Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_contact_author_name 'Marius Andruh' _publ_contact_author_address ; University of Bucharest Faculty of Chemistry Inorganic Chemistry Laboratory Str. Dumbrava Rosie Nr. 23 70254-Bucharest Romania ; _publ_contact_author_email 'marius.andruh@dnt.ro' _publ_section_title ; Construction of 3d-4f heterometallic coordination polymers by simultaneous use of hexacyano-metallate building-blocks and exo-bidentate ligands ; _publ_requested_journal 'Chem.Comm.' _publ_requested_coeditor_name ? _publ_contact_letter ; ; #=========================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) #=========================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ;? ; loop_ _publ_author_name _publ_author_address 'Tanase, Stefania' ; University of Bucharest Faculty of Chemistry Inorganic Chemistry Laboratory Str. Dumbrava Rosie Nr. 23 70254-Bucharest Romania ; 'Andruh, Marius' ; University of Bucharest Faculty of Chemistry Inorganic Chemistry Laboratory Str. Dumbrava Rosie Nr. 23 70254-Bucharest Romania ; 'Muller, Achim' ; Fakultat f. Chemie Universitat Bielefeld 33501 Bielefeld Germany ; 'Schmidtmann, Marc' ; Fakultat f. Chemie Universitat Bielefeld 33501 Bielefeld Germany ; 'Mathoniere, Corine' ; Laboratoire des Sciences Moléculaires Institut de Chimie de la Matière Condensée de Bordeaux 33608 Pessac France ; 'Rombaut, Guillaume' ; Laboratoire des Sciences Moléculaires Institut de Chimie de la Matière Condensée de Bordeaux 33608 Pessac France ; #=========================================================================== # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; #=========================================================================== data_mari1 _database_code_CSD 158134 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C31 H38 Fe N11 O14 Pr' _chemical_formula_weight 985.48 _chemical_melting_point ? _chemical_compound_source ? 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pr' 'Pr' -0.2180 2.8214 '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' 'N' 'N' 0.0061 0.0033 '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 8.3607(2) _cell_length_b 15.4388(4) _cell_length_c 15.4924(4) _cell_angle_alpha 84.7800(10) _cell_angle_beta 80.6710(10) _cell_angle_gamma 85.6550(10) _cell_volume 1961.32(9) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 6100 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 30.01 _exptl_crystal_description irregular _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_method ? _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 1.677 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker AXS SMART' _diffrn_measurement_method omega-scan _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 28265 _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 30.01 _reflns_number_total 11383 _reflns_number_observed 10330 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Bruker AXS SMART' _computing_cell_refinement 'Bruker AXS SAINT' _computing_data_reduction 'Bruker AXS SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Crystal Impact: DIAMOND; Bruker AXS: SHELXTL' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 37 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.0400P)^2^+0.6000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11346 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0282 _refine_ls_R_factor_obs 0.0236 _refine_ls_wR_factor_all 0.0727 _refine_ls_wR_factor_obs 0.0637 _refine_ls_goodness_of_fit_all 1.051 _refine_ls_goodness_of_fit_obs 1.071 _refine_ls_restrained_S_all 1.163 _refine_ls_restrained_S_obs 1.071 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pr1 Pr -0.190141(10) 0.257758(6) -0.346821(5) 0.01599(3) Uani 1 d . . Fe1 Fe 0.08052(3) 0.23418(2) -0.70417(2) 0.02209(6) Uani 1 d . . O1 O 0.0283(2) 0.24696(10) -0.24956(9) 0.0290(3) Uani 1 d . . O2 O -0.4935(2) 0.28291(9) -0.31006(10) 0.0279(3) Uani 1 d . . O3 O 0.0505(2) 0.34797(10) -0.40996(10) 0.0311(3) Uani 1 d . . O4 O -0.2965(2) 0.39188(9) -0.43198(10) 0.0307(3) Uani 1 d . . O5 O -0.3450(2) 0.12887(9) -0.37534(9) 0.0246(3) Uani 1 d . . O6 O -0.2290(2) 0.38169(9) -0.25345(9) 0.0279(3) Uani 1 d . . O7 O -0.0141(2) 0.12772(9) -0.36417(9) 0.0268(3) Uani 1 d . . O8 O -0.2957(2) 0.18153(9) -0.20030(8) 0.0229(3) Uani 1 d . . O9 O -1.1105(2) 0.66124(13) 0.12841(12) 0.0453(4) Uani 1 d . . O10 O 0.3224(2) 0.14171(9) -0.26386(9) 0.0257(3) Uani 1 d . . C1 C -0.0991(3) 0.19013(14) -0.74906(13) 0.0307(4) Uani 1 d . . C2 C -0.0120(3) 0.35251(14) -0.71937(13) 0.0305(4) Uani 1 d . . C3 C 0.1819(2) 0.11790(13) -0.68503(12) 0.0258(4) Uani 1 d . . C4 C 0.2621(3) 0.27870(13) -0.66253(13) 0.0282(4) Uani 1 d . . C5 C -0.0402(2) 0.23126(12) -0.58561(12) 0.0233(3) Uani 1 d . . C6 C 0.1924(3) 0.2454(2) -0.82398(14) 0.0339(4) Uani 1 d . . C7 C -0.4480(2) 0.36914(12) -0.14079(12) 0.0237(3) Uani 1 d . . H7A H -0.4215(2) 0.30837(12) -0.13212(12) 0.028 Uiso 1 calc R . C8 C -0.5762(2) 0.40722(12) -0.08678(12) 0.0234(3) Uani 1 d . . H8A H -0.6363(2) 0.37266(12) -0.04067(12) 0.028 Uiso 1 calc R . C9 C -0.6185(2) 0.49630(12) -0.09928(12) 0.0221(3) Uani 1 d . . C10 C -0.5274(3) 0.54344(13) -0.16892(13) 0.0285(4) Uani 1 d . . H10A H -0.5542(3) 0.60383(13) -0.18049(13) 0.034 Uiso 1 calc R . C11 C -0.3990(3) 0.50334(13) -0.22099(13) 0.0279(4) Uani 1 d . . H11A H -0.3377(3) 0.53635(13) -0.26789(13) 0.033 Uiso 1 calc R . C12 C -0.9517(3) 0.65723(14) -0.0084(2) 0.0346(5) Uani 1 d . . H12A H -1.0049(3) 0.71058(14) -0.0270(2) 0.041 Uiso 1 calc R . C13 C -0.8319(3) 0.61745(14) -0.06606(14) 0.0306(4) Uani 1 d . . H13A H -0.8033(3) 0.64349(14) -0.12394(14) 0.037 Uiso 1 calc R . C14 C -0.7522(2) 0.53899(12) -0.03987(12) 0.0231(3) Uani 1 d . . C15 C -0.8029(2) 0.50317(13) 0.04461(13) 0.0266(4) Uani 1 d . . H15A H -0.7539(2) 0.44892(13) 0.06411(13) 0.032 Uiso 1 calc R . C16 C -0.9232(2) 0.5449(2) 0.10100(14) 0.0314(4) Uani 1 d . . H16A H -0.9556(2) 0.5194(2) 0.15877(14) 0.038 Uiso 1 calc R . C17 C 0.2339(2) 0.14465(12) -0.45405(12) 0.0232(3) Uani 1 d . . H17A H 0.2094(2) 0.20563(12) -0.46256(12) 0.028 Uiso 1 calc R . C18 C 0.3806(2) 0.10857(12) -0.49265(12) 0.0236(3) Uani 1 d . . H18A H 0.4558(2) 0.14505(12) -0.52834(12) 0.028 Uiso 1 calc R . C19 C 0.4209(2) 0.01983(12) -0.48048(12) 0.0217(3) Uani 1 d . . C20 C 0.3033(3) -0.02996(14) -0.4299(2) 0.0441(6) Uani 1 d . . H20A H 0.3243(3) -0.09118(14) -0.4209(2) 0.053 Uiso 1 calc R . C21 C 0.1573(3) 0.00761(14) -0.3928(2) 0.0425(6) Uani 1 d . . H21A H 0.0784(3) -0.02781(14) -0.3588(2) 0.051 Uiso 1 calc R . C22 C -0.1320(3) 0.05793(13) -0.17194(12) 0.0276(4) Uani 1 d . . H22A H -0.1349(3) 0.04102(13) -0.22910(12) 0.033 Uiso 1 calc R . C23 C -0.0480(3) 0.00541(13) -0.11587(12) 0.0284(4) Uani 1 d . . H23A H 0.0072(3) -0.04723(13) -0.13486(12) 0.034 Uiso 1 calc R . C24 C -0.0427(2) 0.02858(11) -0.03102(11) 0.0197(3) Uani 1 d . . C25 C -0.1258(3) 0.10660(13) -0.00765(13) 0.0278(4) Uani 1 d . . H25A H -0.1257(3) 0.12495(13) 0.04923(13) 0.033 Uiso 1 calc R . C26 C -0.2079(3) 0.15750(13) -0.06579(13) 0.0279(4) Uani 1 d . . H26A H -0.2637(3) 0.21064(13) -0.04867(13) 0.033 Uiso 1 calc R . C27 C 0.4326(3) 0.01994(13) -0.19098(13) 0.0273(4) Uani 1 d . . H27A H 0.4441(3) -0.00976(13) -0.24292(13) 0.033 Uiso 1 calc R . C28 C 0.4877(3) -0.02077(13) -0.11732(13) 0.0281(4) Uani 1 d . . H28A H 0.5388(3) -0.07781(13) -0.11942(13) 0.034 Uiso 1 calc R . C29 C 0.4692(2) 0.02099(12) -0.03978(12) 0.0218(3) Uani 1 d . . C30 C 0.3900(2) 0.10408(13) -0.04038(12) 0.0260(4) Uani 1 d . . H30A H 0.3718(2) 0.13402(13) 0.01159(12) 0.031 Uiso 1 calc R . C31 C 0.3383(2) 0.14305(13) -0.11538(13) 0.0266(4) Uani 1 d . . H31A H 0.2850(2) 0.19962(13) -0.11476(13) 0.032 Uiso 1 calc R . N1 N -0.2015(3) 0.1648(2) -0.7791(2) 0.0498(5) Uani 1 d . . N2 N -0.0670(3) 0.42291(13) -0.72348(14) 0.0455(5) Uani 1 d . . N3 N 0.2423(2) 0.04964(12) -0.67180(12) 0.0322(4) Uani 1 d . . N4 N 0.3656(3) 0.30904(13) -0.63636(15) 0.0404(4) Uani 1 d . . N5 N -0.1118(2) 0.23574(11) -0.51574(11) 0.0282(3) Uani 1 d . . N6 N 0.2552(3) 0.2547(2) -0.89586(13) 0.0511(6) Uani 1 d . . N7 N -0.3597(2) 0.41730(10) -0.20589(10) 0.0225(3) Uani 1 d . . N8 N -0.9949(2) 0.62174(13) 0.07412(13) 0.0330(4) Uani 1 d . . N9 N 0.1252(2) 0.09388(10) -0.40432(10) 0.0215(3) Uani 1 d . . N10 N -0.2101(2) 0.13283(10) -0.14680(10) 0.0202(3) Uani 1 d . . N11 N 0.3627(2) 0.10141(10) -0.18979(10) 0.0221(3) Uani 1 d . . O11 O -0.1343(2) 0.54800(10) -0.43243(11) 0.0374(3) Uani 1 d . . O12 O -0.4027(3) 0.2410(2) -0.9051(2) 0.0636(6) Uani 1 d . . O13 O -0.3791(2) 0.40290(12) -0.59723(12) 0.0455(4) Uani 1 d . . O14A O -0.7089(7) 0.4255(4) -0.3344(4) 0.0371(11) Uani 0.50 d P . O14B O -0.7413(7) 0.4096(3) -0.3020(4) 0.0374(11) Uani 0.50 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 Pr1 0.01549(5) 0.01719(5) 0.01496(5) -0.00250(3) -0.00191(3) 0.00170(3) Fe1 0.02796(13) 0.02094(12) 0.01668(11) -0.00328(9) -0.00146(9) 0.00066(10) O1 0.0232(7) 0.0365(8) 0.0297(7) -0.0111(6) -0.0101(5) 0.0064(6) O2 0.0178(6) 0.0248(7) 0.0392(8) 0.0017(6) -0.0031(5) 0.0028(5) O3 0.0283(7) 0.0354(8) 0.0296(7) 0.0006(6) -0.0029(6) -0.0099(6) O4 0.0369(8) 0.0226(7) 0.0330(7) 0.0033(5) -0.0107(6) -0.0003(6) O5 0.0252(6) 0.0226(6) 0.0275(7) -0.0058(5) -0.0061(5) -0.0018(5) O6 0.0236(7) 0.0295(7) 0.0306(7) -0.0149(6) 0.0019(5) 0.0004(5) O7 0.0203(6) 0.0263(7) 0.0299(7) -0.0045(5) 0.0049(5) 0.0084(5) O8 0.0229(6) 0.0267(7) 0.0184(6) 0.0041(5) -0.0066(5) 0.0036(5) O9 0.0245(7) 0.0631(11) 0.0530(10) -0.0394(9) -0.0080(7) 0.0132(7) O10 0.0259(7) 0.0279(7) 0.0231(6) 0.0028(5) -0.0067(5) 0.0004(5) C1 0.0345(11) 0.0300(10) 0.0279(9) -0.0076(8) -0.0061(8) 0.0050(8) C2 0.0385(11) 0.0294(10) 0.0224(9) -0.0023(7) -0.0016(8) -0.0003(8) C3 0.0290(9) 0.0257(9) 0.0234(8) -0.0065(7) -0.0037(7) -0.0030(7) C4 0.0324(10) 0.0224(9) 0.0283(9) -0.0020(7) -0.0019(8) 0.0008(7) C5 0.0285(9) 0.0212(8) 0.0207(8) -0.0024(6) -0.0052(7) -0.0004(7) C6 0.0373(11) 0.0372(11) 0.0252(9) -0.0050(8) -0.0020(8) 0.0070(9) C7 0.0269(9) 0.0188(8) 0.0254(8) -0.0041(6) -0.0044(7) 0.0018(7) C8 0.0260(9) 0.0219(8) 0.0225(8) -0.0042(6) -0.0040(7) 0.0009(7) C9 0.0238(8) 0.0217(8) 0.0221(8) -0.0066(6) -0.0063(6) 0.0023(7) C10 0.0361(11) 0.0218(9) 0.0266(9) -0.0028(7) -0.0041(8) 0.0042(8) C11 0.0330(10) 0.0245(9) 0.0245(9) -0.0014(7) -0.0002(7) -0.0008(8) C12 0.0288(10) 0.0292(10) 0.0492(13) -0.0159(9) -0.0140(9) 0.0083(8) C13 0.0331(10) 0.0263(10) 0.0337(10) -0.0078(8) -0.0089(8) 0.0052(8) C14 0.0225(8) 0.0231(8) 0.0253(8) -0.0089(7) -0.0063(7) 0.0014(7) C15 0.0249(9) 0.0293(10) 0.0268(9) -0.0096(7) -0.0054(7) 0.0019(7) C16 0.0232(9) 0.0431(12) 0.0298(10) -0.0151(8) -0.0046(7) 0.0007(8) C17 0.0199(8) 0.0218(8) 0.0263(9) 0.0005(7) -0.0025(7) 0.0039(6) C18 0.0201(8) 0.0247(9) 0.0238(8) 0.0009(7) -0.0009(6) 0.0035(7) C19 0.0178(8) 0.0218(8) 0.0255(8) -0.0078(6) -0.0014(6) 0.0015(6) C20 0.0284(11) 0.0179(9) 0.077(2) -0.0071(10) 0.0203(11) 0.0010(8) C21 0.0260(10) 0.0214(10) 0.071(2) -0.0038(10) 0.0197(10) -0.0001(8) C22 0.0361(10) 0.0295(10) 0.0171(8) -0.0042(7) -0.0070(7) 0.0081(8) C23 0.0381(11) 0.0259(9) 0.0201(8) -0.0045(7) -0.0062(7) 0.0111(8) C24 0.0216(8) 0.0195(8) 0.0178(7) 0.0005(6) -0.0040(6) -0.0005(6) C25 0.0410(11) 0.0230(9) 0.0218(8) -0.0051(7) -0.0130(8) 0.0051(8) C26 0.0392(11) 0.0217(9) 0.0241(9) -0.0049(7) -0.0113(8) 0.0074(8) C27 0.0352(10) 0.0229(9) 0.0235(9) -0.0037(7) -0.0043(7) 0.0016(8) C28 0.0391(11) 0.0205(9) 0.0242(9) -0.0023(7) -0.0047(8) 0.0023(8) C29 0.0218(8) 0.0213(8) 0.0212(8) -0.0009(6) -0.0006(6) -0.0019(6) C30 0.0292(9) 0.0256(9) 0.0229(8) -0.0053(7) -0.0037(7) 0.0038(7) C31 0.0278(9) 0.0243(9) 0.0271(9) -0.0043(7) -0.0044(7) 0.0047(7) N1 0.0462(12) 0.0537(14) 0.0551(13) -0.0184(11) -0.0181(10) 0.0003(10) N2 0.0609(14) 0.0298(10) 0.0409(11) 0.0000(8) 0.0000(10) 0.0084(9) N3 0.0353(9) 0.0259(9) 0.0360(9) -0.0058(7) -0.0070(7) 0.0007(7) N4 0.0374(10) 0.0353(10) 0.0500(12) -0.0052(9) -0.0092(9) -0.0042(8) N5 0.0342(9) 0.0282(8) 0.0214(7) -0.0033(6) -0.0024(6) 0.0005(7) N6 0.0512(13) 0.069(2) 0.0266(10) -0.0017(9) 0.0040(9) 0.0140(11) N7 0.0232(7) 0.0240(8) 0.0211(7) -0.0084(6) -0.0033(6) 0.0013(6) N8 0.0204(8) 0.0426(10) 0.0404(10) -0.0254(8) -0.0088(7) 0.0049(7) N9 0.0168(7) 0.0230(7) 0.0240(7) -0.0060(6) -0.0010(5) 0.0033(6) N10 0.0215(7) 0.0197(7) 0.0191(7) 0.0022(5) -0.0046(5) 0.0001(6) N11 0.0197(7) 0.0242(8) 0.0222(7) -0.0001(6) -0.0029(6) -0.0021(6) O11 0.0467(9) 0.0277(8) 0.0362(8) -0.0034(6) 0.0000(7) -0.0043(7) O12 0.0458(11) 0.0694(15) 0.076(2) -0.0173(12) -0.0043(10) -0.0052(10) O13 0.0446(10) 0.0496(10) 0.0473(10) -0.0090(8) -0.0209(8) 0.0000(8) O14A 0.029(2) 0.033(3) 0.049(3) -0.008(2) -0.005(2) 0.005(2) O14B 0.042(3) 0.020(2) 0.054(3) -0.008(2) -0.021(2) 0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O7 2.4064(13) . ? Pr1 O6 2.4731(13) . ? Pr1 O2 2.5159(13) . ? Pr1 O8 2.5177(12) . ? Pr1 O4 2.5343(14) . ? Pr1 O1 2.5366(13) . ? Pr1 O3 2.5464(14) . ? Pr1 O5 2.5629(13) . ? Pr1 N5 2.639(2) . ? Fe1 C4 1.937(2) . ? Fe1 C6 1.937(2) . ? Fe1 C2 1.939(2) . ? Fe1 C1 1.945(2) . ? Fe1 C3 1.945(2) . ? Fe1 C5 1.946(2) . ? O6 N7 1.327(2) . ? O7 N9 1.322(2) . ? O8 N10 1.327(2) . ? O9 N8 1.325(2) . ? O10 N11 1.335(2) . ? C1 N1 1.147(3) . ? C2 N2 1.148(3) . ? C3 N3 1.150(3) . ? C4 N4 1.158(3) . ? C5 N5 1.154(2) . ? C6 N6 1.153(3) . ? C7 N7 1.349(2) . ? C7 C8 1.378(3) . ? C8 C9 1.398(3) . ? C9 C10 1.396(3) . ? C9 C14 1.482(2) . ? C10 C11 1.376(3) . ? C11 N7 1.353(2) . ? C12 N8 1.348(3) . ? C12 C13 1.377(3) . ? C13 C14 1.397(3) . ? C14 C15 1.386(3) . ? C15 C16 1.382(3) . ? C16 N8 1.351(3) . ? C17 N9 1.344(2) . ? C17 C18 1.375(2) . ? C18 C19 1.389(3) . ? C19 C20 1.388(3) . ? C19 C19 1.475(3) 2_654 ? C20 C21 1.372(3) . ? C21 N9 1.340(3) . ? C22 N10 1.342(2) . ? C22 C23 1.374(3) . ? C23 C24 1.402(2) . ? C24 C25 1.391(3) . ? C24 C24 1.478(3) 2 ? C25 C26 1.375(3) . ? C26 N10 1.348(2) . ? C27 N11 1.346(2) . ? C27 C28 1.381(3) . ? C28 C29 1.396(3) . ? C29 C30 1.398(3) . ? C29 C29 1.488(4) 2_655 ? C30 C31 1.377(3) . ? C31 N11 1.350(2) . ? O14A O14B 0.574(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 O7 Pr1 O6 137.63(5) . . ? O7 Pr1 O2 132.67(5) . . ? O6 Pr1 O2 75.68(5) . . ? O7 Pr1 O8 83.83(4) . . ? O6 Pr1 O8 79.51(5) . . ? O2 Pr1 O8 68.92(4) . . ? O7 Pr1 O4 142.38(5) . . ? O6 Pr1 O4 70.75(5) . . ? O2 Pr1 O4 67.85(5) . . ? O8 Pr1 O4 132.08(5) . . ? O7 Pr1 O1 67.56(5) . . ? O6 Pr1 O1 70.19(5) . . ? O2 Pr1 O1 130.67(5) . . ? O8 Pr1 O1 70.67(5) . . ? O4 Pr1 O1 128.06(5) . . ? O7 Pr1 O3 89.06(5) . . ? O6 Pr1 O3 77.25(5) . . ? O2 Pr1 O3 137.22(5) . . ? O8 Pr1 O3 136.30(4) . . ? O4 Pr1 O3 72.25(5) . . ? O1 Pr1 O3 66.81(5) . . ? O7 Pr1 O5 68.47(5) . . ? O6 Pr1 O5 139.01(4) . . ? O2 Pr1 O5 66.73(5) . . ? O8 Pr1 O5 72.38(4) . . ? O4 Pr1 O5 107.55(5) . . ? O1 Pr1 O5 124.39(5) . . ? O3 Pr1 O5 142.87(5) . . ? O7 Pr1 N5 71.21(5) . . ? O6 Pr1 N5 136.75(5) . . ? O2 Pr1 N5 109.11(5) . . ? O8 Pr1 N5 143.32(5) . . ? O4 Pr1 N5 71.91(5) . . ? O1 Pr1 N5 120.19(5) . . ? O3 Pr1 N5 71.22(5) . . ? O5 Pr1 N5 73.61(5) . . ? C4 Fe1 C6 90.84(9) . . ? C4 Fe1 C2 89.19(9) . . ? C6 Fe1 C2 89.49(9) . . ? C4 Fe1 C1 178.53(9) . . ? C6 Fe1 C1 87.70(9) . . ? C2 Fe1 C1 90.62(9) . . ? C4 Fe1 C3 87.62(8) . . ? C6 Fe1 C3 91.32(9) . . ? C2 Fe1 C3 176.73(9) . . ? C1 Fe1 C3 92.58(8) . . ? C4 Fe1 C5 89.66(8) . . ? C6 Fe1 C5 175.75(9) . . ? C2 Fe1 C5 86.30(8) . . ? C1 Fe1 C5 91.78(8) . . ? C3 Fe1 C5 92.92(8) . . ? N7 O6 Pr1 132.25(11) . . ? N9 O7 Pr1 145.49(11) . . ? N10 O8 Pr1 127.24(10) . . ? N1 C1 Fe1 177.1(2) . . ? N2 C2 Fe1 176.2(2) . . ? N3 C3 Fe1 178.4(2) . . ? N4 C4 Fe1 176.5(2) . . ? N5 C5 Fe1 175.3(2) . . ? N6 C6 Fe1 177.5(2) . . ? N7 C7 C8 120.7(2) . . ? C7 C8 C9 120.5(2) . . ? C10 C9 C8 117.2(2) . . ? C10 C9 C14 121.6(2) . . ? C8 C9 C14 121.3(2) . . ? C11 C10 C9 120.7(2) . . ? N7 C11 C10 120.5(2) . . ? N8 C12 C13 121.1(2) . . ? C12 C13 C14 120.3(2) . . ? C15 C14 C13 117.0(2) . . ? C15 C14 C9 121.4(2) . . ? C13 C14 C9 121.6(2) . . ? C16 C15 C14 121.3(2) . . ? N8 C16 C15 120.1(2) . . ? N9 C17 C18 120.2(2) . . ? C17 C18 C19 121.3(2) . . ? C20 C19 C18 116.3(2) . . ? C20 C19 C19 121.6(2) . 2_654 ? C18 C19 C19 122.1(2) . 2_654 ? C21 C20 C19 121.2(2) . . ? N9 C21 C20 120.5(2) . . ? N10 C22 C23 120.7(2) . . ? C22 C23 C24 120.8(2) . . ? C25 C24 C23 116.6(2) . . ? C25 C24 C24 122.0(2) . 2 ? C23 C24 C24 121.4(2) . 2 ? C26 C25 C24 120.9(2) . . ? N10 C26 C25 120.7(2) . . ? N11 C27 C28 120.5(2) . . ? C27 C28 C29 120.7(2) . . ? C28 C29 C30 116.9(2) . . ? C28 C29 C29 121.5(2) . 2_655 ? C30 C29 C29 121.6(2) . 2_655 ? C31 C30 C29 120.8(2) . . ? N11 C31 C30 120.4(2) . . ? C5 N5 Pr1 162.9(2) . . ? O6 N7 C7 120.4(2) . . ? O6 N7 C11 119.1(2) . . ? C7 N7 C11 120.4(2) . . ? O9 N8 C12 120.0(2) . . ? O9 N8 C16 119.8(2) . . ? C12 N8 C16 120.2(2) . . ? O7 N9 C21 118.4(2) . . ? O7 N9 C17 121.1(2) . . ? C21 N9 C17 120.5(2) . . ? O8 N10 C22 120.20(15) . . ? O8 N10 C26 119.39(15) . . ? C22 N10 C26 120.4(2) . . ? O10 N11 C27 119.2(2) . . ? O10 N11 C31 120.2(2) . . ? C27 N11 C31 120.6(2) . . ? _refine_diff_density_max 0.865 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.083