Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_sad _database_code_CSD 195714 _journal_coden_Cambridge 182 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Judith A. K. Howard' 'Ivana Radosavljevic Evans' 'Andres E. Goeta' 'Malcolm A. Halcrow' 'Victoria A. Money' _publ_contact_author_name 'Prof Judith A. K Howard' _publ_contact_author_address ; Prof Judith A. K Howard Chemistry University of Durham Science Site South Road Durham DH1 3LE UNITED KINGDOM ; _publ_contact_author_email 'J.A.K.HOWARD@DURHAM.AC.UK' _publ_section_title ; Light induced excited state spin trapping in [FeL2](BF4)2 (L = 2,6-di(pyrazol-1-yl)pyridine) ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H18 B2 F8 Fe N10' _chemical_formula_weight 651.93 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.4615(17) _cell_length_b 8.3695(17) _cell_length_c 18.759(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.15(3) _cell_angle_gamma 90.00 _cell_volume 1318.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 30(2) _cell_measurement_reflns_used 9499 _cell_measurement_theta_min 2.785 _cell_measurement_theta_max 27.418 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 0.663 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.810271 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 30(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 'Brucker Smart' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11729 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 27.46 _reflns_number_total 5269 _reflns_number_gt 5071 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.060 (Bruker, 1999)' _computing_cell_refinement 'SMART version 5.060 (Bruker, 1999)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 5.10 (Bruker, 1997)' _computing_publication_material 'SHELXTL version 5.10 (Bruker, 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^)+(0.0424P)^2^+0.0678P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.023(11) _refine_ls_number_reflns 5269 _refine_ls_number_parameters 388 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0759 _refine_ls_wR_factor_gt 0.0749 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 0.24185(3) 0.89641(4) 0.246479(14) 0.00877(8) Uani 1 1 d . . . N1 N 0.0003(2) 0.9761(2) 0.20646(9) 0.0103(3) Uani 1 1 d . . . N2 N -0.02873(19) 0.9832(2) 0.13296(9) 0.0099(3) Uani 1 1 d . . . C1 C -0.1330(2) 1.0256(3) 0.22956(12) 0.0110(4) Uani 1 1 d . . . H1 H -0.1488 1.0310 0.2777 0.013 Uiso 1 1 calc R . . C2 C -0.2480(3) 1.0691(3) 0.17183(12) 0.0126(4) Uani 1 1 d . . . H2 H -0.3496 1.1093 0.1743 0.015 Uiso 1 1 calc R . . C3 C -0.1778(2) 1.0392(3) 0.11135(12) 0.0116(4) Uani 1 1 d . . . H3 H -0.2236 1.0545 0.0641 0.014 Uiso 1 1 calc R . . N3 N 0.22299(18) 0.8845(3) 0.13243(9) 0.0097(3) Uani 1 1 d . . . C4 C 0.0918(2) 0.9369(2) 0.09163(11) 0.0098(4) Uani 1 1 d . . . C5 C 0.0773(2) 0.9419(3) 0.01782(11) 0.0111(4) Uani 1 1 d . . . H5 H -0.0157 0.9771 -0.0093 0.013 Uiso 1 1 calc R . . C6 C 0.2082(2) 0.8919(3) -0.01434(10) 0.0110(4) Uani 1 1 d . . . H6 H 0.2033 0.8952 -0.0641 0.013 Uiso 1 1 calc R . . C7 C 0.3460(2) 0.8373(3) 0.02618(11) 0.0106(4) Uani 1 1 d . . . H7 H 0.4341 0.8041 0.0050 0.013 Uiso 1 1 calc R . . C8 C 0.3451(2) 0.8349(3) 0.10003(11) 0.0100(4) Uani 1 1 d . . . N4 N 0.47286(19) 0.7773(2) 0.14868(9) 0.0095(3) Uani 1 1 d . . . N5 N 0.4654(2) 0.7974(2) 0.22074(9) 0.0112(4) Uani 1 1 d . . . C9 C 0.6024(2) 0.6900(3) 0.13694(12) 0.0124(4) Uani 1 1 d . . . H9 H 0.6313 0.6605 0.0925 0.015 Uiso 1 1 calc R . . C10 C 0.6824(2) 0.6537(3) 0.20287(12) 0.0132(4) Uani 1 1 d . . . H10 H 0.7761 0.5951 0.2124 0.016 Uiso 1 1 calc R . . N6 N 0.3455(2) 1.1133(2) 0.29624(9) 0.0109(3) Uani 1 1 d . . . N7 N 0.34658(19) 1.1189(2) 0.36938(9) 0.0102(4) Uani 1 1 d . . . C11 C 0.5939(2) 0.7233(3) 0.25290(11) 0.0117(4) Uani 1 1 d . . . H11 H 0.6214 0.7184 0.3024 0.014 Uiso 1 1 calc R . . C12 C 0.4157(2) 1.2469(3) 0.27933(11) 0.0119(4) Uani 1 1 d . . . H12 H 0.4312 1.2759 0.2329 0.014 Uiso 1 1 calc R . . C13 C 0.4638(2) 1.3396(3) 0.34101(11) 0.0124(4) Uani 1 1 d . . . H13 H 0.5161 1.4375 0.3431 0.015 Uiso 1 1 calc R . . C14 C 0.4173(2) 1.2548(3) 0.39699(11) 0.0116(4) Uani 1 1 d . . . H14 H 0.4315 1.2846 0.4451 0.014 Uiso 1 1 calc R . . N8 N 0.23495(19) 0.8706(2) 0.35920(9) 0.0099(4) Uani 1 1 d . . . C15 C 0.2870(2) 0.9874(3) 0.40437(11) 0.0100(4) Uani 1 1 d . . . C16 C 0.2839(2) 0.9788(3) 0.47808(11) 0.0110(4) Uani 1 1 d . . . H16 H 0.3201 1.0624 0.5085 0.013 Uiso 1 1 calc R . . C17 C 0.2241(2) 0.8392(3) 0.50390(11) 0.0111(4) Uani 1 1 d . . . H17 H 0.2188 0.8290 0.5529 0.013 Uiso 1 1 calc R . . C18 C 0.1720(2) 0.7140(3) 0.45840(11) 0.0117(4) Uani 1 1 d . . . H18 H 0.1336 0.6192 0.4757 0.014 Uiso 1 1 calc R . . C19 C 0.1801(2) 0.7376(3) 0.38629(11) 0.0111(4) Uani 1 1 d . . . N9 N 0.13246(19) 0.6221(2) 0.33271(9) 0.0107(4) Uani 1 1 d . . . N10 N 0.1543(2) 0.6550(2) 0.26360(9) 0.0116(4) Uani 1 1 d . . . C20 C 0.0699(2) 0.4742(3) 0.33867(12) 0.0129(4) Uani 1 1 d . . . H20 H 0.0443 0.4266 0.3806 0.016 Uiso 1 1 calc R . . C21 C 0.0513(2) 0.4080(3) 0.27122(10) 0.0132(4) Uani 1 1 d . . . H21 H 0.0112 0.3075 0.2579 0.016 Uiso 1 1 calc R . . C22 C 0.1062(2) 0.5255(3) 0.22678(11) 0.0117(4) Uani 1 1 d . . . H22 H 0.1083 0.5137 0.1776 0.014 Uiso 1 1 calc R . . B1 B 0.2210(3) 0.3428(3) 0.56943(13) 0.0124(5) Uani 1 1 d . . . F1 F 0.15443(14) 0.33706(16) 0.49702(6) 0.0141(3) Uani 1 1 d . . . F2 F 0.17387(17) 0.48198(19) 0.60080(7) 0.0227(3) Uani 1 1 d . . . F3 F 0.17489(15) 0.20942(17) 0.60556(7) 0.0163(3) Uani 1 1 d . . . F4 F 0.38805(14) 0.33991(18) 0.57133(7) 0.0192(3) Uani 1 1 d . . . B2 B 0.2971(3) 0.3286(3) 0.07843(13) 0.0117(5) Uani 1 1 d . . . F5 F 0.27404(14) 0.26632(16) 0.00844(6) 0.0142(3) Uani 1 1 d . . . F6 F 0.18736(15) 0.26277(16) 0.11957(7) 0.0144(3) Uani 1 1 d . . . F7 F 0.27688(15) 0.49435(17) 0.07482(7) 0.0144(3) Uani 1 1 d . . . F8 F 0.45199(14) 0.29215(18) 0.10946(6) 0.0175(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 0.00677(12) 0.01101(15) 0.00809(13) -0.00065(12) -0.00089(9) -0.00002(12) N1 0.0098(8) 0.0112(9) 0.0092(8) -0.0006(7) -0.0014(6) -0.0012(7) N2 0.0068(7) 0.0126(9) 0.0095(8) 0.0003(7) -0.0018(6) 0.0003(7) C1 0.0105(9) 0.0094(11) 0.0133(10) -0.0006(8) 0.0018(8) -0.0011(8) C2 0.0099(10) 0.0106(11) 0.0171(11) 0.0001(9) 0.0011(8) -0.0003(8) C3 0.0082(9) 0.0106(11) 0.0150(10) 0.0022(9) -0.0033(8) 0.0004(8) N3 0.0074(7) 0.0094(9) 0.0116(7) 0.0016(8) -0.0015(6) 0.0014(8) C4 0.0080(8) 0.0076(11) 0.0135(9) -0.0006(7) 0.0004(7) -0.0014(7) C5 0.0075(8) 0.0122(11) 0.0128(10) 0.0015(8) -0.0022(7) -0.0013(7) C6 0.0131(8) 0.0116(10) 0.0076(8) -0.0010(9) -0.0020(7) -0.0010(10) C7 0.0078(9) 0.0110(10) 0.0127(10) 0.0000(8) 0.0002(8) -0.0001(7) C8 0.0087(9) 0.0083(10) 0.0123(9) 0.0007(8) -0.0011(8) -0.0009(7) N4 0.0077(8) 0.0129(9) 0.0073(7) 0.0011(7) -0.0013(6) -0.0006(7) N5 0.0108(8) 0.0126(10) 0.0101(8) 0.0008(7) 0.0009(6) 0.0001(7) C9 0.0109(9) 0.0109(11) 0.0157(10) -0.0005(8) 0.0033(8) 0.0003(8) C10 0.0093(9) 0.0124(11) 0.0172(11) 0.0013(9) -0.0008(8) 0.0003(8) N6 0.0088(8) 0.0148(9) 0.0085(8) 0.0002(7) -0.0016(6) 0.0017(7) N7 0.0082(8) 0.0139(10) 0.0081(8) -0.0017(7) -0.0009(6) 0.0010(7) C11 0.0081(9) 0.0139(11) 0.0119(10) 0.0032(9) -0.0032(8) -0.0021(8) C12 0.0083(9) 0.0166(12) 0.0104(10) 0.0021(9) 0.0001(7) 0.0014(8) C13 0.0089(9) 0.0139(11) 0.0140(9) 0.0007(8) -0.0005(8) -0.0024(8) C14 0.0078(9) 0.0141(12) 0.0125(10) -0.0023(8) -0.0008(8) -0.0014(8) N8 0.0069(7) 0.0111(11) 0.0114(8) -0.0012(7) -0.0004(6) 0.0006(7) C15 0.0055(8) 0.0103(11) 0.0138(10) -0.0013(9) -0.0007(7) 0.0021(8) C16 0.0079(9) 0.0138(11) 0.0105(9) -0.0021(9) -0.0024(7) 0.0023(8) C17 0.0071(9) 0.0166(11) 0.0091(9) 0.0002(8) -0.0009(7) 0.0021(7) C18 0.0097(9) 0.0135(11) 0.0118(10) 0.0039(8) 0.0001(8) 0.0004(8) C19 0.0046(9) 0.0123(11) 0.0161(10) -0.0018(9) -0.0003(8) 0.0009(8) N9 0.0081(8) 0.0135(9) 0.0101(8) -0.0002(7) -0.0007(6) 0.0015(7) N10 0.0098(8) 0.0145(10) 0.0101(8) 0.0013(7) 0.0006(7) 0.0015(7) C20 0.0088(9) 0.0136(11) 0.0166(10) 0.0018(9) 0.0022(8) -0.0005(8) C21 0.0091(8) 0.0148(11) 0.0153(9) -0.0014(10) -0.0005(7) 0.0008(9) C22 0.0071(9) 0.0153(12) 0.0121(10) -0.0014(9) -0.0010(8) 0.0026(8) B1 0.0121(11) 0.0147(12) 0.0102(10) 0.0012(9) 0.0011(9) 0.0007(9) F1 0.0132(6) 0.0172(7) 0.0115(6) 0.0018(5) -0.0003(5) 0.0010(5) F2 0.0332(8) 0.0208(8) 0.0140(6) -0.0023(6) 0.0023(6) 0.0081(6) F3 0.0116(6) 0.0215(8) 0.0149(6) 0.0057(6) -0.0021(5) -0.0021(5) F4 0.0104(6) 0.0315(8) 0.0151(6) 0.0007(6) -0.0006(5) -0.0066(5) B2 0.0098(10) 0.0129(12) 0.0120(11) 0.0024(9) 0.0000(9) 0.0013(9) F5 0.0143(6) 0.0164(7) 0.0116(6) -0.0012(5) 0.0011(5) -0.0005(5) F6 0.0138(6) 0.0141(7) 0.0158(6) -0.0009(5) 0.0040(5) -0.0033(5) F7 0.0139(6) 0.0122(7) 0.0162(6) 0.0010(5) -0.0018(5) -0.0010(5) F8 0.0105(6) 0.0275(8) 0.0138(6) 0.0030(6) -0.0008(5) 0.0058(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 N3 2.1278(17) . ? Fe1 N8 2.1335(17) . ? Fe1 N5 2.1737(18) . ? Fe1 N6 2.175(2) . ? Fe1 N10 2.189(2) . ? Fe1 N1 2.1920(18) . ? N1 C1 1.324(3) . ? N1 N2 1.371(2) . ? N2 C3 1.359(3) . ? N2 C4 1.410(3) . ? C1 C2 1.410(3) . ? C2 C3 1.368(3) . ? N3 C8 1.329(3) . ? N3 C4 1.341(3) . ? C4 C5 1.375(3) . ? C5 C6 1.390(3) . ? C6 C7 1.388(3) . ? C7 C8 1.386(3) . ? C8 N4 1.410(3) . ? N4 C9 1.358(3) . ? N4 N5 1.371(2) . ? N5 C11 1.329(3) . ? C9 C10 1.368(3) . ? C10 C11 1.399(3) . ? N6 C12 1.323(3) . ? N6 N7 1.372(2) . ? N7 C14 1.358(3) . ? N7 C15 1.407(3) . ? C12 C13 1.410(3) . ? C13 C14 1.365(3) . ? N8 C19 1.330(3) . ? N8 C15 1.332(3) . ? C15 C16 1.388(3) . ? C16 C17 1.384(3) . ? C17 C18 1.389(3) . ? C18 C19 1.377(3) . ? C19 N9 1.417(3) . ? N9 C20 1.357(3) . ? N9 N10 1.360(2) . ? N10 C22 1.322(3) . ? C20 C21 1.372(3) . ? C21 C22 1.405(3) . ? B1 F2 1.386(3) . ? B1 F3 1.387(3) . ? B1 F1 1.405(3) . ? B1 F4 1.410(3) . ? B2 F6 1.393(3) . ? B2 F7 1.398(3) . ? B2 F8 1.400(3) . ? B2 F5 1.403(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Fe1 N8 169.68(8) . . ? N3 Fe1 N5 73.57(7) . . ? N8 Fe1 N5 108.26(7) . . ? N3 Fe1 N6 116.51(7) . . ? N8 Fe1 N6 73.66(7) . . ? N5 Fe1 N6 95.62(7) . . ? N3 Fe1 N10 96.88(7) . . ? N8 Fe1 N10 73.11(7) . . ? N5 Fe1 N10 90.01(7) . . ? N6 Fe1 N10 146.39(7) . . ? N3 Fe1 N1 73.73(7) . . ? N8 Fe1 N1 103.35(7) . . ? N5 Fe1 N1 147.15(7) . . ? N6 Fe1 N1 101.67(7) . . ? N10 Fe1 N1 90.74(7) . . ? C1 N1 N2 105.21(17) . . ? C1 N1 Fe1 141.18(15) . . ? N2 N1 Fe1 113.58(12) . . ? C3 N2 N1 110.99(17) . . ? C3 N2 C4 129.69(18) . . ? N1 N2 C4 119.32(16) . . ? N1 C1 C2 111.32(19) . . ? C3 C2 C1 105.11(19) . . ? N2 C3 C2 107.35(19) . . ? C8 N3 C4 118.46(18) . . ? C8 N3 Fe1 120.62(13) . . ? C4 N3 Fe1 120.77(14) . . ? N3 C4 C5 123.26(19) . . ? N3 C4 N2 112.33(18) . . ? C5 C4 N2 124.41(18) . . ? C4 C5 C6 116.85(18) . . ? C7 C6 C5 121.47(18) . . ? C8 C7 C6 116.31(18) . . ? N3 C8 C7 123.64(19) . . ? N3 C8 N4 112.82(18) . . ? C7 C8 N4 123.53(18) . . ? C9 N4 N5 111.29(17) . . ? C9 N4 C8 130.42(18) . . ? N5 N4 C8 118.05(17) . . ? C11 N5 N4 104.75(17) . . ? C11 N5 Fe1 139.65(15) . . ? N4 N5 Fe1 114.45(12) . . ? N4 C9 C10 106.94(19) . . ? C9 C10 C11 105.55(19) . . ? C12 N6 N7 105.29(18) . . ? C12 N6 Fe1 140.49(15) . . ? N7 N6 Fe1 114.18(14) . . ? C14 N7 N6 110.96(18) . . ? C14 N7 C15 130.10(17) . . ? N6 N7 C15 118.82(18) . . ? N5 C11 C10 111.46(19) . . ? N6 C12 C13 111.14(19) . . ? C14 C13 C12 105.3(2) . . ? N7 C14 C13 107.32(19) . . ? C19 N8 C15 118.30(18) . . ? C19 N8 Fe1 121.15(15) . . ? C15 N8 Fe1 120.55(15) . . ? N8 C15 C16 123.4(2) . . ? N8 C15 N7 112.74(18) . . ? C16 C15 N7 123.9(2) . . ? C17 C16 C15 116.4(2) . . ? C16 C17 C18 121.60(19) . . ? C19 C18 C17 116.4(2) . . ? N8 C19 C18 123.9(2) . . ? N8 C19 N9 112.44(18) . . ? C18 C19 N9 123.6(2) . . ? C20 N9 N10 111.34(18) . . ? C20 N9 C19 130.09(18) . . ? N10 N9 C19 118.53(18) . . ? C22 N10 N9 105.23(18) . . ? C22 N10 Fe1 140.15(15) . . ? N9 N10 Fe1 114.52(14) . . ? N9 C20 C21 107.06(19) . . ? C20 C21 C22 104.8(2) . . ? N10 C22 C21 111.52(19) . . ? F2 B1 F3 110.84(17) . . ? F2 B1 F1 109.72(19) . . ? F3 B1 F1 109.97(19) . . ? F2 B1 F4 110.14(19) . . ? F3 B1 F4 108.41(18) . . ? F1 B1 F4 107.69(17) . . ? F6 B2 F7 109.45(19) . . ? F6 B2 F8 109.73(19) . . ? F7 B2 F8 109.8(2) . . ? F6 B2 F5 110.28(19) . . ? F7 B2 F5 108.7(2) . . ? F8 B2 F5 108.81(18) . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.582 _refine_diff_density_min -0.639 _refine_diff_density_rms 0.064 data_30ffcor _database_code_CSD 195715 _journal_coden_Cambridge 182 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Judith A. K. Howard' 'Ivana Radosavljevic Evans' 'Andres E. Goeta' 'Malcolm A. Halcrow' 'Victoria A. Money' _publ_contact_author_name 'Prof Judith A. K Howard' _publ_contact_author_address ; Prof Judith A. K Howard Chemistry University of Durham Science Site South Road Durham DH1 3LE UNITED KINGDOM ; _publ_contact_author_email 'J.A.K.HOWARD@DURHAM.AC.UK' _publ_section_title ; Light induced excited state spin trapping in [FeL2](BF4)2 (L = 2,6-di(pyrazol-1-yl)pyridine) ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H18 B2 F8 Fe N10' _chemical_formula_weight 651.93 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.4098(4) _cell_length_b 8.4731(4) _cell_length_c 18.2909(9) _cell_angle_alpha 90.00 _cell_angle_beta 98.5750(10) _cell_angle_gamma 90.00 _cell_volume 1288.79(11) _cell_formula_units_Z 2 _cell_measurement_temperature 30(2) _cell_measurement_reflns_used 7139 _cell_measurement_theta_min 2.6545 _cell_measurement_theta_max 27.4285 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 0.679 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.878917 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 30(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 'Bruker Smart' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11476 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 27.45 _reflns_number_total 5434 _reflns_number_gt 5038 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.060 (Bruker, 1999)' _computing_cell_refinement 'SMART version 5.060 (Bruker, 1999)' _computing_data_reduction 'SAINT version 6.02A (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL version 5.10 (Bruker, 1997)' _computing_publication_material 'SHELXTL version 5.10 (Bruker, 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^)+(0.0262P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.022(11) _refine_ls_number_reflns 5434 _refine_ls_number_parameters 388 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0691 _refine_ls_wR_factor_gt 0.0675 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.023 _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 0.21379(4) 0.89126(4) 0.246267(17) 0.00784(8) Uani 1 1 d . . . N1 N -0.0024(2) 0.9857(2) 0.21844(11) 0.0098(4) Uani 1 1 d . . . N2 N -0.0376(2) 1.0136(2) 0.14311(11) 0.0092(4) Uani 1 1 d . . . C1 C -0.1316(3) 1.0338(3) 0.24598(14) 0.0110(5) Uani 1 1 d . . . H1 H -0.1428 1.0295 0.2958 0.013 Uiso 1 1 calc R . . C2 C -0.2495(3) 1.0924(3) 0.18967(13) 0.0118(5) Uani 1 1 d . . . H2 H -0.3497 1.1332 0.1951 0.014 Uiso 1 1 calc R . . C3 C -0.1864(3) 1.0770(3) 0.12564(14) 0.0112(5) Uani 1 1 d . . . H3 H -0.2363 1.1050 0.0786 0.013 Uiso 1 1 calc R . . N3 N 0.2097(2) 0.9108(3) 0.14276(10) 0.0090(4) Uani 1 1 d . . . C4 C 0.0800(3) 0.9707(3) 0.10008(13) 0.0103(5) Uani 1 1 d . . . C5 C 0.0709(3) 0.9844(3) 0.02460(13) 0.0113(5) Uani 1 1 d . . . H5 H -0.0195 1.0264 -0.0044 0.014 Uiso 1 1 calc R . . C6 C 0.2028(3) 0.9327(3) -0.00630(13) 0.0109(5) Uani 1 1 d . . . H6 H 0.2006 0.9412 -0.0571 0.013 Uiso 1 1 calc R . . C7 C 0.3368(3) 0.8691(3) 0.03598(12) 0.0117(5) Uani 1 1 d . . . H7 H 0.4245 0.8342 0.0149 0.014 Uiso 1 1 calc R . . C8 C 0.3347(3) 0.8597(3) 0.11117(12) 0.0095(5) Uani 1 1 d . . . N4 N 0.4541(2) 0.7949(3) 0.16475(10) 0.0096(4) Uani 1 1 d . . . N5 N 0.4258(2) 0.8024(3) 0.23689(11) 0.0104(4) Uani 1 1 d . . . C9 C 0.5947(3) 0.7207(3) 0.15991(13) 0.0108(5) Uani 1 1 d . . . H9 H 0.6382 0.7011 0.1170 0.013 Uiso 1 1 calc R . . C10 C 0.6604(3) 0.6801(3) 0.23029(13) 0.0130(5) Uani 1 1 d . . . H10 H 0.7572 0.6278 0.2449 0.016 Uiso 1 1 calc R . . N6 N 0.3124(2) 1.0948(2) 0.28333(11) 0.0097(4) Uani 1 1 d . . . N7 N 0.3306(2) 1.1051(2) 0.35941(10) 0.0095(4) Uani 1 1 d . . . C11 C 0.5517(3) 0.7337(3) 0.27603(13) 0.0110(5) Uani 1 1 d . . . H11 H 0.5663 0.7223 0.3272 0.013 Uiso 1 1 calc R . . C12 C 0.3786(3) 1.2246(3) 0.26165(13) 0.0113(5) Uani 1 1 d . . . H12 H 0.3832 1.2501 0.2126 0.014 Uiso 1 1 calc R . . C13 C 0.4412(3) 1.3194(3) 0.32222(13) 0.0118(5) Uani 1 1 d . . . H13 H 0.4936 1.4158 0.3211 0.014 Uiso 1 1 calc R . . C14 C 0.4082(3) 1.2387(3) 0.38358(14) 0.0123(5) Uani 1 1 d . . . H14 H 0.4345 1.2705 0.4326 0.015 Uiso 1 1 calc R . . N8 N 0.2177(2) 0.8626(2) 0.34962(10) 0.0088(4) Uani 1 1 d . . . C15 C 0.2777(3) 0.9753(3) 0.39739(13) 0.0091(5) Uani 1 1 d . . . C16 C 0.2863(3) 0.9588(3) 0.47241(13) 0.0113(5) Uani 1 1 d . . . H16 H 0.3273 1.0385 0.5048 0.014 Uiso 1 1 calc R . . C17 C 0.2305(3) 0.8171(3) 0.49800(13) 0.0120(5) Uani 1 1 d . . . H17 H 0.2344 0.8020 0.5486 0.014 Uiso 1 1 calc R . . C18 C 0.1697(3) 0.6985(3) 0.44983(13) 0.0123(5) Uani 1 1 d . . . H18 H 0.1330 0.6038 0.4668 0.015 Uiso 1 1 calc R . . C19 C 0.1659(3) 0.7273(3) 0.37568(13) 0.0100(5) Uani 1 1 d . . . N9 N 0.1109(2) 0.6245(2) 0.31707(11) 0.0105(4) Uani 1 1 d . . . N10 N 0.1239(2) 0.6773(2) 0.24683(10) 0.0099(4) Uani 1 1 d . . . C20 C 0.0545(3) 0.4741(3) 0.31519(14) 0.0122(5) Uani 1 1 d . . . H20 H 0.0357 0.4141 0.3556 0.015 Uiso 1 1 calc R . . C21 C 0.0307(3) 0.4271(3) 0.24279(13) 0.0126(5) Uani 1 1 d . . . H21 H -0.0077 0.3300 0.2241 0.015 Uiso 1 1 calc R . . C22 C 0.0766(3) 0.5567(3) 0.20278(13) 0.0109(5) Uani 1 1 d . . . H22 H 0.0740 0.5578 0.1518 0.013 Uiso 1 1 calc R . . B1 B 0.2117(3) 0.3244(4) 0.55361(16) 0.0136(6) Uani 1 1 d . . . F1 F 0.13470(16) 0.30982(18) 0.48033(7) 0.0136(3) Uani 1 1 d . . . F2 F 0.15555(19) 0.45908(18) 0.58510(8) 0.0190(3) Uani 1 1 d . . . F3 F 0.18229(16) 0.19080(17) 0.59434(7) 0.0134(3) Uani 1 1 d . . . F4 F 0.37809(16) 0.33622(18) 0.55284(7) 0.0171(3) Uani 1 1 d . . . B2 B 0.3001(3) 0.3526(3) 0.06101(15) 0.0107(6) Uani 1 1 d . . . F5 F 0.26826(17) 0.29974(18) -0.01251(7) 0.0153(3) Uani 1 1 d . . . F6 F 0.17841(16) 0.30206(18) 0.09990(7) 0.0137(3) Uani 1 1 d . . . F7 F 0.30462(17) 0.51765(17) 0.06080(8) 0.0144(3) Uani 1 1 d . . . F8 F 0.44794(17) 0.29224(19) 0.09402(7) 0.0181(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 0.00850(15) 0.00793(16) 0.00711(15) -0.00003(15) 0.00124(11) 0.00025(15) N1 0.0120(10) 0.0080(11) 0.0089(10) 0.0008(8) 0.0000(8) -0.0035(8) N2 0.0084(9) 0.0111(11) 0.0081(10) 0.0017(8) 0.0015(8) 0.0015(9) C1 0.0130(12) 0.0092(13) 0.0115(12) -0.0033(10) 0.0038(10) -0.0023(10) C2 0.0114(12) 0.0086(12) 0.0155(13) -0.0006(10) 0.0027(10) 0.0001(10) C3 0.0084(12) 0.0077(13) 0.0157(13) 0.0001(10) -0.0042(10) -0.0001(10) N3 0.0106(9) 0.0065(11) 0.0100(9) -0.0006(9) 0.0019(7) -0.0017(9) C4 0.0116(12) 0.0063(12) 0.0134(12) -0.0022(10) 0.0036(9) -0.0025(9) C5 0.0116(12) 0.0099(13) 0.0116(12) 0.0029(10) -0.0011(9) 0.0000(10) C6 0.0163(12) 0.0089(13) 0.0077(11) -0.0011(9) 0.0019(9) -0.0038(10) C7 0.0135(11) 0.0102(14) 0.0121(11) -0.0035(10) 0.0043(9) -0.0018(10) C8 0.0115(11) 0.0056(14) 0.0109(11) -0.0011(9) 0.0001(9) -0.0013(9) N4 0.0110(10) 0.0100(11) 0.0080(10) -0.0009(8) 0.0026(8) -0.0007(8) N5 0.0134(10) 0.0100(11) 0.0087(10) -0.0010(9) 0.0044(8) -0.0004(9) C9 0.0119(12) 0.0095(13) 0.0120(12) 0.0010(10) 0.0051(10) 0.0004(10) C10 0.0092(11) 0.0108(13) 0.0189(13) 0.0017(11) 0.0020(10) 0.0018(10) N6 0.0106(10) 0.0115(11) 0.0066(9) -0.0002(8) -0.0001(8) 0.0003(8) N7 0.0115(10) 0.0109(11) 0.0060(9) -0.0019(8) 0.0013(8) -0.0007(9) C11 0.0108(12) 0.0111(13) 0.0104(12) 0.0018(10) -0.0004(10) -0.0027(10) C12 0.0117(12) 0.0126(13) 0.0103(12) 0.0014(10) 0.0042(10) 0.0007(10) C13 0.0086(11) 0.0108(13) 0.0163(12) 0.0019(10) 0.0025(10) -0.0014(10) C14 0.0127(12) 0.0110(13) 0.0127(12) -0.0023(10) 0.0004(10) 0.0004(10) N8 0.0077(9) 0.0088(12) 0.0095(9) -0.0002(8) 0.0005(7) 0.0017(8) C15 0.0064(11) 0.0071(13) 0.0144(12) -0.0003(10) 0.0033(9) 0.0007(9) C16 0.0091(11) 0.0146(13) 0.0103(12) -0.0052(10) 0.0022(9) 0.0012(10) C17 0.0111(12) 0.0145(13) 0.0103(12) 0.0052(11) 0.0012(10) 0.0016(11) C18 0.0117(12) 0.0102(13) 0.0154(13) 0.0022(10) 0.0039(10) 0.0003(10) C19 0.0093(11) 0.0091(13) 0.0114(12) 0.0002(10) 0.0009(9) 0.0012(10) N9 0.0106(10) 0.0121(12) 0.0089(10) 0.0017(9) 0.0015(8) 0.0007(9) N10 0.0102(10) 0.0111(11) 0.0084(10) 0.0001(8) 0.0016(8) 0.0000(9) C20 0.0111(12) 0.0098(13) 0.0158(13) 0.0025(11) 0.0022(10) 0.0006(10) C21 0.0098(11) 0.0115(15) 0.0157(12) -0.0026(10) -0.0009(9) 0.0009(10) C22 0.0092(12) 0.0142(14) 0.0090(12) -0.0043(10) 0.0000(10) 0.0017(10) B1 0.0165(14) 0.0139(15) 0.0107(14) 0.0006(12) 0.0034(12) -0.0002(12) F1 0.0147(7) 0.0159(8) 0.0099(7) 0.0014(6) 0.0011(6) 0.0019(6) F2 0.0287(9) 0.0144(8) 0.0147(8) -0.0013(6) 0.0059(7) 0.0032(7) F3 0.0141(7) 0.0151(8) 0.0107(7) 0.0039(6) 0.0008(6) -0.0008(6) F4 0.0127(7) 0.0256(9) 0.0131(7) 0.0008(6) 0.0023(6) -0.0060(6) B2 0.0136(13) 0.0086(16) 0.0097(13) -0.0014(10) 0.0011(11) -0.0003(10) F5 0.0201(8) 0.0155(8) 0.0111(7) -0.0014(6) 0.0046(6) -0.0009(7) F6 0.0161(7) 0.0133(8) 0.0125(7) 0.0005(6) 0.0052(6) -0.0006(6) F7 0.0180(8) 0.0110(8) 0.0137(8) 0.0009(6) 0.0012(6) -0.0023(7) F8 0.0150(7) 0.0267(9) 0.0130(7) 0.0053(7) 0.0033(6) 0.0058(7) _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 N3 1.8956(18) . ? Fe1 N8 1.9014(19) . ? Fe1 N10 1.965(2) . ? Fe1 N5 1.966(2) . ? Fe1 N1 1.982(2) . ? Fe1 N6 1.988(2) . ? N1 C1 1.328(3) . ? N1 N2 1.386(3) . ? N2 C3 1.356(3) . ? N2 C4 1.400(3) . ? C1 C2 1.409(3) . ? C2 C3 1.362(3) . ? N3 C4 1.343(3) . ? N3 C8 1.345(3) . ? C4 C5 1.376(3) . ? C5 C6 1.389(3) . ? C6 C7 1.378(3) . ? C7 C8 1.380(3) . ? C8 N4 1.406(3) . ? N4 C9 1.354(3) . ? N4 N5 1.377(3) . ? N5 C11 1.322(3) . ? C9 C10 1.367(3) . ? C10 C11 1.404(3) . ? N6 C12 1.320(3) . ? N6 N7 1.380(3) . ? N7 C14 1.347(3) . ? N7 C15 1.408(3) . ? C12 C13 1.405(3) . ? C13 C14 1.377(3) . ? N8 C19 1.339(3) . ? N8 C15 1.341(3) . ? C15 C16 1.370(3) . ? C16 C17 1.395(4) . ? C17 C18 1.383(4) . ? C18 C19 1.374(3) . ? C19 N9 1.405(3) . ? N9 C20 1.359(3) . ? N9 N10 1.380(3) . ? N10 C22 1.325(3) . ? C20 C21 1.369(3) . ? C21 C22 1.406(3) . ? B1 F2 1.392(3) . ? B1 F3 1.398(3) . ? B1 F1 1.405(3) . ? B1 F4 1.405(3) . ? B2 F8 1.396(3) . ? B2 F6 1.398(3) . ? B2 F7 1.399(3) . ? B2 F5 1.405(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Fe1 N8 177.68(10) . . ? N3 Fe1 N10 97.83(9) . . ? N8 Fe1 N10 80.01(8) . . ? N3 Fe1 N5 80.11(8) . . ? N8 Fe1 N5 99.00(8) . . ? N10 Fe1 N5 90.11(9) . . ? N3 Fe1 N1 80.14(8) . . ? N8 Fe1 N1 100.72(8) . . ? N10 Fe1 N1 92.00(8) . . ? N5 Fe1 N1 160.23(8) . . ? N3 Fe1 N6 102.08(9) . . ? N8 Fe1 N6 80.05(8) . . ? N10 Fe1 N6 160.00(8) . . ? N5 Fe1 N6 91.39(9) . . ? N1 Fe1 N6 93.29(8) . . ? C1 N1 N2 105.0(2) . . ? C1 N1 Fe1 142.90(18) . . ? N2 N1 Fe1 112.09(14) . . ? C3 N2 N1 110.78(19) . . ? C3 N2 C4 132.4(2) . . ? N1 N2 C4 116.78(19) . . ? N1 C1 C2 110.9(2) . . ? C3 C2 C1 105.8(2) . . ? N2 C3 C2 107.4(2) . . ? C4 N3 C8 119.4(2) . . ? C4 N3 Fe1 120.40(15) . . ? C8 N3 Fe1 120.12(16) . . ? N3 C4 C5 122.3(2) . . ? N3 C4 N2 110.6(2) . . ? C5 C4 N2 127.1(2) . . ? C4 C5 C6 117.0(2) . . ? C7 C6 C5 122.1(2) . . ? C6 C7 C8 116.8(2) . . ? N3 C8 C7 122.5(2) . . ? N3 C8 N4 110.44(19) . . ? C7 C8 N4 127.1(2) . . ? C9 N4 N5 111.22(18) . . ? C9 N4 C8 132.5(2) . . ? N5 N4 C8 116.24(18) . . ? C11 N5 N4 105.03(19) . . ? C11 N5 Fe1 141.74(17) . . ? N4 N5 Fe1 112.97(14) . . ? N4 C9 C10 106.8(2) . . ? C9 C10 C11 105.8(2) . . ? C12 N6 N7 105.2(2) . . ? C12 N6 Fe1 142.50(18) . . ? N7 N6 Fe1 112.15(15) . . ? C14 N7 N6 111.10(19) . . ? C14 N7 C15 131.8(2) . . ? N6 N7 C15 116.89(19) . . ? N5 C11 C10 111.1(2) . . ? N6 C12 C13 111.4(2) . . ? C14 C13 C12 105.2(2) . . ? N7 C14 C13 107.2(2) . . ? C19 N8 C15 119.2(2) . . ? C19 N8 Fe1 120.33(16) . . ? C15 N8 Fe1 120.38(16) . . ? N8 C15 C16 122.5(2) . . ? N8 C15 N7 110.5(2) . . ? C16 C15 N7 126.9(2) . . ? C15 C16 C17 117.0(2) . . ? C18 C17 C16 121.5(2) . . ? C19 C18 C17 116.8(2) . . ? N8 C19 C18 122.9(2) . . ? N8 C19 N9 110.3(2) . . ? C18 C19 N9 126.9(2) . . ? C20 N9 N10 110.85(19) . . ? C20 N9 C19 132.4(2) . . ? N10 N9 C19 116.6(2) . . ? C22 N10 N9 105.0(2) . . ? C22 N10 Fe1 142.10(17) . . ? N9 N10 Fe1 112.79(15) . . ? N9 C20 C21 107.3(2) . . ? C20 C21 C22 105.3(2) . . ? N10 C22 C21 111.5(2) . . ? F2 B1 F3 110.2(2) . . ? F2 B1 F1 109.3(2) . . ? F3 B1 F1 110.1(2) . . ? F2 B1 F4 110.2(2) . . ? F3 B1 F4 108.6(2) . . ? F1 B1 F4 108.4(2) . . ? F8 B2 F6 109.9(2) . . ? F8 B2 F7 110.1(2) . . ? F6 B2 F7 109.3(2) . . ? F8 B2 F5 109.12(19) . . ? F6 B2 F5 109.9(2) . . ? F7 B2 F5 108.5(2) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.423 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.060