# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_op234 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[4-(3,5-dimethyl-1H-pyrazol-1-yl)-2-(pyridin-2-yl)-6-methylpyrimidine] iron(II) ditetrafluoroborate hydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H30 Fe N10 2+, (B F4 1-)2, 0.11(H2 O)' _chemical_formula_sum 'C30 H30.22 B2 F8 Fe N10 O1.11' _chemical_formula_weight 778.06 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' B B 0.0013 0.0007 '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 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.035(2) _cell_length_b 19.525(4) _cell_length_c 15.481(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.034(12) _cell_angle_gamma 90.00 _cell_volume 3459.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 1221 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 18.80 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1555.4 _exptl_absorpt_coefficient_mu 0.518 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.814 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_process_details SADABS-2008/1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19935 _diffrn_reflns_av_R_equivalents 0.1489 _diffrn_reflns_av_sigmaI/netI 0.2126 _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 -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.13 _reflns_number_total 6041 _reflns_number_gt 2643 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0907P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6041 _refine_ls_number_parameters 494 _refine_ls_number_restraints 319 _refine_ls_R_factor_all 0.1964 _refine_ls_R_factor_gt 0.0692 _refine_ls_wR_factor_ref 0.2104 _refine_ls_wR_factor_gt 0.1435 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.001 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 -0.03827(9) 0.73690(5) 1.11445(6) 0.0255(3) Uani 1 1 d . . . N1 N -0.0407(5) 0.6406(3) 1.3470(3) 0.0290(14) Uani 1 1 d U . . C1 C -0.0248(6) 0.6824(3) 1.2851(4) 0.0254(17) Uani 1 1 d U . . N2 N -0.0470(5) 0.6676(3) 1.1962(3) 0.0223(13) Uani 1 1 d U . . C2 C -0.0884(6) 0.6054(4) 1.1679(4) 0.0285(18) Uani 1 1 d U . . N3 N 0.0175(5) 0.7897(3) 1.2297(3) 0.0251(14) Uani 1 1 d U . . C3 C -0.1093(6) 0.5583(3) 1.2255(4) 0.0313(18) Uani 1 1 d U . . H3A H -0.1400 0.5143 1.2052 0.038 Uiso 1 1 calc R . . N4 N -0.1116(5) 0.5994(3) 1.0732(4) 0.0310(15) Uani 1 1 d U . . C4 C -0.0833(6) 0.5782(4) 1.3167(5) 0.0326(18) Uani 1 1 d U . . N5 N -0.0969(5) 0.6595(3) 1.0288(3) 0.0259(14) Uani 1 1 d U . . C5 C -0.1061(7) 0.5313(4) 1.3849(4) 0.048(2) Uani 1 1 d U . . H5A H -0.0836 0.5537 1.4444 0.072 Uiso 1 1 calc R . . H5B H -0.0604 0.4892 1.3885 0.072 Uiso 1 1 calc R . . H5C H -0.1895 0.5199 1.3667 0.072 Uiso 1 1 calc R . . N6 N -0.1317(5) 0.9062(3) 0.9540(4) 0.0319(15) Uani 1 1 d U . . C6 C 0.0158(6) 0.7541(3) 1.3049(4) 0.0302(18) Uani 1 1 d U . . N7 N -0.0343(5) 0.8083(3) 1.0349(3) 0.0243(14) Uani 1 1 d U . . C7 C 0.0459(7) 0.7845(3) 1.3909(4) 0.0342(18) Uani 1 1 d U . . H7A H 0.0487 0.7578 1.4428 0.041 Uiso 1 1 calc R . . N8 N -0.1958(5) 0.7762(3) 1.0978(3) 0.0238(13) Uani 1 1 d U . . C8 C 0.0712(7) 0.8530(4) 1.3996(5) 0.041(2) Uani 1 1 d U . . H8A H 0.0882 0.8750 1.4570 0.049 Uiso 1 1 calc R . . N9 N 0.1422(5) 0.7683(3) 1.0397(3) 0.0300(14) Uani 1 1 d U . . C9 C 0.0717(7) 0.8891(4) 1.3246(5) 0.039(2) Uani 1 1 d U . . H9A H 0.0898 0.9366 1.3294 0.047 Uiso 1 1 calc R . . N10 N 0.1212(5) 0.7248(3) 1.1049(3) 0.0288(14) Uani 1 1 d U . . C10 C 0.0459(6) 0.8565(4) 1.2410(4) 0.0344(19) Uani 1 1 d U . . H10A H 0.0484 0.8824 1.1897 0.041 Uiso 1 1 calc R . . C11 C -0.1197(7) 0.6414(4) 0.9420(4) 0.035(2) Uani 1 1 d U . . C12 C -0.1482(7) 0.5715(4) 0.9312(5) 0.043(2) Uani 1 1 d U . . H12A H -0.1673 0.5467 0.8758 0.051 Uiso 1 1 calc R . . C13 C -0.1440(7) 0.5454(4) 1.0136(5) 0.041(2) Uani 1 1 d U . . C14 C -0.1159(8) 0.6922(4) 0.8708(4) 0.050(2) Uani 1 1 d U . . H14A H -0.0932 0.7372 0.8990 0.075 Uiso 1 1 calc R . . H14B H -0.1933 0.6955 0.8253 0.075 Uiso 1 1 calc R . . H14C H -0.0587 0.6774 0.8413 0.075 Uiso 1 1 calc R . . C15 C -0.1696(8) 0.4751(4) 1.0398(5) 0.058(3) Uani 1 1 d U . . H15A H -0.1899 0.4454 0.9861 0.088 Uiso 1 1 calc R . . H15B H -0.2353 0.4769 1.0646 0.088 Uiso 1 1 calc R . . H15C H -0.1005 0.4568 1.0858 0.088 Uiso 1 1 calc R . . C16 C -0.1248(6) 0.8524(4) 1.0081(4) 0.0257(17) Uani 1 1 d U . . C17 C 0.0572(6) 0.8185(3) 1.0052(4) 0.0269(17) Uani 1 1 d U . . C18 C 0.0578(7) 0.8734(4) 0.9478(4) 0.0332(19) Uani 1 1 d U . . H18A H 0.1218 0.8810 0.9254 0.040 Uiso 1 1 calc R . . C19 C -0.0385(7) 0.9166(3) 0.9247(4) 0.0311(18) Uani 1 1 d U . . C20 C -0.0407(7) 0.9786(4) 0.8671(5) 0.046(2) Uani 1 1 d U . . H20A H -0.1141 1.0035 0.8583 0.068 Uiso 1 1 calc R . . H20B H -0.0347 0.9644 0.8080 0.068 Uiso 1 1 calc R . . H20C H 0.0253 1.0085 0.8975 0.068 Uiso 1 1 calc R . . C21 C -0.2185(6) 0.8345(3) 1.0469(4) 0.0263(17) Uani 1 1 d U . . C22 C -0.3178(7) 0.8721(4) 1.0344(4) 0.0339(19) Uani 1 1 d U . . H22A H -0.3320 0.9116 0.9967 0.041 Uiso 1 1 calc R . . C23 C -0.3978(7) 0.8517(4) 1.0777(5) 0.041(2) Uani 1 1 d U . . H23A H -0.4660 0.8781 1.0719 0.049 Uiso 1 1 calc R . . C24 C -0.3769(7) 0.7934(4) 1.1283(5) 0.0364(19) Uani 1 1 d U . . H24A H -0.4309 0.7782 1.1578 0.044 Uiso 1 1 calc R . . C25 C -0.2758(6) 0.7564(4) 1.1364(4) 0.0347(19) Uani 1 1 d U . . H25A H -0.2628 0.7153 1.1709 0.042 Uiso 1 1 calc R . . C26 C 0.2150(7) 0.6841(4) 1.1305(5) 0.037(2) Uani 1 1 d U . . C27 C 0.2934(7) 0.7007(4) 1.0836(5) 0.045(2) Uani 1 1 d U . . H27A H 0.3660 0.6789 1.0901 0.054 Uiso 1 1 calc R . . C28 C 0.2475(7) 0.7532(4) 1.0277(5) 0.040(2) Uani 1 1 d U . . C29 C 0.2255(7) 0.6300(4) 1.1997(5) 0.047(2) Uani 1 1 d U . . H29A H 0.1560 0.6305 1.2198 0.071 Uiso 1 1 calc R . . H29B H 0.2951 0.6384 1.2517 0.071 Uiso 1 1 calc R . . H29C H 0.2324 0.5852 1.1731 0.071 Uiso 1 1 calc R . . C30 C 0.2934(8) 0.7911(4) 0.9615(6) 0.067(3) Uani 1 1 d U . . H30A H 0.3698 0.7724 0.9636 0.101 Uiso 1 1 calc R . . H30B H 0.3016 0.8398 0.9777 0.101 Uiso 1 1 calc R . . H30C H 0.2388 0.7859 0.9000 0.101 Uiso 1 1 calc R . . F1 F 0.9548(6) 0.6038(4) 0.7108(4) 0.096(3) Uani 0.948(12) 1 d PU . . B1 B 0.8519(10) 0.5687(5) 0.6715(7) 0.050(3) Uani 1 1 d DU . . F2 F 0.8483(5) 0.5473(3) 0.5866(3) 0.0920(19) Uani 1 1 d DU . . F3 F 0.7558(5) 0.6104(4) 0.6658(4) 0.080(2) Uani 0.948(12) 1 d PU . . F4 F 0.8466(6) 0.5146(3) 0.7245(4) 0.086(3) Uani 0.948(12) 1 d PU . . F1A F 0.749(3) 0.564(5) 0.688(4) 0.05(3) Uiso 0.052(12) 1 d PD . . F3A F 0.934(5) 0.545(4) 0.744(2) 0.05(3) Uiso 0.052(12) 1 d PD . . F4A F 0.874(9) 0.6377(14) 0.667(4) 0.08(4) Uiso 0.052(12) 1 d PD . . B2 B 0.0835(11) 0.9220(6) 0.6774(7) 0.059(3) Uani 1 1 d DU . . F5 F 0.1165(12) 0.8694(6) 0.7417(6) 0.134(5) Uani 0.855(17) 1 d PU . . F6 F 0.1360(5) 0.9821(4) 0.7186(6) 0.094(4) Uani 0.855(17) 1 d PU . . F7 F 0.1346(7) 0.9055(4) 0.6112(3) 0.070(3) Uani 0.855(17) 1 d PU . . F8 F -0.0325(7) 0.9298(6) 0.6467(8) 0.094(4) Uani 0.855(17) 1 d PU . . F5A F 0.071(5) 0.8742(19) 0.609(2) 0.093(18) Uiso 0.145(17) 1 d PD . . F6A F -0.029(2) 0.938(3) 0.670(3) 0.032(13) Uiso 0.145(17) 1 d PD . . F7A F 0.131(4) 0.976(2) 0.647(4) 0.14(3) Uiso 0.145(17) 1 d PD . . F8A F 0.141(3) 0.896(2) 0.7572(17) 0.046(14) Uiso 0.145(17) 1 d PD . . O1 O 0.176(6) 0.107(3) 0.615(4) 0.085 Uiso 0.105(10) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0336(6) 0.0201(6) 0.0255(5) 0.0032(5) 0.0131(4) 0.0030(6) N1 0.039(4) 0.020(4) 0.030(3) 0.006(3) 0.014(3) 0.002(3) C1 0.034(5) 0.014(4) 0.030(4) 0.004(3) 0.012(3) 0.004(3) N2 0.031(4) 0.013(3) 0.024(3) 0.000(2) 0.010(3) -0.004(3) C2 0.033(5) 0.027(5) 0.030(4) 0.002(3) 0.015(4) 0.006(4) N3 0.029(4) 0.017(3) 0.030(3) 0.004(3) 0.011(3) 0.000(3) C3 0.043(5) 0.018(4) 0.036(4) 0.001(3) 0.016(4) 0.004(4) N4 0.043(4) 0.020(3) 0.033(3) 0.001(3) 0.016(3) -0.003(3) C4 0.034(5) 0.023(4) 0.046(4) 0.010(4) 0.020(4) 0.010(4) N5 0.035(4) 0.021(3) 0.027(3) 0.000(3) 0.017(3) 0.001(3) C5 0.071(6) 0.034(5) 0.040(4) 0.010(4) 0.020(4) -0.010(5) N6 0.044(4) 0.024(4) 0.031(3) 0.004(3) 0.017(3) -0.001(3) C6 0.038(5) 0.025(4) 0.031(4) 0.004(3) 0.015(3) -0.005(4) N7 0.035(4) 0.021(3) 0.021(3) 0.002(2) 0.015(3) 0.005(3) C7 0.045(5) 0.033(5) 0.027(4) 0.006(4) 0.015(4) -0.002(4) N8 0.029(4) 0.020(3) 0.023(3) 0.000(3) 0.009(3) 0.002(3) C8 0.056(6) 0.030(5) 0.040(4) -0.007(4) 0.020(4) -0.006(4) N9 0.032(4) 0.024(3) 0.038(3) 0.005(3) 0.016(3) 0.002(3) C9 0.053(6) 0.022(4) 0.040(4) -0.004(4) 0.012(4) -0.012(4) N10 0.038(4) 0.024(4) 0.028(3) 0.008(3) 0.015(3) 0.001(3) C10 0.046(5) 0.023(5) 0.029(4) 0.002(3) 0.003(4) -0.007(4) C11 0.044(5) 0.040(5) 0.022(4) -0.003(3) 0.011(4) 0.004(4) C12 0.060(6) 0.035(5) 0.036(4) -0.012(4) 0.019(4) -0.008(4) C13 0.050(6) 0.026(5) 0.048(5) -0.016(4) 0.015(4) -0.011(4) C14 0.071(7) 0.055(6) 0.026(4) -0.009(4) 0.019(4) -0.008(5) C15 0.097(8) 0.032(5) 0.047(5) -0.010(4) 0.022(5) -0.014(5) C16 0.034(5) 0.024(4) 0.020(3) 0.000(3) 0.008(3) 0.002(4) C17 0.029(4) 0.030(4) 0.019(3) 0.002(3) 0.003(3) -0.002(4) C18 0.037(5) 0.032(5) 0.036(4) 0.004(4) 0.020(4) -0.003(4) C19 0.048(5) 0.020(4) 0.023(4) 0.002(3) 0.008(4) 0.002(4) C20 0.067(6) 0.030(5) 0.043(4) 0.009(4) 0.022(4) -0.006(4) C21 0.031(5) 0.022(4) 0.023(3) -0.002(3) 0.004(3) 0.006(4) C22 0.037(5) 0.031(5) 0.036(4) 0.000(3) 0.014(4) 0.007(4) C23 0.040(5) 0.033(5) 0.052(5) -0.007(4) 0.017(4) 0.007(4) C24 0.034(5) 0.040(5) 0.042(4) -0.002(4) 0.021(4) 0.001(4) C25 0.038(5) 0.038(5) 0.029(4) -0.003(3) 0.011(4) -0.001(4) C26 0.040(5) 0.024(5) 0.050(5) 0.004(4) 0.019(4) 0.006(4) C27 0.037(5) 0.040(5) 0.060(5) 0.016(4) 0.020(4) 0.017(4) C28 0.033(5) 0.037(5) 0.060(5) 0.001(4) 0.026(4) -0.003(4) C29 0.046(6) 0.045(5) 0.052(5) 0.017(4) 0.016(4) 0.015(4) C30 0.061(7) 0.065(7) 0.095(7) 0.022(5) 0.051(6) 0.012(5) F1 0.068(5) 0.127(6) 0.110(5) -0.054(5) 0.052(4) -0.047(5) B1 0.054(7) 0.055(7) 0.054(6) -0.012(5) 0.037(6) -0.012(6) F2 0.112(5) 0.120(5) 0.061(3) -0.025(3) 0.051(3) -0.020(4) F3 0.079(5) 0.072(5) 0.090(4) -0.002(4) 0.028(4) 0.016(4) F4 0.102(6) 0.085(5) 0.073(4) 0.032(3) 0.033(4) -0.003(4) B2 0.069(9) 0.056(8) 0.046(6) -0.008(6) 0.011(6) 0.000(7) F5 0.228(12) 0.104(8) 0.092(6) 0.023(6) 0.083(6) 0.040(9) F6 0.058(5) 0.094(6) 0.130(7) -0.069(5) 0.026(4) -0.008(4) F7 0.075(6) 0.089(6) 0.051(4) -0.016(3) 0.028(3) 0.012(5) F8 0.067(6) 0.101(7) 0.119(9) -0.047(6) 0.036(5) -0.028(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 N7 1.870(5) . ? Fe1 N2 1.877(5) . ? Fe1 N10 1.984(6) . ? Fe1 N8 1.987(6) . ? Fe1 N3 1.989(5) . ? Fe1 N5 1.991(5) . ? N1 C1 1.318(7) . ? N1 C4 1.348(9) . ? C1 N2 1.349(7) . ? C1 C6 1.482(9) . ? N2 C2 1.334(8) . ? C2 C3 1.358(9) . ? C2 N4 1.409(8) . ? N3 C10 1.347(8) . ? N3 C6 1.361(7) . ? C3 C4 1.403(9) . ? C3 H3A 0.9500 . ? N4 C13 1.375(8) . ? N4 N5 1.400(7) . ? C4 C5 1.487(9) . ? N5 C11 1.332(8) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? N6 C16 1.329(8) . ? N6 C19 1.351(9) . ? C6 C7 1.399(9) . ? N7 C17 1.333(8) . ? N7 C16 1.349(8) . ? C7 C8 1.369(9) . ? C7 H7A 0.9500 . ? N8 C25 1.338(8) . ? N8 C21 1.363(8) . ? C8 C9 1.360(9) . ? C8 H8A 0.9500 . ? N9 C28 1.369(9) . ? N9 C17 1.398(8) . ? N9 N10 1.402(7) . ? C9 C10 1.387(9) . ? C9 H9A 0.9500 . ? N10 C26 1.337(9) . ? C10 H10A 0.9500 . ? C11 C12 1.404(10) . ? C11 C14 1.495(9) . ? C12 C13 1.359(9) . ? C12 H12A 0.9500 . ? C13 C15 1.491(10) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.475(9) . ? C17 C18 1.394(9) . ? C18 C19 1.387(10) . ? C18 H18A 0.9500 . ? C19 C20 1.498(9) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.364(9) . ? C22 C23 1.391(10) . ? C22 H22A 0.9500 . ? C23 C24 1.361(10) . ? C23 H23A 0.9500 . ? C24 C25 1.387(10) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 C27 1.394(10) . ? C26 C29 1.482(9) . ? C27 C28 1.344(10) . ? C27 H27A 0.9500 . ? C28 C30 1.502(10) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? F1 F4A 1.20(9) . ? F1 F3A 1.31(8) . ? F1 B1 1.380(11) . ? B1 F3A 1.331(18) . ? B1 F1A 1.345(18) . ? B1 F4 1.353(11) . ? B1 F2 1.366(10) . ? B1 F4A 1.378(19) . ? B1 F3 1.395(11) . ? F3 F1A 0.99(9) . ? F3 F4A 1.51(8) . ? F4 F3A 1.16(8) . ? F4 F1A 1.49(8) . ? B2 F8A 1.316(17) . ? B2 F8 1.337(14) . ? B2 F7A 1.351(17) . ? B2 F6A 1.354(18) . ? B2 F5A 1.381(17) . ? B2 F7 1.386(12) . ? B2 F5 1.399(13) . ? B2 F6 1.391(12) . ? F5 F8A 0.61(4) . ? F6 F7A 1.10(5) . ? F6 F8A 1.78(3) . ? F7 F5A 0.97(5) . ? F7 F7A 1.48(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 N7 Fe1 N2 177.4(2) . . ? N7 Fe1 N10 79.5(2) . . ? N2 Fe1 N10 102.8(2) . . ? N7 Fe1 N8 81.1(2) . . ? N2 Fe1 N8 96.6(2) . . ? N10 Fe1 N8 160.5(2) . . ? N7 Fe1 N3 97.7(2) . . ? N2 Fe1 N3 80.9(2) . . ? N10 Fe1 N3 93.6(2) . . ? N8 Fe1 N3 87.7(2) . . ? N7 Fe1 N5 101.7(2) . . ? N2 Fe1 N5 79.6(2) . . ? N10 Fe1 N5 90.6(2) . . ? N8 Fe1 N5 94.6(2) . . ? N3 Fe1 N5 160.6(2) . . ? C1 N1 C4 115.5(5) . . ? N1 C1 N2 125.6(6) . . ? N1 C1 C6 123.1(6) . . ? N2 C1 C6 111.2(5) . . ? C2 N2 C1 117.7(5) . . ? C2 N2 Fe1 121.9(4) . . ? C1 N2 Fe1 119.9(4) . . ? N2 C2 C3 121.8(6) . . ? N2 C2 N4 110.6(6) . . ? C3 C2 N4 127.5(7) . . ? C10 N3 C6 117.0(5) . . ? C10 N3 Fe1 128.3(4) . . ? C6 N3 Fe1 114.3(4) . . ? C2 C3 C4 116.4(7) . . ? C2 C3 H3A 121.8 . . ? C4 C3 H3A 121.8 . . ? C13 N4 N5 111.4(5) . . ? C13 N4 C2 133.4(6) . . ? N5 N4 C2 115.2(5) . . ? N1 C4 C3 122.9(6) . . ? N1 C4 C5 116.3(6) . . ? C3 C4 C5 120.7(7) . . ? C11 N5 N4 104.8(5) . . ? C11 N5 Fe1 142.5(5) . . ? N4 N5 Fe1 112.4(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C16 N6 C19 115.7(6) . . ? N3 C6 C7 121.9(6) . . ? N3 C6 C1 113.4(5) . . ? C7 C6 C1 124.7(6) . . ? C17 N7 C16 118.2(6) . . ? C17 N7 Fe1 122.1(5) . . ? C16 N7 Fe1 119.7(5) . . ? C8 C7 C6 119.5(6) . . ? C8 C7 H7A 120.2 . . ? C6 C7 H7A 120.2 . . ? C25 N8 C21 117.1(6) . . ? C25 N8 Fe1 128.4(5) . . ? C21 N8 Fe1 114.2(4) . . ? C9 C8 C7 118.8(6) . . ? C9 C8 H8A 120.6 . . ? C7 C8 H8A 120.6 . . ? C28 N9 C17 134.3(6) . . ? C28 N9 N10 110.4(6) . . ? C17 N9 N10 115.2(6) . . ? C8 C9 C10 120.0(6) . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C26 N10 N9 104.4(6) . . ? C26 N10 Fe1 142.8(5) . . ? N9 N10 Fe1 112.1(4) . . ? N3 C10 C9 122.7(6) . . ? N3 C10 H10A 118.7 . . ? C9 C10 H10A 118.7 . . ? N5 C11 C12 110.1(6) . . ? N5 C11 C14 121.6(7) . . ? C12 C11 C14 128.3(6) . . ? C13 C12 C11 108.4(6) . . ? C13 C12 H12A 125.8 . . ? C11 C12 H12A 125.8 . . ? C12 C13 N4 105.3(6) . . ? C12 C13 C15 130.5(7) . . ? N4 C13 C15 124.2(6) . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N6 C16 N7 125.8(6) . . ? N6 C16 C21 122.4(6) . . ? N7 C16 C21 111.7(6) . . ? N7 C17 C18 120.2(7) . . ? N7 C17 N9 110.3(6) . . ? C18 C17 N9 129.4(7) . . ? C19 C18 C17 117.6(7) . . ? C19 C18 H18A 121.2 . . ? C17 C18 H18A 121.2 . . ? N6 C19 C18 122.4(6) . . ? N6 C19 C20 117.3(7) . . ? C18 C19 C20 120.3(7) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 N8 122.8(6) . . ? C22 C21 C16 124.1(6) . . ? N8 C21 C16 113.0(6) . . ? C21 C22 C23 118.9(7) . . ? C21 C22 H22A 120.5 . . ? C23 C22 H22A 120.5 . . ? C24 C23 C22 119.0(7) . . ? C24 C23 H23A 120.5 . . ? C22 C23 H23A 120.5 . . ? C23 C24 C25 119.2(7) . . ? C23 C24 H24A 120.4 . . ? C25 C24 H24A 120.4 . . ? N8 C25 C24 122.9(7) . . ? N8 C25 H25A 118.6 . . ? C24 C25 H25A 118.6 . . ? N10 C26 C27 110.7(6) . . ? N10 C26 C29 120.9(7) . . ? C27 C26 C29 128.5(7) . . ? C28 C27 C26 107.7(7) . . ? C28 C27 H27A 126.2 . . ? C26 C27 H27A 126.2 . . ? C27 C28 N9 106.9(6) . . ? C27 C28 C30 130.6(8) . . ? N9 C28 C30 122.5(7) . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? F4A F1 F3A 119(3) . . ? F4A F1 B1 64(2) . . ? F3A F1 B1 59.2(19) . . ? F3A B1 F1A 108(3) . . ? F3A B1 F4 51(4) . . ? F1A B1 F4 67(4) . . ? F3A B1 F2 120(2) . . ? F1A B1 F2 114(2) . . ? F4 B1 F2 110.6(8) . . ? F3A B1 F4A 107(3) . . ? F1A B1 F4A 106(3) . . ? F4 B1 F4A 147(2) . . ? F2 B1 F4A 101(2) . . ? F3A B1 F1 58(4) . . ? F1A B1 F1 135(3) . . ? F4 B1 F1 108.9(9) . . ? F2 B1 F1 109.5(7) . . ? F4A B1 F1 52(4) . . ? F3A B1 F3 130(2) . . ? F1A B1 F3 42(4) . . ? F4 B1 F3 107.5(7) . . ? F2 B1 F3 109.8(8) . . ? F4A B1 F3 66(4) . . ? F1 B1 F3 110.6(8) . . ? F1A F3 B1 66(2) . . ? F1A F3 F4A 120(3) . . ? B1 F3 F4A 56(2) . . ? F3A F4 B1 63(2) . . ? F3A F4 F1A 108(3) . . ? B1 F4 F1A 56(2) . . ? F3 F1A B1 72(3) . . ? F3 F1A F4 126(2) . . ? B1 F1A F4 57(2) . . ? F4 F3A B1 65(2) . . ? F4 F3A F1 127.3(19) . . ? B1 F3A F1 63(2) . . ? F1 F4A B1 64(2) . . ? F1 F4A F3 114(2) . . ? B1 F4A F3 58(2) . . ? F8A B2 F8 124(2) . . ? F8A B2 F7A 118(2) . . ? F8 B2 F7A 107(2) . . ? F8A B2 F6A 113(2) . . ? F8 B2 F6A 16(2) . . ? F7A B2 F6A 108(2) . . ? F8A B2 F5A 111(2) . . ? F8 B2 F5A 87(2) . . ? F7A B2 F5A 102(2) . . ? F6A B2 F5A 103(2) . . ? F8A B2 F7 112(2) . . ? F8 B2 F7 114.6(10) . . ? F7A B2 F7 66(2) . . ? F6A B2 F7 130(2) . . ? F5A B2 F7 41(2) . . ? F8A B2 F5 25.6(18) . . ? F8 B2 F5 111.8(12) . . ? F7A B2 F5 140(2) . . ? F6A B2 F5 107(2) . . ? F5A B2 F5 89.4(19) . . ? F7 B2 F5 105.3(9) . . ? F8A B2 F6 82.2(18) . . ? F8 B2 F6 110.0(10) . . ? F7A B2 F6 47(2) . . ? F6A B2 F6 98(2) . . ? F5A B2 F6 148(2) . . ? F7 B2 F6 107.0(9) . . ? F5 B2 F6 107.7(10) . . ? F8A F5 B2 70(2) . . ? F7A F6 B2 64.4(14) . . ? F7A F6 F8A 103(2) . . ? B2 F6 F8A 47.1(10) . . ? F5A F7 B2 69.2(14) . . ? F5A F7 F7A 119(2) . . ? B2 F7 F7A 56.1(14) . . ? F7 F5A B2 69.7(18) . . ? F6 F7A B2 68.2(17) . . ? F6 F7A F7 119(2) . . ? B2 F7A F7 58.3(15) . . ? F5 F8A B2 85(3) . . ? F5 F8A F6 135(3) . . ? B2 F8A F6 50.7(11) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.13 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.455 _refine_diff_density_min -0.612 _refine_diff_density_rms 0.159 _database_code_depnum_ccdc_archive 'CCDC 948843'