Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_c:\word_f~1\papers\inorga~1\adbmkw\12_bat~1\bath147 _database_code_depnum_ccdc_archive 'CCDC 616340' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H42 Cl2 Fe N2 O12 P4' _chemical_formula_weight 801.23 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P42bc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z+1/2' '-x, -y, z' 'y, -x, z+1/2' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 21.5338(7) _cell_length_b 21.5338(7) _cell_length_c 15.5334(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7202.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2473 _cell_measurement_theta_min 2.187 _cell_measurement_theta_max 23.047 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3328 _exptl_absorpt_coefficient_mu 0.802 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.9823 _exptl_absorpt_correction_T_max 0.9715 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6751 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker APEXII CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 10 _diffrn_reflns_number 20213 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 23.65 _reflns_number_total 4868 _reflns_number_gt 3485 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0975P)^2^+1.4655P] 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 0.07(5) _refine_ls_number_reflns 4868 _refine_ls_number_parameters 405 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0822 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1646 _refine_ls_wR_factor_gt 0.1454 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.5000 1.0000 0.69263(9) 0.0449(3) Uani 1 2 d S . . Fe2 Fe 0.0000 1.0000 0.99321(9) 0.0449(4) Uani 1 2 d S . . Cl1 Cl 0.55267(9) 0.94028(9) 0.79803(12) 0.0599(5) Uani 1 1 d . . . Cl2 Cl -0.04441(9) 1.06410(9) 1.09912(14) 0.0628(5) Uani 1 1 d . . . P1 P 0.54279(9) 0.95123(9) 0.58627(12) 0.0512(5) Uani 1 1 d . . . P2 P 0.42300(9) 0.93093(9) 0.70018(14) 0.0500(4) Uani 1 1 d . A . P3 P 0.08480(9) 1.05828(9) 1.00037(16) 0.0601(5) Uani 1 1 d . . . P5 P 0.03688(10) 0.94652(10) 0.88714(14) 0.0614(6) Uani 1 1 d D . . O1 O 0.6073(3) 0.8648(3) 0.5164(5) 0.0894(19) Uani 1 1 d . . . O2 O 0.6557(9) 0.7873(6) 0.5642(9) 0.217(7) Uani 1 1 d . . . O3 O 0.3922(6) 0.8099(6) 0.7283(9) 0.057(3) Uiso 0.50 1 d P A 1 O4 O 0.4530(7) 0.7368(6) 0.7886(10) 0.089(4) Uiso 0.50 1 d P A 1 O5 O 0.3195(2) 0.9979(2) 0.7021(4) 0.0672(14) Uani 1 1 d . A . O6 O 0.2501(3) 1.0090(4) 0.8066(7) 0.125(3) Uani 1 1 d . A . O7 O 0.1301(4) 1.1693(3) 1.0405(7) 0.129(3) Uani 1 1 d . . . O8 O 0.1059(8) 1.2305(8) 1.1438(16) 0.332(16) Uani 1 1 d . . . O9 O 0.1773(2) 0.9790(3) 0.9973(4) 0.0729(14) Uani 1 1 d . . . O10 O 0.2651(4) 0.9756(5) 1.0751(6) 0.140(3) Uani 1 1 d . . . O11 O 0.0932(6) 0.8458(6) 0.8265(8) 0.063(3) Uiso 0.50 1 d PD B 1 O12 O 0.1553(11) 0.7807(11) 0.9017(17) 0.167(8) Uiso 0.50 1 d PD B 1 O3A O 0.3856(6) 0.8213(6) 0.7558(9) 0.063(4) Uiso 0.50 1 d P A 2 O4A O 0.4327(6) 0.7472(7) 0.8294(9) 0.080(3) Uiso 0.50 1 d P A 2 O11A O 0.0760(8) 0.8301(8) 0.8548(11) 0.100(5) Uiso 0.50 1 d PD C 2 O12A O 0.0973(10) 0.7530(10) 0.9249(16) 0.157(7) Uiso 0.50 1 d PD C 2 N1 N 0.4200(3) 0.9336(3) 0.5206(4) 0.0584(16) Uani 1 1 d . . . N2 N 0.0854(4) 1.0575(4) 0.8217(5) 0.080(2) Uani 1 1 d . . . C1 C 0.4059(4) 0.9992(4) 0.5185(5) 0.061(2) Uani 1 1 d . . . H1A H 0.3625 1.0052 0.5375 0.074 Uiso 1 1 calc R . . H1B H 0.4088 1.0138 0.4582 0.074 Uiso 1 1 calc R . . C2 C 0.4849(4) 0.9205(4) 0.5061(5) 0.064(2) Uani 1 1 d . . . H2A H 0.4961 0.9372 0.4488 0.076 Uiso 1 1 calc R . . H2B H 0.4899 0.8749 0.5033 0.076 Uiso 1 1 calc R . . C3 C 0.3945(3) 0.9026(3) 0.5949(5) 0.0583(18) Uani 1 1 d . . . H3A H 0.4039 0.8577 0.5903 0.070 Uiso 1 1 calc R . . H3B H 0.3487 0.9072 0.5935 0.070 Uiso 1 1 calc R . . C4 C 0.5921(4) 0.8841(4) 0.6032(6) 0.070(2) Uani 1 1 d . . . H4A H 0.6299 0.8954 0.6359 0.084 Uiso 1 1 calc R . . H4B H 0.5696 0.8510 0.6345 0.084 Uiso 1 1 calc R . . C5 C 0.6345(7) 0.8149(6) 0.5025(10) 0.113(4) Uani 1 1 d . . . C6 C 0.6457(6) 0.7947(6) 0.4111(8) 0.114(4) Uani 1 1 d . . . H6A H 0.6816 0.8169 0.3878 0.171 Uiso 1 1 calc R . . H6B H 0.6089 0.8040 0.3762 0.171 Uiso 1 1 calc R . . H6C H 0.6537 0.7499 0.4097 0.171 Uiso 1 1 calc R . . C7 C 0.4385(4) 0.8590(4) 0.7600(6) 0.068(2) Uani 1 1 d . . . H7A H 0.4816 0.8449 0.7496 0.082 Uiso 1 1 calc R A 1 H7B H 0.4331 0.8660 0.8226 0.082 Uiso 1 1 calc R A 1 C8 C 0.4076(9) 0.7511(9) 0.7525(11) 0.065(5) Uiso 0.50 1 d P A 1 C9 C 0.3597(8) 0.7081(8) 0.7226(13) 0.070(4) Uiso 0.50 1 d P A 1 H9A H 0.3722 0.6902 0.6672 0.104 Uiso 0.50 1 calc PR A 1 H9B H 0.3203 0.7304 0.7157 0.104 Uiso 0.50 1 calc PR A 1 H9C H 0.3544 0.6747 0.7649 0.104 Uiso 0.50 1 calc PR A 1 C10 C 0.3487(4) 0.9519(4) 0.7538(5) 0.067(2) Uani 1 1 d . . . H10A H 0.3217 0.9149 0.7590 0.080 Uiso 1 1 calc R A . H10B H 0.3568 0.9684 0.8122 0.080 Uiso 1 1 calc R . . C11 C 0.2663(5) 1.0221(5) 0.7349(8) 0.088(3) Uani 1 1 d . . . C12 C 0.2371(5) 1.0653(6) 0.6740(10) 0.119(5) Uani 1 1 d . A . H12A H 0.1919 1.0607 0.6767 0.178 Uiso 1 1 calc R . . H12B H 0.2516 1.0561 0.6155 0.178 Uiso 1 1 calc R . . H12C H 0.2485 1.1080 0.6891 0.178 Uiso 1 1 calc R . . C13 C 0.0231(4) 1.0813(5) 0.8090(6) 0.081(3) Uani 1 1 d . . . H13A H 0.0094 1.0700 0.7502 0.098 Uiso 1 1 calc R . . H13B H 0.0247 1.1272 0.8119 0.098 Uiso 1 1 calc R . . C14 C 0.1157(5) 1.0853(5) 0.8942(8) 0.094(3) Uani 1 1 d . . . H14A H 0.1110 1.1309 0.8906 0.113 Uiso 1 1 calc R . . H14B H 0.1606 1.0757 0.8914 0.113 Uiso 1 1 calc R . . C15 C 0.0914(4) 0.9913(5) 0.8170(6) 0.083(3) Uani 1 1 d . . . H15A H 0.1345 0.9800 0.8328 0.100 Uiso 1 1 calc R . . H15B H 0.0848 0.9783 0.7566 0.100 Uiso 1 1 calc R . . C16 C 0.1564(4) 1.0291(4) 1.0510(6) 0.071(2) Uani 1 1 d . . . H16A H 0.1882 1.0623 1.0539 0.085 Uiso 1 1 calc R . . H16B H 0.1479 1.0141 1.1101 0.085 Uiso 1 1 calc R . . C17 C 0.2333(4) 0.9555(5) 1.0165(7) 0.083(3) Uani 1 1 d . . . C18 C 0.2526(5) 0.9056(5) 0.9556(7) 0.093(3) Uani 1 1 d . . . H18A H 0.2339 0.8661 0.9734 0.139 Uiso 1 1 calc R . . H18B H 0.2979 0.9018 0.9560 0.139 Uiso 1 1 calc R . . H18C H 0.2385 0.9161 0.8974 0.139 Uiso 1 1 calc R . . C19 C 0.0784(5) 1.1324(4) 1.0603(8) 0.091(3) Uani 1 1 d . . . H19A H 0.0397 1.1542 1.0438 0.109 Uiso 1 1 calc R . . H19B H 0.0770 1.1241 1.1230 0.109 Uiso 1 1 calc R . . C20 C 0.1395(8) 1.2195(6) 1.089(2) 0.213(12) Uani 1 1 d . . . C21 C 0.1922(7) 1.2574(6) 1.0526(14) 0.196(11) Uani 1 1 d . . . H21A H 0.1999 1.2933 1.0899 0.294 Uiso 1 1 calc R . . H21B H 0.1812 1.2718 0.9947 0.294 Uiso 1 1 calc R . . H21C H 0.2297 1.2317 1.0495 0.294 Uiso 1 1 calc R . . C22 C 0.0882(7) 0.8805(7) 0.9021(10) 0.048(4) Uiso 0.50 1 d PD B 1 H22A H 0.1298 0.8954 0.9195 0.057 Uiso 0.50 1 calc PR B 1 H22B H 0.0719 0.8538 0.9488 0.057 Uiso 0.50 1 calc PR B 1 C23 C 0.1381(12) 0.7966(13) 0.828(2) 0.143(10) Uiso 0.50 1 d PD B 1 C24 C 0.147(2) 0.781(2) 0.730(4) 0.25(2) Uiso 0.50 1 d PD B 1 H24A H 0.1212 0.8087 0.6956 0.373 Uiso 0.50 1 calc PR B 1 H24B H 0.1346 0.7377 0.7198 0.373 Uiso 0.50 1 calc PR B 1 H24C H 0.1908 0.7863 0.7146 0.373 Uiso 0.50 1 calc PR B 1 C8A C 0.3875(8) 0.7636(8) 0.7866(12) 0.062(4) Uiso 0.50 1 d P A 2 C9A C 0.3341(11) 0.7239(11) 0.7603(16) 0.092(6) Uiso 0.50 1 d P A 2 H9A1 H 0.3347 0.6852 0.7936 0.138 Uiso 0.50 1 calc PR A 2 H9A2 H 0.3373 0.7143 0.6988 0.138 Uiso 0.50 1 calc PR A 2 H9A3 H 0.2952 0.7461 0.7713 0.138 Uiso 0.50 1 calc PR A 2 C22A C 0.0658(9) 0.8660(6) 0.9206(11) 0.058(4) Uiso 0.50 1 d PD C 2 H22C H 0.1048 0.8706 0.9540 0.069 Uiso 0.50 1 calc PR C 2 H22D H 0.0346 0.8463 0.9586 0.069 Uiso 0.50 1 calc PR C 2 C23A C 0.0931(8) 0.7729(11) 0.8536(15) 0.094(6) Uiso 0.50 1 d PD C 2 C24A C 0.1001(11) 0.7431(10) 0.7613(15) 0.098(6) Uiso 0.50 1 d PD C 2 H24D H 0.0931 0.7750 0.7174 0.147 Uiso 0.50 1 calc PR C 2 H24E H 0.0694 0.7098 0.7544 0.147 Uiso 0.50 1 calc PR C 2 H24F H 0.1420 0.7259 0.7549 0.147 Uiso 0.50 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0586(9) 0.0450(8) 0.0310(6) 0.000 0.000 -0.0044(5) Fe2 0.0492(8) 0.0437(7) 0.0418(8) 0.000 0.000 0.0037(6) Cl1 0.0760(12) 0.0610(11) 0.0426(9) 0.0091(9) -0.0052(9) 0.0006(9) Cl2 0.0694(12) 0.0646(12) 0.0544(10) -0.0094(9) 0.0138(10) -0.0015(10) P1 0.0627(11) 0.0520(10) 0.0390(9) -0.0064(8) 0.0084(8) -0.0130(9) P2 0.0577(11) 0.0482(10) 0.0441(9) 0.0031(8) 0.0093(9) -0.0027(8) P3 0.0569(11) 0.0550(11) 0.0683(12) -0.0001(11) 0.0127(11) -0.0016(9) P5 0.0629(12) 0.0715(13) 0.0500(11) -0.0136(10) -0.0132(10) 0.0276(10) O1 0.094(4) 0.083(4) 0.091(5) -0.025(4) 0.019(4) 0.005(4) O2 0.35(2) 0.148(10) 0.152(11) 0.000(8) 0.016(12) 0.114(12) O5 0.063(3) 0.063(3) 0.076(4) -0.009(3) 0.011(3) 0.008(3) O6 0.088(5) 0.132(7) 0.157(8) -0.012(6) 0.067(6) 0.003(4) O7 0.105(6) 0.083(5) 0.200(9) -0.036(5) 0.036(6) -0.035(4) O8 0.214(14) 0.231(16) 0.55(3) -0.28(2) 0.209(19) -0.118(12) O9 0.051(3) 0.092(4) 0.075(3) -0.004(4) -0.007(3) 0.010(3) O10 0.086(5) 0.174(8) 0.159(8) -0.025(7) -0.064(6) 0.030(5) N1 0.064(4) 0.067(4) 0.044(3) -0.013(3) 0.004(3) -0.018(3) N2 0.082(5) 0.095(6) 0.062(5) 0.027(4) 0.028(4) 0.030(4) C1 0.065(5) 0.082(6) 0.037(4) 0.004(4) -0.005(3) -0.016(4) C2 0.070(5) 0.073(5) 0.049(4) -0.016(4) 0.007(4) -0.021(4) C3 0.053(4) 0.059(4) 0.063(4) -0.013(4) 0.015(4) -0.010(3) C4 0.088(6) 0.065(5) 0.058(4) -0.011(4) 0.016(5) 0.002(4) C5 0.154(11) 0.080(7) 0.106(9) 0.020(8) 0.008(9) 0.005(8) C6 0.128(10) 0.108(9) 0.106(8) -0.049(7) 0.039(7) -0.011(7) C7 0.051(5) 0.064(5) 0.089(6) 0.031(4) 0.005(4) -0.010(4) C10 0.061(5) 0.085(6) 0.055(5) 0.002(4) 0.011(4) 0.003(4) C11 0.063(6) 0.087(7) 0.114(8) -0.026(7) 0.010(6) 0.009(5) C12 0.069(7) 0.112(9) 0.176(14) -0.025(8) -0.011(7) 0.029(6) C13 0.080(6) 0.104(7) 0.060(5) 0.027(5) 0.028(5) 0.050(5) C14 0.067(6) 0.108(8) 0.108(9) 0.028(7) 0.043(6) 0.006(5) C15 0.084(6) 0.107(8) 0.058(6) 0.001(5) 0.014(5) 0.039(6) C16 0.060(5) 0.078(6) 0.073(5) -0.013(5) -0.011(4) 0.001(4) C17 0.055(5) 0.101(7) 0.093(7) 0.002(6) -0.020(5) 0.005(5) C18 0.074(6) 0.108(8) 0.096(7) -0.011(6) -0.013(5) 0.022(5) C19 0.083(6) 0.057(5) 0.134(9) -0.032(6) 0.029(6) -0.027(5) C20 0.127(12) 0.068(8) 0.45(4) -0.098(15) 0.086(18) -0.020(8) C21 0.136(12) 0.080(8) 0.37(3) -0.038(12) 0.049(15) -0.051(8) _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 P1 2.164(2) 3_675 ? Fe1 P1 2.164(2) . ? Fe1 P2 2.2304(18) . ? Fe1 P2 2.2304(18) 3_675 ? Fe1 Cl1 2.371(2) . ? Fe1 Cl1 2.371(2) 3_675 ? Fe2 P5 2.161(2) 3_575 ? Fe2 P5 2.161(2) . ? Fe2 P3 2.219(2) . ? Fe2 P3 2.219(2) 3_575 ? Fe2 Cl2 2.351(2) . ? Fe2 Cl2 2.351(2) 3_575 ? P1 C4 1.812(9) . ? P1 C1 1.861(7) 3_675 ? P1 C2 1.882(8) . ? P2 C7 1.838(8) . ? P2 C3 1.851(8) . ? P2 C10 1.859(8) . ? P3 C16 1.841(8) . ? P3 C19 1.852(9) . ? P3 C14 1.870(10) . ? P5 C22 1.815(11) . ? P5 C15 1.869(10) . ? P5 C13 1.871(9) 3_575 ? P5 C22A 1.915(13) . ? O1 C5 1.242(13) . ? O1 C4 1.449(11) . ? O2 C5 1.217(16) . ? O3 C8 1.36(2) . ? O3 C7 1.533(14) . ? O4 C8 1.17(2) . ? O5 C11 1.358(11) . ? O5 C10 1.422(10) . ? O6 C11 1.201(13) . ? O7 C20 1.333(19) . ? O7 C19 1.402(11) . ? O8 C20 1.14(2) . ? O9 C17 1.341(10) . ? O9 C16 1.436(10) . ? O10 C17 1.217(12) . ? O11 C22 1.397(18) . ? O11 C23 1.43(3) . ? O12 C23 1.24(4) . ? O3A C8A 1.33(2) . ? O3A C7 1.399(14) . ? O4A C8A 1.230(19) . ? O11A C23A 1.29(2) . ? O11A C22A 1.30(2) . ? O12A C23A 1.19(3) . ? N1 C3 1.441(10) . ? N1 C2 1.443(10) . ? N1 C1 1.447(10) . ? N2 C14 1.433(14) . ? N2 C15 1.434(12) . ? N2 C13 1.450(11) . ? C1 P1 1.861(7) 3_675 ? C5 C6 1.504(17) . ? C8 C9 1.46(2) . ? C11 C12 1.468(17) . ? C13 P5 1.871(8) 3_575 ? C17 C18 1.491(14) . ? C20 C21 1.51(2) . ? C23 C24 1.57(6) . ? C8A C9A 1.49(3) . ? C23A C24A 1.58(3) . ? 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 P1 Fe1 P1 80.44(13) 3_675 . ? P1 Fe1 P2 92.70(8) 3_675 . ? P1 Fe1 P2 91.90(8) . . ? P1 Fe1 P2 91.90(8) 3_675 3_675 ? P1 Fe1 P2 92.70(8) . 3_675 ? P2 Fe1 P2 173.97(14) . 3_675 ? P1 Fe1 Cl1 173.89(10) 3_675 . ? P1 Fe1 Cl1 93.45(7) . . ? P2 Fe1 Cl1 87.57(8) . . ? P2 Fe1 Cl1 88.27(8) 3_675 . ? P1 Fe1 Cl1 93.45(7) 3_675 3_675 ? P1 Fe1 Cl1 173.89(10) . 3_675 ? P2 Fe1 Cl1 88.27(8) . 3_675 ? P2 Fe1 Cl1 87.57(8) 3_675 3_675 ? Cl1 Fe1 Cl1 92.65(12) . 3_675 ? P5 Fe2 P5 80.67(13) 3_575 . ? P5 Fe2 P3 92.25(10) 3_575 . ? P5 Fe2 P3 92.13(9) . . ? P5 Fe2 P3 92.13(9) 3_575 3_575 ? P5 Fe2 P3 92.25(10) . 3_575 ? P3 Fe2 P3 174.25(16) . 3_575 ? P5 Fe2 Cl2 94.08(8) 3_575 . ? P5 Fe2 Cl2 174.75(10) . . ? P3 Fe2 Cl2 88.14(8) . . ? P3 Fe2 Cl2 87.83(9) 3_575 . ? P5 Fe2 Cl2 174.75(10) 3_575 3_575 ? P5 Fe2 Cl2 94.08(8) . 3_575 ? P3 Fe2 Cl2 87.83(9) . 3_575 ? P3 Fe2 Cl2 88.14(8) 3_575 3_575 ? Cl2 Fe2 Cl2 91.17(13) . 3_575 ? C4 P1 C1 101.1(4) . 3_675 ? C4 P1 C2 101.8(4) . . ? C1 P1 C2 102.7(4) 3_675 . ? C4 P1 Fe1 121.7(3) . . ? C1 P1 Fe1 114.0(3) 3_675 . ? C2 P1 Fe1 113.2(3) . . ? C7 P2 C3 103.3(4) . . ? C7 P2 C10 97.7(4) . . ? C3 P2 C10 101.0(4) . . ? C7 P2 Fe1 117.0(3) . . ? C3 P2 Fe1 114.8(2) . . ? C10 P2 Fe1 120.1(3) . . ? C16 P3 C19 98.2(5) . . ? C16 P3 C14 100.6(5) . . ? C19 P3 C14 101.6(5) . . ? C16 P3 Fe2 121.2(3) . . ? C19 P3 Fe2 116.8(3) . . ? C14 P3 Fe2 115.1(4) . . ? C22 P5 C15 95.5(7) . . ? C22 P5 C13 104.6(6) . 3_575 ? C15 P5 C13 102.7(5) . 3_575 ? C22 P5 C22A 19.6(6) . . ? C15 P5 C22A 114.9(7) . . ? C13 P5 C22A 96.4(6) 3_575 . ? C22 P5 Fe2 122.9(5) . . ? C15 P5 Fe2 113.6(3) . . ? C13 P5 Fe2 114.3(3) 3_575 . ? C22A P5 Fe2 113.3(5) . . ? C5 O1 C4 121.2(10) . . ? C8 O3 C7 113.2(11) . . ? C11 O5 C10 115.4(8) . . ? C20 O7 C19 117.2(12) . . ? C17 O9 C16 115.8(7) . . ? C22 O11 C23 115.4(17) . . ? C8A O3A C7 119.9(12) . . ? C23A O11A C22A 129.0(19) . . ? C3 N1 C2 113.8(6) . . ? C3 N1 C1 113.0(6) . . ? C2 N1 C1 112.9(6) . . ? C14 N2 C15 114.5(8) . . ? C14 N2 C13 112.4(8) . . ? C15 N2 C13 115.3(9) . . ? N1 C1 P1 115.0(5) . 3_675 ? N1 C2 P1 118.0(5) . . ? N1 C3 P2 115.4(5) . . ? O1 C4 P1 103.1(6) . . ? O2 C5 O1 117.5(14) . . ? O2 C5 C6 122.9(13) . . ? O1 C5 C6 119.4(12) . . ? O3A C7 O3 19.5(7) . . ? O3A C7 P2 108.5(7) . . ? O3 C7 P2 107.5(6) . . ? O4 C8 O3 125.5(17) . . ? O4 C8 C9 125.2(18) . . ? O3 C8 C9 109.3(15) . . ? O5 C10 P2 107.3(5) . . ? O6 C11 O5 120.2(11) . . ? O6 C11 C12 128.5(10) . . ? O5 C11 C12 111.2(11) . . ? N2 C13 P5 115.9(5) . 3_575 ? N2 C14 P3 113.7(7) . . ? N2 C15 P5 115.3(6) . . ? O9 C16 P3 105.8(5) . . ? O10 C17 O9 122.6(10) . . ? O10 C17 C18 125.0(9) . . ? O9 C17 C18 112.3(8) . . ? O7 C19 P3 108.6(6) . . ? O8 C20 O7 119.4(15) . . ? O8 C20 C21 130.2(15) . . ? O7 C20 C21 110.0(18) . . ? O11 C22 P5 111.0(10) . . ? O12 C23 O11 115(3) . . ? O12 C23 C24 142(4) . . ? O11 C23 C24 103(3) . . ? O4A C8A O3A 119.0(16) . . ? O4A C8A C9A 126.5(17) . . ? O3A C8A C9A 114.4(16) . . ? O11A C22A P5 112.3(12) . . ? O12A C23A O11A 111(2) . . ? O12A C23A C24A 134(2) . . ? O11A C23A C24A 115(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.65 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.401 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.064 data_c:\word_f~1\papers\inorga~1\adbmkw\14_k06~1\k06adb2 _database_code_depnum_ccdc_archive 'CCDC 616341' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H43 Fe N8 O12.50 P4' _chemical_formula_weight 823.39 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2nn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' 'x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 7.6260(1) _cell_length_b 13.8310(2) _cell_length_c 16.7350(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1765.13(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 28703 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 858 _exptl_absorpt_coefficient_mu 0.679 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31335 _diffrn_reflns_av_R_equivalents 0.0626 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.82 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4022 _reflns_number_gt 3773 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0184P)^2^+0.9028P] 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 -0.011(15) _refine_ls_number_reflns 4022 _refine_ls_number_parameters 234 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0598 _refine_ls_wR_factor_gt 0.0587 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.12523(6) 0.5000 0.0000 0.01061(9) Uani 1 2 d S . . P1 P 0.11279(8) 0.46906(4) 0.13053(3) 0.01303(11) Uani 1 1 d . . . P2 P 0.34664(7) 0.59942(4) 0.01654(3) 0.01212(12) Uani 1 1 d . . . O1 O 0.0461(2) 0.27980(11) 0.13130(9) 0.0216(4) Uani 1 1 d . . . O2 O -0.1437(3) 0.19676(14) 0.20696(12) 0.0461(5) Uani 1 1 d . . . O3 O 0.0444(2) 0.53879(11) 0.27529(8) 0.0202(3) Uani 1 1 d . . . O4 O -0.0631(3) 0.68217(13) 0.31431(11) 0.0330(5) Uani 1 1 d . . . O5 O 0.2311(2) 0.74994(11) 0.09905(9) 0.0191(3) Uani 1 1 d . . . O6 O 0.2766(3) 0.90693(13) 0.07861(13) 0.0511(6) Uani 1 1 d . . . N1 N 0.4794(2) 0.47042(13) 0.13209(10) 0.0149(4) Uani 1 1 d . . . N2 N -0.0752(2) 0.40615(14) -0.01851(12) 0.0163(4) Uani 1 1 d . . . N3 N -0.1116(2) 0.32296(13) -0.02578(11) 0.0182(4) Uani 1 1 d . . . N4 N -0.1630(3) 0.24427(15) -0.03272(14) 0.0362(5) Uani 1 1 d . . . C1 C 0.3267(3) 0.44745(16) 0.18017(12) 0.0175(5) Uani 1 1 d . . . H1A H 0.3311 0.4865 0.2297 0.021 Uiso 1 1 calc R . . H1B H 0.3332 0.3785 0.1958 0.021 Uiso 1 1 calc R . . C2 C 0.4859(3) 0.57094(16) 0.10558(12) 0.0164(4) Uani 1 1 d . . . H2A H 0.6091 0.5874 0.0928 0.020 Uiso 1 1 calc R . . H2B H 0.4487 0.6129 0.1504 0.020 Uiso 1 1 calc R . . C3 C 0.5111(3) 0.40141(15) 0.06783(12) 0.0167(4) Uani 1 1 d . . . H3A H 0.5150 0.3358 0.0914 0.020 Uiso 1 1 calc R . . H3B H 0.6283 0.4148 0.0450 0.020 Uiso 1 1 calc R . . C4 C -0.0206(3) 0.36733(15) 0.16674(13) 0.0178(5) Uani 1 1 d . . . H4A H -0.0137 0.3632 0.2257 0.021 Uiso 1 1 calc R . . H4B H -0.1449 0.3768 0.1515 0.021 Uiso 1 1 calc R . . C5 C -0.0322(3) 0.19759(17) 0.15681(16) 0.0273(6) Uani 1 1 d . . . C6 C 0.0368(4) 0.11094(17) 0.11336(18) 0.0385(7) Uani 1 1 d . . . H6A H -0.0333 0.0541 0.1275 0.058 Uiso 1 1 calc R . . H6B H 0.1593 0.1000 0.1285 0.058 Uiso 1 1 calc R . . H6C H 0.0295 0.1221 0.0556 0.058 Uiso 1 1 calc R . . C7 C 0.0140(3) 0.56464(16) 0.19267(13) 0.0195(5) Uani 1 1 d . . . H7C H 0.0686 0.6279 0.1806 0.023 Uiso 1 1 calc R . . H7D H -0.1134 0.5693 0.1820 0.023 Uiso 1 1 calc R . . C8 C 0.0076(3) 0.60739(16) 0.33052(13) 0.0202(5) Uani 1 1 d . . . C9 C 0.0613(3) 0.57611(19) 0.41235(13) 0.0254(5) Uani 1 1 d . . . H9A H 0.1354 0.6260 0.4366 0.038 Uiso 1 1 calc R . . H9B H 0.1272 0.5154 0.4088 0.038 Uiso 1 1 calc R . . H9C H -0.0433 0.5663 0.4454 0.038 Uiso 1 1 calc R . . C10 C 0.3289(3) 0.73096(14) 0.02752(13) 0.0168(5) Uani 1 1 d . . . H10A H 0.4471 0.7602 0.0313 0.020 Uiso 1 1 calc R . . H10B H 0.2681 0.7591 -0.0193 0.020 Uiso 1 1 calc R . . C11 C 0.2129(3) 0.84476(17) 0.11784(15) 0.0234(5) Uani 1 1 d . . . C12 C 0.1015(4) 0.85748(17) 0.18986(14) 0.0301(6) Uani 1 1 d . . . H12A H 0.1249 0.9209 0.2138 0.045 Uiso 1 1 calc R . . H12B H 0.1286 0.8066 0.2287 0.045 Uiso 1 1 calc R . . H12C H -0.0223 0.8533 0.1746 0.045 Uiso 1 1 calc R . . O7 O 0.6867(10) 0.7611(6) 0.1936(5) 0.043(2) Uani 0.25 1 d P . . 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 0.00940(18) 0.01185(19) 0.01057(18) 0.00066(15) 0.000 0.000 P1 0.0127(2) 0.0148(2) 0.0116(2) 0.00105(18) 0.0006(3) -0.0006(2) P2 0.0111(3) 0.0123(3) 0.0130(2) -0.0007(2) 0.0004(2) -0.0012(2) O1 0.0224(8) 0.0176(8) 0.0247(9) 0.0040(6) 0.0044(7) -0.0019(6) O2 0.0538(13) 0.0328(11) 0.0515(13) 0.0013(9) 0.0261(12) -0.0150(10) O3 0.0299(9) 0.0202(8) 0.0104(8) -0.0011(6) 0.0029(6) 0.0022(7) O4 0.0452(12) 0.0273(10) 0.0263(10) -0.0029(8) 0.0072(8) 0.0094(8) O5 0.0251(8) 0.0146(8) 0.0177(8) -0.0033(6) 0.0070(7) 0.0005(6) O6 0.0763(16) 0.0169(9) 0.0600(14) -0.0058(9) 0.0403(12) -0.0070(10) N1 0.0134(9) 0.0177(9) 0.0138(9) 0.0006(7) -0.0020(7) -0.0007(7) N2 0.0134(9) 0.0158(10) 0.0197(10) -0.0003(9) -0.0016(8) -0.0026(8) N3 0.0133(10) 0.0216(11) 0.0198(10) 0.0012(8) -0.0001(8) -0.0015(8) N4 0.0380(14) 0.0202(11) 0.0504(14) -0.0053(10) 0.0027(12) -0.0089(10) C1 0.0140(11) 0.0244(12) 0.0140(10) 0.0020(9) -0.0040(9) -0.0004(9) C2 0.0136(11) 0.0201(11) 0.0153(11) -0.0002(9) -0.0030(9) -0.0024(9) C3 0.0151(11) 0.0185(11) 0.0166(11) -0.0012(9) -0.0049(9) 0.0027(9) C4 0.0186(11) 0.0194(11) 0.0153(11) 0.0023(9) 0.0028(9) -0.0029(9) C5 0.0266(13) 0.0196(13) 0.0356(15) 0.0058(11) -0.0024(12) -0.0037(10) C6 0.0335(15) 0.0190(14) 0.063(2) 0.0052(13) 0.0071(14) -0.0022(11) C7 0.0241(13) 0.0191(11) 0.0153(11) 0.0014(9) 0.0033(10) 0.0037(10) C8 0.0201(12) 0.0227(13) 0.0177(12) -0.0043(9) 0.0050(10) -0.0029(10) C9 0.0300(13) 0.0322(13) 0.0140(11) -0.0052(10) 0.0020(9) -0.0006(10) C10 0.0204(12) 0.0121(10) 0.0180(11) 0.0001(9) 0.0043(10) -0.0010(9) C11 0.0271(12) 0.0176(12) 0.0256(13) -0.0032(10) 0.0035(11) 0.0005(10) C12 0.0393(16) 0.0229(12) 0.0280(13) -0.0020(9) 0.0080(13) 0.0063(12) O7 0.037(5) 0.044(5) 0.048(5) -0.016(4) 0.009(4) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.0292(19) . ? Fe1 N2 2.0292(19) 2_565 ? Fe1 P2 2.1951(6) . ? Fe1 P2 2.1951(6) 2_565 ? Fe1 P1 2.2279(5) . ? Fe1 P1 2.2279(5) 2_565 ? P1 C4 1.839(2) . ? P1 C7 1.843(2) . ? P1 C1 1.855(2) . ? P2 C10 1.834(2) . ? P2 C2 1.872(2) . ? P2 C3 1.888(2) 2_565 ? O1 C5 1.353(3) . ? O1 C4 1.441(3) . ? O2 C5 1.195(3) . ? O3 C8 1.354(3) . ? O3 C7 1.447(3) . ? O4 C8 1.198(3) . ? O5 C11 1.356(3) . ? O5 C10 1.435(2) . ? O6 C11 1.186(3) . ? N1 C1 1.451(3) . ? N1 C3 1.458(3) . ? N1 C2 1.460(3) . ? N2 N3 1.190(3) . ? N3 N4 1.163(3) . ? C3 P2 1.888(2) 2_565 ? C5 C6 1.497(4) . ? C8 C9 1.493(3) . ? C11 C12 1.485(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N2 82.24(11) . 2_565 ? N2 Fe1 P2 178.08(7) . . ? N2 Fe1 P2 99.18(5) 2_565 . ? N2 Fe1 P2 99.18(5) . 2_565 ? N2 Fe1 P2 178.08(7) 2_565 2_565 ? P2 Fe1 P2 79.44(3) . 2_565 ? N2 Fe1 P1 89.70(6) . . ? N2 Fe1 P1 86.62(6) 2_565 . ? P2 Fe1 P1 91.69(2) . . ? P2 Fe1 P1 92.07(2) 2_565 . ? N2 Fe1 P1 86.62(6) . 2_565 ? N2 Fe1 P1 89.70(6) 2_565 2_565 ? P2 Fe1 P1 92.07(2) . 2_565 ? P2 Fe1 P1 91.69(2) 2_565 2_565 ? P1 Fe1 P1 175.12(4) . 2_565 ? C4 P1 C7 97.86(10) . . ? C4 P1 C1 102.45(10) . . ? C7 P1 C1 102.85(10) . . ? C4 P1 Fe1 119.57(7) . . ? C7 P1 Fe1 115.65(7) . . ? C1 P1 Fe1 115.64(7) . . ? C10 P2 C2 99.85(10) . . ? C10 P2 C3 97.47(10) . 2_565 ? C2 P2 C3 102.54(10) . 2_565 ? C10 P2 Fe1 125.27(8) . . ? C2 P2 Fe1 113.89(7) . . ? C3 P2 Fe1 114.37(7) 2_565 . ? C5 O1 C4 114.86(18) . . ? C8 O3 C7 116.48(17) . . ? C11 O5 C10 115.07(17) . . ? C1 N1 C3 113.51(17) . . ? C1 N1 C2 113.86(17) . . ? C3 N1 C2 113.17(16) . . ? N3 N2 Fe1 144.07(16) . . ? N4 N3 N2 173.8(2) . . ? N1 C1 P1 114.97(14) . . ? N1 C2 P2 115.01(14) . . ? N1 C3 P2 116.44(15) . 2_565 ? O1 C4 P1 108.18(14) . . ? O2 C5 O1 122.9(2) . . ? O2 C5 C6 125.7(2) . . ? O1 C5 C6 111.4(2) . . ? O3 C7 P1 107.24(14) . . ? O4 C8 O3 123.0(2) . . ? O4 C8 C9 125.6(2) . . ? O3 C8 C9 111.47(19) . . ? O5 C10 P2 107.67(14) . . ? O6 C11 O5 122.1(2) . . ? O6 C11 C12 126.7(2) . . ? O5 C11 C12 111.2(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.334 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.058 data_k06adb1 _database_code_depnum_ccdc_archive 'CCDC 616342' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H32 Cl2 Fe N2 O7 P4' _chemical_formula_weight 567.03 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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' _cell_length_a 8.0020(1) _cell_length_b 17.3350(2) _cell_length_c 15.6440(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.004(1) _cell_angle_gamma 90.00 _cell_volume 2130.15(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 36600 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description plate _exptl_crystal_colour ? _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 1.298 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40066 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 30.06 _reflns_number_total 6234 _reflns_number_gt 5759 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0185P)^2^+1.7461P] 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 6234 _refine_ls_number_parameters 285 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0639 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.40897(3) 0.202464(12) 0.655049(13) 0.00904(5) Uani 1 1 d . . . P1 P 0.40444(5) 0.32022(2) 0.59334(3) 0.01155(8) Uani 1 1 d . . . P2 P 0.19173(5) 0.22857(2) 0.71599(2) 0.01048(8) Uani 1 1 d . . . P3 P 0.20367(5) 0.16415(2) 0.55312(2) 0.01058(8) Uani 1 1 d . . . P4 P 0.43681(5) 0.08285(2) 0.71252(3) 0.01108(8) Uani 1 1 d . . . Cl1 Cl 0.61868(5) 0.24563(2) 0.77639(2) 0.01596(8) Uani 1 1 d . . . Cl2 Cl 0.62935(5) 0.17015(2) 0.57651(3) 0.01667(8) Uani 1 1 d . . . N1 N 0.04760(16) 0.31147(8) 0.56267(8) 0.0129(2) Uani 1 1 d . . . N2 N 0.08098(16) 0.07438(8) 0.68095(9) 0.0141(3) Uani 1 1 d . . . O1 O 0.47123(16) 0.40384(8) 0.45625(9) 0.0239(3) Uani 1 1 d D . . H1 H 0.5754(17) 0.4222(14) 0.4674(16) 0.041(7) Uiso 1 1 d D . . O2 O 0.69290(15) 0.38910(7) 0.67979(8) 0.0208(3) Uani 1 1 d D . . H2 H 0.705(3) 0.3471(9) 0.7130(13) 0.031(6) Uiso 1 1 d D . . O3 O 0.27765(16) 0.34596(7) 0.83231(8) 0.0210(3) Uani 1 1 d D . . H3 H 0.3895(13) 0.3436(15) 0.8399(16) 0.039(7) Uiso 1 1 d D . . O4 O 0.10010(14) 0.09269(7) 0.39979(8) 0.0169(2) Uani 1 1 d D . . H4 H 0.134(3) 0.0551(10) 0.3694(13) 0.030(6) Uiso 1 1 d D . . O5 O 0.56814(16) -0.00701(7) 0.85217(8) 0.0206(2) Uani 1 1 d D . . H5 H 0.649(3) -0.0336(15) 0.8339(18) 0.060(9) Uiso 1 1 d D . . O6 O 0.71345(15) 0.01696(7) 0.66603(9) 0.0236(3) Uani 1 1 d D . . H6 H 0.727(3) 0.0629(8) 0.6436(16) 0.042(7) Uiso 1 1 d D . . C1 C 0.4870(2) 0.32776(10) 0.49085(11) 0.0203(3) Uani 1 1 d . . . H1A H 0.6084 0.3124 0.5020 0.024 Uiso 1 1 calc R . . H1B H 0.4236 0.2916 0.4474 0.024 Uiso 1 1 calc R . . C2 C 0.5146(2) 0.40169(9) 0.65666(11) 0.0163(3) Uani 1 1 d . . . H2A H 0.4930 0.4495 0.6218 0.020 Uiso 1 1 calc R . . H2B H 0.4675 0.4088 0.7102 0.020 Uiso 1 1 calc R . . C3 C 0.2117(2) 0.27052(10) 0.82619(10) 0.0155(3) Uani 1 1 d . . . H3A H 0.0981 0.2711 0.8426 0.019 Uiso 1 1 calc R . . H3B H 0.2870 0.2372 0.8683 0.019 Uiso 1 1 calc R . . C4 C 0.25108(19) 0.12313(10) 0.45188(10) 0.0153(3) Uani 1 1 d . . . H4A H 0.2989 0.1637 0.4190 0.018 Uiso 1 1 calc R . . H4B H 0.3370 0.0817 0.4661 0.018 Uiso 1 1 calc R . . C5 C 0.5652(2) 0.07089(9) 0.82291(10) 0.0164(3) Uani 1 1 d . . . H5A H 0.6833 0.0881 0.8230 0.020 Uiso 1 1 calc R . . H5B H 0.5180 0.1041 0.8639 0.020 Uiso 1 1 calc R . . C6 C 0.5346(2) 0.00678(9) 0.65520(11) 0.0170(3) Uani 1 1 d . . . H6A H 0.5103 -0.0444 0.6782 0.020 Uiso 1 1 calc R . . H6B H 0.4835 0.0081 0.5924 0.020 Uiso 1 1 calc R . . C7 C 0.19064(19) 0.36294(9) 0.55768(11) 0.0163(3) Uani 1 1 d . . . H7D H 0.1814 0.4090 0.5939 0.020 Uiso 1 1 calc R . . H7C H 0.1803 0.3805 0.4967 0.020 Uiso 1 1 calc R . . C8 C 0.03182(19) 0.29622(9) 0.65286(10) 0.0144(3) Uani 1 1 d . . . H8A H -0.0832 0.2750 0.6525 0.017 Uiso 1 1 calc R . . H8B H 0.0397 0.3460 0.6843 0.017 Uiso 1 1 calc R . . C9 C 0.04439(19) 0.24121(9) 0.51026(10) 0.0142(3) Uani 1 1 d . . . H9A H 0.0621 0.2562 0.4516 0.017 Uiso 1 1 calc R . . H9B H -0.0709 0.2184 0.5032 0.017 Uiso 1 1 calc R . . C10 C 0.05271(19) 0.14363(9) 0.72896(11) 0.0153(3) Uani 1 1 d . . . H10A H 0.0700 0.1305 0.7916 0.018 Uiso 1 1 calc R . . H10B H -0.0676 0.1594 0.7103 0.018 Uiso 1 1 calc R . . C11 C 0.0665(2) 0.08625(10) 0.58743(10) 0.0160(3) Uani 1 1 d . . . H11A H -0.0539 0.0983 0.5624 0.019 Uiso 1 1 calc R . . H11B H 0.0943 0.0370 0.5613 0.019 Uiso 1 1 calc R . . C12 C 0.2352(2) 0.03328(9) 0.72102(12) 0.0173(3) Uani 1 1 d . . . H12A H 0.2345 -0.0181 0.6934 0.021 Uiso 1 1 calc R . . H12B H 0.2326 0.0251 0.7834 0.021 Uiso 1 1 calc R . . O7 O -0.18632(17) 0.43174(8) 0.47969(9) 0.0245(3) Uani 1 1 d D . . H7A H -0.135(3) 0.3895(10) 0.5035(17) 0.050(8) Uiso 1 1 d D . . H7B H -0.158(3) 0.4678(12) 0.5201(14) 0.050(8) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.00727(9) 0.01032(10) 0.00942(10) -0.00050(7) 0.00128(7) -0.00039(7) P1 0.01026(17) 0.01197(18) 0.01234(18) 0.00098(14) 0.00191(13) -0.00061(13) P2 0.00915(16) 0.01240(18) 0.00992(17) -0.00081(13) 0.00192(13) 0.00027(13) P3 0.00879(16) 0.01267(18) 0.01005(17) -0.00200(13) 0.00127(13) -0.00043(13) P4 0.00992(16) 0.01051(17) 0.01291(18) -0.00013(13) 0.00247(13) 0.00038(13) Cl1 0.01610(17) 0.01536(17) 0.01433(17) -0.00046(13) -0.00240(13) -0.00234(13) Cl2 0.01174(16) 0.01923(18) 0.02046(18) 0.00096(14) 0.00666(13) 0.00165(13) N1 0.0108(6) 0.0151(6) 0.0127(6) 0.0005(5) 0.0016(5) 0.0008(5) N2 0.0116(6) 0.0148(6) 0.0162(6) 0.0000(5) 0.0036(5) -0.0016(5) O1 0.0221(6) 0.0244(7) 0.0254(7) 0.0109(5) 0.0049(5) -0.0019(5) O2 0.0133(5) 0.0180(6) 0.0297(7) 0.0026(5) 0.0002(5) -0.0036(5) O3 0.0190(6) 0.0186(6) 0.0245(6) -0.0066(5) 0.0018(5) -0.0020(5) O4 0.0152(5) 0.0180(6) 0.0158(5) -0.0067(4) -0.0013(4) 0.0019(4) O5 0.0226(6) 0.0161(6) 0.0234(6) 0.0067(5) 0.0048(5) 0.0057(5) O6 0.0155(6) 0.0183(6) 0.0392(8) -0.0028(5) 0.0108(5) 0.0017(5) C1 0.0256(8) 0.0190(8) 0.0186(8) 0.0024(6) 0.0100(7) -0.0013(7) C2 0.0147(7) 0.0130(7) 0.0203(8) -0.0015(6) 0.0011(6) -0.0003(6) C3 0.0155(7) 0.0200(8) 0.0112(7) -0.0025(6) 0.0028(5) -0.0010(6) C4 0.0125(7) 0.0200(8) 0.0130(7) -0.0049(6) 0.0014(5) 0.0003(6) C5 0.0187(7) 0.0141(7) 0.0155(7) 0.0018(6) 0.0009(6) 0.0020(6) C6 0.0160(7) 0.0142(7) 0.0216(8) -0.0035(6) 0.0057(6) 0.0016(6) C7 0.0118(7) 0.0150(7) 0.0207(8) 0.0046(6) -0.0002(6) 0.0010(5) C8 0.0121(7) 0.0179(7) 0.0134(7) 0.0010(6) 0.0026(5) 0.0046(6) C9 0.0109(6) 0.0172(7) 0.0130(7) -0.0009(6) -0.0015(5) 0.0018(5) C10 0.0123(7) 0.0163(7) 0.0184(7) -0.0016(6) 0.0059(6) -0.0025(6) C11 0.0135(7) 0.0180(8) 0.0162(7) -0.0028(6) 0.0023(6) -0.0059(6) C12 0.0133(7) 0.0130(7) 0.0260(8) 0.0044(6) 0.0051(6) -0.0010(6) O7 0.0222(6) 0.0272(7) 0.0235(7) 0.0028(6) 0.0026(5) -0.0002(5) _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 P3 2.1639(4) . ? Fe1 P2 2.1836(4) . ? Fe1 P4 2.2541(4) . ? Fe1 P1 2.2553(4) . ? Fe1 Cl2 2.4001(4) . ? Fe1 Cl1 2.4006(4) . ? P1 C2 1.8491(16) . ? P1 C7 1.8499(16) . ? P1 C1 1.8516(17) . ? P2 C3 1.8497(16) . ? P2 C8 1.8722(15) . ? P2 C10 1.8796(16) . ? P3 C4 1.8406(16) . ? P3 C9 1.8795(16) . ? P3 C11 1.8821(16) . ? P4 C5 1.8449(16) . ? P4 C6 1.8502(16) . ? P4 C12 1.8550(16) . ? N1 C8 1.465(2) . ? N1 C7 1.465(2) . ? N1 C9 1.466(2) . ? N2 C10 1.456(2) . ? N2 C12 1.459(2) . ? N2 C11 1.460(2) . ? O1 C1 1.422(2) . ? O2 C2 1.4206(19) . ? O3 C3 1.407(2) . ? O4 C4 1.4235(18) . ? O5 C5 1.425(2) . ? O6 C6 1.420(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P3 Fe1 P2 80.191(15) . . ? P3 Fe1 P4 90.854(16) . . ? P2 Fe1 P4 92.453(16) . . ? P3 Fe1 P1 90.829(16) . . ? P2 Fe1 P1 92.877(16) . . ? P4 Fe1 P1 174.612(17) . . ? P3 Fe1 Cl2 94.577(16) . . ? P2 Fe1 Cl2 174.760(17) . . ? P4 Fe1 Cl2 87.892(15) . . ? P1 Fe1 Cl2 86.872(15) . . ? P3 Fe1 Cl1 174.945(17) . . ? P2 Fe1 Cl1 94.862(15) . . ? P4 Fe1 Cl1 88.302(15) . . ? P1 Fe1 Cl1 90.462(15) . . ? Cl2 Fe1 Cl1 90.374(15) . . ? C2 P1 C7 100.05(7) . . ? C2 P1 C1 101.40(8) . . ? C7 P1 C1 99.95(8) . . ? C2 P1 Fe1 119.66(6) . . ? C7 P1 Fe1 115.45(5) . . ? C1 P1 Fe1 117.09(6) . . ? C3 P2 C8 100.03(7) . . ? C3 P2 C10 98.91(7) . . ? C8 P2 C10 100.87(7) . . ? C3 P2 Fe1 123.65(5) . . ? C8 P2 Fe1 114.86(5) . . ? C10 P2 Fe1 114.94(5) . . ? C4 P3 C9 101.81(7) . . ? C4 P3 C11 101.27(7) . . ? C9 P3 C11 102.65(7) . . ? C4 P3 Fe1 120.03(5) . . ? C9 P3 Fe1 114.36(5) . . ? C11 P3 Fe1 114.35(5) . . ? C5 P4 C6 99.32(8) . . ? C5 P4 C12 102.57(8) . . ? C6 P4 C12 99.13(8) . . ? C5 P4 Fe1 118.15(5) . . ? C6 P4 Fe1 118.75(6) . . ? C12 P4 Fe1 115.70(5) . . ? C8 N1 C7 111.91(12) . . ? C8 N1 C9 113.17(13) . . ? C7 N1 C9 114.00(12) . . ? C10 N2 C12 112.52(13) . . ? C10 N2 C11 114.21(13) . . ? C12 N2 C11 113.48(13) . . ? O1 C1 P1 112.02(12) . . ? O2 C2 P1 111.83(11) . . ? O3 C3 P2 113.16(11) . . ? O4 C4 P3 110.12(10) . . ? O5 C5 P4 112.29(11) . . ? O6 C6 P4 111.32(11) . . ? N1 C7 P1 115.28(11) . . ? N1 C8 P2 116.44(10) . . ? N1 C9 P3 116.92(10) . . ? N2 C10 P2 115.89(10) . . ? N2 C11 P3 116.59(11) . . ? N2 C12 P4 114.77(11) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.492 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.074 data_c:\word_f~1\papers\inorga~1\adbmkw\3_k02d~1\dd01 _database_code_depnum_ccdc_archive 'CCDC 616343' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H34 Fe N4 O8 P4 S2' _chemical_formula_weight 630.30 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' O O 0.0106 0.0060 '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' P P 0.1023 0.0942 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 15.7040(5) _cell_length_b 9.7750(3) _cell_length_c 17.6430(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.309(2) _cell_angle_gamma 90.00 _cell_volume 2539.95(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 29214 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Pale_Yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 1.057 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33992 _diffrn_reflns_av_R_equivalents 0.1231 _diffrn_reflns_av_sigmaI/netI 0.0819 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.65 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5804 _reflns_number_gt 3791 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^+3.2381P] 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 5804 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0944 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1118 _refine_ls_wR_factor_gt 0.0947 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.17796(3) 0.94073(5) 0.24576(3) 0.01706(13) Uani 1 1 d . . . S1 S 0.12586(7) 0.55341(10) 0.38885(6) 0.0281(2) Uani 1 1 d . . . S2 S -0.13500(7) 1.04331(10) 0.11271(6) 0.0263(2) Uani 1 1 d . . . P1 P 0.17938(7) 0.80037(10) 0.14642(5) 0.0189(2) Uani 1 1 d . . . P2 P 0.22085(7) 1.11350(10) 0.18916(5) 0.0181(2) Uani 1 1 d . . . P3 P 0.32514(7) 0.92284(10) 0.30621(5) 0.0190(2) Uani 1 1 d . . . P4 P 0.16180(7) 1.07732(10) 0.34231(6) 0.0203(2) Uani 1 1 d . A . O1 O 0.08796(19) 0.7229(3) -0.00862(15) 0.0260(6) Uani 1 1 d . . . H1 H 0.1013 0.7722 -0.0419 0.066(18) Uiso 1 1 calc R . . O2 O 0.2688(2) 0.5862(3) 0.23057(18) 0.0398(8) Uani 1 1 d . . . H2 H 0.3041 0.5464 0.2112 0.11(3) Uiso 1 1 calc R . . O3 O 0.17772(19) 1.3067(3) 0.07562(16) 0.0286(6) Uani 1 1 d . . . H3 H 0.1386 1.3471 0.0371 0.054(16) Uiso 1 1 calc R . . O4 O 0.3537(2) 0.8318(3) 0.45422(17) 0.0403(8) Uani 1 1 d . . . H4 H 0.3526 0.7612 0.4811 0.10(2) Uiso 1 1 calc R . . O5 O 0.1221(3) 1.0752(3) 0.48128(18) 0.0508(9) Uani 1 1 d . A 1 O6 O 0.0659(2) 1.2958(3) 0.25812(17) 0.0356(7) Uani 1 1 d . A . H6 H 0.0789 1.3723 0.2810 0.048(15) Uiso 1 1 calc R . . O7 O 0.4456(2) 0.9448(3) 0.04954(19) 0.0275(7) Uani 1 1 d . . . O8 O 0.4320(3) 1.4269(4) 0.4139(2) 0.0599(10) Uani 1 1 d . . . N1 N 0.1507(2) 0.7821(3) 0.30141(18) 0.0220(7) Uani 1 1 d . . . N2 N 0.0485(2) 0.9687(3) 0.18764(18) 0.0199(7) Uani 1 1 d . . . N3 N 0.3412(2) 0.9281(3) 0.15146(17) 0.0201(7) Uani 1 1 d . . . N4 N 0.3228(2) 1.2048(3) 0.34694(17) 0.0216(7) Uani 1 1 d . . . C1 C 0.1406(2) 0.6866(4) 0.3364(2) 0.0208(8) Uani 1 1 d . . . C2 C -0.0273(3) 0.9979(4) 0.1560(2) 0.0211(8) Uani 1 1 d . . . C3 C 0.2729(3) 0.8268(4) 0.1072(2) 0.0227(8) Uani 1 1 d . . . H3A H 0.3038 0.7381 0.1084 0.027 Uiso 1 1 calc R . . H3B H 0.2466 0.8559 0.0500 0.027 Uiso 1 1 calc R . . C4 C 0.3887(3) 0.8893(4) 0.2362(2) 0.0239(8) Uani 1 1 d . . . H4A H 0.4470 0.9396 0.2563 0.029 Uiso 1 1 calc R . . H4B H 0.4031 0.7905 0.2382 0.029 Uiso 1 1 calc R . . C5 C 0.3808(3) 1.0834(4) 0.3586(2) 0.0233(8) Uani 1 1 d . . . H5A H 0.4070 1.0644 0.4173 0.028 Uiso 1 1 calc R . . H5B H 0.4318 1.1056 0.3399 0.028 Uiso 1 1 calc R . . C6 C 0.2576(3) 1.1962(4) 0.3892(2) 0.0241(8) Uani 1 1 d . . . H6A H 0.2327 1.2887 0.3913 0.029 Uiso 1 1 calc R . . H6B H 0.2900 1.1666 0.4456 0.029 Uiso 1 1 calc R . . C7 C 0.2822(3) 1.2495(4) 0.2620(2) 0.0229(8) Uani 1 1 d . . . H7C H 0.3310 1.2867 0.2444 0.028 Uiso 1 1 calc R . . H7D H 0.2391 1.3249 0.2592 0.028 Uiso 1 1 calc R . . C8 C 0.3064(3) 1.0685(4) 0.1405(2) 0.0236(8) Uani 1 1 d . . . H8C H 0.2785 1.0861 0.0818 0.028 Uiso 1 1 calc R . . H8D H 0.3587 1.1315 0.1619 0.028 Uiso 1 1 calc R . . C9 C 0.0779(3) 0.8066(4) 0.0541(2) 0.0226(8) Uani 1 1 d . . . H9A H 0.0244 0.7754 0.0669 0.027 Uiso 1 1 calc R . . H9B H 0.0668 0.9024 0.0349 0.027 Uiso 1 1 calc R . . C10 C 0.1854(3) 0.6154(4) 0.1675(2) 0.0247(8) Uani 1 1 d . . . H10A H 0.1338 0.5875 0.1841 0.030 Uiso 1 1 calc R . . H10B H 0.1817 0.5636 0.1183 0.030 Uiso 1 1 calc R . . C11 C 0.1347(3) 1.2071(4) 0.1080(2) 0.0233(8) Uani 1 1 d . . . H11A H 0.1003 1.1426 0.0650 0.028 Uiso 1 1 calc R . . H11B H 0.0915 1.2520 0.1297 0.028 Uiso 1 1 calc R . . C12 C 0.3761(3) 0.7945(4) 0.3845(2) 0.0276(9) Uani 1 1 d . . . H12A H 0.3517 0.7026 0.3651 0.033 Uiso 1 1 calc R . . H12B H 0.4428 0.7927 0.3983 0.033 Uiso 1 1 calc R . . C13 C 0.1467(3) 0.9856(4) 0.4280(2) 0.0306(10) Uani 1 1 d . . . H13A H 0.0988 0.9154 0.4070 0.037 Uiso 1 1 calc R A 1 H13B H 0.2039 0.9380 0.4588 0.037 Uiso 1 1 calc R A 1 C14 C 0.0630(3) 1.1955(4) 0.3157(2) 0.0265(9) Uani 1 1 d . . . H14A H 0.0063 1.1418 0.2933 0.032 Uiso 1 1 calc R A . H14B H 0.0621 1.2418 0.3652 0.032 Uiso 1 1 calc R . . H7B H 0.446(4) 1.028(7) 0.037(4) 0.08(2) Uiso 1 1 d . . . H7A H 0.428(4) 0.951(6) 0.084(4) 0.07(2) 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 0.0198(3) 0.0136(3) 0.0197(3) 0.0003(2) 0.0092(2) 0.0001(2) S1 0.0350(6) 0.0206(5) 0.0276(5) 0.0056(4) 0.0096(4) -0.0049(4) S2 0.0197(5) 0.0285(5) 0.0303(5) 0.0063(4) 0.0084(4) 0.0009(4) P1 0.0217(5) 0.0155(5) 0.0215(5) -0.0009(4) 0.0100(4) -0.0002(4) P2 0.0210(5) 0.0146(5) 0.0195(4) 0.0007(4) 0.0079(4) 0.0006(4) P3 0.0215(5) 0.0169(5) 0.0197(5) 0.0021(4) 0.0084(4) 0.0017(4) P4 0.0252(5) 0.0165(5) 0.0222(5) -0.0007(4) 0.0123(4) -0.0001(4) O1 0.0365(17) 0.0219(15) 0.0221(13) -0.0034(12) 0.0133(13) -0.0036(12) O2 0.050(2) 0.0314(18) 0.0378(17) 0.0048(14) 0.0154(16) 0.0130(15) O3 0.0283(16) 0.0239(15) 0.0335(16) 0.0119(12) 0.0107(13) -0.0007(12) O4 0.065(2) 0.0312(18) 0.0284(15) 0.0055(14) 0.0215(16) 0.0079(16) O5 0.103(3) 0.0255(17) 0.0426(18) -0.0081(14) 0.0494(19) -0.0065(18) O6 0.0450(19) 0.0237(17) 0.0395(16) 0.0034(14) 0.0165(15) 0.0071(14) O7 0.0328(17) 0.0242(17) 0.0312(16) -0.0014(13) 0.0184(14) 0.0010(13) O8 0.064(3) 0.051(2) 0.072(2) -0.0158(19) 0.033(2) -0.0184(19) N1 0.0263(18) 0.0171(17) 0.0253(16) -0.0002(13) 0.0123(14) 0.0000(13) N2 0.0222(18) 0.0165(16) 0.0236(16) -0.0012(13) 0.0111(14) -0.0027(13) N3 0.0228(17) 0.0176(16) 0.0216(15) -0.0012(13) 0.0098(13) 0.0010(13) N4 0.0234(17) 0.0192(17) 0.0224(15) -0.0021(13) 0.0083(13) -0.0020(13) C1 0.021(2) 0.018(2) 0.0213(18) -0.0036(16) 0.0043(15) 0.0000(15) C2 0.028(2) 0.0150(18) 0.0241(19) 0.0004(15) 0.0136(17) -0.0024(16) C3 0.026(2) 0.021(2) 0.0242(19) -0.0012(16) 0.0125(16) 0.0010(16) C4 0.021(2) 0.025(2) 0.0252(19) -0.0016(16) 0.0069(16) 0.0050(16) C5 0.019(2) 0.025(2) 0.0249(19) -0.0005(16) 0.0063(16) -0.0012(16) C6 0.031(2) 0.0178(19) 0.0243(19) -0.0027(16) 0.0105(17) -0.0003(16) C7 0.029(2) 0.0156(19) 0.0257(19) -0.0007(15) 0.0115(17) -0.0036(16) C8 0.022(2) 0.021(2) 0.029(2) 0.0013(16) 0.0116(16) 0.0004(16) C9 0.024(2) 0.0184(19) 0.0261(19) -0.0035(16) 0.0101(16) -0.0017(16) C10 0.031(2) 0.021(2) 0.0253(19) -0.0007(16) 0.0134(17) 0.0019(17) C11 0.027(2) 0.019(2) 0.0249(19) 0.0008(16) 0.0094(17) 0.0002(16) C12 0.035(2) 0.023(2) 0.025(2) 0.0040(16) 0.0096(18) 0.0040(18) C13 0.045(3) 0.022(2) 0.032(2) -0.0061(17) 0.023(2) -0.0033(19) C14 0.029(2) 0.021(2) 0.032(2) -0.0052(17) 0.0133(18) 0.0007(17) _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 N2 1.952(3) . ? Fe1 N1 1.960(3) . ? Fe1 P2 2.1840(11) . ? Fe1 P3 2.1907(11) . ? Fe1 P1 2.2320(10) . ? Fe1 P4 2.2469(11) . ? S1 C1 1.660(4) . ? S2 C2 1.656(4) . ? P1 C9 1.843(4) . ? P1 C10 1.842(4) . ? P1 C3 1.846(4) . ? P2 C11 1.836(4) . ? P2 C7 1.867(4) . ? P2 C8 1.880(4) . ? P3 C12 1.831(4) . ? P3 C4 1.866(4) . ? P3 C5 1.876(4) . ? P4 C13 1.843(4) . ? P4 C6 1.853(4) . ? P4 C14 1.859(4) . ? O1 C9 1.429(4) . ? O2 C10 1.422(5) . ? O3 C11 1.414(4) . ? O4 C12 1.439(5) . ? O5 C13 1.432(5) . ? O6 C14 1.424(5) . ? N1 C1 1.160(5) . ? N2 C2 1.162(5) . ? N3 C8 1.465(5) . ? N3 C3 1.469(5) . ? N3 C4 1.470(4) . ? N4 C6 1.465(5) . ? N4 C5 1.465(5) . ? N4 C7 1.477(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 N2 Fe1 N1 90.30(13) . . ? N2 Fe1 P2 94.67(9) . . ? N1 Fe1 P2 175.02(10) . . ? N2 Fe1 P3 175.67(9) . . ? N1 Fe1 P3 94.02(10) . . ? P2 Fe1 P3 81.00(4) . . ? N2 Fe1 P1 88.06(9) . . ? N1 Fe1 P1 88.32(9) . . ? P2 Fe1 P1 91.58(4) . . ? P3 Fe1 P1 92.11(4) . . ? N2 Fe1 P4 86.78(9) . . ? N1 Fe1 P4 89.34(9) . . ? P2 Fe1 P4 91.21(4) . . ? P3 Fe1 P4 93.21(4) . . ? P1 Fe1 P4 174.32(4) . . ? C9 P1 C10 100.33(18) . . ? C9 P1 C3 102.75(17) . . ? C10 P1 C3 102.81(18) . . ? C9 P1 Fe1 115.62(12) . . ? C10 P1 Fe1 117.28(12) . . ? C3 P1 Fe1 115.74(12) . . ? C11 P2 C7 104.24(17) . . ? C11 P2 C8 102.15(17) . . ? C7 P2 C8 101.60(18) . . ? C11 P2 Fe1 118.76(13) . . ? C7 P2 Fe1 113.79(12) . . ? C8 P2 Fe1 114.23(12) . . ? C12 P3 C4 100.67(18) . . ? C12 P3 C5 101.25(18) . . ? C4 P3 C5 102.02(18) . . ? C12 P3 Fe1 122.18(14) . . ? C4 P3 Fe1 114.07(12) . . ? C5 P3 Fe1 113.90(12) . . ? C13 P4 C6 104.73(18) . . ? C13 P4 C14 100.13(19) . . ? C6 P4 C14 101.53(18) . . ? C13 P4 Fe1 114.44(13) . . ? C6 P4 Fe1 115.08(12) . . ? C14 P4 Fe1 118.77(13) . . ? C1 N1 Fe1 175.5(3) . . ? C2 N2 Fe1 173.5(3) . . ? C8 N3 C3 113.1(3) . . ? C8 N3 C4 114.2(3) . . ? C3 N3 C4 112.7(3) . . ? C6 N4 C5 113.1(3) . . ? C6 N4 C7 113.7(3) . . ? C5 N4 C7 114.2(3) . . ? N1 C1 S1 178.1(3) . . ? N2 C2 S2 178.3(4) . . ? N3 C3 P1 115.1(2) . . ? N3 C4 P3 115.4(2) . . ? N4 C5 P3 116.6(3) . . ? N4 C6 P4 114.3(2) . . ? N4 C7 P2 115.2(2) . . ? N3 C8 P2 116.9(3) . . ? O1 C9 P1 111.8(3) . . ? O2 C10 P1 108.9(3) . . ? O3 C11 P2 109.4(3) . . ? O4 C12 P3 107.4(3) . . ? O5 C13 P4 112.5(3) . . ? O6 C14 P4 112.3(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.175 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.102 data_c:\word_f~1\papers\inorga~1\adbmkw\4_k05ak2\k05ak2 _database_code_depnum_ccdc_archive 'CCDC 616344' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H31.63 Fe N8 O6.81 P4' _chemical_formula_weight 576.81 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.1620(4) _cell_length_b 9.6070(1) _cell_length_c 27.8860(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.686(1) _cell_angle_gamma 90.00 _cell_volume 8865.75(19) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 67625 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Plate _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.29 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4802 _exptl_absorpt_coefficient_mu 1.023 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54686 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.64 _diffrn_reflns_theta_max 27.47 _reflns_number_total 9984 _reflns_number_gt 8615 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0335P)^2^+27.3733P] 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 9984 _refine_ls_number_parameters 635 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0925 _refine_ls_wR_factor_gt 0.0883 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.125208(9) 0.33814(3) 0.177818(11) 0.00984(8) Uani 1 1 d . . . Fe2 Fe 0.122232(10) 0.99066(3) 0.429504(12) 0.01114(8) Uani 1 1 d . . . P1 P 0.183338(18) 0.23285(6) 0.20036(2) 0.01188(13) Uani 1 1 d . . . P2 P 0.144871(18) 0.53277(6) 0.21244(2) 0.01219(13) Uani 1 1 d . . . P3 P 0.101489(18) 0.30528(6) 0.24787(2) 0.01174(13) Uani 1 1 d . . . P4 P 0.066698(18) 0.43265(7) 0.14882(2) 0.01345(13) Uani 1 1 d . . . P5 P 0.068301(19) 0.85563(7) 0.40765(2) 0.01405(13) Uani 1 1 d . A . P6 P 0.10753(2) 0.99729(7) 0.50449(2) 0.01823(14) Uani 1 1 d . A . P7 P 0.155987(19) 0.80803(7) 0.45605(2) 0.01423(13) Uani 1 1 d . A . P8 P 0.176672(19) 1.12387(7) 0.44502(2) 0.01372(13) Uani 1 1 d . A . O1 O 0.22034(5) -0.0198(2) 0.21083(7) 0.0238(4) Uani 1 1 d . . . H1 H 0.2346 -0.0268 0.1871 0.036 Uiso 1 1 calc R . . O2 O 0.23939(6) 0.41607(19) 0.17596(7) 0.0253(4) Uani 1 1 d . . . H2 H 0.2631 0.4196 0.1885 0.038 Uiso 1 1 calc R . . O3 O 0.14520(6) 0.7264(2) 0.14113(7) 0.0267(4) Uani 1 1 d . . . H3 H 0.1296 0.7869 0.1514 0.040 Uiso 1 1 calc R . . O4 O 0.06299(6) 0.1412(2) 0.30946(7) 0.0307(5) Uani 1 1 d . . . H4 H 0.0811 0.1152 0.3299 0.046 Uiso 1 1 calc R . . O5 O 0.03160(6) 0.5884(2) 0.07569(7) 0.0290(5) Uani 1 1 d . . . H5 H 0.0278 0.6588 0.0927 0.043 Uiso 1 1 calc R . . O6 O 0.01439(6) 0.2491(2) 0.17915(7) 0.0272(4) Uani 1 1 d . . . H6 H -0.0100 0.2254 0.1773 0.041 Uiso 1 1 calc R . . O7 O -0.01038(10) 0.8358(3) 0.38232(13) 0.0432(8) Uani 0.70 1 d P A 1 H7 H -0.0319 0.8728 0.3710 0.065 Uiso 0.70 1 calc PR A 1 O8 O 0.10425(6) 0.6459(2) 0.36031(7) 0.0266(4) Uani 1 1 d . A . H8 H 0.0960 0.5735 0.3734 0.040 Uiso 1 1 calc R . . O9 O 0.03369(10) 1.1047(4) 0.50639(14) 0.0462(9) Uani 0.70 1 d P A 1 H9 H 0.0316 1.1204 0.4767 0.069 Uiso 0.70 1 calc PR A 1 O10 O 0.21237(7) 0.6160(2) 0.44288(9) 0.0411(6) Uani 1 1 d . A . H10 H 0.2254 0.5687 0.4238 0.062 Uiso 1 1 calc R . . O11 O 0.14514(6) 1.3299(2) 0.49348(7) 0.0281(4) Uani 1 1 d . A . H11 H 0.1217 1.3538 0.4835 0.042 Uiso 1 1 calc R . . O12 O 0.24895(5) 1.20061(19) 0.41204(7) 0.0208(4) Uani 1 1 d . A . H12 H 0.2685 1.1457 0.4170 0.031 Uiso 1 1 calc R . . O30 O 0.01459(14) 0.5978(6) -0.02292(16) 0.0514(14) Uani 0.50 1 d P . . O40 O 0.0000 0.8076(14) 0.2500 0.054(4) Uani 0.25 2 d SP . . N1 N 0.18069(6) 0.3705(2) 0.28858(7) 0.0142(4) Uani 1 1 d . . . N2 N 0.06327(6) 0.5667(2) 0.23750(8) 0.0171(4) Uani 1 1 d . . . N3 N 0.10546(6) 0.1559(2) 0.14796(7) 0.0151(4) Uani 1 1 d . . . N4 N 0.09438(6) 0.0435(2) 0.15634(7) 0.0156(4) Uani 1 1 d . . . N5 N 0.08375(7) -0.0724(2) 0.16217(10) 0.0297(6) Uani 1 1 d . . . N6 N 0.14877(6) 0.3750(2) 0.11369(7) 0.0161(4) Uani 1 1 d . . . N7 N 0.16877(6) 0.4503(2) 0.09213(7) 0.0152(4) Uani 1 1 d . . . N8 N 0.18879(7) 0.5181(3) 0.06733(8) 0.0250(5) Uani 1 1 d . . . N9 N 0.08418(7) 0.7128(2) 0.49383(8) 0.0198(5) Uani 1 1 d . A . N10 N 0.19091(7) 0.9799(2) 0.53161(8) 0.0234(5) Uani 1 1 d . A . N11 N 0.13475(7) 0.9902(2) 0.35838(8) 0.0207(5) Uani 1 1 d . . . N12 N 0.15460(7) 0.9272(2) 0.33222(8) 0.0206(5) Uani 1 1 d . . . N13 N 0.17387(8) 0.8699(3) 0.30406(9) 0.0323(6) Uani 1 1 d . . . N14 N 0.08792(7) 1.1597(2) 0.41074(10) 0.0289(6) Uani 1 1 d . . . N15 N 0.08299(6) 1.2789(2) 0.40679(8) 0.0185(5) Uani 1 1 d . . . N16 N 0.07599(8) 1.3990(3) 0.40134(11) 0.0352(6) Uani 1 1 d . . . C1 C 0.18258(7) 0.0411(3) 0.19601(9) 0.0167(5) Uani 1 1 d . . . H1A H 0.1616 0.0042 0.2162 0.020 Uiso 1 1 calc R . . H1B H 0.1752 0.0140 0.1623 0.020 Uiso 1 1 calc R . . C2 C 0.22836(7) 0.2752(3) 0.16727(9) 0.0181(5) Uani 1 1 d . . . H2A H 0.2510 0.2133 0.1780 0.022 Uiso 1 1 calc R . . H2B H 0.2223 0.2603 0.1324 0.022 Uiso 1 1 calc R . . C3 C 0.20258(7) 0.2623(3) 0.26335(9) 0.0149(5) Uani 1 1 d . . . H3A H 0.2009 0.1738 0.2813 0.018 Uiso 1 1 calc R . . H3B H 0.2314 0.2889 0.2636 0.018 Uiso 1 1 calc R . . C4 C 0.17025(8) 0.6724(3) 0.18014(9) 0.0184(5) Uani 1 1 d . . . H4A H 0.1777 0.7487 0.2029 0.022 Uiso 1 1 calc R . . H4B H 0.1954 0.6352 0.1678 0.022 Uiso 1 1 calc R . . C5 C 0.18168(7) 0.5078(3) 0.26543(9) 0.0154(5) Uani 1 1 d . . . H5A H 0.2093 0.5237 0.2550 0.018 Uiso 1 1 calc R . . H5B H 0.1764 0.5796 0.2897 0.018 Uiso 1 1 calc R . . C6 C 0.13992(7) 0.3282(3) 0.29997(8) 0.0157(5) Uani 1 1 d . . . H6A H 0.1294 0.3986 0.3219 0.019 Uiso 1 1 calc R . . H6B H 0.1421 0.2391 0.3178 0.019 Uiso 1 1 calc R . . C7 C 0.10312(7) 0.6317(3) 0.23988(9) 0.0162(5) Uani 1 1 d . . . H7C H 0.1114 0.6489 0.2741 0.019 Uiso 1 1 calc R . . H7D H 0.1006 0.7236 0.2239 0.019 Uiso 1 1 calc R . . C8 C 0.04421(8) 0.5616(3) 0.18876(9) 0.0191(5) Uani 1 1 d . . . H8A H 0.0460 0.6551 0.1741 0.023 Uiso 1 1 calc R . . H8B H 0.0152 0.5396 0.1907 0.023 Uiso 1 1 calc R . . C9 C 0.06197(7) 0.4338(3) 0.26308(9) 0.0167(5) Uani 1 1 d . . . H9A H 0.0351 0.3911 0.2560 0.020 Uiso 1 1 calc R . . H9B H 0.0649 0.4524 0.2981 0.020 Uiso 1 1 calc R . . C10 C 0.07820(8) 0.1382(3) 0.26295(9) 0.0175(5) Uani 1 1 d . . . H10A H 0.0558 0.1171 0.2388 0.021 Uiso 1 1 calc R . . H10B H 0.0985 0.0631 0.2617 0.021 Uiso 1 1 calc R . . C11 C 0.06900(8) 0.5248(3) 0.09106(9) 0.0191(5) Uani 1 1 d . . . H11A H 0.0902 0.5972 0.0943 0.023 Uiso 1 1 calc R . . H11B H 0.0767 0.4579 0.0662 0.023 Uiso 1 1 calc R . . C12 C 0.02389(8) 0.3143(3) 0.13544(9) 0.0190(5) Uani 1 1 d . . . H12A H 0.0003 0.3670 0.1217 0.023 Uiso 1 1 calc R . . H12B H 0.0312 0.2432 0.1118 0.023 Uiso 1 1 calc R . . C13 C 0.01960(8) 0.9403(3) 0.39110(12) 0.0281(6) Uani 1 1 d . . . H13A H 0.0120 1.0020 0.4175 0.034 Uiso 1 1 calc R A 1 H13B H 0.0219 0.9977 0.3619 0.034 Uiso 1 1 calc R A 1 C14 C 0.07205(8) 0.7431(3) 0.35407(9) 0.0212(6) Uani 1 1 d . . . H14A H 0.0463 0.6922 0.3478 0.025 Uiso 1 1 calc R A . H14B H 0.0763 0.8022 0.3257 0.025 Uiso 1 1 calc R . . C15 C 0.05429(8) 0.7290(3) 0.45345(9) 0.0194(5) Uani 1 1 d . . . H15A H 0.0284 0.7585 0.4660 0.023 Uiso 1 1 calc R A . H15B H 0.0498 0.6373 0.4378 0.023 Uiso 1 1 calc R . . C16 C 0.08547(8) 0.8309(3) 0.52646(9) 0.0221(6) Uani 1 1 d . . . H16A H 0.1012 0.8032 0.5563 0.026 Uiso 1 1 calc R A . H16B H 0.0575 0.8504 0.5351 0.026 Uiso 1 1 calc R . . C17 C 0.07211(11) 1.1274(4) 0.52334(14) 0.0424(9) Uani 1 1 d . . . H17A H 0.0731 1.1292 0.5589 0.051 Uiso 1 1 calc R A 1 H17B H 0.0808 1.2200 0.5123 0.051 Uiso 1 1 calc R A 1 C18 C 0.12371(8) 0.6670(3) 0.47940(9) 0.0196(5) Uani 1 1 d . . . H18A H 0.1195 0.5948 0.4542 0.024 Uiso 1 1 calc R A . H18B H 0.1385 0.6231 0.5074 0.024 Uiso 1 1 calc R . . C19 C 0.19022(8) 0.7202(3) 0.41701(10) 0.0246(6) Uani 1 1 d . . . H19A H 0.1744 0.6776 0.3894 0.030 Uiso 1 1 calc R A . H19B H 0.2091 0.7889 0.4043 0.030 Uiso 1 1 calc R . . C20 C 0.19088(9) 0.8404(3) 0.51108(10) 0.0264(6) Uani 1 1 d . . . H20A H 0.1838 0.7738 0.5363 0.032 Uiso 1 1 calc R A . H20B H 0.2188 0.8186 0.5028 0.032 Uiso 1 1 calc R . . C21 C 0.15184(9) 1.0219(3) 0.54858(10) 0.0296(7) Uani 1 1 d . . . H21A H 0.1534 1.1214 0.5577 0.035 Uiso 1 1 calc R A . H21B H 0.1470 0.9681 0.5780 0.035 Uiso 1 1 calc R . . C22 C 0.20848(8) 1.0816(3) 0.50019(9) 0.0192(5) Uani 1 1 d . . . H22A H 0.2348 1.0456 0.4907 0.023 Uiso 1 1 calc R A . H22B H 0.2138 1.1685 0.5186 0.023 Uiso 1 1 calc R . . C23 C 0.16936(8) 1.3123(3) 0.45386(10) 0.0199(5) Uani 1 1 d . . . H23A H 0.1958 1.3588 0.4603 0.024 Uiso 1 1 calc R A . H23B H 0.1558 1.3541 0.4246 0.024 Uiso 1 1 calc R . . C24 C 0.21340(7) 1.1233(3) 0.39812(9) 0.0194(5) Uani 1 1 d . . . H24A H 0.2210 1.0260 0.3912 0.023 Uiso 1 1 calc R A . H24B H 0.2006 1.1636 0.3682 0.023 Uiso 1 1 calc R . . O7A O 0.0047(2) 1.0262(7) 0.4258(4) 0.047(2) Uani 0.30 1 d P A 2 H7A H -0.0095 0.9792 0.4437 0.070 Uiso 0.30 1 calc PR A 2 O9A O 0.0588(4) 1.1330(15) 0.5618(5) 0.088(4) Uani 0.30 1 d P A 2 H9C H 0.0778 1.1354 0.5832 0.132 Uiso 0.30 1 calc PR A 2 O20A O 0.26395(11) -0.0553(3) 0.13497(12) 0.0232(7) Uani 0.60 1 d PD B 1 O20B O 0.24296(16) -0.0274(6) 0.11230(18) 0.0272(12) Uani 0.40 1 d PD C 2 H20C H 0.2868(9) -0.084(6) 0.1506(18) 0.036(16) Uiso 0.60 1 d PD . . H20D H 0.225(2) 0.005(9) 0.090(2) 0.04(3) Uiso 0.40 1 d PD . . H20E H 0.2511(10) -0.1155(13) 0.1155(12) 0.074(15) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01048(16) 0.00986(16) 0.00913(16) 0.00014(13) 0.00026(12) 0.00047(12) Fe2 0.01273(17) 0.00961(17) 0.01101(17) 0.00024(13) 0.00021(13) 0.00020(13) P1 0.0109(3) 0.0120(3) 0.0127(3) 0.0000(2) 0.0001(2) 0.0009(2) P2 0.0139(3) 0.0100(3) 0.0126(3) -0.0003(2) 0.0003(2) 0.0000(2) P3 0.0119(3) 0.0135(3) 0.0099(3) 0.0004(2) 0.0011(2) 0.0002(2) P4 0.0131(3) 0.0134(3) 0.0135(3) 0.0010(2) -0.0019(2) 0.0020(2) P5 0.0134(3) 0.0136(3) 0.0150(3) 0.0002(2) -0.0004(2) -0.0008(2) P6 0.0230(3) 0.0177(3) 0.0148(3) -0.0043(3) 0.0069(3) -0.0029(3) P7 0.0158(3) 0.0120(3) 0.0145(3) 0.0005(2) -0.0017(2) 0.0013(2) P8 0.0152(3) 0.0126(3) 0.0132(3) -0.0009(2) -0.0004(2) -0.0017(2) O1 0.0170(9) 0.0197(10) 0.0338(11) 0.0012(9) -0.0054(8) 0.0071(8) O2 0.0200(9) 0.0210(10) 0.0351(11) 0.0065(9) 0.0038(8) -0.0032(8) O3 0.0387(12) 0.0199(10) 0.0213(10) 0.0048(8) 0.0010(9) 0.0044(9) O4 0.0298(11) 0.0391(12) 0.0235(10) 0.0065(9) 0.0040(9) 0.0016(9) O5 0.0344(11) 0.0280(11) 0.0236(11) 0.0049(9) -0.0052(9) 0.0164(9) O6 0.0239(10) 0.0348(12) 0.0229(10) 0.0020(9) 0.0024(8) -0.0103(9) O7 0.0337(18) 0.0394(19) 0.055(2) 0.0083(17) -0.0064(16) -0.0005(15) O8 0.0309(11) 0.0231(10) 0.0259(11) -0.0049(9) 0.0027(8) 0.0014(8) O9 0.0333(18) 0.050(2) 0.057(2) -0.0099(19) 0.0149(16) 0.0101(16) O10 0.0458(14) 0.0342(13) 0.0432(14) 0.0011(11) 0.0019(11) 0.0116(11) O11 0.0284(11) 0.0251(11) 0.0313(11) -0.0073(9) 0.0060(9) 0.0027(9) O12 0.0124(8) 0.0194(9) 0.0305(11) 0.0014(8) -0.0003(8) -0.0011(7) O30 0.040(3) 0.094(4) 0.020(2) -0.002(2) 0.002(2) 0.030(3) O40 0.057(9) 0.030(7) 0.078(11) 0.000 0.031(8) 0.000 N1 0.0130(10) 0.0152(10) 0.0142(10) -0.0014(8) -0.0010(8) -0.0007(8) N2 0.0160(10) 0.0180(11) 0.0173(11) -0.0018(9) 0.0007(8) 0.0029(9) N3 0.0167(10) 0.0121(10) 0.0162(10) -0.0009(8) -0.0017(8) -0.0012(8) N4 0.0129(10) 0.0163(11) 0.0172(11) -0.0016(9) -0.0008(8) 0.0006(8) N5 0.0271(13) 0.0155(12) 0.0462(16) 0.0040(11) -0.0001(11) -0.0031(10) N6 0.0172(10) 0.0189(11) 0.0126(10) 0.0019(8) 0.0041(8) -0.0019(9) N7 0.0178(10) 0.0168(11) 0.0105(10) -0.0021(8) -0.0023(8) -0.0003(9) N8 0.0285(12) 0.0294(13) 0.0169(11) 0.0029(10) 0.0008(9) -0.0125(10) N9 0.0242(11) 0.0183(11) 0.0169(11) 0.0017(9) 0.0009(9) -0.0058(9) N10 0.0303(13) 0.0228(12) 0.0163(11) 0.0019(9) -0.0048(9) -0.0081(10) N11 0.0258(12) 0.0273(12) 0.0093(10) 0.0000(9) 0.0040(9) -0.0077(10) N12 0.0228(11) 0.0265(12) 0.0123(10) 0.0032(9) -0.0007(9) -0.0096(10) N13 0.0307(14) 0.0397(15) 0.0269(13) -0.0030(12) 0.0049(11) -0.0019(12) N14 0.0269(13) 0.0144(12) 0.0439(15) 0.0023(11) -0.0095(11) 0.0014(10) N15 0.0153(10) 0.0179(12) 0.0223(11) 0.0006(9) 0.0009(8) 0.0010(9) N16 0.0301(14) 0.0146(12) 0.0593(19) 0.0003(12) -0.0084(13) 0.0017(10) C1 0.0147(12) 0.0138(12) 0.0212(13) -0.0018(10) -0.0024(10) 0.0028(10) C2 0.0129(11) 0.0212(13) 0.0206(13) 0.0019(11) 0.0039(10) 0.0000(10) C3 0.0155(12) 0.0151(12) 0.0136(11) 0.0000(10) -0.0021(9) 0.0017(10) C4 0.0203(13) 0.0141(12) 0.0209(13) 0.0014(10) 0.0021(10) -0.0018(10) C5 0.0160(12) 0.0145(12) 0.0152(12) -0.0014(10) -0.0022(9) -0.0013(10) C6 0.0158(12) 0.0216(13) 0.0095(11) -0.0003(10) -0.0007(9) -0.0021(10) C7 0.0185(12) 0.0133(12) 0.0170(12) -0.0035(10) 0.0023(10) 0.0023(10) C8 0.0198(13) 0.0180(13) 0.0192(13) -0.0016(10) -0.0012(10) 0.0061(10) C9 0.0157(12) 0.0200(13) 0.0145(12) -0.0017(10) 0.0027(9) 0.0022(10) C10 0.0206(12) 0.0176(13) 0.0145(12) 0.0026(10) 0.0020(10) -0.0038(10) C11 0.0214(13) 0.0187(13) 0.0167(13) 0.0040(10) -0.0034(10) 0.0018(10) C12 0.0168(12) 0.0215(13) 0.0182(13) 0.0000(10) -0.0022(10) -0.0010(10) C13 0.0154(13) 0.0236(15) 0.0447(18) 0.0062(13) -0.0030(12) 0.0001(11) C14 0.0263(14) 0.0187(13) 0.0179(13) -0.0028(10) -0.0034(11) -0.0044(11) C15 0.0208(13) 0.0187(13) 0.0188(13) 0.0011(10) 0.0016(10) -0.0055(10) C16 0.0273(14) 0.0243(14) 0.0151(12) 0.0016(11) 0.0053(10) -0.0068(11) C17 0.049(2) 0.0306(18) 0.052(2) -0.0118(16) 0.0346(18) -0.0017(15) C18 0.0252(13) 0.0141(12) 0.0190(13) 0.0054(10) -0.0033(10) -0.0011(10) C19 0.0249(14) 0.0200(14) 0.0292(15) -0.0005(12) 0.0048(12) 0.0041(11) C20 0.0317(15) 0.0187(14) 0.0269(15) 0.0058(11) -0.0134(12) -0.0026(12) C21 0.0389(17) 0.0386(17) 0.0115(13) -0.0056(12) 0.0030(12) -0.0130(14) C22 0.0222(13) 0.0201(13) 0.0147(12) 0.0005(10) -0.0038(10) -0.0041(11) C23 0.0210(13) 0.0156(13) 0.0231(14) -0.0009(10) 0.0009(10) -0.0018(10) C24 0.0167(12) 0.0223(14) 0.0193(13) -0.0023(11) 0.0012(10) -0.0034(10) O7A 0.025(4) 0.018(4) 0.100(7) 0.010(4) 0.024(4) 0.009(3) O9A 0.083(8) 0.102(10) 0.080(8) -0.024(8) 0.012(7) -0.022(7) O20A 0.0251(18) 0.0219(17) 0.0225(18) -0.0003(14) 0.0006(15) -0.0006(15) O20B 0.031(3) 0.033(3) 0.017(3) -0.006(2) -0.007(2) 0.017(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N6 2.028(2) . ? Fe1 N3 2.029(2) . ? Fe1 P3 2.1753(7) . ? Fe1 P2 2.1846(7) . ? Fe1 P1 2.2313(7) . ? Fe1 P4 2.2453(7) . ? Fe2 N14 2.032(2) . ? Fe2 N11 2.052(2) . ? Fe2 P6 2.1783(7) . ? Fe2 P7 2.1847(7) . ? Fe2 P8 2.2324(7) . ? Fe2 P5 2.2611(7) . ? P1 C1 1.846(3) . ? P1 C2 1.850(3) . ? P1 C3 1.852(2) . ? P2 C4 1.848(3) . ? P2 C5 1.871(2) . ? P2 C7 1.882(2) . ? P3 C10 1.841(3) . ? P3 C9 1.869(2) . ? P3 C6 1.883(2) . ? P4 C12 1.838(3) . ? P4 C11 1.844(3) . ? P4 C8 1.854(3) . ? P5 C13 1.841(3) . ? P5 C15 1.845(3) . ? P5 C14 1.855(3) . ? P6 C17 1.816(3) . ? P6 C21 1.869(3) . ? P6 C16 1.877(3) . ? P7 C19 1.829(3) . ? P7 C18 1.869(3) . ? P7 C20 1.887(3) . ? P8 C24 1.844(3) . ? P8 C23 1.845(3) . ? P8 C22 1.854(3) . ? O1 C1 1.420(3) . ? O2 C2 1.419(3) . ? O3 C4 1.424(3) . ? O4 C10 1.422(3) . ? O5 C11 1.424(3) . ? O6 C12 1.424(3) . ? O7 C13 1.423(4) . ? O8 C14 1.421(3) . ? O9 C17 1.348(5) . ? O10 C19 1.412(3) . ? O11 C23 1.417(3) . ? O12 C24 1.426(3) . ? N1 C6 1.466(3) . ? N1 C5 1.470(3) . ? N1 C3 1.472(3) . ? N2 C7 1.459(3) . ? N2 C8 1.462(3) . ? N2 C9 1.465(3) . ? N3 N4 1.169(3) . ? N4 N5 1.182(3) . ? N6 N7 1.173(3) . ? N7 N8 1.185(3) . ? N9 C16 1.454(3) . ? N9 C15 1.460(3) . ? N9 C18 1.463(3) . ? N10 C20 1.457(4) . ? N10 C22 1.459(3) . ? N10 C21 1.464(4) . ? N11 N12 1.180(3) . ? N12 N13 1.180(3) . ? N14 N15 1.161(3) . ? N15 N16 1.185(3) . ? C13 O7A 1.386(9) . ? C17 O9A 1.189(12) . ? 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 N6 Fe1 N3 85.48(8) . . ? N6 Fe1 P3 177.68(6) . . ? N3 Fe1 P3 96.75(6) . . ? N6 Fe1 P2 96.86(6) . . ? N3 Fe1 P2 177.61(6) . . ? P3 Fe1 P2 80.92(3) . . ? N6 Fe1 P1 87.29(6) . . ? N3 Fe1 P1 88.55(6) . . ? P3 Fe1 P1 92.11(2) . . ? P2 Fe1 P1 92.04(3) . . ? N6 Fe1 P4 89.14(6) . . ? N3 Fe1 P4 87.27(6) . . ? P3 Fe1 P4 91.61(3) . . ? P2 Fe1 P4 92.26(3) . . ? P1 Fe1 P4 174.71(3) . . ? N14 Fe2 N11 84.12(10) . . ? N14 Fe2 P6 93.88(8) . . ? N11 Fe2 P6 178.00(7) . . ? N14 Fe2 P7 174.44(8) . . ? N11 Fe2 P7 101.23(7) . . ? P6 Fe2 P7 80.77(3) . . ? N14 Fe2 P8 91.39(7) . . ? N11 Fe2 P8 88.70(6) . . ? P6 Fe2 P8 91.45(3) . . ? P7 Fe2 P8 90.25(3) . . ? N14 Fe2 P5 88.23(7) . . ? N11 Fe2 P5 86.78(6) . . ? P6 Fe2 P5 93.07(3) . . ? P7 Fe2 P5 90.56(3) . . ? P8 Fe2 P5 175.48(3) . . ? C1 P1 C2 101.22(12) . . ? C1 P1 C3 102.56(11) . . ? C2 P1 C3 101.52(12) . . ? C1 P1 Fe1 115.21(8) . . ? C2 P1 Fe1 118.04(9) . . ? C3 P1 Fe1 115.89(8) . . ? C4 P2 C5 100.58(11) . . ? C4 P2 C7 101.62(12) . . ? C5 P2 C7 101.73(11) . . ? C4 P2 Fe1 122.55(9) . . ? C5 P2 Fe1 113.59(8) . . ? C7 P2 Fe1 113.93(8) . . ? C10 P3 C9 102.32(12) . . ? C10 P3 C6 101.47(11) . . ? C9 P3 C6 101.38(11) . . ? C10 P3 Fe1 120.85(8) . . ? C9 P3 Fe1 114.04(8) . . ? C6 P3 Fe1 114.20(8) . . ? C12 P4 C11 101.21(12) . . ? C12 P4 C8 101.56(12) . . ? C11 P4 C8 104.16(12) . . ? C12 P4 Fe1 117.45(9) . . ? C11 P4 Fe1 115.18(9) . . ? C8 P4 Fe1 115.18(8) . . ? C13 P5 C15 102.07(13) . . ? C13 P5 C14 99.14(14) . . ? C15 P5 C14 101.91(12) . . ? C13 P5 Fe2 118.69(10) . . ? C15 P5 Fe2 114.95(8) . . ? C14 P5 Fe2 117.30(9) . . ? C17 P6 C21 102.60(16) . . ? C17 P6 C16 102.62(14) . . ? C21 P6 C16 101.50(13) . . ? C17 P6 Fe2 119.14(13) . . ? C21 P6 Fe2 114.84(9) . . ? C16 P6 Fe2 113.86(9) . . ? C19 P7 C18 105.31(13) . . ? C19 P7 C20 100.86(14) . . ? C18 P7 C20 99.85(12) . . ? C19 P7 Fe2 119.54(9) . . ? C18 P7 Fe2 114.06(8) . . ? C20 P7 Fe2 114.66(9) . . ? C24 P8 C23 101.31(12) . . ? C24 P8 C22 102.80(12) . . ? C23 P8 C22 100.18(12) . . ? C24 P8 Fe2 115.07(8) . . ? C23 P8 Fe2 118.47(9) . . ? C22 P8 Fe2 116.44(9) . . ? C6 N1 C5 113.01(19) . . ? C6 N1 C3 113.45(19) . . ? C5 N1 C3 113.44(19) . . ? C7 N2 C8 113.1(2) . . ? C7 N2 C9 113.95(19) . . ? C8 N2 C9 113.5(2) . . ? N4 N3 Fe1 144.32(18) . . ? N3 N4 N5 176.1(3) . . ? N7 N6 Fe1 145.30(18) . . ? N6 N7 N8 174.4(3) . . ? C16 N9 C15 113.0(2) . . ? C16 N9 C18 114.6(2) . . ? C15 N9 C18 113.3(2) . . ? C20 N10 C22 111.7(2) . . ? C20 N10 C21 113.7(2) . . ? C22 N10 C21 113.9(2) . . ? N12 N11 Fe2 138.9(2) . . ? N13 N12 N11 176.2(3) . . ? N15 N14 Fe2 152.4(2) . . ? N14 N15 N16 176.3(3) . . ? O1 C1 P1 112.59(17) . . ? O2 C2 P1 109.38(17) . . ? N1 C3 P1 114.27(16) . . ? O3 C4 P2 112.06(17) . . ? N1 C5 P2 115.49(16) . . ? N1 C6 P3 116.95(16) . . ? N2 C7 P2 116.93(17) . . ? N2 C8 P4 114.46(17) . . ? N2 C9 P3 114.98(17) . . ? O4 C10 P3 111.68(18) . . ? O5 C11 P4 112.65(18) . . ? O6 C12 P4 107.99(16) . . ? O7A C13 O7 105.3(4) . . ? O7A C13 P5 115.7(4) . . ? O7 C13 P5 108.9(2) . . ? O8 C14 P5 111.91(17) . . ? N9 C15 P5 114.56(17) . . ? N9 C16 P6 117.17(18) . . ? O9A C17 O9 85.7(6) . . ? O9A C17 P6 125.3(8) . . ? O9 C17 P6 113.7(3) . . ? N9 C18 P7 114.89(17) . . ? O10 C19 P7 110.2(2) . . ? N10 C20 P7 117.12(18) . . ? N10 C21 P6 115.28(18) . . ? N10 C22 P8 114.67(17) . . ? O11 C23 P8 107.85(17) . . ? O12 C24 P8 112.19(17) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.232 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.081 data_c:\word_f~1\papers\inorga~1\adbmkw\6_k03d~1\dd02 _database_code_depnum_ccdc_archive 'CCDC 616345' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H33.40 Fe N2 O10.70 P4' _chemical_formula_weight 568.75 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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' _cell_length_a 8.6900(1) _cell_length_b 16.3080(2) _cell_length_c 32.2980(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.948(1) _cell_angle_gamma 90.00 _cell_volume 4574.51(10) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14103 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 0.995 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 0.84 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15715 _diffrn_reflns_av_R_equivalents 0.1020 _diffrn_reflns_av_sigmaI/netI 0.2184 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 3.68 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7791 _reflns_number_gt 3670 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0781P)^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 7791 _refine_ls_number_parameters 605 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1983 _refine_ls_R_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.1973 _refine_ls_wR_factor_gt 0.1521 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.78865(14) 0.31603(7) 0.25031(3) 0.0151(3) Uani 1 1 d . . . Fe2 Fe 0.79104(14) 0.76244(7) 0.01312(3) 0.0145(3) Uani 1 1 d . . . P1 P 0.7914(3) 0.39543(14) 0.30628(7) 0.0205(6) Uani 1 1 d . A . P2 P 0.7958(3) 0.22652(14) 0.19815(7) 0.0185(6) Uani 1 1 d . A . P3 P 0.8275(3) 0.42077(14) 0.21031(6) 0.0178(6) Uani 1 1 d . A . P4 P 0.5514(3) 0.34540(14) 0.23431(7) 0.0203(6) Uani 1 1 d . A . P5 P 0.8005(3) 0.68009(14) 0.06774(6) 0.0167(6) Uani 1 1 d . . . P6 P 0.7995(3) 0.85418(13) -0.03851(7) 0.0182(6) Uani 1 1 d . B . P7 P 0.5528(3) 0.73255(14) -0.00158(7) 0.0179(6) Uani 1 1 d . . . P8 P 0.8239(3) 0.65996(13) -0.02931(7) 0.0176(6) Uani 1 1 d . . . O1 O 0.9999(6) 0.2762(3) 0.27150(16) 0.0181(14) Uani 1 1 d . . . O2 O 0.7896(6) 0.2145(3) 0.28898(16) 0.0199(15) Uani 1 1 d . . . O3 O 1.0188(7) 0.1612(3) 0.30999(17) 0.0281(17) Uani 1 1 d . . . O4A O 0.5586(15) 0.3353(8) 0.3484(4) 0.040(4) Uani 0.50 1 d P A 2 H4C H 0.5142 0.3807 0.3449 0.047 Uiso 0.50 1 calc PR A 2 O5 O 1.0438(10) 0.4737(6) 0.2931(3) 0.037(3) Uani 0.70 1 d P A 1 H5 H 1.1325 0.4900 0.3002 0.044 Uiso 0.70 1 calc PR A 1 O6 O 0.7064(9) 0.0664(5) 0.1835(2) 0.068(3) Uani 1 1 d . A . H6 H 0.6827 0.0789 0.1588 0.082 Uiso 1 1 calc R . . O7 O 1.0845(7) 0.2442(4) 0.16965(18) 0.0343(17) Uani 1 1 d . A . H7 H 1.0997 0.2795 0.1882 0.041 Uiso 1 1 calc R . . O8 O 1.0322(7) 0.5090(4) 0.16562(17) 0.0329(17) Uani 1 1 d . A . H8 H 0.9863 0.5518 0.1729 0.039 Uiso 1 1 calc R . . O9 O 0.2557(7) 0.3082(4) 0.23721(18) 0.0378(18) Uani 1 1 d . A . H9 H 0.1844 0.2805 0.2472 0.045 Uiso 1 1 calc R . . O10 O 1.0006(6) 0.8053(3) 0.03279(17) 0.0220(15) Uani 1 1 d . . . O11 O 0.7898(7) 0.8600(3) 0.05349(16) 0.0195(15) Uani 1 1 d . . . O12 O 1.0194(7) 0.9162(4) 0.07356(18) 0.0343(18) Uani 1 1 d . . . O13 O 1.0638(7) 0.5991(4) 0.05773(18) 0.0329(17) Uani 1 1 d . . . H13 H 1.1515 0.5853 0.0670 0.039 Uiso 1 1 calc R . . O14 O 0.7099(7) 0.6712(3) 0.14891(16) 0.0268(16) Uani 1 1 d . . . H14 H 0.7974 0.6529 0.1558 0.032 Uiso 1 1 calc R . . O15 O 0.7158(13) 1.0110(7) -0.0584(4) 0.024(3) Uani 0.50 1 d P B 1 H15 H 0.8040 1.0187 -0.0675 0.029 Uiso 0.50 1 calc PR B 1 O16 O 1.0070(10) 0.9270(5) -0.0878(3) 0.081(3) Uani 1 1 d . B 1 H16 H 1.0996 0.9342 -0.0934 0.097 Uiso 1 1 calc R B 1 O17 O 0.2569(7) 0.7561(4) 0.00454(19) 0.045(2) Uani 1 1 d . . . H17 H 0.1826 0.7817 0.0144 0.054 Uiso 1 1 calc R . . O18 O 1.1136(8) 0.6740(4) -0.0606(2) 0.0423(19) Uani 1 1 d . . . H18 H 1.1300 0.7141 -0.0447 0.051 Uiso 1 1 calc R . . N1 N 0.6213(8) 0.5079(4) 0.2593(2) 0.0226(19) Uani 1 1 d . A . N2 N 0.6319(9) 0.3412(4) 0.1502(2) 0.0217(19) Uani 1 1 d . A . N3 N 0.6229(8) 0.5688(4) 0.0212(2) 0.0197(18) Uani 1 1 d . . . N4 N 0.6262(9) 0.7454(4) -0.0863(2) 0.0224(19) Uani 1 1 d . . . C1 C 0.9376(10) 0.2154(5) 0.2913(3) 0.018(2) Uani 1 1 d . . . C2 C 0.7193(11) 0.3479(6) 0.3530(3) 0.029(2) Uani 1 1 d . . . H2A H 0.6181 0.3231 0.3456 0.035 Uiso 0.50 1 calc PR A 1 H2B H 0.7899 0.3024 0.3608 0.035 Uiso 0.50 1 calc PR A 1 H2AA H 0.811(19) 0.290(9) 0.356(5) 0.035 Uiso 0.50 1 d P C 2 H2BB H 0.79(2) 0.374(10) 0.399(5) 0.035 Uiso 0.50 1 d P D 2 C3 C 0.9841(12) 0.4302(6) 0.3243(3) 0.030(3) Uani 1 1 d . . . H3A H 0.9764 0.4648 0.3493 0.036 Uiso 0.70 1 calc PR A 1 H3B H 1.0506 0.3825 0.3313 0.036 Uiso 0.70 1 calc PR A 1 H3AA H 1.02(4) 0.40(2) 0.338(10) 0.036 Uiso 0.30 1 d P E 2 H3BB H 1.11(3) 0.457(18) 0.332(9) 0.036 Uiso 0.30 1 d P F 2 C4 C 0.6814(11) 0.4922(5) 0.3010(3) 0.028(2) Uani 1 1 d . . . H4A H 0.5943 0.4904 0.3200 0.034 Uiso 1 1 calc R A . H4B H 0.7490 0.5383 0.3098 0.034 Uiso 1 1 calc R . . C5 C 0.4965(10) 0.4523(5) 0.2465(3) 0.026(2) Uani 1 1 d . . . H5A H 0.4429 0.4759 0.2217 0.032 Uiso 1 1 calc R A . H5B H 0.4215 0.4507 0.2689 0.032 Uiso 1 1 calc R . . C6 C 0.7413(10) 0.5179(5) 0.2291(3) 0.026(2) Uani 1 1 d . . . H6A H 0.8246 0.5521 0.2418 0.031 Uiso 1 1 calc R A . H6B H 0.6974 0.5483 0.2050 0.031 Uiso 1 1 calc R . . C7 C 0.7337(11) 0.4107(5) 0.1571(2) 0.026(2) Uani 1 1 d . . . H7A H 0.6742 0.4614 0.1512 0.032 Uiso 1 1 calc R A . H7B H 0.8161 0.4077 0.1367 0.032 Uiso 1 1 calc R . . C8 C 0.5017(10) 0.3396(6) 0.1774(2) 0.025(2) Uani 1 1 d . . . H8A H 0.4429 0.2885 0.1720 0.030 Uiso 1 1 calc R A . H8B H 0.4331 0.3862 0.1700 0.030 Uiso 1 1 calc R . . C9 C 0.7128(10) 0.2644(5) 0.1478(2) 0.023(2) Uani 1 1 d . . . H9A H 0.7972 0.2706 0.1282 0.027 Uiso 1 1 calc R A . H9B H 0.6411 0.2224 0.1363 0.027 Uiso 1 1 calc R . . C10 C 0.6845(12) 0.1326(6) 0.2084(3) 0.036(3) Uani 1 1 d . . . H10A H 0.7083 0.1157 0.2373 0.043 Uiso 1 1 calc R A . H10B H 0.5738 0.1470 0.2065 0.043 Uiso 1 1 calc R . . C11 C 0.9849(10) 0.1832(5) 0.1840(3) 0.025(2) Uani 1 1 d . . . H11A H 1.0335 0.1560 0.2085 0.029 Uiso 1 1 calc R A . H11B H 0.9684 0.1413 0.1621 0.029 Uiso 1 1 calc R . . C12 C 1.0249(10) 0.4502(5) 0.1969(3) 0.024(2) Uani 1 1 d . . . H12A H 1.0791 0.4717 0.2221 0.029 Uiso 1 1 calc R A . H12B H 1.0804 0.4005 0.1881 0.029 Uiso 1 1 calc R . . C13 C 0.3975(10) 0.2850(5) 0.2563(3) 0.024(2) Uani 1 1 d . . . H13A H 0.4162 0.2259 0.2516 0.028 Uiso 1 1 calc R A . H13B H 0.3949 0.2946 0.2865 0.028 Uiso 1 1 calc R . . C14 C 0.9379(12) 0.8630(6) 0.0543(2) 0.022(2) Uani 1 1 d . . . C15 C 0.7228(10) 0.7254(5) 0.1147(3) 0.026(2) Uani 1 1 d . . . H15A H 0.7896 0.7719 0.1235 0.031 Uiso 1 1 calc R . . H15B H 0.6195 0.7479 0.1076 0.031 Uiso 1 1 calc R . . C16 C 0.9911(10) 0.6497(6) 0.0872(3) 0.027(2) Uani 1 1 d . . . H16A H 1.0546 0.6991 0.0927 0.032 Uiso 1 1 calc R . . H16B H 0.9821 0.6194 0.1136 0.032 Uiso 1 1 calc R . . C17 C 0.6985(10) 0.5816(5) 0.0621(2) 0.022(2) Uani 1 1 d . . . H17A H 0.7729 0.5366 0.0675 0.027 Uiso 1 1 calc R . . H17B H 0.6196 0.5784 0.0835 0.027 Uiso 1 1 calc R . . C18 C 0.4974(10) 0.6257(5) 0.0131(3) 0.022(2) Uani 1 1 d . . . H18A H 0.4352 0.6287 0.0382 0.027 Uiso 1 1 calc R . . H18B H 0.4304 0.6029 -0.0095 0.027 Uiso 1 1 calc R . . C19 C 0.7303(10) 0.5627(5) -0.0128(2) 0.019(2) Uani 1 1 d . . . H19A H 0.6739 0.5392 -0.0372 0.023 Uiso 1 1 calc R . . H19B H 0.8124 0.5234 -0.0045 0.023 Uiso 1 1 calc R . . C20 C 0.7364(10) 0.6782(5) -0.0823(2) 0.024(2) Uani 1 1 d . . . H20A H 0.8208 0.6889 -0.1015 0.029 Uiso 1 1 calc R . . H20B H 0.6843 0.6272 -0.0917 0.029 Uiso 1 1 calc R . . C21 C 0.5007(11) 0.7383(5) -0.0584(2) 0.025(2) Uani 1 1 d . . . H21A H 0.4410 0.6885 -0.0660 0.030 Uiso 1 1 calc R . . H21B H 0.4317 0.7860 -0.0630 0.030 Uiso 1 1 calc R . . C22 C 0.6954(11) 0.8260(5) -0.0874(2) 0.027(2) Uani 1 1 d . . . H22A H 0.6137 0.8671 -0.0933 0.032 Uiso 1 1 calc R . . H22B H 0.7680 0.8280 -0.1103 0.032 Uiso 1 1 calc R . . C23 C 0.7251(12) 0.9571(5) -0.0264(3) 0.031(3) Uani 1 1 d . . . H23A H 0.6210 0.9508 -0.0153 0.037 Uiso 0.50 1 calc PR B 1 H23B H 0.7920 0.9812 -0.0042 0.037 Uiso 0.50 1 calc PR B 1 H23C H 0.795(18) 0.979(9) 0.007(5) 0.037 Uiso 0.50 1 d P G 2 H23D H 0.79(2) 1.035(11) -0.052(5) 0.037 Uiso 0.50 1 d P H 2 C25 C 0.3956(10) 0.7897(6) 0.0201(3) 0.032(3) Uani 1 1 d . . . H25A H 0.4008 0.7859 0.0507 0.038 Uiso 1 1 calc R . . H25B H 0.4025 0.8482 0.0122 0.038 Uiso 1 1 calc R . . C26 C 1.0122(10) 0.6182(6) -0.0417(3) 0.028(2) Uani 1 1 d . . . H26A H 1.0628 0.5976 -0.0158 0.033 Uiso 1 1 calc R . . H26B H 0.9961 0.5707 -0.0605 0.033 Uiso 1 1 calc R . . O4 O 0.7013(14) 0.3936(7) 0.3869(3) 0.027(3) Uani 0.50 1 d P A 1 H4 H 0.7869 0.4127 0.3950 0.033 Uiso 0.50 1 calc PR A 1 O5A O 1.002(2) 0.4916(11) 0.3513(5) 0.025(5) Uani 0.30 1 d P A 2 H5A1 H 0.9593 0.4791 0.3735 0.030 Uiso 0.30 1 calc PR A 2 O15A O 0.5690(16) 0.9509(8) -0.0162(4) 0.050(4) Uani 0.50 1 d P B 2 H15C H 0.5348 0.9977 -0.0107 0.060 Uiso 0.50 1 calc PR B 2 O1S O 0.2696(7) 0.5221(3) 0.11108(17) 0.0313(17) Uani 1 1 d . . . O2S O 0.4174(7) 0.6210(4) 0.1679(2) 0.046(2) Uani 1 1 d . . . O3S O 0.5596(10) 0.9386(6) 0.0884(3) 0.045(3) Uani 0.70 1 d P . . O4S O 0.6762(10) 0.0849(5) 0.1017(3) 0.034(2) Uani 0.70 1 d P . . C24 C 0.9988(12) 0.8779(6) -0.0532(3) 0.048(3) Uani 1 1 d . . . H24A H 1.0530 0.9056 -0.0296 0.057 Uiso 1 1 calc R B 1 H24B H 1.0535 0.8258 -0.0584 0.057 Uiso 1 1 calc R B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0130(7) 0.0164(8) 0.0158(6) 0.0017(5) 0.0005(5) 0.0005(6) Fe2 0.0121(7) 0.0163(7) 0.0151(6) -0.0017(5) 0.0001(5) -0.0020(5) P1 0.0215(14) 0.0223(15) 0.0177(12) -0.0003(10) -0.0007(11) -0.0008(11) P2 0.0179(14) 0.0196(14) 0.0176(12) 0.0007(10) -0.0023(11) -0.0019(11) P3 0.0168(13) 0.0191(14) 0.0176(12) 0.0041(10) 0.0013(11) -0.0007(11) P4 0.0132(13) 0.0265(15) 0.0210(13) 0.0016(11) -0.0017(11) 0.0007(11) P5 0.0160(13) 0.0202(14) 0.0140(12) 0.0001(10) 0.0017(10) 0.0014(11) P6 0.0187(14) 0.0171(14) 0.0190(12) 0.0017(10) 0.0004(11) 0.0005(11) P7 0.0137(13) 0.0212(14) 0.0186(12) -0.0023(10) -0.0002(10) -0.0006(11) P8 0.0184(14) 0.0151(14) 0.0195(12) -0.0025(10) 0.0018(11) -0.0019(10) O1 0.015(3) 0.022(4) 0.017(3) 0.003(3) -0.002(3) -0.003(3) O2 0.014(4) 0.021(4) 0.025(3) 0.008(3) -0.002(3) 0.000(3) O3 0.025(4) 0.026(4) 0.032(4) 0.011(3) -0.010(3) 0.007(3) O4A 0.034(9) 0.047(9) 0.038(8) -0.005(7) 0.007(7) -0.011(7) O5 0.029(6) 0.050(7) 0.032(6) 0.002(5) -0.001(5) -0.021(5) O6 0.050(6) 0.085(7) 0.070(6) -0.001(5) 0.005(5) 0.004(5) O7 0.029(4) 0.043(5) 0.032(4) -0.008(3) 0.012(3) 0.000(3) O8 0.040(4) 0.026(4) 0.033(4) 0.005(3) 0.006(3) -0.002(3) O9 0.012(4) 0.061(5) 0.041(4) 0.017(3) -0.001(3) -0.008(3) O10 0.012(3) 0.024(4) 0.030(4) -0.005(3) -0.003(3) -0.004(3) O11 0.016(4) 0.024(4) 0.018(3) -0.004(3) -0.002(3) 0.001(3) O12 0.038(4) 0.025(4) 0.039(4) -0.002(3) -0.011(4) -0.010(3) O13 0.022(4) 0.047(4) 0.030(4) -0.010(3) -0.001(3) 0.012(3) O14 0.023(4) 0.039(4) 0.018(3) 0.007(3) -0.001(3) 0.003(3) O15 0.003(7) 0.019(8) 0.049(9) 0.004(6) -0.006(6) 0.000(5) O16 0.056(6) 0.103(8) 0.083(6) -0.004(6) 0.009(5) -0.013(5) O17 0.016(4) 0.065(5) 0.054(4) -0.024(4) -0.002(3) 0.007(3) O18 0.039(5) 0.046(5) 0.042(4) -0.008(4) 0.004(4) -0.001(4) N1 0.020(5) 0.021(5) 0.027(4) -0.002(3) -0.004(4) 0.013(3) N2 0.024(5) 0.024(5) 0.017(4) -0.004(3) -0.002(4) 0.000(4) N3 0.021(4) 0.016(4) 0.023(4) 0.001(3) 0.001(4) 0.005(3) N4 0.022(5) 0.031(5) 0.014(4) -0.003(4) 0.000(4) -0.001(4) C1 0.018(6) 0.017(5) 0.021(5) -0.002(4) 0.007(4) -0.007(4) C2 0.017(6) 0.054(7) 0.018(5) 0.004(5) 0.008(4) 0.001(5) C3 0.034(7) 0.023(7) 0.032(6) 0.000(5) -0.023(5) -0.011(5) C4 0.029(6) 0.026(6) 0.029(5) -0.007(4) 0.002(5) 0.005(5) C5 0.029(6) 0.021(6) 0.029(5) -0.002(4) 0.005(5) 0.007(5) C6 0.020(6) 0.033(6) 0.026(5) -0.005(4) 0.010(4) 0.001(4) C7 0.031(6) 0.021(6) 0.027(5) 0.005(4) -0.005(5) -0.004(5) C8 0.014(5) 0.040(6) 0.021(5) 0.010(4) -0.003(4) 0.005(4) C9 0.023(6) 0.028(6) 0.016(5) 0.000(4) -0.004(4) -0.003(4) C10 0.056(8) 0.026(6) 0.026(6) -0.004(5) 0.005(5) -0.006(5) C11 0.023(6) 0.027(6) 0.024(5) -0.007(4) 0.007(4) 0.002(5) C12 0.018(5) 0.029(6) 0.024(5) 0.012(4) 0.001(4) -0.006(4) C13 0.016(5) 0.031(6) 0.024(5) 0.005(4) 0.003(4) -0.010(4) C14 0.037(7) 0.021(6) 0.009(5) 0.006(4) 0.001(5) 0.000(5) C15 0.013(5) 0.036(6) 0.028(5) 0.005(4) 0.009(4) 0.004(4) C16 0.020(6) 0.041(6) 0.019(5) -0.002(4) -0.003(4) -0.002(5) C17 0.024(6) 0.016(5) 0.028(5) 0.009(4) 0.005(4) -0.005(4) C18 0.015(5) 0.025(6) 0.026(5) -0.006(4) 0.002(4) -0.009(4) C19 0.020(5) 0.020(5) 0.018(5) -0.003(4) 0.003(4) -0.003(4) C20 0.031(6) 0.026(6) 0.016(5) -0.004(4) 0.000(4) -0.002(5) C21 0.022(6) 0.029(6) 0.023(5) -0.002(4) -0.009(5) -0.001(4) C22 0.033(6) 0.028(6) 0.019(5) 0.001(4) -0.001(4) -0.009(5) C23 0.037(7) 0.018(6) 0.037(6) 0.003(5) 0.005(5) 0.011(5) C25 0.014(5) 0.040(6) 0.041(6) -0.018(5) -0.001(5) 0.003(5) C26 0.022(6) 0.027(6) 0.035(6) 0.006(5) 0.018(5) 0.001(5) O4 0.016(7) 0.043(9) 0.023(7) -0.010(6) -0.004(6) 0.006(6) O5A 0.045(15) 0.021(13) 0.011(10) -0.005(9) 0.000(10) -0.006(10) O15A 0.043(10) 0.040(9) 0.069(10) 0.012(8) 0.041(8) 0.021(8) O1S 0.034(4) 0.028(4) 0.032(4) -0.008(3) -0.001(3) 0.009(3) O2S 0.024(4) 0.051(5) 0.063(5) -0.023(4) 0.007(4) -0.012(3) O3S 0.021(6) 0.044(7) 0.071(7) -0.026(5) 0.016(5) 0.004(5) O4S 0.027(6) 0.023(6) 0.055(6) 0.005(5) 0.016(5) 0.010(4) C24 0.059(8) 0.040(7) 0.046(7) 0.039(6) 0.023(6) 0.014(6) _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 O1 2.044(5) . ? Fe1 O2 2.073(5) . ? Fe1 P4 2.162(2) . ? Fe1 P3 2.175(3) . ? Fe1 P1 2.223(3) . ? Fe1 P2 2.232(3) . ? Fe1 C1 2.451(9) . ? Fe2 O10 2.032(5) . ? Fe2 O11 2.057(5) . ? Fe2 P7 2.164(2) . ? Fe2 P8 2.186(3) . ? Fe2 P5 2.216(2) . ? Fe2 P6 2.243(3) . ? Fe2 C14 2.445(9) . ? P1 C2 1.827(9) . ? P1 C3 1.843(9) . ? P1 C4 1.850(8) . ? P2 C10 1.847(10) . ? P2 C11 1.860(9) . ? P2 C9 1.861(7) . ? P3 C12 1.847(9) . ? P3 C6 1.863(9) . ? P3 C7 1.883(7) . ? P4 C13 1.824(9) . ? P4 C5 1.854(8) . ? P4 C8 1.876(8) . ? P5 C16 1.820(8) . ? P5 C15 1.837(9) . ? P5 C17 1.841(8) . ? P6 C23 1.846(9) . ? P6 C22 1.850(7) . ? P6 C24 1.852(11) . ? P7 C25 1.814(9) . ? P7 C18 1.873(8) . ? P7 C21 1.877(8) . ? P8 C26 1.829(9) . ? P8 C19 1.868(8) . ? P8 C20 1.874(7) . ? O1 C1 1.307(9) . ? O2 C1 1.286(10) . ? O3 C1 1.271(9) . ? O4A C2 1.414(15) . ? O5 C3 1.350(13) . ? O6 C10 1.363(10) . ? O7 C11 1.406(10) . ? O8 C12 1.397(9) . ? O9 C13 1.410(9) . ? O10 C14 1.301(10) . ? O11 C14 1.288(11) . ? O12 C14 1.269(9) . ? O13 C16 1.424(10) . ? O14 C15 1.421(9) . ? O15 C23 1.355(14) . ? O16 C24 1.379(11) . ? O17 C25 1.401(10) . ? O18 C26 1.418(10) . ? N1 C4 1.453(9) . ? N1 C6 1.459(11) . ? N1 C5 1.462(10) . ? N2 C9 1.439(10) . ? N2 C7 1.451(10) . ? N2 C8 1.455(11) . ? N3 C18 1.449(10) . ? N3 C19 1.468(11) . ? N3 C17 1.471(9) . ? N4 C21 1.442(12) . ? N4 C22 1.447(10) . ? N4 C20 1.458(10) . ? C2 O4 1.337(13) . ? C3 O5A 1.334(19) . ? C23 O15A 1.410(16) . ? 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 O1 Fe1 O2 63.8(2) . . ? O1 Fe1 P4 171.50(19) . . ? O2 Fe1 P4 107.76(17) . . ? O1 Fe1 P3 107.05(18) . . ? O2 Fe1 P3 170.85(18) . . ? P4 Fe1 P3 81.37(9) . . ? O1 Fe1 P1 85.88(16) . . ? O2 Fe1 P1 88.59(17) . . ? P4 Fe1 P1 92.81(10) . . ? P3 Fe1 P1 91.60(9) . . ? O1 Fe1 P2 89.82(16) . . ? O2 Fe1 P2 86.16(17) . . ? P4 Fe1 P2 90.89(9) . . ? P3 Fe1 P2 93.24(9) . . ? P1 Fe1 P2 174.30(9) . . ? O1 Fe1 C1 32.2(2) . . ? O2 Fe1 C1 31.7(2) . . ? P4 Fe1 C1 139.4(2) . . ? P3 Fe1 C1 139.2(2) . . ? P1 Fe1 C1 87.7(2) . . ? P2 Fe1 C1 86.7(2) . . ? O10 Fe2 O11 63.9(2) . . ? O10 Fe2 P7 170.6(2) . . ? O11 Fe2 P7 106.72(18) . . ? O10 Fe2 P8 108.9(2) . . ? O11 Fe2 P8 172.79(18) . . ? P7 Fe2 P8 80.49(9) . . ? O10 Fe2 P5 87.19(17) . . ? O11 Fe2 P5 87.99(16) . . ? P7 Fe2 P5 92.72(10) . . ? P8 Fe2 P5 91.93(9) . . ? O10 Fe2 P6 87.22(17) . . ? O11 Fe2 P6 87.50(16) . . ? P7 Fe2 P6 92.43(9) . . ? P8 Fe2 P6 92.04(9) . . ? P5 Fe2 P6 173.96(9) . . ? O10 Fe2 C14 32.1(3) . . ? O11 Fe2 C14 31.8(3) . . ? P7 Fe2 C14 138.5(3) . . ? P8 Fe2 C14 141.0(3) . . ? P5 Fe2 C14 88.20(19) . . ? P6 Fe2 C14 85.84(19) . . ? C2 P1 C3 101.7(4) . . ? C2 P1 C4 104.3(5) . . ? C3 P1 C4 103.2(4) . . ? C2 P1 Fe1 115.5(3) . . ? C3 P1 Fe1 114.8(4) . . ? C4 P1 Fe1 115.5(3) . . ? C10 P2 C11 101.7(5) . . ? C10 P2 C9 104.0(4) . . ? C11 P2 C9 103.3(4) . . ? C10 P2 Fe1 112.3(3) . . ? C11 P2 Fe1 118.8(3) . . ? C9 P2 Fe1 115.0(3) . . ? C12 P3 C6 104.0(4) . . ? C12 P3 C7 100.7(4) . . ? C6 P3 C7 101.9(4) . . ? C12 P3 Fe1 120.5(3) . . ? C6 P3 Fe1 113.7(3) . . ? C7 P3 Fe1 113.7(3) . . ? C13 P4 C5 103.2(4) . . ? C13 P4 C8 101.9(4) . . ? C5 P4 C8 101.7(4) . . ? C13 P4 Fe1 119.6(3) . . ? C5 P4 Fe1 114.1(3) . . ? C8 P4 Fe1 114.1(3) . . ? C16 P5 C15 100.4(4) . . ? C16 P5 C17 103.1(4) . . ? C15 P5 C17 104.0(4) . . ? C16 P5 Fe2 116.7(3) . . ? C15 P5 Fe2 114.2(3) . . ? C17 P5 Fe2 116.5(2) . . ? C23 P6 C22 104.0(4) . . ? C23 P6 C24 101.6(5) . . ? C22 P6 C24 105.6(5) . . ? C23 P6 Fe2 115.4(3) . . ? C22 P6 Fe2 116.2(3) . . ? C24 P6 Fe2 112.6(3) . . ? C25 P7 C18 100.2(4) . . ? C25 P7 C21 101.0(4) . . ? C18 P7 C21 103.8(4) . . ? C25 P7 Fe2 121.8(3) . . ? C18 P7 Fe2 114.0(3) . . ? C21 P7 Fe2 113.6(3) . . ? C26 P8 C19 98.5(4) . . ? C26 P8 C20 101.4(4) . . ? C19 P8 C20 103.2(4) . . ? C26 P8 Fe2 124.0(3) . . ? C19 P8 Fe2 113.8(3) . . ? C20 P8 Fe2 113.2(3) . . ? C1 O1 Fe1 91.3(5) . . ? C1 O2 Fe1 90.6(5) . . ? C14 O10 Fe2 91.7(5) . . ? C14 O11 Fe2 90.9(5) . . ? C4 N1 C6 113.4(7) . . ? C4 N1 C5 113.1(7) . . ? C6 N1 C5 115.0(7) . . ? C9 N2 C7 113.0(7) . . ? C9 N2 C8 114.1(7) . . ? C7 N2 C8 113.8(7) . . ? C18 N3 C19 113.7(6) . . ? C18 N3 C17 112.4(7) . . ? C19 N3 C17 114.0(7) . . ? C21 N4 C22 114.3(7) . . ? C21 N4 C20 113.2(7) . . ? C22 N4 C20 114.4(8) . . ? O3 C1 O2 123.9(8) . . ? O3 C1 O1 121.8(8) . . ? O2 C1 O1 114.2(7) . . ? O3 C1 Fe1 175.6(7) . . ? O2 C1 Fe1 57.8(4) . . ? O1 C1 Fe1 56.5(4) . . ? O4 C2 O4A 91.5(10) . . ? O4 C2 P1 119.5(8) . . ? O4A C2 P1 109.8(7) . . ? O5A C3 O5 93.2(11) . . ? O5A C3 P1 121.3(12) . . ? O5 C3 P1 107.1(6) . . ? N1 C4 P1 113.8(6) . . ? N1 C5 P4 116.7(6) . . ? N1 C6 P3 115.2(6) . . ? N2 C7 P3 116.8(6) . . ? N2 C8 P4 115.6(5) . . ? N2 C9 P2 114.7(6) . . ? O6 C10 P2 117.8(8) . . ? O7 C11 P2 111.8(6) . . ? O8 C12 P3 114.4(5) . . ? O9 C13 P4 109.1(5) . . ? O12 C14 O11 125.3(9) . . ? O12 C14 O10 121.3(9) . . ? O11 C14 O10 113.4(7) . . ? O12 C14 Fe2 176.1(7) . . ? O11 C14 Fe2 57.3(4) . . ? O10 C14 Fe2 56.2(4) . . ? O14 C15 P5 115.7(6) . . ? O13 C16 P5 110.2(5) . . ? N3 C17 P5 114.3(5) . . ? N3 C18 P7 116.3(6) . . ? N3 C19 P8 116.7(6) . . ? N4 C20 P8 116.4(6) . . ? N4 C21 P7 116.9(5) . . ? N4 C22 P6 113.3(5) . . ? O15 C23 O15A 101.1(9) . . ? O15 C23 P6 116.2(8) . . ? O15A C23 P6 109.3(8) . . ? O17 C25 P7 108.1(6) . . ? O18 C26 P8 115.4(6) . . ? O16 C24 P6 113.7(7) . . ? _diffrn_measured_fraction_theta_max 0.742 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.742 _refine_diff_density_max 1.044 _refine_diff_density_min -0.707 _refine_diff_density_rms 0.138 data_c:\word_f~1\papers\inorga~1\adbmkw\6_fepco\fepco _database_code_depnum_ccdc_archive 'CCDC 616346' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H32 Fe N2 O13 P4 S' _chemical_formula_weight 648.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.3463 0.8444 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 16.3440(8) _cell_length_b 14.2436(7) _cell_length_c 20.7566(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4832.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6723 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.782 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 1.044 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33194 _diffrn_reflns_av_R_equivalents 0.0743 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 28.28 _reflns_number_total 5968 _reflns_number_gt 4439 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0465P)^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 5968 _refine_ls_number_parameters 330 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0854 _refine_ls_wR_factor_gt 0.0787 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.429052(19) 0.75246(2) 0.345874(15) 0.01152(8) Uani 1 1 d . . . S1 S 0.73204(3) 0.49273(4) 0.39841(3) 0.01748(13) Uani 1 1 d . . . P1 P 0.46893(3) 0.90441(4) 0.33261(3) 0.01361(13) Uani 1 1 d . . . P2 P 0.35322(4) 0.82370(4) 0.42310(3) 0.01426(13) Uani 1 1 d . . . P3 P 0.32700(3) 0.76732(4) 0.27291(3) 0.01434(13) Uani 1 1 d . . . P4 P 0.53260(4) 0.72404(4) 0.41575(3) 0.01343(13) Uani 1 1 d . . . O1 O 0.53843(10) 0.68906(13) 0.24269(8) 0.0227(4) Uani 1 1 d . . . O2 O 0.36555(11) 0.56448(14) 0.37707(10) 0.0305(5) Uani 1 1 d . . . O3 O 0.57558(11) 1.02937(13) 0.28002(9) 0.0252(4) Uani 1 1 d . . . H3 H 0.6176 1.0229 0.3029 0.030 Uiso 1 1 calc R . . O4 O 0.34823(12) 0.69698(15) 0.51356(10) 0.0343(5) Uani 1 1 d . . . H4 H 0.3225 0.6615 0.5388 0.041 Uiso 1 1 calc R . . O5 O 0.20992(11) 0.68654(13) 0.34460(8) 0.0230(4) Uani 1 1 d . . . H5 H 0.1683 0.7212 0.3445 0.028 Uiso 1 1 calc R . . O6 O 0.41829(10) 0.82614(13) 0.17329(9) 0.0211(4) Uani 1 1 d . . . H6 H 0.3950 0.8736 0.1578 0.025 Uiso 1 1 calc R . . O7 O 0.59060(10) 0.60971(14) 0.50943(8) 0.0232(4) Uani 1 1 d . . . H7 H 0.6322 0.5862 0.4919 0.028 Uiso 1 1 calc R . . O8 O 0.64844(10) 0.79476(12) 0.33848(8) 0.0202(4) Uani 1 1 d . . . H8 H 0.6749 0.8340 0.3604 0.024 Uiso 1 1 calc R . . O9 O 0.64934(11) 0.48386(14) 0.37048(10) 0.0293(4) Uani 1 1 d . . . O10 O 0.72825(11) 0.54958(14) 0.45722(9) 0.0271(4) Uani 1 1 d . . . O11 O 0.76200(11) 0.39685(13) 0.41516(9) 0.0284(4) Uani 1 1 d . . . O12 O 0.78735(12) 0.53490(14) 0.35122(10) 0.0319(5) Uani 1 1 d . . . O13 O 0.08182(12) 0.80470(18) 0.37098(10) 0.0360(5) Uani 1 1 d D . . N1 N 0.29812(12) 0.94609(14) 0.32640(10) 0.0167(4) Uani 1 1 d . . . N2 N 0.50226(12) 0.90285(14) 0.46682(9) 0.0168(4) Uani 1 1 d . . . C1 C 0.49550(14) 0.71323(17) 0.28192(11) 0.0156(5) Uani 1 1 d . . . C2 C 0.38906(13) 0.63641(18) 0.36558(11) 0.0167(5) Uani 1 1 d . . . C3 C 0.37936(14) 0.98505(18) 0.31822(13) 0.0201(5) Uani 1 1 d . . . H3A H 0.3848 1.0393 0.3477 0.024 Uiso 1 1 calc R . . H3B H 0.3836 1.0095 0.2737 0.024 Uiso 1 1 calc R . . C4 C 0.51798(15) 0.95277(17) 0.40726(11) 0.0186(5) Uani 1 1 d . . . H4A H 0.5779 0.9544 0.4003 0.022 Uiso 1 1 calc R . . H4B H 0.4994 1.0184 0.4127 0.022 Uiso 1 1 calc R . . C5 C 0.54093(14) 0.94035(17) 0.26754(12) 0.0183(5) Uani 1 1 d . . . H5A H 0.5852 0.8932 0.2638 0.022 Uiso 1 1 calc R . . H5B H 0.5113 0.9423 0.2260 0.022 Uiso 1 1 calc R . . C6 C 0.41629(14) 0.89218(18) 0.48168(11) 0.0184(5) Uani 1 1 d . . . H6A H 0.3921 0.9556 0.4857 0.022 Uiso 1 1 calc R . . H6B H 0.4117 0.8616 0.5243 0.022 Uiso 1 1 calc R . . C7 C 0.28034(14) 0.91295(18) 0.39094(11) 0.0189(5) Uani 1 1 d . . . H7A H 0.2246 0.8856 0.3912 0.023 Uiso 1 1 calc R . . H7B H 0.2800 0.9675 0.4205 0.023 Uiso 1 1 calc R . . C8 C 0.29197(15) 0.75119(19) 0.47744(12) 0.0204(5) Uani 1 1 d . . . H8A H 0.2587 0.7912 0.5063 0.025 Uiso 1 1 calc R . . H8B H 0.2548 0.7099 0.4526 0.025 Uiso 1 1 calc R . . C9 C 0.27347(14) 0.88192(18) 0.27592(12) 0.0191(5) Uani 1 1 d . . . H9A H 0.2815 0.9137 0.2340 0.023 Uiso 1 1 calc R . . H9B H 0.2142 0.8697 0.2807 0.023 Uiso 1 1 calc R . . C10 C 0.24269(14) 0.68163(18) 0.28140(11) 0.0190(5) Uani 1 1 d . . . H10A H 0.1993 0.6956 0.2495 0.023 Uiso 1 1 calc R . . H10B H 0.2634 0.6175 0.2730 0.023 Uiso 1 1 calc R . . C11 C 0.35888(14) 0.75636(18) 0.18773(11) 0.0175(5) Uani 1 1 d . . . H11A H 0.3823 0.6932 0.1801 0.021 Uiso 1 1 calc R . . H11B H 0.3108 0.7642 0.1592 0.021 Uiso 1 1 calc R . . C12 C 0.55011(15) 0.81821(18) 0.47563(12) 0.0207(5) Uani 1 1 d . . . H12A H 0.5383 0.7927 0.5190 0.025 Uiso 1 1 calc R . . H12B H 0.6088 0.8354 0.4746 0.025 Uiso 1 1 calc R . . C13 C 0.52617(14) 0.61515(18) 0.46371(11) 0.0185(5) Uani 1 1 d . . . H13C H 0.4729 0.6131 0.4865 0.022 Uiso 1 1 calc R . . H13D H 0.5289 0.5602 0.4346 0.022 Uiso 1 1 calc R . . C14 C 0.63314(13) 0.71370(18) 0.37615(12) 0.0177(5) Uani 1 1 d . . . H14A H 0.6765 0.7067 0.4091 0.021 Uiso 1 1 calc R . . H14B H 0.6340 0.6573 0.3483 0.021 Uiso 1 1 calc R . . H13A H 0.0303(10) 0.806(3) 0.3582(19) 0.081(15) Uiso 1 1 d D . . H13B H 0.081(2) 0.837(2) 0.4073(10) 0.050(11) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.00958(15) 0.01178(15) 0.01320(15) 0.00007(13) -0.00021(12) -0.00005(12) S1 0.0150(3) 0.0155(3) 0.0220(3) -0.0013(2) 0.0021(2) 0.0025(2) P1 0.0117(3) 0.0123(3) 0.0169(3) -0.0004(2) 0.0012(2) -0.0007(2) P2 0.0124(3) 0.0161(3) 0.0143(3) 0.0002(2) 0.0018(2) 0.0004(2) P3 0.0119(3) 0.0153(3) 0.0158(3) 0.0006(2) -0.0015(2) -0.0003(2) P4 0.0117(3) 0.0139(3) 0.0147(3) -0.0002(2) -0.0012(2) 0.0007(2) O1 0.0203(9) 0.0255(10) 0.0224(9) -0.0048(8) 0.0013(7) 0.0025(8) O2 0.0298(10) 0.0220(10) 0.0398(12) 0.0076(9) -0.0063(9) -0.0064(9) O3 0.0216(9) 0.0208(10) 0.0331(10) 0.0076(8) -0.0049(8) -0.0078(8) O4 0.0274(10) 0.0393(12) 0.0363(12) 0.0235(10) 0.0059(8) 0.0042(9) O5 0.0194(9) 0.0286(10) 0.0211(9) 0.0025(8) 0.0010(7) -0.0004(8) O6 0.0159(8) 0.0225(10) 0.0248(9) 0.0077(8) 0.0012(7) -0.0003(7) O7 0.0213(9) 0.0323(11) 0.0160(8) 0.0010(8) -0.0004(7) 0.0109(8) O8 0.0186(9) 0.0202(9) 0.0218(9) 0.0014(7) 0.0001(7) -0.0052(7) O9 0.0207(9) 0.0239(10) 0.0433(12) -0.0112(9) -0.0082(8) 0.0027(8) O10 0.0228(9) 0.0316(11) 0.0269(10) -0.0080(8) -0.0029(8) 0.0064(8) O11 0.0269(10) 0.0211(10) 0.0373(11) 0.0077(9) 0.0099(8) 0.0098(8) O12 0.0287(10) 0.0283(11) 0.0386(11) 0.0080(9) 0.0135(9) 0.0031(9) O13 0.0240(10) 0.0558(15) 0.0284(11) -0.0146(10) -0.0052(8) 0.0074(10) N1 0.0128(9) 0.0155(10) 0.0218(10) 0.0001(8) 0.0012(8) 0.0029(8) N2 0.0151(9) 0.0168(10) 0.0186(10) -0.0022(8) 0.0014(8) -0.0009(8) C1 0.0129(11) 0.0157(11) 0.0181(11) 0.0010(9) -0.0029(9) -0.0011(9) C2 0.0118(10) 0.0211(13) 0.0172(11) -0.0025(10) -0.0036(9) 0.0015(10) C3 0.0148(11) 0.0151(12) 0.0303(14) 0.0047(11) 0.0006(10) 0.0021(10) C4 0.0199(12) 0.0160(11) 0.0199(11) -0.0049(10) -0.0002(9) -0.0049(10) C5 0.0150(11) 0.0189(12) 0.0211(12) 0.0009(10) 0.0023(9) -0.0037(10) C6 0.0180(11) 0.0209(12) 0.0163(11) -0.0061(10) 0.0014(9) -0.0007(10) C7 0.0166(11) 0.0207(13) 0.0193(12) 0.0004(10) 0.0025(9) 0.0062(10) C8 0.0160(11) 0.0247(13) 0.0205(12) 0.0045(11) 0.0065(9) 0.0007(10) C9 0.0160(11) 0.0215(13) 0.0198(12) 0.0022(10) -0.0043(9) 0.0041(10) C10 0.0138(11) 0.0224(13) 0.0208(12) 0.0009(10) -0.0027(9) -0.0054(10) C11 0.0169(11) 0.0193(12) 0.0163(11) -0.0002(10) -0.0021(9) -0.0009(10) C12 0.0193(12) 0.0246(14) 0.0182(11) -0.0050(10) -0.0057(9) 0.0030(10) C13 0.0147(11) 0.0215(13) 0.0193(12) 0.0045(10) 0.0004(9) 0.0031(10) C14 0.0135(11) 0.0184(12) 0.0214(12) 0.0010(10) -0.0003(9) 0.0016(10) _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 1.804(2) . ? Fe1 C2 1.824(3) . ? Fe1 P3 2.2628(7) . ? Fe1 P4 2.2653(6) . ? Fe1 P2 2.2660(7) . ? Fe1 P1 2.2771(7) . ? S1 O12 1.4620(19) . ? S1 O10 1.4660(19) . ? S1 O9 1.4762(18) . ? S1 O11 1.4919(19) . ? P1 C5 1.863(2) . ? P1 C4 1.876(2) . ? P1 C3 1.885(2) . ? P2 C8 1.828(2) . ? P2 C7 1.866(2) . ? P2 C6 1.869(2) . ? P3 C10 1.849(2) . ? P3 C11 1.850(2) . ? P3 C9 1.853(3) . ? P4 C14 1.843(2) . ? P4 C13 1.846(2) . ? P4 C12 1.851(3) . ? O1 C1 1.129(3) . ? O2 C2 1.120(3) . ? O3 C5 1.413(3) . ? O4 C8 1.416(3) . ? O5 C10 1.419(3) . ? O6 C11 1.421(3) . ? O7 C13 1.420(3) . ? O8 C14 1.417(3) . ? N1 C9 1.448(3) . ? N1 C3 1.449(3) . ? N1 C7 1.450(3) . ? N2 C6 1.447(3) . ? N2 C12 1.449(3) . ? N2 C4 1.449(3) . ? 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 95.74(11) . . ? C1 Fe1 P3 88.86(7) . . ? C2 Fe1 P3 88.32(7) . . ? C1 Fe1 P4 88.05(7) . . ? C2 Fe1 P4 87.84(7) . . ? P3 Fe1 P4 174.81(3) . . ? C1 Fe1 P2 171.32(8) . . ? C2 Fe1 P2 92.93(8) . . ? P3 Fe1 P2 91.63(2) . . ? P4 Fe1 P2 92.05(2) . . ? C1 Fe1 P1 91.90(8) . . ? C2 Fe1 P1 172.34(8) . . ? P3 Fe1 P1 92.36(2) . . ? P4 Fe1 P1 91.92(2) . . ? P2 Fe1 P1 79.43(2) . . ? O12 S1 O10 110.92(12) . . ? O12 S1 O9 109.77(12) . . ? O10 S1 O9 109.61(11) . . ? O12 S1 O11 109.22(11) . . ? O10 S1 O11 108.99(12) . . ? O9 S1 O11 108.28(11) . . ? C5 P1 C4 103.18(11) . . ? C5 P1 C3 102.02(11) . . ? C4 P1 C3 103.84(12) . . ? C5 P1 Fe1 121.98(8) . . ? C4 P1 Fe1 111.81(8) . . ? C3 P1 Fe1 112.09(8) . . ? C8 P2 C7 104.84(11) . . ? C8 P2 C6 101.28(11) . . ? C7 P2 C6 103.26(12) . . ? C8 P2 Fe1 118.88(9) . . ? C7 P2 Fe1 113.66(8) . . ? C6 P2 Fe1 113.10(8) . . ? C10 P3 C11 104.20(11) . . ? C10 P3 C9 103.08(11) . . ? C11 P3 C9 103.86(11) . . ? C10 P3 Fe1 115.07(8) . . ? C11 P3 Fe1 115.10(8) . . ? C9 P3 Fe1 114.07(8) . . ? C14 P4 C13 102.95(11) . . ? C14 P4 C12 102.68(12) . . ? C13 P4 C12 104.80(12) . . ? C14 P4 Fe1 113.26(8) . . ? C13 P4 Fe1 116.93(8) . . ? C12 P4 Fe1 114.58(8) . . ? C9 N1 C3 114.33(19) . . ? C9 N1 C7 114.0(2) . . ? C3 N1 C7 114.63(19) . . ? C6 N2 C12 114.2(2) . . ? C6 N2 C4 113.94(19) . . ? C12 N2 C4 114.85(19) . . ? O1 C1 Fe1 178.6(2) . . ? O2 C2 Fe1 178.8(2) . . ? N1 C3 P1 117.37(17) . . ? N2 C4 P1 116.66(16) . . ? O3 C5 P1 111.52(17) . . ? N2 C6 P2 116.86(16) . . ? N1 C7 P2 115.12(16) . . ? O4 C8 P2 106.22(16) . . ? N1 C9 P3 116.70(16) . . ? O5 C10 P3 109.69(16) . . ? O6 C11 P3 109.57(16) . . ? N2 C12 P4 115.78(16) . . ? O7 C13 P4 111.36(17) . . ? O8 C14 P4 109.77(16) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.610 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.090 data_c:\x-ray\kappa\k05ak1\maxus\k05ak1 _database_code_depnum_ccdc_archive 'CCDC 616347' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27.90 H49.80 Fe N2 O17.30 P4 S' _chemical_formula_weight 901.89 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' S S 0.1246 0.1234 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 9.4460(2) _cell_length_b 16.4950(3) _cell_length_c 13.4620(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.274(1) _cell_angle_gamma 90.00 _cell_volume 2097.51(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 103663 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Tabloid _exptl_crystal_colour Red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 943 _exptl_absorpt_coefficient_mu 0.631 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39066 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0612 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9522 _reflns_number_gt 8726 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0668P)^2^+1.2389P] 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 0.013(19) _refine_ls_number_reflns 9522 _refine_ls_number_parameters 517 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1281 _refine_ls_wR_factor_gt 0.1251 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.79024(7) 0.74451(5) 0.63306(8) 0.01901(14) Uani 1 1 d . . . S1 S 1.07009(13) 0.73752(9) 0.63460(16) 0.0317(3) Uani 1 1 d . . . P1 P 0.80963(14) 0.87561(8) 0.59650(12) 0.0257(3) Uani 1 1 d . . . P2 P 0.79306(16) 0.61277(8) 0.67223(13) 0.0280(3) Uani 1 1 d . . . P3 P 0.61413(15) 0.72797(8) 0.52976(11) 0.0208(3) Uani 1 1 d . . . P4 P 0.61398(15) 0.76796(9) 0.73270(11) 0.0222(3) Uani 1 1 d . . . O1 O 0.9692(5) 0.7583(3) 0.7178(4) 0.0302(10) Uani 1 1 d . . . O2 O 0.9667(4) 0.7238(3) 0.5492(3) 0.0293(10) Uani 1 1 d . . . O3 O 1.1642(5) 0.8060(3) 0.6146(4) 0.0483(12) Uani 1 1 d . . . O4 O 1.1499(4) 0.6646(3) 0.6573(4) 0.0432(12) Uani 1 1 d . . . O5 O 0.8511(5) 0.8826(3) 0.3985(4) 0.0440(12) Uani 1 1 d . . . O6 O 1.0062(8) 0.9625(5) 0.3221(5) 0.075(2) Uani 1 1 d . . . O7 O 0.8840(6) 1.0156(3) 0.6760(4) 0.0500(13) Uani 1 1 d . . . O8 O 1.0312(8) 1.0427(4) 0.8079(5) 0.0716(19) Uani 1 1 d . . . O9 O 0.7055(5) 0.6250(3) 0.3886(4) 0.0413(12) Uani 1 1 d . . . O10 O 0.6137(11) 0.6144(4) 0.2390(5) 0.094(3) Uani 1 1 d . . . O11 O 0.7073(5) 0.8664(3) 0.8781(4) 0.0373(11) Uani 1 1 d . . . O12 O 0.6100(10) 0.8831(4) 1.0264(6) 0.085(2) Uani 1 1 d . . . O13 O 0.8239(6) 0.6076(3) 0.8701(4) 0.0509(13) Uani 1 1 d . . . O14 O 0.9955(7) 0.5451(4) 0.9584(5) 0.0667(17) Uani 1 1 d . . . O15 O 0.8533(6) 0.4649(3) 0.6091(5) 0.0625(17) Uani 1 1 d . . . O16 O 0.9796(8) 0.4240(4) 0.4776(6) 0.0718(19) Uani 1 1 d . . . O17 O 0.3005(11) 0.7005(7) 0.3595(8) 0.085(2) Uani 0.65 1 d PDU . . O18 O 0.6134(13) 0.1439(7) 0.5551(8) 0.090(3) Uani 0.65 1 d PDU . . N1 N 0.5139(6) 0.8818(3) 0.5905(5) 0.0297(12) Uani 1 1 d . . . N2 N 0.5005(5) 0.6185(3) 0.6691(4) 0.0289(12) Uani 1 1 d . . . C1 C 0.6425(6) 0.9313(3) 0.5802(6) 0.0331(15) Uani 1 1 d . . . H1A H 0.6392 0.9756 0.6297 0.040 Uiso 1 1 calc R . . H1B H 0.6420 0.9565 0.5134 0.040 Uiso 1 1 calc R . . C2 C 0.4985(6) 0.8204(3) 0.5150(5) 0.0258(12) Uani 1 1 d . . . H2A H 0.5190 0.8453 0.4497 0.031 Uiso 1 1 calc R . . H2B H 0.3985 0.8026 0.5137 0.031 Uiso 1 1 calc R . . C3 C 0.4946(6) 0.8537(3) 0.6910(5) 0.0301(14) Uani 1 1 d . . . H3A H 0.3951 0.8358 0.6982 0.036 Uiso 1 1 calc R . . H3B H 0.5092 0.9001 0.7364 0.036 Uiso 1 1 calc R . . C4 C 0.6167(6) 0.5626(3) 0.6870(6) 0.0364(16) Uani 1 1 d . . . H4A H 0.6094 0.5167 0.6399 0.044 Uiso 1 1 calc R . . H4B H 0.6091 0.5406 0.7552 0.044 Uiso 1 1 calc R . . C5 C 0.4849(6) 0.6482(4) 0.5674(5) 0.0293(14) Uani 1 1 d . . . H5A H 0.3880 0.6702 0.5592 0.035 Uiso 1 1 calc R . . H5B H 0.4942 0.6017 0.5214 0.035 Uiso 1 1 calc R . . C6 C 0.4848(7) 0.6823(4) 0.7425(5) 0.0345(15) Uani 1 1 d . . . H6A H 0.4941 0.6580 0.8094 0.041 Uiso 1 1 calc R . . H6B H 0.3879 0.7048 0.7368 0.041 Uiso 1 1 calc R . . C7 C 0.9180(7) 0.9094(4) 0.4911(5) 0.0367(15) Uani 1 1 d . . . H7A H 0.9262 0.9692 0.4916 0.044 Uiso 1 1 calc R . . H7B H 1.0144 0.8861 0.4966 0.044 Uiso 1 1 calc R . . C8 C 0.9086(8) 0.9139(6) 0.3174(7) 0.056(2) Uani 1 1 d . . . C9 C 0.8353(13) 0.8843(8) 0.2235(8) 0.087(4) Uani 1 1 d . . . H9A H 0.7792 0.9284 0.1947 0.130 Uiso 1 1 calc R . . H9B H 0.7729 0.8388 0.2398 0.130 Uiso 1 1 calc R . . H9C H 0.9065 0.8665 0.1755 0.130 Uiso 1 1 calc R . . C10 C 0.9090(7) 0.9306(4) 0.6951(5) 0.0393(16) Uani 1 1 d . . . H10A H 0.8740 0.9153 0.7617 0.047 Uiso 1 1 calc R . . H10B H 1.0113 0.9180 0.6914 0.047 Uiso 1 1 calc R . . C11 C 0.9566(10) 1.0677(4) 0.7441(7) 0.056(2) Uani 1 1 d . . . C12 C 0.9159(12) 1.1514(4) 0.7153(7) 0.070(2) Uani 1 1 d . . . H12A H 0.8715 1.1786 0.7719 0.104 Uiso 1 1 calc R . . H12B H 0.8489 1.1494 0.6595 0.104 Uiso 1 1 calc R . . H12C H 1.0006 1.1816 0.6954 0.104 Uiso 1 1 calc R . . C13 C 0.6421(7) 0.7057(4) 0.3977(5) 0.0308(14) Uani 1 1 d . . . H13A H 0.5506 0.7074 0.3616 0.037 Uiso 1 1 calc R . . H13B H 0.7057 0.7469 0.3683 0.037 Uiso 1 1 calc R . . C14 C 0.6872(9) 0.5844(5) 0.3032(6) 0.0453(18) Uani 1 1 d . . . C15 C 0.7592(8) 0.5071(5) 0.3024(7) 0.055(2) Uani 1 1 d . . . H15A H 0.7113 0.4696 0.3475 0.082 Uiso 1 1 calc R . . H15B H 0.8576 0.5146 0.3241 0.082 Uiso 1 1 calc R . . H15C H 0.7577 0.4848 0.2349 0.082 Uiso 1 1 calc R . . C16 C 0.6355(7) 0.7923(4) 0.8655(5) 0.0342(14) Uani 1 1 d . . . H16A H 0.5413 0.7957 0.8970 0.041 Uiso 1 1 calc R . . H16B H 0.6895 0.7485 0.8987 0.041 Uiso 1 1 calc R . . C17 C 0.6870(8) 0.9064(5) 0.9637(6) 0.0450(18) Uani 1 1 d . . . C18 C 0.7696(9) 0.9823(5) 0.9691(6) 0.054(2) Uani 1 1 d . . . H18A H 0.7241 1.0198 1.0155 0.081 Uiso 1 1 calc R . . H18B H 0.7738 1.0072 0.9031 0.081 Uiso 1 1 calc R . . H18C H 0.8658 0.9703 0.9924 0.081 Uiso 1 1 calc R . . C19 C 0.8938(7) 0.5796(4) 0.7832(5) 0.0372(15) Uani 1 1 d . . . H19A H 0.9003 0.5197 0.7844 0.045 Uiso 1 1 calc R . . H19B H 0.9911 0.6019 0.7809 0.045 Uiso 1 1 calc R . . C20 C 0.8904(10) 0.5837(6) 0.9564(7) 0.059(2) Uani 1 1 d . . . C21 C 0.8200(13) 0.6181(11) 1.0432(8) 0.126(6) Uani 1 1 d . . . H21A H 0.7402 0.5834 1.0621 0.189 Uiso 1 1 calc R . . H21B H 0.7850 0.6725 1.0272 0.189 Uiso 1 1 calc R . . H21C H 0.8874 0.6214 1.0986 0.189 Uiso 1 1 calc R . . C22 C 0.8822(7) 0.5488(4) 0.5822(6) 0.0408(16) Uani 1 1 d . . . H22A H 0.8462 0.5602 0.5144 0.049 Uiso 1 1 calc R . . H22B H 0.9854 0.5592 0.5836 0.049 Uiso 1 1 calc R . . C23 C 0.9136(11) 0.4082(5) 0.5480(8) 0.067(3) Uani 1 1 d . . . C24 C 0.8788(13) 0.3242(4) 0.5895(9) 0.089(4) Uani 1 1 d . . . H24A H 0.8209 0.3300 0.6493 0.133 Uiso 1 1 calc R . . H24B H 0.9669 0.2959 0.6063 0.133 Uiso 1 1 calc R . . H24C H 0.8264 0.2930 0.5395 0.133 Uiso 1 1 calc R . . C25 C 0.0714(15) 0.6929(11) 0.3040(11) 0.084(3) Uani 0.65 1 d PDU . . H25A H 0.0920 0.7439 0.2696 0.127 Uiso 0.65 1 calc PR . . H25B H -0.0083 0.7009 0.3494 0.127 Uiso 0.65 1 calc PR . . H25C H 0.0469 0.6511 0.2552 0.127 Uiso 0.65 1 calc PR . . C26 C 0.1881(13) 0.6689(8) 0.3570(9) 0.070(2) Uani 0.65 1 d PDU . . C27 C 0.1658(12) 0.5964(7) 0.4046(10) 0.057(3) Uani 0.65 1 d PDU . . H27A H 0.2413 0.5582 0.3871 0.085 Uiso 0.65 1 calc PR . . H27B H 0.0741 0.5740 0.3840 0.085 Uiso 0.65 1 calc PR . . H27C H 0.1661 0.6051 0.4766 0.085 Uiso 0.65 1 calc PR . . C28 C 0.5377(17) 0.2320(9) 0.4544(11) 0.072(3) Uani 0.65 1 d PDU . . H28A H 0.4671 0.2165 0.4043 0.107 Uiso 0.65 1 calc PR . . H28B H 0.5922 0.2785 0.4303 0.107 Uiso 0.65 1 calc PR . . H28C H 0.4899 0.2466 0.5163 0.107 Uiso 0.65 1 calc PR . . C29 C 0.6254(13) 0.1695(7) 0.4712(10) 0.065(2) Uani 0.65 1 d PDU . . C30 C 0.7054(13) 0.1304(8) 0.4001(9) 0.057(3) Uani 0.65 1 d PDU . . H30A H 0.7947 0.1121 0.4299 0.086 Uiso 0.65 1 calc PR . . H30B H 0.7253 0.1678 0.3454 0.086 Uiso 0.65 1 calc PR . . H30C H 0.6529 0.0834 0.3747 0.086 Uiso 0.65 1 calc PR . . 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 0.0133(2) 0.0214(3) 0.0224(3) -0.0004(3) -0.0008(4) -0.0007(3) S1 0.0162(5) 0.0432(9) 0.0357(7) -0.0048(8) 0.0002(7) 0.0005(6) P1 0.0241(7) 0.0249(6) 0.0281(8) -0.0006(5) 0.0025(6) -0.0059(5) P2 0.0228(7) 0.0236(6) 0.0377(9) 0.0028(5) -0.0067(7) 0.0030(7) P3 0.0191(7) 0.0192(6) 0.0240(8) -0.0028(6) -0.0021(6) 0.0005(6) P4 0.0173(7) 0.0261(6) 0.0233(8) 0.0014(6) 0.0001(6) -0.0014(6) O1 0.024(2) 0.040(2) 0.026(2) -0.0032(18) -0.0074(18) -0.0005(15) O2 0.019(2) 0.037(2) 0.032(3) -0.004(2) 0.0080(17) 0.0032(17) O3 0.030(2) 0.069(3) 0.046(3) -0.003(3) 0.000(2) -0.009(2) O4 0.0189(19) 0.062(3) 0.049(3) -0.003(2) -0.0081(19) 0.0133(19) O5 0.049(3) 0.055(3) 0.028(3) 0.009(2) 0.008(2) -0.003(2) O6 0.072(4) 0.099(5) 0.055(4) 0.038(4) 0.011(3) -0.018(4) O7 0.066(3) 0.031(2) 0.053(3) -0.018(2) -0.006(2) -0.015(2) O8 0.102(5) 0.052(3) 0.060(4) -0.011(3) -0.025(4) -0.031(3) O9 0.040(3) 0.041(3) 0.043(3) -0.013(2) -0.004(2) 0.005(2) O10 0.147(7) 0.101(5) 0.034(4) -0.018(4) -0.023(4) 0.043(5) O11 0.036(2) 0.048(3) 0.028(3) -0.017(2) 0.004(2) -0.008(2) O12 0.119(6) 0.081(4) 0.056(5) -0.022(4) 0.030(5) -0.020(5) O13 0.042(3) 0.073(3) 0.037(3) 0.008(2) -0.002(2) 0.016(2) O14 0.066(4) 0.071(4) 0.063(4) 0.032(3) -0.008(3) 0.019(3) O15 0.065(3) 0.029(2) 0.094(5) -0.002(3) 0.002(3) 0.006(2) O16 0.092(5) 0.051(3) 0.072(5) -0.016(3) 0.019(4) 0.016(3) O17 0.061(4) 0.118(6) 0.076(5) 0.023(5) 0.006(4) -0.035(5) O18 0.099(5) 0.092(5) 0.079(5) -0.011(5) 0.018(5) -0.016(5) N1 0.029(2) 0.020(2) 0.040(3) 0.002(2) 0.003(2) 0.0080(19) N2 0.020(2) 0.030(2) 0.037(3) 0.002(2) -0.002(2) -0.0080(19) C1 0.035(3) 0.019(3) 0.046(4) 0.004(3) 0.003(3) 0.000(2) C2 0.021(3) 0.030(3) 0.026(3) 0.004(2) -0.006(2) 0.012(2) C3 0.019(3) 0.027(3) 0.044(4) -0.008(3) 0.002(3) 0.014(2) C4 0.025(3) 0.022(3) 0.062(5) 0.014(3) 0.001(3) -0.008(2) C5 0.022(3) 0.027(3) 0.039(4) 0.004(3) -0.007(3) -0.008(2) C6 0.027(3) 0.037(3) 0.040(4) 0.004(3) 0.007(3) -0.010(2) C7 0.036(3) 0.046(3) 0.028(3) 0.010(3) 0.008(3) -0.018(3) C8 0.036(4) 0.092(6) 0.039(5) 0.018(4) 0.003(3) 0.000(4) C9 0.070(6) 0.157(11) 0.034(5) 0.001(6) -0.001(5) 0.002(7) C10 0.043(4) 0.040(3) 0.035(4) -0.012(3) -0.008(3) -0.020(3) C11 0.067(5) 0.035(4) 0.067(6) -0.016(4) 0.021(5) -0.021(4) C12 0.095(7) 0.035(4) 0.079(6) -0.011(4) -0.001(6) -0.007(4) C13 0.042(3) 0.036(3) 0.015(3) -0.011(3) -0.005(3) 0.005(3) C14 0.046(4) 0.062(5) 0.029(4) -0.017(4) -0.009(3) -0.012(3) C15 0.043(4) 0.046(4) 0.074(6) -0.034(4) -0.003(4) -0.002(3) C16 0.030(3) 0.043(3) 0.030(4) 0.001(3) 0.001(3) -0.001(3) C17 0.040(4) 0.055(4) 0.039(5) -0.008(4) -0.016(4) 0.002(3) C18 0.065(5) 0.063(4) 0.034(4) -0.017(3) -0.007(4) -0.009(4) C19 0.038(3) 0.036(3) 0.038(4) 0.004(3) 0.002(3) 0.011(3) C20 0.060(5) 0.076(6) 0.040(5) 0.021(4) -0.008(4) -0.009(4) C21 0.073(7) 0.27(2) 0.032(6) 0.025(8) -0.010(6) 0.025(10) C22 0.040(3) 0.034(3) 0.047(4) 0.002(3) -0.005(3) 0.014(3) C23 0.080(6) 0.036(4) 0.086(7) -0.021(4) -0.014(6) 0.021(4) C24 0.126(9) 0.025(3) 0.116(9) -0.003(4) 0.029(7) -0.002(4) C25 0.068(5) 0.120(7) 0.066(6) -0.001(6) 0.021(5) -0.029(6) C26 0.047(4) 0.105(6) 0.059(5) -0.005(4) 0.019(4) -0.024(4) C27 0.035(4) 0.074(6) 0.061(6) -0.025(5) 0.011(4) -0.009(4) C28 0.078(6) 0.088(6) 0.049(6) -0.010(5) -0.007(5) 0.008(5) C29 0.067(5) 0.074(5) 0.054(5) -0.008(4) 0.005(4) -0.005(4) C30 0.054(5) 0.071(6) 0.046(5) 0.004(5) 0.014(5) -0.002(5) _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 O2 2.046(4) . ? Fe1 O1 2.047(4) . ? Fe1 P4 2.1776(17) . ? Fe1 P3 2.1803(17) . ? Fe1 P1 2.2256(16) . ? Fe1 P2 2.2362(16) . ? Fe1 S1 2.6460(13) . ? S1 O4 1.451(5) . ? S1 O3 1.463(5) . ? S1 O1 1.513(5) . ? S1 O2 1.523(5) . ? P1 C1 1.839(6) . ? P1 C7 1.840(6) . ? P1 C10 1.858(6) . ? P2 C22 1.817(7) . ? P2 C19 1.850(7) . ? P2 C4 1.872(6) . ? P3 C13 1.836(6) . ? P3 C5 1.867(6) . ? P3 C2 1.885(5) . ? P4 C16 1.842(7) . ? P4 C6 1.871(6) . ? P4 C3 1.892(6) . ? O5 C8 1.327(9) . ? O5 C7 1.462(9) . ? O6 C8 1.223(11) . ? O7 C11 1.429(9) . ? O7 C10 1.445(8) . ? O8 C11 1.182(11) . ? O9 C14 1.341(9) . ? O9 C13 1.465(7) . ? O10 C14 1.211(10) . ? O11 C17 1.342(9) . ? O11 C16 1.408(8) . ? O12 C17 1.181(11) . ? O13 C20 1.376(10) . ? O13 C19 1.423(9) . ? O14 C20 1.180(11) . ? O15 C23 1.371(10) . ? O15 C22 1.456(8) . ? O16 C23 1.167(12) . ? O17 C26 1.182(16) . ? O18 C29 1.212(16) . ? N1 C2 1.441(8) . ? N1 C3 1.443(9) . ? N1 C1 1.471(8) . ? N2 C4 1.452(8) . ? N2 C6 1.452(9) . ? N2 C5 1.461(9) . ? C8 C9 1.519(13) . ? C11 C12 1.485(12) . ? C14 C15 1.445(11) . ? C17 C18 1.477(11) . ? C20 C21 1.462(15) . ? C23 C24 1.529(12) . ? C25 C26 1.369(14) . ? C26 C27 1.374(13) . ? C28 C29 1.341(13) . ? C29 C30 1.381(13) . ? 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 O2 Fe1 O1 69.74(15) . . ? O2 Fe1 P4 175.33(14) . . ? O1 Fe1 P4 105.59(14) . . ? O2 Fe1 P3 104.35(14) . . ? O1 Fe1 P3 174.07(15) . . ? P4 Fe1 P3 80.32(5) . . ? O2 Fe1 P1 88.41(13) . . ? O1 Fe1 P1 86.93(13) . . ? P4 Fe1 P1 91.58(6) . . ? P3 Fe1 P1 92.52(6) . . ? O2 Fe1 P2 87.64(13) . . ? O1 Fe1 P2 88.16(13) . . ? P4 Fe1 P2 92.04(7) . . ? P3 Fe1 P2 92.12(6) . . ? P1 Fe1 P2 174.54(6) . . ? O2 Fe1 S1 35.00(14) . . ? O1 Fe1 S1 34.74(15) . . ? P4 Fe1 S1 140.32(8) . . ? P3 Fe1 S1 139.35(8) . . ? P1 Fe1 S1 87.76(6) . . ? P2 Fe1 S1 86.85(6) . . ? O4 S1 O3 111.3(3) . . ? O4 S1 O1 111.1(3) . . ? O3 S1 O1 110.2(3) . . ? O4 S1 O2 111.5(3) . . ? O3 S1 O2 111.4(3) . . ? O1 S1 O2 100.87(19) . . ? O4 S1 Fe1 123.74(19) . . ? O3 S1 Fe1 124.9(2) . . ? O1 S1 Fe1 50.44(17) . . ? O2 S1 Fe1 50.44(16) . . ? C1 P1 C7 103.7(3) . . ? C1 P1 C10 105.8(3) . . ? C7 P1 C10 97.0(3) . . ? C1 P1 Fe1 116.13(19) . . ? C7 P1 Fe1 120.7(2) . . ? C10 P1 Fe1 111.0(2) . . ? C22 P2 C19 97.4(3) . . ? C22 P2 C4 103.3(3) . . ? C19 P2 C4 103.8(3) . . ? C22 P2 Fe1 114.3(2) . . ? C19 P2 Fe1 118.9(2) . . ? C4 P2 Fe1 116.42(19) . . ? C13 P3 C5 102.7(3) . . ? C13 P3 C2 98.4(3) . . ? C5 P3 C2 102.7(3) . . ? C13 P3 Fe1 122.0(2) . . ? C5 P3 Fe1 114.4(2) . . ? C2 P3 Fe1 113.94(19) . . ? C16 P4 C6 99.5(3) . . ? C16 P4 C3 100.8(3) . . ? C6 P4 C3 101.3(3) . . ? C16 P4 Fe1 123.7(2) . . ? C6 P4 Fe1 114.2(2) . . ? C3 P4 Fe1 114.0(2) . . ? S1 O1 Fe1 94.8(2) . . ? S1 O2 Fe1 94.6(2) . . ? C8 O5 C7 114.0(6) . . ? C11 O7 C10 113.1(6) . . ? C14 O9 C13 118.3(6) . . ? C17 O11 C16 117.3(6) . . ? C20 O13 C19 112.9(6) . . ? C23 O15 C22 114.9(7) . . ? C2 N1 C3 115.0(5) . . ? C2 N1 C1 113.8(5) . . ? C3 N1 C1 112.1(6) . . ? C4 N2 C6 115.3(6) . . ? C4 N2 C5 116.2(6) . . ? C6 N2 C5 112.6(5) . . ? N1 C1 P1 114.8(4) . . ? N1 C2 P3 115.9(4) . . ? N1 C3 P4 116.1(4) . . ? N2 C4 P2 112.0(4) . . ? N2 C5 P3 115.3(4) . . ? N2 C6 P4 115.5(4) . . ? O5 C7 P1 109.0(4) . . ? O6 C8 O5 121.6(8) . . ? O6 C8 C9 126.5(9) . . ? O5 C8 C9 111.9(8) . . ? O7 C10 P1 105.4(4) . . ? O8 C11 O7 122.6(7) . . ? O8 C11 C12 131.8(8) . . ? O7 C11 C12 105.6(8) . . ? O9 C13 P3 108.9(4) . . ? O10 C14 O9 118.6(8) . . ? O10 C14 C15 128.6(7) . . ? O9 C14 C15 112.8(7) . . ? O11 C16 P4 110.9(5) . . ? O12 C17 O11 123.0(7) . . ? O12 C17 C18 124.5(8) . . ? O11 C17 C18 112.4(7) . . ? O13 C19 P2 109.2(4) . . ? O14 C20 O13 123.7(9) . . ? O14 C20 C21 125.2(9) . . ? O13 C20 C21 110.9(8) . . ? O15 C22 P2 107.4(5) . . ? O16 C23 O15 124.0(8) . . ? O16 C23 C24 128.0(8) . . ? O15 C23 C24 108.0(9) . . ? O17 C26 C25 127.4(13) . . ? O17 C26 C27 120.7(13) . . ? C25 C26 C27 111.7(12) . . ? O18 C29 C28 111.4(13) . . ? O18 C29 C30 122.5(13) . . ? C28 C29 C30 125.6(14) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.610 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.100