.0796(3) 0.0555(10) Uani 1 1 d . . . H35A H -0.1875 0.2431 0.0779 0.067 Uiso 1 1 calc R . . C11 C 0.5356(3) -0.2275(3) -0.0609(3) 0.0606(11) Uani 1 1 d . . . H11A H 0.4731 -0.2620 -0.0382 0.073 Uiso 1 1 calc R . . H11B H 0.5666 -0.2350 -0.0030 0.073 Uiso 1 1 calc R . . C30 C 0.0240(3) 0.4702(3) -0.1810(3) 0.0657(12) Uani 1 1 d . . . H30A H 0.0490 0.5360 -0.2209 0.079 Uiso 1 1 calc R . . H30B H -0.0491 0.4801 -0.1665 0.079 Uiso 1 1 calc R . . C16 C 0.6478(3) 0.1053(3) -0.0963(4) 0.0647(12) Uani 1 1 d . . . C4 C 0.5228(3) -0.2835(3) -0.3671(3) 0.0622(11) Uani 1 1 d . . . C6 C 0.6766(4) -0.0989(5) -0.5299(4) 0.0931(17) Uani 1 1 d . . . H6A H 0.7006 -0.0494 -0.5930 0.140 Uiso 1 1 calc R . . H6B H 0.6033 -0.0937 -0.5232 0.140 Uiso 1 1 calc R . . H6C H 0.7013 -0.1651 -0.5248 0.140 Uiso 1 1 calc R . . C5 C 0.8607(3) -0.0745(4) -0.4671(4) 0.0931(17) Uani 1 1 d . . . H5A H 0.8730 -0.0296 -0.5353 0.140 Uiso 1 1 calc R . . H5B H 0.8892 -0.1412 -0.4570 0.140 Uiso 1 1 calc R . . H5C H 0.8919 -0.0514 -0.4270 0.140 Uiso 1 1 calc R . . C22 C 0.3383(4) 0.3888(4) -0.3613(4) 0.0825(15) Uani 1 1 d . . . C21 C 0.1702(4) 0.3998(5) -0.4290(4) 0.0972(19) Uani 1 1 d . . . C7 C 0.6837(4) 0.0559(3) -0.4661(4) 0.0973(18) Uani 1 1 d . . . H7A H 0.7043 0.0941 -0.5345 0.146 Uiso 1 1 calc R . . H7B H 0.7151 0.0794 -0.4266 0.146 Uiso 1 1 calc R . . H7C H 0.6108 0.0641 -0.4549 0.146 Uiso 1 1 calc R . . C28 C 0.2582(5) 0.6475(4) -0.3452(5) 0.1035(19) Uani 1 1 d . . . H28A H 0.2542 0.7185 -0.3867 0.155 Uiso 1 1 calc R . . H28B H 0.3281 0.6239 -0.3330 0.155 Uiso 1 1 calc R . . H28C H 0.2181 0.6355 -0.2838 0.155 Uiso 1 1 calc R . . C10 C 0.6832(6) -0.5162(4) -0.1127(6) 0.136(3) Uani 1 1 d . . . H10A H 0.7046 -0.5835 -0.1062 0.205 Uiso 1 1 calc R . . H10B H 0.6442 -0.5189 -0.0531 0.205 Uiso 1 1 calc R . . H10C H 0.7421 -0.4794 -0.1242 0.205 Uiso 1 1 calc R . . C24 C -0.0729(4) 0.1614(5) -0.1589(6) 0.128(3) Uani 1 1 d . . . H24A H -0.1100 0.1191 -0.1751 0.193 Uiso 1 1 calc R . . H24B H -0.1046 0.2289 -0.1843 0.193 Uiso 1 1 calc R . . H24C H -0.0733 0.1360 -0.0886 0.193 Uiso 1 1 calc R . . C8 C 0.6821(6) -0.4781(5) -0.3106(5) 0.147(3) Uani 1 1 d . . . H8A H 0.7047 -0.5484 -0.2868 0.220 Uiso 1 1 calc R . . H8B H 0.7403 -0.4387 -0.3317 0.220 Uiso 1 1 calc R . . H8C H 0.6420 -0.4601 -0.3652 0.220 Uiso 1 1 calc R . . C9 C 0.5084(4) -0.5399(4) -0.1822(7) 0.149(4) Uani 1 1 d . . . H9A H 0.5394 -0.6068 -0.1678 0.224 Uiso 1 1 calc R . . H9B H 0.4672 -0.5195 -0.2364 0.224 Uiso 1 1 calc R . . H9C H 0.4662 -0.5394 -0.1253 0.224 Uiso 1 1 calc R . . C25 C 0.0964(5) 0.0273(4) -0.1603(6) 0.130(3) Uani 1 1 d . . . H25A H 0.0507 -0.0087 -0.1759 0.194 Uiso 1 1 calc R . . H25B H 0.0958 0.0025 -0.0900 0.194 Uiso 1 1 calc R . . H25C H 0.1643 0.0173 -0.1878 0.194 Uiso 1 1 calc R . . C26 C 0.2878(7) 0.6242(5) -0.5210(5) 0.152(3) Uani 1 1 d . . . H26A H 0.2841 0.6966 -0.5500 0.228 Uiso 1 1 calc R . . H26B H 0.2638 0.6013 -0.5650 0.228 Uiso 1 1 calc R . . H26C H 0.3572 0.5982 -0.5094 0.228 Uiso 1 1 calc R . . C27 C 0.0881(5) 0.6526(5) -0.4383(6) 0.151(3) Uani 1 1 d . . . H27A H 0.0988 0.7231 -0.4717 0.227 Uiso 1 1 calc R . . H27B H 0.0434 0.6407 -0.3794 0.227 Uiso 1 1 calc R . . H27C H 0.0577 0.6320 -0.4808 0.227 Uiso 1 1 calc R . . C23 C 0.0467(6) 0.1831(6) -0.3376(5) 0.149(3) Uani 1 1 d . . . H23A H 0.0018 0.1375 -0.3394 0.223 Uiso 1 1 calc R . . H23B H 0.1134 0.1719 -0.3669 0.223 Uiso 1 1 calc R . . H23C H 0.0205 0.2514 -0.3738 0.223 Uiso 1 1 calc R . . N1 N 0.5095(2) -0.1224(2) -0.1170(3) 0.0530(8) Uani 1 1 d . . . N3 N 0.0709(2) 0.4278(2) -0.0902(2) 0.0558(8) Uani 1 1 d . . . N4 N -0.1362(3) 0.1672(3) 0.2581(3) 0.0715(10) Uani 1 1 d . . . N2 N 0.6905(3) 0.1861(4) -0.0858(5) 0.0947(17) Uani 1 1 d . . . O1 O 0.8429(2) -0.3225(2) -0.2998(3) 0.0833(10) Uani 1 1 d . . . O2 O 0.8023(2) -0.0550(2) -0.2257(3) 0.0768(9) Uani 1 1 d . . . O3 O 0.3435(2) -0.3555(3) -0.1468(3) 0.0839(10) Uani 1 1 d . . . O7 O 0.1117(3) 0.1279(2) 0.0275(2) 0.0829(10) Uani 1 1 d . . . O12 O -0.2166(3) 0.1354(3) 0.2556(3) 0.0931(11) Uani 1 1 d . . . O11 O -0.0997(3) 0.1438(4) 0.3353(3) 0.1171(15) Uani 1 1 d . . . O8 O 0.3270(3) 0.1430(3) -0.2382(3) 0.0995(12) Uani 1 1 d . . . O4 O 0.5087(3) -0.2772(3) -0.4436(3) 0.1009(12) Uani 1 1 d . . . O5 O 0.7251(3) 0.1696(4) -0.0093(4) 0.1262(19) Uani 1 1 d . . . O6 O 0.6900(3) 0.2695(3) -0.1558(5) 0.139(2) Uani 1 1 d . . . O10 O 0.4226(3) 0.3743(4) -0.3836(4) 0.1341(18) Uani 1 1 d . . . O9 O 0.1464(4) 0.3928(5) -0.4958(3) 0.158(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0386(3) 0.0371(3) 0.0403(3) -0.0116(2) -0.0066(2) -0.0028(2) Fe3 0.0411(3) 0.0489(3) 0.0491(3) -0.0191(3) -0.0021(2) -0.0027(2) Fe2 0.0468(3) 0.0398(3) 0.0447(3) -0.0189(2) -0.0035(2) -0.0072(2) Fe4 0.0614(3) 0.0685(4) 0.0482(4) -0.0246(3) 0.0110(3) -0.0241(3) S2 0.0562(5) 0.0386(4) 0.0403(5) -0.0126(4) -0.0078(4) -0.0051(4) S1 0.0429(5) 0.0413(5) 0.0534(6) -0.0179(4) -0.0119(4) 0.0005(4) P2 0.0508(5) 0.0416(5) 0.0574(6) -0.0243(5) 0.0014(5) -0.0079(4) P1 0.0557(6) 0.0567(6) 0.0457(6) -0.0056(5) -0.0013(5) -0.0074(5) P3 0.0600(6) 0.0653(7) 0.0675(8) -0.0322(6) 0.0014(5) -0.0140(5) S3 0.0499(5) 0.0551(5) 0.0458(6) -0.0094(5) -0.0055(4) -0.0032(4) P4 0.0804(8) 0.0711(8) 0.0549(7) -0.0120(6) 0.0022(6) -0.0275(6) N1 0.0526(18) 0.0542(19) 0.061(2) -0.0314(17) -0.0026(15) -0.0091(15) S4 0.0444(5) 0.0745(7) 0.0585(6) -0.0328(6) 0.0035(4) -0.0150(5) N3 0.0575(19) 0.0571(19) 0.051(2) -0.0224(17) 0.0016(16) -0.0044(16) O1 0.0582(18) 0.076(2) 0.127(3) -0.057(2) -0.0102(18) 0.0110(16) C31 0.048(2) 0.048(2) 0.050(2) -0.0227(18) 0.0010(17) -0.0033(17) O2 0.076(2) 0.081(2) 0.091(3) -0.045(2) -0.0146(17) -0.0244(17) C1 0.049(2) 0.049(2) 0.061(3) -0.0235(19) -0.0065(18) -0.0053(18) C13 0.0400(18) 0.052(2) 0.060(2) -0.035(2) 0.0005(17) -0.0010(16) O3 0.0580(18) 0.097(2) 0.101(3) -0.048(2) 0.0213(18) -0.0251(18) C36 0.0424(19) 0.075(3) 0.049(2) -0.030(2) -0.0055(17) 0.0068(19) C2 0.049(2) 0.047(2) 0.054(2) -0.0179(19) -0.0043(18) -0.0043(17) O7 0.109(3) 0.072(2) 0.049(2) -0.0089(17) -0.0072(18) 0.0016(19) C12 0.0428(19) 0.062(2) 0.080(3) -0.044(2) -0.0077(19) -0.0020(18) O12 0.083(2) 0.098(3) 0.088(3) -0.025(2) 0.015(2) -0.043(2) C17 0.051(2) 0.088(3) 0.081(3) -0.054(3) -0.015(2) -0.003(2) C20 0.055(2) 0.069(3) 0.074(3) -0.030(3) -0.011(2) 0.007(2) C32 0.050(2) 0.074(3) 0.054(3) -0.030(2) -0.0052(18) -0.017(2) N4 0.076(3) 0.064(2) 0.061(3) -0.015(2) 0.008(2) -0.015(2) O11 0.122(3) 0.140(4) 0.055(2) 0.001(2) -0.003(2) -0.045(3) C18 0.054(2) 0.061(2) 0.066(3) -0.033(2) -0.010(2) -0.0037(19) C34 0.049(2) 0.051(2) 0.050(2) -0.0199(19) 0.0070(17) -0.0078(17) O8 0.070(2) 0.101(3) 0.125(3) -0.056(3) -0.002(2) 0.028(2) C14 0.052(2) 0.055(2) 0.067(3) -0.029(2) -0.0119(19) 0.0030(18) C3 0.060(2) 0.054(2) 0.063(3) -0.026(2) -0.005(2) -0.004(2) C15 0.053(2) 0.046(2) 0.105(4) -0.029(2) -0.002(2) -0.0010(19) O4 0.142(3) 0.114(3) 0.065(2) -0.047(2) -0.022(2) -0.025(3) N2 0.050(2) 0.094(4) 0.179(6) -0.097(4) 0.003(3) -0.007(2) C19 0.060(2) 0.054(2) 0.060(3) -0.023(2) -0.006(2) 0.0035(19) C33 0.064(2) 0.073(3) 0.050(3) -0.023(2) -0.007(2) -0.016(2) C29 0.066(3) 0.077(3) 0.062(3) -0.036(2) 0.014(2) -0.031(2) C35 0.0403(19) 0.068(3) 0.064(3) -0.032(2) -0.0031(18) -0.0057(18) C11 0.079(3) 0.056(2) 0.050(2) -0.027(2) 0.011(2) -0.016(2) O5 0.091(3) 0.178(5) 0.185(5) -0.143(5) 0.012(3) -0.050(3) O6 0.104(3) 0.067(3) 0.273(7) -0.088(4) -0.054(4) 0.001(2) C30 0.075(3) 0.053(2) 0.053(3) -0.014(2) 0.008(2) 0.009(2) C16 0.042(2) 0.064(3) 0.110(4) -0.059(3) -0.001(2) -0.0026(19) C4 0.079(3) 0.060(2) 0.057(3) -0.030(2) -0.008(2) -0.014(2) O10 0.085(3) 0.178(5) 0.151(4) -0.092(4) 0.052(3) -0.030(3) O9 0.195(5) 0.245(6) 0.068(3) -0.079(4) 0.033(3) -0.134(5) C6 0.104(4) 0.116(4) 0.047(3) -0.018(3) -0.012(3) -0.017(3) C5 0.065(3) 0.114(4) 0.067(3) -0.008(3) 0.012(2) -0.015(3) C22 0.081(3) 0.101(4) 0.074(3) -0.046(3) 0.023(3) -0.030(3) C21 0.107(4) 0.143(5) 0.056(3) -0.044(3) 0.020(3) -0.074(4) C7 0.116(4) 0.056(3) 0.083(4) 0.003(3) 0.004(3) -0.009(3) C28 0.132(5) 0.068(3) 0.110(5) -0.026(3) -0.022(4) -0.035(3) C10 0.199(8) 0.067(3) 0.163(7) -0.060(4) -0.102(6) 0.052(4) C24 0.064(3) 0.153(6) 0.205(8) -0.109(6) 0.021(4) -0.042(4) C8 0.207(8) 0.088(4) 0.144(6) -0.075(5) 0.090(6) -0.018(5) C9 0.083(4) 0.052(3) 0.301(11) -0.062(5) -0.012(5) -0.013(3) C25 0.140(6) 0.068(4) 0.187(8) -0.056(5) -0.021(5) -0.013(4) C26 0.253(9) 0.108(5) 0.082(5) -0.033(4) 0.078(5) -0.084(6) C27 0.121(5) 0.117(5) 0.133(6) 0.041(5) -0.051(5) -0.015(4) C23 0.217(9) 0.172(7) 0.082(5) -0.053(5) -0.016(5) -0.099(7) #------------------------------------------------------------------------------ _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^)+(0.0629P)^2^+0.7871P] 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 11823 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0818 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1383 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.002 _refine_diff_density_max 0.680 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.082 #------------------------------------------------------------------------------ _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 1.744(4) . ? Fe1 C2 1.769(4) . ? Fe1 P1 2.2124(15) . ? Fe1 S1 2.2633(11) . ? Fe1 S2 2.2679(14) . ? Fe1 Fe2 2.5671(10) . ? Fe3 C20 1.756(4) . ? Fe3 C19 1.772(5) . ? Fe3 P3 2.2138(14) . ? Fe3 S4 2.2705(13) . ? Fe3 S3 2.2706(14) . ? Fe3 Fe4 2.5280(14) . ? Fe2 C4 1.760(5) . ? Fe2 C3 1.773(4) . ? Fe2 P2 2.2427(12) . ? Fe2 S1 2.2606(12) . ? Fe2 S2 2.2644(12) . ? Fe4 C21 1.756(6) . ? Fe4 C22 1.768(5) . ? Fe4 P4 2.2324(16) . ? Fe4 S3 2.2704(13) . ? Fe4 S4 2.2911(14) . ? S2 C11 1.847(4) . ? S1 C12 1.853(4) . ? P2 C8 1.787(5) . ? P2 C10 1.790(6) . ? P2 C9 1.794(5) . ? P1 C7 1.818(5) . ? P1 C6 1.821(5) . ? P1 C5 1.824(5) . ? P3 C24 1.778(5) . ? P3 C23 1.794(6) . ? P3 C25 1.829(6) . ? S3 C30 1.857(4) . ? P4 C26 1.794(6) . ? P4 C27 1.812(6) . ? P4 C28 1.818(6) . ? N1 C13 1.389(5) . ? N1 C12 1.423(5) . ? N1 C11 1.432(5) . ? S4 C29 1.850(4) . ? N3 C31 1.393(5) . ? N3 C30 1.430(5) . ? N3 C29 1.450(5) . ? O1 C1 1.159(4) . ? C31 C32 1.400(5) . ? C31 C36 1.406(5) . ? O2 C2 1.147(5) . ? C13 C18 1.397(5) . ? C13 C14 1.404(5) . ? O3 C3 1.142(5) . ? C36 C35 1.369(6) . ? O7 C19 1.150(5) . ? O12 N4 1.227(5) . ? C17 C16 1.363(6) . ? C17 C18 1.370(6) . ? C20 O8 1.152(5) . ? C32 C33 1.371(6) . ? N4 O11 1.211(5) . ? N4 C34 1.450(5) . ? C34 C35 1.368(6) . ? C34 C33 1.376(6) . ? C14 C15 1.360(6) . ? C15 C16 1.381(7) . ? O4 C4 1.152(5) . ? N2 O5 1.212(7) . ? N2 O6 1.230(7) . ? N2 C16 1.449(6) . ? O10 C22 1.144(6) . ? O9 C21 1.138(6) . ? #------------------------------------------------------------------------------ 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 102.68(17) . . ? C1 Fe1 P1 88.40(14) . . ? C2 Fe1 P1 87.63(14) . . ? C1 Fe1 S1 140.68(13) . . ? C2 Fe1 S1 116.34(12) . . ? P1 Fe1 S1 88.53(5) . . ? C1 Fe1 S2 91.56(14) . . ? C2 Fe1 S2 101.89(13) . . ? P1 Fe1 S2 170.24(5) . . ? S1 Fe1 S2 85.32(5) . . ? C1 Fe1 Fe2 91.07(13) . . ? C2 Fe1 Fe2 154.20(13) . . ? P1 Fe1 Fe2 114.81(5) . . ? S1 Fe1 Fe2 55.38(3) . . ? S2 Fe1 Fe2 55.44(4) . . ? C20 Fe3 C19 103.9(2) . . ? C20 Fe3 P3 88.05(16) . . ? C19 Fe3 P3 87.94(15) . . ? C20 Fe3 S4 91.90(16) . . ? C19 Fe3 S4 98.98(15) . . ? P3 Fe3 S4 172.88(5) . . ? C20 Fe3 S3 138.50(16) . . ? C19 Fe3 S3 117.51(13) . . ? P3 Fe3 S3 90.28(5) . . ? S4 Fe3 S3 85.04(5) . . ? C20 Fe3 Fe4 87.89(16) . . ? C19 Fe3 Fe4 153.82(14) . . ? P3 Fe3 Fe4 116.16(5) . . ? S4 Fe3 Fe4 56.73(4) . . ? S3 Fe3 Fe4 56.17(4) . . ? C4 Fe2 C3 99.4(2) . . ? C4 Fe2 P2 88.28(15) . . ? C3 Fe2 P2 93.10(13) . . ? C4 Fe2 S1 90.24(14) . . ? C3 Fe2 S1 100.35(13) . . ? P2 Fe2 S1 166.53(4) . . ? C4 Fe2 S2 159.52(15) . . ? C3 Fe2 S2 101.04(14) . . ? P2 Fe2 S2 91.28(5) . . ? S1 Fe2 S2 85.46(5) . . ? C4 Fe2 Fe1 105.94(15) . . ? C3 Fe2 Fe1 144.22(13) . . ? P2 Fe2 Fe1 112.22(4) . . ? S1 Fe2 Fe1 55.48(3) . . ? S2 Fe2 Fe1 55.56(4) . . ? C21 Fe4 C22 91.7(3) . . ? C21 Fe4 P4 93.8(2) . . ? C22 Fe4 P4 94.92(19) . . ? C21 Fe4 S3 90.24(18) . . ? C22 Fe4 S3 162.73(19) . . ? P4 Fe4 S3 102.06(6) . . ? C21 Fe4 S4 157.9(2) . . ? C22 Fe4 S4 87.16(18) . . ? P4 Fe4 S4 108.36(6) . . ? S3 Fe4 S4 84.57(5) . . ? C21 Fe4 Fe3 103.59(19) . . ? C22 Fe4 Fe3 106.76(19) . . ? P4 Fe4 Fe3 151.51(5) . . ? S3 Fe4 Fe3 56.17(4) . . ? S4 Fe4 Fe3 55.96(4) . . ? C11 S2 Fe2 109.15(15) . . ? C11 S2 Fe1 111.03(13) . . ? Fe2 S2 Fe1 69.00(4) . . ? C12 S1 Fe2 106.55(14) . . ? C12 S1 Fe1 111.39(13) . . ? Fe2 S1 Fe1 69.15(4) . . ? C8 P2 C10 102.4(4) . . ? C8 P2 C9 101.6(4) . . ? C10 P2 C9 101.7(4) . . ? C8 P2 Fe2 117.2(2) . . ? C10 P2 Fe2 118.58(19) . . ? C9 P2 Fe2 112.90(18) . . ? C7 P1 C6 102.1(3) . . ? C7 P1 C5 102.4(3) . . ? C6 P1 C5 102.5(3) . . ? C7 P1 Fe1 114.85(19) . . ? C6 P1 Fe1 119.40(19) . . ? C5 P1 Fe1 113.45(17) . . ? C24 P3 C23 105.7(4) . . ? C24 P3 C25 101.7(3) . . ? C23 P3 C25 99.9(4) . . ? C24 P3 Fe3 114.6(2) . . ? C23 P3 Fe3 118.7(2) . . ? C25 P3 Fe3 113.9(2) . . ? C30 S3 Fe4 107.59(16) . . ? C30 S3 Fe3 110.46(14) . . ? Fe4 S3 Fe3 67.66(5) . . ? C26 P4 C27 103.4(4) . . ? C26 P4 C28 100.4(3) . . ? C27 P4 C28 100.1(4) . . ? C26 P4 Fe4 114.6(2) . . ? C27 P4 Fe4 117.5(2) . . ? C28 P4 Fe4 118.05(19) . . ? C13 N1 C12 122.2(3) . . ? C13 N1 C11 121.9(3) . . ? C12 N1 C11 113.6(3) . . ? C29 S4 Fe3 110.28(13) . . ? C29 S4 Fe4 115.66(16) . . ? Fe3 S4 Fe4 67.31(5) . . ? C31 N3 C30 120.3(3) . . ? C31 N3 C29 122.6(4) . . ? C30 N3 C29 114.6(3) . . ? N3 C31 C32 120.7(4) . . ? N3 C31 C36 121.2(4) . . ? C32 C31 C36 118.1(4) . . ? O1 C1 Fe1 177.1(3) . . ? N1 C13 C18 121.1(4) . . ? N1 C13 C14 120.6(4) . . ? C18 C13 C14 118.2(4) . . ? C35 C36 C31 120.6(4) . . ? O2 C2 Fe1 176.0(4) . . ? N1 C12 S1 115.1(2) . . ? C16 C17 C18 120.2(4) . . ? O8 C20 Fe3 177.1(4) . . ? C33 C32 C31 120.8(4) . . ? O11 N4 O12 121.3(4) . . ? O11 N4 C34 119.0(4) . . ? O12 N4 C34 119.7(4) . . ? C17 C18 C13 120.2(4) . . ? C35 C34 C33 121.4(4) . . ? C35 C34 N4 120.2(4) . . ? C33 C34 N4 118.4(4) . . ? C15 C14 C13 120.8(4) . . ? O3 C3 Fe2 179.4(4) . . ? C14 C15 C16 119.5(4) . . ? O5 N2 O6 122.5(5) . . ? O5 N2 C16 119.3(6) . . ? O6 N2 C16 118.2(6) . . ? O7 C19 Fe3 176.1(4) . . ? C32 C33 C34 119.4(4) . . ? N3 C29 S4 114.5(3) . . ? C34 C35 C36 119.8(4) . . ? N1 C11 S2 115.3(3) . . ? N3 C30 S3 115.4(3) . . ? C17 C16 C15 120.9(4) . . ? C17 C16 N2 119.4(5) . . ? C15 C16 N2 119.7(5) . . ? O4 C4 Fe2 179.0(5) . . ? O10 C22 Fe4 179.2(6) . . ? O9 C21 Fe4 178.7(6) . . ? #===END # Copyright The Royal Society of Chemistry, 2005 # CCDC Number: 279852 data_FeHFe _database_code_depnum_ccdc_archive 'CCDC 279852' #------------------------------------------------------------------------------ _audit_creation_date 'Jul 10 10:01:24 2005' _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 750.15 _chemical_formula_analytical ? _chemical_formula_sum 'C18 H27 F6 Fe2 N2 O6 P3 S2' _chemical_formula_moiety 'C18 H27 F6 Fe2 N2 O6 P3 S2' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 11.3070(6) _cell_length_b 14.1755(5) _cell_length_c 18.9123(9) _cell_angle_alpha 90.00 _cell_angle_beta 104.846(3) _cell_angle_gamma 90.00 _cell_volume 2930.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _exptl_crystal_description block _exptl_crystal_colour 'deep red' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.700 _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 1.371 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2813 _exptl_absorpt_correction_T_max 0.3448 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 20789 _reflns_number_observed 4388 _reflns_number_total 7212 _reflns_observed_criterion >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_av_sigmaI/netI 0.0701 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 28.28 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.994 #------------------------------------------------------------------------------ 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 0.37803(6) 0.82550(4) 0.26595(3) 0.02930(17) Uani 1 1 d . . . H1 H 0.271(4) 0.879(3) 0.304(2) 0.046(13) Uiso 1 1 d . . . Fe2 Fe 0.16177(6) 0.89763(4) 0.21933(3) 0.03059(17) Uani 1 1 d . . . S1 S 0.22047(10) 0.75870(7) 0.18022(6) 0.0372(3) Uani 1 1 d . . . S2 S 0.33476(10) 0.95536(7) 0.19452(5) 0.0319(2) Uani 1 1 d . . . P1 P 0.50126(11) 0.91554(8) 0.35144(6) 0.0336(3) Uani 1 1 d . . . P2 P 0.02211(11) 0.81763(8) 0.26203(7) 0.0390(3) Uani 1 1 d . . . P3 P -0.25962(13) 1.08158(10) 0.13750(8) 0.0517(4) Uani 1 1 d . . . F1 F -0.4020(6) 1.0664(4) 0.1130(3) 0.153(2) Uani 1 1 d U . . F2 F -0.2831(6) 1.1894(3) 0.1228(4) 0.144(2) Uani 1 1 d . . . F3 F -0.2409(6) 0.9760(3) 0.1594(3) 0.158(3) Uani 1 1 d . . . F4 F -0.2686(6) 1.1090(4) 0.2167(3) 0.139(2) Uani 1 1 d . . . F5 F -0.1195(4) 1.0981(4) 0.1649(3) 0.141(2) Uani 1 1 d . . . F6 F -0.2540(7) 1.0559(6) 0.0624(2) 0.205(4) Uani 1 1 d . . . O1 O 0.3879(4) 0.6683(2) 0.3677(2) 0.0604(10) Uani 1 1 d . . . O2 O 0.5934(4) 0.7629(3) 0.2214(2) 0.0653(11) Uani 1 1 d . . . O3 O -0.0049(4) 0.9445(3) 0.0788(2) 0.0818(14) Uani 1 1 d . . . O4 O 0.1156(4) 1.0644(2) 0.2979(2) 0.0585(10) Uani 1 1 d . . . O5 O 0.7253(6) 0.5576(4) -0.0060(3) 0.111(2) Uani 1 1 d . . . O6 O 0.8176(6) 0.6894(5) -0.0055(4) 0.129(2) Uani 1 1 d . . . N1 N 0.3492(4) 0.8282(3) 0.0851(2) 0.0448(10) Uani 1 1 d . . . N2 N 0.7328(6) 0.6435(5) 0.0027(3) 0.0790(17) Uani 1 1 d . . . C1 C 0.3851(4) 0.7294(3) 0.3278(3) 0.0410(11) Uani 1 1 d . . . C2 C 0.5089(5) 0.7852(3) 0.2372(2) 0.0403(11) Uani 1 1 d . . . C3 C 0.0568(5) 0.9286(4) 0.1342(3) 0.0482(12) Uani 1 1 d . . . C4 C 0.1347(4) 1.0012(3) 0.2665(3) 0.0373(10) Uani 1 1 d . . . C5 C 0.5829(5) 0.8547(4) 0.4331(3) 0.0538(13) Uani 1 1 d . . . H9A H 0.5258 0.8216 0.4539 0.080 Uiso 1 1 calc . . . H9B H 0.6274 0.8996 0.4679 0.080 Uiso 1 1 calc . . . H9C H 0.6390 0.8105 0.4211 0.080 Uiso 1 1 calc . . . C6 C 0.4282(5) 1.0127(3) 0.3861(3) 0.0491(12) Uani 1 1 d . . . H10A H 0.3816 1.0494 0.3459 0.080 Uiso 1 1 calc . . . H10B H 0.4896 1.0519 0.4169 0.080 Uiso 1 1 calc . . . H10C H 0.3749 0.9884 0.4139 0.080 Uiso 1 1 calc . . . C7 C 0.6222(5) 0.9740(5) 0.3207(3) 0.0652(16) Uani 1 1 d . . . H8A H 0.5873 1.0083 0.2765 0.080 Uiso 1 1 calc . . . H8B H 0.6785 0.9277 0.3115 0.080 Uiso 1 1 calc . . . H8C H 0.6649 1.0169 0.3578 0.080 Uiso 1 1 calc . . . C8 C 0.0826(5) 0.7175(3) 0.3195(3) 0.0540(13) Uani 1 1 d . . . H2A H 0.1258 0.6768 0.2941 0.080 Uiso 1 1 calc . . . H2B H 0.0164 0.6833 0.3308 0.080 Uiso 1 1 calc . . . H2C H 0.1375 0.7393 0.3640 0.080 Uiso 1 1 calc . . . C9 C -0.0553(6) 0.8825(4) 0.3188(4) 0.0630(16) Uani 1 1 d . . . H1B H -0.0909 0.9386 0.2937 0.080 Uiso 1 1 calc . . . H1C H 0.0022 0.8995 0.3638 0.080 Uiso 1 1 calc . . . H1D H -0.1186 0.8439 0.3292 0.080 Uiso 1 1 calc . . . C10 C -0.1009(5) 0.7673(4) 0.1913(3) 0.0650(16) Uani 1 1 d . . . H3A H -0.0672 0.7313 0.1582 0.080 Uiso 1 1 calc . . . H3B H -0.1511 0.8171 0.1651 0.080 Uiso 1 1 calc . . . H3C H -0.1496 0.7269 0.2133 0.080 Uiso 1 1 calc . . . C11 C 0.2392(5) 0.7783(4) 0.0873(3) 0.0524(13) Uani 1 1 d . . . H11A H 0.2391 0.7177 0.0636 0.080 Uiso 1 1 calc . . . H11B H 0.1692 0.8137 0.0594 0.080 Uiso 1 1 calc . . . C12 C 0.3469(5) 0.9270(3) 0.1011(3) 0.0494(13) Uani 1 1 d . . . H12A H 0.2782 0.9555 0.0661 0.080 Uiso 1 1 calc . . . H12B H 0.4210 0.9557 0.0940 0.080 Uiso 1 1 calc . . . C13 C 0.4438(5) 0.7837(3) 0.0645(2) 0.0413(11) Uani 1 1 d . . . C14 C 0.5411(5) 0.8349(3) 0.0491(3) 0.0522(13) Uani 1 1 d . . . H18 H 0.5417 0.9004 0.0521 0.080 Uiso 1 1 calc . . . C15 C 0.6346(6) 0.7893(5) 0.0297(3) 0.0614(15) Uani 1 1 d . . . H17 H 0.6985 0.8240 0.0199 0.080 Uiso 1 1 calc . . . C16 C 0.6349(5) 0.6927(4) 0.0245(3) 0.0555(14) Uani 1 1 d . . . C17 C 0.5412(6) 0.6400(4) 0.0396(3) 0.0634(16) Uani 1 1 d . . . H15 H 0.5424 0.5746 0.0365 0.080 Uiso 1 1 calc . . . C18 C 0.4464(6) 0.6846(4) 0.0594(3) 0.0576(14) Uani 1 1 d . . . H14 H 0.3835 0.6490 0.0694 0.080 Uiso 1 1 calc . . . 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 0.0281(3) 0.0259(3) 0.0336(3) -0.0005(2) 0.0073(3) 0.0020(2) Fe2 0.0292(3) 0.0258(3) 0.0364(3) -0.0016(2) 0.0079(3) 0.0033(2) S1 0.0336(6) 0.0277(5) 0.0488(7) -0.0101(4) 0.0080(5) -0.0010(4) S2 0.0363(6) 0.0277(5) 0.0325(5) -0.0008(4) 0.0102(5) 0.0007(4) P1 0.0303(6) 0.0380(6) 0.0312(6) 0.0002(4) 0.0057(5) -0.0013(4) P2 0.0294(6) 0.0342(6) 0.0541(7) 0.0015(5) 0.0121(5) 0.0010(5) P3 0.0418(8) 0.0532(8) 0.0587(8) 0.0035(6) 0.0102(7) 0.0065(6) F1 0.149(2) 0.151(2) 0.156(2) -0.0046(10) 0.0373(11) -0.0002(10) F2 0.159(6) 0.074(3) 0.195(6) 0.042(3) 0.036(4) 0.009(3) F3 0.215(7) 0.057(3) 0.161(5) 0.016(3) -0.025(5) 0.019(3) F4 0.176(6) 0.160(5) 0.114(4) -0.036(3) 0.093(4) -0.037(4) F5 0.050(3) 0.211(6) 0.160(5) -0.064(4) 0.025(3) -0.006(3) F6 0.244(8) 0.324(9) 0.046(3) -0.008(4) 0.038(4) 0.099(7) O1 0.064(3) 0.045(2) 0.074(3) 0.0265(18) 0.022(2) 0.0098(17) O2 0.051(3) 0.098(3) 0.053(2) 0.006(2) 0.0222(19) 0.034(2) O3 0.075(3) 0.118(4) 0.044(2) 0.009(2) -0.002(2) 0.036(3) O4 0.071(3) 0.039(2) 0.075(3) -0.0160(18) 0.034(2) -0.0026(17) O5 0.134(5) 0.098(4) 0.120(4) 0.006(3) 0.064(4) 0.066(4) O6 0.086(5) 0.156(6) 0.171(6) 0.019(4) 0.082(5) 0.030(4) N1 0.048(3) 0.046(2) 0.044(2) -0.0116(17) 0.019(2) 0.0005(18) N2 0.077(4) 0.103(5) 0.064(3) 0.009(3) 0.030(3) 0.037(4) C1 0.035(3) 0.035(2) 0.051(3) -0.003(2) 0.007(2) 0.0017(19) C2 0.039(3) 0.046(3) 0.033(2) 0.0032(19) 0.003(2) 0.006(2) C3 0.039(3) 0.052(3) 0.052(3) -0.002(2) 0.010(2) 0.011(2) C4 0.037(3) 0.026(2) 0.051(3) 0.0011(19) 0.016(2) -0.0002(17) C5 0.058(4) 0.058(3) 0.038(3) 0.000(2) -0.001(2) 0.008(3) C6 0.050(3) 0.043(3) 0.052(3) -0.016(2) 0.009(2) -0.002(2) C7 0.049(4) 0.082(4) 0.065(4) -0.012(3) 0.016(3) -0.026(3) C8 0.043(3) 0.041(3) 0.080(4) 0.016(3) 0.019(3) 0.002(2) C9 0.061(4) 0.054(3) 0.090(4) 0.008(3) 0.047(3) 0.006(3) C10 0.041(3) 0.071(4) 0.080(4) -0.003(3) 0.010(3) -0.012(3) C11 0.046(3) 0.067(3) 0.042(3) -0.026(2) 0.008(2) 0.000(2) C12 0.070(4) 0.045(3) 0.037(2) 0.005(2) 0.021(2) 0.013(2) C13 0.046(3) 0.046(3) 0.033(2) -0.0034(19) 0.011(2) 0.003(2) C14 0.059(4) 0.049(3) 0.051(3) -0.001(2) 0.017(3) 0.008(2) C15 0.051(4) 0.083(4) 0.055(3) 0.006(3) 0.023(3) -0.002(3) C16 0.057(4) 0.071(4) 0.043(3) 0.002(2) 0.022(3) 0.022(3) C17 0.078(5) 0.052(3) 0.062(4) -0.005(3) 0.023(3) 0.017(3) C18 0.063(4) 0.056(3) 0.060(3) -0.007(3) 0.029(3) 0.005(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^)+(0.0917P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7212 _refine_ls_number_parameters 356 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0968 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1654 _refine_ls_wR_factor_gt 0.1382 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.536 _refine_diff_density_min -0.944 _refine_diff_density_rms 0.102 #------------------------------------------------------------------------------ _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 1.784(5) . ? Fe1 C2 1.795(5) . ? Fe1 P1 2.2428(12) . ? Fe1 S2 2.2614(11) . ? Fe1 S1 2.2845(12) . ? Fe1 Fe2 2.5879(8) . ? Fe1 H1 1.72(5) . ? Fe2 C4 1.785(4) . ? Fe2 C3 1.793(5) . ? Fe2 P2 2.2551(13) . ? Fe2 S1 2.2622(12) . ? Fe2 S2 2.2772(13) . ? Fe2 H1 1.77(5) . ? S1 C11 1.844(5) . ? S2 C12 1.852(5) . ? P1 C5 1.803(5) . ? P1 C6 1.813(5) . ? P1 C7 1.817(6) . ? P2 C9 1.802(6) . ? P2 C10 1.810(6) . ? P2 C8 1.812(5) . ? P3 F6 1.483(5) . ? P3 F3 1.553(4) . ? P3 F5 1.554(5) . ? P3 F2 1.564(4) . ? P3 F1 1.571(7) . ? P3 F4 1.575(5) . ? O1 C1 1.143(5) . ? O2 C2 1.118(6) . ? O3 C3 1.124(6) . ? O4 C4 1.126(5) . ? O5 N2 1.229(8) . ? O6 N2 1.201(8) . ? N1 C13 1.382(6) . ? N1 C12 1.434(6) . ? N1 C11 1.441(7) . ? N2 C16 1.453(7) . ? C5 H9A 0.9600 . ? C5 H9B 0.9600 . ? C5 H9C 0.9600 . ? C6 H10A 0.9600 . ? C6 H10B 0.9600 . ? C6 H10C 0.9600 . ? C7 H8A 0.9600 . ? C7 H8B 0.9600 . ? C7 H8C 0.9600 . ? C8 H2A 0.9600 . ? C8 H2B 0.9600 . ? C8 H2C 0.9600 . ? C9 H1B 0.9600 . ? C9 H1C 0.9600 . ? C9 H1D 0.9600 . ? C10 H3A 0.9600 . ? C10 H3B 0.9600 . ? C10 H3C 0.9600 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C18 1.410(7) . ? C13 C14 1.409(7) . ? C14 C15 1.367(8) . ? C14 H18 0.9300 . ? C15 C16 1.374(8) . ? C15 H17 0.9300 . ? C16 C17 1.385(9) . ? C17 C18 1.376(8) . ? C17 H15 0.9300 . ? C18 H14 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 C1 Fe1 C2 93.1(2) . . ? C1 Fe1 P1 92.65(15) . . ? C2 Fe1 P1 89.50(15) . . ? C1 Fe1 S2 168.45(16) . . ? C2 Fe1 S2 98.46(15) . . ? P1 Fe1 S2 88.09(4) . . ? C1 Fe1 S1 92.58(15) . . ? C2 Fe1 S1 101.93(15) . . ? P1 Fe1 S1 167.15(5) . . ? S2 Fe1 S1 84.46(4) . . ? C1 Fe1 Fe2 113.89(16) . . ? C2 Fe1 Fe2 143.39(14) . . ? P1 Fe1 Fe2 112.27(4) . . ? S2 Fe1 Fe2 55.52(3) . . ? S1 Fe1 Fe2 54.90(3) . . ? C1 Fe1 H1 89.1(15) . . ? C2 Fe1 H1 169.2(15) . . ? P1 Fe1 H1 79.8(15) . . ? S2 Fe1 H1 79.7(15) . . ? S1 Fe1 H1 88.5(15) . . ? Fe2 Fe1 H1 42.9(15) . . ? C4 Fe2 C3 95.1(2) . . ? C4 Fe2 P2 90.54(15) . . ? C3 Fe2 P2 94.67(18) . . ? C4 Fe2 S1 169.06(15) . . ? C3 Fe2 S1 95.84(16) . . ? P2 Fe2 S1 88.30(5) . . ? C4 Fe2 S2 94.22(15) . . ? C3 Fe2 S2 97.64(18) . . ? P2 Fe2 S2 166.34(5) . . ? S1 Fe2 S2 84.61(4) . . ? C4 Fe2 Fe1 115.00(15) . . ? C3 Fe2 Fe1 138.86(16) . . ? P2 Fe2 Fe1 111.50(4) . . ? S1 Fe2 Fe1 55.71(3) . . ? S2 Fe2 Fe1 54.95(3) . . ? C4 Fe2 H1 81.0(15) . . ? C3 Fe2 H1 174.1(15) . . ? P2 Fe2 H1 89.8(15) . . ? S1 Fe2 H1 88.1(15) . . ? S2 Fe2 H1 78.4(16) . . ? Fe1 Fe2 H1 41.5(16) . . ? C11 S1 Fe2 107.16(17) . . ? C11 S1 Fe1 110.77(17) . . ? Fe2 S1 Fe1 69.38(4) . . ? C12 S2 Fe1 109.63(15) . . ? C12 S2 Fe2 113.37(19) . . ? Fe1 S2 Fe2 69.53(4) . . ? C5 P1 C6 103.5(2) . . ? C5 P1 C7 103.3(3) . . ? C6 P1 C7 102.7(3) . . ? C5 P1 Fe1 115.63(18) . . ? C6 P1 Fe1 115.91(17) . . ? C7 P1 Fe1 114.09(19) . . ? C9 P2 C10 104.0(3) . . ? C9 P2 C8 102.0(3) . . ? C10 P2 C8 103.6(3) . . ? C9 P2 Fe2 116.66(19) . . ? C10 P2 Fe2 114.2(2) . . ? C8 P2 Fe2 114.69(18) . . ? F6 P3 F3 89.0(4) . . ? F6 P3 F5 93.8(4) . . ? F3 P3 F5 89.9(3) . . ? F6 P3 F2 96.7(4) . . ? F3 P3 F2 174.1(4) . . ? F5 P3 F2 91.4(3) . . ? F6 P3 F1 88.6(4) . . ? F3 P3 F1 90.3(3) . . ? F5 P3 F1 177.6(3) . . ? F2 P3 F1 88.1(3) . . ? F6 P3 F4 178.8(4) . . ? F3 P3 F4 91.2(3) . . ? F5 P3 F4 87.4(3) . . ? F2 P3 F4 83.0(3) . . ? F1 P3 F4 90.2(3) . . ? C13 N1 C12 124.2(4) . . ? C13 N1 C11 121.4(4) . . ? C12 N1 C11 114.3(4) . . ? O6 N2 O5 123.3(6) . . ? O6 N2 C16 117.9(7) . . ? O5 N2 C16 118.8(7) . . ? O1 C1 Fe1 178.9(4) . . ? O2 C2 Fe1 177.0(5) . . ? O3 C3 Fe2 175.7(5) . . ? O4 C4 Fe2 177.3(4) . . ? P1 C5 H9A 109.5 . . ? P1 C5 H9B 109.5 . . ? H9A C5 H9B 109.5 . . ? P1 C5 H9C 109.5 . . ? H9A C5 H9C 109.5 . . ? H9B C5 H9C 109.5 . . ? P1 C6 H10A 109.5 . . ? P1 C6 H10B 109.5 . . ? H10A C6 H10B 109.5 . . ? P1 C6 H10C 109.5 . . ? H10A C6 H10C 109.5 . . ? H10B C6 H10C 109.5 . . ? P1 C7 H8A 109.5 . . ? P1 C7 H8B 109.5 . . ? H8A C7 H8B 109.5 . . ? P1 C7 H8C 109.5 . . ? H8A C7 H8C 109.5 . . ? H8B C7 H8C 109.5 . . ? P2 C8 H2A 109.5 . . ? P2 C8 H2B 109.5 . . ? H2A C8 H2B 109.5 . . ? P2 C8 H2C 109.5 . . ? H2A C8 H2C 109.5 . . ? H2B C8 H2C 109.5 . . ? P2 C9 H1B 109.5 . . ? P2 C9 H1C 109.5 . . ? H1B C9 H1C 109.5 . . ? P2 C9 H1D 109.5 . . ? H1B C9 H1D 109.5 . . ? H1C C9 H1D 109.5 . . ? P2 C10 H3A 109.5 . . ? P2 C10 H3B 109.5 . . ? H3A C10 H3B 109.5 . . ? P2 C10 H3C 109.5 . . ? H3A C10 H3C 109.5 . . ? H3B C10 H3C 109.5 . . ? N1 C11 S1 114.4(3) . . ? N1 C11 H11A 108.7 . . ? S1 C11 H11A 108.7 . . ? N1 C11 H11B 108.7 . . ? S1 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? N1 C12 S2 115.0(3) . . ? N1 C12 H12A 108.5 . . ? S2 C12 H12A 108.5 . . ? N1 C12 H12B 108.5 . . ? S2 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? N1 C13 C18 120.4(5) . . ? N1 C13 C14 121.7(4) . . ? C18 C13 C14 117.9(5) . . ? C15 C14 C13 120.7(5) . . ? C15 C14 H18 119.7 . . ? C13 C14 H18 119.7 . . ? C14 C15 C16 120.5(5) . . ? C14 C15 H17 119.8 . . ? C16 C15 H17 119.8 . . ? C15 C16 C17 120.4(5) . . ? C15 C16 N2 121.0(6) . . ? C17 C16 N2 118.6(6) . . ? C18 C17 C16 120.0(5) . . ? C18 C17 H15 120.0 . . ? C16 C17 H15 120.0 . . ? C17 C18 C13 120.5(5) . . ? C17 C18 H14 119.8 . . ? C13 C18 H14 119.8 . . ? #===END