Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Roland Meier' _publ_contact_author_address ; Institut fur Anorganische Chemie Universitat Erlangen-Nurnberg Egerlandstrasse 1 Erlangen Bavaria D-91058 GERMANY ; _publ_contact_author_email ROLAND.MEIER@CHEMIE.UNI-ERLANGEN.DE _publ_section_title ; Structure of sodium bis(N-methyl-iminodiacetato)iron(III). Trans-meridional N-coordination in the solid state and in solution ; loop_ _publ_author_name 'Roland Meier' 'Christopher E. Anson' 'Bernd Kallies' 'Michel Molinier' 'Annie K. Powell' 'R.Van Eldik' # Attachment 'B605056E_Na[Fe(mida)2]x3H2Ox2NaClO4_rev.CIF' data_mida _database_code_depnum_ccdc_archive 'CCDC 180651' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Trisodium [bis(N-methyl-iminodiacetate)iron(III)] diperchlorate trihydrate ; _chemical_name_common ;Trisodium (bis(N-methyl-iminodiacetate)iron(iii)) diperchlorate trihydrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H20 Cl2 Fe N2 Na3 O19' _chemical_formula_weight 668.00 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2324(14) _cell_length_b 11.9903(10) _cell_length_c 9.9676(18) _cell_angle_alpha 96.561(10) _cell_angle_beta 96.066(14) _cell_angle_gamma 91.311(9) _cell_volume 1207.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 24.66 _cell_measurement_theta_max 24.95 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.837 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 678 _exptl_absorpt_coefficient_mu 0.990 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.9231 _exptl_absorpt_correction_T_max 0.9998 _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 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 7369 _diffrn_reflns_av_R_equivalents 0.0090 _diffrn_reflns_av_sigmaI/netI 0.0185 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 30.00 _reflns_number_total 7009 _reflns_number_gt 6154 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'AFC7R Control Software (MSC, 1994)' _computing_cell_refinement 'AFC7R Control Software (MSC, 1994)' _computing_data_reduction 'TEXSAN 1.6 (MSC, 1996)' _computing_structure_solution 'XS: SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_structure_refinement 'XL: SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_molecular_graphics 'XP: SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_publication_material 'XCIF: SHELXTL 5.1 (Bruker AXS Inc., 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. The methyl hydrogens (on C(5) and C(10)) were constrained to tetrahedral geometry, with the torsion angle and common C-H distance for each methyl allowed to refine. O-H bond distances were restrained to 0.86(4) \%A. All other hydrogens were freely refined. All H-atoms were refined with independent isotropic temperature factors. ; _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^)+(0.0573P)^2^+0.8243P] 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 SHELXL _refine_ls_extinction_coef 0.0042(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7009 _refine_ls_number_parameters 444 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.1107 _refine_ls_wR_factor_gt 0.1063 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.23900(2) 0.127082(19) 0.21993(2) 0.02192(8) Uani 1 1 d . . . N1 N 0.22995(15) 0.30570(12) 0.21508(16) 0.0256(3) Uani 1 1 d . . . C1 C 0.0974(2) 0.32487(17) 0.1500(2) 0.0352(4) Uani 1 1 d . . . H1A H 0.098(3) 0.305(3) 0.043(3) 0.057(9) Uiso 1 1 d . . . H1B H 0.075(3) 0.400(3) 0.173(3) 0.048(8) Uiso 1 1 d . . . C2 C 0.00007(18) 0.24297(16) 0.1973(2) 0.0314(4) Uani 1 1 d . . . O1 O 0.04872(13) 0.14900(11) 0.22456(16) 0.0327(3) Uani 1 1 d . . . O2 O -0.11548(15) 0.26414(14) 0.2041(2) 0.0462(4) Uani 1 1 d . . . C3 C 0.34044(19) 0.33550(16) 0.1403(2) 0.0334(4) Uani 1 1 d . . . H3A H 0.367(3) 0.415(3) 0.160(3) 0.050(8) Uiso 1 1 d . . . H3B H 0.311(3) 0.315(2) 0.038(3) 0.047(8) Uiso 1 1 d . . . C4 C 0.45679(18) 0.26389(15) 0.1790(2) 0.0294(3) Uani 1 1 d . . . O3 O 0.42824(13) 0.17124(11) 0.22619(15) 0.0321(3) Uani 1 1 d . . . O4 O 0.56929(14) 0.29169(14) 0.16287(19) 0.0425(4) Uani 1 1 d . . . C5 C 0.2483(3) 0.3627(2) 0.3565(2) 0.0464(5) Uani 1 1 d . . . H5A H 0.246(2) 0.4447(15) 0.3549(3) 0.064(9) Uiso 1 1 d R . . H5B H 0.3338(18) 0.3433(14) 0.4015(11) 0.068(10) Uiso 1 1 d R . . H5C H 0.1771(17) 0.3380(14) 0.4068(11) 0.054(8) Uiso 1 1 d R . . N2 N 0.27119(15) -0.05006(12) 0.18222(15) 0.0251(3) Uani 1 1 d . . . C6 C 0.3345(2) -0.06647(16) 0.05596(19) 0.0314(4) Uani 1 1 d . . . H6A H 0.319(3) -0.141(3) 0.010(3) 0.049(8) Uiso 1 1 d . . . H6B H 0.432(3) -0.048(2) 0.082(3) 0.043(7) Uiso 1 1 d . . . C7 C 0.28220(19) 0.01834(15) -0.03817(18) 0.0283(3) Uani 1 1 d . . . O5 O 0.22094(15) 0.10030(12) 0.01633(14) 0.0326(3) Uani 1 1 d . . . O6 O 0.30457(18) 0.00604(13) -0.15750(14) 0.0418(4) Uani 1 1 d . . . C8 C 0.3537(2) -0.07865(18) 0.3031(2) 0.0372(4) Uani 1 1 d . . . H8A H 0.451(3) -0.064(3) 0.296(3) 0.054(8) Uiso 1 1 d . . . H8B H 0.337(3) -0.165(3) 0.308(3) 0.062(9) Uiso 1 1 d . . . C9 C 0.32185(19) -0.00440(16) 0.42837(18) 0.0301(4) Uani 1 1 d . A . O7 O 0.25936(14) 0.08537(11) 0.40705(13) 0.0302(3) Uani 1 1 d . A . O8 O 0.35723(18) -0.02920(15) 0.54244(15) 0.0434(4) Uani 1 1 d . A . C10 C 0.1415(2) -0.11089(19) 0.1641(3) 0.0442(5) Uani 1 1 d . . . H10A H 0.0854(12) -0.0822(12) 0.0927(19) 0.057(9) Uiso 1 1 d R . . H10B H 0.1013(12) -0.0999(13) 0.2479(16) 0.054(9) Uiso 1 1 d R . . H10C H 0.1533(4) -0.1901(15) 0.140(2) 0.057(9) Uiso 1 1 d R . . Na1 Na 0.24011(9) 0.12095(7) 0.66906(10) 0.0396(2) Uani 1 1 d . . . Na2 Na 0.31129(10) -0.15874(7) 0.69415(9) 0.0410(2) Uani 1 1 d . . . Na3 Na 0.25603(9) -0.42158(7) 0.78085(12) 0.0457(2) Uani 1 1 d . . . O31 O 0.0880(3) -0.0403(3) 0.6075(3) 0.0766(8) Uani 1 1 d D . . H311 H 0.042(5) -0.062(4) 0.663(4) 0.121(18) Uiso 1 1 d D . . H312 H 0.065(4) -0.083(3) 0.540(3) 0.074(13) Uiso 1 1 d D . . O32 O 0.2779(3) -0.3354(2) 0.5579(2) 0.0692(6) Uani 1 1 d D . . H321 H 0.327(4) -0.314(4) 0.507(4) 0.091(16) Uiso 1 1 d D . . H322 H 0.212(3) -0.345(4) 0.500(4) 0.090(14) Uiso 1 1 d D . . O33 O 0.2271(5) -0.4259(4) 1.0107(4) 0.1059(11) Uani 1 1 d D . . H331 H 0.270(7) -0.363(4) 1.029(8) 0.19(4) Uiso 1 1 d D . . H332 H 0.182(8) -0.421(7) 1.080(7) 0.23(5) Uiso 1 1 d D . . Cl1 Cl 0.03333(5) 0.34524(5) 0.69437(6) 0.04321(13) Uani 1 1 d . . . O11 O 0.0979(3) 0.4409(2) 0.6606(3) 0.0839(8) Uani 1 1 d . . . O121 O -0.1002(11) 0.3575(15) 0.6998(15) 0.097(4) Uani 0.50 1 d P A 1 O131 O 0.0873(15) 0.3378(16) 0.8258(10) 0.217(8) Uani 0.50 1 d P A 1 O141 O 0.0625(8) 0.2479(5) 0.6199(13) 0.117(4) Uani 0.50 1 d P A 1 O122 O -0.0736(13) 0.3734(15) 0.7647(16) 0.121(6) Uani 0.50 1 d P A 2 O132 O 0.1125(6) 0.2747(5) 0.7731(7) 0.0704(17) Uani 0.50 1 d P A 2 O142 O -0.0045(9) 0.2770(6) 0.5697(7) 0.102(2) Uani 0.50 1 d P A 2 Cl2 Cl 0.46900(6) 0.35581(6) 0.72720(8) 0.05500(17) Uani 1 1 d . . . O211 O 0.4027(4) 0.2614(3) 0.6553(5) 0.0809(13) Uani 0.65 1 d P A 3 O221 O 0.6002(4) 0.3626(3) 0.7029(7) 0.0901(16) Uani 0.65 1 d P A 3 O231 O 0.4690(11) 0.3678(16) 0.8612(7) 0.300(9) Uani 0.65 1 d P A 3 O241 O 0.4027(6) 0.4495(4) 0.6834(11) 0.157(3) Uani 0.65 1 d P . 3 O212 O 0.4123(10) 0.2536(9) 0.7752(11) 0.096(3) Uiso 0.35 1 d P A 4 O232 O 0.4110(7) 0.4309(6) 0.8211(8) 0.0616(15) Uiso 0.35 1 d P . 4 O222 O 0.6011(9) 0.3418(7) 0.7933(9) 0.075(2) Uiso 0.35 1 d P A 4 O242 O 0.4825(16) 0.4178(13) 0.6121(16) 0.152(5) Uiso 0.35 1 d P A 4 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 0.02370(12) 0.01906(12) 0.02479(13) 0.00609(8) 0.00638(8) 0.00474(8) N1 0.0258(7) 0.0212(6) 0.0306(7) 0.0047(5) 0.0044(5) 0.0031(5) C1 0.0289(9) 0.0304(9) 0.0492(11) 0.0153(8) 0.0047(8) 0.0089(7) C2 0.0248(8) 0.0300(8) 0.0395(10) 0.0039(7) 0.0028(7) 0.0053(6) O1 0.0260(6) 0.0284(6) 0.0471(8) 0.0117(6) 0.0108(5) 0.0047(5) O2 0.0237(7) 0.0428(8) 0.0736(12) 0.0108(8) 0.0060(7) 0.0094(6) C3 0.0295(9) 0.0271(8) 0.0462(11) 0.0131(8) 0.0070(8) 0.0012(7) C4 0.0253(8) 0.0278(8) 0.0347(9) 0.0033(7) 0.0023(7) -0.0006(6) O3 0.0254(6) 0.0293(6) 0.0444(8) 0.0140(5) 0.0048(5) 0.0048(5) O4 0.0251(7) 0.0403(8) 0.0628(10) 0.0089(7) 0.0052(6) -0.0041(6) C5 0.0560(14) 0.0394(11) 0.0403(11) -0.0105(9) 0.0056(10) 0.0006(10) N2 0.0326(7) 0.0212(6) 0.0232(6) 0.0050(5) 0.0068(5) 0.0044(5) C6 0.0425(10) 0.0288(8) 0.0253(8) 0.0048(6) 0.0112(7) 0.0115(7) C7 0.0343(9) 0.0279(8) 0.0230(7) 0.0042(6) 0.0041(6) 0.0003(6) O5 0.0427(8) 0.0314(6) 0.0253(6) 0.0080(5) 0.0042(5) 0.0114(6) O6 0.0656(11) 0.0388(8) 0.0229(6) 0.0054(5) 0.0111(6) 0.0070(7) C8 0.0539(12) 0.0352(10) 0.0251(8) 0.0092(7) 0.0062(8) 0.0220(9) C9 0.0340(9) 0.0333(9) 0.0252(8) 0.0087(6) 0.0069(7) 0.0062(7) O7 0.0405(7) 0.0292(6) 0.0231(6) 0.0057(5) 0.0083(5) 0.0088(5) O8 0.0535(9) 0.0546(9) 0.0261(7) 0.0156(6) 0.0077(6) 0.0176(7) C10 0.0481(12) 0.0314(10) 0.0536(13) 0.0022(9) 0.0136(10) -0.0110(9) Na1 0.0441(5) 0.0347(4) 0.0421(5) 0.0091(3) 0.0085(4) 0.0047(3) Na2 0.0593(6) 0.0316(4) 0.0324(4) 0.0036(3) 0.0062(4) 0.0045(4) Na3 0.0325(4) 0.0305(4) 0.0742(7) 0.0051(4) 0.0080(4) 0.0000(3) O31 0.0671(15) 0.109(2) 0.0571(13) 0.0218(14) 0.0161(11) -0.0357(14) O32 0.0826(17) 0.0642(14) 0.0549(12) -0.0125(11) 0.0027(12) -0.0056(12) O33 0.126(3) 0.119(3) 0.081(2) 0.038(2) 0.015(2) 0.034(3) Cl1 0.0373(3) 0.0425(3) 0.0511(3) 0.0086(2) 0.0078(2) -0.0024(2) O11 0.0897(18) 0.0628(14) 0.101(2) 0.0150(13) 0.0204(15) -0.0289(13) O121 0.038(3) 0.093(7) 0.171(12) 0.043(8) 0.032(5) 0.017(3) O131 0.207(14) 0.37(2) 0.073(6) 0.090(10) -0.060(7) -0.108(14) O141 0.087(5) 0.052(3) 0.220(12) -0.001(5) 0.062(6) 0.015(3) O122 0.115(11) 0.078(6) 0.202(16) 0.047(9) 0.118(11) 0.039(8) O132 0.058(3) 0.063(3) 0.094(5) 0.030(3) 0.000(3) 0.023(2) O142 0.145(7) 0.072(4) 0.074(4) -0.018(3) -0.015(4) -0.026(4) Cl2 0.0358(3) 0.0461(3) 0.0789(5) -0.0086(3) 0.0043(3) 0.0003(2) O211 0.057(2) 0.0406(16) 0.134(4) -0.0143(19) -0.009(2) -0.0157(14) O221 0.0458(18) 0.055(2) 0.172(5) 0.000(3) 0.041(3) -0.0026(15) O231 0.196(10) 0.65(3) 0.055(4) 0.066(8) 0.007(5) -0.108(14) O241 0.092(4) 0.057(3) 0.316(11) -0.005(4) 0.017(5) 0.043(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 2.1516(14) . yes Fe1 O1 1.9753(14) . yes Fe1 O3 1.9884(14) . yes Fe1 N2 2.1534(14) . yes Fe1 O5 2.0062(14) . yes Fe1 O7 1.9769(13) . yes N1 C1 1.475(2) . ? N1 C3 1.477(2) . ? N1 C5 1.486(3) . ? C1 C2 1.529(3) . ? C1 H1A 1.07(3) . ? C1 H1B 0.95(3) . ? C2 O2 1.222(2) . ? C2 O1 1.288(2) . ? O2 Na3 2.3999(18) 2_556 ? O2 Na2 2.692(2) 2_556 ? C3 C4 1.526(3) . ? C3 H3A 0.98(3) . ? C3 H3B 1.03(3) . ? C4 O4 1.223(2) . ? C4 O3 1.294(2) . ? C4 Na2 2.947(2) 2_656 ? O3 Na2 2.7119(17) 2_656 ? O4 Na3 2.3229(18) 2_656 ? O4 Na2 2.511(2) 2_656 ? C5 H5A 0.9854 . ? C5 H5B 0.9854 . ? C5 H5C 0.9854 . ? N2 C6 1.471(2) . ? N2 C8 1.475(2) . ? N2 C10 1.484(3) . ? C6 C7 1.529(3) . ? C6 H6A 0.96(3) . ? C6 H6B 1.02(3) . ? C7 O6 1.228(2) . ? C7 O5 1.277(2) . ? O6 Na2 2.3356(18) 1_554 ? O6 Na1 2.3806(18) 1_554 ? C8 C9 1.517(3) . ? C8 H8A 1.02(3) . ? C8 H8B 1.05(3) . ? C9 O8 1.228(2) . ? C9 O7 1.291(2) . ? C9 Na1 2.893(2) . ? O7 Na1 2.6266(16) . ? O8 Na2 2.3608(18) . ? O8 Na1 2.4838(19) . ? C10 H10A 0.9662 . ? C10 H10B 0.9662 . ? C10 H10C 0.9662 . ? Na1 O211 2.365(4) . ? Na1 O6 2.3806(18) 1_556 ? Na1 O212 2.418(11) . ? Na1 O31 2.434(3) . ? Na1 O141 2.443(8) . ? Na1 O132 2.478(6) . ? Na1 Na2 3.4792(13) . ? Na2 O6 2.3356(18) 1_556 ? Na2 O32 2.379(2) . ? Na2 O4 2.511(2) 2_656 ? Na2 O2 2.692(2) 2_556 ? Na2 O3 2.7119(17) 2_656 ? Na2 O31 2.827(3) . ? Na2 C4 2.947(2) 2_656 ? Na2 Na3 3.4122(13) . ? Na2 H321 2.50(5) . ? Na3 O4 2.3229(18) 2_656 ? Na3 O33 2.347(4) . ? Na3 O241 2.379(6) 1_545 ? Na3 O2 2.3999(18) 2_556 ? Na3 O11 2.406(3) 1_545 ? Na3 O232 2.441(7) 1_545 ? Na3 O32 2.584(3) . ? Na3 H331 2.48(8) . ? O31 H311 0.82(3) . ? O31 H312 0.81(3) . ? O32 H321 0.81(3) . ? O32 H322 0.84(3) . ? O33 H331 0.85(4) . ? O33 H332 0.87(4) . ? Cl1 O141 1.366(7) . ? Cl1 O131 1.380(9) . ? Cl1 O121 1.384(11) . ? Cl1 O122 1.389(13) . ? Cl1 O11 1.402(2) . ? Cl1 O142 1.420(6) . ? Cl1 O132 1.427(5) . ? O11 Na3 2.406(3) 1_565 ? Cl2 O231 1.327(7) . ? Cl2 O211 1.390(3) . ? Cl2 O221 1.391(3) . ? Cl2 O232 1.410(7) . ? Cl2 O241 1.413(6) . ? Cl2 O242 1.453(16) . ? Cl2 O222 1.462(9) . ? Cl2 O212 1.493(10) . ? O241 Na3 2.379(6) 1_565 ? O232 Na3 2.441(7) 1_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 O1 78.91(6) . . yes N1 Fe1 O3 78.46(6) . . yes N1 Fe1 N2 166.42(6) . . yes N1 Fe1 O5 91.19(6) . . yes N1 Fe1 O7 112.56(6) . . yes N2 Fe1 O1 108.79(6) . . yes N2 Fe1 O3 94.12(6) . . yes N2 Fe1 O5 77.51(6) . . yes N2 Fe1 O7 78.92(6) . . yes O1 Fe1 O3 157.08(6) . . yes O1 Fe1 O5 92.68(6) . . yes O1 Fe1 O7 92.13(6) . . yes O3 Fe1 O5 91.38(6) . . yes O3 Fe1 O7 93.18(6) . . yes O5 Fe1 O7 156.25(6) . . yes? C1 N1 C3 115.72(15) . . ? C1 N1 C5 110.38(17) . . ? C3 N1 C5 110.46(17) . . ? C1 N1 Fe1 105.78(11) . . ? C3 N1 Fe1 105.04(11) . . ? C5 N1 Fe1 109.06(13) . . ? N1 C1 C2 108.27(15) . . ? N1 C1 H1A 107.7(17) . . ? C2 C1 H1A 108.0(17) . . ? N1 C1 H1B 109.7(18) . . ? C2 C1 H1B 111.2(18) . . ? H1A C1 H1B 112(2) . . ? O2 C2 O1 123.06(19) . . ? O2 C2 C1 122.30(18) . . ? O1 C2 C1 114.59(16) . . ? C2 O1 Fe1 119.57(12) . . ? C2 O2 Na3 140.38(15) . 2_556 ? C2 O2 Na2 132.33(15) . 2_556 ? Na3 O2 Na2 83.95(6) 2_556 2_556 ? N1 C3 C4 108.69(15) . . ? N1 C3 H3A 112.4(18) . . ? C4 C3 H3A 109.5(18) . . ? N1 C3 H3B 107.2(16) . . ? C4 C3 H3B 108.2(16) . . ? H3A C3 H3B 111(2) . . ? O4 C4 O3 122.55(18) . . ? O4 C4 C3 121.61(17) . . ? O3 C4 C3 115.82(16) . . ? O4 C4 Na2 57.47(11) . 2_656 ? O3 C4 Na2 66.79(10) . 2_656 ? C3 C4 Na2 168.06(14) . 2_656 ? C4 O3 Fe1 117.47(12) . . ? C4 O3 Na2 87.21(11) . 2_656 ? Fe1 O3 Na2 154.78(7) . 2_656 ? C4 O4 Na3 147.69(15) . 2_656 ? C4 O4 Na2 98.28(13) . 2_656 ? Na3 O4 Na2 89.71(6) 2_656 2_656 ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C6 N2 C8 114.11(15) . . ? C6 N2 C10 110.32(16) . . ? C8 N2 C10 111.59(17) . . ? C6 N2 Fe1 106.37(11) . . ? C8 N2 Fe1 105.82(11) . . ? C10 N2 Fe1 108.22(13) . . ? N2 C6 C7 109.07(14) . . ? N2 C6 H6A 111.9(18) . . ? C7 C6 H6A 109.4(18) . . ? N2 C6 H6B 106.9(16) . . ? C7 C6 H6B 107.4(16) . . ? H6A C6 H6B 112(2) . . ? O6 C7 O5 124.61(18) . . ? O6 C7 C6 119.13(17) . . ? O5 C7 C6 116.21(15) . . ? C7 O5 Fe1 117.38(12) . . ? C7 O6 Na2 129.59(14) . 1_554 ? C7 O6 Na1 128.24(14) . 1_554 ? Na2 O6 Na1 95.07(6) 1_554 1_554 ? N2 C8 C9 109.89(15) . . ? N2 C8 H8A 111.4(18) . . ? C9 C8 H8A 106.1(18) . . ? N2 C8 H8B 106.8(19) . . ? C9 C8 H8B 113.9(19) . . ? H8A C8 H8B 109(3) . . ? O8 C9 O7 123.22(18) . . ? O8 C9 C8 120.49(18) . . ? O7 C9 C8 116.27(16) . . ? O8 C9 Na1 58.53(11) . . ? O7 C9 Na1 65.15(10) . . ? C8 C9 Na1 174.24(15) . . ? C9 O7 Fe1 117.81(11) . . ? C9 O7 Na1 88.35(10) . . ? Fe1 O7 Na1 153.62(7) . . ? C9 O8 Na2 141.63(16) . . ? C9 O8 Na1 96.54(13) . . ? Na2 O8 Na1 91.77(6) . . ? N2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O211 Na1 O6 111.70(13) . 1_556 ? O211 Na1 O212 29.1(2) . . ? O6 Na1 O212 87.1(3) 1_556 . ? O211 Na1 O31 161.31(14) . . ? O6 Na1 O31 78.36(8) 1_556 . ? O212 Na1 O31 165.5(3) . . ? O211 Na1 O141 92.0(2) . . ? O6 Na1 O141 136.7(3) 1_556 . ? O212 Na1 O141 100.7(3) . . ? O31 Na1 O141 90.4(2) . . ? O211 Na1 O132 86.10(19) . . ? O6 Na1 O132 106.87(16) 1_556 . ? O212 Na1 O132 78.0(3) . . ? O31 Na1 O132 106.52(18) . . ? O141 Na1 O132 36.8(3) . . ? O211 Na1 O8 93.80(11) . . ? O6 Na1 O8 78.49(6) 1_556 . ? O212 Na1 O8 104.5(2) . . ? O31 Na1 O8 72.25(9) . . ? O141 Na1 O8 137.6(3) . . ? O132 Na1 O8 174.29(16) . . ? O211 Na1 O7 81.36(13) . . ? O6 Na1 O7 129.36(6) 1_556 . ? O212 Na1 O7 109.3(3) . . ? O31 Na1 O7 80.18(7) . . ? O141 Na1 O7 88.3(3) . . ? O132 Na1 O7 123.11(16) . . ? O8 Na1 O7 51.31(5) . . ? O211 Na1 C9 89.29(12) . . ? O6 Na1 C9 102.94(6) 1_556 . ? O212 Na1 C9 110.5(3) . . ? O31 Na1 C9 72.80(8) . . ? O141 Na1 C9 113.4(3) . . ? O132 Na1 C9 149.41(16) . . ? O8 Na1 C9 24.94(5) . . ? O7 Na1 C9 26.49(5) . . ? O211 Na1 Na2 123.19(10) . . ? O6 Na1 Na2 41.97(4) 1_556 . ? O212 Na1 Na2 114.2(2) . . ? O31 Na1 Na2 53.67(8) . . ? O141 Na1 Na2 143.84(19) . . ? O132 Na1 Na2 141.06(16) . . ? O8 Na1 Na2 42.71(4) . . ? O7 Na1 Na2 89.05(4) . . ? C9 Na1 Na2 63.92(4) . . ? O6 Na2 O8 81.91(6) 1_556 . ? O6 Na2 O32 168.75(10) 1_556 . ? O8 Na2 O32 105.21(9) . . ? O6 Na2 O4 103.98(7) 1_556 2_656 ? O8 Na2 O4 139.19(7) . 2_656 ? O32 Na2 O4 76.51(8) . 2_656 ? O6 Na2 O2 94.25(7) 1_556 2_556 ? O8 Na2 O2 143.71(7) . 2_556 ? O32 Na2 O2 74.82(9) . 2_556 ? O4 Na2 O2 76.87(6) 2_656 2_556 ? O6 Na2 O3 89.91(6) 1_556 2_656 ? O8 Na2 O3 90.48(6) . 2_656 ? O32 Na2 O3 98.60(9) . 2_656 ? O4 Na2 O3 49.82(5) 2_656 2_656 ? O2 Na2 O3 125.71(6) 2_556 2_656 ? O6 Na2 O31 71.48(8) 1_556 . ? O8 Na2 O31 67.26(6) . . ? O32 Na2 O31 102.89(10) . . ? O4 Na2 O31 153.29(7) 2_656 . ? O2 Na2 O31 77.25(6) 2_556 . ? O3 Na2 O31 152.33(7) 2_656 . ? O6 Na2 C4 101.12(7) 1_556 2_656 ? O8 Na2 C4 115.09(7) . 2_656 ? O32 Na2 C4 83.92(8) . 2_656 ? O4 Na2 C4 24.25(5) 2_656 2_656 ? O2 Na2 C4 101.10(6) 2_556 2_656 ? O3 Na2 C4 26.01(5) 2_656 2_656 ? O31 Na2 C4 172.13(8) . 2_656 ? O6 Na2 Na3 124.00(5) 1_556 . ? O8 Na2 Na3 154.07(6) . . ? O32 Na2 Na3 49.12(7) . . ? O4 Na2 Na3 42.90(4) 2_656 . ? O2 Na2 Na3 44.38(4) 2_556 . ? O3 Na2 Na3 90.33(4) 2_656 . ? O31 Na2 Na3 116.94(6) . . ? C4 Na2 Na3 64.58(4) 2_656 . ? O6 Na2 Na1 42.97(4) 1_556 . ? O8 Na2 Na1 45.53(5) . . ? O32 Na2 Na1 138.27(8) . . ? O4 Na2 Na1 145.07(5) 2_656 . ? O2 Na2 Na1 110.63(5) 2_556 . ? O3 Na2 Na1 108.71(4) 2_656 . ? O31 Na2 Na1 43.91(6) . . ? C4 Na2 Na1 131.81(5) 2_656 . ? Na3 Na2 Na1 154.92(4) . . ? O6 Na2 H321 170.4(9) 1_556 . ? O8 Na2 H321 88.5(8) . . ? O32 Na2 H321 18.9(7) . . ? O4 Na2 H321 83.3(10) 2_656 . ? O2 Na2 H321 93.5(7) 2_556 . ? O3 Na2 H321 90.1(9) 2_656 . ? O31 Na2 H321 104.9(10) . . ? C4 Na2 H321 82.9(10) 2_656 . ? Na3 Na2 H321 65.6(8) . . ? Na1 Na2 H321 128.4(10) . . ? O4 Na3 O33 91.38(15) 2_656 . ? O4 Na3 O241 88.89(16) 2_656 1_545 ? O33 Na3 O241 117.7(3) . 1_545 ? O4 Na3 O2 86.54(7) 2_656 2_556 ? O33 Na3 O2 84.50(11) . 2_556 ? O241 Na3 O2 157.5(3) 1_545 2_556 ? O4 Na3 O11 163.74(10) 2_656 1_545 ? O33 Na3 O11 104.52(16) . 1_545 ? O241 Na3 O11 80.82(18) 1_545 1_545 ? O2 Na3 O11 98.15(9) 2_556 1_545 ? O4 Na3 O232 88.06(18) 2_656 1_545 ? O33 Na3 O232 83.7(2) . 1_545 ? O241 Na3 O232 34.0(3) 1_545 1_545 ? O2 Na3 O232 166.9(2) 2_556 1_545 ? O11 Na3 O232 90.32(19) 1_545 1_545 ? O4 Na3 O32 76.05(8) 2_656 . ? O33 Na3 O32 157.72(13) . . ? O241 Na3 O32 81.0(2) 1_545 . ? O2 Na3 O32 76.56(8) 2_556 . ? O11 Na3 O32 89.85(10) 1_545 . ? O232 Na3 O32 113.6(2) 1_545 . ? O4 Na3 Na2 47.38(5) 2_656 . ? O33 Na3 Na2 114.21(12) . . ? O241 Na3 Na2 110.8(2) 1_545 . ? O2 Na3 Na2 51.67(5) 2_556 . ? O11 Na3 Na2 125.30(8) 1_545 . ? O232 Na3 Na2 129.64(18) 1_545 . ? O32 Na3 Na2 44.12(6) . . ? O4 Na3 H331 72.4(11) 2_656 . ? O33 Na3 H331 20.2(9) . . ? O241 Na3 H331 122(2) 1_545 . ? O2 Na3 H331 76.9(19) 2_556 . ? O11 Na3 H331 123.7(11) 1_545 . ? O232 Na3 H331 90.1(19) 1_545 . ? O32 Na3 H331 139.6(12) . . ? Na2 Na3 H331 95.5(12) . . ? Na1 O31 Na2 82.42(8) . . ? Na1 O31 H311 121(3) . . ? Na2 O31 H311 95(4) . . ? Na1 O31 H312 136(3) . . ? Na2 O31 H312 96(3) . . ? H311 O31 H312 102(4) . . ? Na2 O32 Na3 86.76(8) . . ? Na2 O32 H321 89(3) . . ? Na3 O32 H321 147(3) . . ? Na2 O32 H322 118(3) . . ? Na3 O32 H322 115(3) . . ? H321 O32 H322 96(3) . . ? Na3 O33 H331 89(6) . . ? Na3 O33 H332 154(7) . . ? H331 O33 H332 98(5) . . ? O141 Cl1 O131 106.0(9) . . ? O141 Cl1 O121 113.3(8) . . ? O131 Cl1 O121 106.3(9) . . ? O141 Cl1 O122 131.6(8) . . ? O131 Cl1 O122 79.6(9) . . ? O121 Cl1 O122 28.3(10) . . ? O141 Cl1 O11 113.6(4) . . ? O131 Cl1 O11 103.1(6) . . ? O121 Cl1 O11 113.5(8) . . ? O122 Cl1 O11 111.5(7) . . ? O141 Cl1 O142 37.9(4) . . ? O131 Cl1 O142 141.1(9) . . ? O121 Cl1 O142 85.1(8) . . ? O122 Cl1 O142 112.1(8) . . ? O11 Cl1 O142 106.0(4) . . ? O141 Cl1 O132 67.5(5) . . ? O131 Cl1 O132 38.6(8) . . ? O121 Cl1 O132 124.4(8) . . ? O122 Cl1 O132 107.1(7) . . ? O11 Cl1 O132 115.8(3) . . ? O142 Cl1 O132 104.2(4) . . ? Cl1 O11 Na3 134.61(19) . 1_565 ? Cl1 O141 Na1 128.5(7) . . ? Cl1 O132 Na1 122.7(4) . . ? O231 Cl2 O211 117.0(7) . . ? O231 Cl2 O221 106.2(6) . . ? O211 Cl2 O221 112.3(3) . . ? O231 Cl2 O232 45.4(8) . . ? O211 Cl2 O232 123.1(4) . . ? O221 Cl2 O232 124.4(4) . . ? O231 Cl2 O241 105.0(9) . . ? O211 Cl2 O241 106.1(4) . . ? O221 Cl2 O241 109.8(4) . . ? O232 Cl2 O241 59.9(4) . . ? O231 Cl2 O242 143.0(10) . . ? O211 Cl2 O242 97.3(7) . . ? O221 Cl2 O242 69.8(7) . . ? O232 Cl2 O242 104.9(7) . . ? O241 Cl2 O242 48.6(6) . . ? O231 Cl2 O222 69.7(6) . . ? O211 Cl2 O222 117.7(4) . . ? O221 Cl2 O222 39.3(3) . . ? O232 Cl2 O222 104.3(5) . . ? O241 Cl2 O222 133.2(4) . . ? O242 Cl2 O222 107.5(7) . . ? O231 Cl2 O212 68.5(8) . . ? O211 Cl2 O212 49.2(4) . . ? O221 Cl2 O212 121.2(4) . . ? O232 Cl2 O212 94.0(5) . . ? O241 Cl2 O212 128.5(5) . . ? O242 Cl2 O212 146.4(8) . . ? O222 Cl2 O212 94.0(5) . . ? Cl2 O211 Na1 143.2(3) . . ? Cl2 O241 Na3 134.3(6) . 1_565 ? Cl2 O212 Na1 130.8(6) . . ? Cl2 O232 Na3 129.7(5) . 1_565 ? 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 O31 H311 O1 0.82(3) 1.91(3) 2.714(3) 165(5) 2_556 O31 H312 O141 0.81(3) 2.62(3) 3.392(10) 160(4) 2_556 O31 H312 O142 0.81(3) 2.49(3) 3.214(7) 150(4) 2_556 O32 H321 O221 0.81(3) 2.31(4) 2.989(6) 142(4) 2_656 O32 H321 O242 0.81(3) 2.65(4) 3.235(17) 131(4) 2_656 O32 H322 O121 0.84(3) 2.18(4) 2.968(14) 157(4) 2_556 O32 H322 O142 0.84(3) 2.35(4) 3.077(10) 145(4) 2_556 O33 H331 O222 0.85(4) 2.09(8) 2.582(10) 116(7) 2_657 O33 H332 O122 0.87(4) 2.03(5) 2.888(15) 168(8) 2_557 O33 H332 O121 0.87(4) 2.47(5) 3.314(15) 163(8) 2_557 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.843 _refine_diff_density_min -0.679 _refine_diff_density_rms 0.069