# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email KEITH.S.MURRAY@SCI.MONASH.EDU.AU _publ_contact_author_name 'Professor Keith Murray' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_address ; School of Chemistry Monash University PO Box 23 Clayton, Victoria Melbourne 3800 AUSTRALIA ; _publ_section_title ; Structure and magnetism of a new pyrazolate bridged iron(II) spin crossover complex displaying a single HS-HS to LS-LS transition ; loop_ _publ_author_name K.Murray J.D.Cashion B.A.Leita B.Moubaraki J.P.Smith data_pbca_123K_Original _database_code_depnum_ccdc_archive 'CCDC 220710' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H26 Fe2 N14 O2 Se2' _chemical_formula_weight 932.31 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7857(2) _cell_length_b 17.2422(4) _cell_length_c 20.1713(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3751.24(15) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Irregular plates' _exptl_crystal_colour Yellow-orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 2.767 _exptl_absorpt_correction_type 'not measured' _exptl_absorpt_correction_T_min 0.5749 _exptl_absorpt_correction_T_max 0.8741 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38404 _diffrn_reflns_av_R_equivalents 0.1019 _diffrn_reflns_av_sigmaI/netI 0.0729 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 28.26 _reflns_number_total 4635 _reflns_number_gt 3110 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1273P)^2^+7.8607P] 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 4635 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1262 _refine_ls_R_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.2367 _refine_ls_wR_factor_gt 0.1887 _refine_ls_goodness_of_fit_ref 1.160 _refine_ls_restrained_S_all 1.160 _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 Se1 Se 0.36972(8) 0.23043(5) 0.30291(4) 0.0510(3) Uani 1 1 d . . . Fe1 Fe 0.61237(7) 0.04374(4) 0.43071(4) 0.0140(2) Uani 1 1 d . . . O1 O 0.5797(6) 0.1401(4) 0.2075(3) 0.0582(17) Uani 1 1 d . . . N1 N 0.4900(4) 0.1087(3) 0.3841(2) 0.0208(10) Uani 1 1 d . . . N2 N 0.5665(4) 0.0766(2) 0.5212(2) 0.0140(9) Uani 1 1 d . . . N3 N 0.5007(4) 0.0469(2) 0.5726(2) 0.0144(9) Uani 1 1 d . . . N4 N 0.7160(4) 0.1404(3) 0.4369(2) 0.0171(10) Uani 1 1 d . . . N5 N 0.6934(4) 0.0103(3) 0.3477(2) 0.0210(10) Uani 1 1 d . . . N6 N 0.6737(5) 0.0185(3) 0.2827(3) 0.0318(13) Uani 1 1 d . . . H6A H 0.6157 0.0481 0.2655 0.038 Uiso 1 1 calc R . . N7 N 0.7504(4) -0.0217(3) 0.4679(2) 0.0176(10) Uani 1 1 d . . . C1 C 0.4413(6) 0.1548(4) 0.3536(3) 0.0300(15) Uani 1 1 d . . . C2 C 0.6344(5) 0.1362(3) 0.5445(3) 0.0158(11) Uani 1 1 d . . . C3 C 0.6143(5) 0.1458(3) 0.6127(3) 0.0200(12) Uani 1 1 d . . . H3 H 0.6506 0.1826 0.6419 0.024 Uiso 1 1 calc R . . C4 C 0.5294(5) 0.0888(3) 0.6269(3) 0.0186(11) Uani 1 1 d . . . H4 H 0.4952 0.0801 0.6696 0.022 Uiso 1 1 calc R . . C5 C 0.7128(5) 0.1755(3) 0.4966(3) 0.0169(11) Uani 1 1 d . . . C6 C 0.7753(5) 0.2444(3) 0.5088(3) 0.0201(12) Uani 1 1 d . . . H6 H 0.7729 0.2677 0.5515 0.024 Uiso 1 1 calc R . . C7 C 0.8413(6) 0.2784(3) 0.4576(3) 0.0233(13) Uani 1 1 d . . . H7 H 0.8856 0.3252 0.4648 0.028 Uiso 1 1 calc R . . C8 C 0.8420(6) 0.2436(4) 0.3961(3) 0.0252(13) Uani 1 1 d . . . H8 H 0.8846 0.2672 0.3602 0.030 Uiso 1 1 calc R . . C9 C 0.7800(5) 0.1737(3) 0.3870(3) 0.0227(13) Uani 1 1 d . . . H9 H 0.7827 0.1491 0.3449 0.027 Uiso 1 1 calc R . . C10 C 0.7540(8) -0.0245(5) 0.2468(4) 0.050(2) Uani 1 1 d . . . H10 H 0.7583 -0.0271 0.1998 0.060 Uiso 1 1 calc R . . C11 C 0.8287(8) -0.0639(5) 0.2910(4) 0.049(2) Uani 1 1 d . . . H11 H 0.8935 -0.0994 0.2812 0.059 Uiso 1 1 calc R . . C12 C 0.7873(6) -0.0397(4) 0.3537(3) 0.0290(14) Uani 1 1 d . . . C13 C 0.8243(6) -0.0563(4) 0.4214(3) 0.0247(13) Uani 1 1 d . . . C14 C 0.9269(6) -0.1010(4) 0.4390(3) 0.0307(15) Uani 1 1 d . . . H14 H 0.9770 -0.1244 0.4058 0.037 Uiso 1 1 calc R . . C15 C 0.9547(6) -0.1107(4) 0.5049(4) 0.0323(15) Uani 1 1 d . . . H15 H 1.0252 -0.1401 0.5177 0.039 Uiso 1 1 calc R . . C16 C 0.8798(6) -0.0774(4) 0.5524(3) 0.0284(14) Uani 1 1 d . . . H16 H 0.8973 -0.0843 0.5981 0.034 Uiso 1 1 calc R . . C17 C 0.7781(5) -0.0335(3) 0.5322(3) 0.0215(12) Uani 1 1 d . . . H17 H 0.7262 -0.0111 0.5651 0.026 Uiso 1 1 calc R . . 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 Se1 0.0582(6) 0.0670(6) 0.0277(4) 0.0097(3) 0.0030(3) 0.0406(4) Fe1 0.0133(4) 0.0133(4) 0.0153(4) -0.0013(3) 0.0014(3) 0.0010(3) O1 0.071(4) 0.071(4) 0.032(3) 0.007(3) 0.003(3) 0.042(3) N1 0.023(3) 0.023(3) 0.017(2) -0.002(2) -0.0004(19) 0.001(2) N2 0.014(2) 0.012(2) 0.016(2) -0.0002(17) -0.0012(17) 0.0023(18) N3 0.017(2) 0.014(2) 0.013(2) -0.0014(16) 0.0004(17) 0.0016(18) N4 0.014(2) 0.014(2) 0.023(2) 0.0012(18) 0.0004(18) -0.0013(18) N5 0.019(2) 0.023(3) 0.021(2) -0.002(2) 0.0036(19) 0.001(2) N6 0.035(3) 0.039(3) 0.021(3) 0.001(2) 0.006(2) 0.012(3) N7 0.013(2) 0.015(2) 0.025(2) 0.0001(18) -0.0009(19) -0.0032(18) C1 0.028(3) 0.046(4) 0.016(3) -0.005(3) 0.004(3) 0.008(3) C2 0.014(3) 0.014(3) 0.019(3) 0.000(2) -0.001(2) 0.003(2) C3 0.022(3) 0.019(3) 0.019(3) -0.006(2) 0.000(2) 0.004(2) C4 0.021(3) 0.019(3) 0.015(3) -0.002(2) -0.004(2) 0.002(2) C5 0.015(3) 0.016(3) 0.020(3) -0.001(2) -0.002(2) 0.006(2) C6 0.017(3) 0.015(3) 0.028(3) -0.003(2) 0.000(2) 0.001(2) C7 0.020(3) 0.015(3) 0.035(3) -0.003(2) -0.001(3) 0.000(2) C8 0.025(3) 0.022(3) 0.029(3) 0.002(2) 0.002(3) -0.002(3) C9 0.023(3) 0.023(3) 0.022(3) 0.000(2) 0.001(2) -0.004(2) C10 0.053(5) 0.074(6) 0.022(3) 0.005(3) 0.017(3) 0.033(4) C11 0.049(5) 0.064(5) 0.036(4) 0.005(4) 0.017(4) 0.036(4) C12 0.025(3) 0.029(4) 0.032(3) -0.003(3) 0.008(3) 0.006(3) C13 0.016(3) 0.024(3) 0.034(3) 0.001(2) 0.003(3) 0.004(2) C14 0.019(3) 0.029(4) 0.044(4) 0.003(3) 0.006(3) 0.007(3) C15 0.021(3) 0.028(4) 0.048(4) 0.004(3) -0.007(3) 0.009(3) C16 0.028(3) 0.023(3) 0.034(3) 0.007(3) -0.013(3) 0.004(3) C17 0.016(3) 0.023(3) 0.026(3) -0.001(2) -0.007(2) 0.003(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 Se1 C1 1.828(7) . ? Fe1 N1 1.970(5) . ? Fe1 N2 1.974(4) . ? Fe1 N5 1.976(5) . ? Fe1 N3 1.984(5) 5_656 ? Fe1 N4 2.011(5) . ? Fe1 N7 2.014(5) . ? N1 C1 1.134(8) . ? N2 C2 1.347(7) . ? N2 N3 1.357(6) . ? N3 C4 1.348(7) . ? N3 Fe1 1.984(4) 5_656 ? N4 C5 1.348(7) . ? N4 C9 1.349(7) . ? N5 N6 1.334(7) . ? N5 C12 1.335(8) . ? N6 C10 1.350(8) . ? N7 C17 1.346(7) . ? N7 C13 1.369(8) . ? C2 C3 1.402(8) . ? C2 C5 1.452(8) . ? C3 C4 1.372(8) . ? C5 C6 1.388(8) . ? C6 C7 1.384(9) . ? C7 C8 1.378(9) . ? C8 C9 1.390(8) . ? C10 C11 1.380(11) . ? C11 C12 1.405(9) . ? C12 C13 1.451(9) . ? C13 C14 1.394(9) . ? C14 C15 1.372(9) . ? C15 C16 1.377(9) . ? C16 C17 1.394(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 N1 Fe1 N2 96.30(18) . . ? N1 Fe1 N5 93.3(2) . . ? N2 Fe1 N5 168.2(2) . . ? N1 Fe1 N3 91.13(19) . 5_656 ? N2 Fe1 N3 95.93(18) . 5_656 ? N5 Fe1 N3 90.77(19) . 5_656 ? N1 Fe1 N4 86.01(19) . . ? N2 Fe1 N4 81.04(19) . . ? N5 Fe1 N4 92.8(2) . . ? N3 Fe1 N4 175.56(18) 5_656 . ? N1 Fe1 N7 172.80(19) . . ? N2 Fe1 N7 90.10(18) . . ? N5 Fe1 N7 80.0(2) . . ? N3 Fe1 N7 91.48(18) 5_656 . ? N4 Fe1 N7 91.75(18) . . ? C1 N1 Fe1 165.4(5) . . ? C2 N2 N3 107.8(4) . . ? C2 N2 Fe1 113.9(4) . . ? N3 N2 Fe1 136.8(3) . . ? C4 N3 N2 107.3(4) . . ? C4 N3 Fe1 126.2(4) . 5_656 ? N2 N3 Fe1 126.4(3) . 5_656 ? C5 N4 C9 119.2(5) . . ? C5 N4 Fe1 114.4(4) . . ? C9 N4 Fe1 126.3(4) . . ? N6 N5 C12 106.2(5) . . ? N6 N5 Fe1 137.0(4) . . ? C12 N5 Fe1 116.5(4) . . ? N5 N6 C10 111.5(6) . . ? C17 N7 C13 117.8(5) . . ? C17 N7 Fe1 127.4(4) . . ? C13 N7 Fe1 114.8(4) . . ? N1 C1 Se1 177.4(6) . . ? N2 C2 C3 110.4(5) . . ? N2 C2 C5 116.1(5) . . ? C3 C2 C5 133.5(5) . . ? C4 C3 C2 102.9(5) . . ? N3 C4 C3 111.5(5) . . ? N4 C5 C6 122.0(5) . . ? N4 C5 C2 113.6(5) . . ? C6 C5 C2 124.3(5) . . ? C7 C6 C5 118.6(5) . . ? C8 C7 C6 119.4(5) . . ? C7 C8 C9 119.6(6) . . ? N4 C9 C8 121.1(6) . . ? N6 C10 C11 107.3(6) . . ? C10 C11 C12 104.5(6) . . ? N5 C12 C11 110.5(6) . . ? N5 C12 C13 115.0(5) . . ? C11 C12 C13 134.5(6) . . ? N7 C13 C14 121.9(6) . . ? N7 C13 C12 113.5(5) . . ? C14 C13 C12 124.6(6) . . ? C15 C14 C13 119.2(6) . . ? C14 C15 C16 119.6(6) . . ? C15 C16 C17 119.0(6) . . ? N7 C17 C16 122.5(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.870 _refine_diff_density_min -1.756 _refine_diff_density_rms 0.475 #=END data_pbca_123K_Repeat _database_code_depnum_ccdc_archive 'CCDC 220711' _chemical_name_common (Fe(mu-PyPz)(PyPzH)(NCSe))2.2H2O _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H26 Fe2 N14 O2 Se2' _chemical_formula_weight 932.31 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7857(6) _cell_length_b 17.2490(17) _cell_length_c 20.1370(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3746.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Irregular plates' _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 2.770 _exptl_absorpt_correction_type 'not measured' _exptl_absorpt_correction_T_min 0.3380 _exptl_absorpt_correction_T_max 0.7233 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30223 _diffrn_reflns_av_R_equivalents 0.1624 _diffrn_reflns_av_sigmaI/netI 0.1142 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.82 _reflns_number_total 4117 _reflns_number_gt 2231 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1797P)^2^+25.2274P] 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 4117 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2082 _refine_ls_R_factor_gt 0.1112 _refine_ls_wR_factor_ref 0.3453 _refine_ls_wR_factor_gt 0.2654 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _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 Se1 Se 0.36952(15) 0.23066(10) 0.30299(7) 0.0575(6) Uani 1 1 d . . . Fe1 Fe 0.61197(13) 0.04391(9) 0.43049(7) 0.0200(4) Uani 1 1 d . . . O1 O 0.5798(10) 0.1412(6) 0.2077(5) 0.061(3) Uani 1 1 d . . . N1 N 0.4895(7) 0.1084(5) 0.3843(4) 0.025(2) Uani 1 1 d . . . N2 N 0.5655(7) 0.0772(5) 0.5213(4) 0.0171(17) Uani 1 1 d . . . N3 N 0.5002(7) 0.0476(5) 0.5726(4) 0.0194(17) Uani 1 1 d . . . N4 N 0.7150(7) 0.1402(5) 0.4370(4) 0.0229(19) Uani 1 1 d . . . N5 N 0.6925(8) 0.0101(5) 0.3469(4) 0.027(2) Uani 1 1 d . . . N6 N 0.6731(9) 0.0190(6) 0.2822(5) 0.036(2) Uani 1 1 d . . . H6A H 0.6152 0.0486 0.2648 0.043 Uiso 1 1 calc R . . N7 N 0.7516(8) -0.0223(5) 0.4677(4) 0.0230(19) Uani 1 1 d . . . C1 C 0.4392(11) 0.1559(8) 0.3535(5) 0.036(3) Uani 1 1 d . . . C2 C 0.6350(8) 0.1374(6) 0.5450(5) 0.021(2) Uani 1 1 d . . . C3 C 0.6146(9) 0.1453(7) 0.6126(5) 0.026(2) Uani 1 1 d . . . H3 H 0.6518 0.1812 0.6424 0.032 Uiso 1 1 calc R . . C4 C 0.5286(9) 0.0895(6) 0.6266(5) 0.025(2) Uani 1 1 d . . . H4 H 0.4932 0.0814 0.6692 0.030 Uiso 1 1 calc R . . C5 C 0.7111(8) 0.1760(6) 0.4965(5) 0.021(2) Uani 1 1 d . . . C6 C 0.7745(9) 0.2443(6) 0.5089(6) 0.026(2) Uani 1 1 d . . . H6 H 0.7727 0.2673 0.5517 0.031 Uiso 1 1 calc R . . C7 C 0.8415(10) 0.2789(6) 0.4569(6) 0.029(2) Uani 1 1 d . . . H7 H 0.8855 0.3260 0.4637 0.035 Uiso 1 1 calc R . . C8 C 0.8418(10) 0.2433(7) 0.3968(6) 0.029(3) Uani 1 1 d . . . H8 H 0.8848 0.2666 0.3608 0.035 Uiso 1 1 calc R . . C9 C 0.7813(10) 0.1744(6) 0.3871(6) 0.030(3) Uani 1 1 d . . . H9 H 0.7855 0.1499 0.3449 0.035 Uiso 1 1 calc R . . C10 C 0.7557(13) -0.0243(9) 0.2464(7) 0.060(4) Uani 1 1 d . . . H10 H 0.7614 -0.0268 0.1993 0.072 Uiso 1 1 calc R . . C11 C 0.8278(14) -0.0632(10) 0.2904(7) 0.059(5) Uani 1 1 d . . . H11 H 0.8926 -0.0988 0.2807 0.071 Uiso 1 1 calc R . . C12 C 0.7864(11) -0.0397(7) 0.3531(6) 0.034(3) Uani 1 1 d . . . C13 C 0.8248(10) -0.0572(6) 0.4220(6) 0.030(3) Uani 1 1 d . . . C14 C 0.9263(11) -0.1001(7) 0.4392(6) 0.038(3) Uani 1 1 d . . . H14 H 0.9774 -0.1223 0.4058 0.046 Uiso 1 1 calc R . . C15 C 0.9537(11) -0.1108(7) 0.5048(7) 0.040(3) Uani 1 1 d . . . H15 H 1.0238 -0.1408 0.5175 0.049 Uiso 1 1 calc R . . C16 C 0.8792(10) -0.0778(7) 0.5523(6) 0.035(3) Uani 1 1 d . . . H16 H 0.8957 -0.0854 0.5982 0.042 Uiso 1 1 calc R . . C17 C 0.7788(9) -0.0331(6) 0.5319(6) 0.028(2) Uani 1 1 d . . . H17 H 0.7278 -0.0094 0.5646 0.033 Uiso 1 1 calc R . . 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 Se1 0.0588(10) 0.0751(13) 0.0386(8) 0.0096(7) 0.0038(7) 0.0397(8) Fe1 0.0174(7) 0.0200(9) 0.0225(7) -0.0001(6) 0.0019(6) 0.0002(6) O1 0.073(7) 0.066(7) 0.044(6) 0.007(5) -0.003(5) 0.030(6) N1 0.019(4) 0.028(5) 0.026(5) 0.002(4) 0.005(4) -0.003(4) N2 0.012(4) 0.018(5) 0.022(4) -0.002(3) 0.002(3) 0.001(3) N3 0.019(4) 0.020(5) 0.019(4) 0.000(3) 0.000(3) 0.002(3) N4 0.016(4) 0.021(5) 0.031(5) 0.001(4) -0.002(3) -0.002(3) N5 0.021(4) 0.024(5) 0.036(5) -0.001(4) 0.010(4) -0.007(4) N6 0.032(5) 0.050(7) 0.027(5) 0.002(4) 0.004(4) 0.008(5) N7 0.019(4) 0.016(5) 0.033(5) 0.003(4) -0.009(4) 0.003(3) C1 0.028(6) 0.052(9) 0.028(6) -0.010(5) -0.007(5) 0.008(6) C2 0.016(5) 0.016(6) 0.032(5) -0.006(4) -0.001(4) -0.004(4) C3 0.025(5) 0.028(7) 0.026(5) 0.003(4) -0.002(4) 0.007(5) C4 0.025(5) 0.020(6) 0.029(5) -0.001(4) -0.002(4) 0.001(4) C5 0.011(4) 0.020(6) 0.033(6) 0.001(4) -0.003(4) -0.001(4) C6 0.024(5) 0.014(6) 0.039(6) 0.005(5) -0.004(5) 0.004(4) C7 0.028(6) 0.019(6) 0.039(6) 0.000(5) 0.001(5) 0.005(5) C8 0.021(5) 0.026(7) 0.039(7) -0.003(5) 0.001(5) -0.002(5) C9 0.027(6) 0.021(7) 0.041(7) 0.004(5) 0.007(5) 0.002(5) C10 0.058(9) 0.094(12) 0.026(6) 0.006(7) 0.019(6) 0.041(9) C11 0.054(9) 0.085(12) 0.039(8) 0.001(7) 0.017(7) 0.042(9) C12 0.029(6) 0.040(8) 0.034(6) -0.006(5) 0.009(5) 0.002(5) C13 0.025(6) 0.017(6) 0.048(7) -0.002(5) 0.002(5) 0.003(4) C14 0.029(6) 0.033(7) 0.052(8) -0.006(6) 0.005(5) 0.013(5) C15 0.026(6) 0.033(8) 0.063(9) 0.003(6) -0.002(6) 0.008(5) C16 0.027(6) 0.028(7) 0.049(7) 0.001(5) -0.011(5) 0.005(5) C17 0.017(5) 0.020(6) 0.045(7) -0.002(5) -0.009(5) 0.001(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 Se1 C1 1.807(13) . ? Fe1 N1 1.961(9) . ? Fe1 N2 1.981(8) . ? Fe1 N5 1.982(9) . ? Fe1 N3 1.990(8) 5_656 ? Fe1 N4 2.002(8) . ? Fe1 N7 2.033(8) . ? N1 C1 1.162(14) . ? N2 N3 1.351(11) . ? N2 C2 1.367(12) . ? N3 C4 1.340(13) . ? N3 Fe1 1.990(8) 5_656 ? N4 C5 1.348(13) . ? N4 C9 1.367(13) . ? N5 N6 1.328(12) . ? N5 C12 1.333(15) . ? N6 C10 1.368(15) . ? N7 C17 1.337(13) . ? N7 C13 1.355(14) . ? C2 C3 1.386(15) . ? C2 C5 1.439(14) . ? C3 C4 1.366(15) . ? C5 C6 1.385(14) . ? C6 C7 1.405(15) . ? C7 C8 1.358(16) . ? C8 C9 1.369(15) . ? C10 C11 1.357(19) . ? C11 C12 1.401(16) . ? C12 C13 1.479(16) . ? C13 C14 1.365(16) . ? C14 C15 1.367(17) . ? C15 C16 1.373(17) . ? C16 C17 1.392(14) . ? 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 N2 95.9(3) . . ? N1 Fe1 N5 93.4(4) . . ? N2 Fe1 N5 168.5(3) . . ? N1 Fe1 N3 91.5(3) . 5_656 ? N2 Fe1 N3 96.1(3) . 5_656 ? N5 Fe1 N3 90.4(3) . 5_656 ? N1 Fe1 N4 86.2(3) . . ? N2 Fe1 N4 80.8(3) . . ? N5 Fe1 N4 93.2(4) . . ? N3 Fe1 N4 175.9(3) 5_656 . ? N1 Fe1 N7 172.8(4) . . ? N2 Fe1 N7 90.5(3) . . ? N5 Fe1 N7 79.8(4) . . ? N3 Fe1 N7 90.9(3) 5_656 . ? N4 Fe1 N7 91.8(3) . . ? C1 N1 Fe1 165.3(9) . . ? N3 N2 C2 107.8(8) . . ? N3 N2 Fe1 136.8(6) . . ? C2 N2 Fe1 113.8(6) . . ? C4 N3 N2 107.3(8) . . ? C4 N3 Fe1 126.3(7) . 5_656 ? N2 N3 Fe1 126.4(6) . 5_656 ? C5 N4 C9 118.1(9) . . ? C5 N4 Fe1 114.9(7) . . ? C9 N4 Fe1 126.9(7) . . ? N6 N5 C12 106.6(9) . . ? N6 N5 Fe1 136.9(8) . . ? C12 N5 Fe1 116.2(7) . . ? N5 N6 C10 110.6(10) . . ? C17 N7 C13 117.8(9) . . ? C17 N7 Fe1 126.7(7) . . ? C13 N7 Fe1 115.5(7) . . ? N1 C1 Se1 176.6(11) . . ? N2 C2 C3 109.3(9) . . ? N2 C2 C5 115.3(9) . . ? C3 C2 C5 135.4(10) . . ? C4 C3 C2 103.9(10) . . ? N3 C4 C3 111.6(10) . . ? N4 C5 C6 122.3(9) . . ? N4 C5 C2 114.1(9) . . ? C6 C5 C2 123.6(10) . . ? C5 C6 C7 118.8(11) . . ? C8 C7 C6 118.2(11) . . ? C7 C8 C9 121.3(11) . . ? N4 C9 C8 121.3(11) . . ? C11 C10 N6 107.4(11) . . ? C10 C11 C12 105.2(12) . . ? N5 C12 C11 110.1(11) . . ? N5 C12 C13 115.7(9) . . ? C11 C12 C13 134.2(11) . . ? N7 C13 C14 122.4(11) . . ? N7 C13 C12 112.5(9) . . ? C14 C13 C12 125.0(11) . . ? C13 C14 C15 119.5(11) . . ? C14 C15 C16 119.3(11) . . ? C15 C16 C17 118.7(12) . . ? N7 C17 C16 122.2(11) . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 2.537 _refine_diff_density_min -2.664 _refine_diff_density_rms 0.483 #=END data_pbca_298K_Repeat _database_code_depnum_ccdc_archive 'CCDC 220712' _chemical_name_common (Fe(mu-PyPz)(PyPzH)(NCSe))2.2H2O _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H26 Fe2 N14 O2 Se2' _chemical_formula_weight 932.31 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 11.0548(3) _cell_length_b 17.3638(6) _cell_length_c 20.6543(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3964.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Irregular plates' _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 2.618 _exptl_absorpt_correction_type 'not measured' _exptl_absorpt_correction_T_min 0.3544 _exptl_absorpt_correction_T_max 0.7356 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39043 _diffrn_reflns_av_R_equivalents 0.1483 _diffrn_reflns_av_sigmaI/netI 0.1118 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 27.83 _reflns_number_total 4658 _reflns_number_gt 1991 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 4658 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2346 _refine_ls_R_factor_gt 0.1058 _refine_ls_wR_factor_ref 0.3639 _refine_ls_wR_factor_gt 0.2763 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 Se1 Se 0.38688(17) 0.24165(10) 0.28880(8) 0.1198(8) Uani 1 1 d . . . Fe1 Fe 0.60324(10) 0.04851(6) 0.42833(6) 0.0435(5) Uani 1 1 d . . . O1 O 0.5971(16) 0.1422(9) 0.2021(5) 0.215(8) Uani 1 1 d . . . N1 N 0.4835(8) 0.1196(5) 0.3733(4) 0.071(2) Uani 1 1 d . . . N2 N 0.5717(6) 0.0795(4) 0.5258(3) 0.0398(15) Uani 1 1 d . . . N3 N 0.5120(6) 0.0478(3) 0.5759(3) 0.0419(15) Uani 1 1 d . . . N4 N 0.7142(6) 0.1533(4) 0.4420(4) 0.0523(19) Uani 1 1 d . . . N5 N 0.7016(7) 0.0122(4) 0.3407(4) 0.063(2) Uani 1 1 d . . . N6 N 0.6827(11) 0.0171(6) 0.2778(6) 0.100(3) Uani 1 1 d . . . H6A H 0.6342 0.0499 0.2606 0.121 Uiso 1 1 calc R . . N7 N 0.7629(7) -0.0259(4) 0.4617(4) 0.061(2) Uani 1 1 d . . . C1 C 0.4442(10) 0.1672(6) 0.3395(5) 0.066(3) Uani 1 1 d . . . C2 C 0.6388(8) 0.1380(5) 0.5483(4) 0.046(2) Uani 1 1 d . . . C3 C 0.6248(9) 0.1463(6) 0.6137(5) 0.067(3) Uani 1 1 d . . . H3 H 0.6617 0.1818 0.6411 0.080 Uiso 1 1 calc R . . C4 C 0.5424(8) 0.0890(5) 0.6295(4) 0.057(2) Uani 1 1 d . . . H4 H 0.5122 0.0800 0.6709 0.068 Uiso 1 1 calc R . . C5 C 0.7144(7) 0.1815(5) 0.5013(5) 0.052(2) Uani 1 1 d . . . C6 C 0.7783(9) 0.2476(5) 0.5179(6) 0.066(3) Uani 1 1 d . . . H6 H 0.7783 0.2662 0.5602 0.079 Uiso 1 1 calc R . . C7 C 0.8424(10) 0.2849(6) 0.4691(7) 0.076(3) Uani 1 1 d . . . H7 H 0.8859 0.3295 0.4778 0.092 Uiso 1 1 calc R . . C8 C 0.8401(11) 0.2544(6) 0.4076(8) 0.082(4) Uani 1 1 d . . . H8 H 0.8824 0.2783 0.3743 0.099 Uiso 1 1 calc R . . C9 C 0.7778(9) 0.1915(6) 0.3962(5) 0.070(3) Uani 1 1 d . . . H9 H 0.7775 0.1720 0.3543 0.084 Uiso 1 1 calc R . . C10 C 0.7478(19) -0.0353(11) 0.2427(8) 0.163(8) Uani 1 1 d . . . H10 H 0.7435 -0.0457 0.1986 0.196 Uiso 1 1 calc R . . C11 C 0.821(2) -0.0688(11) 0.2883(8) 0.158(8) Uani 1 1 d . . . H11 H 0.8825 -0.1038 0.2796 0.190 Uiso 1 1 calc R . . C12 C 0.7886(10) -0.0420(6) 0.3505(6) 0.080(3) Uani 1 1 d . . . C13 C 0.8291(9) -0.0573(5) 0.4151(5) 0.061(3) Uani 1 1 d . . . C14 C 0.9277(11) -0.1012(7) 0.4278(7) 0.089(4) Uani 1 1 d . . . H14 H 0.9739 -0.1213 0.3942 0.107 Uiso 1 1 calc R . . C15 C 0.9565(11) -0.1149(8) 0.4877(10) 0.109(5) Uani 1 1 d . . . H15 H 1.0216 -0.1472 0.4964 0.131 Uiso 1 1 calc R . . C16 C 0.8933(11) -0.0827(8) 0.5395(8) 0.095(4) Uani 1 1 d . . . H16 H 0.9157 -0.0902 0.5825 0.114 Uiso 1 1 calc R . . C17 C 0.7934(10) -0.0380(6) 0.5214(6) 0.074(3) Uani 1 1 d . . . H17 H 0.7465 -0.0159 0.5538 0.089 Uiso 1 1 calc R . . 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 Se1 0.1367(16) 0.1356(14) 0.0870(11) 0.0231(8) -0.0057(9) 0.0674(11) Fe1 0.0367(7) 0.0463(8) 0.0476(8) 0.0008(5) 0.0034(5) 0.0005(5) O1 0.30(2) 0.243(15) 0.103(9) 0.018(9) -0.008(10) 0.170(14) N1 0.063(6) 0.086(5) 0.064(5) 0.003(4) -0.010(5) 0.015(5) N2 0.032(4) 0.043(4) 0.045(4) 0.003(3) 0.000(3) -0.003(3) N3 0.039(4) 0.043(4) 0.044(4) -0.001(3) -0.003(3) -0.002(3) N4 0.041(4) 0.044(4) 0.072(5) 0.005(4) 0.004(4) -0.001(3) N5 0.060(5) 0.070(5) 0.058(5) -0.003(4) 0.013(4) 0.007(4) N6 0.106(9) 0.111(8) 0.084(8) 0.007(6) 0.017(7) 0.033(7) N7 0.044(5) 0.062(5) 0.076(6) 0.008(4) -0.006(4) 0.002(4) C1 0.057(6) 0.077(7) 0.064(7) -0.005(5) -0.003(5) 0.017(5) C2 0.037(5) 0.045(5) 0.056(5) -0.001(4) -0.001(4) 0.007(4) C3 0.069(7) 0.060(6) 0.070(7) -0.004(5) -0.023(6) 0.000(5) C4 0.045(5) 0.079(6) 0.047(5) -0.004(5) 0.002(4) 0.001(5) C5 0.036(5) 0.042(5) 0.077(6) -0.007(4) -0.009(5) 0.006(4) C6 0.050(6) 0.052(5) 0.095(8) -0.009(5) -0.005(6) -0.006(5) C7 0.048(6) 0.055(6) 0.126(11) 0.004(7) 0.009(7) -0.013(5) C8 0.065(7) 0.063(7) 0.120(12) 0.028(7) 0.011(7) -0.009(6) C9 0.063(7) 0.067(6) 0.079(7) 0.012(5) 0.012(6) -0.016(5) C10 0.19(2) 0.218(18) 0.083(11) -0.007(12) 0.062(12) 0.090(16) C11 0.21(2) 0.183(16) 0.082(10) 0.015(10) 0.043(12) 0.132(15) C12 0.063(7) 0.075(7) 0.102(10) -0.004(6) 0.044(7) 0.014(6) C13 0.049(6) 0.057(6) 0.076(7) 0.010(5) 0.014(5) 0.014(5) C14 0.061(8) 0.098(10) 0.108(11) 0.016(8) 0.019(7) 0.022(7) C15 0.040(7) 0.098(9) 0.189(18) 0.008(11) -0.003(9) 0.024(6) C16 0.065(8) 0.093(9) 0.128(12) 0.025(8) -0.035(8) 0.014(7) C17 0.064(7) 0.072(7) 0.088(8) 0.001(6) -0.021(6) 0.010(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 Se1 C1 1.780(10) . ? Fe1 N3 2.104(6) 5_656 ? Fe1 N2 2.113(7) . ? Fe1 N1 2.137(8) . ? Fe1 N5 2.204(8) . ? Fe1 N4 2.212(7) . ? Fe1 N7 2.294(8) . ? N1 C1 1.166(11) . ? N2 C2 1.340(10) . ? N2 N3 1.345(9) . ? N3 C4 1.361(10) . ? N3 Fe1 2.104(6) 5_656 ? N4 C5 1.319(11) . ? N4 C9 1.352(11) . ? N5 N6 1.318(13) . ? N5 C12 1.361(13) . ? N6 C10 1.368(17) . ? N7 C17 1.295(13) . ? N7 C13 1.325(12) . ? C2 C3 1.369(13) . ? C2 C5 1.487(13) . ? C3 C4 1.388(13) . ? C5 C6 1.391(12) . ? C6 C7 1.393(16) . ? C7 C8 1.376(18) . ? C8 C9 1.313(15) . ? C10 C11 1.37(2) . ? C11 C12 1.412(18) . ? C12 C13 1.433(16) . ? C13 C14 1.356(15) . ? C14 C15 1.300(17) . ? C15 C16 1.39(2) . ? C16 C17 1.401(14) . ? 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 N3 Fe1 N2 98.2(2) 5_656 . ? N3 Fe1 N1 93.6(3) 5_656 . ? N2 Fe1 N1 104.9(3) . . ? N3 Fe1 N5 92.1(3) 5_656 . ? N2 Fe1 N5 159.5(3) . . ? N1 Fe1 N5 92.0(3) . . ? N3 Fe1 N4 174.0(3) 5_656 . ? N2 Fe1 N4 76.1(3) . . ? N1 Fe1 N4 86.4(3) . . ? N5 Fe1 N4 93.8(3) . . ? N3 Fe1 N7 91.7(3) 5_656 . ? N2 Fe1 N7 89.1(3) . . ? N1 Fe1 N7 164.1(3) . . ? N5 Fe1 N7 72.9(3) . . ? N4 Fe1 N7 89.9(3) . . ? C1 N1 Fe1 163.4(9) . . ? C2 N2 N3 108.4(7) . . ? C2 N2 Fe1 115.6(5) . . ? N3 N2 Fe1 135.2(5) . . ? N2 N3 C4 106.9(7) . . ? N2 N3 Fe1 126.2(5) . 5_656 ? C4 N3 Fe1 126.9(6) . 5_656 ? C5 N4 C9 117.8(8) . . ? C5 N4 Fe1 115.1(6) . . ? C9 N4 Fe1 127.1(7) . . ? N6 N5 C12 107.7(9) . . ? N6 N5 Fe1 135.4(7) . . ? C12 N5 Fe1 115.1(7) . . ? N5 N6 C10 113.3(12) . . ? C17 N7 C13 118.7(9) . . ? C17 N7 Fe1 125.3(7) . . ? C13 N7 Fe1 116.0(7) . . ? N1 C1 Se1 178.5(10) . . ? N2 C2 C3 111.1(8) . . ? N2 C2 C5 118.1(8) . . ? C3 C2 C5 130.9(8) . . ? C2 C3 C4 103.4(8) . . ? N3 C4 C3 110.3(8) . . ? N4 C5 C6 122.5(9) . . ? N4 C5 C2 114.6(7) . . ? C6 C5 C2 122.9(9) . . ? C5 C6 C7 117.5(11) . . ? C8 C7 C6 118.7(10) . . ? C9 C8 C7 119.7(11) . . ? C8 C9 N4 123.8(11) . . ? N6 C10 C11 103.2(14) . . ? C10 C11 C12 109.6(13) . . ? N5 C12 C11 105.8(12) . . ? N5 C12 C13 119.1(9) . . ? C11 C12 C13 135.1(11) . . ? N7 C13 C14 122.4(11) . . ? N7 C13 C12 115.3(9) . . ? C14 C13 C12 122.3(11) . . ? C15 C14 C13 118.9(12) . . ? C14 C15 C16 122.3(12) . . ? C15 C16 C17 114.3(13) . . ? N7 C17 C16 123.3(12) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.989 _refine_diff_density_min -1.920 _refine_diff_density_rms 0.288 #=END