Electronic Supplementary Material for CrystEngComm This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Prof. G.De Munno' _publ_contact_author_address ; Prof. G. De Munno Dipartimento di Chimica Universita degli Studi della Calabria I-87030 Arcavacata di Rende, Cosenza Italy ; _publ_contact_author_phone +390984492068 _publ_contact_author_fax +390984493309 _publ_contact_author_email demunno@unical.it _publ_section_title ; Bis- and Tris-(oxalato)ferrate(III) Complexes as Precursors of Polynuclear Compounds ; loop_ _publ_author_name _publ_author_address 'Donatella Armentano' ; Dipartimento di Chimica Universita degli Studi della Calabria I-87030 Arcavacata di Rende, Cosenza Italy ; 'G.De Munno' ; Dipartimento di Chimica Universita degli Studi della Calabria I-87030 Arcavacata di Rende, Cosenza Italy ; 'Francesc Lloret' ; Departament de Quimica Inorganica/Instituto de Ciencia Molecular Facultat de Quimica, Dr. Moliner 50 46100 Burjassot, Valencia Spain ; 'Miguel Julve' ; Departament de Quimica Inorganica/Instituto de Ciencia Molecular Facultat de Quimica, Dr. Moliner 50 46100 Burjassot, Valencia Spain ; data_1 _database_code_depnum_ccdc_archive 'CCDC 255482' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H10 Fe Na3 O17' _chemical_formula_weight 478.96 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' H H 0.0000 0.0000 '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 17.404(4) _cell_length_b 12.702(3) _cell_length_c 15.220(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.46(2) _cell_angle_gamma 90.00 _cell_volume 3308.7(15) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 15 _cell_measurement_theta_max 30 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.923 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 1.080 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'R3m/V automatic four-circle diffractometer' _diffrn_measurement_method omega/2-theta-scans _diffrn_standards_decay_% 2.9 _diffrn_reflns_number 3944 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -2 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.05 _reflns_number_total 3629 _reflns_number_gt 2988 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (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^)+(0.0772P)^2^+12.8908P] 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 3629 _refine_ls_number_parameters 275 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1534 _refine_ls_wR_factor_gt 0.1434 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.095 _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 0.19164(3) 0.13442(4) 0.73278(4) 0.02342(17) Uani 1 1 d . . . O1 O 0.26811(15) 0.1034(2) 0.65219(18) 0.0317(6) Uani 1 1 d . . . O2 O 0.29220(15) 0.1715(2) 0.81618(18) 0.0303(6) Uani 1 1 d . . . C1 C 0.3406(2) 0.1176(3) 0.6873(3) 0.0264(8) Uani 1 1 d . . . C2 C 0.3548(2) 0.1522(3) 0.7863(3) 0.0251(8) Uani 1 1 d . . . O3 O 0.39657(16) 0.1080(3) 0.6487(2) 0.0379(7) Uani 1 1 d . . . O4 O 0.42193(16) 0.1598(2) 0.82757(19) 0.0328(6) Uani 1 1 d . . . Na1 Na 0.5000 0.00220(18) 0.7500 0.0377(6) Uani 1 2 d S . . O5 O 0.10322(16) 0.0578(2) 0.65358(18) 0.0304(6) Uani 1 1 d . . . O6 O 0.19392(16) -0.0017(2) 0.80016(19) 0.0324(6) Uani 1 1 d . . . C3 C 0.1399(2) -0.0677(3) 0.7699(2) 0.0258(7) Uani 1 1 d . . . C4 C 0.0851(2) -0.0325(3) 0.6825(2) 0.0263(8) Uani 1 1 d . . . O7 O 0.03159(17) -0.0895(2) 0.6488(2) 0.0382(7) Uani 1 1 d . . . O8 O 0.12823(17) -0.1525(2) 0.8042(2) 0.0340(7) Uani 1 1 d . . . Na2 Na 0.0000 -0.22967(17) 0.7500 0.0327(5) Uani 1 2 d S . . O9 O 0.12927(17) 0.1995(2) 0.81847(19) 0.0338(6) Uani 1 1 d . . . O10 O 0.16442(17) 0.2714(2) 0.67124(18) 0.0318(6) Uani 1 1 d . . . C5 C 0.1045(2) 0.2932(3) 0.7989(3) 0.0315(8) Uani 1 1 d . . . C6 C 0.1251(2) 0.3364(3) 0.7111(3) 0.0279(8) Uani 1 1 d . . . O11 O 0.0671(2) 0.3478(3) 0.8427(2) 0.0516(9) Uani 1 1 d . . . O12 O 0.10352(18) 0.4237(2) 0.6831(2) 0.0414(7) Uani 1 1 d . . . Na3 Na 0.04287(11) 0.11190(16) 0.50017(13) 0.0451(5) Uani 1 1 d . . . Na4 Na 0.12115(15) 0.36955(19) 0.51643(15) 0.0621(6) Uani 1 1 d . . . O13 O -0.0032(2) 0.2943(3) 0.5040(2) 0.0543(9) Uani 1 1 d D . . H1W H -0.040(2) 0.314(5) 0.4506(18) 0.060 Uiso 1 1 d D . . H2W H -0.035(2) 0.315(5) 0.547(2) 0.060 Uiso 1 1 d D . . O14 O -0.0831(2) 0.0651(3) 0.5364(2) 0.0498(8) Uani 1 1 d D . . H3W H -0.129(2) 0.088(4) 0.497(3) 0.060 Uiso 1 1 d D . . H4W H -0.087(3) 0.099(4) 0.5916(18) 0.060 Uiso 1 1 d D . . O15 O 0.1647(2) 0.1940(3) 0.4843(2) 0.0518(9) Uani 1 1 d D . . H5W H 0.2158(15) 0.174(5) 0.516(3) 0.060 Uiso 1 1 d D . . H6W H 0.171(3) 0.174(5) 0.4253(14) 0.060 Uiso 1 1 d D . . O16 O 0.2028(4) 0.5053(6) 0.5253(3) 0.117(3) Uani 1 1 d D . . H7W H 0.237(2) 0.518(5) 0.5812(16) 0.060 Uiso 1 1 d D . . H8W H 0.238(2) 0.503(5) 0.484(2) 0.060 Uiso 1 1 d D . . O17 O 0.2863(4) 0.6567(8) 0.4310(7) 0.196(5) Uani 1 1 d D . . H9W H 0.2370(18) 0.621(4) 0.423(3) 0.060 Uiso 1 1 d D . . H10W H 0.290(3) 0.666(5) 0.3696(13) 0.060 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 0.0195(3) 0.0222(3) 0.0294(3) -0.0003(2) 0.0068(2) -0.0017(2) O1 0.0229(13) 0.0420(16) 0.0310(14) -0.0096(12) 0.0068(11) -0.0015(12) O2 0.0247(13) 0.0355(15) 0.0315(14) -0.0073(12) 0.0073(11) -0.0053(12) C1 0.0208(17) 0.0246(18) 0.035(2) 0.0008(15) 0.0077(15) 0.0001(14) C2 0.0234(18) 0.0218(17) 0.0316(19) 0.0051(14) 0.0086(15) -0.0044(14) O3 0.0272(14) 0.0496(18) 0.0400(16) 0.0006(14) 0.0150(12) 0.0030(13) O4 0.0239(13) 0.0355(15) 0.0370(15) 0.0023(12) 0.0001(11) -0.0047(11) Na1 0.0267(11) 0.0270(11) 0.0612(16) 0.000 0.0124(11) 0.000 O5 0.0285(14) 0.0285(14) 0.0328(14) 0.0068(12) 0.0018(11) -0.0059(11) O6 0.0302(14) 0.0264(14) 0.0374(15) 0.0046(12) -0.0026(12) -0.0045(11) C3 0.0251(17) 0.0241(18) 0.0295(18) -0.0001(15) 0.0081(15) 0.0020(15) C4 0.0240(18) 0.0293(19) 0.0257(18) 0.0002(15) 0.0050(14) -0.0026(15) O7 0.0358(16) 0.0388(17) 0.0371(16) 0.0040(13) -0.0011(12) -0.0149(13) O8 0.0354(15) 0.0267(14) 0.0378(16) 0.0077(12) 0.0015(12) -0.0032(12) Na2 0.0276(11) 0.0254(11) 0.0487(13) 0.000 0.0163(10) 0.000 O9 0.0344(15) 0.0337(15) 0.0374(15) 0.0063(12) 0.0172(12) 0.0076(12) O10 0.0381(15) 0.0266(14) 0.0349(15) 0.0030(11) 0.0174(12) 0.0024(12) C5 0.031(2) 0.033(2) 0.033(2) 0.0013(17) 0.0119(16) 0.0056(17) C6 0.0254(18) 0.0287(19) 0.0302(19) 0.0016(15) 0.0067(15) -0.0021(15) O11 0.061(2) 0.049(2) 0.054(2) 0.0066(16) 0.0338(17) 0.0234(17) O12 0.0434(18) 0.0286(15) 0.0567(19) 0.0106(14) 0.0209(15) 0.0086(13) Na3 0.0402(10) 0.0479(11) 0.0452(10) 0.0053(8) 0.0025(8) -0.0039(8) Na4 0.0738(15) 0.0656(14) 0.0498(12) -0.0032(10) 0.0194(11) -0.0255(12) O13 0.051(2) 0.069(2) 0.0427(19) 0.0008(18) 0.0089(15) 0.0042(18) O14 0.0426(19) 0.060(2) 0.048(2) -0.0019(17) 0.0105(15) 0.0053(16) O15 0.048(2) 0.066(2) 0.0406(18) -0.0046(17) 0.0060(15) -0.0060(18) O16 0.145(5) 0.158(6) 0.056(3) -0.038(3) 0.037(3) -0.104(5) O17 0.070(4) 0.255(10) 0.264(10) 0.221(9) 0.036(5) 0.025(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 O10 1.992(3) . ? Fe1 O1 2.006(3) . ? Fe1 O6 2.006(3) . ? Fe1 O9 2.019(3) . ? Fe1 O2 2.022(3) . ? Fe1 O5 2.024(3) . ? O1 C1 1.289(5) . ? O2 C2 1.278(4) . ? C1 O3 1.232(5) . ? C1 C2 1.547(5) . ? C2 O4 1.225(5) . ? C2 Na2 3.073(4) 3 ? O3 Na4 2.493(4) 7_556 ? O3 Na1 2.533(3) . ? O3 Na2 2.977(4) 3 ? O4 Na2 2.407(3) 3 ? O4 Na1 2.798(3) . ? Na1 O12 2.437(3) 3_545 ? Na1 O12 2.437(3) 4_546 ? Na1 O3 2.533(3) 2_656 ? Na1 O11 2.569(4) 4_546 ? Na1 O11 2.569(4) 3_545 ? Na1 O4 2.798(3) 2_656 ? Na1 Na2 3.406(3) 3 ? O5 C4 1.288(5) . ? O5 Na3 2.477(3) . ? O6 C3 1.282(5) . ? C3 O8 1.230(5) . ? C3 C4 1.555(5) . ? C4 O7 1.216(5) . ? O7 Na3 2.415(4) 5_556 ? O7 Na2 2.481(3) . ? O8 Na2 2.440(3) . ? Na2 O4 2.407(3) 3_445 ? Na2 O4 2.407(3) 4_546 ? Na2 O8 2.440(3) 2_556 ? Na2 O7 2.481(3) 2_556 ? Na2 O3 2.977(4) 3_445 ? Na2 O3 2.977(4) 4_546 ? O9 C5 1.283(5) . ? O10 C6 1.292(5) . ? O10 Na4 2.651(4) . ? C5 O11 1.227(5) . ? C5 C6 1.545(5) . ? C6 O12 1.223(5) . ? O11 Na1 2.569(4) 3_455 ? O12 Na1 2.437(3) 3_455 ? O12 Na4 2.700(4) . ? Na3 O15 2.413(4) . ? Na3 O7 2.415(4) 5_556 ? Na3 O14 2.429(4) . ? Na3 O14 2.448(4) 5_556 ? Na3 O13 2.456(5) . ? Na4 O16 2.223(5) . ? Na4 O13 2.342(5) . ? Na4 O15 2.433(5) . ? Na4 O3 2.493(4) 7_556 ? O14 Na3 2.448(4) 5_556 ? 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 O10 Fe1 O1 90.66(12) . . ? O10 Fe1 O6 166.83(12) . . ? O1 Fe1 O6 100.94(13) . . ? O10 Fe1 O9 80.57(11) . . ? O1 Fe1 O9 165.82(12) . . ? O6 Fe1 O9 89.17(12) . . ? O10 Fe1 O2 101.33(12) . . ? O1 Fe1 O2 80.49(11) . . ? O6 Fe1 O2 86.86(12) . . ? O9 Fe1 O2 90.27(12) . . ? O10 Fe1 O5 92.87(12) . . ? O1 Fe1 O5 93.36(12) . . ? O6 Fe1 O5 80.35(11) . . ? O9 Fe1 O5 98.16(12) . . ? O2 Fe1 O5 164.53(12) . . ? C1 O1 Fe1 115.3(2) . . ? C2 O2 Fe1 115.4(2) . . ? O3 C1 O1 126.0(4) . . ? O3 C1 C2 119.5(3) . . ? O1 C1 C2 114.6(3) . . ? O4 C2 O2 126.7(4) . . ? O4 C2 C1 119.4(3) . . ? O2 C2 C1 113.8(3) . . ? C1 O3 Na4 120.4(3) . 7_556 ? C1 O3 Na1 107.4(3) . . ? Na4 O3 Na1 128.21(13) 7_556 . ? C1 O3 Na2 98.1(3) . 3 ? Na4 O3 Na2 113.30(12) 7_556 3 ? Na1 O3 Na2 75.89(10) . 3 ? C2 O4 Na2 111.4(2) . 3 ? C2 O4 Na1 102.6(2) . . ? Na2 O4 Na1 81.36(10) 3 . ? O12 Na1 O12 131.72(17) 3_545 4_546 ? O12 Na1 O3 88.49(11) 3_545 2_656 ? O12 Na1 O3 117.41(10) 4_546 2_656 ? O12 Na1 O3 117.41(10) 3_545 . ? O12 Na1 O3 88.49(11) 4_546 . ? O3 Na1 O3 115.90(17) 2_656 . ? O12 Na1 O11 75.85(12) 3_545 4_546 ? O12 Na1 O11 67.69(11) 4_546 4_546 ? O3 Na1 O11 160.26(14) 2_656 4_546 ? O3 Na1 O11 82.45(12) . 4_546 ? O12 Na1 O11 67.69(11) 3_545 3_545 ? O12 Na1 O11 75.85(12) 4_546 3_545 ? O3 Na1 O11 82.45(12) 2_656 3_545 ? O3 Na1 O11 160.26(14) . 3_545 ? O11 Na1 O11 80.5(2) 4_546 3_545 ? O12 Na1 O4 70.37(9) 3_545 2_656 ? O12 Na1 O4 157.08(12) 4_546 2_656 ? O3 Na1 O4 62.05(10) 2_656 2_656 ? O3 Na1 O4 73.11(10) . 2_656 ? O11 Na1 O4 121.43(10) 4_546 2_656 ? O11 Na1 O4 124.78(10) 3_545 2_656 ? O12 Na1 O4 157.08(12) 3_545 . ? O12 Na1 O4 70.37(9) 4_546 . ? O3 Na1 O4 73.11(10) 2_656 . ? O3 Na1 O4 62.05(10) . . ? O11 Na1 O4 124.78(10) 4_546 . ? O11 Na1 O4 121.43(10) 3_545 . ? O4 Na1 O4 88.64(14) 2_656 . ? C4 O5 Fe1 115.6(2) . . ? C4 O5 Na3 118.7(2) . . ? Fe1 O5 Na3 125.05(13) . . ? C3 O6 Fe1 115.8(2) . . ? O8 C3 O6 126.0(4) . . ? O8 C3 C4 119.5(3) . . ? O6 C3 C4 114.5(3) . . ? O7 C4 O5 127.0(4) . . ? O7 C4 C3 119.6(3) . . ? O5 C4 C3 113.4(3) . . ? C4 O7 Na3 134.9(3) . 5_556 ? C4 O7 Na2 113.8(3) . . ? Na3 O7 Na2 110.89(12) 5_556 . ? C3 O8 Na2 114.8(3) . . ? O4 Na2 O4 108.65(17) 3_445 4_546 ? O4 Na2 O8 129.17(10) 3_445 . ? O4 Na2 O8 80.61(10) 4_546 . ? O4 Na2 O8 80.61(10) 3_445 2_556 ? O4 Na2 O8 129.17(10) 4_546 2_556 ? O8 Na2 O8 132.65(16) . 2_556 ? O4 Na2 O7 84.57(11) 3_445 2_556 ? O4 Na2 O7 158.71(10) 4_546 2_556 ? O8 Na2 O7 78.11(11) . 2_556 ? O8 Na2 O7 68.25(10) 2_556 2_556 ? O4 Na2 O7 158.71(10) 3_445 . ? O4 Na2 O7 84.57(11) 4_546 . ? O8 Na2 O7 68.25(10) . . ? O8 Na2 O7 78.11(11) 2_556 . ? O7 Na2 O7 88.26(17) 2_556 . ? O4 Na2 O3 60.52(10) 3_445 3_445 ? O4 Na2 O3 71.59(10) 4_546 3_445 ? O8 Na2 O3 152.04(11) . 3_445 ? O8 Na2 O3 70.91(9) 2_556 3_445 ? O7 Na2 O3 129.60(9) 2_556 3_445 ? O7 Na2 O3 110.91(9) . 3_445 ? O4 Na2 O3 71.59(10) 3_445 4_546 ? O4 Na2 O3 60.52(10) 4_546 4_546 ? O8 Na2 O3 70.91(9) . 4_546 ? O8 Na2 O3 152.04(11) 2_556 4_546 ? O7 Na2 O3 110.91(9) 2_556 4_546 ? O7 Na2 O3 129.60(9) . 4_546 ? O3 Na2 O3 92.32(14) 3_445 4_546 ? C5 O9 Fe1 115.3(2) . . ? C6 O10 Fe1 116.0(2) . . ? C6 O10 Na4 91.6(2) . . ? Fe1 O10 Na4 146.45(14) . . ? O11 C5 O9 126.0(4) . . ? O11 C5 C6 119.9(4) . . ? O9 C5 C6 114.2(3) . . ? O12 C6 O10 124.8(4) . . ? O12 C6 C5 121.2(4) . . ? O10 C6 C5 113.9(3) . . ? C5 O11 Na1 111.5(3) . 3_455 ? C6 O12 Na1 115.4(3) . 3_455 ? C6 O12 Na4 90.9(3) . . ? Na1 O12 Na4 135.68(15) 3_455 . ? O15 Na3 O7 106.76(13) . 5_556 ? O15 Na3 O14 166.81(16) . . ? O7 Na3 O14 80.31(13) 5_556 . ? O15 Na3 O14 94.67(14) . 5_556 ? O7 Na3 O14 78.76(13) 5_556 5_556 ? O14 Na3 O14 97.68(13) . 5_556 ? O15 Na3 O13 83.76(14) . . ? O7 Na3 O13 90.66(13) 5_556 . ? O14 Na3 O13 85.05(14) . . ? O14 Na3 O13 168.40(15) 5_556 . ? O15 Na3 O5 89.11(12) . . ? O7 Na3 O5 156.26(13) 5_556 . ? O14 Na3 O5 87.92(12) . . ? O14 Na3 O5 82.51(12) 5_556 . ? O13 Na3 O5 108.91(13) . . ? O16 Na4 O13 153.2(3) . . ? O16 Na4 O15 120.3(3) . . ? O13 Na4 O15 85.78(15) . . ? O16 Na4 O3 86.17(17) . 7_556 ? O13 Na4 O3 91.24(14) . 7_556 ? O15 Na4 O3 83.57(13) . 7_556 ? O16 Na4 O10 103.6(2) . . ? O13 Na4 O10 89.39(13) . . ? O15 Na4 O10 72.50(13) . . ? O3 Na4 O10 155.96(15) 7_556 . ? O16 Na4 O12 85.74(16) . . ? O13 Na4 O12 85.36(14) . . ? O15 Na4 O12 121.01(14) . . ? O3 Na4 O12 154.72(15) 7_556 . ? O10 Na4 O12 49.22(9) . . ? Na4 O13 Na3 94.93(16) . . ? Na3 O14 Na3 82.32(13) . 5_556 ? Na3 O15 Na4 93.71(15) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O13 H1W O4 0.966(10) 1.901(19) 2.824(5) 159(4) 8_455 O13 H2W O11 0.969(10) 1.907(17) 2.844(5) 162(4) 2_556 O14 H3W O17 0.954(10) 1.844(16) 2.788(7) 170(5) 3_445 O14 H4W O9 0.954(10) 2.11(2) 3.014(5) 159(4) 2_556 O15 H6W O8 0.961(10) 1.88(3) 2.750(5) 149(4) 6 O16 H7W O6 0.959(10) 2.00(2) 2.926(7) 163(5) 4_556 O16 H8W O17 0.953(10) 2.33(5) 2.937(8) 121(4) . O17 H9W O16 0.957(10) 2.30(4) 2.937(8) 123(4) . O17 H10W O2 0.956(10) 2.22(5) 2.809(6) 119(5) 6_565 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.821 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.105 #==END data_2 _database_code_depnum_ccdc_archive 'CCDC 255483' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H45 As2 Fe O12.50' _chemical_formula_weight 1087.58 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.231(3) _cell_length_b 13.395(3) _cell_length_c 15.823(3) _cell_angle_alpha 85.60(3) _cell_angle_beta 86.42(3) _cell_angle_gamma 62.85(3) _cell_volume 2486.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 15 _cell_measurement_theta_max 30 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1110 _exptl_absorpt_coefficient_mu 1.687 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.5174 _exptl_absorpt_correction_T_max 0.8232 _exptl_absorpt_process_details psi-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'R3m/V automatic four-circle diffractometer' _diffrn_measurement_method omega/2-theta-scans _diffrn_standards_decay_% 1.2 _diffrn_reflns_number 8403 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 24.05 _reflns_number_total 7844 _reflns_number_gt 5756 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (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^)+(0.0887P)^2^+0.5128P] 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 7844 _refine_ls_number_parameters 629 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1378 _refine_ls_wR_factor_gt 0.1213 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _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 0.93645(5) 0.93528(5) 0.15406(4) 0.04532(19) Uani 1 1 d . . . O1 O 0.8066(3) 0.9210(3) 0.1100(2) 0.0607(9) Uani 1 1 d . . . O2 O 0.9725(3) 0.7826(3) 0.2023(2) 0.0564(8) Uani 1 1 d . . . C1 C 1.0304(6) 0.9809(5) 0.2873(4) 0.0764(17) Uani 1 1 d . . . C2 C 0.9012(6) 1.0409(4) 0.3049(4) 0.0750(17) Uani 1 1 d . . . O3 O 0.8607(5) 1.0933(4) 0.3682(3) 0.1194(18) Uani 1 1 d . . . O4 O 1.0972(5) 0.9752(5) 0.3409(3) 0.1255(19) Uani 1 1 d . . . C3 C 0.9000(5) 0.7459(4) 0.1889(3) 0.0569(13) Uani 1 1 d . . . C4 C 0.8001(5) 0.8306(5) 0.1374(4) 0.0627(14) Uani 1 1 d . . . O5 O 0.8444(3) 1.0285(3) 0.2470(2) 0.0615(9) Uani 1 1 d . . . O6 O 1.0593(3) 0.9380(3) 0.2154(2) 0.0732(10) Uani 1 1 d . . . O7 O 0.7194(4) 0.8121(4) 0.1245(4) 0.1034(16) Uani 1 1 d . . . O8 O 0.9097(4) 0.6542(3) 0.2126(3) 0.0826(12) Uani 1 1 d . . . O9 O 0.8976(3) 1.0790(2) 0.07393(19) 0.0523(8) Uani 1 1 d . . . O10 O 1.0497(3) 0.8683(2) 0.05171(19) 0.0504(8) Uani 1 1 d . . . C5 C 0.9560(4) 1.0604(3) 0.0066(3) 0.0428(10) Uani 1 1 d . . . As1 As 0.62983(4) 0.49275(4) 0.16373(3) 0.04441(15) Uani 1 1 d . . . C6 C 0.7100(4) 0.4615(4) 0.2666(3) 0.0530(12) Uani 1 1 d . . . C7 C 0.7070(6) 0.3845(5) 0.3273(4) 0.0807(18) Uani 1 1 d . . . H7 H 0.6679 0.3435 0.3188 0.097 Uiso 1 1 calc R . . C8 C 0.7638(7) 0.3685(6) 0.4026(4) 0.101(2) Uani 1 1 d . . . H8 H 0.7616 0.3170 0.4446 0.121 Uiso 1 1 calc R . . C9 C 0.8216(6) 0.4261(6) 0.4151(4) 0.0880(19) Uani 1 1 d . . . H9 H 0.8589 0.4145 0.4656 0.106 Uiso 1 1 calc R . . C10 C 0.8256(6) 0.5013(6) 0.3539(4) 0.0860(19) Uani 1 1 d . . . H10 H 0.8660 0.5409 0.3626 0.103 Uiso 1 1 calc R . . C11 C 0.7707(6) 0.5190(5) 0.2799(4) 0.0801(18) Uani 1 1 d . . . H11 H 0.7743 0.5702 0.2382 0.096 Uiso 1 1 calc R . . C12 C 0.5054(4) 0.6391(4) 0.1669(3) 0.0528(12) Uani 1 1 d . . . C13 C 0.4665(5) 0.6879(5) 0.2434(4) 0.0845(18) Uani 1 1 d . . . H13 H 0.5029 0.6513 0.2932 0.101 Uiso 1 1 calc R . . C14 C 0.3730(6) 0.7915(6) 0.2453(6) 0.105(2) Uani 1 1 d . . . H14 H 0.3465 0.8255 0.2966 0.126 Uiso 1 1 calc R . . C15 C 0.3190(6) 0.8448(5) 0.1724(6) 0.097(2) Uani 1 1 d . . . H15 H 0.2560 0.9149 0.1744 0.116 Uiso 1 1 calc R . . C16 C 0.3561(6) 0.7967(5) 0.0973(5) 0.098(2) Uani 1 1 d . . . H16 H 0.3185 0.8333 0.0479 0.117 Uiso 1 1 calc R . . C17 C 0.4507(5) 0.6924(5) 0.0942(4) 0.0786(17) Uani 1 1 d . . . H17 H 0.4767 0.6589 0.0426 0.094 Uiso 1 1 calc R . . C18 C 0.5748(4) 0.3856(4) 0.1522(3) 0.0449(11) Uani 1 1 d . . . C19 C 0.4584(4) 0.4236(4) 0.1432(3) 0.0504(11) Uani 1 1 d . . . H19 H 0.4080 0.4995 0.1465 0.060 Uiso 1 1 calc R . . C20 C 0.4192(4) 0.3473(4) 0.1293(3) 0.0586(13) Uani 1 1 d . . . H20 H 0.3418 0.3714 0.1237 0.070 Uiso 1 1 calc R . . C21 C 0.4947(5) 0.2351(5) 0.1236(3) 0.0625(14) Uani 1 1 d . . . H21 H 0.4680 0.1844 0.1122 0.075 Uiso 1 1 calc R . . C22 C 0.6101(4) 0.1970(4) 0.1347(3) 0.0607(13) Uani 1 1 d . . . H22 H 0.6601 0.1210 0.1321 0.073 Uiso 1 1 calc R . . C23 C 0.6494(4) 0.2719(4) 0.1495(3) 0.0539(12) Uani 1 1 d . . . H23 H 0.7264 0.2468 0.1578 0.065 Uiso 1 1 calc R . . C24 C 0.7287(4) 0.4899(3) 0.0696(3) 0.0418(10) Uani 1 1 d . . . C25 C 0.7716(4) 0.4040(4) 0.0153(3) 0.0536(12) Uani 1 1 d . . . H25 H 0.7498 0.3469 0.0214 0.064 Uiso 1 1 calc R . . C26 C 0.8483(4) 0.4036(4) -0.0492(3) 0.0610(14) Uani 1 1 d . . . H26 H 0.8772 0.3462 -0.0867 0.073 Uiso 1 1 calc R . . C27 C 0.8814(4) 0.4858(4) -0.0578(3) 0.0604(13) Uani 1 1 d . . . H27 H 0.9335 0.4842 -0.1006 0.072 Uiso 1 1 calc R . . C28 C 0.8378(4) 0.5713(4) -0.0033(3) 0.0599(13) Uani 1 1 d . . . H28 H 0.8606 0.6277 -0.0096 0.072 Uiso 1 1 calc R . . C29 C 0.7608(4) 0.5752(4) 0.0606(3) 0.0512(11) Uani 1 1 d . . . H29 H 0.7309 0.6340 0.0970 0.061 Uiso 1 1 calc R . . As2 As 0.25289(4) 0.22932(5) 0.34767(3) 0.05725(17) Uani 1 1 d . . . C30 C 0.2667(5) 0.3654(5) 0.3425(3) 0.0645(14) Uani 1 1 d . . . C31 C 0.1925(5) 0.4584(5) 0.2961(4) 0.0768(17) Uani 1 1 d . . . H31 H 0.1379 0.4538 0.2646 0.092 Uiso 1 1 calc R . . C32 C 0.1988(6) 0.5585(6) 0.2960(4) 0.095(2) Uani 1 1 d . . . H32 H 0.1479 0.6218 0.2653 0.114 Uiso 1 1 calc R . . C33 C 0.2793(8) 0.5635(7) 0.3409(5) 0.106(2) Uani 1 1 d . . . H33 H 0.2844 0.6306 0.3395 0.127 Uiso 1 1 calc R . . C34 C 0.3536(7) 0.4735(8) 0.3883(5) 0.113(3) Uani 1 1 d . . . H34 H 0.4076 0.4798 0.4193 0.136 Uiso 1 1 calc R . . C35 C 0.3482(6) 0.3724(6) 0.3900(4) 0.0860(19) Uani 1 1 d . . . H35 H 0.3982 0.3103 0.4223 0.103 Uiso 1 1 calc R . . C36 C 0.3984(4) 0.1016(5) 0.3597(3) 0.0642(14) Uani 1 1 d . . . C37 C 0.4060(6) 0.0039(5) 0.3995(4) 0.0862(18) Uani 1 1 d . . . H37 H 0.3416 0.0013 0.4243 0.103 Uiso 1 1 calc R . . C38 C 0.5102(7) -0.0906(7) 0.4026(5) 0.119(3) Uani 1 1 d . . . H38 H 0.5167 -0.1576 0.4291 0.143 Uiso 1 1 calc R . . C39 C 0.6043(7) -0.0840(8) 0.3658(6) 0.128(3) Uani 1 1 d . . . H39 H 0.6740 -0.1480 0.3664 0.153 Uiso 1 1 calc R . . C40 C 0.5979(6) 0.0127(8) 0.3291(5) 0.123(3) Uani 1 1 d . . . H40 H 0.6629 0.0161 0.3064 0.147 Uiso 1 1 calc R . . C41 C 0.4950(5) 0.1055(6) 0.3257(4) 0.095(2) Uani 1 1 d . . . H41 H 0.4899 0.1724 0.3000 0.114 Uiso 1 1 calc R . . C42 C 0.1878(4) 0.2179(4) 0.2465(3) 0.0558(12) Uani 1 1 d . . . C43 C 0.0722(5) 0.2763(6) 0.2371(4) 0.092(2) Uani 1 1 d . . . H43 H 0.0259 0.3203 0.2801 0.110 Uiso 1 1 calc R . . C44 C 0.0246(6) 0.2694(7) 0.1631(4) 0.097(2) Uani 1 1 d . . . H44 H -0.0534 0.3090 0.1562 0.117 Uiso 1 1 calc R . . C45 C 0.0930(6) 0.2045(5) 0.1010(4) 0.0727(16) Uani 1 1 d . . . H45 H 0.0612 0.1989 0.0519 0.087 Uiso 1 1 calc R . . C46 C 0.2075(5) 0.1474(5) 0.1098(3) 0.0661(14) Uani 1 1 d . . . H46 H 0.2536 0.1041 0.0664 0.079 Uiso 1 1 calc R . . C47 C 0.2555(4) 0.1540(4) 0.1838(3) 0.0575(13) Uani 1 1 d . . . H47 H 0.3337 0.1147 0.1902 0.069 Uiso 1 1 calc R . . C48 C 0.1545(4) 0.2313(4) 0.4419(3) 0.0569(12) Uani 1 1 d . . . C49 C 0.1400(5) 0.2958(5) 0.5091(3) 0.0681(15) Uani 1 1 d . . . H49 H 0.1744 0.3429 0.5083 0.082 Uiso 1 1 calc R . . C50 C 0.0725(5) 0.2895(5) 0.5786(3) 0.0759(16) Uani 1 1 d . . . H50 H 0.0622 0.3325 0.6249 0.091 Uiso 1 1 calc R . . C51 C 0.0222(5) 0.2221(5) 0.5795(4) 0.0726(15) Uani 1 1 d . . . H51 H -0.0223 0.2188 0.6265 0.087 Uiso 1 1 calc R . . C52 C 0.0352(5) 0.1581(5) 0.5125(4) 0.0750(16) Uani 1 1 d . . . H52 H -0.0007 0.1123 0.5136 0.090 Uiso 1 1 calc R . . C53 C 0.1031(5) 0.1621(5) 0.4427(4) 0.0714(15) Uani 1 1 d . . . H53 H 0.1135 0.1185 0.3969 0.086 Uiso 1 1 calc R . . O11 O 0.2515(6) 0.8572(5) 0.4723(4) 0.144(2) Uani 1 1 d D . . H1W H 0.296(3) 0.797(2) 0.436(2) 0.060 Uiso 1 1 d D . . H2W H 0.199(3) 0.914(3) 0.434(2) 0.060 Uiso 1 1 d D . . O12 O 0.5005(5) 0.9782(6) 0.0942(5) 0.168(3) Uani 1 1 d D . . H3W H 0.5791(16) 0.923(3) 0.099(3) 0.060 Uiso 1 1 d D . . H4W H 0.489(4) 0.968(4) 0.0369(12) 0.060 Uiso 1 1 d D . . O13 O 0.4515(13) 0.6695(13) 0.4703(10) 0.182(6) Uiso 0.50 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 0.0475(4) 0.0449(4) 0.0444(4) -0.0059(3) 0.0048(3) -0.0220(3) O1 0.057(2) 0.056(2) 0.073(2) -0.0057(18) -0.0098(18) -0.0277(18) O2 0.066(2) 0.0490(19) 0.053(2) 0.0058(15) -0.0046(17) -0.0261(18) C1 0.108(5) 0.061(4) 0.073(4) -0.008(3) -0.018(4) -0.047(4) C2 0.118(5) 0.051(3) 0.052(3) -0.008(3) 0.003(3) -0.034(4) O3 0.185(5) 0.093(3) 0.066(3) -0.037(3) 0.015(3) -0.048(3) O4 0.151(5) 0.126(4) 0.115(4) -0.021(3) -0.059(4) -0.067(4) C3 0.069(3) 0.061(3) 0.049(3) -0.013(2) 0.016(3) -0.037(3) C4 0.058(3) 0.065(3) 0.076(4) -0.031(3) 0.015(3) -0.035(3) O5 0.067(2) 0.058(2) 0.049(2) -0.0123(16) 0.0137(17) -0.0206(18) O6 0.063(2) 0.087(3) 0.079(3) -0.019(2) -0.007(2) -0.039(2) O7 0.069(3) 0.078(3) 0.177(5) -0.035(3) -0.002(3) -0.041(2) O8 0.115(3) 0.066(3) 0.083(3) 0.002(2) 0.011(2) -0.058(3) O9 0.0561(19) 0.0389(17) 0.0498(19) -0.0054(14) 0.0144(16) -0.0127(15) O10 0.056(2) 0.0378(17) 0.0486(18) -0.0028(14) 0.0103(15) -0.0150(15) C5 0.040(2) 0.040(2) 0.046(3) -0.006(2) 0.003(2) -0.016(2) As1 0.0418(3) 0.0404(3) 0.0495(3) -0.0032(2) 0.0037(2) -0.0179(2) C6 0.053(3) 0.057(3) 0.051(3) -0.004(2) 0.005(2) -0.028(3) C7 0.111(5) 0.074(4) 0.074(4) 0.014(3) -0.017(4) -0.057(4) C8 0.145(7) 0.092(5) 0.079(5) 0.031(4) -0.044(5) -0.064(5) C9 0.104(5) 0.101(5) 0.066(4) -0.005(4) -0.027(4) -0.049(4) C10 0.114(5) 0.116(5) 0.062(4) -0.015(4) -0.006(4) -0.080(5) C11 0.115(5) 0.105(5) 0.058(3) -0.003(3) -0.001(3) -0.083(4) C12 0.046(3) 0.044(3) 0.065(3) -0.006(2) 0.010(2) -0.018(2) C13 0.086(4) 0.064(4) 0.082(4) -0.015(3) 0.019(4) -0.017(3) C14 0.104(6) 0.068(4) 0.121(6) -0.035(4) 0.043(5) -0.021(4) C15 0.072(4) 0.049(4) 0.149(7) -0.014(4) 0.037(5) -0.013(3) C16 0.073(4) 0.058(4) 0.127(6) 0.013(4) -0.003(4) -0.002(3) C17 0.071(4) 0.055(3) 0.081(4) -0.010(3) 0.006(3) -0.005(3) C18 0.039(2) 0.042(3) 0.052(3) -0.003(2) 0.007(2) -0.017(2) C19 0.041(3) 0.048(3) 0.054(3) -0.001(2) 0.000(2) -0.013(2) C20 0.042(3) 0.072(4) 0.066(3) 0.004(3) -0.005(2) -0.031(3) C21 0.067(4) 0.070(4) 0.070(3) 0.001(3) -0.001(3) -0.048(3) C22 0.059(3) 0.044(3) 0.078(4) 0.006(3) 0.001(3) -0.024(3) C23 0.042(3) 0.043(3) 0.074(3) 0.004(2) 0.002(2) -0.019(2) C24 0.041(2) 0.041(2) 0.042(2) 0.003(2) -0.004(2) -0.018(2) C25 0.061(3) 0.038(2) 0.057(3) -0.004(2) 0.005(2) -0.019(2) C26 0.062(3) 0.046(3) 0.052(3) -0.006(2) 0.010(3) -0.006(3) C27 0.048(3) 0.061(3) 0.060(3) 0.012(3) 0.002(2) -0.018(3) C28 0.057(3) 0.062(3) 0.070(3) 0.012(3) -0.009(3) -0.037(3) C29 0.053(3) 0.055(3) 0.053(3) 0.000(2) 0.000(2) -0.032(2) As2 0.0536(3) 0.0734(4) 0.0417(3) -0.0037(2) -0.0035(2) -0.0259(3) C30 0.066(3) 0.075(4) 0.049(3) -0.005(3) 0.003(3) -0.030(3) C31 0.075(4) 0.077(4) 0.056(3) -0.006(3) -0.004(3) -0.014(3) C32 0.090(5) 0.079(5) 0.080(5) 0.002(4) 0.009(4) -0.009(4) C33 0.122(7) 0.088(5) 0.104(6) 0.002(5) 0.011(5) -0.048(5) C34 0.114(6) 0.133(7) 0.122(7) 0.002(6) -0.010(5) -0.082(6) C35 0.092(5) 0.099(5) 0.082(4) 0.010(4) -0.016(4) -0.057(4) C36 0.051(3) 0.081(4) 0.053(3) -0.001(3) -0.010(2) -0.022(3) C37 0.077(4) 0.080(4) 0.094(5) 0.006(4) -0.009(4) -0.030(4) C38 0.101(6) 0.093(6) 0.127(7) 0.020(5) -0.024(5) -0.013(5) C39 0.069(5) 0.144(8) 0.110(6) 0.019(6) -0.006(5) 0.000(5) C40 0.065(5) 0.159(8) 0.100(6) 0.038(6) 0.008(4) -0.020(5) C41 0.062(4) 0.117(6) 0.082(4) 0.024(4) 0.005(3) -0.024(4) C42 0.055(3) 0.070(3) 0.040(3) -0.005(2) -0.001(2) -0.026(3) C43 0.054(3) 0.140(6) 0.059(4) -0.027(4) -0.002(3) -0.021(4) C44 0.061(4) 0.143(7) 0.078(5) -0.004(4) -0.020(3) -0.036(4) C45 0.099(5) 0.083(4) 0.056(3) 0.002(3) -0.018(3) -0.057(4) C46 0.084(4) 0.065(3) 0.050(3) -0.004(3) -0.001(3) -0.035(3) C47 0.062(3) 0.064(3) 0.047(3) 0.004(2) -0.005(2) -0.030(3) C48 0.054(3) 0.069(3) 0.045(3) -0.008(2) -0.001(2) -0.026(3) C49 0.085(4) 0.077(4) 0.052(3) -0.013(3) 0.009(3) -0.046(3) C50 0.098(5) 0.088(4) 0.050(3) -0.014(3) 0.007(3) -0.049(4) C51 0.077(4) 0.077(4) 0.060(4) -0.005(3) 0.011(3) -0.034(3) C52 0.079(4) 0.085(4) 0.069(4) -0.008(3) 0.004(3) -0.045(3) C53 0.081(4) 0.082(4) 0.059(3) -0.019(3) 0.004(3) -0.042(3) O11 0.155(6) 0.113(5) 0.131(5) 0.005(4) 0.044(4) -0.039(4) O12 0.089(4) 0.167(6) 0.229(8) -0.079(6) 0.004(5) -0.033(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O6 1.961(3) . ? Fe1 O5 1.968(3) . ? Fe1 O2 1.977(3) . ? Fe1 O1 1.986(3) . ? Fe1 O10 2.090(3) . ? Fe1 O9 2.094(3) . ? O1 C4 1.293(6) . ? O2 C3 1.295(6) . ? C1 O4 1.236(7) . ? C1 O6 1.271(7) . ? C1 C2 1.538(9) . ? C2 O3 1.218(6) . ? C2 O5 1.286(7) . ? C3 O8 1.208(6) . ? C3 C4 1.525(8) . ? C4 O7 1.232(6) . ? O9 C5 1.247(5) . ? O10 C5 1.255(5) 2_775 ? C5 O10 1.255(5) 2_775 ? C5 C5 1.523(8) 2_775 ? As1 C12 1.901(5) . ? As1 C18 1.906(4) . ? As1 C24 1.911(4) . ? As1 C6 1.912(5) . ? C6 C7 1.367(7) . ? C6 C11 1.377(7) . ? C7 C8 1.398(8) . ? C8 C9 1.342(8) . ? C9 C10 1.359(9) . ? C10 C11 1.365(8) . ? C12 C17 1.366(7) . ? C12 C13 1.376(7) . ? C13 C14 1.376(9) . ? C14 C15 1.365(10) . ? C15 C16 1.350(10) . ? C16 C17 1.388(8) . ? C18 C23 1.389(6) . ? C18 C19 1.398(6) . ? C19 C20 1.377(6) . ? C20 C21 1.380(7) . ? C21 C22 1.390(7) . ? C22 C23 1.364(6) . ? C24 C25 1.370(6) . ? C24 C29 1.385(6) . ? C25 C26 1.392(7) . ? C26 C27 1.352(7) . ? C27 C28 1.369(7) . ? C28 C29 1.375(7) . ? As2 C30 1.909(6) . ? As2 C48 1.910(5) . ? As2 C42 1.913(5) . ? As2 C36 1.913(5) . ? C30 C31 1.373(8) . ? C30 C35 1.393(8) . ? C31 C32 1.381(9) . ? C32 C33 1.346(10) . ? C33 C34 1.361(10) . ? C34 C35 1.386(9) . ? C36 C37 1.370(8) . ? C36 C41 1.378(8) . ? C37 C38 1.383(9) . ? C38 C39 1.378(11) . ? C39 C40 1.347(11) . ? C40 C41 1.362(9) . ? C42 C47 1.356(7) . ? C42 C43 1.376(7) . ? C43 C44 1.392(8) . ? C44 C45 1.357(9) . ? C45 C46 1.361(8) . ? C46 C47 1.395(7) . ? C48 C49 1.370(7) . ? C48 C53 1.377(7) . ? C49 C50 1.396(7) . ? C50 C51 1.343(8) . ? C51 C52 1.367(8) . ? C52 C53 1.394(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Fe1 O5 81.48(16) . . ? O6 Fe1 O2 91.65(16) . . ? O5 Fe1 O2 101.51(14) . . ? O6 Fe1 O1 170.35(16) . . ? O5 Fe1 O1 93.47(15) . . ? O2 Fe1 O1 81.26(14) . . ? O6 Fe1 O10 89.35(15) . . ? O5 Fe1 O10 164.82(13) . . ? O2 Fe1 O10 90.76(13) . . ? O1 Fe1 O10 97.24(14) . . ? O6 Fe1 O9 98.34(15) . . ? O5 Fe1 O9 90.72(13) . . ? O2 Fe1 O9 165.26(13) . . ? O1 Fe1 O9 89.90(14) . . ? O10 Fe1 O9 78.60(12) . . ? C4 O1 Fe1 114.2(3) . . ? C3 O2 Fe1 116.1(3) . . ? O4 C1 O6 124.9(7) . . ? O4 C1 C2 121.0(6) . . ? O6 C1 C2 114.1(5) . . ? O3 C2 O5 125.6(7) . . ? O3 C2 C1 121.3(6) . . ? O5 C2 C1 113.1(5) . . ? O8 C3 O2 124.8(5) . . ? O8 C3 C4 122.5(5) . . ? O2 C3 C4 112.7(4) . . ? O7 C4 O1 123.9(6) . . ? O7 C4 C3 120.8(5) . . ? O1 C4 C3 115.3(4) . . ? C2 O5 Fe1 115.3(4) . . ? C1 O6 Fe1 115.2(4) . . ? C5 O9 Fe1 113.7(3) . . ? C5 O10 Fe1 114.2(3) 2_775 . ? O9 C5 O10 126.5(4) . 2_775 ? O9 C5 C5 117.3(5) . 2_775 ? O10 C5 C5 116.2(5) 2_775 2_775 ? C12 As1 C18 109.58(19) . . ? C12 As1 C24 108.82(19) . . ? C18 As1 C24 110.08(18) . . ? C12 As1 C6 108.3(2) . . ? C18 As1 C6 110.6(2) . . ? C24 As1 C6 109.39(19) . . ? C7 C6 C11 119.6(5) . . ? C7 C6 As1 121.4(4) . . ? C11 C6 As1 119.0(4) . . ? C6 C7 C8 118.7(6) . . ? C9 C8 C7 121.1(6) . . ? C8 C9 C10 119.9(6) . . ? C9 C10 C11 120.4(6) . . ? C10 C11 C6 120.3(5) . . ? C17 C12 C13 120.2(5) . . ? C17 C12 As1 119.9(4) . . ? C13 C12 As1 119.7(4) . . ? C14 C13 C12 119.1(7) . . ? C15 C14 C13 120.4(7) . . ? C16 C15 C14 120.7(6) . . ? C15 C16 C17 119.7(7) . . ? C12 C17 C16 119.9(6) . . ? C23 C18 C19 120.3(4) . . ? C23 C18 As1 120.7(3) . . ? C19 C18 As1 119.0(3) . . ? C20 C19 C18 119.1(4) . . ? C19 C20 C21 120.0(4) . . ? C20 C21 C22 120.8(5) . . ? C23 C22 C21 119.5(5) . . ? C22 C23 C18 120.2(4) . . ? C25 C24 C29 120.7(4) . . ? C25 C24 As1 121.9(3) . . ? C29 C24 As1 117.4(3) . . ? C24 C25 C26 119.0(4) . . ? C27 C26 C25 120.8(5) . . ? C26 C27 C28 119.7(5) . . ? C27 C28 C29 121.2(5) . . ? C28 C29 C24 118.7(5) . . ? C30 As2 C48 108.5(2) . . ? C30 As2 C42 110.4(2) . . ? C48 As2 C42 108.5(2) . . ? C30 As2 C36 110.8(2) . . ? C48 As2 C36 110.2(2) . . ? C42 As2 C36 108.4(2) . . ? C31 C30 C35 119.8(6) . . ? C31 C30 As2 120.3(5) . . ? C35 C30 As2 119.7(5) . . ? C30 C31 C32 120.3(6) . . ? C33 C32 C31 119.2(7) . . ? C32 C33 C34 122.2(8) . . ? C33 C34 C35 119.6(7) . . ? C34 C35 C30 118.8(7) . . ? C37 C36 C41 119.7(6) . . ? C37 C36 As2 119.7(4) . . ? C41 C36 As2 120.5(5) . . ? C36 C37 C38 119.5(7) . . ? C39 C38 C37 118.9(8) . . ? C40 C39 C38 121.8(8) . . ? C39 C40 C41 119.1(7) . . ? C40 C41 C36 120.9(7) . . ? C47 C42 C43 120.2(5) . . ? C47 C42 As2 120.1(4) . . ? C43 C42 As2 119.7(4) . . ? C42 C43 C44 119.9(6) . . ? C45 C44 C43 119.5(6) . . ? C44 C45 C46 120.8(5) . . ? C45 C46 C47 119.9(5) . . ? C42 C47 C46 119.7(5) . . ? C49 C48 C53 120.7(5) . . ? C49 C48 As2 120.8(4) . . ? C53 C48 As2 118.4(4) . . ? C48 C49 C50 118.7(5) . . ? C51 C50 C49 120.7(5) . . ? C50 C51 C52 121.2(6) . . ? C51 C52 C53 119.2(6) . . ? C48 C53 C52 119.5(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O11 H1W O13 0.958(10) 2.06(4) 2.693(17) 122(3) . O11 H2W O4 0.957(10) 1.93(2) 2.841(8) 158(4) 1_455 O12 H3W O7 0.966(10) 1.817(14) 2.774(8) 170(4) . O12 H4W O12 0.959(10) 2.16(3) 2.994(18) 145(4) 2_675 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.657 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.064 #==END data_3 _database_code_depnum_ccdc_archive 'CCDC 255484' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H30 As Fe N2 O9' _chemical_formula_weight 789.41 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' N N 0.0061 0.0033 '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' 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.565(3) _cell_length_b 13.618(3) _cell_length_c 18.393(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.28(3) _cell_angle_gamma 90.00 _cell_volume 3399.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 15 _cell_measurement_theta_max 30 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1612 _exptl_absorpt_coefficient_mu 1.471 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.4724 _exptl_absorpt_correction_T_max 0.8990 _exptl_absorpt_process_details psi-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'R3m/V automatic four-circle diffractometer' _diffrn_measurement_method omega/2-theta-scans _diffrn_standards_decay_% 2.2 _diffrn_reflns_number 6402 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.05 _reflns_number_total 6015 _reflns_number_gt 4825 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (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^)+(0.0544P)^2^+1.9236P] 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 6015 _refine_ls_number_parameters 468 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1003 _refine_ls_wR_factor_gt 0.0923 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 0.48725(3) 0.11445(3) 0.18901(2) 0.03166(13) Uani 1 1 d . . . N1 N 0.44029(19) 0.18611(19) 0.07596(14) 0.0353(6) Uani 1 1 d . . . N2 N 0.43755(19) -0.00280(18) 0.10645(14) 0.0335(6) Uani 1 1 d . . . C1 C 0.4484(3) 0.2820(3) 0.0650(2) 0.0485(9) Uani 1 1 d . . . H1 H 0.4765 0.3222 0.1083 0.058 Uiso 1 1 calc R . . C2 C 0.4167(3) 0.3235(3) -0.0082(2) 0.0610(11) Uani 1 1 d . . . H2 H 0.4260 0.3901 -0.0145 0.073 Uiso 1 1 calc R . . C3 C 0.3713(4) 0.2649(3) -0.0711(2) 0.0687(12) Uani 1 1 d . . . H3 H 0.3468 0.2919 -0.1209 0.082 Uiso 1 1 calc R . . C4 C 0.3618(3) 0.1666(3) -0.0610(2) 0.0579(10) Uani 1 1 d . . . H4 H 0.3307 0.1264 -0.1037 0.069 Uiso 1 1 calc R . . C5 C 0.3987(2) 0.1274(2) 0.01360(18) 0.0366(7) Uani 1 1 d . . . C6 C 0.3980(2) 0.0219(2) 0.03056(17) 0.0345(7) Uani 1 1 d . . . C7 C 0.3605(3) -0.0485(3) -0.0269(2) 0.0474(9) Uani 1 1 d . . . H7 H 0.3335 -0.0306 -0.0792 0.057 Uiso 1 1 calc R . . C8 C 0.3640(3) -0.1456(3) -0.0049(2) 0.0553(10) Uani 1 1 d . . . H8 H 0.3402 -0.1942 -0.0427 0.066 Uiso 1 1 calc R . . C9 C 0.4021(3) -0.1701(3) 0.0715(2) 0.0548(10) Uani 1 1 d . . . H9 H 0.4032 -0.2354 0.0868 0.066 Uiso 1 1 calc R . . C10 C 0.4394(3) -0.0970(2) 0.1266(2) 0.0450(8) Uani 1 1 d . . . H10 H 0.4666 -0.1141 0.1791 0.054 Uiso 1 1 calc R . . O1 O 0.54954(18) 0.23533(17) 0.24403(13) 0.0456(6) Uani 1 1 d . . . O2 O 0.62274(16) 0.09207(17) 0.19095(12) 0.0403(5) Uani 1 1 d . . . C11 C 0.6415(3) 0.2471(3) 0.25405(19) 0.0448(8) Uani 1 1 d . . . C12 C 0.6824(2) 0.1650(3) 0.21579(18) 0.0424(8) Uani 1 1 d . . . O3 O 0.7629(2) 0.1728(2) 0.21105(17) 0.0710(8) Uani 1 1 d . . . O4 O 0.6938(2) 0.3144(2) 0.28842(16) 0.0648(8) Uani 1 1 d . . . O5 O 0.35318(16) 0.13847(17) 0.19033(13) 0.0434(6) Uani 1 1 d . . . O6 O 0.49498(16) 0.02801(17) 0.27652(12) 0.0396(5) Uani 1 1 d . . . C14 C 0.4198(3) 0.0300(3) 0.29848(18) 0.0404(8) Uani 1 1 d . . . C13 C 0.3326(2) 0.0904(2) 0.24295(19) 0.0394(8) Uani 1 1 d . . . O7 O 0.4159(2) -0.0082(2) 0.35684(14) 0.0603(7) Uani 1 1 d . . . O8 O 0.2533(2) 0.0909(2) 0.25080(18) 0.0646(8) Uani 1 1 d . . . As1 As 0.03714(2) 0.78398(2) 0.480727(18) 0.03391(11) Uani 1 1 d . . . C15 C -0.0579(2) 0.8347(2) 0.38679(18) 0.0390(8) Uani 1 1 d . . . C16 C -0.1522(3) 0.7958(3) 0.3591(2) 0.0520(9) Uani 1 1 d . . . H16 H -0.1668 0.7403 0.3823 0.062 Uiso 1 1 calc R . . C17 C -0.2244(3) 0.8401(3) 0.2968(2) 0.0632(11) Uani 1 1 d . . . H17 H -0.2880 0.8148 0.2776 0.076 Uiso 1 1 calc R . . C18 C -0.2003(3) 0.9228(3) 0.2635(2) 0.0654(12) Uani 1 1 d . . . H18 H -0.2491 0.9542 0.2226 0.079 Uiso 1 1 calc R . . C19 C -0.1068(3) 0.9591(3) 0.2891(2) 0.0565(10) Uani 1 1 d . . . H19 H -0.0917 1.0129 0.2644 0.068 Uiso 1 1 calc R . . C20 C -0.0349(3) 0.9161(3) 0.3517(2) 0.0475(9) Uani 1 1 d . . . H20 H 0.0287 0.9415 0.3704 0.057 Uiso 1 1 calc R . . C21 C 0.0665(2) 0.6493(2) 0.46968(19) 0.0386(7) Uani 1 1 d . . . C22 C 0.0172(3) 0.5988(3) 0.4016(2) 0.0508(9) Uani 1 1 d . . . H22 H -0.0321 0.6294 0.3606 0.061 Uiso 1 1 calc R . . C23 C 0.0421(3) 0.5016(3) 0.3950(3) 0.0638(11) Uani 1 1 d . . . H23 H 0.0102 0.4674 0.3489 0.077 Uiso 1 1 calc R . . C24 C 0.1135(3) 0.4561(3) 0.4559(3) 0.0582(10) Uani 1 1 d . . . H24 H 0.1292 0.3909 0.4512 0.070 Uiso 1 1 calc R . . C25 C 0.1620(3) 0.5064(3) 0.5240(2) 0.0541(10) Uani 1 1 d . . . H25 H 0.2095 0.4747 0.5655 0.065 Uiso 1 1 calc R . . C26 C 0.1399(3) 0.6041(3) 0.5306(2) 0.0451(8) Uani 1 1 d . . . H26 H 0.1743 0.6391 0.5757 0.054 Uiso 1 1 calc R . . C27 C 0.1575(2) 0.8544(2) 0.50722(18) 0.0362(7) Uani 1 1 d . . . C28 C 0.1985(3) 0.9006(3) 0.57868(19) 0.0442(8) Uani 1 1 d . . . H28 H 0.1654 0.9008 0.6135 0.053 Uiso 1 1 calc R . . C29 C 0.2885(3) 0.9464(3) 0.5981(2) 0.0510(9) Uani 1 1 d . . . H29 H 0.3167 0.9774 0.6461 0.061 Uiso 1 1 calc R . . C30 C 0.3365(3) 0.9460(3) 0.5463(2) 0.0545(10) Uani 1 1 d . . . H30 H 0.3981 0.9754 0.5604 0.065 Uiso 1 1 calc R . . C31 C 0.2957(3) 0.9030(3) 0.4739(2) 0.0528(10) Uani 1 1 d . . . H31 H 0.3280 0.9060 0.4387 0.063 Uiso 1 1 calc R . . C32 C 0.2054(2) 0.8548(3) 0.4540(2) 0.0427(8) Uani 1 1 d . . . H32 H 0.1776 0.8235 0.4060 0.051 Uiso 1 1 calc R . . C33 C -0.0154(2) 0.8004(2) 0.56185(18) 0.0336(7) Uani 1 1 d . . . C34 C 0.0301(3) 0.7563(3) 0.63331(19) 0.0449(8) Uani 1 1 d . . . H34 H 0.0869 0.7191 0.6427 0.054 Uiso 1 1 calc R . . C35 C -0.0089(3) 0.7674(3) 0.6909(2) 0.0537(10) Uani 1 1 d . . . H35 H 0.0208 0.7366 0.7388 0.064 Uiso 1 1 calc R . . C36 C -0.0916(3) 0.8240(3) 0.6775(2) 0.0526(9) Uani 1 1 d . . . H36 H -0.1175 0.8314 0.7165 0.063 Uiso 1 1 calc R . . C37 C -0.1360(3) 0.8698(3) 0.6067(2) 0.0516(9) Uani 1 1 d . . . H37 H -0.1915 0.9086 0.5980 0.062 Uiso 1 1 calc R . . C38 C -0.0980(3) 0.8580(3) 0.5484(2) 0.0450(8) Uani 1 1 d . . . H38 H -0.1279 0.8888 0.5004 0.054 Uiso 1 1 calc R . . O9 O 0.8388(2) 0.4070(3) 0.22959(19) 0.0698(8) Uani 1 1 d D . . H1W H 0.798(3) 0.359(3) 0.241(4) 0.14(2) Uiso 1 1 d D . . H2W H 0.800(3) 0.4652(19) 0.224(3) 0.099(18) 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 0.0300(2) 0.0429(3) 0.0248(2) -0.00307(18) 0.01313(18) 0.00087(19) N1 0.0371(15) 0.0402(15) 0.0310(14) 0.0020(11) 0.0154(12) 0.0033(12) N2 0.0373(15) 0.0363(14) 0.0319(14) -0.0026(11) 0.0187(12) -0.0015(12) C1 0.060(2) 0.043(2) 0.046(2) 0.0014(16) 0.0244(18) 0.0081(17) C2 0.085(3) 0.049(2) 0.057(2) 0.014(2) 0.035(2) 0.015(2) C3 0.085(3) 0.078(3) 0.046(2) 0.029(2) 0.027(2) 0.016(2) C4 0.064(3) 0.075(3) 0.0310(19) 0.0027(18) 0.0128(18) -0.002(2) C5 0.0297(17) 0.053(2) 0.0300(16) 0.0011(14) 0.0141(13) -0.0004(15) C6 0.0305(17) 0.0504(19) 0.0293(16) -0.0064(14) 0.0188(13) -0.0052(14) C7 0.047(2) 0.065(2) 0.0362(18) -0.0144(17) 0.0230(16) -0.0142(18) C8 0.063(3) 0.061(2) 0.055(2) -0.0255(19) 0.038(2) -0.021(2) C9 0.076(3) 0.040(2) 0.065(3) -0.0110(18) 0.044(2) -0.0099(19) C10 0.056(2) 0.046(2) 0.0413(19) 0.0004(15) 0.0263(17) -0.0031(17) O1 0.0452(15) 0.0519(14) 0.0432(14) -0.0159(11) 0.0203(11) -0.0064(12) O2 0.0326(12) 0.0530(14) 0.0386(12) -0.0084(10) 0.0170(10) 0.0023(11) C11 0.050(2) 0.054(2) 0.0320(17) 0.0006(16) 0.0169(16) -0.0089(18) C12 0.035(2) 0.063(2) 0.0306(17) 0.0013(16) 0.0129(14) 0.0000(17) O3 0.0378(16) 0.103(2) 0.078(2) -0.0151(17) 0.0288(15) -0.0104(15) O4 0.0658(19) 0.0639(17) 0.0655(18) -0.0218(15) 0.0249(15) -0.0269(15) O5 0.0367(13) 0.0557(14) 0.0432(13) 0.0037(11) 0.0209(11) 0.0097(11) O6 0.0351(12) 0.0575(14) 0.0280(11) 0.0030(10) 0.0136(9) 0.0024(10) C14 0.046(2) 0.049(2) 0.0310(17) -0.0065(14) 0.0190(15) -0.0065(16) C13 0.040(2) 0.0434(19) 0.0421(19) -0.0078(15) 0.0233(16) 0.0005(15) O7 0.0659(18) 0.0831(19) 0.0408(14) 0.0106(13) 0.0300(13) -0.0044(15) O8 0.0504(16) 0.0734(18) 0.089(2) 0.0104(16) 0.0480(16) 0.0097(14) As1 0.03232(19) 0.04188(19) 0.02834(17) 0.00060(13) 0.01198(13) -0.00437(14) C15 0.042(2) 0.0451(19) 0.0289(16) -0.0006(14) 0.0119(14) -0.0014(15) C16 0.046(2) 0.056(2) 0.045(2) -0.0023(17) 0.0049(17) -0.0082(18) C17 0.050(2) 0.066(3) 0.054(2) -0.014(2) -0.0042(19) 0.003(2) C18 0.077(3) 0.058(3) 0.040(2) -0.0042(19) -0.004(2) 0.019(2) C19 0.075(3) 0.050(2) 0.041(2) 0.0045(17) 0.016(2) 0.007(2) C20 0.054(2) 0.048(2) 0.0392(19) 0.0020(16) 0.0149(17) -0.0010(17) C21 0.0383(19) 0.0449(18) 0.0376(18) -0.0015(15) 0.0198(15) -0.0063(15) C22 0.055(2) 0.054(2) 0.0395(19) -0.0025(16) 0.0133(17) -0.0055(18) C23 0.078(3) 0.053(2) 0.066(3) -0.017(2) 0.033(2) -0.013(2) C24 0.061(3) 0.044(2) 0.083(3) -0.004(2) 0.042(2) -0.0040(19) C25 0.040(2) 0.059(2) 0.069(3) 0.009(2) 0.0271(19) 0.0060(18) C26 0.0369(19) 0.055(2) 0.046(2) -0.0033(16) 0.0189(16) -0.0001(16) C27 0.0336(17) 0.0396(17) 0.0332(17) 0.0028(14) 0.0097(14) -0.0040(14) C28 0.042(2) 0.054(2) 0.0354(18) 0.0018(15) 0.0121(15) -0.0032(16) C29 0.039(2) 0.057(2) 0.047(2) -0.0008(17) 0.0037(17) -0.0083(18) C30 0.036(2) 0.051(2) 0.068(3) 0.0155(19) 0.0081(18) -0.0063(17) C31 0.040(2) 0.065(2) 0.060(2) 0.020(2) 0.0258(18) -0.0003(18) C32 0.0383(19) 0.052(2) 0.0414(19) 0.0045(16) 0.0181(15) -0.0029(16) C33 0.0323(17) 0.0372(17) 0.0329(16) -0.0025(13) 0.0138(13) -0.0047(13) C34 0.040(2) 0.061(2) 0.0369(18) 0.0064(16) 0.0180(15) 0.0154(17) C35 0.059(2) 0.069(3) 0.040(2) 0.0095(18) 0.0247(18) 0.011(2) C36 0.050(2) 0.066(2) 0.052(2) -0.0076(19) 0.0313(19) -0.0015(19) C37 0.039(2) 0.065(2) 0.057(2) 0.0004(19) 0.0247(18) 0.0101(18) C38 0.041(2) 0.051(2) 0.0411(19) 0.0067(16) 0.0123(16) 0.0052(16) O9 0.0593(19) 0.079(2) 0.078(2) 0.0109(17) 0.0328(16) 0.0087(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 O6 1.964(2) . ? Fe1 O1 1.972(2) . ? Fe1 O2 1.984(2) . ? Fe1 O5 1.989(2) . ? Fe1 N2 2.140(3) . ? Fe1 N1 2.171(3) . ? N1 C1 1.333(4) . ? N1 C5 1.348(4) . ? N2 C10 1.333(4) . ? N2 C6 1.345(4) . ? C1 C2 1.376(5) . ? C2 C3 1.363(6) . ? C3 C4 1.366(6) . ? C4 C5 1.386(5) . ? C5 C6 1.470(5) . ? C6 C7 1.384(4) . ? C7 C8 1.378(5) . ? C8 C9 1.353(5) . ? C9 C10 1.383(5) . ? O1 C11 1.294(4) . ? O2 C12 1.289(4) . ? C11 O4 1.212(4) . ? C11 C12 1.550(5) . ? C12 O3 1.211(4) . ? O5 C13 1.291(4) . ? O6 C14 1.297(4) . ? C14 O7 1.212(4) . ? C14 C13 1.547(5) . ? C13 O8 1.215(4) . ? As1 C27 1.900(3) . ? As1 C15 1.908(3) . ? As1 C21 1.911(3) . ? As1 C33 1.921(3) . ? C15 C20 1.383(5) . ? C15 C16 1.385(5) . ? C16 C17 1.381(5) . ? C17 C18 1.388(6) . ? C18 C19 1.362(6) . ? C19 C20 1.376(5) . ? C21 C22 1.380(5) . ? C21 C26 1.381(5) . ? C22 C23 1.388(5) . ? C23 C24 1.368(6) . ? C24 C25 1.377(6) . ? C25 C26 1.385(5) . ? C27 C28 1.382(5) . ? C27 C32 1.393(4) . ? C28 C29 1.376(5) . ? C29 C30 1.370(5) . ? C30 C31 1.376(5) . ? C31 C32 1.395(5) . ? C33 C34 1.377(4) . ? C33 C38 1.382(5) . ? C34 C35 1.380(5) . ? C35 C36 1.374(5) . ? C36 C37 1.376(5) . ? C37 C38 1.383(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Fe1 O1 101.59(10) . . ? O6 Fe1 O2 97.61(10) . . ? O1 Fe1 O2 81.35(10) . . ? O6 Fe1 O5 81.55(10) . . ? O1 Fe1 O5 97.32(10) . . ? O2 Fe1 O5 178.27(9) . . ? O6 Fe1 N2 92.20(10) . . ? O1 Fe1 N2 163.88(9) . . ? O2 Fe1 N2 88.64(10) . . ? O5 Fe1 N2 92.90(10) . . ? O6 Fe1 N1 163.52(10) . . ? O1 Fe1 N1 92.44(10) . . ? O2 Fe1 N1 92.97(10) . . ? O5 Fe1 N1 88.18(10) . . ? N2 Fe1 N1 75.40(10) . . ? C1 N1 C5 119.3(3) . . ? C1 N1 Fe1 124.8(2) . . ? C5 N1 Fe1 115.9(2) . . ? C10 N2 C6 119.1(3) . . ? C10 N2 Fe1 123.6(2) . . ? C6 N2 Fe1 117.2(2) . . ? N1 C1 C2 122.2(4) . . ? C3 C2 C1 118.5(4) . . ? C2 C3 C4 120.0(4) . . ? C3 C4 C5 119.4(4) . . ? N1 C5 C4 120.4(3) . . ? N1 C5 C6 115.8(3) . . ? C4 C5 C6 123.8(3) . . ? N2 C6 C7 121.4(3) . . ? N2 C6 C5 115.5(3) . . ? C7 C6 C5 123.1(3) . . ? C8 C7 C6 118.6(3) . . ? C9 C8 C7 119.9(3) . . ? C8 C9 C10 119.2(4) . . ? N2 C10 C9 121.8(3) . . ? C11 O1 Fe1 115.8(2) . . ? C12 O2 Fe1 115.2(2) . . ? O4 C11 O1 126.1(4) . . ? O4 C11 C12 120.6(3) . . ? O1 C11 C12 113.2(3) . . ? O3 C12 O2 125.9(3) . . ? O3 C12 C11 120.7(3) . . ? O2 C12 C11 113.3(3) . . ? C13 O5 Fe1 115.0(2) . . ? C14 O6 Fe1 116.0(2) . . ? O7 C14 O6 125.7(3) . . ? O7 C14 C13 121.4(3) . . ? O6 C14 C13 112.9(3) . . ? O8 C13 O5 125.2(3) . . ? O8 C13 C14 120.9(3) . . ? O5 C13 C14 113.9(3) . . ? C27 As1 C15 110.38(14) . . ? C27 As1 C21 106.90(14) . . ? C15 As1 C21 111.57(14) . . ? C27 As1 C33 109.43(13) . . ? C15 As1 C33 107.39(14) . . ? C21 As1 C33 111.19(13) . . ? C20 C15 C16 120.7(3) . . ? C20 C15 As1 119.6(3) . . ? C16 C15 As1 119.4(3) . . ? C17 C16 C15 119.5(4) . . ? C16 C17 C18 118.9(4) . . ? C19 C18 C17 121.6(4) . . ? C18 C19 C20 119.8(4) . . ? C19 C20 C15 119.5(4) . . ? C22 C21 C26 120.6(3) . . ? C22 C21 As1 120.8(3) . . ? C26 C21 As1 118.6(3) . . ? C21 C22 C23 119.2(4) . . ? C24 C23 C22 120.3(4) . . ? C23 C24 C25 120.4(4) . . ? C24 C25 C26 119.9(4) . . ? C21 C26 C25 119.5(4) . . ? C28 C27 C32 120.8(3) . . ? C28 C27 As1 120.9(2) . . ? C32 C27 As1 118.2(2) . . ? C29 C28 C27 119.7(3) . . ? C30 C29 C28 119.7(3) . . ? C29 C30 C31 121.6(3) . . ? C30 C31 C32 119.3(3) . . ? C27 C32 C31 118.8(3) . . ? C34 C33 C38 120.3(3) . . ? C34 C33 As1 120.1(2) . . ? C38 C33 As1 119.5(2) . . ? C33 C34 C35 119.7(3) . . ? C36 C35 C34 120.2(3) . . ? C35 C36 C37 120.3(3) . . ? C36 C37 C38 119.9(3) . . ? C33 C38 C37 119.7(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H1W O4 0.955(10) 2.09(3) 2.980(4) 154(5) . O9 H2W O8 0.955(10) 2.004(19) 2.924(4) 161(4) 2_655 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.689 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.070 #==END data_4 _database_code_depnum_ccdc_archive 'CCDC 255485' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H30 As Fe N2 O9' _chemical_formula_weight 813.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4991(19) _cell_length_b 14.279(3) _cell_length_c 14.557(3) _cell_angle_alpha 103.57(3) _cell_angle_beta 99.94(3) _cell_angle_gamma 105.77(3) _cell_volume 1787.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 15 _cell_measurement_theta_max 30 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 830 _exptl_absorpt_coefficient_mu 1.401 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.5409 _exptl_absorpt_correction_T_max 0.7669 _exptl_absorpt_process_details psi-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'R3m/V automatic four-circle diffractometer' _diffrn_measurement_method omega/2-theta-scans _diffrn_standards_decay_% 2.4 _diffrn_reflns_number 7663 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 26.06 _reflns_number_total 7058 _reflns_number_gt 4854 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (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^)+(0.0688P)^2^+1.0123P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7058 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0865 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1424 _refine_ls_wR_factor_gt 0.1241 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 0.60832(7) 0.49280(5) 0.28448(4) 0.04906(18) Uani 1 1 d . . . N1 N 0.8089(4) 0.5478(3) 0.2367(2) 0.0497(8) Uani 1 1 d . . . N2 N 0.7856(4) 0.5542(2) 0.4179(2) 0.0464(8) Uani 1 1 d . . . C1 C 0.8181(5) 0.5454(4) 0.1458(3) 0.0577(11) Uani 1 1 d . . . H1A H 0.7302 0.5166 0.0955 0.069 Uiso 1 1 calc R . . C2 C 0.9541(6) 0.5844(4) 0.1238(4) 0.0685(13) Uani 1 1 d . . . H2A H 0.9559 0.5813 0.0595 0.082 Uiso 1 1 calc R . . C3 C 1.0851(6) 0.6274(4) 0.1957(4) 0.0661(13) Uani 1 1 d . . . H3A H 1.1765 0.6533 0.1810 0.079 Uiso 1 1 calc R . . C4 C 1.0799(5) 0.6320(3) 0.2927(3) 0.0552(11) Uani 1 1 d . . . C5 C 1.2105(5) 0.6765(4) 0.3746(4) 0.0628(12) Uani 1 1 d . . . H5A H 1.3049 0.7044 0.3644 0.075 Uiso 1 1 calc R . . C6 C 1.1982(5) 0.6785(4) 0.4652(3) 0.0623(12) Uani 1 1 d . . . H6A H 1.2845 0.7077 0.5168 0.075 Uiso 1 1 calc R . . C7 C 1.0549(5) 0.6368(3) 0.4847(3) 0.0490(10) Uani 1 1 d . . . C8 C 1.0328(5) 0.6387(3) 0.5782(3) 0.0545(11) Uani 1 1 d . . . H8A H 1.1151 0.6662 0.6326 0.065 Uiso 1 1 calc R . . C9 C 0.8924(5) 0.6007(4) 0.5889(3) 0.0604(12) Uani 1 1 d . . . H9A H 0.8776 0.6028 0.6507 0.072 Uiso 1 1 calc R . . C10 C 0.7691(5) 0.5582(3) 0.5070(3) 0.0530(10) Uani 1 1 d . . . H10A H 0.6728 0.5320 0.5154 0.064 Uiso 1 1 calc R . . C11 C 0.9391(5) 0.5906(3) 0.3090(3) 0.0464(9) Uani 1 1 d . . . C12 C 0.9261(5) 0.5936(3) 0.4065(3) 0.0461(9) Uani 1 1 d . . . O1 O 0.6383(3) 0.3576(2) 0.2526(2) 0.0566(7) Uani 1 1 d . . . O2 O 0.4628(3) 0.4242(2) 0.3481(2) 0.0578(7) Uani 1 1 d . . . C13 C 0.5608(5) 0.2924(4) 0.2876(3) 0.0561(11) Uani 1 1 d . . . C14 C 0.4545(5) 0.3323(4) 0.3440(3) 0.0592(11) Uani 1 1 d . . . O3 O 0.3718(4) 0.2777(3) 0.3796(3) 0.0860(11) Uani 1 1 d . . . O4 O 0.5710(4) 0.2079(3) 0.2808(3) 0.0808(10) Uani 1 1 d . . . O5 O 0.4755(3) 0.4736(2) 0.1568(2) 0.0604(8) Uani 1 1 d . . . O6 O 0.5768(4) 0.6270(2) 0.3136(2) 0.0635(8) Uani 1 1 d . . . C15 C 0.4963(5) 0.6430(4) 0.2423(4) 0.0614(12) Uani 1 1 d . . . C16 C 0.4241(5) 0.5471(4) 0.1516(3) 0.0625(12) Uani 1 1 d . . . O7 O 0.4732(4) 0.7223(3) 0.2431(3) 0.0858(11) Uani 1 1 d . . . O8 O 0.3289(4) 0.5467(3) 0.0836(3) 0.0902(12) Uani 1 1 d . . . As1 As 0.94878(5) 0.03174(3) 0.20906(3) 0.05228(15) Uani 1 1 d . . . C17 C 1.1099(5) -0.0242(3) 0.2009(3) 0.0552(11) Uani 1 1 d . . . C18 C 1.2435(6) 0.0183(5) 0.2706(5) 0.106(2) Uani 1 1 d . . . H18A H 1.2580 0.0754 0.3222 0.127 Uiso 1 1 calc R . . C19 C 1.3571(7) -0.0238(5) 0.2638(5) 0.113(3) Uani 1 1 d . . . H19A H 1.4475 0.0047 0.3121 0.135 Uiso 1 1 calc R . . C20 C 1.3399(7) -0.1055(4) 0.1887(5) 0.0848(17) Uani 1 1 d . . . H20A H 1.4171 -0.1335 0.1852 0.102 Uiso 1 1 calc R . . C21 C 1.2087(7) -0.1457(4) 0.1188(4) 0.0864(17) Uani 1 1 d . . . H21A H 1.1964 -0.2017 0.0666 0.104 Uiso 1 1 calc R . . C22 C 1.0919(6) -0.1058(4) 0.1231(4) 0.0720(14) Uani 1 1 d . . . H22A H 1.0025 -0.1338 0.0738 0.086 Uiso 1 1 calc R . . C23 C 0.7707(5) -0.0644(4) 0.1163(3) 0.0594(11) Uani 1 1 d . . . C24 C 0.7166(7) -0.1623(4) 0.1231(4) 0.0880(18) Uani 1 1 d . . . H24A H 0.7633 -0.1806 0.1744 0.106 Uiso 1 1 calc R . . C25 C 0.5922(7) -0.2322(5) 0.0526(5) 0.101(2) Uani 1 1 d . . . H25A H 0.5529 -0.2976 0.0571 0.121 Uiso 1 1 calc R . . C26 C 0.5266(6) -0.2051(5) -0.0241(4) 0.0893(19) Uani 1 1 d . . . H26A H 0.4433 -0.2529 -0.0716 0.107 Uiso 1 1 calc R . . C27 C 0.5808(6) -0.1094(5) -0.0323(4) 0.0806(16) Uani 1 1 d . . . H27A H 0.5355 -0.0923 -0.0850 0.097 Uiso 1 1 calc R . . C28 C 0.7033(5) -0.0386(4) 0.0384(3) 0.0667(13) Uani 1 1 d . . . H28A H 0.7408 0.0269 0.0336 0.080 Uiso 1 1 calc R . . C29 C 0.9942(5) 0.1567(3) 0.1757(3) 0.0479(9) Uani 1 1 d . . . C30 C 0.8934(5) 0.2109(3) 0.1813(3) 0.0516(10) Uani 1 1 d . . . H30A H 0.8054 0.1865 0.2004 0.062 Uiso 1 1 calc R . . C31 C 0.9248(6) 0.3007(4) 0.1585(3) 0.0592(12) Uani 1 1 d . . . H31A H 0.8575 0.3373 0.1616 0.071 Uiso 1 1 calc R . . C32 C 1.0560(6) 0.3373(4) 0.1307(3) 0.0635(12) Uani 1 1 d . . . H32A H 1.0769 0.3985 0.1155 0.076 Uiso 1 1 calc R . . C33 C 1.1561(6) 0.2830(4) 0.1256(3) 0.0632(12) Uani 1 1 d . . . H33A H 1.2445 0.3080 0.1070 0.076 Uiso 1 1 calc R . . C34 C 1.1256(5) 0.1924(3) 0.1478(3) 0.0575(11) Uani 1 1 d . . . H34A H 1.1926 0.1555 0.1441 0.069 Uiso 1 1 calc R . . C35 C 0.9230(6) 0.0597(4) 0.3384(3) 0.0621(12) Uani 1 1 d . . . C36 C 0.7936(7) 0.0074(6) 0.3590(5) 0.0941(19) Uani 1 1 d . . . H36A H 0.7149 -0.0422 0.3096 0.113 Uiso 1 1 calc R . . C37 C 0.7828(10) 0.0308(7) 0.4571(6) 0.116(3) Uani 1 1 d . . . H37A H 0.6955 -0.0022 0.4727 0.140 Uiso 1 1 calc R . . C38 C 0.9007(12) 0.1015(7) 0.5280(5) 0.112(3) Uani 1 1 d . . . H38A H 0.8925 0.1173 0.5921 0.134 Uiso 1 1 calc R . . C39 C 1.0302(10) 0.1497(5) 0.5077(4) 0.100(2) Uani 1 1 d . . . H39A H 1.1115 0.1955 0.5579 0.120 Uiso 1 1 calc R . . C40 C 1.0412(7) 0.1305(4) 0.4126(4) 0.0770(15) Uani 1 1 d . . . H40A H 1.1286 0.1654 0.3982 0.092 Uiso 1 1 calc R . . O9 O 0.4299(8) 0.1774(6) 0.5241(5) 0.201(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0475(4) 0.0571(4) 0.0422(3) 0.0118(3) 0.0089(3) 0.0206(3) N1 0.052(2) 0.060(2) 0.0394(17) 0.0157(16) 0.0131(15) 0.0209(17) N2 0.047(2) 0.053(2) 0.0390(17) 0.0093(15) 0.0099(15) 0.0205(16) C1 0.062(3) 0.076(3) 0.040(2) 0.019(2) 0.013(2) 0.029(2) C2 0.076(3) 0.092(4) 0.056(3) 0.037(3) 0.028(3) 0.036(3) C3 0.060(3) 0.082(3) 0.070(3) 0.036(3) 0.027(3) 0.028(3) C4 0.056(3) 0.062(3) 0.053(2) 0.018(2) 0.016(2) 0.026(2) C5 0.049(3) 0.072(3) 0.068(3) 0.020(2) 0.017(2) 0.019(2) C6 0.047(3) 0.071(3) 0.060(3) 0.012(2) 0.005(2) 0.019(2) C7 0.051(2) 0.048(2) 0.050(2) 0.0094(18) 0.0098(19) 0.025(2) C8 0.058(3) 0.062(3) 0.038(2) 0.0032(19) 0.0028(19) 0.027(2) C9 0.068(3) 0.076(3) 0.040(2) 0.013(2) 0.012(2) 0.033(3) C10 0.059(3) 0.062(3) 0.039(2) 0.0097(19) 0.0148(19) 0.025(2) C11 0.047(2) 0.050(2) 0.044(2) 0.0129(18) 0.0119(18) 0.0208(19) C12 0.048(2) 0.049(2) 0.044(2) 0.0101(18) 0.0094(18) 0.0248(19) O1 0.0609(19) 0.0572(18) 0.0559(17) 0.0129(15) 0.0203(15) 0.0255(15) O2 0.0567(19) 0.063(2) 0.0575(18) 0.0157(15) 0.0201(15) 0.0244(15) C13 0.055(3) 0.059(3) 0.048(2) 0.012(2) 0.007(2) 0.017(2) C14 0.053(3) 0.072(3) 0.046(2) 0.012(2) 0.007(2) 0.016(2) O3 0.089(3) 0.080(3) 0.096(3) 0.032(2) 0.047(2) 0.021(2) O4 0.092(3) 0.063(2) 0.097(3) 0.026(2) 0.031(2) 0.034(2) O5 0.0575(19) 0.073(2) 0.0469(16) 0.0166(15) 0.0042(14) 0.0214(16) O6 0.072(2) 0.066(2) 0.0544(18) 0.0122(15) 0.0086(16) 0.0350(17) C15 0.053(3) 0.077(3) 0.071(3) 0.037(3) 0.027(2) 0.027(2) C16 0.053(3) 0.088(4) 0.053(3) 0.032(3) 0.017(2) 0.022(3) O7 0.101(3) 0.084(3) 0.105(3) 0.052(2) 0.038(2) 0.054(2) O8 0.074(2) 0.132(3) 0.070(2) 0.045(2) -0.0013(19) 0.040(2) As1 0.0502(3) 0.0578(3) 0.0512(3) 0.0177(2) 0.01066(19) 0.0213(2) C17 0.056(3) 0.050(2) 0.061(3) 0.019(2) 0.013(2) 0.021(2) C18 0.075(4) 0.084(4) 0.115(5) -0.037(4) -0.023(3) 0.046(3) C19 0.065(4) 0.104(5) 0.141(6) -0.010(4) -0.017(4) 0.049(4) C20 0.084(4) 0.078(4) 0.111(5) 0.031(4) 0.030(4) 0.050(3) C21 0.108(5) 0.077(4) 0.082(4) 0.012(3) 0.025(4) 0.051(4) C22 0.082(4) 0.077(3) 0.055(3) 0.009(2) 0.009(2) 0.038(3) C23 0.052(3) 0.068(3) 0.056(3) 0.019(2) 0.017(2) 0.014(2) C24 0.085(4) 0.086(4) 0.075(4) 0.033(3) 0.017(3) -0.006(3) C25 0.101(5) 0.084(4) 0.088(4) 0.023(3) 0.031(4) -0.020(4) C26 0.054(3) 0.116(5) 0.062(3) -0.008(3) 0.017(3) 0.000(3) C27 0.063(3) 0.099(4) 0.065(3) 0.004(3) 0.004(3) 0.029(3) C28 0.060(3) 0.072(3) 0.061(3) 0.008(2) 0.005(2) 0.027(3) C29 0.049(2) 0.053(2) 0.041(2) 0.0110(18) 0.0090(18) 0.019(2) C30 0.049(2) 0.059(3) 0.045(2) 0.0086(19) 0.0089(19) 0.022(2) C31 0.071(3) 0.061(3) 0.048(2) 0.010(2) 0.009(2) 0.033(2) C32 0.084(4) 0.055(3) 0.047(2) 0.013(2) 0.008(2) 0.022(3) C33 0.068(3) 0.063(3) 0.053(3) 0.015(2) 0.021(2) 0.012(2) C34 0.048(3) 0.064(3) 0.060(3) 0.012(2) 0.017(2) 0.020(2) C35 0.074(3) 0.070(3) 0.063(3) 0.029(2) 0.026(3) 0.042(3) C36 0.089(4) 0.136(6) 0.083(4) 0.049(4) 0.037(3) 0.053(4) C37 0.144(7) 0.150(7) 0.115(6) 0.074(6) 0.076(6) 0.085(6) C38 0.191(9) 0.126(6) 0.076(4) 0.053(5) 0.063(5) 0.104(7) C39 0.169(7) 0.092(4) 0.060(3) 0.025(3) 0.025(4) 0.077(5) C40 0.105(4) 0.072(3) 0.065(3) 0.024(3) 0.020(3) 0.045(3) O9 0.180(6) 0.193(7) 0.155(6) 0.036(5) -0.001(5) -0.017(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 1.964(3) . ? Fe1 O5 1.970(3) . ? Fe1 O6 1.979(3) . ? Fe1 O1 1.987(3) . ? Fe1 N1 2.152(3) . ? Fe1 N2 2.155(3) . ? N1 C1 1.335(5) . ? N1 C11 1.359(5) . ? N2 C10 1.323(5) . ? N2 C12 1.355(5) . ? C1 C2 1.384(6) . ? C2 C3 1.361(7) . ? C3 C4 1.409(6) . ? C4 C11 1.393(6) . ? C4 C5 1.438(6) . ? C5 C6 1.339(6) . ? C6 C7 1.435(6) . ? C7 C12 1.398(6) . ? C7 C8 1.408(6) . ? C8 C9 1.347(6) . ? C9 C10 1.398(6) . ? C11 C12 1.438(5) . ? O1 C13 1.284(5) . ? O2 C14 1.279(6) . ? C13 O4 1.219(5) . ? C13 C14 1.548(7) . ? C14 O3 1.222(6) . ? O5 C16 1.284(6) . ? O6 C15 1.284(5) . ? C15 O7 1.208(5) . ? C15 C16 1.555(7) . ? C16 O8 1.218(5) . ? As1 C35 1.904(5) . ? As1 C23 1.910(5) . ? As1 C29 1.915(4) . ? As1 C17 1.918(4) . ? C17 C18 1.362(7) . ? C17 C22 1.369(6) . ? C18 C19 1.377(7) . ? C19 C20 1.348(8) . ? C20 C21 1.348(8) . ? C21 C22 1.382(7) . ? C23 C28 1.380(6) . ? C23 C24 1.386(7) . ? C24 C25 1.381(8) . ? C25 C26 1.370(9) . ? C26 C27 1.364(8) . ? C27 C28 1.376(7) . ? C29 C34 1.383(6) . ? C29 C30 1.386(6) . ? C30 C31 1.367(6) . ? C31 C32 1.381(7) . ? C32 C33 1.381(7) . ? C33 C34 1.375(6) . ? C35 C36 1.375(7) . ? C35 C40 1.379(7) . ? C36 C37 1.417(9) . ? C37 C38 1.355(11) . ? C38 C39 1.355(10) . ? C39 C40 1.375(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Fe1 O5 101.25(13) . . ? O2 Fe1 O6 98.88(14) . . ? O5 Fe1 O6 81.80(13) . . ? O2 Fe1 O1 81.51(13) . . ? O5 Fe1 O1 97.18(13) . . ? O6 Fe1 O1 178.95(12) . . ? O2 Fe1 N1 163.10(13) . . ? O5 Fe1 N1 92.16(13) . . ? O6 Fe1 N1 93.12(14) . . ? O1 Fe1 N1 86.70(13) . . ? O2 Fe1 N2 92.18(13) . . ? O5 Fe1 N2 163.75(13) . . ? O6 Fe1 N2 87.16(13) . . ? O1 Fe1 N2 93.80(13) . . ? N1 Fe1 N2 76.51(13) . . ? C1 N1 C11 117.7(4) . . ? C1 N1 Fe1 127.4(3) . . ? C11 N1 Fe1 114.9(3) . . ? C10 N2 C12 118.7(3) . . ? C10 N2 Fe1 126.6(3) . . ? C12 N2 Fe1 114.7(2) . . ? N1 C1 C2 122.3(4) . . ? C3 C2 C1 120.5(4) . . ? C2 C3 C4 119.0(4) . . ? C11 C4 C3 117.2(4) . . ? C11 C4 C5 118.9(4) . . ? C3 C4 C5 123.8(4) . . ? C6 C5 C4 121.0(4) . . ? C5 C6 C7 121.6(4) . . ? C12 C7 C8 116.7(4) . . ? C12 C7 C6 118.5(4) . . ? C8 C7 C6 124.7(4) . . ? C9 C8 C7 119.9(4) . . ? C8 C9 C10 120.0(4) . . ? N2 C10 C9 121.8(4) . . ? N1 C11 C4 123.4(4) . . ? N1 C11 C12 116.7(4) . . ? C4 C11 C12 119.9(4) . . ? N2 C12 C7 122.8(4) . . ? N2 C12 C11 117.1(3) . . ? C7 C12 C11 120.0(4) . . ? C13 O1 Fe1 115.1(3) . . ? C14 O2 Fe1 115.8(3) . . ? O4 C13 O1 124.4(4) . . ? O4 C13 C14 122.0(4) . . ? O1 C13 C14 113.6(4) . . ? O3 C14 O2 125.4(5) . . ? O3 C14 C13 120.7(5) . . ? O2 C14 C13 113.9(4) . . ? C16 O5 Fe1 115.1(3) . . ? C15 O6 Fe1 115.4(3) . . ? O7 C15 O6 125.5(5) . . ? O7 C15 C16 121.5(5) . . ? O6 C15 C16 113.0(4) . . ? O8 C16 O5 125.9(5) . . ? O8 C16 C15 120.2(5) . . ? O5 C16 C15 113.9(4) . . ? C35 As1 C23 111.9(2) . . ? C35 As1 C29 108.20(19) . . ? C23 As1 C29 108.72(19) . . ? C35 As1 C17 110.46(19) . . ? C23 As1 C17 107.4(2) . . ? C29 As1 C17 110.09(18) . . ? C18 C17 C22 119.8(5) . . ? C18 C17 As1 120.5(4) . . ? C22 C17 As1 119.7(4) . . ? C17 C18 C19 119.5(5) . . ? C20 C19 C18 121.4(6) . . ? C21 C20 C19 118.8(5) . . ? C20 C21 C22 121.5(5) . . ? C17 C22 C21 118.9(5) . . ? C28 C23 C24 120.1(5) . . ? C28 C23 As1 119.8(4) . . ? C24 C23 As1 119.9(4) . . ? C25 C24 C23 119.1(6) . . ? C26 C25 C24 119.9(6) . . ? C27 C26 C25 121.4(5) . . ? C26 C27 C28 119.2(6) . . ? C27 C28 C23 120.3(5) . . ? C34 C29 C30 120.9(4) . . ? C34 C29 As1 120.5(3) . . ? C30 C29 As1 118.6(3) . . ? C31 C30 C29 119.3(4) . . ? C30 C31 C32 120.4(4) . . ? C33 C32 C31 120.1(4) . . ? C34 C33 C32 120.2(5) . . ? C33 C34 C29 119.1(4) . . ? C36 C35 C40 120.4(5) . . ? C36 C35 As1 121.4(4) . . ? C40 C35 As1 118.2(4) . . ? C35 C36 C37 118.5(7) . . ? C38 C37 C36 119.5(7) . . ? C37 C38 C39 121.6(7) . . ? C38 C39 C40 119.8(7) . . ? C39 C40 C35 120.1(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.644 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.069 #==END data_5 _database_code_depnum_ccdc_archive 'CCDC 255486' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H38 Fe2 N6 Na O19' _chemical_formula_weight 1065.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.436(2) _cell_length_b 29.919(6) _cell_length_c 14.882(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.47(3) _cell_angle_gamma 90.00 _cell_volume 4583.4(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.46 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2188 _exptl_absorpt_coefficient_mu 0.728 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.6611 _exptl_absorpt_correction_T_max 0.7307 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'R3m/V automatic four-circle diffractometer' _diffrn_measurement_method omega/2-theta-scans _diffrn_standards_decay_% 2.0 _diffrn_reflns_number 8572 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.1057 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.02 _reflns_number_total 8102 _reflns_number_gt 4335 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (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^)+(0.1508P)^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 8102 _refine_ls_number_parameters 622 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1441 _refine_ls_R_factor_gt 0.0794 _refine_ls_wR_factor_ref 0.2587 _refine_ls_wR_factor_gt 0.2155 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _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 0.15966(11) 0.87539(4) 0.30531(8) 0.0434(3) Uani 1 1 d . . . O1 O 0.1293(6) 0.89785(18) 0.1765(4) 0.0518(15) Uani 1 1 d . . . O2 O 0.1012(5) 0.81879(17) 0.2392(4) 0.0459(14) Uani 1 1 d . . . C1 C 0.0912(8) 0.8693(3) 0.1143(6) 0.051(2) Uani 1 1 d . . . C2 C 0.0722(7) 0.8213(3) 0.1512(6) 0.0431(19) Uani 1 1 d . . . O3 O 0.0353(6) 0.7907(2) 0.1011(4) 0.0622(17) Uani 1 1 d . . . O4 O 0.0685(7) 0.8764(2) 0.0321(4) 0.080(2) Uani 1 1 d . . . O5 O 0.2402(5) 0.93485(19) 0.3530(4) 0.0577(16) Uani 1 1 d . . . O6 O 0.3480(6) 0.8605(2) 0.3183(4) 0.0564(15) Uani 1 1 d . . . C3 C 0.3643(9) 0.9350(3) 0.3682(6) 0.054(2) Uani 1 1 d . . . C4 C 0.4277(8) 0.8900(3) 0.3480(6) 0.051(2) Uani 1 1 d . . . O7 O 0.5461(6) 0.8854(3) 0.3636(5) 0.079(2) Uani 1 1 d . . . O8 O 0.4338(7) 0.9673(3) 0.3925(6) 0.093(2) Uani 1 1 d . . . O9 O -0.0121(5) 0.8995(2) 0.3291(4) 0.0492(14) Uani 1 1 d . . . O10 O 0.1488(6) 0.8456(2) 0.4253(4) 0.0554(16) Uani 1 1 d . . . C5 C -0.0467(8) 0.8876(3) 0.4042(6) 0.052(2) Uani 1 1 d . . . C6 C 0.0478(9) 0.8538(3) 0.4595(6) 0.055(2) Uani 1 1 d . . . O11 O 0.0231(8) 0.8393(3) 0.5308(5) 0.093(3) Uani 1 1 d . . . O12 O -0.1458(6) 0.8998(3) 0.4329(5) 0.088(2) Uani 1 1 d . . . Na1 Na 0.6734(5) 0.9479(2) 0.4274(4) 0.121(2) Uani 1 1 d . . . Fe2 Fe 0.57587(10) 0.64016(3) 0.38353(6) 0.0287(3) Uani 1 1 d . . . N1 N 0.6876(6) 0.58938(18) 0.3612(4) 0.0310(13) Uani 1 1 d . . . N2 N 0.4513(6) 0.59152(19) 0.3988(4) 0.0326(14) Uani 1 1 d . . . C7 C 0.8103(7) 0.5890(3) 0.3437(5) 0.0400(18) Uani 1 1 d . . . H7A H 0.8547 0.6159 0.3434 0.048 Uiso 1 1 calc R . . C8 C 0.8734(8) 0.5492(3) 0.3259(6) 0.053(2) Uani 1 1 d . . . H8A H 0.9578 0.5503 0.3135 0.063 Uiso 1 1 calc R . . C9 C 0.8135(9) 0.5095(3) 0.3265(6) 0.054(2) Uani 1 1 d . . . H9A H 0.8556 0.4833 0.3149 0.065 Uiso 1 1 calc R . . C10 C 0.6844(9) 0.5084(2) 0.3453(6) 0.047(2) Uani 1 1 d . . . C11 C 0.6112(10) 0.4675(3) 0.3497(6) 0.057(2) Uani 1 1 d . . . H11A H 0.6484 0.4401 0.3395 0.068 Uiso 1 1 calc R . . C12 C 0.4877(10) 0.4693(3) 0.3688(6) 0.059(2) Uani 1 1 d . . . H12A H 0.4415 0.4427 0.3694 0.071 Uiso 1 1 calc R . . C13 C 0.4267(8) 0.5099(3) 0.3878(5) 0.044(2) Uani 1 1 d . . . C14 C 0.3019(8) 0.5144(3) 0.4090(6) 0.054(2) Uani 1 1 d . . . H14A H 0.2502 0.4892 0.4107 0.064 Uiso 1 1 calc R . . C15 C 0.2551(8) 0.5554(3) 0.4273(6) 0.051(2) Uani 1 1 d . . . H15A H 0.1728 0.5581 0.4430 0.062 Uiso 1 1 calc R . . C16 C 0.3322(7) 0.5935(3) 0.4222(5) 0.0435(19) Uani 1 1 d . . . H16A H 0.2996 0.6212 0.4355 0.052 Uiso 1 1 calc R . . C17 C 0.4974(7) 0.5504(2) 0.3836(5) 0.0351(17) Uani 1 1 d . . . C18 C 0.6270(7) 0.5490(2) 0.3622(5) 0.0369(17) Uani 1 1 d . . . N3 N 0.6372(5) 0.6412(2) 0.5158(4) 0.0307(13) Uani 1 1 d . . . N4 N 0.4552(5) 0.68692(18) 0.4146(4) 0.0298(13) Uani 1 1 d . . . C19 C 0.7370(7) 0.6199(3) 0.5654(5) 0.0397(18) Uani 1 1 d . . . H19A H 0.7902 0.6023 0.5355 0.048 Uiso 1 1 calc R . . C20 C 0.7652(8) 0.6230(3) 0.6610(5) 0.0435(19) Uani 1 1 d . . . H20A H 0.8355 0.6075 0.6931 0.052 Uiso 1 1 calc R . . C21 C 0.6895(8) 0.6486(3) 0.7059(5) 0.047(2) Uani 1 1 d . . . H21A H 0.7069 0.6505 0.7691 0.056 Uiso 1 1 calc R . . C22 C 0.5838(7) 0.6726(3) 0.6567(5) 0.0376(18) Uani 1 1 d . . . C23 C 0.4972(8) 0.7014(3) 0.6965(5) 0.050(2) Uani 1 1 d . . . H23A H 0.5081 0.7045 0.7595 0.060 Uiso 1 1 calc R . . C24 C 0.4004(8) 0.7241(3) 0.6438(5) 0.051(2) Uani 1 1 d . . . H24A H 0.3441 0.7417 0.6712 0.061 Uiso 1 1 calc R . . C25 C 0.3837(7) 0.7213(3) 0.5462(5) 0.0395(18) Uani 1 1 d . . . C26 C 0.2910(8) 0.7464(3) 0.4863(6) 0.048(2) Uani 1 1 d . . . H26A H 0.2353 0.7661 0.5091 0.058 Uiso 1 1 calc R . . C27 C 0.2851(8) 0.7412(3) 0.3948(6) 0.047(2) Uani 1 1 d . . . H27A H 0.2256 0.7578 0.3546 0.057 Uiso 1 1 calc R . . C28 C 0.3676(7) 0.7114(3) 0.3611(5) 0.0392(18) Uani 1 1 d . . . H28A H 0.3611 0.7083 0.2983 0.047 Uiso 1 1 calc R . . C29 C 0.4644(7) 0.6925(2) 0.5062(4) 0.0313(16) Uani 1 1 d . . . C30 C 0.5638(6) 0.6680(2) 0.5614(4) 0.0271(15) Uani 1 1 d . . . N5 N 0.7041(5) 0.68507(18) 0.3582(4) 0.0286(13) Uani 1 1 d . . . N6 N 0.5159(6) 0.6451(2) 0.2503(4) 0.0355(14) Uani 1 1 d . . . C31 C 0.7970(7) 0.7068(2) 0.4144(5) 0.0395(18) Uani 1 1 d . . . H31A H 0.8050 0.7010 0.4765 0.047 Uiso 1 1 calc R . . C32 C 0.8811(8) 0.7369(3) 0.3861(6) 0.049(2) Uani 1 1 d . . . H32A H 0.9438 0.7510 0.4284 0.059 Uiso 1 1 calc R . . C33 C 0.8719(8) 0.7463(3) 0.2946(6) 0.052(2) Uani 1 1 d . . . H33A H 0.9272 0.7671 0.2746 0.063 Uiso 1 1 calc R . . C34 C 0.7780(8) 0.7241(3) 0.2319(5) 0.0434(19) Uani 1 1 d . . . C35 C 0.7591(10) 0.7298(3) 0.1343(6) 0.062(3) Uani 1 1 d . . . H35A H 0.8154 0.7484 0.1093 0.074 Uiso 1 1 calc R . . C36 C 0.6642(10) 0.7094(3) 0.0790(5) 0.058(2) Uani 1 1 d . . . H36A H 0.6550 0.7140 0.0165 0.069 Uiso 1 1 calc R . . C37 C 0.5747(9) 0.6800(3) 0.1150(5) 0.051(2) Uani 1 1 d . . . C38 C 0.4689(10) 0.6591(3) 0.0616(6) 0.060(2) Uani 1 1 d . . . H38A H 0.4530 0.6632 -0.0012 0.072 Uiso 1 1 calc R . . C39 C 0.3889(9) 0.6324(3) 0.1028(6) 0.058(2) Uani 1 1 d . . . H39A H 0.3173 0.6187 0.0682 0.070 Uiso 1 1 calc R . . C40 C 0.4155(8) 0.6257(3) 0.1979(5) 0.048(2) Uani 1 1 d . . . H40A H 0.3612 0.6071 0.2249 0.057 Uiso 1 1 calc R . . C41 C 0.5931(7) 0.6720(2) 0.2094(5) 0.0353(17) Uani 1 1 d . . . C42 C 0.6956(7) 0.6943(2) 0.2671(5) 0.0332(16) Uani 1 1 d . . . O13 O 0.6565(12) 0.9423(5) 0.5844(9) 0.174(5) Uiso 1 1 d . . . O14 O 0.812(2) 0.9792(8) 0.2926(16) 0.333(12) Uiso 1 1 d . . . O15 O 0.863(2) 1.0110(8) 0.5191(16) 0.338(12) Uiso 1 1 d . . . O16 O 0.1339(7) 0.7074(2) 0.1849(4) 0.0709(19) Uani 1 1 d D . . H7W H 0.126(8) 0.6901(18) 0.130(3) 0.060 Uiso 1 1 d D . . H8W H 0.109(8) 0.7362(11) 0.159(4) 0.060 Uiso 1 1 d D . . O17 O 0.0665(10) 0.6463(3) 0.3204(8) 0.132(4) Uani 1 1 d D . . H9W H 0.073(10) 0.6293(19) 0.266(3) 0.060 Uiso 1 1 d D . . H10W H 0.080(8) 0.6755(10) 0.297(4) 0.060 Uiso 1 1 d D . . O18 O 0.8735(11) 0.8882(4) 0.6401(8) 0.146(4) Uiso 1 1 d . . . O20 O 0.130(2) 0.9375(8) 0.6751(16) 0.155(8) Uiso 0.50 1 d P . . O19 O -0.0449(17) 0.9641(6) 0.0495(11) 0.102(5) Uiso 0.50 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 0.0410(7) 0.0417(7) 0.0468(7) -0.0002(5) 0.0056(5) 0.0009(5) O1 0.066(4) 0.036(3) 0.054(4) 0.006(3) 0.010(3) -0.011(3) O2 0.053(3) 0.037(3) 0.048(3) 0.005(2) 0.012(3) -0.011(3) C1 0.048(5) 0.062(6) 0.045(5) 0.011(4) 0.009(4) -0.008(4) C2 0.034(4) 0.046(5) 0.050(5) 0.002(4) 0.011(4) -0.005(4) O3 0.072(4) 0.050(4) 0.062(4) -0.013(3) 0.005(3) -0.014(3) O4 0.102(6) 0.085(5) 0.050(4) 0.019(4) 0.001(4) -0.020(4) O5 0.039(3) 0.049(4) 0.082(5) -0.011(3) 0.001(3) 0.004(3) O6 0.048(4) 0.048(4) 0.075(4) -0.002(3) 0.014(3) 0.004(3) C3 0.053(6) 0.061(6) 0.047(5) -0.009(4) 0.002(4) -0.006(5) C4 0.033(5) 0.073(6) 0.050(5) 0.005(4) 0.012(4) 0.010(4) O7 0.045(4) 0.105(6) 0.089(5) -0.009(4) 0.020(3) 0.000(4) O8 0.066(5) 0.091(6) 0.118(7) -0.035(5) 0.005(4) -0.009(4) O9 0.038(3) 0.066(4) 0.042(3) 0.006(3) 0.000(2) 0.014(3) O10 0.058(4) 0.063(4) 0.045(3) 0.011(3) 0.008(3) 0.022(3) C5 0.037(5) 0.062(6) 0.052(5) -0.008(4) -0.006(4) -0.001(4) C6 0.065(6) 0.059(6) 0.040(5) 0.006(4) 0.007(4) 0.009(5) O11 0.103(6) 0.113(7) 0.071(5) 0.037(5) 0.036(4) 0.031(5) O12 0.043(4) 0.139(7) 0.085(5) 0.010(5) 0.021(4) 0.030(4) Na1 0.062(3) 0.131(5) 0.165(5) -0.025(4) 0.003(3) 0.019(3) Fe2 0.0316(5) 0.0275(5) 0.0274(5) 0.0006(4) 0.0057(4) -0.0024(4) N1 0.036(3) 0.025(3) 0.032(3) -0.005(2) 0.006(3) -0.003(3) N2 0.033(3) 0.034(4) 0.031(3) 0.002(3) 0.004(3) -0.003(3) C7 0.043(5) 0.033(4) 0.047(5) 0.000(3) 0.016(4) 0.001(3) C8 0.044(5) 0.055(6) 0.065(6) 0.000(4) 0.029(4) 0.006(4) C9 0.063(6) 0.032(5) 0.074(6) -0.012(4) 0.032(5) 0.009(4) C10 0.063(6) 0.024(4) 0.054(5) -0.009(4) 0.011(4) -0.004(4) C11 0.078(7) 0.035(5) 0.060(6) -0.008(4) 0.018(5) -0.007(5) C12 0.078(7) 0.033(5) 0.066(6) -0.005(4) 0.012(5) -0.019(5) C13 0.050(5) 0.043(5) 0.040(4) -0.001(4) 0.010(4) -0.018(4) C14 0.051(5) 0.048(6) 0.064(6) -0.006(4) 0.016(4) -0.023(4) C15 0.048(5) 0.055(6) 0.051(5) 0.001(4) 0.009(4) -0.013(4) C16 0.039(5) 0.041(5) 0.051(5) -0.004(4) 0.012(4) -0.010(4) C17 0.036(4) 0.041(5) 0.027(4) -0.001(3) 0.002(3) -0.006(3) C18 0.043(4) 0.040(5) 0.028(4) -0.002(3) 0.008(3) -0.001(4) N3 0.027(3) 0.039(3) 0.026(3) 0.008(3) 0.003(2) -0.004(3) N4 0.033(3) 0.028(3) 0.028(3) 0.003(2) 0.004(3) -0.003(3) C19 0.033(4) 0.044(5) 0.042(4) 0.009(4) 0.005(3) -0.008(3) C20 0.040(4) 0.047(5) 0.039(4) 0.016(4) -0.006(4) -0.008(4) C21 0.055(5) 0.055(5) 0.029(4) 0.001(4) 0.004(4) -0.015(4) C22 0.044(4) 0.041(4) 0.028(4) 0.002(3) 0.005(3) -0.012(4) C23 0.062(6) 0.064(6) 0.028(4) -0.009(4) 0.017(4) -0.009(5) C24 0.055(5) 0.068(6) 0.031(4) -0.015(4) 0.014(4) -0.001(5) C25 0.032(4) 0.044(5) 0.044(4) -0.008(4) 0.010(3) -0.009(3) C26 0.045(5) 0.044(5) 0.056(5) -0.009(4) 0.009(4) 0.008(4) C27 0.045(5) 0.043(5) 0.050(5) 0.004(4) -0.002(4) 0.007(4) C28 0.034(4) 0.049(5) 0.035(4) 0.010(3) 0.008(3) 0.005(4) C29 0.035(4) 0.034(4) 0.026(4) -0.003(3) 0.008(3) -0.007(3) C30 0.029(4) 0.029(4) 0.024(3) -0.001(3) 0.006(3) -0.006(3) N5 0.031(3) 0.027(3) 0.027(3) 0.004(2) 0.003(2) -0.004(2) N6 0.038(3) 0.039(4) 0.028(3) -0.002(3) 0.004(3) 0.001(3) C31 0.047(5) 0.035(4) 0.038(4) -0.005(3) 0.011(4) -0.007(4) C32 0.055(5) 0.037(5) 0.059(6) -0.002(4) 0.019(4) -0.014(4) C33 0.051(5) 0.042(5) 0.068(6) 0.012(4) 0.019(5) -0.003(4) C34 0.047(5) 0.041(5) 0.044(5) 0.008(4) 0.015(4) 0.005(4) C35 0.075(7) 0.066(6) 0.052(6) 0.026(5) 0.036(5) 0.008(5) C36 0.085(7) 0.066(6) 0.027(4) 0.018(4) 0.021(5) 0.007(5) C37 0.061(6) 0.061(6) 0.031(4) 0.004(4) 0.006(4) 0.023(5) C38 0.076(7) 0.070(6) 0.031(4) -0.002(4) 0.003(4) 0.009(5) C39 0.065(6) 0.061(6) 0.043(5) -0.011(4) -0.009(4) -0.006(5) C40 0.052(5) 0.055(5) 0.035(4) -0.005(4) 0.002(4) -0.002(4) C41 0.044(4) 0.035(4) 0.030(4) 0.002(3) 0.016(3) 0.008(3) C42 0.034(4) 0.032(4) 0.034(4) 0.005(3) 0.008(3) 0.008(3) O16 0.073(5) 0.061(4) 0.074(5) -0.006(3) -0.003(4) -0.002(4) O17 0.091(7) 0.080(7) 0.222(13) 0.022(7) 0.015(8) -0.018(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 O6 1.993(6) . ? Fe1 O2 2.002(5) . ? Fe1 O1 2.006(6) . ? Fe1 O10 2.016(6) . ? Fe1 O9 2.017(5) . ? Fe1 O5 2.044(6) . ? O1 C1 1.274(10) . ? O2 C2 1.297(9) . ? C1 O4 1.226(10) . ? C1 C2 1.561(11) . ? C2 O3 1.203(9) . ? O5 C3 1.278(10) . ? O6 C4 1.244(10) . ? C3 O8 1.226(11) . ? C3 C4 1.551(13) . ? C4 O7 1.227(10) . ? O7 Na1 2.397(9) . ? O8 Na1 2.537(9) . ? O9 C5 1.281(10) . ? O10 C6 1.267(10) . ? C5 O12 1.236(10) . ? C5 C6 1.553(12) . ? C6 O11 1.213(10) . ? O12 Na1 2.363(8) 1_455 ? Na1 O12 2.363(8) 1_655 ? Na1 O13 2.377(14) . ? Na1 O14 2.82(2) . ? Na1 O15 2.91(2) . ? Fe2 N3 1.968(5) . ? Fe2 N5 1.976(5) . ? Fe2 N1 1.977(6) . ? Fe2 N6 1.984(6) . ? Fe2 N4 1.987(6) . ? Fe2 N2 1.989(6) . ? N1 C7 1.348(9) . ? N1 C18 1.364(9) . ? N2 C16 1.346(9) . ? N2 C17 1.354(9) . ? C7 C8 1.408(11) . ? C8 C9 1.341(12) . ? C9 C10 1.421(12) . ? C10 C18 1.395(10) . ? C10 C11 1.449(11) . ? C11 C12 1.366(13) . ? C12 C13 1.423(12) . ? C13 C14 1.397(11) . ? C13 C17 1.424(10) . ? C14 C15 1.363(12) . ? C15 C16 1.405(11) . ? C17 C18 1.440(10) . ? N3 C19 1.334(9) . ? N3 C30 1.366(8) . ? N4 C28 1.329(9) . ? N4 C29 1.362(8) . ? C19 C20 1.408(10) . ? C20 C21 1.355(11) . ? C21 C22 1.414(11) . ? C22 C30 1.406(9) . ? C22 C23 1.445(11) . ? C23 C24 1.355(12) . ? C24 C25 1.437(10) . ? C25 C29 1.404(10) . ? C25 C26 1.418(11) . ? C26 C27 1.362(11) . ? C27 C28 1.391(11) . ? C29 C30 1.417(10) . ? N5 C31 1.340(9) . ? N5 C42 1.371(8) . ? N6 C40 1.332(10) . ? N6 C41 1.352(9) . ? C31 C32 1.373(10) . ? C32 C33 1.378(11) . ? C33 C34 1.405(12) . ? C34 C42 1.399(10) . ? C34 C35 1.444(11) . ? C35 C36 1.328(13) . ? C36 C37 1.448(12) . ? C37 C38 1.397(12) . ? C37 C41 1.407(10) . ? C38 C39 1.373(13) . ? C39 C40 1.411(11) . ? C41 C42 1.422(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Fe1 O2 94.3(2) . . ? O6 Fe1 O1 99.5(2) . . ? O2 Fe1 O1 80.0(2) . . ? O6 Fe1 O10 90.8(2) . . ? O2 Fe1 O10 90.2(2) . . ? O1 Fe1 O10 166.2(3) . . ? O6 Fe1 O9 162.4(2) . . ? O2 Fe1 O9 100.5(2) . . ? O1 Fe1 O9 92.4(2) . . ? O10 Fe1 O9 79.7(2) . . ? O6 Fe1 O5 79.5(2) . . ? O2 Fe1 O5 168.8(2) . . ? O1 Fe1 O5 91.8(2) . . ? O10 Fe1 O5 99.1(3) . . ? O9 Fe1 O5 87.3(2) . . ? C1 O1 Fe1 116.8(5) . . ? C2 O2 Fe1 116.6(5) . . ? O4 C1 O1 126.6(8) . . ? O4 C1 C2 119.6(8) . . ? O1 C1 C2 113.8(7) . . ? O3 C2 O2 125.4(8) . . ? O3 C2 C1 121.9(8) . . ? O2 C2 C1 112.8(7) . . ? C3 O5 Fe1 114.3(6) . . ? C4 O6 Fe1 117.8(5) . . ? O8 C3 O5 126.0(9) . . ? O8 C3 C4 119.4(8) . . ? O5 C3 C4 114.4(8) . . ? O7 C4 O6 125.5(9) . . ? O7 C4 C3 120.6(9) . . ? O6 C4 C3 113.8(7) . . ? C4 O7 Na1 117.6(7) . . ? C3 O8 Na1 113.2(7) . . ? C5 O9 Fe1 116.1(5) . . ? C6 O10 Fe1 116.2(5) . . ? O12 C5 O9 126.2(8) . . ? O12 C5 C6 120.3(9) . . ? O9 C5 C6 113.4(7) . . ? O11 C6 O10 126.4(9) . . ? O11 C6 C5 119.2(9) . . ? O10 C6 C5 114.3(7) . . ? C5 O12 Na1 151.1(7) . 1_455 ? O12 Na1 O13 96.4(4) 1_655 . ? O12 Na1 O7 85.8(3) 1_655 . ? O13 Na1 O7 102.1(4) . . ? O12 Na1 O8 154.3(4) 1_655 . ? O13 Na1 O8 89.3(4) . . ? O7 Na1 O8 68.5(3) . . ? O12 Na1 O14 74.1(5) 1_655 . ? O13 Na1 O14 148.4(6) . . ? O7 Na1 O14 107.0(6) . . ? O8 Na1 O14 112.5(6) . . ? O12 Na1 O15 84.4(5) 1_655 . ? O13 Na1 O15 74.9(6) . . ? O7 Na1 O15 169.3(6) . . ? O8 Na1 O15 121.2(5) . . ? O14 Na1 O15 74.3(7) . . ? N3 Fe2 N5 93.5(2) . . ? N3 Fe2 N1 94.4(2) . . ? N5 Fe2 N1 93.1(2) . . ? N3 Fe2 N6 174.9(2) . . ? N5 Fe2 N6 82.6(2) . . ? N1 Fe2 N6 89.2(2) . . ? N3 Fe2 N4 82.6(2) . . ? N5 Fe2 N4 92.3(2) . . ? N1 Fe2 N4 173.9(2) . . ? N6 Fe2 N4 94.2(2) . . ? N3 Fe2 N2 90.4(2) . . ? N5 Fe2 N2 174.4(2) . . ? N1 Fe2 N2 82.6(2) . . ? N6 Fe2 N2 93.7(2) . . ? N4 Fe2 N2 92.1(2) . . ? C7 N1 C18 116.8(6) . . ? C7 N1 Fe2 130.1(5) . . ? C18 N1 Fe2 113.0(5) . . ? C16 N2 C17 116.9(6) . . ? C16 N2 Fe2 130.3(5) . . ? C17 N2 Fe2 112.9(5) . . ? N1 C7 C8 122.1(7) . . ? C9 C8 C7 121.0(8) . . ? C8 C9 C10 118.7(7) . . ? C18 C10 C9 117.7(7) . . ? C18 C10 C11 118.8(8) . . ? C9 C10 C11 123.5(8) . . ? C12 C11 C10 120.0(8) . . ? C11 C12 C13 122.8(8) . . ? C14 C13 C12 126.3(8) . . ? C14 C13 C17 115.9(8) . . ? C12 C13 C17 117.8(7) . . ? C15 C14 C13 120.6(8) . . ? C14 C15 C16 119.5(8) . . ? N2 C16 C15 122.7(8) . . ? N2 C17 C13 124.3(7) . . ? N2 C17 C18 115.8(6) . . ? C13 C17 C18 119.8(7) . . ? N1 C18 C10 123.7(7) . . ? N1 C18 C17 115.5(6) . . ? C10 C18 C17 120.7(7) . . ? C19 N3 C30 117.1(6) . . ? C19 N3 Fe2 129.9(5) . . ? C30 N3 Fe2 112.9(4) . . ? C28 N4 C29 117.4(6) . . ? C28 N4 Fe2 130.4(5) . . ? C29 N4 Fe2 112.1(4) . . ? N3 C19 C20 122.9(7) . . ? C21 C20 C19 119.5(7) . . ? C20 C21 C22 120.0(7) . . ? C30 C22 C21 116.5(7) . . ? C30 C22 C23 118.2(7) . . ? C21 C22 C23 125.3(7) . . ? C24 C23 C22 121.3(7) . . ? C23 C24 C25 120.7(8) . . ? C29 C25 C26 117.0(7) . . ? C29 C25 C24 118.9(7) . . ? C26 C25 C24 124.2(7) . . ? C27 C26 C25 118.8(7) . . ? C26 C27 C28 120.3(7) . . ? N4 C28 C27 122.9(7) . . ? N4 C29 C25 123.5(7) . . ? N4 C29 C30 116.2(6) . . ? C25 C29 C30 120.3(6) . . ? N3 C30 C22 123.8(6) . . ? N3 C30 C29 115.7(6) . . ? C22 C30 C29 120.5(6) . . ? C31 N5 C42 116.3(6) . . ? C31 N5 Fe2 130.8(5) . . ? C42 N5 Fe2 112.9(4) . . ? C40 N6 C41 117.8(6) . . ? C40 N6 Fe2 129.8(5) . . ? C41 N6 Fe2 112.4(5) . . ? N5 C31 C32 124.0(7) . . ? C31 C32 C33 119.6(8) . . ? C32 C33 C34 119.2(8) . . ? C42 C34 C33 117.2(7) . . ? C42 C34 C35 117.5(8) . . ? C33 C34 C35 125.2(8) . . ? C36 C35 C34 122.2(8) . . ? C35 C36 C37 120.7(7) . . ? C38 C37 C41 117.2(8) . . ? C38 C37 C36 124.0(8) . . ? C41 C37 C36 118.8(8) . . ? C39 C38 C37 119.2(8) . . ? C38 C39 C40 119.9(8) . . ? N6 C40 C39 122.0(8) . . ? N6 C41 C37 123.8(7) . . ? N6 C41 C42 116.8(6) . . ? C37 C41 C42 119.3(7) . . ? N5 C42 C34 123.7(7) . . ? N5 C42 C41 115.0(6) . . ? C34 C42 C41 121.3(6) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O17 H10W O16 0.963(10) 2.07(4) 2.894(12) 142(5) . O17 H9W O18 0.971(10) 2.62(9) 3.248(16) 123(7) 4_475 O17 H9W O20 0.971(10) 2.54(4) 3.45(3) 156(7) 4_575 O16 H8W O3 0.962(10) 1.945(18) 2.900(9) 172(7) . O16 H7W O11 0.958(10) 1.89(4) 2.770(9) 151(7) 4_575 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.379 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.116 #==END