# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr Andres Goeta' _publ_contact_author_address ; Department of Chemistry University of Durham South Road Durham DH1 3LE UNITED KINGDOM ; _publ_contact_author_email A.E.GOETA@DURHAM.AC.UK _publ_section_title ; Thermal and light induced polymorphism in iron(II) spin crossover compounds ; loop_ _publ_author_name 'Andres Goeta' 'Ana Galet' 'M. Carmen Munoz' 'Jose Antonio Real' 'Amber L. Thompson' #====================================================================== data_bipy1 _database_code_depnum_ccdc_archive 'CCDC 233281' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,2'-Bipyridine-bis[di(hydro)bis(1-pyrazolyl)borate iron(II) ; _chemical_name_common "2,2'-Bipyridine-bis(di(hydro)bis(1-pyrazolyl)borate iron(ii)" _chemical_melting_point 'not measured' _chemical_formula_moiety 'C22 H24 B2 Fe N10' _chemical_formula_sum 'C22 H24 B2 Fe N10' _chemical_formula_weight 505.98 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.2215(15) _cell_length_b 15.0254(15) _cell_length_c 11.0397(11) _cell_angle_alpha 90.00 _cell_angle_beta 114.858(4) _cell_angle_gamma 90.00 _cell_volume 2441.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 2265 _cell_measurement_theta_min 4.699 _cell_measurement_theta_max 49.588 _exptl_crystal_description block _exptl_crystal_colour clear_intense_red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.650 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8810 _exptl_absorpt_correction_T_max 0.9559 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 3 sets of \w scans each set at different \f and/or 2\q angles and each scan (7s exposure) covering 0.3\% in \w. Crystal to detector distance 4.51. ; _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 SMART CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 8856 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0825 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 30.51 _reflns_number_total 3510 _reflns_number_gt 2240 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SMART-NT V6.1 (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0075P)^2^+1.8569P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3510 _refine_ls_number_parameters 207 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0987 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.0886 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 0.5000 0.27028(3) 0.7500 0.02770(13) Uani 1 2 d S . . B1 B 0.47976(19) 0.20490(19) 1.0411(3) 0.0390(6) Uani 1 1 d . . . H1B H 0.5163(15) 0.2715(15) 1.083(2) 0.043(6) Uiso 1 1 d . . . H2B H 0.4636(15) 0.1671(14) 1.115(2) 0.043(6) Uiso 1 1 d . . . N1 N 0.56190(12) 0.38795(11) 0.87514(17) 0.0323(4) Uani 1 1 d . . . N2 N 0.56762(12) 0.17076(11) 0.90076(17) 0.0327(4) Uani 1 1 d . . . N3 N 0.38559(12) 0.26584(12) 0.80473(16) 0.0326(4) Uani 1 1 d . . . N4 N 0.54359(12) 0.14714(12) 1.00161(17) 0.0343(4) Uani 1 1 d . . . N5 N 0.38910(12) 0.22306(12) 0.91630(16) 0.0334(4) Uani 1 1 d . . . C1 C 0.62264(16) 0.38336(17) 1.0029(2) 0.0402(6) Uani 1 1 d . . . H1 H 0.6415(15) 0.3246(15) 1.039(2) 0.037(6) Uiso 1 1 d . . . C2 C 0.65707(18) 0.4580(2) 1.0812(3) 0.0509(7) Uani 1 1 d . . . H2 H 0.6982(18) 0.4531(16) 1.171(3) 0.055(8) Uiso 1 1 d . . . C3 C 0.6294(2) 0.5398(2) 1.0258(3) 0.0591(8) Uani 1 1 d . . . H3 H 0.6499(18) 0.5897(19) 1.072(3) 0.066(8) Uiso 1 1 d . . . C4 C 0.56755(19) 0.54606(18) 0.8937(3) 0.0523(7) Uani 1 1 d . . . H4 H 0.5464(17) 0.6003(17) 0.851(2) 0.055(8) Uiso 1 1 d . . . C5 C 0.53416(14) 0.46875(14) 0.8209(2) 0.0340(5) Uani 1 1 d . . . C6 C 0.62446(17) 0.10733(15) 0.8974(3) 0.0403(6) Uani 1 1 d . . . H6 H 0.6488(15) 0.1105(14) 0.831(2) 0.034(6) Uiso 1 1 d . . . C7 C 0.63870(18) 0.04418(16) 0.9948(3) 0.0492(7) Uani 1 1 d . . . H7 H 0.6766(18) -0.0059(18) 1.011(2) 0.065(8) Uiso 1 1 d . . . C8 C 0.58652(17) 0.07137(16) 1.0576(3) 0.0444(6) Uani 1 1 d . . . H8 H 0.5771(17) 0.0494(16) 1.129(2) 0.051(7) Uiso 1 1 d . . . C9 C 0.29700(15) 0.28106(16) 0.7296(2) 0.0363(5) Uani 1 1 d . . . H9 H 0.2823(14) 0.3070(13) 0.652(2) 0.026(6) Uiso 1 1 d . . . C10 C 0.24350(17) 0.24977(16) 0.7901(2) 0.0415(6) Uani 1 1 d . . . H10 H 0.1798(18) 0.2529(15) 0.761(2) 0.054(8) Uiso 1 1 d . . . C11 C 0.30475(17) 0.21297(16) 0.9082(2) 0.0402(6) Uani 1 1 d . . . H11 H 0.2929(16) 0.1847(16) 0.977(2) 0.049(7) Uiso 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 0.0271(2) 0.0234(2) 0.0274(2) 0.000 0.00635(18) 0.000 B1 0.0388(16) 0.0452(17) 0.0292(13) 0.0017(11) 0.0105(12) 0.0062(12) N1 0.0286(11) 0.0310(10) 0.0341(10) -0.0052(8) 0.0101(8) -0.0002(8) N2 0.0324(11) 0.0280(10) 0.0350(10) 0.0013(8) 0.0114(8) 0.0022(8) N3 0.0329(10) 0.0332(10) 0.0266(9) -0.0003(8) 0.0075(8) 0.0033(8) N4 0.0316(11) 0.0332(10) 0.0311(10) 0.0065(8) 0.0063(8) 0.0019(8) N5 0.0348(11) 0.0347(10) 0.0303(9) 0.0009(8) 0.0133(8) 0.0043(8) C1 0.0342(14) 0.0419(15) 0.0395(14) -0.0100(11) 0.0105(11) 0.0011(11) C2 0.0370(15) 0.066(2) 0.0471(17) -0.0254(14) 0.0148(13) -0.0073(13) C3 0.0508(18) 0.0508(18) 0.076(2) -0.0396(16) 0.0275(16) -0.0130(14) C4 0.0493(17) 0.0340(15) 0.074(2) -0.0155(14) 0.0261(16) -0.0025(12) C5 0.0269(12) 0.0280(12) 0.0496(14) -0.0061(10) 0.0187(10) -0.0010(9) C6 0.0364(14) 0.0318(13) 0.0508(15) -0.0014(11) 0.0165(12) 0.0035(10) C7 0.0409(16) 0.0287(13) 0.0732(19) 0.0115(12) 0.0193(14) 0.0105(11) C8 0.0370(15) 0.0409(14) 0.0506(16) 0.0173(12) 0.0137(12) 0.0034(11) C9 0.0338(13) 0.0414(14) 0.0285(11) -0.0039(11) 0.0081(10) 0.0057(10) C10 0.0290(13) 0.0513(17) 0.0414(13) -0.0120(11) 0.0120(11) 0.0037(10) C11 0.0400(14) 0.0432(15) 0.0426(13) -0.0028(11) 0.0225(12) 0.0026(11) _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 N2 2.1621(17) 2_656 ? Fe1 N2 2.1621(17) . ? Fe1 N3 2.1811(17) . ? Fe1 N3 2.1811(17) 2_656 ? Fe1 N1 2.2083(17) . ? Fe1 N1 2.2083(17) 2_656 ? B1 N4 1.548(3) . ? B1 N5 1.560(3) . ? B1 H1B 1.16(2) . ? B1 H2B 1.11(2) . ? N1 C1 1.341(3) . ? N1 C5 1.345(3) . ? N2 C6 1.337(3) . ? N2 N4 1.372(2) . ? N3 C9 1.343(3) . ? N3 N5 1.369(2) . ? N4 C8 1.342(3) . ? N5 C11 1.342(3) . ? C1 C2 1.383(3) . ? C1 H1 0.96(2) . ? C2 C3 1.362(4) . ? C2 H2 0.94(2) . ? C3 C4 1.382(4) . ? C3 H3 0.89(3) . ? C4 C5 1.387(3) . ? C4 H4 0.93(2) . ? C5 C5 1.490(4) 2_656 ? C6 C7 1.379(3) . ? C6 H6 0.97(2) . ? C7 C8 1.363(4) . ? C7 H7 0.94(3) . ? C8 H8 0.92(2) . ? C9 C10 1.381(3) . ? C9 H9 0.881(19) . ? C10 C11 1.380(3) . ? C10 H10 0.95(3) . ? C11 H11 0.95(2) . ? 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 N2 Fe1 N2 92.48(9) 2_656 . ? N2 Fe1 N3 88.66(6) 2_656 . ? N2 Fe1 N3 88.91(7) . . ? N2 Fe1 N3 88.91(7) 2_656 2_656 ? N2 Fe1 N3 88.66(6) . 2_656 ? N3 Fe1 N3 176.49(9) . 2_656 ? N2 Fe1 N1 170.22(7) 2_656 . ? N2 Fe1 N1 97.01(7) . . ? N3 Fe1 N1 93.86(6) . . ? N3 Fe1 N1 88.95(6) 2_656 . ? N2 Fe1 N1 97.01(6) 2_656 2_656 ? N2 Fe1 N1 170.22(7) . 2_656 ? N3 Fe1 N1 88.95(6) . 2_656 ? N3 Fe1 N1 93.86(6) 2_656 2_656 ? N1 Fe1 N1 73.62(9) . 2_656 ? N4 B1 N5 110.06(18) . . ? N4 B1 H1B 108.0(11) . . ? N5 B1 H1B 109.8(11) . . ? N4 B1 H2B 108.2(11) . . ? N5 B1 H2B 108.1(12) . . ? H1B B1 H2B 112.7(15) . . ? C1 N1 C5 118.39(19) . . ? C1 N1 Fe1 123.84(15) . . ? C5 N1 Fe1 117.71(14) . . ? C6 N2 N4 105.81(18) . . ? C6 N2 Fe1 127.17(15) . . ? N4 N2 Fe1 125.34(13) . . ? C9 N3 N5 105.33(18) . . ? C9 N3 Fe1 129.66(15) . . ? N5 N3 Fe1 123.03(13) . . ? C8 N4 N2 108.90(19) . . ? C8 N4 B1 128.7(2) . . ? N2 N4 B1 122.38(17) . . ? C11 N5 N3 109.73(18) . . ? C11 N5 B1 126.54(19) . . ? N3 N5 B1 122.97(18) . . ? N1 C1 C2 122.8(3) . . ? N1 C1 H1 116.5(13) . . ? C2 C1 H1 120.7(13) . . ? C3 C2 C1 118.7(3) . . ? C3 C2 H2 120.1(15) . . ? C1 C2 H2 121.2(16) . . ? C2 C3 C4 119.5(2) . . ? C2 C3 H3 121.9(18) . . ? C4 C3 H3 118.6(18) . . ? C3 C4 C5 119.2(3) . . ? C3 C4 H4 122.7(16) . . ? C5 C4 H4 118.1(16) . . ? N1 C5 C4 121.5(2) . . ? N1 C5 C5 115.46(12) . 2_656 ? C4 C5 C5 123.08(16) . 2_656 ? N2 C6 C7 111.1(2) . . ? N2 C6 H6 119.4(13) . . ? C7 C6 H6 129.5(13) . . ? C8 C7 C6 104.7(2) . . ? C8 C7 H7 130.0(16) . . ? C6 C7 H7 125.3(16) . . ? N4 C8 C7 109.4(2) . . ? N4 C8 H8 117.2(15) . . ? C7 C8 H8 133.3(15) . . ? N3 C9 C10 111.8(2) . . ? N3 C9 H9 117.3(14) . . ? C10 C9 H9 130.9(14) . . ? C11 C10 C9 104.1(2) . . ? C11 C10 H10 126.1(14) . . ? C9 C10 H10 129.7(14) . . ? N5 C11 C10 109.0(2) . . ? N5 C11 H11 122.4(15) . . ? C10 C11 H11 128.5(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Fe1 N1 C1 -165.0(3) 2_656 . . . ? N2 Fe1 N1 C1 0.90(18) . . . . ? N3 Fe1 N1 C1 90.27(18) . . . . ? N3 Fe1 N1 C1 -87.63(18) 2_656 . . . ? N1 Fe1 N1 C1 178.0(2) 2_656 . . . ? N2 Fe1 N1 C5 17.6(5) 2_656 . . . ? N2 Fe1 N1 C5 -176.48(16) . . . . ? N3 Fe1 N1 C5 -87.10(16) . . . . ? N3 Fe1 N1 C5 94.99(16) 2_656 . . . ? N1 Fe1 N1 C5 0.66(11) 2_656 . . . ? N2 Fe1 N2 C6 59.19(18) 2_656 . . . ? N3 Fe1 N2 C6 147.81(19) . . . . ? N3 Fe1 N2 C6 -29.66(19) 2_656 . . . ? N1 Fe1 N2 C6 -118.44(19) . . . . ? N1 Fe1 N2 C6 -134.8(4) 2_656 . . . ? N2 Fe1 N2 N4 -103.88(17) 2_656 . . . ? N3 Fe1 N2 N4 -15.26(16) . . . . ? N3 Fe1 N2 N4 167.27(16) 2_656 . . . ? N1 Fe1 N2 N4 78.49(16) . . . . ? N1 Fe1 N2 N4 62.1(5) 2_656 . . . ? N2 Fe1 N3 C9 -58.03(19) 2_656 . . . ? N2 Fe1 N3 C9 -150.54(19) . . . . ? N3 Fe1 N3 C9 -104.28(19) 2_656 . . . ? N1 Fe1 N3 C9 112.51(19) . . . . ? N1 Fe1 N3 C9 39.01(19) 2_656 . . . ? N2 Fe1 N3 N5 103.55(15) 2_656 . . . ? N2 Fe1 N3 N5 11.04(15) . . . . ? N3 Fe1 N3 N5 57.29(15) 2_656 . . . ? N1 Fe1 N3 N5 -85.92(15) . . . . ? N1 Fe1 N3 N5 -159.42(15) 2_656 . . . ? C6 N2 N4 C8 0.6(2) . . . . ? Fe1 N2 N4 C8 166.68(15) . . . . ? C6 N2 N4 B1 178.4(2) . . . . ? Fe1 N2 N4 B1 -15.6(3) . . . . ? N5 B1 N4 C8 -128.3(2) . . . . ? N5 B1 N4 N2 54.4(3) . . . . ? C9 N3 N5 C11 0.0(2) . . . . ? Fe1 N3 N5 C11 -165.42(14) . . . . ? C9 N3 N5 B1 -170.64(19) . . . . ? Fe1 N3 N5 B1 24.0(3) . . . . ? N4 B1 N5 C11 131.3(2) . . . . ? N4 B1 N5 N3 -59.7(3) . . . . ? C5 N1 C1 C2 0.7(3) . . . . ? Fe1 N1 C1 C2 -176.70(19) . . . . ? N1 C1 C2 C3 -1.1(4) . . . . ? C1 C2 C3 C4 0.3(4) . . . . ? C2 C3 C4 C5 0.8(4) . . . . ? C1 N1 C5 C4 0.6(3) . . . . ? Fe1 N1 C5 C4 178.09(18) . . . . ? C1 N1 C5 C5 -179.3(2) . . . 2_656 ? Fe1 N1 C5 C5 -1.8(3) . . . 2_656 ? C3 C4 C5 N1 -1.3(4) . . . . ? C3 C4 C5 C5 178.5(3) . . . 2_656 ? N4 N2 C6 C7 -0.9(3) . . . . ? Fe1 N2 C6 C7 -166.60(16) . . . . ? N2 C6 C7 C8 0.8(3) . . . . ? N2 N4 C8 C7 -0.2(3) . . . . ? B1 N4 C8 C7 -177.7(2) . . . . ? C6 C7 C8 N4 -0.4(3) . . . . ? N5 N3 C9 C10 0.4(2) . . . . ? Fe1 N3 C9 C10 164.41(15) . . . . ? N3 C9 C10 C11 -0.5(3) . . . . ? N3 N5 C11 C10 -0.3(2) . . . . ? B1 N5 C11 C10 169.9(2) . . . . ? C9 C10 C11 N5 0.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.300 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.058 #====================================================================== data_bipy2 _database_code_depnum_ccdc_archive 'CCDC 233282' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,2'-Bipyridine-bis[di(hydro)bis(1-pyrazolyl)borate iron(II) ; _chemical_name_common "2,2'-Bipyridine-bis(di(hydro)bis(1-pyrazolyl)borate iron(ii)" _chemical_melting_point 'not measured' _chemical_formula_moiety 'C22 H24 B2 Fe N10' _chemical_formula_sum 'C22 H24 B2 Fe N10' _chemical_formula_weight 505.98 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.1373(8) _cell_length_b 14.6208(8) _cell_length_c 10.8120(6) _cell_angle_alpha 90.00 _cell_angle_beta 113.775(2) _cell_angle_gamma 90.00 _cell_volume 2334.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2206 _cell_measurement_theta_min 4.813 _cell_measurement_theta_max 60.784 _exptl_crystal_description block _exptl_crystal_colour clear_intense_red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.680 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8760 _exptl_absorpt_correction_T_max 0.9540 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 3 sets of \w scans each set at different \f and/or 2\q angles and each scan (7s exposure) covering 0.3\% in \w. Crystal to detector distance 4.51. ; _diffrn_ambient_temperature 120(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 CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 8408 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_sigmaI/netI 0.0903 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 30.47 _reflns_number_total 3351 _reflns_number_gt 2195 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SMART-NT V6.1 (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0366P)^2^+0.3724P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3351 _refine_ls_number_parameters 207 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0951 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0856 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _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 0.5000 0.27133(3) 0.7500 0.01474(13) Uani 1 2 d S . . B1 B 0.48010(19) 0.20283(18) 1.0399(3) 0.0218(6) Uani 1 1 d . . . H1B H 0.5159(14) 0.2679(15) 1.0925(19) 0.018(6) Uiso 1 1 d . . . H2B H 0.4592(14) 0.1609(14) 1.106(2) 0.018(6) Uiso 1 1 d . . . N1 N 0.55702(12) 0.37394(11) 0.87424(17) 0.0161(4) Uani 1 1 d . . . N2 N 0.56200(12) 0.17106(12) 0.88390(17) 0.0179(4) Uani 1 1 d . . . N3 N 0.39257(12) 0.26934(12) 0.80028(16) 0.0166(4) Uani 1 1 d . . . N4 N 0.54319(12) 0.14679(12) 0.99257(17) 0.0187(4) Uani 1 1 d . . . N5 N 0.39301(12) 0.22703(13) 0.91362(16) 0.0186(4) Uani 1 1 d . . . C1 C 0.61803(15) 0.36814(16) 1.0035(2) 0.0203(5) Uani 1 1 d . . . H1 H 0.6331(15) 0.3111(17) 1.039(2) 0.018(6) Uiso 1 1 d . . . C2 C 0.65414(17) 0.44401(16) 1.0837(2) 0.0243(5) Uani 1 1 d . . . H2 H 0.6981(18) 0.4367(17) 1.174(3) 0.034(7) Uiso 1 1 d . . . C3 C 0.62870(17) 0.53029(17) 1.0295(3) 0.0274(6) Uani 1 1 d . . . H3 H 0.6536(17) 0.5806(18) 1.083(2) 0.030(7) Uiso 1 1 d . . . C4 C 0.56774(17) 0.53784(16) 0.8959(3) 0.0260(5) Uani 1 1 d . . . H4 H 0.5494(17) 0.5939(18) 0.857(2) 0.033(7) Uiso 1 1 d . . . C5 C 0.53246(15) 0.45892(14) 0.8208(2) 0.0189(5) Uani 1 1 d . . . C6 C 0.61941(16) 0.10746(15) 0.8753(2) 0.0215(5) Uani 1 1 d . . . H6 H 0.6395(15) 0.1094(15) 0.805(2) 0.016(6) Uiso 1 1 d . . . C7 C 0.63910(17) 0.04288(16) 0.9778(3) 0.0256(5) Uani 1 1 d . . . H7 H 0.6786(17) -0.0056(18) 0.997(2) 0.030(7) Uiso 1 1 d . . . C8 C 0.59000(17) 0.06993(16) 1.0493(2) 0.0240(5) Uani 1 1 d . . . H8 H 0.5832(16) 0.0440(15) 1.123(2) 0.020(6) Uiso 1 1 d . . . C9 C 0.30560(15) 0.29020(14) 0.7240(2) 0.0190(5) Uani 1 1 d . . . H9 H 0.2922(16) 0.3229(15) 0.640(2) 0.020(6) Uiso 1 1 d . . . C10 C 0.24961(16) 0.26212(16) 0.7871(2) 0.0212(5) Uani 1 1 d . . . H10 H 0.1888(16) 0.2686(15) 0.757(2) 0.016(6) Uiso 1 1 d . . . C11 C 0.30770(16) 0.22154(16) 0.9055(2) 0.0210(5) Uani 1 1 d . . . H11 H 0.2974(15) 0.1929(15) 0.979(2) 0.019(6) Uiso 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 0.0145(2) 0.0117(2) 0.0165(2) 0.000 0.00470(18) 0.000 B1 0.0237(15) 0.0223(13) 0.0200(13) 0.0016(10) 0.0095(11) 0.0011(11) N1 0.0150(10) 0.0140(9) 0.0183(9) -0.0005(7) 0.0056(8) 0.0014(7) N2 0.0182(10) 0.0160(9) 0.0195(10) 0.0010(7) 0.0077(8) -0.0002(7) N3 0.0195(10) 0.0142(8) 0.0156(8) 0.0004(8) 0.0064(7) -0.0004(8) N4 0.0188(10) 0.0166(9) 0.0183(9) 0.0038(7) 0.0051(8) 0.0005(7) N5 0.0212(10) 0.0169(9) 0.0192(9) 0.0025(8) 0.0096(8) 0.0018(8) C1 0.0175(12) 0.0218(12) 0.0206(12) -0.0019(9) 0.0066(10) 0.0007(9) C2 0.0176(12) 0.0315(14) 0.0228(13) -0.0108(10) 0.0070(10) -0.0030(10) C3 0.0243(14) 0.0217(13) 0.0380(15) -0.0149(11) 0.0145(12) -0.0074(10) C4 0.0262(14) 0.0170(12) 0.0367(15) -0.0053(10) 0.0149(12) -0.0010(10) C5 0.0163(12) 0.0156(11) 0.0267(12) -0.0032(9) 0.0105(10) 0.0005(8) C6 0.0211(13) 0.0166(11) 0.0264(13) 0.0005(9) 0.0093(10) -0.0003(9) C7 0.0209(13) 0.0147(12) 0.0397(15) 0.0026(10) 0.0106(11) 0.0023(10) C8 0.0229(13) 0.0197(12) 0.0261(13) 0.0078(10) 0.0065(11) -0.0005(9) C9 0.0203(12) 0.0170(12) 0.0176(11) -0.0013(9) 0.0055(9) 0.0017(8) C10 0.0176(12) 0.0215(12) 0.0241(12) -0.0055(9) 0.0081(10) -0.0008(10) C11 0.0245(12) 0.0186(11) 0.0241(12) 0.0000(10) 0.0140(10) 0.0017(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.9762(17) . ? Fe1 N1 1.9762(17) 2_656 ? Fe1 N3 2.0153(17) . ? Fe1 N3 2.0153(17) 2_656 ? Fe1 N2 2.0195(18) 2_656 ? Fe1 N2 2.0195(18) . ? B1 N4 1.546(3) . ? B1 N5 1.554(3) . ? B1 H1B 1.14(2) . ? B1 H2B 1.09(2) . ? N1 C1 1.349(3) . ? N1 C5 1.360(3) . ? N2 C6 1.342(3) . ? N2 N4 1.373(2) . ? N3 C9 1.345(3) . ? N3 N5 1.370(2) . ? N4 C8 1.355(3) . ? N5 C11 1.346(3) . ? C1 C2 1.384(3) . ? C1 H1 0.91(2) . ? C2 C3 1.382(3) . ? C2 H2 0.95(3) . ? C3 C4 1.386(3) . ? C3 H3 0.92(3) . ? C4 C5 1.393(3) . ? C4 H4 0.92(3) . ? C5 C5 1.466(4) 2_656 ? C6 C7 1.392(3) . ? C6 H6 0.94(2) . ? C7 C8 1.369(4) . ? C7 H7 0.92(3) . ? C8 H8 0.93(2) . ? C9 C10 1.395(3) . ? C9 H9 0.97(2) . ? C10 C11 1.379(3) . ? C10 H10 0.91(2) . ? C11 H11 0.97(2) . ? 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 N1 81.22(10) . 2_656 ? N1 Fe1 N3 92.47(7) . . ? N1 Fe1 N3 88.79(7) 2_656 . ? N1 Fe1 N3 88.79(7) . 2_656 ? N1 Fe1 N3 92.47(7) 2_656 2_656 ? N3 Fe1 N3 178.35(10) . 2_656 ? N1 Fe1 N2 177.15(8) . 2_656 ? N1 Fe1 N2 95.94(7) 2_656 2_656 ? N3 Fe1 N2 87.22(7) . 2_656 ? N3 Fe1 N2 91.58(7) 2_656 2_656 ? N1 Fe1 N2 95.94(7) . . ? N1 Fe1 N2 177.15(8) 2_656 . ? N3 Fe1 N2 91.58(7) . . ? N3 Fe1 N2 87.22(7) 2_656 . ? N2 Fe1 N2 86.90(10) 2_656 . ? N4 B1 N5 108.25(18) . . ? N4 B1 H1B 109.8(11) . . ? N5 B1 H1B 110.2(11) . . ? N4 B1 H2B 109.7(11) . . ? N5 B1 H2B 107.1(11) . . ? H1B B1 H2B 111.8(14) . . ? C1 N1 C5 117.61(18) . . ? C1 N1 Fe1 126.99(15) . . ? C5 N1 Fe1 115.38(14) . . ? C6 N2 N4 106.08(17) . . ? C6 N2 Fe1 127.58(15) . . ? N4 N2 Fe1 125.76(14) . . ? C9 N3 N5 106.20(17) . . ? C9 N3 Fe1 129.00(14) . . ? N5 N3 Fe1 123.57(13) . . ? C8 N4 N2 109.04(18) . . ? C8 N4 B1 127.69(19) . . ? N2 N4 B1 123.25(17) . . ? C11 N5 N3 109.40(17) . . ? C11 N5 B1 125.64(18) . . ? N3 N5 B1 124.39(17) . . ? N1 C1 C2 123.1(2) . . ? N1 C1 H1 116.9(14) . . ? C2 C1 H1 119.9(14) . . ? C3 C2 C1 119.2(2) . . ? C3 C2 H2 120.6(15) . . ? C1 C2 H2 120.2(15) . . ? C2 C3 C4 118.7(2) . . ? C2 C3 H3 118.9(15) . . ? C4 C3 H3 122.5(15) . . ? C3 C4 C5 119.5(2) . . ? C3 C4 H4 120.9(16) . . ? C5 C4 H4 119.5(16) . . ? N1 C5 C4 121.9(2) . . ? N1 C5 C5 114.01(12) . 2_656 ? C4 C5 C5 124.09(14) . 2_656 ? N2 C6 C7 110.9(2) . . ? N2 C6 H6 120.6(14) . . ? C7 C6 H6 128.5(14) . . ? C8 C7 C6 104.8(2) . . ? C8 C7 H7 127.1(15) . . ? C6 C7 H7 128.1(15) . . ? N4 C8 C7 109.1(2) . . ? N4 C8 H8 119.3(14) . . ? C7 C8 H8 131.5(14) . . ? N3 C9 C10 110.8(2) . . ? N3 C9 H9 117.9(14) . . ? C10 C9 H9 131.2(14) . . ? C11 C10 C9 104.4(2) . . ? C11 C10 H10 127.9(13) . . ? C9 C10 H10 127.7(13) . . ? N5 C11 C10 109.24(19) . . ? N5 C11 H11 118.7(14) . . ? C10 C11 H11 132.0(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Fe1 N1 C1 -178.6(2) 2_656 . . . ? N3 Fe1 N1 C1 93.00(18) . . . . ? N3 Fe1 N1 C1 -85.92(18) 2_656 . . . ? N2 Fe1 N1 C1 176.5(15) 2_656 . . . ? N2 Fe1 N1 C1 1.15(18) . . . . ? N1 Fe1 N1 C5 0.03(11) 2_656 . . . ? N3 Fe1 N1 C5 -88.37(15) . . . . ? N3 Fe1 N1 C5 92.71(15) 2_656 . . . ? N2 Fe1 N1 C5 -4.8(16) 2_656 . . . ? N2 Fe1 N1 C5 179.78(16) . . . . ? N1 Fe1 N2 C6 -117.56(19) . . . . ? N1 Fe1 N2 C6 -112.7(15) 2_656 . . . ? N3 Fe1 N2 C6 149.79(19) . . . . ? N3 Fe1 N2 C6 -29.07(19) 2_656 . . . ? N2 Fe1 N2 C6 62.67(17) 2_656 . . . ? N1 Fe1 N2 N4 72.49(16) . . . . ? N1 Fe1 N2 N4 77.3(16) 2_656 . . . ? N3 Fe1 N2 N4 -20.16(17) . . . . ? N3 Fe1 N2 N4 160.98(17) 2_656 . . . ? N2 Fe1 N2 N4 -107.28(18) 2_656 . . . ? N1 Fe1 N3 C9 112.93(18) . . . . ? N1 Fe1 N3 C9 31.78(19) 2_656 . . . ? N3 Fe1 N3 C9 -107.66(18) 2_656 . . . ? N2 Fe1 N3 C9 -64.23(19) 2_656 . . . ? N2 Fe1 N3 C9 -151.05(18) . . . . ? N1 Fe1 N3 N5 -81.57(16) . . . . ? N1 Fe1 N3 N5 -162.73(16) 2_656 . . . ? N3 Fe1 N3 N5 57.83(15) 2_656 . . . ? N2 Fe1 N3 N5 101.27(16) 2_656 . . . ? N2 Fe1 N3 N5 14.44(16) . . . . ? C6 N2 N4 C8 0.8(2) . . . . ? Fe1 N2 N4 C8 172.50(15) . . . . ? C6 N2 N4 B1 179.2(2) . . . . ? Fe1 N2 N4 B1 -9.1(3) . . . . ? N5 B1 N4 C8 -135.5(2) . . . . ? N5 B1 N4 N2 46.4(3) . . . . ? C9 N3 N5 C11 0.6(2) . . . . ? Fe1 N3 N5 C11 -167.72(14) . . . . ? C9 N3 N5 B1 -171.11(19) . . . . ? Fe1 N3 N5 B1 20.6(3) . . . . ? N4 B1 N5 C11 136.2(2) . . . . ? N4 B1 N5 N3 -53.5(3) . . . . ? C5 N1 C1 C2 1.8(3) . . . . ? Fe1 N1 C1 C2 -179.58(17) . . . . ? N1 C1 C2 C3 -1.5(4) . . . . ? C1 C2 C3 C4 -0.2(4) . . . . ? C2 C3 C4 C5 1.3(4) . . . . ? C1 N1 C5 C4 -0.6(3) . . . . ? Fe1 N1 C5 C4 -179.37(17) . . . . ? C1 N1 C5 C5 178.7(2) . . . 2_656 ? Fe1 N1 C5 C5 -0.1(3) . . . 2_656 ? C3 C4 C5 N1 -0.9(4) . . . . ? C3 C4 C5 C5 179.8(3) . . . 2_656 ? N4 N2 C6 C7 -0.8(3) . . . . ? Fe1 N2 C6 C7 -172.30(15) . . . . ? N2 C6 C7 C8 0.5(3) . . . . ? N2 N4 C8 C7 -0.5(3) . . . . ? B1 N4 C8 C7 -178.8(2) . . . . ? C6 C7 C8 N4 0.0(3) . . . . ? N5 N3 C9 C10 0.2(2) . . . . ? Fe1 N3 C9 C10 167.70(15) . . . . ? N3 C9 C10 C11 -1.0(2) . . . . ? N3 N5 C11 C10 -1.2(2) . . . . ? B1 N5 C11 C10 170.4(2) . . . . ? C9 C10 C11 N5 1.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 30.47 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 0.379 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.077 #====================================================================== data_bipy3 _database_code_depnum_ccdc_archive 'CCDC 233283' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,2'-Bipyridine-bis[di(hydro)bis(1-pyrazolyl)borate iron(II) ; _chemical_name_common "2,2'-Bipyridine-bis(di(hydro)bis(1-pyrazolyl)borate iron(ii)" _chemical_melting_point 'not measured' _chemical_formula_moiety 'C22 H24 B2 Fe N10' _chemical_formula_sum 'C22 H24 B2 Fe N10' _chemical_formula_weight 505.98 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.1106(11) _cell_length_b 14.5909(10) _cell_length_c 10.8281(8) _cell_angle_alpha 90.00 _cell_angle_beta 113.895(3) _cell_angle_gamma 90.00 _cell_volume 2327.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 30(2) _cell_measurement_reflns_used 1925 _cell_measurement_theta_min 6.450 _cell_measurement_theta_max 55.047 _exptl_crystal_description block _exptl_crystal_colour clear_intense_red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.682 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8757 _exptl_absorpt_correction_T_max 0.9538 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 3 sets of \w scans each set at different \f and/or 2\q angles and each scan (10s exposure) covering 0.9\% in \w. Crystal to detector distance 5.51. ; _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 CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 6333 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_sigmaI/netI 0.0981 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 28.53 _reflns_number_total 2662 _reflns_number_gt 1784 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SMART-NT V6.1 (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0343P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 2662 _refine_ls_number_parameters 207 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0946 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.0935 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 0.5000 0.27104(4) 0.7500 0.01013(16) Uani 1 2 d S . . B1 B 0.4799(2) 0.2020(2) 1.0401(3) 0.0138(7) Uani 1 1 d . . . H1B H 0.5178(17) 0.2667(18) 1.090(2) 0.017(7) Uiso 1 1 d . . . H2B H 0.4595(17) 0.1582(16) 1.111(2) 0.008(7) Uiso 1 1 d . . . N1 N 0.55697(15) 0.37432(14) 0.8741(2) 0.0109(5) Uani 1 1 d . . . N2 N 0.56253(15) 0.17062(14) 0.8843(2) 0.0111(5) Uani 1 1 d . . . N3 N 0.39219(14) 0.26869(15) 0.79997(19) 0.0117(5) Uani 1 1 d . . . N4 N 0.54363(15) 0.14588(14) 0.9933(2) 0.0113(5) Uani 1 1 d . . . N5 N 0.39245(14) 0.22619(15) 0.91336(19) 0.0113(5) Uani 1 1 d . . . C1 C 0.61837(19) 0.3681(2) 1.0050(3) 0.0130(6) Uani 1 1 d . . . H1 H 0.6374(17) 0.3074(18) 1.039(2) 0.005(7) Uiso 1 1 d . . . C2 C 0.65388(19) 0.44429(19) 1.0846(3) 0.0131(6) Uani 1 1 d . . . H2 H 0.6986(19) 0.4357(18) 1.178(3) 0.017(7) Uiso 1 1 d . . . C3 C 0.62861(19) 0.5308(2) 1.0302(3) 0.0142(6) Uani 1 1 d . . . H3 H 0.6516(18) 0.5810(18) 1.078(2) 0.009(7) Uiso 1 1 d . . . C4 C 0.56766(19) 0.53864(19) 0.8958(3) 0.0140(6) Uani 1 1 d . . . H4 H 0.5471(17) 0.5992(17) 0.855(2) 0.008(7) Uiso 1 1 d . . . C5 C 0.53281(18) 0.45944(17) 0.8211(2) 0.0121(6) Uani 1 1 d . . . C6 C 0.62017(19) 0.10696(18) 0.8760(3) 0.0128(6) Uani 1 1 d . . . H6 H 0.6424(18) 0.1100(17) 0.804(2) 0.012(7) Uiso 1 1 d . . . C7 C 0.64036(19) 0.04218(19) 0.9787(3) 0.0140(6) Uani 1 1 d . . . H7 H 0.6797(18) -0.0081(18) 0.995(2) 0.011(7) Uiso 1 1 d . . . C8 C 0.59072(19) 0.06927(18) 1.0508(3) 0.0126(6) Uani 1 1 d . . . H8 H 0.584(2) 0.0441(18) 1.130(3) 0.023(8) Uiso 1 1 d . . . C9 C 0.30490(19) 0.28944(18) 0.7238(3) 0.0119(6) Uani 1 1 d . . . H9 H 0.2917(19) 0.3190(18) 0.640(3) 0.015(7) Uiso 1 1 d . . . C10 C 0.24824(19) 0.26157(19) 0.7858(3) 0.0129(6) Uani 1 1 d . . . H10 H 0.1859(19) 0.2668(18) 0.757(2) 0.017(7) Uiso 1 1 d . . . C11 C 0.30672(19) 0.22105(18) 0.9050(3) 0.0129(6) Uani 1 1 d . . . H11 H 0.2956(18) 0.1930(18) 0.981(2) 0.014(7) Uiso 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 0.0103(3) 0.0090(3) 0.0104(3) 0.000 0.0036(2) 0.000 B1 0.0141(18) 0.0146(17) 0.0135(16) 0.0006(13) 0.0064(14) 0.0014(13) N1 0.0102(13) 0.0129(13) 0.0098(11) -0.0002(9) 0.0040(10) 0.0014(9) N2 0.0120(13) 0.0100(12) 0.0109(12) -0.0001(9) 0.0041(10) -0.0011(9) N3 0.0143(13) 0.0103(11) 0.0093(11) -0.0015(10) 0.0035(10) -0.0009(10) N4 0.0129(13) 0.0108(12) 0.0100(12) 0.0021(9) 0.0046(10) -0.0023(9) N5 0.0126(12) 0.0102(11) 0.0102(11) 0.0000(10) 0.0038(10) -0.0004(10) C1 0.0106(15) 0.0149(16) 0.0141(15) 0.0030(12) 0.0057(13) 0.0013(11) C2 0.0095(15) 0.0203(16) 0.0089(14) -0.0022(12) 0.0033(12) -0.0017(12) C3 0.0136(16) 0.0135(15) 0.0155(15) -0.0068(12) 0.0058(13) -0.0036(11) C4 0.0126(15) 0.0131(15) 0.0189(16) -0.0010(12) 0.0089(13) 0.0013(12) C5 0.0104(15) 0.0124(14) 0.0139(14) -0.0008(11) 0.0055(12) -0.0005(11) C6 0.0124(16) 0.0127(15) 0.0134(15) -0.0014(11) 0.0052(13) -0.0023(11) C7 0.0127(16) 0.0097(15) 0.0163(15) 0.0006(11) 0.0024(13) 0.0012(12) C8 0.0139(16) 0.0094(14) 0.0110(14) 0.0013(11) 0.0014(13) -0.0024(11) C9 0.0156(16) 0.0128(15) 0.0069(13) -0.0011(11) 0.0040(12) 0.0001(11) C10 0.0092(15) 0.0132(15) 0.0140(14) -0.0022(11) 0.0024(12) 0.0020(12) C11 0.0172(15) 0.0111(14) 0.0134(14) -0.0036(12) 0.0093(12) -0.0015(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.980(2) . ? Fe1 N1 1.980(2) 2_656 ? Fe1 N3 2.018(2) 2_656 ? Fe1 N3 2.018(2) . ? Fe1 N2 2.022(2) 2_656 ? Fe1 N2 2.022(2) . ? B1 N4 1.551(4) . ? B1 N5 1.557(4) . ? B1 H1B 1.14(3) . ? B1 H2B 1.14(2) . ? N1 C5 1.357(3) . ? N1 C1 1.363(3) . ? N2 C6 1.342(3) . ? N2 N4 1.381(3) . ? N3 C9 1.345(3) . ? N3 N5 1.374(3) . ? N4 C8 1.353(3) . ? N5 C11 1.349(3) . ? C1 C2 1.381(4) . ? C1 H1 0.96(3) . ? C2 C3 1.382(4) . ? C2 H2 0.99(3) . ? C3 C4 1.392(4) . ? C3 H3 0.89(3) . ? C4 C5 1.392(3) . ? C4 H4 0.98(2) . ? C5 C5 1.473(5) 2_656 ? C6 C7 1.394(4) . ? C6 H6 0.98(2) . ? C7 C8 1.382(4) . ? C7 H7 0.94(3) . ? C8 H8 0.98(3) . ? C9 C10 1.395(4) . ? C9 H9 0.94(3) . ? C10 C11 1.385(4) . ? C10 H10 0.93(3) . ? C11 H11 1.00(2) . ? 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 N1 80.88(13) . 2_656 ? N1 Fe1 N3 88.98(9) . 2_656 ? N1 Fe1 N3 92.50(9) 2_656 2_656 ? N1 Fe1 N3 92.50(9) . . ? N1 Fe1 N3 88.98(9) 2_656 . ? N3 Fe1 N3 178.05(13) 2_656 . ? N1 Fe1 N2 176.85(10) . 2_656 ? N1 Fe1 N2 96.00(8) 2_656 2_656 ? N3 Fe1 N2 91.56(9) 2_656 2_656 ? N3 Fe1 N2 87.03(8) . 2_656 ? N1 Fe1 N2 96.00(8) . . ? N1 Fe1 N2 176.85(10) 2_656 . ? N3 Fe1 N2 87.03(8) 2_656 . ? N3 Fe1 N2 91.56(9) . . ? N2 Fe1 N2 87.12(12) 2_656 . ? N4 B1 N5 108.3(2) . . ? N4 B1 H1B 107.3(13) . . ? N5 B1 H1B 110.7(13) . . ? N4 B1 H2B 109.3(12) . . ? N5 B1 H2B 108.3(13) . . ? H1B B1 H2B 112.9(16) . . ? C5 N1 C1 117.6(2) . . ? C5 N1 Fe1 115.77(17) . . ? C1 N1 Fe1 126.62(18) . . ? C6 N2 N4 105.9(2) . . ? C6 N2 Fe1 127.61(17) . . ? N4 N2 Fe1 125.85(17) . . ? C9 N3 N5 105.9(2) . . ? C9 N3 Fe1 129.13(17) . . ? N5 N3 Fe1 123.77(16) . . ? C8 N4 N2 109.4(2) . . ? C8 N4 B1 127.5(2) . . ? N2 N4 B1 123.1(2) . . ? C11 N5 N3 109.4(2) . . ? C11 N5 B1 125.6(2) . . ? N3 N5 B1 124.3(2) . . ? N1 C1 C2 122.5(3) . . ? N1 C1 H1 116.4(15) . . ? C2 C1 H1 121.1(15) . . ? C1 C2 C3 119.5(3) . . ? C1 C2 H2 119.1(16) . . ? C3 C2 H2 121.4(16) . . ? C2 C3 C4 118.8(3) . . ? C2 C3 H3 121.4(17) . . ? C4 C3 H3 119.7(17) . . ? C5 C4 C3 119.1(3) . . ? C5 C4 H4 120.1(15) . . ? C3 C4 H4 120.7(15) . . ? N1 C5 C4 122.4(2) . . ? N1 C5 C5 113.79(14) . 2_656 ? C4 C5 C5 123.86(16) . 2_656 ? N2 C6 C7 111.1(2) . . ? N2 C6 H6 120.4(15) . . ? C7 C6 H6 128.5(15) . . ? C8 C7 C6 104.8(2) . . ? C8 C7 H7 128.0(15) . . ? C6 C7 H7 127.2(15) . . ? N4 C8 C7 108.7(2) . . ? N4 C8 H8 118.4(17) . . ? C7 C8 H8 132.8(17) . . ? N3 C9 C10 111.4(2) . . ? N3 C9 H9 117.6(17) . . ? C10 C9 H9 131.0(17) . . ? C11 C10 C9 104.0(2) . . ? C11 C10 H10 125.9(16) . . ? C9 C10 H10 130.1(16) . . ? N5 C11 C10 109.3(2) . . ? N5 C11 H11 119.2(16) . . ? C10 C11 H11 131.5(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Fe1 N1 C5 -0.12(13) 2_656 . . . ? N3 Fe1 N1 C5 92.58(18) 2_656 . . . ? N3 Fe1 N1 C5 -88.68(18) . . . . ? N2 Fe1 N1 C5 -7.3(18) 2_656 . . . ? N2 Fe1 N1 C5 179.49(19) . . . . ? N1 Fe1 N1 C1 -178.9(3) 2_656 . . . ? N3 Fe1 N1 C1 -86.2(2) 2_656 . . . ? N3 Fe1 N1 C1 92.5(2) . . . . ? N2 Fe1 N1 C1 173.9(16) 2_656 . . . ? N2 Fe1 N1 C1 0.7(2) . . . . ? N1 Fe1 N2 C6 -117.6(2) . . . . ? N1 Fe1 N2 C6 -110.5(17) 2_656 . . . ? N3 Fe1 N2 C6 -29.0(2) 2_656 . . . ? N3 Fe1 N2 C6 149.7(2) . . . . ? N2 Fe1 N2 C6 62.7(2) 2_656 . . . ? N1 Fe1 N2 N4 72.66(19) . . . . ? N1 Fe1 N2 N4 79.8(17) 2_656 . . . ? N3 Fe1 N2 N4 161.3(2) 2_656 . . . ? N3 Fe1 N2 N4 -20.0(2) . . . . ? N2 Fe1 N2 N4 -107.0(2) 2_656 . . . ? N1 Fe1 N3 C9 112.7(2) . . . . ? N1 Fe1 N3 C9 31.9(2) 2_656 . . . ? N3 Fe1 N3 C9 -107.7(2) 2_656 . . . ? N2 Fe1 N3 C9 -64.1(2) 2_656 . . . ? N2 Fe1 N3 C9 -151.2(2) . . . . ? N1 Fe1 N3 N5 -81.69(19) . . . . ? N1 Fe1 N3 N5 -162.51(19) 2_656 . . . ? N3 Fe1 N3 N5 57.88(18) 2_656 . . . ? N2 Fe1 N3 N5 101.43(19) 2_656 . . . ? N2 Fe1 N3 N5 14.39(19) . . . . ? C6 N2 N4 C8 1.1(3) . . . . ? Fe1 N2 N4 C8 172.62(18) . . . . ? C6 N2 N4 B1 179.3(2) . . . . ? Fe1 N2 N4 B1 -9.1(3) . . . . ? N5 B1 N4 C8 -135.8(3) . . . . ? N5 B1 N4 N2 46.3(3) . . . . ? C9 N3 N5 C11 0.3(3) . . . . ? Fe1 N3 N5 C11 -168.07(17) . . . . ? C9 N3 N5 B1 -171.0(2) . . . . ? Fe1 N3 N5 B1 20.6(3) . . . . ? N4 B1 N5 C11 136.7(3) . . . . ? N4 B1 N5 N3 -53.4(3) . . . . ? C5 N1 C1 C2 1.9(4) . . . . ? Fe1 N1 C1 C2 -179.3(2) . . . . ? N1 C1 C2 C3 -1.6(4) . . . . ? C1 C2 C3 C4 0.0(4) . . . . ? C2 C3 C4 C5 1.2(4) . . . . ? C1 N1 C5 C4 -0.7(4) . . . . ? Fe1 N1 C5 C4 -179.6(2) . . . . ? C1 N1 C5 C5 179.2(3) . . . 2_656 ? Fe1 N1 C5 C5 0.3(3) . . . 2_656 ? C3 C4 C5 N1 -0.9(4) . . . . ? C3 C4 C5 C5 179.3(3) . . . 2_656 ? N4 N2 C6 C7 -1.0(3) . . . . ? Fe1 N2 C6 C7 -172.36(18) . . . . ? N2 C6 C7 C8 0.6(3) . . . . ? N2 N4 C8 C7 -0.7(3) . . . . ? B1 N4 C8 C7 -178.9(3) . . . . ? C6 C7 C8 N4 0.1(3) . . . . ? N5 N3 C9 C10 0.3(3) . . . . ? Fe1 N3 C9 C10 167.84(18) . . . . ? N3 C9 C10 C11 -0.7(3) . . . . ? N3 N5 C11 C10 -0.8(3) . . . . ? B1 N5 C11 C10 170.4(2) . . . . ? C9 C10 C11 N5 0.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.896 _diffrn_reflns_theta_full 28.53 _diffrn_measured_fraction_theta_full 0.896 _refine_diff_density_max 0.360 _refine_diff_density_min -0.510 _refine_diff_density_rms 0.085 #====================================================================== data_bipy4 _database_code_depnum_ccdc_archive 'CCDC 233284' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,2'-Bipyridine-bis[di(hydro)bis(1-pyrazolyl)borate iron(II) ; _chemical_name_common "2,2'-Bipyridine-bis(di(hydro)bis(1-pyrazolyl)borate iron(ii)" _chemical_melting_point 'not measured' _chemical_formula_moiety 'C22 H24 B2 Fe N10' _chemical_formula_sum 'C22 H24 B2 Fe N10' _chemical_formula_weight 505.98 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.0350(9) _cell_length_b 14.9377(9) _cell_length_c 11.0470(7) _cell_angle_alpha 90.00 _cell_angle_beta 114.986(2) _cell_angle_gamma 90.00 _cell_volume 2398.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 30(2) _cell_measurement_reflns_used 1820 _cell_measurement_theta_min 6.441 _cell_measurement_theta_max 54.301 _exptl_crystal_description block _exptl_crystal_colour clear_intense_red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.662 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8790 _exptl_absorpt_correction_T_max 0.9551 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 3 sets of \w scans each set at different \f and/or 2\q angles and each scan (7s exposure) covering 0.3\% in \w. Crystal to detector distance 5.51. ; _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 CCD 1K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 6071 _diffrn_reflns_av_R_equivalents 0.0629 _diffrn_reflns_av_sigmaI/netI 0.1026 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 28.32 _reflns_number_total 2700 _reflns_number_gt 1884 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SMART-NT V6.1 (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0407P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 2700 _refine_ls_number_parameters 207 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1089 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1073 _refine_ls_wR_factor_gt 0.0969 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.225 _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 0.5000 0.26910(4) 0.7500 0.01063(19) Uani 1 2 d S . . B1 B 0.4790(3) 0.2033(2) 1.0417(4) 0.0137(8) Uani 1 1 d . . . H1B H 0.515(2) 0.272(2) 1.083(3) 0.020(8) Uiso 1 1 d . . . H2B H 0.460(2) 0.1656(18) 1.115(3) 0.010(7) Uiso 1 1 d . . . N1 N 0.56202(17) 0.38814(16) 0.8759(2) 0.0131(6) Uani 1 1 d . . . N2 N 0.56881(17) 0.16947(16) 0.9018(2) 0.0134(6) Uani 1 1 d . . . N3 N 0.38375(16) 0.26426(16) 0.8037(2) 0.0130(5) Uani 1 1 d . . . N4 N 0.54447(16) 0.14485(16) 1.0021(2) 0.0119(6) Uani 1 1 d . . . N5 N 0.38736(16) 0.22111(16) 0.9152(2) 0.0122(5) Uani 1 1 d . . . C1 C 0.6230(2) 0.3835(2) 1.0051(3) 0.0145(7) Uani 1 1 d . . . H1 H 0.6426(18) 0.3239(19) 1.038(2) 0.000(7) Uiso 1 1 d . . . C2 C 0.6569(2) 0.4586(2) 1.0837(3) 0.0159(7) Uani 1 1 d . . . H2 H 0.700(2) 0.453(2) 1.180(3) 0.022(9) Uiso 1 1 d . . . C3 C 0.6286(2) 0.5425(2) 1.0278(3) 0.0176(7) Uani 1 1 d . . . H3 H 0.649(2) 0.595(2) 1.080(3) 0.013(8) Uiso 1 1 d . . . C4 C 0.5668(2) 0.5485(2) 0.8946(3) 0.0162(7) Uani 1 1 d . . . H4 H 0.550(2) 0.605(2) 0.858(3) 0.017(9) Uiso 1 1 d . . . C5 C 0.5345(2) 0.47011(19) 0.8214(3) 0.0130(7) Uani 1 1 d . . . C6 C 0.6273(2) 0.1059(2) 0.8994(3) 0.0140(7) Uani 1 1 d . . . H6 H 0.6498(19) 0.1097(18) 0.833(3) 0.005(7) Uiso 1 1 d . . . C7 C 0.6425(2) 0.0418(2) 0.9971(3) 0.0147(7) Uani 1 1 d . . . H7 H 0.680(2) -0.010(2) 1.015(3) 0.017(9) Uiso 1 1 d . . . C8 C 0.5886(2) 0.0689(2) 1.0597(3) 0.0149(7) Uani 1 1 d . . . H8 H 0.579(2) 0.047(2) 1.132(3) 0.015(8) Uiso 1 1 d . . . C9 C 0.2938(2) 0.2799(2) 0.7276(3) 0.0121(6) Uani 1 1 d . . . H9 H 0.277(2) 0.3093(18) 0.647(3) 0.007(8) Uiso 1 1 d . . . C10 C 0.2391(2) 0.2486(2) 0.7887(3) 0.0148(7) Uani 1 1 d . . . H10 H 0.168(2) 0.250(2) 0.756(3) 0.030(10) Uiso 1 1 d . . . C11 C 0.3015(2) 0.2115(2) 0.9070(3) 0.0141(7) Uani 1 1 d . . . H11 H 0.289(2) 0.1817(19) 0.977(3) 0.010(8) Uiso 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 0.0067(3) 0.0108(3) 0.0127(3) 0.000 0.0024(3) 0.000 B1 0.0115(19) 0.0167(19) 0.0109(18) 0.0004(14) 0.0029(16) 0.0031(13) N1 0.0088(14) 0.0150(14) 0.0150(14) 0.0008(11) 0.0044(12) 0.0014(10) N2 0.0093(14) 0.0150(14) 0.0147(14) -0.0004(11) 0.0039(12) 0.0010(10) N3 0.0133(13) 0.0123(12) 0.0117(13) -0.0019(11) 0.0037(11) 0.0014(11) N4 0.0075(14) 0.0150(14) 0.0110(13) 0.0008(11) 0.0018(12) -0.0018(10) N5 0.0096(13) 0.0131(14) 0.0127(13) -0.0004(11) 0.0036(11) 0.0014(10) C1 0.0096(17) 0.0169(18) 0.0197(18) -0.0011(14) 0.0089(15) -0.0004(13) C2 0.0074(17) 0.0213(18) 0.0170(18) -0.0036(14) 0.0032(15) -0.0002(13) C3 0.0158(18) 0.0174(18) 0.0232(19) -0.0079(15) 0.0118(16) -0.0014(14) C4 0.0132(17) 0.0141(17) 0.0229(19) 0.0000(14) 0.0093(16) -0.0003(13) C5 0.0075(16) 0.0161(16) 0.0175(17) -0.0002(13) 0.0074(14) 0.0007(12) C6 0.0103(17) 0.0147(17) 0.0152(17) -0.0028(13) 0.0037(14) -0.0022(12) C7 0.0102(17) 0.0128(16) 0.0186(18) 0.0001(14) 0.0034(14) 0.0009(13) C8 0.0148(18) 0.0114(16) 0.0156(17) 0.0027(13) 0.0036(15) -0.0007(12) C9 0.0110(16) 0.0108(16) 0.0109(16) -0.0020(13) 0.0010(13) -0.0003(12) C10 0.0105(16) 0.0178(19) 0.0146(16) -0.0026(12) 0.0037(14) -0.0001(12) C11 0.0126(16) 0.0155(17) 0.0165(16) -0.0004(13) 0.0084(14) 0.0000(12) _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 N2 2.164(2) 2_656 ? Fe1 N2 2.164(2) . ? Fe1 N3 2.183(2) 2_656 ? Fe1 N3 2.183(2) . ? Fe1 N1 2.218(2) . ? Fe1 N1 2.218(2) 2_656 ? B1 N4 1.563(4) . ? B1 N5 1.565(4) . ? B1 H1B 1.16(3) . ? B1 H2B 1.13(3) . ? N1 C1 1.348(4) . ? N1 C5 1.354(4) . ? N2 C6 1.343(4) . ? N2 N4 1.371(3) . ? N3 C9 1.348(4) . ? N3 N5 1.369(3) . ? N4 C8 1.346(4) . ? N5 C11 1.348(4) . ? C1 C2 1.383(4) . ? C1 H1 0.96(3) . ? C2 C3 1.385(4) . ? C2 H2 0.99(3) . ? C3 C4 1.387(5) . ? C3 H3 0.94(3) . ? C4 C5 1.393(4) . ? C4 H4 0.92(3) . ? C5 C5 1.496(6) 2_656 ? C6 C7 1.384(4) . ? C6 H6 0.94(3) . ? C7 C8 1.377(4) . ? C7 H7 0.95(3) . ? C8 H8 0.93(3) . ? C9 C10 1.394(4) . ? C9 H9 0.93(3) . ? C10 C11 1.384(4) . ? C10 H10 1.04(4) . ? C11 H11 0.98(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 N2 Fe1 N2 93.10(13) 2_656 . ? N2 Fe1 N3 88.91(9) 2_656 2_656 ? N2 Fe1 N3 88.48(9) . 2_656 ? N2 Fe1 N3 88.48(9) 2_656 . ? N2 Fe1 N3 88.91(9) . . ? N3 Fe1 N3 176.21(13) 2_656 . ? N2 Fe1 N1 169.90(9) 2_656 . ? N2 Fe1 N1 96.80(9) . . ? N3 Fe1 N1 89.36(9) 2_656 . ? N3 Fe1 N1 93.68(9) . . ? N2 Fe1 N1 96.80(9) 2_656 2_656 ? N2 Fe1 N1 169.90(9) . 2_656 ? N3 Fe1 N1 93.68(9) 2_656 2_656 ? N3 Fe1 N1 89.36(9) . 2_656 ? N1 Fe1 N1 73.38(13) . 2_656 ? N4 B1 N5 109.5(2) . . ? N4 B1 H1B 108.8(15) . . ? N5 B1 H1B 108.7(15) . . ? N4 B1 H2B 109.7(14) . . ? N5 B1 H2B 106.8(16) . . ? H1B B1 H2B 113(2) . . ? C1 N1 C5 118.2(3) . . ? C1 N1 Fe1 123.7(2) . . ? C5 N1 Fe1 118.1(2) . . ? C6 N2 N4 105.4(2) . . ? C6 N2 Fe1 127.1(2) . . ? N4 N2 Fe1 125.78(18) . . ? C9 N3 N5 105.6(2) . . ? C9 N3 Fe1 129.5(2) . . ? N5 N3 Fe1 122.91(17) . . ? C8 N4 N2 109.7(2) . . ? C8 N4 B1 128.2(3) . . ? N2 N4 B1 122.0(2) . . ? C11 N5 N3 109.6(2) . . ? C11 N5 B1 126.0(2) . . ? N3 N5 B1 123.4(2) . . ? N1 C1 C2 122.6(3) . . ? N1 C1 H1 115.0(16) . . ? C2 C1 H1 122.4(16) . . ? C1 C2 C3 119.1(3) . . ? C1 C2 H2 120.9(18) . . ? C3 C2 H2 120.0(18) . . ? C2 C3 C4 119.0(3) . . ? C2 C3 H3 121.0(18) . . ? C4 C3 H3 120.0(18) . . ? C3 C4 C5 119.0(3) . . ? C3 C4 H4 118(2) . . ? C5 C4 H4 123(2) . . ? N1 C5 C4 122.0(3) . . ? N1 C5 C5 115.23(17) . 2_656 ? C4 C5 C5 122.72(19) . 2_656 ? N2 C6 C7 111.6(3) . . ? N2 C6 H6 118.1(17) . . ? C7 C6 H6 130.3(17) . . ? C8 C7 C6 104.3(3) . . ? C8 C7 H7 127.8(18) . . ? C6 C7 H7 127.9(18) . . ? N4 C8 C7 109.0(3) . . ? N4 C8 H8 117.2(19) . . ? C7 C8 H8 133.8(19) . . ? N3 C9 C10 111.5(3) . . ? N3 C9 H9 118.6(19) . . ? C10 C9 H9 129.9(18) . . ? C11 C10 C9 103.8(3) . . ? C11 C10 H10 125.8(17) . . ? C9 C10 H10 130.3(17) . . ? N5 C11 C10 109.4(3) . . ? N5 C11 H11 122.6(18) . . ? C10 C11 H11 128.0(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Fe1 N1 C1 -168.2(5) 2_656 . . . ? N2 Fe1 N1 C1 0.4(2) . . . . ? N3 Fe1 N1 C1 -88.0(2) 2_656 . . . ? N3 Fe1 N1 C1 89.7(2) . . . . ? N1 Fe1 N1 C1 178.0(3) 2_656 . . . ? N2 Fe1 N1 C5 14.4(7) 2_656 . . . ? N2 Fe1 N1 C5 -177.1(2) . . . . ? N3 Fe1 N1 C5 94.6(2) 2_656 . . . ? N3 Fe1 N1 C5 -87.7(2) . . . . ? N1 Fe1 N1 C5 0.52(15) 2_656 . . . ? N2 Fe1 N2 C6 59.6(2) 2_656 . . . ? N3 Fe1 N2 C6 -29.2(3) 2_656 . . . ? N3 Fe1 N2 C6 148.1(3) . . . . ? N1 Fe1 N2 C6 -118.4(3) . . . . ? N1 Fe1 N2 C6 -131.7(5) 2_656 . . . ? N2 Fe1 N2 N4 -103.1(2) 2_656 . . . ? N3 Fe1 N2 N4 168.0(2) 2_656 . . . ? N3 Fe1 N2 N4 -14.7(2) . . . . ? N1 Fe1 N2 N4 78.9(2) . . . . ? N1 Fe1 N2 N4 65.5(6) 2_656 . . . ? N2 Fe1 N3 C9 -58.0(3) 2_656 . . . ? N2 Fe1 N3 C9 -151.1(3) . . . . ? N3 Fe1 N3 C9 -104.6(2) 2_656 . . . ? N1 Fe1 N3 C9 112.1(3) . . . . ? N1 Fe1 N3 C9 38.8(3) 2_656 . . . ? N2 Fe1 N3 N5 103.9(2) 2_656 . . . ? N2 Fe1 N3 N5 10.8(2) . . . . ? N3 Fe1 N3 N5 57.35(19) 2_656 . . . ? N1 Fe1 N3 N5 -86.0(2) . . . . ? N1 Fe1 N3 N5 -159.3(2) 2_656 . . . ? C6 N2 N4 C8 1.0(3) . . . . ? Fe1 N2 N4 C8 166.8(2) . . . . ? C6 N2 N4 B1 177.9(3) . . . . ? Fe1 N2 N4 B1 -16.3(3) . . . . ? N5 B1 N4 C8 -129.1(3) . . . . ? N5 B1 N4 N2 54.6(3) . . . . ? C9 N3 N5 C11 -0.5(3) . . . . ? Fe1 N3 N5 C11 -166.07(18) . . . . ? C9 N3 N5 B1 -169.9(3) . . . . ? Fe1 N3 N5 B1 24.4(3) . . . . ? N4 B1 N5 C11 132.3(3) . . . . ? N4 B1 N5 N3 -60.0(3) . . . . ? C5 N1 C1 C2 1.1(4) . . . . ? Fe1 N1 C1 C2 -176.3(2) . . . . ? N1 C1 C2 C3 -1.1(5) . . . . ? C1 C2 C3 C4 0.3(5) . . . . ? C2 C3 C4 C5 0.5(5) . . . . ? C1 N1 C5 C4 -0.3(4) . . . . ? Fe1 N1 C5 C4 177.3(2) . . . . ? C1 N1 C5 C5 -179.0(3) . . . 2_656 ? Fe1 N1 C5 C5 -1.4(4) . . . 2_656 ? C3 C4 C5 N1 -0.5(5) . . . . ? C3 C4 C5 C5 178.1(3) . . . 2_656 ? N4 N2 C6 C7 -1.1(3) . . . . ? Fe1 N2 C6 C7 -166.6(2) . . . . ? N2 C6 C7 C8 0.8(4) . . . . ? N2 N4 C8 C7 -0.5(3) . . . . ? B1 N4 C8 C7 -177.2(3) . . . . ? C6 C7 C8 N4 -0.1(4) . . . . ? N5 N3 C9 C10 0.8(3) . . . . ? Fe1 N3 C9 C10 165.1(2) . . . . ? N3 C9 C10 C11 -0.8(3) . . . . ? N3 N5 C11 C10 0.0(3) . . . . ? B1 N5 C11 C10 169.1(3) . . . . ? C9 C10 C11 N5 0.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.899 _refine_diff_density_max 0.734 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.083 #====================================================================== #====================================================================== data_phen1 _database_code_depnum_ccdc_archive 'CCDC 233285' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,2'-Phenanthroline-bis[di(hydro)bis(1-pyrazolyl)borate iron(II) ; _chemical_name_common ;2,2'-Phenanthroline-bis(di(hydro)bis(1-pyrazolyl)borate iron(ii) ; _chemical_melting_point 'not measured' _chemical_formula_moiety 'C24 H24 B2 Fe N10' _chemical_formula_sum 'C24 H24 B2 Fe N10' _chemical_formula_weight 530.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.3607(16) _cell_length_b 16.0397(14) _cell_length_c 10.5614(9) _cell_angle_alpha 90.00 _cell_angle_beta 121.617(3) _cell_angle_gamma 90.00 _cell_volume 2504.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 1799 _cell_measurement_theta_min 4.633 _cell_measurement_theta_max 47.774 _exptl_crystal_description plate _exptl_crystal_colour clear_intense_red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.637 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.8417 _exptl_absorpt_correction_T_max 0.9874 _exptl_absorpt_process_details 'XPREP (SHELXTL,1997)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 3 sets of \w scans each set at different \f and/or 2\q angles and each scan (20s exposure) covering 0.3\% in \w. Crystal to detector distance 5.81. ; _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 SMART CCD 6K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 10201 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0694 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 29.12 _reflns_number_total 3370 _reflns_number_gt 2264 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SMART-NT V6.1 (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0326P)^2^+0.4396P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3370 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1037 _refine_ls_wR_factor_gt 0.0919 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 0.5000 0.26025(2) 0.7500 0.03305(14) Uani 1 2 d S . . B1 B 0.5268(2) 0.1831(2) 1.0824(3) 0.0484(7) Uani 1 1 d . . . H1B H 0.5622(18) 0.2401(14) 1.131(3) 0.053(7) Uiso 1 1 d . . . H2B H 0.5186(18) 0.1410(15) 1.153(3) 0.062(7) Uiso 1 1 d . . . N1 N 0.57013(13) 0.36930(11) 0.8912(2) 0.0392(4) Uani 1 1 d . . . N2 N 0.58512(12) 0.16583(10) 0.90649(18) 0.0357(4) Uani 1 1 d . . . N3 N 0.41171(12) 0.25710(11) 0.83917(18) 0.0381(4) Uani 1 1 d . . . N4 N 0.57083(13) 0.13321(11) 1.01186(19) 0.0421(5) Uani 1 1 d . . . N5 N 0.42989(13) 0.21126(11) 0.96096(18) 0.0401(4) Uani 1 1 d . . . C1 C 0.63588(17) 0.36895(16) 1.0332(2) 0.0489(6) Uani 1 1 d . . . H1 H 0.6608 0.3168 1.0791 0.059 Uiso 1 1 calc R . . C2 C 0.67040(19) 0.44088(17) 1.1188(3) 0.0576(7) Uani 1 1 d . . . H2 H 0.7162 0.4374 1.2211 0.069 Uiso 1 1 calc R . . C3 C 0.6374(2) 0.51623(18) 1.0532(3) 0.0642(8) Uani 1 1 d . . . H3 H 0.6604 0.5660 1.1097 0.077 Uiso 1 1 calc R . . C4 C 0.56928(19) 0.52033(14) 0.9021(3) 0.0546(7) Uani 1 1 d . . . C5 C 0.53589(16) 0.44465(13) 0.8259(2) 0.0400(5) Uani 1 1 d . . . C6 C 0.63130(17) 0.10825(14) 0.8828(2) 0.0451(6) Uani 1 1 d . . . H6 H 0.6503 0.1141 0.8137 0.054 Uiso 1 1 calc R . . C7 C 0.6482(2) 0.03910(16) 0.9712(3) 0.0605(7) Uani 1 1 d . . . H7 H 0.6801 -0.0101 0.9759 0.073 Uiso 1 1 calc R . . C8 C 0.6083(2) 0.05771(16) 1.0504(3) 0.0577(7) Uani 1 1 d . . . H8 H 0.6075 0.0223 1.1218 0.069 Uiso 1 1 calc R . . C9 C 0.32470(16) 0.27848(14) 0.7723(2) 0.0442(5) Uani 1 1 d . . . H9 H 0.2931 0.3099 0.6830 0.053 Uiso 1 1 calc R . . C10 C 0.28639(17) 0.24881(15) 0.8503(3) 0.0502(6) Uani 1 1 d . . . H10 H 0.2261 0.2561 0.8274 0.060 Uiso 1 1 calc R . . C11 C 0.35525(17) 0.20651(16) 0.9678(3) 0.0487(6) Uani 1 1 d . . . H11 H 0.3507 0.1782 1.0426 0.058 Uiso 1 1 calc R . . C12 C 0.5319(2) 0.59651(16) 0.8220(4) 0.0776(10) Uani 1 1 d . . . H12 H 0.5532 0.6482 0.8727 0.093 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 Fe1 0.0338(3) 0.0314(2) 0.0296(2) 0.000 0.01354(18) 0.000 B1 0.0431(17) 0.0691(19) 0.0323(13) 0.0025(13) 0.0193(12) 0.0061(14) N1 0.0381(12) 0.0384(10) 0.0385(10) -0.0036(8) 0.0182(9) -0.0014(8) N2 0.0393(11) 0.0374(9) 0.0315(9) 0.0032(7) 0.0193(8) 0.0025(8) N3 0.0361(11) 0.0426(10) 0.0330(9) -0.0070(7) 0.0162(8) 0.0015(8) N4 0.0419(12) 0.0506(11) 0.0348(10) 0.0107(8) 0.0208(9) 0.0053(9) N5 0.0395(11) 0.0493(11) 0.0330(9) -0.0052(8) 0.0200(8) -0.0010(8) C1 0.0456(16) 0.0531(14) 0.0398(13) -0.0071(10) 0.0165(11) -0.0063(11) C2 0.0465(17) 0.0705(18) 0.0483(14) -0.0230(13) 0.0196(12) -0.0119(13) C3 0.0533(18) 0.0574(16) 0.083(2) -0.0370(15) 0.0368(16) -0.0152(13) C4 0.0496(17) 0.0391(12) 0.0799(19) -0.0158(12) 0.0373(15) -0.0058(11) C5 0.0361(14) 0.0367(11) 0.0531(13) -0.0051(9) 0.0275(11) -0.0023(9) C6 0.0511(16) 0.0439(12) 0.0442(13) 0.0056(10) 0.0276(12) 0.0091(11) C7 0.072(2) 0.0456(14) 0.0725(18) 0.0182(13) 0.0440(17) 0.0209(13) C8 0.0632(19) 0.0527(15) 0.0623(16) 0.0288(12) 0.0365(15) 0.0173(13) C9 0.0379(14) 0.0472(13) 0.0384(12) -0.0102(10) 0.0137(10) 0.0043(10) C10 0.0360(14) 0.0673(16) 0.0495(13) -0.0188(12) 0.0239(11) -0.0032(12) C11 0.0439(15) 0.0646(15) 0.0442(13) -0.0136(11) 0.0276(12) -0.0074(12) C12 0.071(3) 0.0355(13) 0.121(3) -0.0129(14) 0.047(2) -0.0065(13) _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 N2 2.1560(17) 2_656 ? Fe1 N2 2.1560(17) . ? Fe1 N3 2.1799(17) 2_656 ? Fe1 N3 2.1799(17) . ? Fe1 N1 2.2049(18) . ? Fe1 N1 2.2049(17) 2_656 ? B1 N4 1.541(3) . ? B1 N5 1.555(3) . ? B1 H1B 1.07(2) . ? B1 H2B 1.07(2) . ? N1 C1 1.326(3) . ? N1 C5 1.364(3) . ? N2 C6 1.330(3) . ? N2 N4 1.365(2) . ? N3 C9 1.334(3) . ? N3 N5 1.367(2) . ? N4 C8 1.333(3) . ? N5 C11 1.337(3) . ? C1 C2 1.392(3) . ? C1 H1 0.9500 . ? C2 C3 1.361(4) . ? C2 H2 0.9500 . ? C3 C4 1.404(4) . ? C3 H3 0.9500 . ? C4 C5 1.403(3) . ? C4 C12 1.433(4) . ? C5 C5 1.424(5) 2_656 ? C6 C7 1.378(3) . ? C6 H6 0.9500 . ? C7 C8 1.370(4) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.386(3) . ? C9 H9 0.9500 . ? C10 C11 1.369(4) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C12 1.331(6) 2_656 ? C12 H12 0.9500 . ? 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 N2 Fe1 N2 90.75(9) 2_656 . ? N2 Fe1 N3 90.41(6) 2_656 2_656 ? N2 Fe1 N3 87.73(6) . 2_656 ? N2 Fe1 N3 87.73(6) 2_656 . ? N2 Fe1 N3 90.41(7) . . ? N3 Fe1 N3 177.35(9) 2_656 . ? N2 Fe1 N1 171.58(7) 2_656 . ? N2 Fe1 N1 97.20(7) . . ? N3 Fe1 N1 92.66(7) 2_656 . ? N3 Fe1 N1 89.44(7) . . ? N2 Fe1 N1 97.20(7) 2_656 2_656 ? N2 Fe1 N1 171.58(7) . 2_656 ? N3 Fe1 N1 89.44(7) 2_656 2_656 ? N3 Fe1 N1 92.66(7) . 2_656 ? N1 Fe1 N1 75.01(10) . 2_656 ? N4 B1 N5 110.41(18) . . ? N4 B1 H1B 112.0(13) . . ? N5 B1 H1B 104.4(14) . . ? N4 B1 H2B 106.8(13) . . ? N5 B1 H2B 106.0(15) . . ? H1B B1 H2B 117.0(18) . . ? C1 N1 C5 117.66(19) . . ? C1 N1 Fe1 127.19(15) . . ? C5 N1 Fe1 114.92(15) . . ? C6 N2 N4 105.79(16) . . ? C6 N2 Fe1 125.62(13) . . ? N4 N2 Fe1 123.35(13) . . ? C9 N3 N5 105.96(18) . . ? C9 N3 Fe1 128.54(15) . . ? N5 N3 Fe1 123.44(13) . . ? C8 N4 N2 109.20(19) . . ? C8 N4 B1 127.6(2) . . ? N2 N4 B1 122.89(18) . . ? C11 N5 N3 109.21(19) . . ? C11 N5 B1 126.8(2) . . ? N3 N5 B1 123.26(19) . . ? N1 C1 C2 123.6(2) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 118.8(3) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 119.9(2) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 117.4(2) . . ? C5 C4 C12 118.4(3) . . ? C3 C4 C12 124.2(2) . . ? N1 C5 C4 122.5(2) . . ? N1 C5 C5 117.47(12) . 2_656 ? C4 C5 C5 120.03(16) . 2_656 ? N2 C6 C7 111.5(2) . . ? N2 C6 H6 124.2 . . ? C7 C6 H6 124.2 . . ? C8 C7 C6 104.0(2) . . ? C8 C7 H7 128.0 . . ? C6 C7 H7 128.0 . . ? N4 C8 C7 109.5(2) . . ? N4 C8 H8 125.3 . . ? C7 C8 H8 125.3 . . ? N3 C9 C10 111.1(2) . . ? N3 C9 H9 124.4 . . ? C10 C9 H9 124.4 . . ? C11 C10 C9 104.2(2) . . ? C11 C10 H10 127.9 . . ? C9 C10 H10 127.9 . . ? N5 C11 C10 109.5(2) . . ? N5 C11 H11 125.3 . . ? C10 C11 H11 125.3 . . ? C12 C12 C4 121.49(16) 2_656 . ? C12 C12 H12 119.3 2_656 . ? C4 C12 H12 119.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Fe1 N1 C1 153.1(4) 2_656 . . . ? N2 Fe1 N1 C1 -7.5(2) . . . . ? N3 Fe1 N1 C1 -95.6(2) 2_656 . . . ? N3 Fe1 N1 C1 82.8(2) . . . . ? N1 Fe1 N1 C1 175.7(2) 2_656 . . . ? N2 Fe1 N1 C5 -21.2(5) 2_656 . . . ? N2 Fe1 N1 C5 178.13(15) . . . . ? N3 Fe1 N1 C5 90.09(16) 2_656 . . . ? N3 Fe1 N1 C5 -91.53(16) . . . . ? N1 Fe1 N1 C5 1.38(11) 2_656 . . . ? N2 Fe1 N2 C6 60.44(17) 2_656 . . . ? N3 Fe1 N2 C6 -29.94(19) 2_656 . . . ? N3 Fe1 N2 C6 148.17(19) . . . . ? N1 Fe1 N2 C6 -122.34(19) . . . . ? N1 Fe1 N2 C6 -100.4(4) 2_656 . . . ? N2 Fe1 N2 N4 -90.28(16) 2_656 . . . ? N3 Fe1 N2 N4 179.34(16) 2_656 . . . ? N3 Fe1 N2 N4 -2.55(16) . . . . ? N1 Fe1 N2 N4 86.94(16) . . . . ? N1 Fe1 N2 N4 108.9(4) 2_656 . . . ? N2 Fe1 N3 C9 -64.93(18) 2_656 . . . ? N2 Fe1 N3 C9 -155.66(18) . . . . ? N3 Fe1 N3 C9 -110.32(18) 2_656 . . . ? N1 Fe1 N3 C9 107.15(18) . . . . ? N1 Fe1 N3 C9 32.18(18) 2_656 . . . ? N2 Fe1 N3 N5 96.38(15) 2_656 . . . ? N2 Fe1 N3 N5 5.65(15) . . . . ? N3 Fe1 N3 N5 50.99(15) 2_656 . . . ? N1 Fe1 N3 N5 -91.54(15) . . . . ? N1 Fe1 N3 N5 -166.51(15) 2_656 . . . ? C6 N2 N4 C8 0.3(3) . . . . ? Fe1 N2 N4 C8 155.88(18) . . . . ? C6 N2 N4 B1 174.3(2) . . . . ? Fe1 N2 N4 B1 -30.1(3) . . . . ? N5 B1 N4 C8 -127.0(3) . . . . ? N5 B1 N4 N2 60.1(3) . . . . ? C9 N3 N5 C11 -0.9(2) . . . . ? Fe1 N3 N5 C11 -165.81(14) . . . . ? C9 N3 N5 B1 -171.9(2) . . . . ? Fe1 N3 N5 B1 23.2(3) . . . . ? N4 B1 N5 C11 134.7(2) . . . . ? N4 B1 N5 N3 -56.0(3) . . . . ? C5 N1 C1 C2 1.0(4) . . . . ? Fe1 N1 C1 C2 -173.19(18) . . . . ? N1 C1 C2 C3 -2.1(4) . . . . ? C1 C2 C3 C4 0.4(4) . . . . ? C2 C3 C4 C5 2.1(4) . . . . ? C2 C3 C4 C12 -178.2(3) . . . . ? C1 N1 C5 C4 1.8(3) . . . . ? Fe1 N1 C5 C4 176.66(18) . . . . ? C1 N1 C5 C5 -178.8(2) . . . 2_656 ? Fe1 N1 C5 C5 -3.9(3) . . . 2_656 ? C3 C4 C5 N1 -3.3(4) . . . . ? C12 C4 C5 N1 177.0(2) . . . . ? C3 C4 C5 C5 177.3(3) . . . 2_656 ? C12 C4 C5 C5 -2.4(4) . . . 2_656 ? N4 N2 C6 C7 -0.5(3) . . . . ? Fe1 N2 C6 C7 -155.39(19) . . . . ? N2 C6 C7 C8 0.5(3) . . . . ? N2 N4 C8 C7 0.0(3) . . . . ? B1 N4 C8 C7 -173.6(3) . . . . ? C6 C7 C8 N4 -0.3(3) . . . . ? N5 N3 C9 C10 1.3(2) . . . . ? Fe1 N3 C9 C10 165.11(15) . . . . ? N3 C9 C10 C11 -1.1(3) . . . . ? N3 N5 C11 C10 0.3(3) . . . . ? B1 N5 C11 C10 170.8(2) . . . . ? C9 C10 C11 N5 0.5(3) . . . . ? C5 C4 C12 C12 -1.1(6) . . . 2_656 ? C3 C4 C12 C12 179.2(4) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 29.12 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.268 _refine_diff_density_min -0.262 _refine_diff_density_rms 0.052 #====================================================================== data_phen2 _database_code_depnum_ccdc_archive 'CCDC 233286' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,2'-Phenanthroline-bis[di(hydro)bis(1-pyrazolyl)borate iron(II) ; _chemical_name_common ;2,2'-Phenanthroline-bis(di(hydro)bis(1-pyrazolyl)borate iron(ii) ; _chemical_melting_point 'not measured' _chemical_formula_moiety 'C24 H24 B2 Fe N10' _chemical_formula_sum 'C24 H24 B2 Fe N10' _chemical_formula_weight 530.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6730(13) _cell_length_b 11.0458(13) _cell_length_c 10.5651(12) _cell_angle_alpha 69.520(3) _cell_angle_beta 109.777(3) _cell_angle_gamma 93.368(3) _cell_volume 1198.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2070 _cell_measurement_theta_min 4.681 _cell_measurement_theta_max 51.995 _exptl_crystal_description plate _exptl_crystal_colour clear_intense_red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 0.666 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.8354 _exptl_absorpt_correction_T_max 0.9868 _exptl_absorpt_process_details 'XPREP (SHELXTL,1997)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 3 sets of \w scans each set at different \f and/or 2\q angles and each scan (20s exposure) covering 0.3\% in \w. Crystal to detector distance 5.81. ; _diffrn_ambient_temperature 100(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 CCD 6K area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 11974 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.1015 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 29.13 _reflns_number_total 6409 _reflns_number_gt 4054 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SMART-NT V6.1 (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0563P)^2^+0.6568P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 6409 _refine_ls_number_parameters 430 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1135 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1473 _refine_ls_wR_factor_gt 0.1296 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 -1.23839(4) 0.76340(5) -1.25659(5) 0.01714(14) Uani 1 1 d . . . B1 B -1.3045(4) 0.6914(4) -0.9466(5) 0.0275(9) Uani 1 1 d . . . H11B H -1.215(4) 0.699(4) -0.877(5) 0.040(12) Uiso 1 1 d . . . H12B H -1.362(4) 0.671(4) -0.881(5) 0.049(13) Uiso 1 1 d . . . B2 B -1.3167(4) 0.6763(4) -1.5553(4) 0.0232(8) Uani 1 1 d . . . H21B H -1.300(3) 0.781(4) -1.625(4) 0.024(10) Uiso 1 1 d . . . H22B H -1.346(3) 0.610(4) -1.623(4) 0.027(10) Uiso 1 1 d . . . N11 N -1.0830(2) 0.8070(3) -1.1358(3) 0.0191(6) Uani 1 1 d . . . N12 N -1.2559(2) 0.5941(3) -1.1092(3) 0.0188(6) Uani 1 1 d . . . N13 N -1.3283(2) 0.8674(3) -1.1931(3) 0.0193(6) Uani 1 1 d . . . N14 N -1.3037(3) 0.5834(3) -1.0052(3) 0.0219(6) Uani 1 1 d . . . N15 N -1.3589(3) 0.8208(3) -1.0720(3) 0.0226(6) Uani 1 1 d . . . N21 N -1.2163(2) 0.9238(3) -1.4032(3) 0.0192(6) Uani 1 1 d . . . N22 N -1.3995(2) 0.7322(3) -1.3844(3) 0.0182(6) Uani 1 1 d . . . N23 N -1.1456(3) 0.6605(3) -1.3175(3) 0.0209(6) Uani 1 1 d . . . N24 N -1.4160(3) 0.6846(3) -1.4920(3) 0.0207(6) Uani 1 1 d . . . N25 N -1.1948(3) 0.6184(3) -1.4296(3) 0.0208(6) Uani 1 1 d . . . C11 C -1.0198(3) 0.7490(4) -0.9978(4) 0.0249(7) Uani 1 1 d D . . H11 H -1.043(3) 0.669(4) -0.945(4) 0.019(9) Uiso 1 1 d . . . C12 C -0.9135(3) 0.7983(4) -0.9253(4) 0.0296(8) Uani 1 1 d . . . H12 H -0.875(3) 0.754(3) -0.825(5) 0.037(12) Uiso 1 1 d D . . C13 C -0.8694(3) 0.9083(4) -1.0000(4) 0.0294(8) Uani 1 1 d D . . H13 H -0.805(4) 0.939(4) -0.959(5) 0.041(13) Uiso 1 1 d . . . C14 C -0.9320(3) 0.9701(3) -1.1463(4) 0.0253(8) Uani 1 1 d . . . C15 C -1.0394(3) 0.9178(3) -1.2090(4) 0.0215(7) Uani 1 1 d . . . C16 C -1.2585(3) 0.4768(3) -1.1205(4) 0.0224(7) Uani 1 1 d D . . H16 H -1.232(3) 0.462(4) -1.191(4) 0.021(9) Uiso 1 1 d . . . C17 C -1.3054(4) 0.3895(4) -1.0221(4) 0.0294(8) Uani 1 1 d . . . H17 H -1.314(4) 0.297(4) -1.007(3) 0.044(13) Uiso 1 1 d D . . C18 C -1.3348(4) 0.4607(4) -0.9534(4) 0.0283(8) Uani 1 1 d D . . H18 H -1.367(3) 0.439(4) -0.876(4) 0.020(9) Uiso 1 1 d . . . C19 C -1.3810(3) 0.9879(3) -1.2650(4) 0.0224(7) Uani 1 1 d . . . H19 H -1.368(4) 1.040(4) -1.350(5) 0.044(13) Uiso 1 1 d . . . C21 C -1.2865(3) 0.9809(3) -1.5400(4) 0.0222(7) Uani 1 1 d . . . H21 H -1.365(4) 0.941(4) -1.572(4) 0.029(11) Uiso 1 1 d . . . C22 C -1.2556(3) 1.0922(3) -1.6343(4) 0.0245(7) Uani 1 1 d . . . H22 H -1.308(3) 1.134(4) -1.738(4) 0.025(10) Uiso 1 1 d . . . C23 C -1.1491(4) 1.1480(3) -1.5857(4) 0.0278(8) Uani 1 1 d . . . H23 H -1.121(3) 1.225(4) -1.639(4) 0.022(10) Uiso 1 1 d . . . C24 C -1.0735(3) 1.0929(3) -1.4410(4) 0.0249(8) Uani 1 1 d . . . C25 C -1.1112(3) 0.9795(3) -1.3556(4) 0.0213(7) Uani 1 1 d . . . C26 C -1.5081(3) 0.7322(3) -1.3669(4) 0.0221(7) Uani 1 1 d . . . H26 H -1.516(3) 0.761(3) -1.300(4) 0.017(9) Uiso 1 1 d . . . C27 C -1.5953(3) 0.6868(3) -1.4641(4) 0.0268(8) Uani 1 1 d . . . H27 H -1.685(4) 0.676(4) -1.475(5) 0.048(13) Uiso 1 1 d . . . C28 C -1.5342(3) 0.6567(3) -1.5400(4) 0.0251(8) Uani 1 1 d . . . H28 H -1.563(3) 0.615(4) -1.616(4) 0.022(9) Uiso 1 1 d . . . C29 C -1.0331(3) 0.6019(3) -1.2456(4) 0.0226(7) Uani 1 1 d D . . H29 H -0.987(4) 0.613(4) -1.164(4) 0.026(10) Uiso 1 1 d . . . C110 C -1.4444(3) 1.0209(4) -1.1900(4) 0.0257(8) Uani 1 1 d . . . H110 H -1.491(4) 1.094(4) -1.219(5) 0.035(12) Uiso 1 1 d . . . C111 C -1.4292(3) 0.9120(4) -1.0701(4) 0.0259(8) Uani 1 1 d . . . H111 H -1.458(4) 0.888(4) -0.988(5) 0.036(12) Uiso 1 1 d . . . C112 C -0.8955(3) 1.0848(4) -1.2371(5) 0.0299(8) Uani 1 1 d . . . H112 H -0.827(4) 1.118(4) -1.198(5) 0.034(11) Uiso 1 1 d . . . C210 C -1.0091(3) 0.5221(4) -1.3113(4) 0.0264(8) Uani 1 1 d . . . H210 H -0.936(3) 0.476(3) -1.285(3) 0.013(8) Uiso 1 1 d D . . C211 C -1.1139(3) 0.5340(3) -1.4266(4) 0.0261(8) Uani 1 1 d D . . H211 H -1.130(4) 0.501(4) -1.497(5) 0.036(12) Uiso 1 1 d . . . C212 C -0.9623(3) 1.1425(4) -1.3778(5) 0.0313(9) Uani 1 1 d . . . H212 H -0.936(3) 1.222(4) -1.436(4) 0.019(9) Uiso 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 0.0153(2) 0.0164(2) 0.0181(3) -0.00369(19) 0.00617(18) -0.00095(17) B1 0.039(2) 0.023(2) 0.022(2) -0.0072(17) 0.0127(19) 0.0014(18) B2 0.0250(19) 0.027(2) 0.0167(19) -0.0065(16) 0.0073(16) -0.0021(16) N11 0.0184(13) 0.0196(14) 0.0204(15) -0.0064(12) 0.0079(12) 0.0014(11) N12 0.0198(14) 0.0179(13) 0.0181(15) -0.0047(12) 0.0070(12) 0.0006(11) N13 0.0185(13) 0.0220(14) 0.0169(15) -0.0079(12) 0.0046(11) -0.0017(11) N14 0.0219(14) 0.0213(14) 0.0213(15) -0.0016(12) 0.0117(12) 0.0010(12) N15 0.0243(15) 0.0239(15) 0.0213(16) -0.0082(13) 0.0093(12) -0.0004(12) N21 0.0157(13) 0.0192(13) 0.0234(16) -0.0068(12) 0.0080(12) 0.0005(11) N22 0.0191(14) 0.0155(13) 0.0190(15) -0.0044(11) 0.0071(12) -0.0022(11) N23 0.0207(14) 0.0201(14) 0.0239(16) -0.0058(12) 0.0119(12) -0.0019(12) N24 0.0201(14) 0.0189(13) 0.0207(15) -0.0060(12) 0.0052(12) -0.0031(11) N25 0.0217(14) 0.0198(14) 0.0201(15) -0.0054(12) 0.0077(12) -0.0014(11) C11 0.0243(18) 0.0236(17) 0.0235(19) -0.0051(15) 0.0062(15) 0.0057(14) C12 0.0237(18) 0.036(2) 0.026(2) -0.0132(17) 0.0005(16) 0.0096(16) C13 0.0220(18) 0.033(2) 0.036(2) -0.0180(18) 0.0061(16) 0.0001(16) C14 0.0184(16) 0.0279(18) 0.035(2) -0.0157(17) 0.0103(15) -0.0009(14) C15 0.0173(16) 0.0182(15) 0.030(2) -0.0100(15) 0.0077(14) -0.0007(13) C16 0.0238(17) 0.0190(16) 0.0243(19) -0.0069(15) 0.0085(15) -0.0014(13) C17 0.036(2) 0.0204(17) 0.030(2) -0.0048(16) 0.0145(17) -0.0056(16) C18 0.033(2) 0.0251(18) 0.029(2) -0.0042(16) 0.0195(17) -0.0054(15) C19 0.0204(16) 0.0214(16) 0.0229(19) -0.0087(15) 0.0029(14) 0.0010(14) C21 0.0212(17) 0.0201(16) 0.0236(18) -0.0051(14) 0.0077(14) 0.0026(13) C22 0.0280(18) 0.0217(17) 0.0211(19) 0.0000(15) 0.0119(15) 0.0044(14) C23 0.032(2) 0.0201(17) 0.034(2) -0.0024(16) 0.0226(17) -0.0007(15) C24 0.0232(17) 0.0202(17) 0.035(2) -0.0078(15) 0.0155(16) -0.0001(14) C25 0.0179(15) 0.0203(16) 0.0273(19) -0.0083(15) 0.0093(14) 0.0005(13) C26 0.0192(16) 0.0196(16) 0.0267(19) -0.0060(15) 0.0089(14) -0.0003(13) C27 0.0194(17) 0.0241(18) 0.033(2) -0.0073(16) 0.0067(15) -0.0040(14) C28 0.0204(17) 0.0211(17) 0.028(2) -0.0091(15) 0.0015(15) -0.0057(14) C29 0.0229(17) 0.0227(17) 0.0200(18) -0.0012(15) 0.0106(15) 0.0030(14) C110 0.0244(18) 0.0245(18) 0.027(2) -0.0096(16) 0.0051(15) 0.0075(15) C111 0.0234(18) 0.0281(19) 0.0241(19) -0.0052(16) 0.0081(15) 0.0083(15) C112 0.0213(18) 0.0279(19) 0.046(2) -0.0181(18) 0.0135(17) -0.0087(15) C210 0.0273(19) 0.0269(18) 0.0234(19) 0.0001(15) 0.0143(15) 0.0083(15) C211 0.034(2) 0.0208(17) 0.025(2) -0.0039(16) 0.0153(17) 0.0038(15) C212 0.0280(19) 0.0234(18) 0.047(3) -0.0115(18) 0.0205(19) -0.0064(15) _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 N21 1.976(3) . ? Fe1 N11 1.977(3) . ? Fe1 N23 2.002(3) . ? Fe1 N22 2.003(3) . ? Fe1 N13 2.007(3) . ? Fe1 N12 2.024(3) . ? B1 N14 1.526(5) . ? B1 N15 1.554(5) . ? B1 H11B 1.08(4) . ? B1 H12B 1.08(5) . ? B2 N24 1.543(5) . ? B2 N25 1.559(5) . ? B2 H21B 1.18(4) . ? B2 H22B 1.16(4) . ? N11 C11 1.325(5) . ? N11 C15 1.374(4) . ? N12 C16 1.340(4) . ? N12 N14 1.360(4) . ? N13 C19 1.342(4) . ? N13 N15 1.362(4) . ? N14 C18 1.351(4) . ? N15 C111 1.345(4) . ? N21 C21 1.334(4) . ? N21 C25 1.359(4) . ? N22 C26 1.341(4) . ? N22 N24 1.366(4) . ? N23 C29 1.342(4) . ? N23 N25 1.358(4) . ? N24 C28 1.357(4) . ? N25 C211 1.350(4) . ? C11 C12 1.412(5) . ? C11 H11 0.95(4) . ? C12 C13 1.376(6) . ? C12 H12 0.95(4) . ? C13 C14 1.395(6) . ? C13 H13 0.85(5) . ? C14 C15 1.402(5) . ? C14 C112 1.438(5) . ? C15 C25 1.419(5) . ? C16 C17 1.390(5) . ? C16 H16 0.96(4) . ? C17 C18 1.365(5) . ? C17 H17 0.98(5) . ? C18 H18 0.96(4) . ? C19 C110 1.393(5) . ? C19 H19 0.94(5) . ? C21 C22 1.403(5) . ? C21 H21 0.99(4) . ? C22 C23 1.374(5) . ? C22 H22 1.01(4) . ? C23 C24 1.409(6) . ? C23 H23 0.95(4) . ? C24 C25 1.410(5) . ? C24 C212 1.420(5) . ? C26 C27 1.391(5) . ? C26 H26 0.91(4) . ? C27 C28 1.365(5) . ? C27 H27 1.02(5) . ? C28 H28 1.01(4) . ? C29 C210 1.388(5) . ? C29 H29 0.89(4) . ? C110 C111 1.375(5) . ? C110 H110 0.90(4) . ? C111 H111 0.98(4) . ? C112 C212 1.354(6) . ? C112 H112 0.90(4) . ? C210 C211 1.377(6) . ? C210 H210 0.93(3) . ? C211 H211 0.90(5) . ? C212 H212 0.98(4) . ? 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 N21 Fe1 N11 82.38(12) . . ? N21 Fe1 N23 89.89(12) . . ? N11 Fe1 N23 90.03(11) . . ? N21 Fe1 N22 94.65(11) . . ? N11 Fe1 N22 176.04(12) . . ? N23 Fe1 N22 92.59(11) . . ? N21 Fe1 N13 89.97(11) . . ? N11 Fe1 N13 88.83(11) . . ? N23 Fe1 N13 178.86(12) . . ? N22 Fe1 N13 88.55(11) . . ? N21 Fe1 N12 177.14(12) . . ? N11 Fe1 N12 97.47(11) . . ? N23 Fe1 N12 87.26(11) . . ? N22 Fe1 N12 85.62(11) . . ? N13 Fe1 N12 92.88(11) . . ? N14 B1 N15 110.3(3) . . ? N14 B1 H11B 111(2) . . ? N15 B1 H11B 113(2) . . ? N14 B1 H12B 111(2) . . ? N15 B1 H12B 106(2) . . ? H11B B1 H12B 105(3) . . ? N24 B2 N25 108.9(3) . . ? N24 B2 H21B 109.9(18) . . ? N25 B2 H21B 108.0(19) . . ? N24 B2 H22B 109.5(19) . . ? N25 B2 H22B 109.3(19) . . ? H21B B2 H22B 111(3) . . ? C11 N11 C15 117.1(3) . . ? C11 N11 Fe1 130.0(2) . . ? C15 N11 Fe1 112.8(2) . . ? C16 N12 N14 106.2(3) . . ? C16 N12 Fe1 126.3(2) . . ? N14 N12 Fe1 124.8(2) . . ? C19 N13 N15 106.6(3) . . ? C19 N13 Fe1 128.2(2) . . ? N15 N13 Fe1 124.9(2) . . ? C18 N14 N12 109.4(3) . . ? C18 N14 B1 126.9(3) . . ? N12 N14 B1 123.2(3) . . ? C111 N15 N13 109.2(3) . . ? C111 N15 B1 125.7(3) . . ? N13 N15 B1 124.5(3) . . ? C21 N21 C25 117.0(3) . . ? C21 N21 Fe1 129.6(2) . . ? C25 N21 Fe1 113.4(2) . . ? C26 N22 N24 106.3(3) . . ? C26 N22 Fe1 127.2(2) . . ? N24 N22 Fe1 125.6(2) . . ? C29 N23 N25 106.6(3) . . ? C29 N23 Fe1 127.9(2) . . ? N25 N23 Fe1 124.6(2) . . ? C28 N24 N22 109.2(3) . . ? C28 N24 B2 126.5(3) . . ? N22 N24 B2 124.1(3) . . ? C211 N25 N23 109.6(3) . . ? C211 N25 B2 125.2(3) . . ? N23 N25 B2 124.5(3) . . ? N11 C11 C12 122.7(4) . . ? N11 C11 H11 120(2) . . ? C12 C11 H11 117(2) . . ? C13 C12 C11 119.7(4) . . ? C13 C12 H12 122.0(7) . . ? C11 C12 H12 118.3(7) . . ? C12 C13 C14 119.1(4) . . ? C12 C13 H13 121(3) . . ? C14 C13 H13 119(3) . . ? C13 C14 C15 117.6(3) . . ? C13 C14 C112 124.8(3) . . ? C15 C14 C112 117.6(4) . . ? N11 C15 C14 123.7(3) . . ? N11 C15 C25 115.7(3) . . ? C14 C15 C25 120.7(3) . . ? N12 C16 C17 110.6(3) . . ? N12 C16 H16 121(2) . . ? C17 C16 H16 128(2) . . ? C18 C17 C16 104.8(3) . . ? C18 C17 H17 128.9(7) . . ? C16 C17 H17 126.3(7) . . ? N14 C18 C17 108.9(3) . . ? N14 C18 H18 118(2) . . ? C17 C18 H18 133(2) . . ? N13 C19 C110 110.6(3) . . ? N13 C19 H19 121(3) . . ? C110 C19 H19 129(3) . . ? N21 C21 C22 123.1(3) . . ? N21 C21 H21 116(2) . . ? C22 C21 H21 121(2) . . ? C23 C22 C21 119.7(4) . . ? C23 C22 H22 118(2) . . ? C21 C22 H22 123(2) . . ? C22 C23 C24 119.2(3) . . ? C22 C23 H23 126(2) . . ? C24 C23 H23 114(2) . . ? C23 C24 C25 116.9(3) . . ? C23 C24 C212 124.4(3) . . ? C25 C24 C212 118.7(4) . . ? N21 C25 C24 124.1(3) . . ? N21 C25 C15 115.7(3) . . ? C24 C25 C15 120.2(3) . . ? N22 C26 C27 110.5(3) . . ? N22 C26 H26 120(2) . . ? C27 C26 H26 130(2) . . ? C28 C27 C26 105.2(3) . . ? C28 C27 H27 127(3) . . ? C26 C27 H27 128(3) . . ? N24 C28 C27 108.8(3) . . ? N24 C28 H28 121(2) . . ? C27 C28 H28 130(2) . . ? N23 C29 C210 110.4(3) . . ? N23 C29 H29 121(3) . . ? C210 C29 H29 129(3) . . ? C111 C110 C19 104.4(3) . . ? C111 C110 H110 128(3) . . ? C19 C110 H110 127(3) . . ? N15 C111 C110 109.3(3) . . ? N15 C111 H111 116(2) . . ? C110 C111 H111 134(2) . . ? C212 C112 C14 122.0(4) . . ? C212 C112 H112 120(3) . . ? C14 C112 H112 118(3) . . ? C211 C210 C29 105.0(3) . . ? C211 C210 H210 128.4(7) . . ? C29 C210 H210 126.5(8) . . ? N25 C211 C210 108.5(3) . . ? N25 C211 H211 121(3) . . ? C210 C211 H211 130(3) . . ? C112 C212 C24 120.8(4) . . ? C112 C212 H212 120(2) . . ? C24 C212 H212 119(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N21 Fe1 N11 C11 176.5(3) . . . . ? N23 Fe1 N11 C11 -93.6(3) . . . . ? N22 Fe1 N11 C11 134.9(17) . . . . ? N13 Fe1 N11 C11 86.4(3) . . . . ? N12 Fe1 N11 C11 -6.4(3) . . . . ? N21 Fe1 N11 C15 -0.8(2) . . . . ? N23 Fe1 N11 C15 89.1(2) . . . . ? N22 Fe1 N11 C15 -42.3(18) . . . . ? N13 Fe1 N11 C15 -90.9(2) . . . . ? N12 Fe1 N11 C15 176.3(2) . . . . ? N21 Fe1 N12 C16 -31(3) . . . . ? N11 Fe1 N12 C16 -118.2(3) . . . . ? N23 Fe1 N12 C16 -28.5(3) . . . . ? N22 Fe1 N12 C16 64.3(3) . . . . ? N13 Fe1 N12 C16 152.6(3) . . . . ? N21 Fe1 N12 N14 170(2) . . . . ? N11 Fe1 N12 N14 83.2(3) . . . . ? N23 Fe1 N12 N14 172.8(3) . . . . ? N22 Fe1 N12 N14 -94.4(3) . . . . ? N13 Fe1 N12 N14 -6.0(3) . . . . ? N21 Fe1 N13 C19 18.8(3) . . . . ? N11 Fe1 N13 C19 101.2(3) . . . . ? N23 Fe1 N13 C19 102(6) . . . . ? N22 Fe1 N13 C19 -75.8(3) . . . . ? N12 Fe1 N13 C19 -161.4(3) . . . . ? N21 Fe1 N13 N15 -169.1(3) . . . . ? N11 Fe1 N13 N15 -86.7(3) . . . . ? N23 Fe1 N13 N15 -86(7) . . . . ? N22 Fe1 N13 N15 96.2(3) . . . . ? N12 Fe1 N13 N15 10.7(3) . . . . ? C16 N12 N14 C18 0.1(4) . . . . ? Fe1 N12 N14 C18 162.3(3) . . . . ? C16 N12 N14 B1 172.9(3) . . . . ? Fe1 N12 N14 B1 -24.8(4) . . . . ? N15 B1 N14 C18 -137.4(4) . . . . ? N15 B1 N14 N12 51.1(5) . . . . ? C19 N13 N15 C111 -0.1(4) . . . . ? Fe1 N13 N15 C111 -173.6(2) . . . . ? C19 N13 N15 B1 -171.7(3) . . . . ? Fe1 N13 N15 B1 14.8(4) . . . . ? N14 B1 N15 C111 143.8(3) . . . . ? N14 B1 N15 N13 -46.0(5) . . . . ? N11 Fe1 N21 C21 179.7(3) . . . . ? N23 Fe1 N21 C21 89.7(3) . . . . ? N22 Fe1 N21 C21 -2.9(3) . . . . ? N13 Fe1 N21 C21 -91.4(3) . . . . ? N12 Fe1 N21 C21 93(2) . . . . ? N11 Fe1 N21 C25 2.2(2) . . . . ? N23 Fe1 N21 C25 -87.9(2) . . . . ? N22 Fe1 N21 C25 179.5(2) . . . . ? N13 Fe1 N21 C25 91.0(2) . . . . ? N12 Fe1 N21 C25 -85(2) . . . . ? N21 Fe1 N22 C26 -115.9(3) . . . . ? N11 Fe1 N22 C26 -74.6(18) . . . . ? N23 Fe1 N22 C26 154.0(3) . . . . ? N13 Fe1 N22 C26 -26.0(3) . . . . ? N12 Fe1 N22 C26 67.0(3) . . . . ? N21 Fe1 N22 N24 76.5(3) . . . . ? N11 Fe1 N22 N24 117.7(17) . . . . ? N23 Fe1 N22 N24 -13.6(3) . . . . ? N13 Fe1 N22 N24 166.3(3) . . . . ? N12 Fe1 N22 N24 -100.7(3) . . . . ? N21 Fe1 N23 C29 108.7(3) . . . . ? N11 Fe1 N23 C29 26.3(3) . . . . ? N22 Fe1 N23 C29 -156.6(3) . . . . ? N13 Fe1 N23 C29 26(7) . . . . ? N12 Fe1 N23 C29 -71.1(3) . . . . ? N21 Fe1 N23 N25 -83.6(3) . . . . ? N11 Fe1 N23 N25 -166.0(3) . . . . ? N22 Fe1 N23 N25 11.1(3) . . . . ? N13 Fe1 N23 N25 -166(6) . . . . ? N12 Fe1 N23 N25 96.6(3) . . . . ? C26 N22 N24 C28 0.4(4) . . . . ? Fe1 N22 N24 C28 170.2(2) . . . . ? C26 N22 N24 B2 175.5(3) . . . . ? Fe1 N22 N24 B2 -14.7(4) . . . . ? N25 B2 N24 C28 -139.5(3) . . . . ? N25 B2 N24 N22 46.3(4) . . . . ? C29 N23 N25 C211 0.4(4) . . . . ? Fe1 N23 N25 C211 -169.5(2) . . . . ? C29 N23 N25 B2 -170.4(3) . . . . ? Fe1 N23 N25 B2 19.7(4) . . . . ? N24 B2 N25 C211 141.3(3) . . . . ? N24 B2 N25 N23 -49.4(4) . . . . ? C15 N11 C11 C12 1.5(5) . . . . ? Fe1 N11 C11 C12 -175.7(3) . . . . ? N11 C11 C12 C13 -2.5(5) . . . . ? C11 C12 C13 C14 0.8(5) . . . . ? C12 C13 C14 C15 1.6(5) . . . . ? C12 C13 C14 C112 -179.5(4) . . . . ? C11 N11 C15 C14 1.2(5) . . . . ? Fe1 N11 C15 C14 178.8(3) . . . . ? C11 N11 C15 C25 -178.3(3) . . . . ? Fe1 N11 C15 C25 -0.6(4) . . . . ? C13 C14 C15 N11 -2.7(5) . . . . ? C112 C14 C15 N11 178.3(3) . . . . ? C13 C14 C15 C25 176.7(3) . . . . ? C112 C14 C15 C25 -2.3(5) . . . . ? N14 N12 C16 C17 -1.2(4) . . . . ? Fe1 N12 C16 C17 -163.1(3) . . . . ? N12 C16 C17 C18 1.8(4) . . . . ? N12 N14 C18 C17 1.0(4) . . . . ? B1 N14 C18 C17 -171.5(4) . . . . ? C16 C17 C18 N14 -1.7(5) . . . . ? N15 N13 C19 C110 0.9(4) . . . . ? Fe1 N13 C19 C110 174.2(2) . . . . ? C25 N21 C21 C22 0.9(5) . . . . ? Fe1 N21 C21 C22 -176.6(2) . . . . ? N21 C21 C22 C23 -0.8(5) . . . . ? C21 C22 C23 C24 -0.8(5) . . . . ? C22 C23 C24 C25 2.1(5) . . . . ? C22 C23 C24 C212 -179.1(3) . . . . ? C21 N21 C25 C24 0.6(5) . . . . ? Fe1 N21 C25 C24 178.5(3) . . . . ? C21 N21 C25 C15 179.0(3) . . . . ? Fe1 N21 C25 C15 -3.1(4) . . . . ? C23 C24 C25 N21 -2.1(5) . . . . ? C212 C24 C25 N21 179.1(3) . . . . ? C23 C24 C25 C15 179.6(3) . . . . ? C212 C24 C25 C15 0.8(5) . . . . ? N11 C15 C25 N21 2.5(4) . . . . ? C14 C15 C25 N21 -177.0(3) . . . . ? N11 C15 C25 C24 -179.0(3) . . . . ? C14 C15 C25 C24 1.5(5) . . . . ? N24 N22 C26 C27 -1.0(4) . . . . ? Fe1 N22 C26 C27 -170.6(2) . . . . ? N22 C26 C27 C28 1.2(4) . . . . ? N22 N24 C28 C27 0.3(4) . . . . ? B2 N24 C28 C27 -174.7(3) . . . . ? C26 C27 C28 N24 -0.9(4) . . . . ? N25 N23 C29 C210 0.2(4) . . . . ? Fe1 N23 C29 C210 169.7(2) . . . . ? N13 C19 C110 C111 -1.4(4) . . . . ? N13 N15 C111 C110 -0.8(4) . . . . ? B1 N15 C111 C110 170.7(3) . . . . ? C19 C110 C111 N15 1.3(4) . . . . ? C13 C14 C112 C212 -178.0(4) . . . . ? C15 C14 C112 C212 0.8(5) . . . . ? N23 C29 C210 C211 -0.7(4) . . . . ? N23 N25 C211 C210 -0.8(4) . . . . ? B2 N25 C211 C210 169.8(3) . . . . ? C29 C210 C211 N25 0.9(4) . . . . ? C14 C112 C212 C24 1.4(6) . . . . ? C23 C24 C212 C112 179.1(4) . . . . ? C25 C24 C212 C112 -2.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.379 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.091 #====================================================================== data_phen3 _database_code_depnum_ccdc_archive 'CCDC 233287' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,2'-Phenanthroline-bis[di(hydro)bis(1-pyrazolyl)borate iron(II) ; _chemical_name_common ;2,2'-Phenanthroline-bis(di(hydro)bis(1-pyrazolyl)borate iron(ii) ; _chemical_melting_point 'not measured' _chemical_formula_moiety 'C24 H24 B2 Fe N10' _chemical_formula_sum 'C24 H24 B2 Fe N10' _chemical_formula_weight 530.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.655(2) _cell_length_b 11.0156(19) _cell_length_c 10.5664(18) _cell_angle_alpha 69.492(3) _cell_angle_beta 109.755(3) _cell_angle_gamma 93.280(3) _cell_volume 1192.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 30(2) _cell_measurement_reflns_used 1688 _cell_measurement_theta_min 4.683 _cell_measurement_theta_max 58.115 _exptl_crystal_description block _exptl_crystal_colour clear_intense_red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 0.669 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.9063 _exptl_absorpt_correction_T_max 0.9484 _exptl_absorpt_process_details 'XPREP (SHELXTL,1997)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 3 sets of \w scans each set at different \f and/or 2\q angles and each scan (20s exposure) covering 0.3\% in \w. Crystal to detector distance 4.965. ; _diffrn_ambient_temperature 30(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'micro-focus X-ray source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker ProteumM with Bede Microsource' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 8374 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.1190 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 29.13 _reflns_number_total 5832 _reflns_number_gt 3893 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SMART-NT V6.1 (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0263P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5832 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0924 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.0983 _refine_ls_wR_factor_gt 0.0894 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.915 _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 -1.23803(4) 0.76340(4) -1.25652(5) 0.00833(11) Uani 1 1 d . . . B1 B -1.3055(3) 0.6920(3) -0.9463(4) 0.0138(7) Uani 1 1 d . . . H11B H -1.213(3) 0.698(3) -0.883(3) 0.017 Uiso 1 1 d . . . H12B H -1.368(3) 0.667(3) -0.883(3) 0.017 Uiso 1 1 d . . . B2 B -1.3160(3) 0.6744(3) -1.5539(4) 0.0113(7) Uani 1 1 d . . . H21B H -1.304(3) 0.777(3) -1.623(3) 0.014 Uiso 1 1 d . . . H22B H -1.344(3) 0.607(3) -1.614(3) 0.014 Uiso 1 1 d . . . N11 N -1.0830(2) 0.8080(2) -1.1366(3) 0.0104(5) Uani 1 1 d . . . N12 N -1.2550(2) 0.5940(2) -1.1086(2) 0.0096(5) Uani 1 1 d . . . N13 N -1.3286(2) 0.8682(2) -1.1942(2) 0.0102(5) Uani 1 1 d . . . N14 N -1.3049(2) 0.5838(2) -1.0052(2) 0.0111(5) Uani 1 1 d . . . N15 N -1.3597(2) 0.8219(2) -1.0726(2) 0.0119(5) Uani 1 1 d . . . N21 N -1.2164(2) 0.9230(2) -1.4044(2) 0.0094(5) Uani 1 1 d . . . N22 N -1.3986(2) 0.7324(2) -1.3840(2) 0.0104(5) Uani 1 1 d . . . N23 N -1.1444(2) 0.6599(2) -1.3169(2) 0.0108(5) Uani 1 1 d . . . N24 N -1.4165(2) 0.6838(2) -1.4915(2) 0.0107(5) Uani 1 1 d . . . N25 N -1.1944(2) 0.6162(2) -1.4283(2) 0.0104(5) Uani 1 1 d . . . C11 C -1.0189(3) 0.7512(3) -0.9978(3) 0.0129(6) Uani 1 1 d . . . H11 H -1.046(3) 0.676(3) -0.942(3) 0.015 Uiso 1 1 d . . . C12 C -0.9132(3) 0.8005(3) -0.9265(3) 0.0140(6) Uani 1 1 d . . . H12 H -0.877(3) 0.750(3) -0.830(3) 0.017 Uiso 1 1 d . . . C13 C -0.8691(3) 0.9105(3) -1.0008(3) 0.0139(6) Uani 1 1 d . . . H13 H -0.802(3) 0.941(3) -0.956(3) 0.017 Uiso 1 1 d . . . C14 C -0.9318(3) 0.9722(3) -1.1483(3) 0.0126(6) Uani 1 1 d . . . C15 C -1.0389(3) 0.9190(3) -1.2102(3) 0.0103(6) Uani 1 1 d . . . C16 C -1.2566(3) 0.4763(3) -1.1189(3) 0.0120(6) Uani 1 1 d . . . H16 H -1.228(3) 0.458(3) -1.186(3) 0.014 Uiso 1 1 d . . . C17 C -1.3053(3) 0.3889(3) -1.0220(3) 0.0137(6) Uani 1 1 d . . . H17 H -1.314(3) 0.302(3) -1.008(3) 0.016 Uiso 1 1 d . . . C18 C -1.3347(3) 0.4608(3) -0.9524(3) 0.0145(6) Uani 1 1 d . . . H18 H -1.368(3) 0.441(3) -0.880(3) 0.017 Uiso 1 1 d . . . C19 C -1.3804(3) 0.9888(3) -1.2648(3) 0.0105(6) Uani 1 1 d . . . H19 H -1.370(3) 1.043(3) -1.350(3) 0.013 Uiso 1 1 d . . . C21 C -1.2872(3) 0.9802(3) -1.5404(3) 0.0116(6) Uani 1 1 d . . . H21 H -1.360(3) 0.941(3) -1.576(3) 0.014 Uiso 1 1 d . . . C22 C -1.2558(3) 1.0917(3) -1.6349(3) 0.0133(6) Uani 1 1 d . . . H22 H -1.314(3) 1.125(3) -1.737(3) 0.016 Uiso 1 1 d . . . C23 C -1.1508(3) 1.1483(3) -1.5883(3) 0.0151(6) Uani 1 1 d . . . H23 H -1.127(3) 1.230(3) -1.641(3) 0.018 Uiso 1 1 d . . . C24 C -1.0739(3) 1.0936(3) -1.4440(3) 0.0115(6) Uani 1 1 d . . . C25 C -1.1117(3) 0.9792(3) -1.3565(3) 0.0110(6) Uani 1 1 d . . . C26 C -1.5085(3) 0.7320(3) -1.3666(3) 0.0115(6) Uani 1 1 d . . . H26 H -1.513(3) 0.762(3) -1.296(3) 0.014 Uiso 1 1 d . . . C27 C -1.5956(3) 0.6869(3) -1.4625(3) 0.0130(6) Uani 1 1 d . . . H27 H -1.678(3) 0.680(3) -1.476(3) 0.016 Uiso 1 1 d . . . C28 C -1.5338(3) 0.6571(3) -1.5393(3) 0.0127(6) Uani 1 1 d . . . H28 H -1.564(3) 0.623(3) -1.611(3) 0.015 Uiso 1 1 d . . . C29 C -1.0321(3) 0.6003(3) -1.2445(3) 0.0122(6) Uani 1 1 d . . . H29 H -0.983(3) 0.615(3) -1.168(3) 0.015 Uiso 1 1 d . . . C110 C -1.4449(3) 1.0229(3) -1.1912(3) 0.0134(6) Uani 1 1 d . . . H110 H -1.487(3) 1.102(3) -1.216(3) 0.016 Uiso 1 1 d . . . C111 C -1.4303(3) 0.9135(3) -1.0708(3) 0.0138(6) Uani 1 1 d . . . H111 H -1.461(3) 0.897(3) -0.988(3) 0.017 Uiso 1 1 d . . . C112 C -0.8946(3) 1.0871(3) -1.2390(3) 0.0142(6) Uani 1 1 d . . . H112 H -0.821(3) 1.122(3) -1.195(3) 0.017 Uiso 1 1 d . . . C210 C -1.0072(3) 0.5204(3) -1.3101(3) 0.0131(6) Uani 1 1 d . . . H210 H -0.939(3) 0.469(3) -1.283(3) 0.016 Uiso 1 1 d . . . C211 C -1.1118(3) 0.5319(3) -1.4243(3) 0.0134(6) Uani 1 1 d . . . H211 H -1.134(3) 0.493(3) -1.500(3) 0.016 Uiso 1 1 d . . . C212 C -0.9623(3) 1.1436(3) -1.3797(3) 0.0153(7) Uani 1 1 d . . . H212 H -0.940(3) 1.218(3) -1.434(3) 0.018 Uiso 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 0.0097(2) 0.0080(2) 0.0078(2) -0.00185(16) 0.00462(16) -0.00080(15) B1 0.0194(19) 0.0120(16) 0.0110(17) -0.0026(14) 0.0077(15) 0.0019(14) B2 0.0128(17) 0.0125(16) 0.0082(16) -0.0028(13) 0.0038(14) 0.0003(13) N11 0.0101(13) 0.0104(12) 0.0103(13) -0.0029(10) 0.0027(10) 0.0049(10) N12 0.0104(13) 0.0113(12) 0.0073(12) -0.0021(10) 0.0044(10) 0.0003(10) N13 0.0093(12) 0.0130(12) 0.0084(13) -0.0034(10) 0.0035(10) -0.0019(10) N14 0.0137(13) 0.0125(12) 0.0074(12) -0.0016(10) 0.0058(10) 0.0008(10) N15 0.0141(13) 0.0130(12) 0.0092(13) -0.0045(10) 0.0044(11) -0.0015(10) N21 0.0094(13) 0.0095(11) 0.0088(13) -0.0016(10) 0.0035(10) 0.0027(10) N22 0.0136(14) 0.0077(11) 0.0109(13) -0.0020(10) 0.0068(11) -0.0018(10) N23 0.0112(13) 0.0118(12) 0.0089(13) -0.0016(10) 0.0051(11) -0.0010(10) N24 0.0140(13) 0.0090(11) 0.0083(12) -0.0015(9) 0.0046(10) -0.0011(10) N25 0.0131(13) 0.0094(11) 0.0098(13) -0.0033(10) 0.0054(10) -0.0019(10) C11 0.0145(16) 0.0116(14) 0.0123(15) -0.0028(12) 0.0056(13) 0.0012(12) C12 0.0156(16) 0.0153(15) 0.0109(15) -0.0055(12) 0.0023(13) 0.0057(12) C13 0.0100(16) 0.0182(15) 0.0167(16) -0.0114(13) 0.0031(13) -0.0010(12) C14 0.0118(15) 0.0134(14) 0.0165(16) -0.0088(12) 0.0059(13) 0.0004(12) C15 0.0118(15) 0.0102(13) 0.0111(15) -0.0040(12) 0.0059(12) 0.0010(11) C16 0.0149(16) 0.0109(14) 0.0115(15) -0.0048(12) 0.0050(13) -0.0003(11) C17 0.0159(16) 0.0106(14) 0.0135(16) -0.0032(12) 0.0047(13) -0.0004(12) C18 0.0177(17) 0.0139(15) 0.0131(16) -0.0023(12) 0.0096(13) -0.0022(12) C19 0.0121(15) 0.0109(14) 0.0065(14) -0.0030(12) 0.0008(12) -0.0009(11) C21 0.0120(15) 0.0108(14) 0.0140(16) -0.0048(12) 0.0064(13) -0.0004(11) C22 0.0151(16) 0.0132(14) 0.0097(15) -0.0006(12) 0.0047(13) 0.0038(12) C23 0.0195(17) 0.0094(14) 0.0179(17) -0.0008(13) 0.0121(14) 0.0011(12) C24 0.0112(15) 0.0100(14) 0.0169(16) -0.0055(12) 0.0086(13) -0.0012(11) C25 0.0133(15) 0.0098(13) 0.0128(15) -0.0058(12) 0.0061(12) 0.0002(11) C26 0.0160(16) 0.0095(13) 0.0099(15) -0.0014(12) 0.0077(13) -0.0008(11) C27 0.0106(15) 0.0103(14) 0.0157(16) -0.0018(12) 0.0041(13) 0.0001(12) C28 0.0127(16) 0.0105(14) 0.0126(16) -0.0032(12) 0.0024(13) -0.0011(12) C29 0.0150(16) 0.0123(14) 0.0082(15) -0.0009(12) 0.0055(13) -0.0026(12) C110 0.0135(16) 0.0111(14) 0.0135(16) -0.0056(12) -0.0004(13) 0.0049(12) C111 0.0138(16) 0.0157(15) 0.0148(16) -0.0074(13) 0.0062(13) -0.0001(12) C112 0.0119(16) 0.0141(15) 0.0205(17) -0.0099(13) 0.0067(13) -0.0034(12) C210 0.0150(17) 0.0125(15) 0.0114(15) -0.0003(12) 0.0077(13) 0.0011(12) C211 0.0189(17) 0.0110(14) 0.0132(16) -0.0043(12) 0.0091(14) -0.0023(12) C212 0.0141(16) 0.0109(14) 0.0219(18) -0.0039(13) 0.0096(14) -0.0019(12) _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 N21 1.971(2) . ? Fe1 N11 1.974(2) . ? Fe1 N22 1.995(2) . ? Fe1 N23 2.005(2) . ? Fe1 N13 2.006(2) . ? Fe1 N12 2.022(2) . ? B1 N14 1.528(4) . ? B1 N15 1.556(4) . ? B1 H11B 1.07(3) . ? B1 H12B 1.11(3) . ? B2 N24 1.549(4) . ? B2 N25 1.555(4) . ? B2 H21B 1.14(3) . ? B2 H22B 1.10(3) . ? N11 C11 1.331(4) . ? N11 C15 1.378(3) . ? N12 C16 1.337(3) . ? N12 N14 1.372(3) . ? N13 C19 1.333(3) . ? N13 N15 1.371(3) . ? N14 C18 1.347(3) . ? N15 C111 1.347(3) . ? N21 C21 1.329(4) . ? N21 C25 1.358(4) . ? N22 C26 1.354(3) . ? N22 N24 1.369(3) . ? N23 C29 1.342(4) . ? N23 N25 1.363(3) . ? N24 C28 1.342(4) . ? N25 C211 1.356(3) . ? C11 C12 1.401(4) . ? C11 H11 0.94(3) . ? C12 C13 1.372(4) . ? C12 H12 0.93(3) . ? C13 C14 1.403(4) . ? C13 H13 0.89(3) . ? C14 C15 1.401(4) . ? C14 C112 1.442(4) . ? C15 C25 1.417(4) . ? C16 C17 1.392(4) . ? C16 H16 0.96(3) . ? C17 C18 1.377(4) . ? C17 H17 0.92(3) . ? C18 H18 0.92(3) . ? C19 C110 1.394(4) . ? C19 H19 0.93(3) . ? C21 C22 1.406(4) . ? C21 H21 0.95(3) . ? C22 C23 1.360(4) . ? C22 H22 1.01(3) . ? C23 C24 1.409(4) . ? C23 H23 0.96(3) . ? C24 C25 1.425(4) . ? C24 C212 1.428(4) . ? C26 C27 1.380(4) . ? C26 H26 0.93(3) . ? C27 C28 1.377(4) . ? C27 H27 0.92(3) . ? C28 H28 0.91(3) . ? C29 C210 1.389(4) . ? C29 H29 0.88(3) . ? C110 C111 1.380(4) . ? C110 H110 0.93(3) . ? C111 H111 1.01(3) . ? C112 C212 1.355(4) . ? C112 H112 0.96(3) . ? C210 C211 1.369(4) . ? C210 H210 0.91(3) . ? C211 H211 0.98(3) . ? C212 H212 0.90(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 N21 Fe1 N11 82.52(10) . . ? N21 Fe1 N22 94.22(10) . . ? N11 Fe1 N22 175.73(10) . . ? N21 Fe1 N23 89.48(9) . . ? N11 Fe1 N23 90.07(10) . . ? N22 Fe1 N23 92.68(10) . . ? N21 Fe1 N13 90.22(9) . . ? N11 Fe1 N13 88.82(10) . . ? N22 Fe1 N13 88.42(10) . . ? N23 Fe1 N13 178.88(11) . . ? N21 Fe1 N12 176.74(10) . . ? N11 Fe1 N12 97.54(10) . . ? N22 Fe1 N12 85.86(9) . . ? N23 Fe1 N12 87.26(9) . . ? N13 Fe1 N12 93.04(9) . . ? N14 B1 N15 109.8(2) . . ? N14 B1 H11B 107.0(16) . . ? N15 B1 H11B 112.2(16) . . ? N14 B1 H12B 107.7(15) . . ? N15 B1 H12B 106.7(15) . . ? H11B B1 H12B 113(2) . . ? N24 B2 N25 109.2(2) . . ? N24 B2 H21B 107.7(14) . . ? N25 B2 H21B 110.1(15) . . ? N24 B2 H22B 108.4(15) . . ? N25 B2 H22B 107.9(15) . . ? H21B B2 H22B 113(2) . . ? C11 N11 C15 116.4(3) . . ? C11 N11 Fe1 130.4(2) . . ? C15 N11 Fe1 113.08(19) . . ? C16 N12 N14 106.2(2) . . ? C16 N12 Fe1 126.33(18) . . ? N14 N12 Fe1 124.53(17) . . ? C19 N13 N15 106.1(2) . . ? C19 N13 Fe1 128.70(19) . . ? N15 N13 Fe1 124.92(17) . . ? C18 N14 N12 109.4(2) . . ? C18 N14 B1 126.7(2) . . ? N12 N14 B1 123.2(2) . . ? C111 N15 N13 109.4(2) . . ? C111 N15 B1 125.3(2) . . ? N13 N15 B1 124.6(2) . . ? C21 N21 C25 117.2(2) . . ? C21 N21 Fe1 129.7(2) . . ? C25 N21 Fe1 113.04(19) . . ? C26 N22 N24 105.4(2) . . ? C26 N22 Fe1 127.3(2) . . ? N24 N22 Fe1 126.28(17) . . ? C29 N23 N25 106.5(2) . . ? C29 N23 Fe1 128.0(2) . . ? N25 N23 Fe1 124.36(18) . . ? C28 N24 N22 109.8(2) . . ? C28 N24 B2 126.8(2) . . ? N22 N24 B2 123.3(2) . . ? C211 N25 N23 108.9(2) . . ? C211 N25 B2 125.8(2) . . ? N23 N25 B2 124.3(2) . . ? N11 C11 C12 123.1(3) . . ? N11 C11 H11 119.7(19) . . ? C12 C11 H11 117.1(19) . . ? C13 C12 C11 120.1(3) . . ? C13 C12 H12 125.9(19) . . ? C11 C12 H12 113.9(19) . . ? C12 C13 C14 118.9(3) . . ? C12 C13 H13 120(2) . . ? C14 C13 H13 121(2) . . ? C15 C14 C13 117.4(3) . . ? C15 C14 C112 118.1(3) . . ? C13 C14 C112 124.5(3) . . ? N11 C15 C14 124.0(3) . . ? N11 C15 C25 114.8(3) . . ? C14 C15 C25 121.1(3) . . ? N12 C16 C17 110.8(2) . . ? N12 C16 H16 122.9(17) . . ? C17 C16 H16 126.2(17) . . ? C18 C17 C16 104.8(3) . . ? C18 C17 H17 128.4(18) . . ? C16 C17 H17 126.8(18) . . ? N14 C18 C17 108.8(2) . . ? N14 C18 H18 117.5(18) . . ? C17 C18 H18 133.7(19) . . ? N13 C19 C110 111.3(3) . . ? N13 C19 H19 123.0(18) . . ? C110 C19 H19 125.7(18) . . ? N21 C21 C22 122.8(3) . . ? N21 C21 H21 118.1(18) . . ? C22 C21 H21 119.1(18) . . ? C23 C22 C21 120.5(3) . . ? C23 C22 H22 123.2(17) . . ? C21 C22 H22 116.3(17) . . ? C22 C23 C24 119.1(3) . . ? C22 C23 H23 126.4(19) . . ? C24 C23 H23 114.0(19) . . ? C23 C24 C25 116.7(3) . . ? C23 C24 C212 125.2(3) . . ? C25 C24 C212 118.1(3) . . ? N21 C25 C15 116.5(2) . . ? N21 C25 C24 123.7(3) . . ? C15 C25 C24 119.8(3) . . ? N22 C26 C27 111.1(3) . . ? N22 C26 H26 117.0(18) . . ? C27 C26 H26 131.9(18) . . ? C28 C27 C26 104.7(3) . . ? C28 C27 H27 126.4(19) . . ? C26 C27 H27 128.9(19) . . ? N24 C28 C27 109.0(3) . . ? N24 C28 H28 122.9(19) . . ? C27 C28 H28 128.0(19) . . ? N23 C29 C210 110.7(3) . . ? N23 C29 H29 122(2) . . ? C210 C29 H29 128(2) . . ? C111 C110 C19 104.2(3) . . ? C111 C110 H110 127.8(18) . . ? C19 C110 H110 128.0(18) . . ? N15 C111 C110 109.0(3) . . ? N15 C111 H111 120.6(16) . . ? C110 C111 H111 130.4(16) . . ? C212 C112 C14 121.0(3) . . ? C212 C112 H112 121.7(18) . . ? C14 C112 H112 117.3(18) . . ? C211 C210 C29 104.7(3) . . ? C211 C210 H210 126.7(19) . . ? C29 C210 H210 129(2) . . ? N25 C211 C210 109.1(3) . . ? N25 C211 H211 118.4(18) . . ? C210 C211 H211 132.4(18) . . ? C112 C212 C24 121.8(3) . . ? C112 C212 H212 120(2) . . ? C24 C212 H212 118(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N21 Fe1 N11 C11 176.5(2) . . . . ? N22 Fe1 N11 C11 136.0(13) . . . . ? N23 Fe1 N11 C11 -94.0(2) . . . . ? N13 Fe1 N11 C11 86.1(2) . . . . ? N12 Fe1 N11 C11 -6.8(2) . . . . ? N21 Fe1 N11 C15 -0.74(18) . . . . ? N22 Fe1 N11 C15 -41.2(14) . . . . ? N23 Fe1 N11 C15 88.73(18) . . . . ? N13 Fe1 N11 C15 -91.12(18) . . . . ? N12 Fe1 N11 C15 175.97(17) . . . . ? N21 Fe1 N12 C16 -27(2) . . . . ? N11 Fe1 N12 C16 -118.0(2) . . . . ? N22 Fe1 N12 C16 64.6(2) . . . . ? N23 Fe1 N12 C16 -28.2(2) . . . . ? N13 Fe1 N12 C16 152.8(2) . . . . ? N21 Fe1 N12 N14 174.9(18) . . . . ? N11 Fe1 N12 N14 84.1(2) . . . . ? N22 Fe1 N12 N14 -93.4(2) . . . . ? N23 Fe1 N12 N14 173.8(2) . . . . ? N13 Fe1 N12 N14 -5.2(2) . . . . ? N21 Fe1 N13 C19 17.7(3) . . . . ? N11 Fe1 N13 C19 100.2(3) . . . . ? N22 Fe1 N13 C19 -76.5(3) . . . . ? N23 Fe1 N13 C19 92(5) . . . . ? N12 Fe1 N13 C19 -162.3(3) . . . . ? N21 Fe1 N13 N15 -169.4(2) . . . . ? N11 Fe1 N13 N15 -86.9(2) . . . . ? N22 Fe1 N13 N15 96.3(2) . . . . ? N23 Fe1 N13 N15 -95(5) . . . . ? N12 Fe1 N13 N15 10.6(2) . . . . ? C16 N12 N14 C18 0.8(3) . . . . ? Fe1 N12 N14 C18 162.5(2) . . . . ? C16 N12 N14 B1 171.9(3) . . . . ? Fe1 N12 N14 B1 -26.4(4) . . . . ? N15 B1 N14 C18 -138.4(3) . . . . ? N15 B1 N14 N12 52.1(4) . . . . ? C19 N13 N15 C111 0.4(3) . . . . ? Fe1 N13 N15 C111 -173.8(2) . . . . ? C19 N13 N15 B1 -171.1(3) . . . . ? Fe1 N13 N15 B1 14.7(4) . . . . ? N14 B1 N15 C111 143.9(3) . . . . ? N14 B1 N15 N13 -46.0(4) . . . . ? N11 Fe1 N21 C21 -179.2(2) . . . . ? N22 Fe1 N21 C21 -1.9(2) . . . . ? N23 Fe1 N21 C21 90.7(2) . . . . ? N13 Fe1 N21 C21 -90.4(2) . . . . ? N12 Fe1 N21 C21 90(2) . . . . ? N11 Fe1 N21 C25 1.72(18) . . . . ? N22 Fe1 N21 C25 178.94(18) . . . . ? N23 Fe1 N21 C25 -88.42(19) . . . . ? N13 Fe1 N21 C25 90.50(19) . . . . ? N12 Fe1 N21 C25 -90(2) . . . . ? N21 Fe1 N22 C26 -116.6(2) . . . . ? N11 Fe1 N22 C26 -76.4(14) . . . . ? N23 Fe1 N22 C26 153.7(2) . . . . ? N13 Fe1 N22 C26 -26.5(2) . . . . ? N12 Fe1 N22 C26 66.7(2) . . . . ? N21 Fe1 N22 N24 76.5(2) . . . . ? N11 Fe1 N22 N24 116.7(13) . . . . ? N23 Fe1 N22 N24 -13.2(2) . . . . ? N13 Fe1 N22 N24 166.6(2) . . . . ? N12 Fe1 N22 N24 -100.2(2) . . . . ? N21 Fe1 N23 C29 109.6(2) . . . . ? N11 Fe1 N23 C29 27.1(2) . . . . ? N22 Fe1 N23 C29 -156.2(2) . . . . ? N13 Fe1 N23 C29 35(5) . . . . ? N12 Fe1 N23 C29 -70.5(2) . . . . ? N21 Fe1 N23 N25 -84.1(2) . . . . ? N11 Fe1 N23 N25 -166.6(2) . . . . ? N22 Fe1 N23 N25 10.1(2) . . . . ? N13 Fe1 N23 N25 -159(5) . . . . ? N12 Fe1 N23 N25 95.8(2) . . . . ? C26 N22 N24 C28 1.1(3) . . . . ? Fe1 N22 N24 C28 170.36(19) . . . . ? C26 N22 N24 B2 176.2(2) . . . . ? Fe1 N22 N24 B2 -14.6(3) . . . . ? N25 B2 N24 C28 -139.6(3) . . . . ? N25 B2 N24 N22 46.2(3) . . . . ? C29 N23 N25 C211 -0.9(3) . . . . ? Fe1 N23 N25 C211 -169.65(18) . . . . ? C29 N23 N25 B2 -170.3(2) . . . . ? Fe1 N23 N25 B2 20.9(3) . . . . ? N24 B2 N25 C211 142.1(3) . . . . ? N24 B2 N25 N23 -50.2(3) . . . . ? C15 N11 C11 C12 1.2(4) . . . . ? Fe1 N11 C11 C12 -176.0(2) . . . . ? N11 C11 C12 C13 -1.8(4) . . . . ? C11 C12 C13 C14 0.1(4) . . . . ? C12 C13 C14 C15 1.9(4) . . . . ? C12 C13 C14 C112 -179.2(3) . . . . ? C11 N11 C15 C14 1.1(4) . . . . ? Fe1 N11 C15 C14 178.7(2) . . . . ? C11 N11 C15 C25 -178.0(2) . . . . ? Fe1 N11 C15 C25 -0.3(3) . . . . ? C13 C14 C15 N11 -2.7(4) . . . . ? C112 C14 C15 N11 178.4(2) . . . . ? C13 C14 C15 C25 176.4(2) . . . . ? C112 C14 C15 C25 -2.6(4) . . . . ? N14 N12 C16 C17 -0.9(3) . . . . ? Fe1 N12 C16 C17 -162.1(2) . . . . ? N12 C16 C17 C18 0.6(4) . . . . ? N12 N14 C18 C17 -0.5(3) . . . . ? B1 N14 C18 C17 -171.2(3) . . . . ? C16 C17 C18 N14 0.0(3) . . . . ? N15 N13 C19 C110 0.3(3) . . . . ? Fe1 N13 C19 C110 174.2(2) . . . . ? C25 N21 C21 C22 2.1(4) . . . . ? Fe1 N21 C21 C22 -177.0(2) . . . . ? N21 C21 C22 C23 -1.8(4) . . . . ? C21 C22 C23 C24 0.0(4) . . . . ? C22 C23 C24 C25 1.1(4) . . . . ? C22 C23 C24 C212 -178.9(3) . . . . ? C21 N21 C25 C15 178.3(2) . . . . ? Fe1 N21 C25 C15 -2.4(3) . . . . ? C21 N21 C25 C24 -0.9(4) . . . . ? Fe1 N21 C25 C24 178.4(2) . . . . ? N11 C15 C25 N21 1.8(3) . . . . ? C14 C15 C25 N21 -177.3(2) . . . . ? N11 C15 C25 C24 -178.9(2) . . . . ? C14 C15 C25 C24 2.0(4) . . . . ? C23 C24 C25 N21 -0.7(4) . . . . ? C212 C24 C25 N21 179.3(2) . . . . ? C23 C24 C25 C15 -179.9(2) . . . . ? C212 C24 C25 C15 0.1(4) . . . . ? N24 N22 C26 C27 -1.3(3) . . . . ? Fe1 N22 C26 C27 -170.39(19) . . . . ? N22 C26 C27 C28 1.0(3) . . . . ? N22 N24 C28 C27 -0.5(3) . . . . ? B2 N24 C28 C27 -175.4(3) . . . . ? C26 C27 C28 N24 -0.3(3) . . . . ? N25 N23 C29 C210 1.5(3) . . . . ? Fe1 N23 C29 C210 169.76(18) . . . . ? N13 C19 C110 C111 -0.8(3) . . . . ? N13 N15 C111 C110 -0.9(3) . . . . ? B1 N15 C111 C110 170.5(3) . . . . ? C19 C110 C111 N15 1.1(3) . . . . ? C15 C14 C112 C212 1.1(4) . . . . ? C13 C14 C112 C212 -177.7(3) . . . . ? N23 C29 C210 C211 -1.6(3) . . . . ? N23 N25 C211 C210 -0.1(3) . . . . ? B2 N25 C211 C210 169.2(2) . . . . ? C29 C210 C211 N25 1.0(3) . . . . ? C14 C112 C212 C24 0.9(4) . . . . ? C23 C24 C212 C112 178.4(3) . . . . ? C25 C24 C212 C112 -1.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 1.048 _refine_diff_density_min -0.635 _refine_diff_density_rms 0.090 #====================================================================== data_phen4 _database_code_depnum_ccdc_archive 'CCDC 233288' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,2'-Phenanthroline-bis[di(hydro)bis(1-pyrazolyl)borate iron(II) ; _chemical_name_common ;2,2'-Phenanthroline-bis(di(hydro)bis(1-pyrazolyl)borate iron(ii) ; _chemical_melting_point 'not measured' _chemical_formula_moiety 'C24 H24 B2 Fe N10' _chemical_formula_sum 'C24 H24 B2 Fe N10' _chemical_formula_weight 530.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.727(7) _cell_length_b 12.415(8) _cell_length_c 10.712(6) _cell_angle_alpha 67.473(15) _cell_angle_beta 110.377(15) _cell_angle_gamma 93.505(11) _cell_volume 1231.0(13) _cell_formula_units_Z 2 _cell_measurement_temperature 30(2) _cell_measurement_reflns_used 858 _cell_measurement_theta_min 5.178 _cell_measurement_theta_max 58.320 _exptl_crystal_description block _exptl_crystal_colour clear_intense_red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 0.648 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.9090 _exptl_absorpt_correction_T_max 0.9500 _exptl_absorpt_process_details 'XPREP (SHELXTL,1997)' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 2 sets of \w scans each set at different \f and/or 2\q angles and each scan (20s exposure) covering 0.3\% in \w. Crystal to detector distance 4.965. ; _diffrn_ambient_temperature 30(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'micro-focus X-ray source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker ProteumM with Bede Microsource' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 5599 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.1196 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 29.27 _reflns_number_total 5369 _reflns_number_gt 3534 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SMART-NT V6.1 (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0865P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5369 _refine_ls_number_parameters 350 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1259 _refine_ls_R_factor_gt 0.0798 _refine_ls_wR_factor_ref 0.1818 _refine_ls_wR_factor_gt 0.1620 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 -1.23459(7) 0.76514(6) -1.24278(7) 0.00987(18) Uani 1 1 d . . . B1 B -1.3107(5) 0.6689(5) -0.9261(6) 0.0156(11) Uani 1 1 d . . . H11B H -1.208(5) 0.686(4) -0.872(5) 0.013(13) Uiso 1 1 d . . . H12B H -1.372(5) 0.637(4) -0.858(5) 0.011(12) Uiso 1 1 d . . . B2 B -1.3157(6) 0.7254(5) -1.5648(6) 0.0176(12) Uani 1 1 d . . . H21B H -1.292(5) 0.815(5) -1.609(5) 0.017(13) Uiso 1 1 d . . . H22B H -1.341(5) 0.692(5) -1.643(6) 0.021(14) Uiso 1 1 d . . . N11 N -1.0486(4) 0.7864(3) -1.0856(4) 0.0118(8) Uani 1 1 d . . . N12 N -1.2574(4) 0.5961(3) -1.0994(4) 0.0134(8) Uani 1 1 d . . . N13 N -1.3510(4) 0.8460(3) -1.1659(4) 0.0143(8) Uani 1 1 d . . . N14 N -1.3072(4) 0.5773(3) -0.9918(4) 0.0135(8) Uani 1 1 d . . . N15 N -1.3862(4) 0.7866(3) -1.0486(4) 0.0128(8) Uani 1 1 d . . . N21 N -1.1721(4) 0.9344(3) -1.3573(4) 0.0121(8) Uani 1 1 d . . . N22 N -1.4216(4) 0.7581(3) -1.4033(4) 0.0142(8) Uani 1 1 d . . . N23 N -1.1278(4) 0.6785(3) -1.3212(4) 0.0140(8) Uani 1 1 d . . . N24 N -1.4275(4) 0.7122(4) -1.5029(4) 0.0194(9) Uani 1 1 d . . . N25 N -1.1850(4) 0.6558(3) -1.4434(4) 0.0149(8) Uani 1 1 d . . . C11 C -0.9888(4) 0.7121(4) -0.9496(5) 0.0124(9) Uani 1 1 d . . . H11 H -1.0212 0.6371 -0.9185 0.015 Uiso 1 1 calc R . . C12 C -0.8809(4) 0.7392(4) -0.8503(5) 0.0127(9) Uani 1 1 d . . . H12 H -0.8426 0.6843 -0.7536 0.015 Uiso 1 1 calc R . . C13 C -0.8309(4) 0.8460(4) -0.8944(5) 0.0133(9) Uani 1 1 d . . . H13 H -0.7575 0.8660 -0.8286 0.016 Uiso 1 1 calc R . . C14 C -0.8894(4) 0.9260(4) -1.0384(5) 0.0123(9) Uani 1 1 d . . . C15 C -0.9998(4) 0.8922(4) -1.1288(5) 0.0104(9) Uani 1 1 d . . . C16 C -1.2636(4) 0.4965(4) -1.1195(5) 0.0150(10) Uani 1 1 d . . . H16 H -1.2362 0.4852 -1.1892 0.018 Uiso 1 1 calc R . . C17 C -1.3151(5) 0.4110(4) -1.0265(5) 0.0172(10) Uani 1 1 d . . . H17 H -1.3292 0.3329 -1.0191 0.021 Uiso 1 1 calc R . . C18 C -1.3412(5) 0.4662(4) -0.9472(5) 0.0165(10) Uani 1 1 d . . . H18 H -1.3774 0.4315 -0.8729 0.020 Uiso 1 1 calc R . . C19 C -1.4249(5) 0.9493(4) -1.2346(5) 0.0160(10) Uani 1 1 d . . . H19 H -1.4217 1.0087 -1.3213 0.019 Uiso 1 1 calc R . . C21 C -1.2261(5) 1.0040(4) -1.4967(5) 0.0156(10) Uani 1 1 d . . . H21 H -1.3042 0.9819 -1.5546 0.019 Uiso 1 1 calc R . . C22 C -1.1738(5) 1.1082(4) -1.5625(5) 0.0169(10) Uani 1 1 d . . . H22 H -1.2126 1.1520 -1.6635 0.020 Uiso 1 1 calc R . . C23 C -1.0674(5) 1.1457(4) -1.4807(5) 0.0157(10) Uani 1 1 d . . . H23 H -1.0329 1.2175 -1.5229 0.019 Uiso 1 1 calc R . . C24 C -1.0080(5) 1.0759(4) -1.3306(5) 0.0143(10) Uani 1 1 d . . . C25 C -1.0623(4) 0.9702(4) -1.2769(5) 0.0112(9) Uani 1 1 d . . . C26 C -1.5378(5) 0.7396(4) -1.3805(5) 0.0163(10) Uani 1 1 d . . . H26 H -1.5616 0.7620 -1.3158 0.020 Uiso 1 1 calc R . . C27 C -1.6191(5) 0.6824(5) -1.4657(6) 0.0241(12) Uani 1 1 d . . . H27 H -1.7063 0.6594 -1.4710 0.029 Uiso 1 1 calc R . . C28 C -1.5443(5) 0.6672(5) -1.5399(6) 0.0210(11) Uani 1 1 d U . . H28 H -1.5716 0.6303 -1.6071 0.025 Uiso 1 1 calc R . . C29 C -1.0104(5) 0.6129(4) -1.2496(5) 0.0158(10) Uani 1 1 d . . . H29 H -0.9486 0.6110 -1.1600 0.019 Uiso 1 1 calc R . . C110 C -1.5070(5) 0.9576(4) -1.1619(6) 0.0180(10) Uani 1 1 d . . . H110 H -1.5684 1.0211 -1.1874 0.022 Uiso 1 1 calc R . . C111 C -1.4787(4) 0.8532(4) -1.0451(5) 0.0151(10) Uani 1 1 d . . . H111 H -1.5181 0.8311 -0.9729 0.018 Uiso 1 1 calc R . . C112 C -0.8421(5) 1.0380(4) -1.0950(5) 0.0142(10) Uani 1 1 d . . . H112 H -0.7702 1.0627 -1.0327 0.017 Uiso 1 1 calc R . . C210 C -0.9912(5) 0.5478(4) -1.3242(5) 0.0189(11) Uani 1 1 d . . . H210 H -0.9171 0.4950 -1.2970 0.023 Uiso 1 1 calc R . . C211 C -1.1045(5) 0.5780(4) -1.4459(6) 0.0204(11) Uani 1 1 d . . . H211 H -1.1230 0.5487 -1.5198 0.024 Uiso 1 1 calc R . . C212 C -0.8981(5) 1.1100(4) -1.2365(5) 0.0152(10) Uani 1 1 d . . . H212 H -0.8637 1.1833 -1.2725 0.018 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 Fe1 0.0088(3) 0.0115(3) 0.0084(3) -0.0049(2) 0.0011(3) -0.0024(2) B1 0.016(3) 0.015(3) 0.018(3) -0.009(2) 0.006(2) -0.004(2) B2 0.020(3) 0.023(3) 0.014(3) -0.012(2) 0.005(2) -0.003(2) N11 0.0144(19) 0.0086(19) 0.016(2) -0.0070(15) 0.0067(17) -0.0017(14) N12 0.0084(18) 0.018(2) 0.015(2) -0.0090(16) 0.0029(16) -0.0029(15) N13 0.0126(19) 0.013(2) 0.018(2) -0.0088(16) 0.0024(17) -0.0026(15) N14 0.0111(18) 0.016(2) 0.013(2) -0.0064(16) 0.0033(16) -0.0032(15) N15 0.0130(19) 0.014(2) 0.015(2) -0.0092(16) 0.0045(17) -0.0039(15) N21 0.0105(18) 0.016(2) 0.0078(19) -0.0048(16) 0.0006(16) -0.0014(15) N22 0.016(2) 0.019(2) 0.013(2) -0.0107(17) 0.0060(17) -0.0057(16) N23 0.0141(19) 0.017(2) 0.012(2) -0.0067(16) 0.0050(17) -0.0033(15) N24 0.013(2) 0.030(2) 0.016(2) -0.0147(19) -0.0002(18) -0.0039(17) N25 0.018(2) 0.017(2) 0.015(2) -0.0112(17) 0.0066(18) -0.0049(16) C11 0.013(2) 0.010(2) 0.013(2) -0.0030(18) 0.0035(19) 0.0005(17) C12 0.012(2) 0.015(2) 0.012(2) -0.0077(18) 0.0023(19) 0.0010(17) C13 0.012(2) 0.014(2) 0.013(2) -0.0071(18) 0.0022(19) -0.0027(17) C14 0.014(2) 0.009(2) 0.014(2) -0.0040(17) 0.004(2) 0.0011(16) C15 0.012(2) 0.008(2) 0.012(2) -0.0055(17) 0.0023(19) -0.0007(16) C16 0.010(2) 0.021(3) 0.013(2) -0.0114(19) -0.0010(19) -0.0038(18) C17 0.014(2) 0.011(2) 0.025(3) -0.008(2) 0.004(2) -0.0044(18) C18 0.014(2) 0.014(2) 0.020(3) -0.0061(19) 0.006(2) -0.0044(18) C19 0.015(2) 0.014(2) 0.017(2) -0.0088(19) 0.000(2) -0.0027(18) C21 0.013(2) 0.015(2) 0.013(2) -0.0025(19) 0.000(2) 0.0040(18) C22 0.018(2) 0.019(3) 0.010(2) -0.0035(19) 0.004(2) 0.0008(19) C23 0.023(3) 0.012(2) 0.016(2) -0.0044(18) 0.012(2) -0.0018(18) C24 0.017(2) 0.013(2) 0.016(2) -0.0042(19) 0.010(2) -0.0004(18) C25 0.011(2) 0.010(2) 0.013(2) -0.0045(17) 0.0048(19) 0.0010(16) C26 0.013(2) 0.021(3) 0.017(2) -0.011(2) 0.004(2) -0.0020(18) C27 0.013(2) 0.036(3) 0.028(3) -0.021(3) 0.003(2) -0.007(2) C28 0.016(2) 0.030(3) 0.017(2) -0.019(2) -0.0035(19) -0.0033(19) C29 0.013(2) 0.016(2) 0.016(2) -0.0026(19) 0.007(2) -0.0043(18) C110 0.014(2) 0.016(2) 0.026(3) -0.014(2) 0.002(2) -0.0005(18) C111 0.011(2) 0.025(3) 0.018(3) -0.018(2) 0.004(2) -0.0067(18) C112 0.017(2) 0.010(2) 0.019(3) -0.0079(19) 0.008(2) -0.0054(17) C210 0.017(2) 0.016(2) 0.022(3) -0.004(2) 0.010(2) -0.0008(19) C211 0.024(3) 0.019(3) 0.027(3) -0.012(2) 0.017(2) -0.007(2) C212 0.018(2) 0.012(2) 0.017(3) -0.0069(19) 0.007(2) -0.0037(18) _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 N12 2.134(4) . ? Fe1 N22 2.163(4) . ? Fe1 N23 2.166(4) . ? Fe1 N13 2.179(4) . ? Fe1 N21 2.190(4) . ? Fe1 N11 2.196(4) . ? B1 N14 1.558(7) . ? B1 N15 1.565(7) . ? B1 H11B 1.10(5) . ? B1 H12B 1.10(5) . ? B2 N24 1.533(7) . ? B2 N25 1.556(7) . ? B2 H21B 1.08(5) . ? B2 H22B 1.02(5) . ? N11 C11 1.333(6) . ? N11 C15 1.353(6) . ? N12 C16 1.327(6) . ? N12 N14 1.369(5) . ? N13 C19 1.345(6) . ? N13 N15 1.362(5) . ? N14 C18 1.349(6) . ? N15 C111 1.348(6) . ? N21 C21 1.335(6) . ? N21 C25 1.360(6) . ? N22 C26 1.341(6) . ? N22 N24 1.372(6) . ? N23 C29 1.345(6) . ? N23 N25 1.367(6) . ? N24 C28 1.334(6) . ? N25 C211 1.348(6) . ? C11 C12 1.398(6) . ? C11 H11 0.9500 . ? C12 C13 1.370(6) . ? C12 H12 0.9500 . ? C13 C14 1.410(6) . ? C13 H13 0.9500 . ? C14 C15 1.403(6) . ? C14 C112 1.429(6) . ? C15 C25 1.437(6) . ? C16 C17 1.388(7) . ? C16 H16 0.9500 . ? C17 C18 1.379(7) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C110 1.393(7) . ? C19 H19 0.9500 . ? C21 C22 1.404(7) . ? C21 H21 0.9500 . ? C22 C23 1.356(7) . ? C22 H22 0.9500 . ? C23 C24 1.424(6) . ? C23 H23 0.9500 . ? C24 C25 1.398(6) . ? C24 C212 1.423(7) . ? C26 C27 1.401(7) . ? C26 H26 0.9500 . ? C27 C28 1.374(7) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C210 1.402(7) . ? C29 H29 0.9500 . ? C110 C111 1.371(7) . ? C110 H110 0.9500 . ? C111 H111 0.9500 . ? C112 C212 1.360(6) . ? C112 H112 0.9500 . ? C210 C211 1.376(7) . ? C210 H210 0.9500 . ? C211 H211 0.9500 . ? C212 H212 0.9500 . ? 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 N12 Fe1 N22 89.60(15) . . ? N12 Fe1 N23 87.81(15) . . ? N22 Fe1 N23 90.61(15) . . ? N12 Fe1 N13 90.21(15) . . ? N22 Fe1 N13 86.88(15) . . ? N23 Fe1 N13 176.81(15) . . ? N12 Fe1 N21 168.67(14) . . ? N22 Fe1 N21 101.63(15) . . ? N23 Fe1 N21 90.61(15) . . ? N13 Fe1 N21 91.82(15) . . ? N12 Fe1 N11 93.90(15) . . ? N22 Fe1 N11 175.70(15) . . ? N23 Fe1 N11 92.01(15) . . ? N13 Fe1 N11 90.61(15) . . ? N21 Fe1 N11 74.94(14) . . ? N14 B1 N15 110.0(4) . . ? N14 B1 H11B 109(3) . . ? N15 B1 H11B 109(3) . . ? N14 B1 H12B 107(3) . . ? N15 B1 H12B 105(2) . . ? H11B B1 H12B 116(4) . . ? N24 B2 N25 109.8(4) . . ? N24 B2 H21B 114(3) . . ? N25 B2 H21B 106(3) . . ? N24 B2 H22B 110(3) . . ? N25 B2 H22B 108(3) . . ? H21B B2 H22B 109(4) . . ? C11 N11 C15 117.7(4) . . ? C11 N11 Fe1 126.8(3) . . ? C15 N11 Fe1 115.1(3) . . ? C16 N12 N14 106.2(4) . . ? C16 N12 Fe1 127.3(3) . . ? N14 N12 Fe1 124.1(3) . . ? C19 N13 N15 105.8(4) . . ? C19 N13 Fe1 129.1(3) . . ? N15 N13 Fe1 123.5(3) . . ? C18 N14 N12 109.0(4) . . ? C18 N14 B1 127.0(4) . . ? N12 N14 B1 123.9(4) . . ? C111 N15 N13 109.5(4) . . ? C111 N15 B1 126.5(4) . . ? N13 N15 B1 123.2(4) . . ? C21 N21 C25 116.7(4) . . ? C21 N21 Fe1 127.8(3) . . ? C25 N21 Fe1 115.5(3) . . ? C26 N22 N24 106.1(4) . . ? C26 N22 Fe1 124.3(3) . . ? N24 N22 Fe1 121.9(3) . . ? C29 N23 N25 105.6(4) . . ? C29 N23 Fe1 128.7(3) . . ? N25 N23 Fe1 123.9(3) . . ? C28 N24 N22 109.7(4) . . ? C28 N24 B2 128.9(4) . . ? N22 N24 B2 121.2(4) . . ? C211 N25 N23 110.0(4) . . ? C211 N25 B2 127.9(4) . . ? N23 N25 B2 121.7(4) . . ? N11 C11 C12 123.2(4) . . ? N11 C11 H11 118.4 . . ? C12 C11 H11 118.4 . . ? C13 C12 C11 119.1(4) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C12 C13 C14 119.4(4) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C15 C14 C13 117.3(4) . . ? C15 C14 C112 119.3(4) . . ? C13 C14 C112 123.4(4) . . ? N11 C15 C14 123.3(4) . . ? N11 C15 C25 117.2(4) . . ? C14 C15 C25 119.5(4) . . ? N12 C16 C17 111.8(4) . . ? N12 C16 H16 124.1 . . ? C17 C16 H16 124.1 . . ? C18 C17 C16 103.8(4) . . ? C18 C17 H17 128.1 . . ? C16 C17 H17 128.1 . . ? N14 C18 C17 109.3(4) . . ? N14 C18 H18 125.4 . . ? C17 C18 H18 125.4 . . ? N13 C19 C110 111.1(4) . . ? N13 C19 H19 124.4 . . ? C110 C19 H19 124.4 . . ? N21 C21 C22 123.6(4) . . ? N21 C21 H21 118.2 . . ? C22 C21 H21 118.2 . . ? C23 C22 C21 119.4(4) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 119.0(4) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C25 C24 C212 120.1(4) . . ? C25 C24 C23 117.2(4) . . ? C212 C24 C23 122.7(4) . . ? N21 C25 C24 123.8(4) . . ? N21 C25 C15 116.7(4) . . ? C24 C25 C15 119.5(4) . . ? N22 C26 C27 110.4(4) . . ? N22 C26 H26 124.8 . . ? C27 C26 H26 124.8 . . ? C28 C27 C26 104.5(4) . . ? C28 C27 H27 127.8 . . ? C26 C27 H27 127.8 . . ? N24 C28 C27 109.4(4) . . ? N24 C28 H28 125.3 . . ? C27 C28 H28 125.3 . . ? N23 C29 C210 111.2(4) . . ? N23 C29 H29 124.4 . . ? C210 C29 H29 124.4 . . ? C111 C110 C19 104.1(4) . . ? C111 C110 H110 128.0 . . ? C19 C110 H110 128.0 . . ? N15 C111 C110 109.4(4) . . ? N15 C111 H111 125.3 . . ? C110 C111 H111 125.3 . . ? C212 C112 C14 121.2(4) . . ? C212 C112 H112 119.4 . . ? C14 C112 H112 119.4 . . ? C211 C210 C29 104.0(4) . . ? C211 C210 H210 128.0 . . ? C29 C210 H210 128.0 . . ? N25 C211 C210 109.2(5) . . ? N25 C211 H211 125.4 . . ? C210 C211 H211 125.4 . . ? C112 C212 C24 120.2(4) . . ? C112 C212 H212 119.9 . . ? C24 C212 H212 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N12 Fe1 N11 C11 -2.8(4) . . . . ? N22 Fe1 N11 C11 141.8(19) . . . . ? N23 Fe1 N11 C11 -90.7(4) . . . . ? N13 Fe1 N11 C11 87.5(4) . . . . ? N21 Fe1 N11 C11 179.2(4) . . . . ? N12 Fe1 N11 C15 -174.8(3) . . . . ? N22 Fe1 N11 C15 -30(2) . . . . ? N23 Fe1 N11 C15 97.2(3) . . . . ? N13 Fe1 N11 C15 -84.6(3) . . . . ? N21 Fe1 N11 C15 7.1(3) . . . . ? N22 Fe1 N12 C16 61.8(4) . . . . ? N23 Fe1 N12 C16 -28.8(4) . . . . ? N13 Fe1 N12 C16 148.7(4) . . . . ? N21 Fe1 N12 C16 -110.9(8) . . . . ? N11 Fe1 N12 C16 -120.7(4) . . . . ? N22 Fe1 N12 N14 -97.8(3) . . . . ? N23 Fe1 N12 N14 171.6(3) . . . . ? N13 Fe1 N12 N14 -10.9(3) . . . . ? N21 Fe1 N12 N14 89.5(8) . . . . ? N11 Fe1 N12 N14 79.7(3) . . . . ? N12 Fe1 N13 C19 -153.6(4) . . . . ? N22 Fe1 N13 C19 -64.0(4) . . . . ? N23 Fe1 N13 C19 -102(3) . . . . ? N21 Fe1 N13 C19 37.6(4) . . . . ? N11 Fe1 N13 C19 112.5(4) . . . . ? N12 Fe1 N13 N15 10.4(3) . . . . ? N22 Fe1 N13 N15 100.0(3) . . . . ? N23 Fe1 N13 N15 62(3) . . . . ? N21 Fe1 N13 N15 -158.5(3) . . . . ? N11 Fe1 N13 N15 -83.5(3) . . . . ? C16 N12 N14 C18 0.8(5) . . . . ? Fe1 N12 N14 C18 164.0(3) . . . . ? C16 N12 N14 B1 176.1(4) . . . . ? Fe1 N12 N14 B1 -20.7(6) . . . . ? N15 B1 N14 C18 -130.1(5) . . . . ? N15 B1 N14 N12 55.5(6) . . . . ? C19 N13 N15 C111 -0.7(5) . . . . ? Fe1 N13 N15 C111 -167.8(3) . . . . ? C19 N13 N15 B1 -171.3(4) . . . . ? Fe1 N13 N15 B1 21.6(6) . . . . ? N14 B1 N15 C111 135.4(4) . . . . ? N14 B1 N15 N13 -55.7(5) . . . . ? N12 Fe1 N21 C21 163.2(7) . . . . ? N22 Fe1 N21 C21 -9.4(4) . . . . ? N23 Fe1 N21 C21 81.3(4) . . . . ? N13 Fe1 N21 C21 -96.6(4) . . . . ? N11 Fe1 N21 C21 173.2(4) . . . . ? N12 Fe1 N21 C25 -14.4(10) . . . . ? N22 Fe1 N21 C25 173.0(3) . . . . ? N23 Fe1 N21 C25 -96.3(3) . . . . ? N13 Fe1 N21 C25 85.8(3) . . . . ? N11 Fe1 N21 C25 -4.3(3) . . . . ? N12 Fe1 N22 C26 55.4(4) . . . . ? N23 Fe1 N22 C26 143.2(4) . . . . ? N13 Fe1 N22 C26 -34.9(4) . . . . ? N21 Fe1 N22 C26 -126.1(4) . . . . ? N11 Fe1 N22 C26 -89(2) . . . . ? N12 Fe1 N22 N24 -89.7(3) . . . . ? N23 Fe1 N22 N24 -1.9(3) . . . . ? N13 Fe1 N22 N24 -180.0(3) . . . . ? N21 Fe1 N22 N24 88.8(3) . . . . ? N11 Fe1 N22 N24 125.6(19) . . . . ? N12 Fe1 N23 C29 -64.7(4) . . . . ? N22 Fe1 N23 C29 -154.3(4) . . . . ? N13 Fe1 N23 C29 -116(3) . . . . ? N21 Fe1 N23 C29 104.0(4) . . . . ? N11 Fe1 N23 C29 29.1(4) . . . . ? N12 Fe1 N23 N25 97.4(3) . . . . ? N22 Fe1 N23 N25 7.8(3) . . . . ? N13 Fe1 N23 N25 46(3) . . . . ? N21 Fe1 N23 N25 -93.8(3) . . . . ? N11 Fe1 N23 N25 -168.8(3) . . . . ? C26 N22 N24 C28 0.2(5) . . . . ? Fe1 N22 N24 C28 150.7(3) . . . . ? C26 N22 N24 B2 175.3(4) . . . . ? Fe1 N22 N24 B2 -34.2(6) . . . . ? N25 B2 N24 C28 -119.7(5) . . . . ? N25 B2 N24 N22 66.2(6) . . . . ? C29 N23 N25 C211 0.2(5) . . . . ? Fe1 N23 N25 C211 -165.4(3) . . . . ? C29 N23 N25 B2 -173.0(4) . . . . ? Fe1 N23 N25 B2 21.4(6) . . . . ? N24 B2 N25 C211 129.7(5) . . . . ? N24 B2 N25 N23 -58.4(6) . . . . ? C15 N11 C11 C12 1.1(6) . . . . ? Fe1 N11 C11 C12 -170.8(3) . . . . ? N11 C11 C12 C13 -1.6(7) . . . . ? C11 C12 C13 C14 0.1(7) . . . . ? C12 C13 C14 C15 1.8(6) . . . . ? C12 C13 C14 C112 -178.4(4) . . . . ? C11 N11 C15 C14 0.9(6) . . . . ? Fe1 N11 C15 C14 173.8(3) . . . . ? C11 N11 C15 C25 178.1(4) . . . . ? Fe1 N11 C15 C25 -9.1(5) . . . . ? C13 C14 C15 N11 -2.3(7) . . . . ? C112 C14 C15 N11 177.8(4) . . . . ? C13 C14 C15 C25 -179.4(4) . . . . ? C112 C14 C15 C25 0.7(6) . . . . ? N14 N12 C16 C17 -0.7(5) . . . . ? Fe1 N12 C16 C17 -163.2(3) . . . . ? N12 C16 C17 C18 0.4(5) . . . . ? N12 N14 C18 C17 -0.6(5) . . . . ? B1 N14 C18 C17 -175.7(4) . . . . ? C16 C17 C18 N14 0.1(5) . . . . ? N15 N13 C19 C110 0.5(5) . . . . ? Fe1 N13 C19 C110 166.7(3) . . . . ? C25 N21 C21 C22 1.6(7) . . . . ? Fe1 N21 C21 C22 -176.0(4) . . . . ? N21 C21 C22 C23 -4.1(7) . . . . ? C21 C22 C23 C24 2.4(7) . . . . ? C22 C23 C24 C25 1.4(7) . . . . ? C22 C23 C24 C212 -178.6(4) . . . . ? C21 N21 C25 C24 2.6(7) . . . . ? Fe1 N21 C25 C24 -179.5(3) . . . . ? C21 N21 C25 C15 -176.7(4) . . . . ? Fe1 N21 C25 C15 1.2(5) . . . . ? C212 C24 C25 N21 175.9(4) . . . . ? C23 C24 C25 N21 -4.1(7) . . . . ? C212 C24 C25 C15 -4.8(7) . . . . ? C23 C24 C25 C15 175.2(4) . . . . ? N11 C15 C25 N21 5.3(6) . . . . ? C14 C15 C25 N21 -177.4(4) . . . . ? N11 C15 C25 C24 -174.0(4) . . . . ? C14 C15 C25 C24 3.2(6) . . . . ? N24 N22 C26 C27 -0.4(5) . . . . ? Fe1 N22 C26 C27 -150.0(4) . . . . ? N22 C26 C27 C28 0.4(6) . . . . ? N22 N24 C28 C27 0.1(6) . . . . ? B2 N24 C28 C27 -174.5(5) . . . . ? C26 C27 C28 N24 -0.3(6) . . . . ? N25 N23 C29 C210 -0.1(5) . . . . ? Fe1 N23 C29 C210 164.5(3) . . . . ? N13 C19 C110 C111 -0.1(5) . . . . ? N13 N15 C111 C110 0.7(5) . . . . ? B1 N15 C111 C110 170.8(4) . . . . ? C19 C110 C111 N15 -0.3(5) . . . . ? C15 C14 C112 C212 -3.2(7) . . . . ? C13 C14 C112 C212 177.0(4) . . . . ? N23 C29 C210 C211 0.0(5) . . . . ? N23 N25 C211 C210 -0.2(5) . . . . ? B2 N25 C211 C210 172.5(4) . . . . ? C29 C210 C211 N25 0.1(5) . . . . ? C14 C112 C212 C24 1.6(7) . . . . ? C25 C24 C212 C112 2.4(7) . . . . ? C23 C24 C212 C112 -177.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.799 _diffrn_reflns_theta_full 29.27 _diffrn_measured_fraction_theta_full 0.799 _refine_diff_density_max 1.152 _refine_diff_density_min -0.999 _refine_diff_density_rms 0.110 #======================================================================