# Supplementary Material (ESI) for Chemical Science # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Chemical Science' _journal_coden_Cambridge 1475 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Matthew Shores' _publ_contact_author_email shores@lamar.colostate.edu _publ_section_title ; Ambient Temperature Anion-Dependent Spin State Switching Observed in Mostly Low Spin Heteroleptic Iron(II) Diimine Complexes ; loop_ _publ_author_name 'Zhaoping Na.' 'Ashley McDaniel' 'Matthew Shores' # Attachment '- 1-4.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 768562' #TrackingRef '- 1-4.cif' _audit_creation_method 'Bruker SHELXTL' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H28 Br2 Fe N8' _chemical_formula_sum 'C16 H28 Br2 Fe N8' _chemical_formula_weight 548.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.5341(6) _cell_length_b 16.1645(12) _cell_length_c 13.7170(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.539(4) _cell_angle_gamma 90.00 _cell_volume 2113.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6522 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 26.32 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.477 _exptl_crystal_size_mid 0.356 _exptl_crystal_size_min 0.344 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 4.513 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.14 _exptl_absorpt_correction_T_max 0.22 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17319 _diffrn_reflns_av_R_equivalents 0.0814 _diffrn_reflns_av_sigmaI/netI 0.0694 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 24.71 _reflns_number_total 3589 _reflns_number_gt 2606 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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. The crystal used for compound 1 is monoclinic with beta ~ 90 degree and showed signs of pseudomerohedral twinning. Both components of the twinned crystal were related by a two-fold rotation around the a axis, requiring the twin law 1 0 0 0 -1 0 0 0 -1 to give a successful refinement. The two components refined to an 80:20 ratio. ; _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^)+(0.1150P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3589 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0845 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1954 _refine_ls_wR_factor_gt 0.1574 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 1.03684(15) 0.24734(9) 0.53234(11) 0.0344(4) Uani 1 1 d . . . N1 N 1.0155(8) 0.2101(5) 0.3846(6) 0.036(2) Uani 1 1 d . . . N2 N 0.9408(10) 0.2580(6) 0.2297(6) 0.046(2) Uani 1 1 d . . . H2 H 0.8929 0.2946 0.1982 0.056 Uiso 1 1 calc R . . N3 N 0.7780(11) 0.3756(5) 0.3238(7) 0.045(2) Uani 1 1 d . . . H3 H 0.7757 0.3704 0.2614 0.054 Uiso 1 1 calc R . . N4 N 0.8847(8) 0.3313(5) 0.4731(6) 0.0339(19) Uani 1 1 d . . . C1 C 1.0903(13) 0.1418(7) 0.3372(9) 0.046(3) Uani 1 1 d . . . H1A H 1.0881 0.0936 0.3793 0.055 Uiso 1 1 calc R . . H1B H 1.1877 0.1575 0.3288 0.055 Uiso 1 1 calc R . . C2 C 1.0279(13) 0.1193(8) 0.2392(10) 0.057(4) Uani 1 1 d . . . H2A H 1.0871 0.0787 0.2078 0.068 Uiso 1 1 calc R . . H2B H 0.9361 0.0949 0.2482 0.068 Uiso 1 1 calc R . . C3 C 1.0148(12) 0.1945(8) 0.1752(9) 0.050(3) Uani 1 1 d . . . H3A H 1.1071 0.2142 0.1572 0.060 Uiso 1 1 calc R . . H3B H 0.9632 0.1809 0.1161 0.060 Uiso 1 1 calc R . . C4 C 0.9450(10) 0.2613(6) 0.3282(8) 0.038(3) Uani 1 1 d . . . C5 C 0.8642(10) 0.3276(6) 0.3786(8) 0.032(2) Uani 1 1 d . . . C6 C 0.6885(11) 0.4368(7) 0.3721(9) 0.045(3) Uani 1 1 d . . . H6A H 0.7315 0.4910 0.3677 0.054 Uiso 1 1 calc R . . H6B H 0.5982 0.4391 0.3390 0.054 Uiso 1 1 calc R . . C7 C 0.6677(12) 0.4157(7) 0.4748(10) 0.050(3) Uani 1 1 d . . . H7A H 0.6064 0.3680 0.4793 0.060 Uiso 1 1 calc R . . H7B H 0.6226 0.4616 0.5076 0.060 Uiso 1 1 calc R . . C8 C 0.8093(12) 0.3963(7) 0.5259(9) 0.046(3) Uani 1 1 d . . . H8A H 0.8662 0.4460 0.5286 0.055 Uiso 1 1 calc R . . H8B H 0.7924 0.3783 0.5922 0.055 Uiso 1 1 calc R . . N5 N 1.0246(9) 0.2870(6) 0.6805(7) 0.036(2) Uani 1 1 d . . . N6 N 0.9426(10) 0.2481(6) 0.8338(6) 0.045(2) Uani 1 1 d . . . H6 H 0.8900 0.2148 0.8658 0.054 Uiso 1 1 calc R . . N7 N 0.7850(11) 0.1241(6) 0.7423(8) 0.052(3) Uani 1 1 d . . . H7 H 0.7834 0.1314 0.8044 0.062 Uiso 1 1 calc R . . N8 N 0.8886(8) 0.1655(5) 0.5963(6) 0.0337(19) Uani 1 1 d . . . C9 C 1.1017(12) 0.3568(7) 0.7239(9) 0.047(3) Uani 1 1 d . . . H9A H 1.0992 0.4032 0.6791 0.057 Uiso 1 1 calc R . . H9B H 1.1990 0.3410 0.7336 0.057 Uiso 1 1 calc R . . C10 C 1.0405(14) 0.3838(8) 0.8214(10) 0.055(3) Uani 1 1 d . . . H10A H 1.1030 0.4235 0.8522 0.066 Uiso 1 1 calc R . . H10B H 0.9509 0.4106 0.8102 0.066 Uiso 1 1 calc R . . C11 C 1.0214(13) 0.3125(8) 0.8867(9) 0.053(3) Uani 1 1 d . . . H11A H 1.1119 0.2911 0.9073 0.064 Uiso 1 1 calc R . . H11B H 0.9702 0.3293 0.9442 0.064 Uiso 1 1 calc R . . C12 C 0.9509(11) 0.2403(6) 0.7367(7) 0.031(2) Uani 1 1 d . . . C13 C 0.8703(10) 0.1726(6) 0.6881(8) 0.033(2) Uani 1 1 d . . . C14 C 0.6965(12) 0.0608(7) 0.6998(8) 0.047(3) Uani 1 1 d . . . H14A H 0.6064 0.0603 0.7320 0.057 Uiso 1 1 calc R . . H14B H 0.7398 0.0070 0.7086 0.057 Uiso 1 1 calc R . . C15 C 0.6764(12) 0.0780(7) 0.5941(9) 0.049(3) Uani 1 1 d . . . H15A H 0.6125 0.1242 0.5859 0.058 Uiso 1 1 calc R . . H15B H 0.6347 0.0300 0.5627 0.058 Uiso 1 1 calc R . . C16 C 0.8141(11) 0.0980(7) 0.5460(8) 0.041(3) Uani 1 1 d . . . H16A H 0.8728 0.0490 0.5459 0.049 Uiso 1 1 calc R . . H16B H 0.7966 0.1138 0.4787 0.049 Uiso 1 1 calc R . . Br1 Br 1.23726(13) 0.35975(6) 0.48462(8) 0.0432(3) Uani 1 1 d . . . Br2 Br 1.23616(13) 0.12574(7) 0.57849(8) 0.0467(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0335(7) 0.0395(8) 0.0303(8) -0.0024(6) -0.0002(7) -0.0007(7) N1 0.034(5) 0.041(5) 0.034(5) -0.004(4) -0.005(4) 0.003(4) N2 0.044(5) 0.065(7) 0.030(5) -0.002(5) -0.005(4) 0.014(5) N3 0.053(6) 0.046(5) 0.038(5) 0.004(4) -0.001(5) 0.017(5) N4 0.036(5) 0.033(5) 0.033(5) -0.004(4) 0.000(4) 0.005(4) C1 0.044(7) 0.046(7) 0.046(7) -0.004(5) -0.009(6) 0.016(5) C2 0.045(7) 0.057(8) 0.069(9) -0.028(7) -0.002(7) 0.014(6) C3 0.046(7) 0.065(9) 0.041(7) -0.007(6) 0.000(5) 0.017(6) C4 0.023(5) 0.038(6) 0.051(7) -0.001(5) -0.006(5) -0.009(4) C5 0.026(5) 0.026(5) 0.045(6) 0.003(5) 0.006(4) -0.006(4) C6 0.043(6) 0.037(6) 0.056(8) 0.005(6) 0.006(5) 0.017(5) C7 0.041(6) 0.045(7) 0.064(8) -0.005(6) 0.008(6) 0.002(5) C8 0.049(7) 0.040(6) 0.050(7) -0.012(6) 0.009(6) 0.006(5) N5 0.035(5) 0.043(5) 0.030(5) 0.005(4) -0.005(4) -0.001(4) N6 0.044(5) 0.060(6) 0.031(5) 0.000(5) -0.004(4) -0.019(5) N7 0.055(7) 0.062(7) 0.039(5) 0.000(5) 0.004(5) -0.027(5) N8 0.031(4) 0.036(5) 0.035(5) -0.004(4) 0.001(4) -0.004(4) C9 0.039(7) 0.054(8) 0.049(7) -0.011(6) 0.013(5) -0.017(5) C10 0.051(8) 0.060(8) 0.055(8) -0.020(7) 0.001(6) -0.006(6) C11 0.053(7) 0.065(8) 0.041(7) -0.008(6) 0.008(6) -0.012(6) C12 0.028(5) 0.039(6) 0.026(5) 0.006(5) -0.004(4) -0.004(4) C13 0.032(5) 0.034(6) 0.032(6) -0.001(5) 0.004(4) -0.003(5) C14 0.047(7) 0.040(7) 0.055(8) -0.003(6) 0.008(5) -0.014(5) C15 0.051(7) 0.043(7) 0.051(8) -0.001(6) 0.001(6) -0.013(5) C16 0.043(6) 0.037(6) 0.043(7) 0.003(5) -0.006(5) -0.005(5) Br1 0.0432(7) 0.0428(6) 0.0439(6) -0.0054(5) 0.0098(5) -0.0057(5) Br2 0.0452(7) 0.0504(7) 0.0445(7) -0.0071(5) -0.0074(6) 0.0049(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 2.122(9) . ? Fe1 N8 2.130(8) . ? Fe1 N5 2.135(9) . ? Fe1 N4 2.141(8) . ? Fe1 Br1 2.7212(18) . ? Fe1 Br2 2.8023(18) . ? N1 C4 1.313(14) . ? N1 C1 1.469(13) . ? N2 C4 1.352(14) . ? N2 C3 1.456(14) . ? N2 H2 0.8600 . ? N3 C5 1.354(14) . ? N3 C6 1.468(14) . ? N3 H3 0.8600 . ? N4 C5 1.310(14) . ? N4 C8 1.467(13) . ? C1 C2 1.509(18) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.503(18) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.493(15) . ? C6 C7 1.464(17) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.547(17) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? N5 C12 1.291(13) . ? N5 C9 1.469(14) . ? N6 C12 1.341(13) . ? N6 C11 1.470(14) . ? N6 H6 0.8600 . ? N7 C13 1.357(14) . ? N7 C14 1.445(14) . ? N7 H7 0.8600 . ? N8 C13 1.278(13) . ? N8 C16 1.471(13) . ? C9 C10 1.527(17) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.472(18) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.491(14) . ? C14 C15 1.487(17) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.510(15) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? 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 N8 99.2(3) . . ? N1 Fe1 N5 171.3(3) . . ? N8 Fe1 N5 75.6(3) . . ? N1 Fe1 N4 76.1(3) . . ? N8 Fe1 N4 95.8(3) . . ? N5 Fe1 N4 97.3(3) . . ? N1 Fe1 Br1 91.2(2) . . ? N8 Fe1 Br1 169.6(2) . . ? N5 Fe1 Br1 94.2(2) . . ? N4 Fe1 Br1 87.7(2) . . ? N1 Fe1 Br2 94.3(2) . . ? N8 Fe1 Br2 85.6(2) . . ? N5 Fe1 Br2 92.2(2) . . ? N4 Fe1 Br2 170.4(2) . . ? Br1 Fe1 Br2 92.66(6) . . ? C4 N1 C1 117.4(9) . . ? C4 N1 Fe1 115.3(7) . . ? C1 N1 Fe1 126.4(7) . . ? C4 N2 C3 122.0(9) . . ? C4 N2 H2 119.0 . . ? C3 N2 H2 119.0 . . ? C5 N3 C6 119.2(9) . . ? C5 N3 H3 120.4 . . ? C6 N3 H3 120.4 . . ? C5 N4 C8 116.9(9) . . ? C5 N4 Fe1 116.1(7) . . ? C8 N4 Fe1 126.9(7) . . ? N1 C1 C2 112.7(9) . . ? N1 C1 H1A 109.0 . . ? C2 C1 H1A 109.0 . . ? N1 C1 H1B 109.0 . . ? C2 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? C3 C2 C1 110.8(10) . . ? C3 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? N2 C3 C2 108.0(10) . . ? N2 C3 H3A 110.1 . . ? C2 C3 H3A 110.1 . . ? N2 C3 H3B 110.1 . . ? C2 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? N1 C4 N2 125.1(10) . . ? N1 C4 C5 116.2(10) . . ? N2 C4 C5 118.7(10) . . ? N4 C5 N3 127.3(9) . . ? N4 C5 C4 114.8(9) . . ? N3 C5 C4 117.9(9) . . ? C7 C6 N3 111.2(9) . . ? C7 C6 H6A 109.4 . . ? N3 C6 H6A 109.4 . . ? C7 C6 H6B 109.4 . . ? N3 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C6 C7 C8 111.0(10) . . ? C6 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? C6 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? N4 C8 C7 110.5(10) . . ? N4 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C12 N5 C9 118.7(9) . . ? C12 N5 Fe1 115.3(7) . . ? C9 N5 Fe1 125.8(7) . . ? C12 N6 C11 121.5(9) . . ? C12 N6 H6 119.3 . . ? C11 N6 H6 119.3 . . ? C13 N7 C14 122.6(10) . . ? C13 N7 H7 118.7 . . ? C14 N7 H7 118.7 . . ? C13 N8 C16 117.3(9) . . ? C13 N8 Fe1 116.6(7) . . ? C16 N8 Fe1 125.9(7) . . ? N5 C9 C10 112.4(9) . . ? N5 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? N5 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C9 111.1(10) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? N6 C11 C10 108.6(10) . . ? N6 C11 H11A 110.0 . . ? C10 C11 H11A 110.0 . . ? N6 C11 H11B 110.0 . . ? C10 C11 H11B 110.0 . . ? H11A C11 H11B 108.3 . . ? N5 C12 N6 125.1(10) . . ? N5 C12 C13 116.3(9) . . ? N6 C12 C13 118.6(9) . . ? N8 C13 N7 125.2(10) . . ? N8 C13 C12 115.6(9) . . ? N7 C13 C12 119.2(9) . . ? N7 C14 C15 109.3(9) . . ? N7 C14 H14A 109.8 . . ? C15 C14 H14A 109.8 . . ? N7 C14 H14B 109.8 . . ? C15 C14 H14B 109.8 . . ? H14A C14 H14B 108.3 . . ? C14 C15 C16 111.2(10) . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? N8 C16 C15 111.8(9) . . ? N8 C16 H16A 109.2 . . ? C15 C16 H16A 109.2 . . ? N8 C16 H16B 109.2 . . ? C15 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N6 H6 Br1 0.86 2.50 3.351(9) 168.4 4_566 N7 H7 Br1 0.86 2.52 3.370(10) 169.9 4_566 N2 H2 Br2 0.86 2.56 3.400(9) 166.4 4_565 N3 H3 Br2 0.86 2.53 3.385(10) 170.0 4_565 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.838 _refine_diff_density_min -0.874 _refine_diff_density_rms 0.117 #===END data_2-BPh4 _database_code_depnum_ccdc_archive 'CCDC 768563' #TrackingRef '- 1-4.cif' _audit_creation_method 'Bruker SHELXTL' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H40 Fe N10, 2(C24 H20 B)' _chemical_formula_sum 'C73 H80 B2 Fe N10' _chemical_formula_weight 1174.94 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 ' _symmetry_space_group_name_Hall ' -P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.1775(3) _cell_length_b 13.2415(3) _cell_length_c 18.3584(4) _cell_angle_alpha 93.4600(10) _cell_angle_beta 97.3300(10) _cell_angle_gamma 90.4710(10) _cell_volume 3170.98(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9807 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 31.13 _exptl_crystal_description slide _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.231 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 0.289 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9172 _exptl_absorpt_correction_T_max 0.9694 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63462 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 26.37 _reflns_number_total 12941 _reflns_number_gt 9498 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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. Responding to errors on checkcif: B: Isotropic non-H atoms in main residues....3. We refined the C23-C25 atoms on the pipi ligand with isotropic displacement parameters because of positional disorder. The occupancy of the main part is 57%. Due to the partial occupancy, atom C24 has large thermal parameters (Ueq = 0.07), which also results in a level C error: Large Non-solvent C Ueq(max)/Ueq(min)...3.03 ratio. ; _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^)+(0.0804P)^2^+6.6373P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12941 _refine_ls_number_parameters 777 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0983 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.1928 _refine_ls_wR_factor_gt 0.1735 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.25830(4) 0.27413(4) 0.73886(3) 0.02764(14) Uani 1 1 d . A . N1 N 0.15976(19) 0.19736(19) 0.78703(14) 0.0239(6) Uani 1 1 d . . . N2 N 0.1405(2) 0.0450(2) 0.84562(16) 0.0338(7) Uani 1 1 d . . . H2 H 0.1691 -0.0107 0.8615 0.041 Uiso 1 1 calc R . . N3 N 0.3412(2) 0.0004(2) 0.81641(18) 0.0383(7) Uani 1 1 d . . . H3 H 0.3015 -0.0478 0.8287 0.046 Uiso 1 1 calc R . . N4 N 0.3489(2) 0.1646(2) 0.77552(16) 0.0347(7) Uani 1 1 d . . . N5 N 0.22984(19) 0.19286(18) 0.64394(14) 0.0216(5) Uani 1 1 d . . . N6 N 0.2927(2) 0.1546(2) 0.53166(18) 0.0381(7) Uani 1 1 d . . . H6 H 0.3349 0.1725 0.5011 0.046 Uiso 1 1 calc R . . N7 N 0.4290(2) 0.3217(2) 0.57004(18) 0.0350(7) Uani 1 1 d . . . H7 H 0.4318 0.2849 0.5288 0.042 Uiso 1 1 calc R . . N8 N 0.3613(2) 0.3326(2) 0.68284(17) 0.0327(7) Uani 1 1 d . . . N9 N 0.1621(2) 0.3803(2) 0.71011(15) 0.0265(6) Uani 1 1 d . A . N10 N 0.2881(3) 0.3693(3) 0.82425(18) 0.0470(9) Uani 1 1 d . . . C1 C 0.0592(3) 0.2331(3) 0.8019(2) 0.0378(8) Uani 1 1 d . . . H1A H 0.0096 0.2214 0.7568 0.045 Uiso 1 1 calc R . . H1B H 0.0635 0.3068 0.8147 0.045 Uiso 1 1 calc R . . C2 C 0.0196(3) 0.1787(3) 0.8657(2) 0.0436(9) Uani 1 1 d . . . H2A H 0.0579 0.2037 0.9134 0.052 Uiso 1 1 calc R . . H2B H -0.0538 0.1928 0.8669 0.052 Uiso 1 1 calc R . . C3 C 0.0346(3) 0.0672(3) 0.8532(2) 0.0365(8) Uani 1 1 d . . . H3A H 0.0140 0.0319 0.8952 0.044 Uiso 1 1 calc R . . H3B H -0.0097 0.0416 0.8081 0.044 Uiso 1 1 calc R . . C4 C 0.1930(3) 0.1130(2) 0.81338(17) 0.0282(7) Uani 1 1 d . . . C5 C 0.3011(3) 0.0920(3) 0.80139(19) 0.0322(8) Uani 1 1 d . . . C6 C 0.4503(3) -0.0195(3) 0.8125(2) 0.0459(10) Uani 1 1 d . . . H6A H 0.4590 -0.0531 0.7641 0.055 Uiso 1 1 calc R . . H6B H 0.4769 -0.0647 0.8513 0.055 Uiso 1 1 calc R . . C7 C 0.5076(3) 0.0797(3) 0.8230(3) 0.0479(10) Uani 1 1 d . . . H7A H 0.5799 0.0693 0.8153 0.058 Uiso 1 1 calc R . . H7B H 0.5064 0.1089 0.8738 0.058 Uiso 1 1 calc R . . C8 C 0.4569(3) 0.1525(3) 0.7674(3) 0.0481(10) Uani 1 1 d . . . H8A H 0.4924 0.2192 0.7754 0.058 Uiso 1 1 calc R . . H8B H 0.4635 0.1256 0.7167 0.058 Uiso 1 1 calc R . . C9 C 0.1531(3) 0.1111(2) 0.62773(19) 0.0291(7) Uani 1 1 d . . . H9A H 0.0891 0.1333 0.6464 0.035 Uiso 1 1 calc R . . H9B H 0.1778 0.0516 0.6545 0.035 Uiso 1 1 calc R . . C10 C 0.1299(3) 0.0802(3) 0.5482(2) 0.0394(9) Uani 1 1 d . . . H10A H 0.0908 0.0154 0.5424 0.047 Uiso 1 1 calc R . . H10B H 0.0863 0.1318 0.5235 0.047 Uiso 1 1 calc R . . C11 C 0.2238(3) 0.0679(3) 0.5118(2) 0.0490(11) Uani 1 1 d . . . H11A H 0.2588 0.0053 0.5270 0.059 Uiso 1 1 calc R . . H11B H 0.2049 0.0616 0.4577 0.059 Uiso 1 1 calc R . . C12 C 0.2922(2) 0.2071(2) 0.59587(18) 0.0241(7) Uani 1 1 d . . . C13 C 0.3659(2) 0.2921(2) 0.61724(18) 0.0270(7) Uani 1 1 d . . . C14 C 0.4924(3) 0.4127(3) 0.5853(2) 0.0455(10) Uani 1 1 d . . . H14A H 0.5558 0.4049 0.5619 0.055 Uiso 1 1 calc R . . H14B H 0.4550 0.4716 0.5653 0.055 Uiso 1 1 calc R . . C15 C 0.5176(3) 0.4284(4) 0.6645(2) 0.0536(12) Uani 1 1 d . . . H15A H 0.5513 0.4956 0.6758 0.064 Uiso 1 1 calc R . . H15B H 0.5675 0.3768 0.6818 0.064 Uiso 1 1 calc R . . C16 C 0.4268(3) 0.4229(3) 0.7069(2) 0.0493(10) Uani 1 1 d . . . H16A H 0.4516 0.4209 0.7601 0.059 Uiso 1 1 calc R . . H16B H 0.3856 0.4846 0.7000 0.059 Uiso 1 1 calc R . . C17 C 0.0920(3) 0.3832(3) 0.64835(19) 0.0302(7) Uani 1 1 d . . . H17 H 0.0865 0.3270 0.6133 0.036 Uiso 1 1 calc R . . C18 C 0.0284(3) 0.4654(3) 0.6350(2) 0.0426(9) Uani 1 1 d . . . H18 H -0.0157 0.4667 0.5899 0.051 Uiso 1 1 calc R . . C19 C 0.0294(3) 0.5437(3) 0.6864(3) 0.0497(11) Uani 1 1 d . . . H19 H -0.0180 0.5970 0.6796 0.060 Uiso 1 1 calc R . . C20 C 0.1004(3) 0.5445(3) 0.7487(2) 0.0451(10) Uani 1 1 d . A . H20 H 0.1051 0.6004 0.7841 0.054 Uiso 1 1 calc R . . C21 C 0.1640(3) 0.4636(3) 0.7588(2) 0.0351(8) Uani 1 1 d . . . C22 C 0.2389(4) 0.4533(3) 0.8225(2) 0.0468(10) Uani 1 1 d . A . H22A H 0.2512 0.5051 0.8607 0.056 Uiso 0.433(13) 1 calc PR A 1 H22B H 0.2510 0.5041 0.8599 0.056 Uiso 0.567(13) 1 d PR A 2 C23A C 0.3328(10) 0.3535(9) 0.8992(6) 0.058(3) Uiso 0.433(13) 1 d PD A 1 H23A H 0.3613 0.2838 0.8967 0.070 Uiso 0.433(13) 1 calc PR A 1 C24A C 0.2623(11) 0.3525(11) 0.9598(8) 0.070(4) Uiso 0.433(13) 1 d PD A 1 H24A H 0.2284 0.4178 0.9637 0.106 Uiso 0.433(13) 1 calc PR A 1 H24B H 0.3030 0.3405 1.0069 0.106 Uiso 0.433(13) 1 calc PR A 1 H24C H 0.2106 0.2984 0.9474 0.106 Uiso 0.433(13) 1 calc PR A 1 C25A C 0.4205(10) 0.4191(11) 0.9271(8) 0.062(4) Uiso 0.433(13) 1 d PD A 1 H25A H 0.4449 0.4043 0.9779 0.093 Uiso 0.433(13) 1 calc PR A 1 H25B H 0.4001 0.4900 0.9255 0.093 Uiso 0.433(13) 1 calc PR A 1 H25C H 0.4754 0.4070 0.8964 0.093 Uiso 0.433(13) 1 calc PR A 1 C23B C 0.3736(6) 0.3495(5) 0.8847(4) 0.038(2) Uiso 0.567(13) 1 d PD A 2 H23B H 0.4210 0.2978 0.8668 0.046 Uiso 0.567(13) 1 calc PR A 2 C24B C 0.3177(7) 0.3083(7) 0.9432(5) 0.055(3) Uiso 0.567(13) 1 d PD A 2 H24D H 0.2675 0.3575 0.9573 0.083 Uiso 0.567(13) 1 calc PR A 2 H24E H 0.3668 0.2956 0.9863 0.083 Uiso 0.567(13) 1 calc PR A 2 H24F H 0.2825 0.2448 0.9242 0.083 Uiso 0.567(13) 1 calc PR A 2 C25B C 0.4331(5) 0.4468(5) 0.9141(4) 0.0273(16) Uiso 0.567(13) 1 d PD A 2 H25D H 0.4693 0.4724 0.8754 0.041 Uiso 0.567(13) 1 calc PR A 2 H25E H 0.4826 0.4323 0.9565 0.041 Uiso 0.567(13) 1 calc PR A 2 H25F H 0.3852 0.4979 0.9292 0.041 Uiso 0.567(13) 1 calc PR A 2 B1 B 0.2610(3) 0.7509(3) 0.4941(2) 0.0260(8) Uani 1 1 d . . . B2 B 0.7720(3) 0.2262(3) 0.0344(2) 0.0271(8) Uani 1 1 d . . . C26 C 0.2387(2) 0.8246(2) 0.42456(17) 0.0224(6) Uani 1 1 d . . . C27 C 0.3149(3) 0.8480(2) 0.38121(18) 0.0278(7) Uani 1 1 d . . . H27 H 0.3807 0.8197 0.3923 0.033 Uiso 1 1 calc R . . C28 C 0.2989(3) 0.9104(3) 0.32290(19) 0.0320(7) Uani 1 1 d . . . H28 H 0.3535 0.9249 0.2958 0.038 Uiso 1 1 calc R . . C29 C 0.2036(3) 0.9516(3) 0.30403(18) 0.0308(7) Uani 1 1 d . . . H29 H 0.1922 0.9948 0.2644 0.037 Uiso 1 1 calc R . . C30 C 0.1251(3) 0.9285(3) 0.34416(18) 0.0299(7) Uani 1 1 d . . . H30 H 0.0589 0.9551 0.3316 0.036 Uiso 1 1 calc R . . C31 C 0.1432(2) 0.8665(2) 0.40295(18) 0.0261(7) Uani 1 1 d . . . H31 H 0.0882 0.8519 0.4296 0.031 Uiso 1 1 calc R . . C32 C 0.1795(3) 0.7743(2) 0.55411(18) 0.0278(7) Uani 1 1 d . . . C33 C 0.0779(3) 0.7387(3) 0.5391(2) 0.0356(8) Uani 1 1 d . . . H33 H 0.0580 0.6983 0.4950 0.043 Uiso 1 1 calc R . . C34 C 0.0052(3) 0.7604(3) 0.5862(2) 0.0425(9) Uani 1 1 d . . . H34 H -0.0631 0.7359 0.5734 0.051 Uiso 1 1 calc R . . C35 C 0.0319(3) 0.8175(3) 0.6516(2) 0.0454(10) Uani 1 1 d . . . H35 H -0.0176 0.8332 0.6837 0.054 Uiso 1 1 calc R . . C36 C 0.1318(3) 0.8512(3) 0.6694(2) 0.0394(9) Uani 1 1 d . . . H36 H 0.1518 0.8888 0.7148 0.047 Uiso 1 1 calc R . . C37 C 0.2037(3) 0.8302(3) 0.62120(19) 0.0328(8) Uani 1 1 d . . . H37 H 0.2718 0.8550 0.6345 0.039 Uiso 1 1 calc R . . C38 C 0.3788(2) 0.7725(2) 0.53666(18) 0.0270(7) Uani 1 1 d . . . C39 C 0.4265(3) 0.8686(3) 0.54167(19) 0.0320(7) Uani 1 1 d . . . H39 H 0.3916 0.9215 0.5169 0.038 Uiso 1 1 calc R . . C40 C 0.5225(3) 0.8898(3) 0.5812(2) 0.0348(8) Uani 1 1 d . . . H40 H 0.5509 0.9563 0.5834 0.042 Uiso 1 1 calc R . . C41 C 0.5766(3) 0.8147(3) 0.61708(19) 0.0354(8) Uani 1 1 d . . . H41 H 0.6423 0.8285 0.6438 0.042 Uiso 1 1 calc R . . C42 C 0.5335(3) 0.7196(3) 0.6134(2) 0.0397(9) Uani 1 1 d . . . H42 H 0.5700 0.6668 0.6373 0.048 Uiso 1 1 calc R . . C43 C 0.4364(3) 0.6998(3) 0.5748(2) 0.0359(8) Uani 1 1 d . . . H43 H 0.4081 0.6336 0.5745 0.043 Uiso 1 1 calc R . . C44 C 0.2449(2) 0.6320(2) 0.4626(2) 0.0296(7) Uani 1 1 d . . . C45 C 0.2337(3) 0.5543(3) 0.5106(2) 0.0364(8) Uani 1 1 d . . . H45 H 0.2328 0.5721 0.5614 0.044 Uiso 1 1 calc R . . C46 C 0.2239(3) 0.4530(3) 0.4862(3) 0.0428(10) Uani 1 1 d . . . H46 H 0.2165 0.4030 0.5202 0.051 Uiso 1 1 calc R . . C47 C 0.2249(3) 0.4245(3) 0.4127(3) 0.0448(10) Uani 1 1 d . . . H47 H 0.2205 0.3550 0.3962 0.054 Uiso 1 1 calc R . . C48 C 0.2322(3) 0.4981(3) 0.3635(3) 0.0437(10) Uani 1 1 d . . . H48 H 0.2311 0.4795 0.3126 0.052 Uiso 1 1 calc R . . C49 C 0.2413(3) 0.6002(3) 0.3886(2) 0.0344(8) Uani 1 1 d . . . H49 H 0.2452 0.6497 0.3537 0.041 Uiso 1 1 calc R . . C50 C 0.7406(3) 0.2852(3) -0.04176(18) 0.0295(7) Uani 1 1 d . . . C51 C 0.7386(3) 0.2405(3) -0.11261(18) 0.0301(7) Uani 1 1 d . . . H51 H 0.7500 0.1699 -0.1185 0.036 Uiso 1 1 calc R . . C52 C 0.7203(3) 0.2958(3) -0.1751(2) 0.0436(10) Uani 1 1 d . . . H52 H 0.7195 0.2623 -0.2225 0.052 Uiso 1 1 calc R . . C53 C 0.7036(3) 0.3979(3) -0.1692(2) 0.0423(9) Uani 1 1 d . . . H53 H 0.6917 0.4353 -0.2120 0.051 Uiso 1 1 calc R . . C54 C 0.7043(4) 0.4456(3) -0.0998(2) 0.0540(12) Uani 1 1 d . . . H54 H 0.6924 0.5161 -0.0945 0.065 Uiso 1 1 calc R . . C55 C 0.7225(4) 0.3895(3) -0.0384(2) 0.0545(12) Uani 1 1 d . . . H55 H 0.7226 0.4235 0.0087 0.065 Uiso 1 1 calc R . . C56 C 0.6899(3) 0.2550(2) 0.09316(17) 0.0264(7) Uani 1 1 d . . . C57 C 0.5858(3) 0.2681(3) 0.06903(19) 0.0361(8) Uani 1 1 d . . . H57 H 0.5636 0.2626 0.0176 0.043 Uiso 1 1 calc R . . C58 C 0.5135(3) 0.2887(3) 0.1167(2) 0.0407(9) Uani 1 1 d . . . H58 H 0.4437 0.2964 0.0976 0.049 Uiso 1 1 calc R . . C59 C 0.5434(3) 0.2979(3) 0.1920(2) 0.0383(9) Uani 1 1 d . . . H59 H 0.4947 0.3131 0.2249 0.046 Uiso 1 1 calc R . . C60 C 0.6446(3) 0.2849(3) 0.21842(19) 0.0344(8) Uani 1 1 d . . . H60 H 0.6659 0.2902 0.2699 0.041 Uiso 1 1 calc R . . C61 C 0.7159(3) 0.2639(2) 0.17000(18) 0.0285(7) Uani 1 1 d . . . H61 H 0.7852 0.2552 0.1898 0.034 Uiso 1 1 calc R . . C62 C 0.8896(3) 0.2614(2) 0.06955(18) 0.0305(7) Uani 1 1 d . . . C63 C 0.9432(4) 0.3434(3) 0.0464(2) 0.0475(10) Uani 1 1 d . . . H63 H 0.9110 0.3801 0.0072 0.057 Uiso 1 1 calc R . . C64 C 1.0416(4) 0.3734(4) 0.0783(3) 0.0598(13) Uani 1 1 d . . . H64 H 1.0742 0.4297 0.0607 0.072 Uiso 1 1 calc R . . C65 C 1.0915(3) 0.3226(3) 0.1345(3) 0.0519(11) Uani 1 1 d . . . H65 H 1.1581 0.3435 0.1565 0.062 Uiso 1 1 calc R . . C66 C 1.0435(3) 0.2404(3) 0.1586(2) 0.0383(8) Uani 1 1 d . . . H66 H 1.0777 0.2035 0.1970 0.046 Uiso 1 1 calc R . . C67 C 0.9446(3) 0.2112(3) 0.12672(19) 0.0309(7) Uani 1 1 d . . . H67 H 0.9132 0.1546 0.1447 0.037 Uiso 1 1 calc R . . C68 C 0.7653(3) 0.1034(2) 0.01264(16) 0.0247(7) Uani 1 1 d . . . C69 C 0.8480(3) 0.0515(2) -0.01222(18) 0.0282(7) Uani 1 1 d . . . H69 H 0.9113 0.0868 -0.0110 0.034 Uiso 1 1 calc R . . C70 C 0.8414(3) -0.0496(2) -0.03858(19) 0.0314(7) Uani 1 1 d . . . H70 H 0.8993 -0.0817 -0.0550 0.038 Uiso 1 1 calc R . . C71 C 0.7501(3) -0.1032(3) -0.0408(2) 0.0352(8) Uani 1 1 d . . . H71 H 0.7449 -0.1719 -0.0590 0.042 Uiso 1 1 calc R . . C72 C 0.6669(3) -0.0554(3) -0.0161(2) 0.0355(8) Uani 1 1 d . . . H72 H 0.6042 -0.0916 -0.0169 0.043 Uiso 1 1 calc R . . C73 C 0.6750(3) 0.0459(2) 0.00998(18) 0.0295(7) Uani 1 1 d . . . H73 H 0.6169 0.0772 0.0266 0.035 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 0.0222(2) 0.0341(3) 0.0254(3) 0.00419(19) -0.00220(18) -0.00936(19) N1 0.0218(13) 0.0264(13) 0.0229(13) -0.0008(10) 0.0024(11) -0.0022(10) N2 0.0316(16) 0.0353(16) 0.0353(16) 0.0051(13) 0.0062(13) -0.0015(12) N3 0.0346(17) 0.0371(16) 0.0459(19) 0.0136(14) 0.0101(14) 0.0034(13) N4 0.0209(14) 0.0471(18) 0.0365(16) 0.0186(14) -0.0020(12) -0.0058(12) N5 0.0173(12) 0.0196(12) 0.0283(14) 0.0036(10) 0.0037(10) 0.0007(10) N6 0.0356(17) 0.0382(17) 0.0441(18) -0.0038(14) 0.0225(14) -0.0049(13) N7 0.0296(15) 0.0318(15) 0.0451(18) 0.0089(13) 0.0080(13) -0.0021(12) N8 0.0223(14) 0.0365(16) 0.0383(17) 0.0096(13) -0.0027(12) -0.0119(12) N9 0.0246(14) 0.0286(14) 0.0260(14) -0.0032(11) 0.0048(11) -0.0079(11) N10 0.052(2) 0.049(2) 0.0351(18) 0.0005(15) -0.0118(15) -0.0142(16) C1 0.0328(19) 0.0359(19) 0.043(2) -0.0018(16) 0.0019(16) 0.0033(15) C2 0.044(2) 0.054(2) 0.038(2) 0.0125(18) 0.0173(18) 0.0133(19) C3 0.0272(18) 0.044(2) 0.039(2) 0.0072(16) 0.0074(15) -0.0024(15) C4 0.0347(18) 0.0279(16) 0.0199(16) -0.0004(13) -0.0031(13) -0.0048(14) C5 0.0299(18) 0.0366(18) 0.0296(18) 0.0036(14) 0.0012(14) -0.0024(15) C6 0.045(2) 0.048(2) 0.048(2) 0.0194(19) 0.0133(19) 0.0130(18) C7 0.0225(18) 0.057(3) 0.065(3) 0.024(2) -0.0013(18) 0.0010(17) C8 0.0269(19) 0.061(3) 0.059(3) 0.028(2) 0.0040(18) -0.0010(18) C9 0.0252(17) 0.0233(16) 0.0397(19) -0.0042(14) 0.0107(14) -0.0054(13) C10 0.038(2) 0.045(2) 0.034(2) -0.0054(16) 0.0022(16) -0.0131(17) C11 0.050(2) 0.044(2) 0.054(3) -0.0186(19) 0.024(2) -0.0113(19) C12 0.0197(15) 0.0218(15) 0.0314(17) 0.0075(13) 0.0024(13) 0.0047(12) C13 0.0190(15) 0.0307(17) 0.0326(18) 0.0133(14) 0.0031(13) 0.0001(13) C14 0.038(2) 0.038(2) 0.064(3) 0.0090(19) 0.016(2) -0.0088(17) C15 0.053(3) 0.057(3) 0.050(3) 0.014(2) 0.002(2) -0.032(2) C16 0.041(2) 0.050(2) 0.055(3) 0.000(2) 0.0010(19) -0.0245(19) C17 0.0288(17) 0.0304(17) 0.0303(18) 0.0010(14) -0.0004(14) 0.0027(14) C18 0.043(2) 0.039(2) 0.045(2) 0.0108(17) -0.0004(18) 0.0101(17) C19 0.036(2) 0.037(2) 0.073(3) 0.000(2) -0.003(2) 0.0080(17) C20 0.046(2) 0.0268(18) 0.062(3) -0.0122(17) 0.015(2) -0.0051(16) C21 0.037(2) 0.0327(18) 0.0350(19) -0.0046(15) 0.0048(16) -0.0095(15) C22 0.071(3) 0.0284(19) 0.037(2) -0.0065(16) -0.003(2) -0.0065(19) B1 0.0227(18) 0.0238(17) 0.0308(19) 0.0043(14) -0.0001(15) -0.0022(14) B2 0.037(2) 0.0243(17) 0.0213(18) 0.0028(14) 0.0088(15) 0.0031(15) C26 0.0244(16) 0.0172(14) 0.0246(16) -0.0019(11) 0.0009(12) -0.0044(12) C27 0.0238(16) 0.0270(16) 0.0324(18) 0.0000(13) 0.0032(13) 0.0003(13) C28 0.0305(18) 0.0394(19) 0.0272(17) 0.0002(14) 0.0093(14) -0.0050(15) C29 0.0341(19) 0.0317(17) 0.0255(17) 0.0057(13) -0.0019(14) -0.0079(14) C30 0.0245(17) 0.0333(18) 0.0313(18) 0.0060(14) -0.0009(14) -0.0013(14) C31 0.0217(16) 0.0271(16) 0.0296(17) 0.0028(13) 0.0036(13) -0.0043(12) C32 0.0275(17) 0.0253(16) 0.0308(17) 0.0118(13) 0.0000(14) -0.0005(13) C33 0.0321(19) 0.0396(19) 0.036(2) 0.0089(16) 0.0043(15) -0.0066(15) C34 0.033(2) 0.052(2) 0.046(2) 0.0171(19) 0.0131(17) -0.0073(17) C35 0.054(3) 0.046(2) 0.042(2) 0.0183(18) 0.0242(19) 0.0041(19) C36 0.057(3) 0.0334(19) 0.0296(19) 0.0096(15) 0.0107(17) 0.0002(17) C37 0.0364(19) 0.0292(17) 0.0324(18) 0.0095(14) -0.0007(15) -0.0026(14) C38 0.0244(16) 0.0286(16) 0.0281(17) 0.0050(13) 0.0031(13) -0.0035(13) C39 0.0311(18) 0.0296(17) 0.0342(19) 0.0023(14) 0.0006(15) -0.0059(14) C40 0.0331(19) 0.0367(19) 0.0338(19) -0.0006(15) 0.0032(15) -0.0133(15) C41 0.0232(17) 0.054(2) 0.0287(18) 0.0058(16) 0.0006(14) -0.0079(15) C42 0.0276(19) 0.045(2) 0.046(2) 0.0149(17) -0.0017(16) 0.0004(16) C43 0.0258(18) 0.0307(18) 0.051(2) 0.0122(16) 0.0009(16) -0.0042(14) C44 0.0184(15) 0.0241(16) 0.046(2) 0.0042(14) 0.0012(14) -0.0013(12) C45 0.0266(18) 0.0269(17) 0.053(2) 0.0096(16) -0.0060(16) -0.0046(14) C46 0.0255(18) 0.0266(18) 0.076(3) 0.0133(18) 0.0010(18) -0.0026(14) C47 0.0248(18) 0.0208(17) 0.090(3) -0.0028(18) 0.0168(19) -0.0028(14) C48 0.033(2) 0.0332(19) 0.067(3) -0.0153(18) 0.0253(19) -0.0125(16) C49 0.0273(18) 0.0257(17) 0.052(2) -0.0021(15) 0.0132(16) -0.0075(14) C50 0.0338(18) 0.0308(17) 0.0263(17) 0.0056(13) 0.0108(14) 0.0035(14) C51 0.0339(18) 0.0300(17) 0.0252(17) 0.0023(13) -0.0009(14) -0.0069(14) C52 0.056(3) 0.049(2) 0.0223(18) 0.0020(16) -0.0053(17) -0.0128(19) C53 0.043(2) 0.052(2) 0.032(2) 0.0196(17) -0.0019(17) -0.0024(18) C54 0.080(3) 0.037(2) 0.052(3) 0.0189(19) 0.026(2) 0.019(2) C55 0.098(4) 0.038(2) 0.034(2) 0.0112(17) 0.031(2) 0.025(2) C56 0.0362(18) 0.0201(15) 0.0240(16) 0.0008(12) 0.0083(14) 0.0000(13) C57 0.041(2) 0.044(2) 0.0240(17) 0.0058(15) 0.0072(15) 0.0097(16) C58 0.038(2) 0.051(2) 0.036(2) 0.0076(17) 0.0088(16) 0.0106(17) C59 0.046(2) 0.041(2) 0.0319(19) 0.0043(15) 0.0188(17) 0.0077(17) C60 0.043(2) 0.0364(19) 0.0242(17) -0.0027(14) 0.0087(15) -0.0006(16) C61 0.0347(18) 0.0240(15) 0.0271(17) -0.0021(13) 0.0066(14) -0.0021(13) C62 0.042(2) 0.0256(16) 0.0259(17) -0.0027(13) 0.0134(15) -0.0020(14) C63 0.062(3) 0.040(2) 0.042(2) 0.0028(17) 0.013(2) -0.0138(19) C64 0.065(3) 0.055(3) 0.061(3) -0.001(2) 0.017(2) -0.030(2) C65 0.046(2) 0.058(3) 0.052(3) -0.011(2) 0.015(2) -0.021(2) C66 0.037(2) 0.044(2) 0.033(2) -0.0103(16) 0.0084(16) 0.0011(16) C67 0.0348(19) 0.0279(17) 0.0312(18) -0.0057(14) 0.0127(15) -0.0023(14) C68 0.0326(17) 0.0254(15) 0.0168(15) 0.0030(12) 0.0043(13) 0.0021(13) C69 0.0326(18) 0.0275(16) 0.0257(17) 0.0013(13) 0.0083(14) -0.0022(13) C70 0.040(2) 0.0255(16) 0.0307(18) -0.0007(13) 0.0115(15) 0.0028(14) C71 0.047(2) 0.0233(16) 0.0346(19) -0.0031(14) 0.0028(16) -0.0020(15) C72 0.0349(19) 0.0311(18) 0.039(2) 0.0014(15) 0.0002(16) -0.0054(15) C73 0.0312(18) 0.0304(17) 0.0268(17) 0.0022(13) 0.0027(14) 0.0034(14) _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 N10 1.949(3) . ? Fe1 N9 1.951(3) . ? Fe1 N1 1.970(3) . ? Fe1 N4 1.981(3) . ? Fe1 N8 1.983(3) . ? Fe1 N5 1.984(3) . ? N1 C4 1.301(4) . ? N1 C1 1.464(4) . ? N2 C4 1.341(4) . ? N2 C3 1.451(5) . ? N2 H2 0.8800 . ? N3 C5 1.357(5) . ? N3 C6 1.473(5) . ? N3 H3 0.8800 . ? N4 C5 1.291(4) . ? N4 C8 1.459(5) . ? N5 C12 1.301(4) . ? N5 C9 1.466(4) . ? N6 C12 1.333(4) . ? N6 C11 1.457(5) . ? N6 H6 0.8800 . ? N7 C13 1.347(4) . ? N7 C14 1.454(5) . ? N7 H7 0.8800 . ? N8 C13 1.298(5) . ? N8 C16 1.481(5) . ? N9 C17 1.371(4) . ? N9 C21 1.375(4) . ? N10 C22 1.291(5) . ? N10 C23A 1.454(12) . ? N10 C23B 1.513(8) . ? C1 C2 1.553(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.499(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.496(5) . ? C6 C7 1.500(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.541(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.485(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.485(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.482(4) . ? C14 C15 1.450(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.513(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.394(5) . ? C17 H17 0.9500 . ? C18 C19 1.357(6) . ? C18 H18 0.9500 . ? C19 C20 1.382(6) . ? C19 H19 0.9500 . ? C20 C21 1.374(5) . ? C20 H20 0.9500 . ? C21 C22 1.444(5) . ? C22 H22A 0.9500 . ? C22 H22B 0.9300 . ? C23A C25A 1.460(13) . ? C23A C24A 1.538(14) . ? C23A H23A 1.0000 . ? C24A H24A 0.9800 . ? C24A H24B 0.9800 . ? C24A H24C 0.9800 . ? C25A H25A 0.9800 . ? C25A H25B 0.9800 . ? C25A H25C 0.9800 . ? C23B C24B 1.504(10) . ? C23B C25B 1.535(9) . ? C23B H23B 1.0000 . ? C24B H24D 0.9800 . ? C24B H24E 0.9800 . ? C24B H24F 0.9800 . ? C25B H25D 0.9800 . ? C25B H25E 0.9800 . ? C25B H25F 0.9800 . ? B1 C44 1.647(5) . ? B1 C26 1.651(5) . ? B1 C32 1.652(5) . ? B1 C38 1.661(5) . ? B2 C68 1.650(5) . ? B2 C50 1.651(5) . ? B2 C62 1.653(5) . ? B2 C56 1.653(5) . ? C26 C31 1.399(4) . ? C26 C27 1.403(5) . ? C27 C28 1.388(5) . ? C27 H27 0.9500 . ? C28 C29 1.385(5) . ? C28 H28 0.9500 . ? C29 C30 1.386(5) . ? C29 H29 0.9500 . ? C30 C31 1.394(5) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C37 1.397(5) . ? C32 C33 1.404(5) . ? C33 C34 1.391(5) . ? C33 H33 0.9500 . ? C34 C35 1.384(6) . ? C34 H34 0.9500 . ? C35 C36 1.379(6) . ? C35 H35 0.9500 . ? C36 C37 1.395(5) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C43 1.397(5) . ? C38 C39 1.408(5) . ? C39 C40 1.393(5) . ? C39 H39 0.9500 . ? C40 C41 1.379(5) . ? C40 H40 0.9500 . ? C41 C42 1.372(5) . ? C41 H41 0.9500 . ? C42 C43 1.395(5) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C49 1.392(5) . ? C44 C45 1.413(5) . ? C45 C46 1.388(5) . ? C45 H45 0.9500 . ? C46 C47 1.380(6) . ? C46 H46 0.9500 . ? C47 C48 1.379(6) . ? C47 H47 0.9500 . ? C48 C49 1.401(5) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? C50 C51 1.393(5) . ? C50 C55 1.403(5) . ? C51 C52 1.395(5) . ? C51 H51 0.9500 . ? C52 C53 1.372(6) . ? C52 H52 0.9500 . ? C53 C54 1.386(6) . ? C53 H53 0.9500 . ? C54 C55 1.385(5) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 C57 1.402(5) . ? C56 C61 1.406(5) . ? C57 C58 1.392(5) . ? C57 H57 0.9500 . ? C58 C59 1.386(5) . ? C58 H58 0.9500 . ? C59 C60 1.376(5) . ? C59 H59 0.9500 . ? C60 C61 1.392(5) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C62 C67 1.403(5) . ? C62 C63 1.406(5) . ? C63 C64 1.398(6) . ? C63 H63 0.9500 . ? C64 C65 1.367(7) . ? C64 H64 0.9500 . ? C65 C66 1.377(6) . ? C65 H65 0.9500 . ? C66 C67 1.400(5) . ? C66 H66 0.9500 . ? C67 H67 0.9500 . ? C68 C73 1.401(5) . ? C68 C69 1.403(5) . ? C69 C70 1.394(5) . ? C69 H69 0.9500 . ? C70 C71 1.386(5) . ? C70 H70 0.9500 . ? C71 C72 1.382(5) . ? C71 H71 0.9500 . ? C72 C73 1.396(5) . ? C72 H72 0.9500 . ? C73 H73 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 N10 Fe1 N9 80.27(13) . . ? N10 Fe1 N1 92.14(13) . . ? N9 Fe1 N1 94.43(11) . . ? N10 Fe1 N4 97.42(14) . . ? N9 Fe1 N4 174.86(12) . . ? N1 Fe1 N4 81.03(11) . . ? N10 Fe1 N8 94.97(14) . . ? N9 Fe1 N8 90.86(12) . . ? N1 Fe1 N8 171.77(12) . . ? N4 Fe1 N8 93.92(12) . . ? N10 Fe1 N5 172.38(13) . . ? N9 Fe1 N5 94.71(10) . . ? N1 Fe1 N5 93.97(10) . . ? N4 Fe1 N5 88.04(12) . . ? N8 Fe1 N5 79.29(11) . . ? C4 N1 C1 118.8(3) . . ? C4 N1 Fe1 115.6(2) . . ? C1 N1 Fe1 125.2(2) . . ? C4 N2 C3 117.2(3) . . ? C4 N2 H2 121.4 . . ? C3 N2 H2 121.4 . . ? C5 N3 C6 121.0(3) . . ? C5 N3 H3 119.5 . . ? C6 N3 H3 119.5 . . ? C5 N4 C8 118.7(3) . . ? C5 N4 Fe1 113.6(2) . . ? C8 N4 Fe1 127.1(2) . . ? C12 N5 C9 118.2(3) . . ? C12 N5 Fe1 116.2(2) . . ? C9 N5 Fe1 125.2(2) . . ? C12 N6 C11 120.5(3) . . ? C12 N6 H6 119.8 . . ? C11 N6 H6 119.8 . . ? C13 N7 C14 121.8(3) . . ? C13 N7 H7 119.1 . . ? C14 N7 H7 119.1 . . ? C13 N8 C16 117.5(3) . . ? C13 N8 Fe1 116.6(2) . . ? C16 N8 Fe1 125.7(3) . . ? C17 N9 C21 115.2(3) . . ? C17 N9 Fe1 129.1(2) . . ? C21 N9 Fe1 115.7(2) . . ? C22 N10 C23A 110.0(6) . . ? C22 N10 C23B 122.4(4) . . ? C22 N10 Fe1 116.6(3) . . ? C23A N10 Fe1 130.7(5) . . ? C23B N10 Fe1 120.6(4) . . ? N1 C1 C2 112.2(3) . . ? N1 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C3 C2 C1 108.5(3) . . ? C3 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? C3 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? N2 C3 C2 111.2(3) . . ? N2 C3 H3A 109.4 . . ? C2 C3 H3A 109.4 . . ? N2 C3 H3B 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? N1 C4 N2 127.5(3) . . ? N1 C4 C5 113.0(3) . . ? N2 C4 C5 119.4(3) . . ? N4 C5 N3 124.9(3) . . ? N4 C5 C4 115.6(3) . . ? N3 C5 C4 119.5(3) . . ? N3 C6 C7 108.3(3) . . ? N3 C6 H6A 110.0 . . ? C7 C6 H6A 110.0 . . ? N3 C6 H6B 110.0 . . ? C7 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? C6 C7 C8 108.9(3) . . ? C6 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? C6 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? N4 C8 C7 110.7(3) . . ? N4 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? N5 C9 C10 113.8(3) . . ? N5 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? N5 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C11 C10 C9 112.5(3) . . ? C11 C10 H10A 109.1 . . ? C9 C10 H10A 109.1 . . ? C11 C10 H10B 109.1 . . ? C9 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? N6 C11 C10 110.3(3) . . ? N6 C11 H11A 109.6 . . ? C10 C11 H11A 109.6 . . ? N6 C11 H11B 109.6 . . ? C10 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? N5 C12 N6 126.1(3) . . ? N5 C12 C13 113.8(3) . . ? N6 C12 C13 120.1(3) . . ? N8 C13 N7 125.8(3) . . ? N8 C13 C12 113.7(3) . . ? N7 C13 C12 120.5(3) . . ? C15 C14 N7 108.1(3) . . ? C15 C14 H14A 110.1 . . ? N7 C14 H14A 110.1 . . ? C15 C14 H14B 110.1 . . ? N7 C14 H14B 110.1 . . ? H14A C14 H14B 108.4 . . ? C14 C15 C16 114.5(4) . . ? C14 C15 H15A 108.6 . . ? C16 C15 H15A 108.6 . . ? C14 C15 H15B 108.6 . . ? C16 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? N8 C16 C15 111.9(4) . . ? N8 C16 H16A 109.2 . . ? C15 C16 H16A 109.2 . . ? N8 C16 H16B 109.2 . . ? C15 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? N9 C17 C18 122.6(3) . . ? N9 C17 H17 118.7 . . ? C18 C17 H17 118.7 . . ? C19 C18 C17 120.0(4) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 119.0(4) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C21 C20 C19 119.0(4) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C20 C21 N9 123.9(3) . . ? C20 C21 C22 124.7(3) . . ? N9 C21 C22 111.4(3) . . ? N10 C22 C21 116.0(3) . . ? N10 C22 H22A 122.0 . . ? C21 C22 H22A 122.0 . . ? N10 C22 H22B 122.0 . . ? C21 C22 H22B 122.0 . . ? N10 C23A C25A 114.9(10) . . ? N10 C23A C24A 118.9(10) . . ? C25A C23A C24A 107.4(11) . . ? N10 C23A H23A 104.7 . . ? C25A C23A H23A 104.7 . . ? C24A C23A H23A 104.7 . . ? C24B C23B N10 103.0(6) . . ? C24B C23B C25B 110.6(6) . . ? N10 C23B C25B 112.0(5) . . ? C24B C23B H23B 110.4 . . ? N10 C23B H23B 110.4 . . ? C25B C23B H23B 110.4 . . ? C23B C24B H24D 109.5 . . ? C23B C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? C23B C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? C23B C25B H25D 109.5 . . ? C23B C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? C23B C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? C44 B1 C26 108.9(3) . . ? C44 B1 C32 108.1(3) . . ? C26 B1 C32 110.5(3) . . ? C44 B1 C38 111.2(3) . . ? C26 B1 C38 109.8(3) . . ? C32 B1 C38 108.3(3) . . ? C68 B2 C50 107.8(3) . . ? C68 B2 C62 110.8(3) . . ? C50 B2 C62 108.5(3) . . ? C68 B2 C56 109.2(3) . . ? C50 B2 C56 109.5(3) . . ? C62 B2 C56 110.9(3) . . ? C31 C26 C27 114.7(3) . . ? C31 C26 B1 123.5(3) . . ? C27 C26 B1 121.8(3) . . ? C28 C27 C26 123.2(3) . . ? C28 C27 H27 118.4 . . ? C26 C27 H27 118.4 . . ? C29 C28 C27 120.3(3) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 118.6(3) . . ? C28 C29 H29 120.7 . . ? C30 C29 H29 120.7 . . ? C29 C30 C31 120.2(3) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C30 C31 C26 123.1(3) . . ? C30 C31 H31 118.5 . . ? C26 C31 H31 118.5 . . ? C37 C32 C33 115.2(3) . . ? C37 C32 B1 124.3(3) . . ? C33 C32 B1 120.4(3) . . ? C34 C33 C32 122.6(4) . . ? C34 C33 H33 118.7 . . ? C32 C33 H33 118.7 . . ? C35 C34 C33 120.3(4) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C36 C35 C34 118.8(4) . . ? C36 C35 H35 120.6 . . ? C34 C35 H35 120.6 . . ? C35 C36 C37 120.3(4) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C36 C37 C32 122.6(3) . . ? C36 C37 H37 118.7 . . ? C32 C37 H37 118.7 . . ? C43 C38 C39 113.9(3) . . ? C43 C38 B1 123.5(3) . . ? C39 C38 B1 122.4(3) . . ? C40 C39 C38 123.3(3) . . ? C40 C39 H39 118.3 . . ? C38 C39 H39 118.3 . . ? C41 C40 C39 120.2(3) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C42 C41 C40 118.6(3) . . ? C42 C41 H41 120.7 . . ? C40 C41 H41 120.7 . . ? C41 C42 C43 120.6(3) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C42 C43 C38 123.3(3) . . ? C42 C43 H43 118.3 . . ? C38 C43 H43 118.3 . . ? C49 C44 C45 115.2(3) . . ? C49 C44 B1 123.8(3) . . ? C45 C44 B1 121.0(3) . . ? C46 C45 C44 122.5(4) . . ? C46 C45 H45 118.8 . . ? C44 C45 H45 118.8 . . ? C47 C46 C45 120.3(4) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C48 C47 C46 119.2(3) . . ? C48 C47 H47 120.4 . . ? C46 C47 H47 120.4 . . ? C47 C48 C49 120.0(4) . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.0 . . ? C44 C49 C48 122.7(4) . . ? C44 C49 H49 118.6 . . ? C48 C49 H49 118.6 . . ? C51 C50 C55 114.9(3) . . ? C51 C50 B2 124.6(3) . . ? C55 C50 B2 120.3(3) . . ? C50 C51 C52 122.3(3) . . ? C50 C51 H51 118.8 . . ? C52 C51 H51 118.8 . . ? C53 C52 C51 120.9(4) . . ? C53 C52 H52 119.6 . . ? C51 C52 H52 119.6 . . ? C52 C53 C54 118.9(3) . . ? C52 C53 H53 120.5 . . ? C54 C53 H53 120.5 . . ? C55 C54 C53 119.4(4) . . ? C55 C54 H54 120.3 . . ? C53 C54 H54 120.3 . . ? C54 C55 C50 123.6(4) . . ? C54 C55 H55 118.2 . . ? C50 C55 H55 118.2 . . ? C57 C56 C61 114.5(3) . . ? C57 C56 B2 121.3(3) . . ? C61 C56 B2 124.1(3) . . ? C58 C57 C56 123.2(3) . . ? C58 C57 H57 118.4 . . ? C56 C57 H57 118.4 . . ? C59 C58 C57 119.9(4) . . ? C59 C58 H58 120.0 . . ? C57 C58 H58 120.0 . . ? C60 C59 C58 119.0(3) . . ? C60 C59 H59 120.5 . . ? C58 C59 H59 120.5 . . ? C59 C60 C61 120.3(3) . . ? C59 C60 H60 119.9 . . ? C61 C60 H60 119.9 . . ? C60 C61 C56 123.0(3) . . ? C60 C61 H61 118.5 . . ? C56 C61 H61 118.5 . . ? C67 C62 C63 113.9(3) . . ? C67 C62 B2 121.9(3) . . ? C63 C62 B2 124.2(3) . . ? C64 C63 C62 123.2(4) . . ? C64 C63 H63 118.4 . . ? C62 C63 H63 118.4 . . ? C65 C64 C63 120.6(4) . . ? C65 C64 H64 119.7 . . ? C63 C64 H64 119.7 . . ? C64 C65 C66 118.8(4) . . ? C64 C65 H65 120.6 . . ? C66 C65 H65 120.6 . . ? C65 C66 C67 120.2(4) . . ? C65 C66 H66 119.9 . . ? C67 C66 H66 119.9 . . ? C66 C67 C62 123.3(3) . . ? C66 C67 H67 118.4 . . ? C62 C67 H67 118.4 . . ? C73 C68 C69 115.2(3) . . ? C73 C68 B2 123.0(3) . . ? C69 C68 B2 121.4(3) . . ? C70 C69 C68 122.9(3) . . ? C70 C69 H69 118.5 . . ? C68 C69 H69 118.5 . . ? C71 C70 C69 119.9(3) . . ? C71 C70 H70 120.1 . . ? C69 C70 H70 120.1 . . ? C72 C71 C70 119.3(3) . . ? C72 C71 H71 120.4 . . ? C70 C71 H71 120.4 . . ? C71 C72 C73 120.0(3) . . ? C71 C72 H72 120.0 . . ? C73 C72 H72 120.0 . . ? C72 C73 C68 122.8(3) . . ? C72 C73 H73 118.6 . . ? C68 C73 H73 118.6 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.880 _refine_diff_density_min -1.325 _refine_diff_density_rms 0.075 #===END data_3-Bph4 _database_code_depnum_ccdc_archive 'CCDC 768564' #TrackingRef '- 1-4.cif' _audit_creation_method 'Bruker SHELXTL' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H36 Fe N10, 2(C24 H20 B)' _chemical_formula_sum 'C74 H76 B2 Fe N10' _chemical_formula_weight 1182.92 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 ' _symmetry_space_group_name_Hall ' -P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.040(3) _cell_length_b 13.169(3) _cell_length_c 22.292(5) _cell_angle_alpha 76.65(3) _cell_angle_beta 79.24(3) _cell_angle_gamma 60.99(3) _cell_volume 3244.7(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9881 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 28.27 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.396 _exptl_crystal_size_mid 0.230 _exptl_crystal_size_min 0.206 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 0.283 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57949 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.94 _diffrn_reflns_theta_max 28.55 _reflns_number_total 15969 _reflns_number_gt 11354 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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. SQUEEZE result: Summary and Remarks : N = NOTE, W = WARNING, E = ERROR #=============================================================================== N: No S.U.'s (esd) on observed/calculated parameters. N: DISORDERED structure - ATOMS with Pop. .LT. 1.0 are not moved or as a group. #------------------------------------------------------------------------------- N: Number of moved primary input atoms: .................................. 209 N: Number of Ignored Lines on INPUT ...................................... 12 of which blank in column 1 ..................................... 12 N: Number of modified (= # ) ATOM labels ................................. 4 N: Total Potential Solvent Accessible Void Vol .................. 206.4 Ang^3 N: Electron Count / Cell = 50 - To be included in D(calc), F000 & Mol.Wght. #=============================================================================== with Z = 2, this works out to about 1.2 MeCN per formula unit Responding to errors on checkcif: A and B: Short Inter XH3..XHn. The bpy ligand and one of the H2bip ligands show positional disorder thererfore we refined them with isotropic displacement parameters. The three ligand sites on the Fe appear occupied as 1) 100% (H2bip) 2) 50% (H2bip)/50%(bpy) 3) 50%(bpy)/50%(H2bip). The overall formula is Fe(H2bip)2bpy(Bph4)2. Due to the nonrigid nature of H2bip ligand, some hydrogens on the H2bip with 50% occupancy show a short interaction with Bph4 anion. ; _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^)+(0.1015P)^2^+0.9030P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15969 _refine_ls_number_parameters 760 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0874 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1831 _refine_ls_wR_factor_gt 0.1704 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.75817(3) 0.78815(2) 0.747628(14) 0.02240(10) Uani 1 1 d . . . N1 N 0.66021(15) 0.86225(15) 0.81870(8) 0.0227(4) Uani 1 1 d . A . C1 C 0.6569(2) 0.79837(18) 0.88222(10) 0.0268(5) Uani 1 1 d . . . H1A H 0.7367 0.7334 0.8901 0.032 Uiso 1 1 calc R A . H1B H 0.6036 0.7632 0.8859 0.032 Uiso 1 1 calc R . . C2 C 0.6159(3) 0.8763(2) 0.93064(12) 0.0442(7) Uani 1 1 d . A . H2A H 0.5942 0.8363 0.9705 0.053 Uiso 1 1 calc R . . H2B H 0.6807 0.8907 0.9368 0.053 Uiso 1 1 calc R . . C3 C 0.5121(3) 0.9911(2) 0.91149(12) 0.0436(7) Uani 1 1 d . . . H3A H 0.4440 0.9776 0.9108 0.052 Uiso 1 1 calc R A . H3B H 0.4909 1.0436 0.9420 0.052 Uiso 1 1 calc R . . N2 N 0.53768(19) 1.04793(17) 0.85017(9) 0.0360(5) Uani 1 1 d . A . H2 H 0.5079 1.1250 0.8407 0.043 Uiso 1 1 calc R . . C4 C 0.60927(18) 0.97700(18) 0.80844(10) 0.0243(4) Uani 1 1 d . . . C5 C 0.6274(2) 1.03204(18) 0.74375(10) 0.0258(4) Uani 1 1 d . A . N3 N 0.5637(2) 1.14945(16) 0.72479(10) 0.0371(5) Uani 1 1 d . . . H3 H 0.5077 1.1920 0.7506 0.044 Uiso 1 1 calc R A . C6 C 0.5848(3) 1.2078(2) 0.66282(13) 0.0543(8) Uani 1 1 d . A . H6A H 0.5745 1.2866 0.6648 0.065 Uiso 1 1 calc R . . H6B H 0.5285 1.2176 0.6351 0.065 Uiso 1 1 calc R . . C7 C 0.7109(4) 1.1306(3) 0.63836(15) 0.0676(11) Uani 1 1 d . . . H7A H 0.7240 1.1605 0.5941 0.081 Uiso 1 1 calc R A . H7B H 0.7670 1.1333 0.6615 0.081 Uiso 1 1 calc R . . C8 C 0.7319(3) 1.0053(2) 0.64562(11) 0.0413(6) Uani 1 1 d . A . H8A H 0.6817 1.0022 0.6185 0.050 Uiso 1 1 calc R . . H8B H 0.8151 0.9554 0.6318 0.050 Uiso 1 1 calc R . . N4 N 0.70643(17) 0.95728(15) 0.70967(8) 0.0258(4) Uani 1 1 d . A . N5 N 0.8954(6) 0.7571(6) 0.7866(3) 0.026(2) Uiso 0.50 1 d P A 1 C9 C 0.9233(6) 0.8666(6) 0.7792(3) 0.0293(17) Uiso 0.50 1 d P A 1 H9A H 0.9284 0.9006 0.7349 0.035 Uiso 0.50 1 calc PR A 1 H9B H 0.8592 0.9286 0.8014 0.035 Uiso 0.50 1 calc PR A 1 C10 C 1.0400(8) 0.8230(7) 0.8061(4) 0.045(2) Uiso 0.50 1 d P A 1 H10A H 1.1055 0.7802 0.7764 0.055 Uiso 0.50 1 calc PR A 1 H10B H 1.0475 0.8918 0.8111 0.055 Uiso 0.50 1 calc PR A 1 C11 C 1.0509(5) 0.7440(5) 0.8669(3) 0.0403(12) Uiso 0.50 1 d P A 1 H11A H 1.1302 0.7131 0.8806 0.048 Uiso 0.50 1 calc PR A 1 H11B H 0.9917 0.7883 0.8985 0.048 Uiso 0.50 1 calc PR A 1 N6 N 1.0323(4) 0.6485(4) 0.8603(2) 0.0335(11) Uiso 0.50 1 d P A 1 H6 H 1.0720 0.5811 0.8840 0.040 Uiso 0.50 1 calc PR A 1 C12 C 0.9522(5) 0.6465(6) 0.8173(3) 0.0298(17) Uiso 0.50 1 d P A 1 C13 C 0.9016(6) 0.5726(5) 0.8155(3) 0.0271(19) Uiso 0.50 1 d P A 1 N7 N 0.9812(5) 0.4652(4) 0.8491(2) 0.0411(12) Uiso 0.50 1 d P A 1 H7 H 1.0389 0.4539 0.8691 0.049 Uiso 0.50 1 calc PR A 1 C14 C 0.9472(6) 0.3769(5) 0.8434(3) 0.0447(14) Uiso 0.50 1 d P A 1 H14A H 0.9764 0.3097 0.8776 0.054 Uiso 0.50 1 calc PR A 1 H14B H 0.9833 0.3471 0.8038 0.054 Uiso 0.50 1 calc PR A 1 C15 C 0.8151(6) 0.4304(5) 0.8455(3) 0.0468(14) Uiso 0.50 1 d P A 1 H15A H 0.7782 0.4544 0.8863 0.056 Uiso 0.50 1 calc PR A 1 H15B H 0.7920 0.3731 0.8384 0.056 Uiso 0.50 1 calc PR A 1 C16 C 0.7754(7) 0.5411(6) 0.7925(3) 0.0400(17) Uiso 0.50 1 d P A 1 H16A H 0.8093 0.5112 0.7528 0.048 Uiso 0.50 1 calc PR A 1 H16B H 0.6889 0.5757 0.7930 0.048 Uiso 0.50 1 calc PR A 1 N8 N 0.7987(5) 0.6272(4) 0.7907(2) 0.0209(15) Uiso 0.50 1 d P A 1 N9 N 0.8477(6) 0.7239(6) 0.6753(3) 0.0243(19) Uiso 0.50 1 d P A 1 C17 C 0.9670(7) 0.6840(7) 0.6574(4) 0.032(2) Uiso 0.50 1 d P A 1 H17 H 1.0156 0.6784 0.6862 0.038 Uiso 0.50 1 calc PR A 1 C18 C 1.0175(5) 0.6531(5) 0.6023(2) 0.0316(10) Uiso 0.50 1 d P A 1 H18 H 1.1003 0.6230 0.5936 0.038 Uiso 0.50 1 calc PR A 1 C19 C 0.9449(8) 0.6654(8) 0.5540(4) 0.041(3) Uiso 0.50 1 d P A 1 H19 H 0.9797 0.6443 0.5144 0.049 Uiso 0.50 1 calc PR A 1 C20 C 0.8207(6) 0.7105(6) 0.5698(3) 0.0304(18) Uiso 0.50 1 d P A 1 H20 H 0.7690 0.7291 0.5395 0.036 Uiso 0.50 1 calc PR A 1 C21 C 0.7759(8) 0.7267(8) 0.6334(4) 0.030(3) Uiso 0.50 1 d P A 1 C22 C 0.6555(6) 0.7763(6) 0.6492(3) 0.0222(19) Uiso 0.50 1 d P A 1 C23 C 0.5776(5) 0.7871(6) 0.6125(3) 0.0329(16) Uiso 0.50 1 d PD A 1 H23 H 0.5929 0.7892 0.5690 0.039 Uiso 0.50 1 calc PR A 1 C24 C 0.4657(6) 0.7954(6) 0.6475(3) 0.0332(16) Uiso 0.50 1 d PD A 1 H24 H 0.4181 0.7739 0.6311 0.040 Uiso 0.50 1 calc PR A 1 C25 C 0.4298(5) 0.8359(5) 0.7058(2) 0.0306(11) Uiso 0.50 1 d P A 1 H25 H 0.3494 0.8712 0.7215 0.037 Uiso 0.50 1 calc PR A 1 C26 C 0.5196(5) 0.8210(5) 0.7390(3) 0.0251(14) Uiso 0.50 1 d P A 1 H26 H 0.5007 0.8338 0.7807 0.030 Uiso 0.50 1 calc PR A 1 N10 N 0.6332(5) 0.7887(5) 0.7136(3) 0.0221(17) Uiso 0.50 1 d P A 1 N9A N 0.8936(6) 0.7731(6) 0.7819(3) 0.0199(19) Uiso 0.50 1 d P A 2 C17A C 0.9314(6) 0.8398(6) 0.7857(3) 0.0303(17) Uiso 0.50 1 d P A 2 H17A H 0.8918 0.9178 0.7642 0.036 Uiso 0.50 1 calc PR A 2 C18A C 1.0219(7) 0.8175(7) 0.8166(4) 0.041(2) Uiso 0.50 1 d P A 2 H18A H 1.0446 0.8763 0.8159 0.049 Uiso 0.50 1 calc PR A 2 C19A C 1.0825(5) 0.7002(5) 0.8505(2) 0.0351(11) Uiso 0.50 1 d P A 2 H19A H 1.1453 0.6808 0.8739 0.042 Uiso 0.50 1 calc PR A 2 C20A C 1.0488(5) 0.6152(5) 0.8489(3) 0.0323(12) Uiso 0.50 1 d P A 2 H20A H 1.0870 0.5340 0.8660 0.039 Uiso 0.50 1 calc PR A 2 C21A C 0.9547(5) 0.6698(5) 0.8195(3) 0.0223(14) Uiso 0.50 1 d PD A 2 C22A C 0.9198(6) 0.5770(5) 0.8199(3) 0.0269(19) Uiso 0.50 1 d PD A 2 C23A C 0.9568(5) 0.4515(4) 0.8388(3) 0.0369(13) Uiso 0.50 1 d PD A 2 H23A H 1.0330 0.4059 0.8532 0.044 Uiso 0.50 1 calc PR A 2 C24A C 0.8948(6) 0.3881(5) 0.8387(3) 0.0379(12) Uiso 0.50 1 d PD A 2 H24A H 0.9281 0.3062 0.8544 0.045 Uiso 0.50 1 calc PR A 2 C25A C 0.7895(5) 0.4441(5) 0.8165(3) 0.0391(12) Uiso 0.50 1 d P A 2 H25A H 0.7490 0.4010 0.8154 0.047 Uiso 0.50 1 calc PR A 2 C26A C 0.7387(6) 0.5629(5) 0.7951(3) 0.0282(13) Uiso 0.50 1 d PD A 2 H26A H 0.6608 0.6068 0.7828 0.034 Uiso 0.50 1 calc PR A 2 N10A N 0.8226(6) 0.6205(5) 0.7930(3) 0.0293(18) Uiso 0.50 1 d P A 2 N5A N 0.8432(6) 0.7377(5) 0.6667(3) 0.0213(18) Uiso 0.50 1 d P A 2 C9A C 0.9652(7) 0.7041(7) 0.6515(4) 0.037(2) Uiso 0.50 1 d P A 2 H9A1 H 1.0114 0.6261 0.6760 0.044 Uiso 0.50 1 calc PR A 2 H9A2 H 0.9830 0.7613 0.6636 0.044 Uiso 0.50 1 calc PR A 2 C10A C 1.0045(5) 0.6979(6) 0.5836(3) 0.0430(13) Uiso 0.50 1 d P A 2 H10C H 0.9811 0.7783 0.5602 0.052 Uiso 0.50 1 calc PR A 2 H10D H 1.0913 0.6527 0.5782 0.052 Uiso 0.50 1 calc PR A 2 C11A C 0.9532(7) 0.6429(8) 0.5600(4) 0.036(2) Uiso 0.50 1 d P A 2 H11C H 0.9661 0.6551 0.5143 0.043 Uiso 0.50 1 calc PR A 2 H11D H 0.9934 0.5571 0.5752 0.043 Uiso 0.50 1 calc PR A 2 N6A N 0.8320(5) 0.6865(5) 0.5774(3) 0.0292(15) Uiso 0.50 1 d P A 2 H6A1 H 0.7859 0.6832 0.5545 0.035 Uiso 0.50 1 calc PR A 2 C12A C 0.7881(7) 0.7328(7) 0.6289(4) 0.021(2) Uiso 0.50 1 d P A 2 C13A C 0.6596(7) 0.7598(7) 0.6575(4) 0.028(2) Uiso 0.50 1 d P A 2 N7A N 0.5808(5) 0.7608(5) 0.6224(3) 0.0362(15) Uiso 0.50 1 d P A 2 H7A1 H 0.6110 0.7240 0.5902 0.043 Uiso 0.50 1 calc PR A 2 C14A C 0.4561(7) 0.8160(8) 0.6341(4) 0.051(2) Uiso 0.50 1 d P A 2 H14C H 0.4204 0.7787 0.6169 0.061 Uiso 0.50 1 calc PR A 2 H14D H 0.4204 0.9012 0.6175 0.061 Uiso 0.50 1 calc PR A 2 C15A C 0.4452(6) 0.7935(7) 0.7027(3) 0.0498(17) Uiso 0.50 1 d P A 2 H15C H 0.4819 0.7076 0.7176 0.060 Uiso 0.50 1 calc PR A 2 H15D H 0.3610 0.8276 0.7182 0.060 Uiso 0.50 1 calc PR A 2 C16A C 0.5048(5) 0.8475(6) 0.7278(3) 0.0305(15) Uiso 0.50 1 d P A 2 H16C H 0.4636 0.9341 0.7158 0.037 Uiso 0.50 1 calc PR A 2 H16D H 0.4991 0.8289 0.7736 0.037 Uiso 0.50 1 calc PR A 2 N8A N 0.6271(5) 0.8035(5) 0.7044(3) 0.0234(18) Uiso 0.50 1 d P A 2 B1 B 0.4235(3) 0.4155(2) 0.85055(14) 0.0339(6) Uani 1 1 d . . . C27 C 0.4318(2) 0.5282(2) 0.86487(12) 0.0352(5) Uani 1 1 d . . . C28 C 0.5018(2) 0.5163(2) 0.90881(14) 0.0405(6) Uani 1 1 d . . . H28 H 0.5563 0.4396 0.9263 0.049 Uiso 1 1 calc R . . C29 C 0.4944(3) 0.6138(3) 0.92792(16) 0.0492(7) Uani 1 1 d . . . H29 H 0.5436 0.6031 0.9577 0.059 Uiso 1 1 calc R . . C30 C 0.4145(3) 0.7265(2) 0.90302(15) 0.0486(7) Uani 1 1 d . . . H30 H 0.4072 0.7927 0.9171 0.058 Uiso 1 1 calc R . . C31 C 0.3457(2) 0.7431(2) 0.85805(14) 0.0438(7) Uani 1 1 d . . . H31 H 0.2924 0.8202 0.8405 0.053 Uiso 1 1 calc R . . C32 C 0.3556(2) 0.6452(2) 0.83883(13) 0.0397(6) Uani 1 1 d . . . H32 H 0.3096 0.6571 0.8070 0.048 Uiso 1 1 calc R . . C33 C 0.3895(2) 0.4443(2) 0.77827(12) 0.0354(5) Uani 1 1 d . . . C34 C 0.4449(3) 0.4980(2) 0.73009(13) 0.0423(6) Uani 1 1 d . . . H34 H 0.5011 0.5159 0.7405 0.051 Uiso 1 1 calc R . . C35 C 0.4206(3) 0.5255(2) 0.66820(13) 0.0463(7) Uani 1 1 d . . . H35 H 0.4583 0.5633 0.6379 0.056 Uiso 1 1 calc R . . C36 C 0.3420(3) 0.4980(2) 0.65105(14) 0.0493(7) Uani 1 1 d . . . H36 H 0.3262 0.5152 0.6090 0.059 Uiso 1 1 calc R . . C37 C 0.2861(3) 0.4448(3) 0.69613(14) 0.0474(7) Uani 1 1 d . . . H37 H 0.2321 0.4249 0.6849 0.057 Uiso 1 1 calc R . . C38 C 0.3092(2) 0.4205(2) 0.75826(13) 0.0400(6) Uani 1 1 d . . . H38 H 0.2681 0.3860 0.7883 0.048 Uiso 1 1 calc R . . C39 C 0.5510(2) 0.2958(2) 0.86195(12) 0.0347(5) Uani 1 1 d . . . C40 C 0.6423(2) 0.2609(2) 0.81476(13) 0.0384(6) Uani 1 1 d . . . H40 H 0.6300 0.3050 0.7742 0.046 Uiso 1 1 calc R . . C41 C 0.7513(2) 0.1625(3) 0.82589(15) 0.0483(7) Uani 1 1 d . . . H41 H 0.8116 0.1417 0.7929 0.058 Uiso 1 1 calc R . . C42 C 0.7730(3) 0.0942(3) 0.88476(16) 0.0515(7) Uani 1 1 d . . . H42 H 0.8469 0.0268 0.8916 0.062 Uiso 1 1 calc R . . C43 C 0.6859(3) 0.1260(3) 0.93276(15) 0.0491(7) Uani 1 1 d . . . H43 H 0.6992 0.0817 0.9732 0.059 Uiso 1 1 calc R . . C44 C 0.5767(2) 0.2254(2) 0.92071(13) 0.0409(6) Uani 1 1 d . . . H44 H 0.5171 0.2462 0.9540 0.049 Uiso 1 1 calc R . . C45 C 0.3229(2) 0.39307(19) 0.90124(11) 0.0321(5) Uani 1 1 d . . . C46 C 0.2940(2) 0.3029(2) 0.90151(12) 0.0346(5) Uani 1 1 d . . . H46 H 0.3353 0.2523 0.8715 0.042 Uiso 1 1 calc R . . C47 C 0.2090(2) 0.2830(2) 0.94273(12) 0.0377(6) Uani 1 1 d . . . H47 H 0.1927 0.2213 0.9400 0.045 Uiso 1 1 calc R . . C48 C 0.1483(2) 0.3532(2) 0.98758(12) 0.0382(6) Uani 1 1 d . . . H48 H 0.0888 0.3419 1.0156 0.046 Uiso 1 1 calc R . . C49 C 0.1764(2) 0.4407(2) 0.99072(11) 0.0355(5) Uani 1 1 d . . . H49 H 0.1368 0.4886 1.0220 0.043 Uiso 1 1 calc R . . C50 C 0.2617(2) 0.4597(2) 0.94873(11) 0.0330(5) Uani 1 1 d . . . H50 H 0.2790 0.5201 0.9525 0.040 Uiso 1 1 calc R . . B2 B 0.1289(3) 0.1584(3) 0.63768(15) 0.0432(7) Uani 1 1 d . . . C51 C 0.1512(3) 0.1333(2) 0.71116(13) 0.0431(6) Uani 1 1 d . . . C52 C 0.0729(3) 0.1092(2) 0.75829(14) 0.0447(7) Uani 1 1 d . . . H52 H 0.0056 0.1108 0.7467 0.054 Uiso 1 1 calc R . . C53 C 0.0904(3) 0.0830(2) 0.82107(14) 0.0454(7) Uani 1 1 d . . . H53 H 0.0356 0.0670 0.8510 0.054 Uiso 1 1 calc R . . C54 C 0.1868(3) 0.0804(2) 0.83989(14) 0.0466(7) Uani 1 1 d . . . H54 H 0.1999 0.0613 0.8825 0.056 Uiso 1 1 calc R . . C55 C 0.2635(3) 0.1061(3) 0.79547(15) 0.0512(7) Uani 1 1 d . . . H55 H 0.3294 0.1062 0.8077 0.061 Uiso 1 1 calc R . . C56 C 0.2458(3) 0.1319(2) 0.73266(15) 0.0475(7) Uani 1 1 d . . . H56 H 0.3005 0.1493 0.7034 0.057 Uiso 1 1 calc R . . C57 C 0.2158(3) 0.2122(3) 0.59553(14) 0.0505(7) Uani 1 1 d . . . C58 C 0.1799(4) 0.3337(3) 0.57632(14) 0.0613(9) Uani 1 1 d . . . H58 H 0.1003 0.3874 0.5864 0.074 Uiso 1 1 calc R . . C59 C 0.2539(5) 0.3794(4) 0.54358(17) 0.0771(12) Uani 1 1 d . . . H59 H 0.2244 0.4620 0.5312 0.093 Uiso 1 1 calc R . . C60 C 0.3698(5) 0.3046(4) 0.52918(16) 0.0762(13) Uani 1 1 d . . . H60 H 0.4214 0.3352 0.5071 0.091 Uiso 1 1 calc R . . C61 C 0.4112(4) 0.1850(4) 0.54682(17) 0.0736(11) Uani 1 1 d . . . H61 H 0.4913 0.1325 0.5367 0.088 Uiso 1 1 calc R . . C62 C 0.3341(3) 0.1406(4) 0.57998(17) 0.0653(9) Uani 1 1 d . . . H62 H 0.3646 0.0578 0.5922 0.078 Uiso 1 1 calc R . . C63 C 0.1588(2) 0.0353(2) 0.61591(13) 0.0390(6) Uani 1 1 d . . . C64 C 0.1859(3) 0.0241(3) 0.55353(15) 0.0560(8) Uani 1 1 d . . . H64 H 0.1909 0.0870 0.5242 0.067 Uiso 1 1 calc R . . C65 C 0.2057(4) -0.0754(3) 0.53335(16) 0.0657(10) Uani 1 1 d . . . H65 H 0.2238 -0.0799 0.4904 0.079 Uiso 1 1 calc R . . C66 C 0.1996(3) -0.1697(3) 0.57456(16) 0.0589(9) Uani 1 1 d . . . H66 H 0.2132 -0.2379 0.5600 0.071 Uiso 1 1 calc R . . C67 C 0.1737(2) -0.1630(2) 0.63640(14) 0.0449(7) Uani 1 1 d . . . H67 H 0.1696 -0.2267 0.6653 0.054 Uiso 1 1 calc R . . C68 C 0.1535(2) -0.0623(2) 0.65633(13) 0.0376(6) Uani 1 1 d . . . H68 H 0.1351 -0.0585 0.6993 0.045 Uiso 1 1 calc R . . C69 C -0.0110(3) 0.2537(2) 0.62645(14) 0.0474(7) Uani 1 1 d . . . C70 C -0.0740(3) 0.2498(3) 0.58459(16) 0.0536(8) Uani 1 1 d . . . H70 H -0.0365 0.1863 0.5618 0.064 Uiso 1 1 calc R . . C71 C -0.1898(3) 0.3335(3) 0.5736(2) 0.0718(11) Uani 1 1 d . . . H71 H -0.2274 0.3268 0.5432 0.086 Uiso 1 1 calc R . . C72 C -0.2484(4) 0.4236(4) 0.6057(2) 0.0893(16) Uani 1 1 d . . . H72 H -0.3274 0.4803 0.5990 0.107 Uiso 1 1 calc R . . C73 C -0.1908(4) 0.4305(3) 0.6481(2) 0.0972(18) Uani 1 1 d . . . H73 H -0.2314 0.4925 0.6718 0.117 Uiso 1 1 calc R . . C74 C -0.0724(4) 0.3486(3) 0.65824(17) 0.0752(12) Uani 1 1 d . . . H74 H -0.0343 0.3587 0.6872 0.090 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 0.02400(17) 0.02146(15) 0.02347(17) -0.00925(11) -0.00030(12) -0.01008(12) N1 0.0237(9) 0.0235(8) 0.0237(9) -0.0078(7) -0.0006(7) -0.0120(7) C1 0.0299(11) 0.0249(10) 0.0253(11) -0.0058(8) 0.0012(9) -0.0130(9) C2 0.0546(17) 0.0359(13) 0.0303(13) -0.0080(10) 0.0017(12) -0.0125(12) C3 0.0533(17) 0.0366(13) 0.0372(14) -0.0147(11) 0.0103(12) -0.0191(12) N2 0.0453(12) 0.0256(9) 0.0332(11) -0.0139(8) 0.0076(9) -0.0133(9) C4 0.0230(10) 0.0246(10) 0.0277(11) -0.0107(8) 0.0005(8) -0.0110(8) C5 0.0294(11) 0.0237(10) 0.0279(11) -0.0076(8) -0.0063(9) -0.0124(9) N3 0.0495(13) 0.0232(9) 0.0329(11) -0.0072(8) -0.0059(9) -0.0105(9) C6 0.099(3) 0.0268(12) 0.0311(14) -0.0018(10) -0.0110(15) -0.0236(14) C7 0.125(3) 0.0438(16) 0.0360(16) -0.0074(13) 0.0134(18) -0.047(2) C8 0.0670(18) 0.0320(12) 0.0251(12) -0.0073(9) 0.0036(12) -0.0244(12) N4 0.0326(10) 0.0266(9) 0.0218(9) -0.0069(7) -0.0015(7) -0.0155(8) B1 0.0346(14) 0.0290(12) 0.0378(15) -0.0139(11) 0.0035(12) -0.0132(11) C27 0.0311(12) 0.0341(12) 0.0412(14) -0.0158(10) 0.0073(10) -0.0152(10) C28 0.0329(13) 0.0380(13) 0.0561(17) -0.0171(12) -0.0002(12) -0.0179(11) C29 0.0414(15) 0.0521(16) 0.070(2) -0.0278(15) 0.0035(14) -0.0290(14) C30 0.0441(16) 0.0440(15) 0.071(2) -0.0289(14) 0.0160(14) -0.0296(13) C31 0.0419(15) 0.0332(12) 0.0546(17) -0.0178(12) 0.0152(13) -0.0181(11) C32 0.0423(14) 0.0336(12) 0.0418(15) -0.0143(11) 0.0053(11) -0.0159(11) C33 0.0330(13) 0.0294(11) 0.0390(14) -0.0137(10) 0.0027(10) -0.0093(10) C34 0.0492(16) 0.0397(13) 0.0403(15) -0.0131(11) 0.0004(12) -0.0210(12) C35 0.0549(17) 0.0352(13) 0.0405(15) -0.0070(11) 0.0021(13) -0.0162(12) C36 0.0542(18) 0.0423(14) 0.0406(16) -0.0115(12) -0.0074(13) -0.0109(13) C37 0.0455(16) 0.0534(16) 0.0453(16) -0.0164(13) -0.0060(13) -0.0200(13) C38 0.0391(14) 0.0409(13) 0.0394(14) -0.0125(11) 0.0004(11) -0.0168(11) C39 0.0339(13) 0.0323(11) 0.0416(14) -0.0184(10) 0.0011(10) -0.0144(10) C40 0.0371(14) 0.0353(12) 0.0458(15) -0.0191(11) 0.0038(11) -0.0161(11) C41 0.0333(14) 0.0494(15) 0.0628(19) -0.0316(14) 0.0101(13) -0.0149(12) C42 0.0333(14) 0.0464(15) 0.067(2) -0.0260(14) -0.0031(13) -0.0054(12) C43 0.0422(16) 0.0435(15) 0.0516(18) -0.0164(13) -0.0084(13) -0.0069(12) C44 0.0358(14) 0.0382(13) 0.0429(15) -0.0192(11) 0.0000(11) -0.0084(11) C45 0.0321(12) 0.0258(10) 0.0328(13) -0.0086(9) -0.0026(10) -0.0074(9) C46 0.0345(13) 0.0288(11) 0.0360(13) -0.0126(10) -0.0012(10) -0.0087(10) C47 0.0388(14) 0.0317(12) 0.0418(14) -0.0046(10) -0.0074(11) -0.0149(11) C48 0.0350(13) 0.0377(13) 0.0342(13) -0.0014(10) -0.0043(11) -0.0124(11) C49 0.0344(13) 0.0316(11) 0.0295(12) -0.0077(9) -0.0019(10) -0.0059(10) C50 0.0330(12) 0.0254(10) 0.0347(13) -0.0108(9) -0.0031(10) -0.0064(9) B2 0.0524(19) 0.0380(15) 0.0432(17) -0.0162(13) 0.0024(14) -0.0222(14) C51 0.0521(16) 0.0294(12) 0.0503(16) -0.0174(11) -0.0005(13) -0.0174(12) C52 0.0512(16) 0.0365(13) 0.0504(17) -0.0201(12) 0.0043(13) -0.0208(12) C53 0.0545(17) 0.0325(12) 0.0472(16) -0.0200(11) 0.0061(13) -0.0164(12) C54 0.0557(18) 0.0294(12) 0.0480(16) -0.0177(11) -0.0047(14) -0.0095(12) C55 0.0550(18) 0.0451(15) 0.0594(19) -0.0234(14) -0.0059(15) -0.0209(14) C56 0.0551(18) 0.0419(14) 0.0539(18) -0.0196(13) 0.0028(14) -0.0264(13) C57 0.068(2) 0.0562(17) 0.0420(16) -0.0168(13) 0.0019(14) -0.0381(16) C58 0.107(3) 0.0589(18) 0.0428(17) -0.0206(14) 0.0039(17) -0.055(2) C59 0.134(4) 0.085(3) 0.054(2) -0.0225(19) 0.004(2) -0.082(3) C60 0.131(4) 0.118(3) 0.0386(18) -0.007(2) -0.009(2) -0.105(3) C61 0.078(3) 0.113(3) 0.055(2) -0.010(2) -0.0055(19) -0.066(3) C62 0.069(2) 0.079(2) 0.061(2) -0.0064(18) -0.0025(18) -0.048(2) C63 0.0339(13) 0.0392(13) 0.0448(15) -0.0175(11) 0.0020(11) -0.0149(11) C64 0.079(2) 0.0478(16) 0.0460(17) -0.0163(13) -0.0004(16) -0.0308(16) C65 0.098(3) 0.065(2) 0.0425(18) -0.0279(15) 0.0064(17) -0.040(2) C66 0.077(2) 0.0524(17) 0.061(2) -0.0323(15) 0.0060(17) -0.0341(17) C67 0.0439(15) 0.0421(14) 0.0571(18) -0.0217(13) 0.0079(13) -0.0247(12) C68 0.0309(13) 0.0403(13) 0.0463(15) -0.0196(11) 0.0048(11) -0.0177(11) C69 0.0574(18) 0.0360(13) 0.0428(16) -0.0110(11) 0.0118(13) -0.0206(13) C70 0.0476(17) 0.0530(17) 0.060(2) -0.0109(14) 0.0079(15) -0.0270(15) C71 0.052(2) 0.068(2) 0.084(3) 0.006(2) 0.0041(19) -0.0302(18) C72 0.064(2) 0.073(3) 0.067(3) 0.017(2) 0.020(2) -0.003(2) C73 0.106(3) 0.049(2) 0.060(2) -0.0083(18) 0.025(2) 0.013(2) C74 0.100(3) 0.0418(17) 0.053(2) -0.0125(14) 0.0015(19) -0.0088(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 N9 1.910(7) . ? Fe1 N10 1.919(6) . ? Fe1 N5 1.958(8) . ? Fe1 N9A 1.959(7) . ? Fe1 N1 1.9603(19) . ? Fe1 N8 1.964(5) . ? Fe1 N5A 2.004(6) . ? Fe1 N4 2.0044(19) . ? Fe1 N8A 2.020(6) . ? Fe1 N10A 2.023(6) . ? N1 C4 1.304(3) . ? N1 C1 1.476(3) . ? C1 C2 1.506(3) . ? C2 C3 1.494(4) . ? C3 N2 1.463(3) . ? N2 C4 1.357(3) . ? C4 C5 1.489(3) . ? C5 N4 1.295(3) . ? C5 N3 1.358(3) . ? N3 C6 1.466(3) . ? C6 C7 1.527(5) . ? C7 C8 1.508(4) . ? C8 N4 1.469(3) . ? N5 C12 1.349(9) . ? N5 C9 1.617(10) . ? C9 C10 1.528(11) . ? C10 C11 1.490(10) . ? C11 N6 1.435(7) . ? N6 C12 1.556(8) . ? C12 C13 1.427(9) . ? C13 N8 1.335(9) . ? C13 N7 1.419(8) . ? N7 C14 1.468(8) . ? C14 C15 1.507(9) . ? C15 C16 1.578(9) . ? C16 N8 1.299(8) . ? N9 C17 1.388(10) . ? N9 C21 1.424(12) . ? C17 C18 1.334(10) . ? C18 C19 1.493(10) . ? C19 C20 1.433(11) . ? C20 C21 1.450(12) . ? C21 C22 1.386(11) . ? C22 C23 1.357(10) . ? C22 N10 1.440(9) . ? C23 C24 1.486(7) . ? C24 C25 1.430(9) . ? C25 C26 1.411(8) . ? C26 N10 1.371(8) . ? N9A C17A 1.221(9) . ? N9A C21A 1.363(8) . ? C17A C18A 1.351(10) . ? C18A C19A 1.443(10) . ? C19A C20A 1.395(8) . ? C20A C21A 1.296(8) . ? C21A C22A 1.495(8) . ? C22A N10A 1.310(10) . ? C22A C23A 1.457(7) . ? C23A C24A 1.415(7) . ? C24A C25A 1.335(9) . ? C25A C26A 1.372(8) . ? C26A N10A 1.594(9) . ? N5A C12A 1.235(10) . ? N5A C9A 1.424(11) . ? C9A C10A 1.511(10) . ? C10A C11A 1.423(10) . ? C11A N6A 1.405(10) . ? N6A C12A 1.325(10) . ? C12A C13A 1.571(11) . ? C13A N8A 1.215(10) . ? C13A N7A 1.396(10) . ? N7A C14A 1.423(9) . ? C14A C15A 1.481(11) . ? C15A C16A 1.517(9) . ? C16A N8A 1.444(9) . ? B1 C27 1.644(4) . ? B1 C39 1.657(4) . ? B1 C45 1.658(4) . ? B1 C33 1.660(4) . ? C27 C28 1.394(4) . ? C27 C32 1.420(4) . ? C28 C29 1.398(4) . ? C29 C30 1.390(4) . ? C30 C31 1.379(4) . ? C31 C32 1.391(4) . ? C33 C38 1.398(4) . ? C33 C34 1.424(4) . ? C34 C35 1.399(4) . ? C35 C36 1.378(4) . ? C36 C37 1.389(4) . ? C37 C38 1.403(4) . ? C39 C40 1.400(3) . ? C39 C44 1.410(4) . ? C40 C41 1.398(4) . ? C41 C42 1.399(5) . ? C42 C43 1.379(4) . ? C43 C44 1.408(4) . ? C45 C50 1.401(3) . ? C45 C46 1.409(3) . ? C46 C47 1.390(4) . ? C47 C48 1.379(4) . ? C48 C49 1.387(4) . ? C49 C50 1.397(4) . ? B2 C63 1.643(4) . ? B2 C51 1.646(4) . ? B2 C57 1.655(5) . ? B2 C69 1.665(5) . ? C51 C56 1.395(4) . ? C51 C52 1.417(4) . ? C52 C53 1.396(4) . ? C53 C54 1.380(4) . ? C54 C55 1.378(4) . ? C55 C56 1.398(4) . ? C57 C62 1.389(5) . ? C57 C58 1.413(4) . ? C58 C59 1.387(5) . ? C59 C60 1.371(6) . ? C60 C61 1.378(6) . ? C61 C62 1.411(5) . ? C63 C64 1.393(4) . ? C63 C68 1.413(4) . ? C64 C65 1.375(4) . ? C65 C66 1.390(5) . ? C66 C67 1.370(4) . ? C67 C68 1.384(3) . ? C69 C70 1.378(5) . ? C69 C74 1.390(4) . ? C70 C71 1.397(5) . ? C71 C72 1.347(6) . ? C72 C73 1.354(7) . ? C73 C74 1.414(6) . ? 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 N9 Fe1 N10 82.8(3) . . ? N9 Fe1 N5 94.6(3) . . ? N10 Fe1 N5 169.7(3) . . ? N9 Fe1 N9A 94.3(3) . . ? N10 Fe1 N9A 175.0(3) . . ? N5 Fe1 N9A 6.0(3) . . ? N9 Fe1 N1 176.6(2) . . ? N10 Fe1 N1 95.49(19) . . ? N5 Fe1 N1 87.6(2) . . ? N9A Fe1 N1 87.6(2) . . ? N9 Fe1 N8 88.5(2) . . ? N10 Fe1 N8 88.8(2) . . ? N5 Fe1 N8 81.1(3) . . ? N9A Fe1 N8 87.1(3) . . ? N1 Fe1 N8 94.34(17) . . ? N9 Fe1 N5A 6.0(3) . . ? N10 Fe1 N5A 81.1(3) . . ? N5 Fe1 N5A 97.2(3) . . ? N9A Fe1 N5A 96.4(3) . . ? N1 Fe1 N5A 170.70(18) . . ? N8 Fe1 N5A 94.3(2) . . ? N9 Fe1 N4 96.2(2) . . ? N10 Fe1 N4 90.64(19) . . ? N5 Fe1 N4 99.6(2) . . ? N9A Fe1 N4 93.7(2) . . ? N1 Fe1 N4 80.89(8) . . ? N8 Fe1 N4 175.13(16) . . ? N5A Fe1 N4 90.45(19) . . ? N9 Fe1 N8A 80.7(3) . . ? N10 Fe1 N8A 6.4(3) . . ? N5 Fe1 N8A 173.9(3) . . ? N9A Fe1 N8A 174.6(3) . . ? N1 Fe1 N8A 97.27(19) . . ? N8 Fe1 N8A 94.8(2) . . ? N5A Fe1 N8A 78.5(3) . . ? N4 Fe1 N8A 84.87(18) . . ? N9 Fe1 N10A 86.8(3) . . ? N10 Fe1 N10A 96.6(3) . . ? N5 Fe1 N10A 73.3(3) . . ? N9A Fe1 N10A 79.2(3) . . ? N1 Fe1 N10A 96.25(18) . . ? N8 Fe1 N10A 8.2(3) . . ? N5A Fe1 N10A 92.8(2) . . ? N4 Fe1 N10A 172.49(19) . . ? N8A Fe1 N10A 102.4(3) . . ? C4 N1 C1 120.01(18) . . ? C4 N1 Fe1 114.74(15) . . ? C1 N1 Fe1 124.51(13) . . ? N1 C1 C2 112.80(18) . . ? C3 C2 C1 110.7(2) . . ? N2 C3 C2 111.0(2) . . ? C4 N2 C3 117.27(19) . . ? N1 C4 N2 125.8(2) . . ? N1 C4 C5 115.47(18) . . ? N2 C4 C5 118.67(18) . . ? N4 C5 N3 125.7(2) . . ? N4 C5 C4 113.36(18) . . ? N3 C5 C4 120.91(19) . . ? C5 N3 C6 122.4(2) . . ? N3 C6 C7 107.6(2) . . ? C8 C7 C6 109.9(3) . . ? N4 C8 C7 112.8(2) . . ? C5 N4 C8 116.64(19) . . ? C5 N4 Fe1 114.48(15) . . ? C8 N4 Fe1 128.04(14) . . ? C12 N5 C9 129.1(7) . . ? C12 N5 Fe1 114.5(5) . . ? C9 N5 Fe1 116.4(5) . . ? C10 C9 N5 109.0(6) . . ? C11 C10 C9 113.2(7) . . ? N6 C11 C10 108.7(5) . . ? C11 N6 C12 129.5(5) . . ? N5 C12 C13 114.2(6) . . ? N5 C12 N6 106.9(6) . . ? C13 C12 N6 135.9(6) . . ? N8 C13 N7 143.9(6) . . ? N8 C13 C12 115.0(6) . . ? N7 C13 C12 100.5(6) . . ? C13 N7 C14 105.7(5) . . ? N7 C14 C15 110.1(5) . . ? C14 C15 C16 106.3(5) . . ? N8 C16 C15 122.1(6) . . ? C16 N8 C13 102.5(5) . . ? C16 N8 Fe1 141.0(5) . . ? C13 N8 Fe1 114.0(4) . . ? C17 N9 C21 118.0(7) . . ? C17 N9 Fe1 129.5(6) . . ? C21 N9 Fe1 112.4(5) . . ? C18 C17 N9 123.9(7) . . ? C17 C18 C19 120.5(6) . . ? C20 C19 C18 117.2(7) . . ? C19 C20 C21 118.1(7) . . ? C22 C21 N9 117.5(7) . . ? C22 C21 C20 119.4(8) . . ? N9 C21 C20 120.8(7) . . ? C23 C22 C21 123.2(7) . . ? C23 C22 N10 126.7(6) . . ? C21 C22 N10 108.9(7) . . ? C22 C23 C24 112.9(6) . . ? C25 C24 C23 119.9(6) . . ? C26 C25 C24 116.7(5) . . ? N10 C26 C25 122.9(5) . . ? C26 N10 C22 116.2(6) . . ? C26 N10 Fe1 127.7(5) . . ? C22 N10 Fe1 114.9(5) . . ? C17A N9A C21A 106.9(6) . . ? C17A N9A Fe1 135.8(6) . . ? C21A N9A Fe1 116.4(5) . . ? N9A C17A C18A 128.6(7) . . ? C17A C18A C19A 116.9(7) . . ? C20A C19A C18A 119.9(6) . . ? C21A C20A C19A 105.9(5) . . ? C20A C21A N9A 140.5(6) . . ? C20A C21A C22A 104.4(5) . . ? N9A C21A C22A 113.9(6) . . ? N10A C22A C23A 106.1(6) . . ? N10A C22A C21A 111.4(5) . . ? C23A C22A C21A 142.5(6) . . ? C24A C23A C22A 129.0(6) . . ? C25A C24A C23A 119.6(5) . . ? C24A C25A C26A 121.0(6) . . ? C25A C26A N10A 113.7(5) . . ? C22A N10A C26A 128.8(6) . . ? C22A N10A Fe1 117.9(4) . . ? C26A N10A Fe1 113.1(4) . . ? C12A N5A C9A 118.5(7) . . ? C12A N5A Fe1 118.6(6) . . ? C9A N5A Fe1 122.9(5) . . ? N5A C9A C10A 113.9(7) . . ? C11A C10A C9A 110.8(6) . . ? N6A C11A C10A 112.9(6) . . ? C12A N6A C11A 118.9(7) . . ? N5A C12A N6A 127.2(7) . . ? N5A C12A C13A 110.3(7) . . ? N6A C12A C13A 120.9(7) . . ? N8A C13A N7A 122.2(7) . . ? N8A C13A C12A 115.8(7) . . ? N7A C13A C12A 120.1(6) . . ? C13A N7A C14A 125.7(6) . . ? N7A C14A C15A 100.0(6) . . ? C14A C15A C16A 110.7(6) . . ? N8A C16A C15A 111.3(5) . . ? C13A N8A C16A 118.8(6) . . ? C13A N8A Fe1 114.6(5) . . ? C16A N8A Fe1 126.1(5) . . ? C27 B1 C39 109.0(2) . . ? C27 B1 C45 108.58(19) . . ? C39 B1 C45 107.0(2) . . ? C27 B1 C33 108.8(2) . . ? C39 B1 C33 111.57(19) . . ? C45 B1 C33 111.8(2) . . ? C28 C27 C32 116.1(2) . . ? C28 C27 B1 122.4(2) . . ? C32 C27 B1 121.0(2) . . ? C27 C28 C29 122.0(3) . . ? C30 C29 C28 119.6(3) . . ? C31 C30 C29 120.6(2) . . ? C30 C31 C32 119.0(3) . . ? C31 C32 C27 122.6(3) . . ? C38 C33 C34 114.1(2) . . ? C38 C33 B1 126.1(2) . . ? C34 C33 B1 119.8(2) . . ? C35 C34 C33 123.2(3) . . ? C36 C35 C34 120.1(3) . . ? C35 C36 C37 119.1(3) . . ? C36 C37 C38 120.1(3) . . ? C33 C38 C37 123.4(3) . . ? C40 C39 C44 115.5(2) . . ? C40 C39 B1 122.4(2) . . ? C44 C39 B1 122.0(2) . . ? C41 C40 C39 121.6(3) . . ? C40 C41 C42 121.2(3) . . ? C43 C42 C41 119.2(3) . . ? C42 C43 C44 118.9(3) . . ? C43 C44 C39 123.7(3) . . ? C50 C45 C46 113.9(2) . . ? C50 C45 B1 123.1(2) . . ? C46 C45 B1 122.9(2) . . ? C47 C46 C45 124.3(2) . . ? C48 C47 C46 119.7(2) . . ? C47 C48 C49 118.3(2) . . ? C48 C49 C50 121.2(2) . . ? C49 C50 C45 122.5(2) . . ? C63 B2 C51 109.9(2) . . ? C63 B2 C57 109.5(2) . . ? C51 B2 C57 109.1(2) . . ? C63 B2 C69 108.1(2) . . ? C51 B2 C69 110.6(2) . . ? C57 B2 C69 109.6(2) . . ? C56 C51 C52 114.5(3) . . ? C56 C51 B2 124.7(3) . . ? C52 C51 B2 120.8(3) . . ? C53 C52 C51 122.9(3) . . ? C54 C53 C52 120.3(3) . . ? C55 C54 C53 118.5(3) . . ? C54 C55 C56 121.0(3) . . ? C51 C56 C55 122.8(3) . . ? C62 C57 C58 114.0(3) . . ? C62 C57 B2 122.1(3) . . ? C58 C57 B2 123.7(3) . . ? C59 C58 C57 123.9(4) . . ? C60 C59 C58 119.6(4) . . ? C59 C60 C61 119.6(4) . . ? C60 C61 C62 119.7(4) . . ? C57 C62 C61 123.1(4) . . ? C64 C63 C68 115.4(2) . . ? C64 C63 B2 120.1(3) . . ? C68 C63 B2 124.3(2) . . ? C65 C64 C63 121.7(3) . . ? C64 C65 C66 121.2(3) . . ? C67 C66 C65 119.2(3) . . ? C66 C67 C68 119.2(3) . . ? C67 C68 C63 123.2(3) . . ? C70 C69 C74 114.4(3) . . ? C70 C69 B2 124.6(2) . . ? C74 C69 B2 120.9(3) . . ? C69 C70 C71 124.0(3) . . ? C72 C71 C70 120.6(4) . . ? C71 C72 C73 117.7(4) . . ? C72 C73 C74 122.3(4) . . ? C69 C74 C73 120.9(4) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 28.55 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.754 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.100 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 156.3 44.5 2 0.500 0.500 0.500 50.4 5.8 _platon_squeeze_details ; ; #===END data_4-BPh4 _database_code_depnum_ccdc_archive 'CCDC 768565' #TrackingRef '- 1-4.cif' _audit_creation_method 'Bruker SHELXTL' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H36 Fe N10, 2(C24 H20 B)' _chemical_formula_sum 'C76 H76 B2 Fe N10' _chemical_formula_weight 1206.94 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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 45.6638(8) _cell_length_b 12.6323(2) _cell_length_c 24.6196(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.8310(10) _cell_angle_gamma 90.00 _cell_volume 14033.2(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9948 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 26.39 _exptl_crystal_description needle _exptl_crystal_colour purple _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5104 _exptl_absorpt_coefficient_mu 0.263 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8824 _exptl_absorpt_correction_T_max 0.9769 _exptl_absorpt_process_details 'SADABS, Bruker(2000)' _exptl_special_details ; ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55026 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -56 _diffrn_reflns_limit_h_max 56 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 0.90 _diffrn_reflns_theta_max 26.39 _reflns_number_total 14371 _reflns_number_gt 9862 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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. SQUEEZE Summary and Remarks : N = NOTE, W = WARNING, E = ERROR #=============================================================================== N: No S.U.'s (esd) on observed/calculated parameters. N: DISORDERED structure - ATOMS with Pop. .LT. 1.0 are not moved or as a group. #------------------------------------------------------------------------------- N: Number of moved primary input atoms: .................................. 45 N: Number of Ignored Lines on INPUT ...................................... 5 of which blank in column 1 ..................................... 5 N: Total Potential Solvent Accessible Void Vol .................. 2327.6 Ang^3 N: Electron Count / Cell = 858 - To be included in D(calc), F000 & Mol.Wght. #=============================================================================== with Z = 8, this works out to 2.55 CH2Cl2 per formula unit Responding to errors on checkcif: B: Isotropic non-H atoms in main residue(s)...1. C7 is the central methylene carbon on the H2bip ligand. We refined it with isotropic displacement parameters due to positional disorder. The occupancy of the majority component is 76%. ; _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^)+(0.1008P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14371 _refine_ls_number_parameters 802 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1653 _refine_ls_wR_factor_gt 0.1542 _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 0.109916(7) 0.18620(3) 0.185437(14) 0.01730(11) Uani 1 1 d . . . N1 N 0.12640(4) 0.13247(16) 0.25948(8) 0.0179(4) Uani 1 1 d . . . N2 N 0.13378(5) 0.17660(17) 0.35407(8) 0.0226(5) Uani 1 1 d . . . H2 H 0.1292 0.2205 0.3792 0.027 Uiso 1 1 calc R . . N3 N 0.09745(5) 0.35564(18) 0.32272(9) 0.0269(5) Uani 1 1 d . A . H3 H 0.1021 0.3381 0.3576 0.032 Uiso 1 1 calc R . . N4 N 0.09970(4) 0.30585(16) 0.23120(8) 0.0185(4) Uani 1 1 d . A . N5 N 0.06996(4) 0.12622(16) 0.18564(8) 0.0192(4) Uani 1 1 d . . . N6 N 0.02223(5) 0.11201(18) 0.13254(9) 0.0271(5) Uani 1 1 d . . . H6 H 0.0111 0.1269 0.1010 0.033 Uiso 1 1 calc R . . N7 N 0.04151(5) 0.26780(18) 0.06275(9) 0.0259(5) Uani 1 1 d . . . H7 H 0.0229 0.2475 0.0572 0.031 Uiso 1 1 calc R . . N8 N 0.08921(5) 0.24665(17) 0.11607(8) 0.0209(5) Uani 1 1 d . . . N9 N 0.12385(4) 0.06339(16) 0.14782(8) 0.0188(4) Uani 1 1 d . . . N10 N 0.14945(5) 0.24142(17) 0.17849(8) 0.0203(5) Uani 1 1 d . . . C1 C 0.14445(6) 0.0366(2) 0.27197(10) 0.0218(6) Uani 1 1 d . . . H1A H 0.1650 0.0518 0.2662 0.026 Uiso 1 1 calc R . . H1B H 0.1366 -0.0200 0.2459 0.026 Uiso 1 1 calc R . . C2 C 0.14497(6) -0.0034(2) 0.33003(10) 0.0235(6) Uani 1 1 d . . . H2A H 0.1596 -0.0614 0.3376 0.028 Uiso 1 1 calc R . . H2B H 0.1252 -0.0317 0.3342 0.028 Uiso 1 1 calc R . . C3 C 0.15317(6) 0.0860(2) 0.37066(11) 0.0274(6) Uani 1 1 d . . . H3A H 0.1507 0.0628 0.4081 0.033 Uiso 1 1 calc R . . H3B H 0.1741 0.1065 0.3711 0.033 Uiso 1 1 calc R . . C4 C 0.12275(5) 0.1936(2) 0.30042(10) 0.0184(5) Uani 1 1 d . . . C5 C 0.10553(5) 0.29166(19) 0.28419(10) 0.0184(5) Uani 1 1 d . . . C6 C 0.08113(7) 0.4540(2) 0.30826(12) 0.0339(7) Uani 1 1 d . . . H6A H 0.0880 0.5094 0.3357 0.041 Uiso 0.762(8) 1 calc PR A 1 H6B H 0.0597 0.4423 0.3083 0.041 Uiso 0.762(8) 1 calc PR A 1 H6C H 0.0663 0.4644 0.3331 0.041 Uiso 0.238(8) 1 d PR A 2 H6D H 0.0950 0.5146 0.3131 0.041 Uiso 0.238(8) 1 d PR A 2 C7A C 0.08621(8) 0.4899(3) 0.25205(13) 0.0232(11) Uiso 0.762(8) 1 d P A 1 H7A H 0.0719 0.5466 0.2390 0.028 Uiso 0.762(8) 1 calc PR A 1 H7B H 0.1064 0.5200 0.2547 0.028 Uiso 0.762(8) 1 calc PR A 1 C7B C 0.0673(3) 0.4515(10) 0.2552(5) 0.027(4) Uiso 0.238(8) 1 d P A 2 H7C H 0.0625 0.5254 0.2439 0.033 Uiso 0.238(8) 1 calc PR A 2 H7D H 0.0483 0.4138 0.2547 0.033 Uiso 0.238(8) 1 calc PR A 2 C8 C 0.08291(6) 0.4018(2) 0.21132(11) 0.0260(6) Uani 1 1 d . . . H8A H 0.0617 0.3834 0.2021 0.031 Uiso 0.762(8) 1 calc PR A 1 H8B H 0.0897 0.4264 0.1772 0.031 Uiso 0.762(8) 1 calc PR A 1 H8C H 0.0681 0.3833 0.1791 0.031 Uiso 0.238(8) 1 d PR A 2 H8D H 0.0967 0.4544 0.1993 0.031 Uiso 0.238(8) 1 d PR A 2 C9 C 0.06121(6) 0.0535(2) 0.22661(10) 0.0226(6) Uani 1 1 d . . . H9A H 0.0557 0.0953 0.2575 0.027 Uiso 1 1 calc R . . H9B H 0.0785 0.0090 0.2414 0.027 Uiso 1 1 calc R . . C10 C 0.03546(6) -0.0181(2) 0.20413(12) 0.0296(6) Uani 1 1 d . . . H10B H 0.0423 -0.0721 0.1797 0.036 Uiso 1 1 calc R . . H10A H 0.0282 -0.0553 0.2349 0.036 Uiso 1 1 calc R . . C11 C 0.01040(6) 0.0455(2) 0.17225(12) 0.0324(7) Uani 1 1 d . . . H11B H -0.0048 -0.0028 0.1530 0.039 Uiso 1 1 calc R . . H11A H 0.0010 0.0901 0.1978 0.039 Uiso 1 1 calc R . . C12 C 0.05005(5) 0.1511(2) 0.14350(10) 0.0204(5) Uani 1 1 d . . . C13 C 0.06099(6) 0.2276(2) 0.10507(10) 0.0202(5) Uani 1 1 d . . . C14 C 0.05248(7) 0.3460(3) 0.02647(12) 0.0354(7) Uani 1 1 d . . . H14B H 0.0510 0.4180 0.0417 0.042 Uiso 1 1 calc R . . H14A H 0.0402 0.3437 -0.0103 0.042 Uiso 1 1 calc R . . C15 C 0.08383(7) 0.3222(3) 0.02164(13) 0.0412(8) Uani 1 1 d . . . H15B H 0.0917 0.3781 -0.0003 0.049 Uiso 1 1 calc R . . H15A H 0.0849 0.2539 0.0024 0.049 Uiso 1 1 calc R . . C16 C 0.10259(6) 0.3163(2) 0.07897(11) 0.0269(6) Uani 1 1 d . . . H16A H 0.1226 0.2898 0.0755 0.032 Uiso 1 1 calc R . . H16B H 0.1048 0.3883 0.0950 0.032 Uiso 1 1 calc R . . C17 C 0.10940(6) -0.0274(2) 0.13012(10) 0.0238(6) Uani 1 1 d . . . H17A H 0.0889 -0.0335 0.1320 0.029 Uiso 1 1 calc R . . C18 C 0.12392(7) -0.1112(2) 0.10931(13) 0.0382(7) Uani 1 1 d . . . H18A H 0.1132 -0.1737 0.0978 0.046 Uiso 1 1 calc R . . C19 C 0.15344(7) -0.1054(2) 0.10511(12) 0.0329(7) Uani 1 1 d . . . H19A H 0.1634 -0.1642 0.0923 0.039 Uiso 1 1 calc R . . C20 C 0.16867(6) -0.0102(2) 0.12021(11) 0.0264(6) Uani 1 1 d . . . C21 C 0.15278(5) 0.0710(2) 0.14123(10) 0.0213(6) Uani 1 1 d . . . C22 C 0.16688(5) 0.1695(2) 0.15817(10) 0.0214(5) Uani 1 1 d . . . C23 C 0.19660(6) 0.1856(2) 0.15350(12) 0.0309(6) Uani 1 1 d . . . C24 C 0.20907(7) 0.2848(3) 0.17132(14) 0.0408(8) Uani 1 1 d . . . H24A H 0.2296 0.2981 0.1717 0.049 Uiso 1 1 calc R . . C25 C 0.19112(6) 0.3610(2) 0.18794(14) 0.0366(7) Uani 1 1 d . . . H25A H 0.1985 0.4306 0.1956 0.044 Uiso 1 1 calc R . . C26 C 0.16168(6) 0.3366(2) 0.19368(11) 0.0244(6) Uani 1 1 d . . . H26A H 0.1501 0.3884 0.2086 0.029 Uiso 1 1 calc R . . B1 B 0.05766(6) 0.2573(2) 0.46860(11) 0.0203(6) Uani 1 1 d . . . B2 B 0.18072(6) 0.6768(2) 0.27696(12) 0.0205(6) Uani 1 1 d . . . C27 C 0.19883(8) 0.0084(3) 0.11600(17) 0.0525(9) Uani 1 1 d . . . H27A H 0.2101 -0.0463 0.1025 0.063 Uiso 1 1 calc R . . C28 C 0.21216(7) 0.1037(3) 0.13094(17) 0.0533(10) Uani 1 1 d . . . H28A H 0.2322 0.1148 0.1261 0.064 Uiso 1 1 calc R . . C29 C 0.05138(6) 0.2726(2) 0.53209(10) 0.0211(5) Uani 1 1 d . . . C30 C 0.02466(6) 0.2393(2) 0.54829(11) 0.0246(6) Uani 1 1 d . . . H30A H 0.0097 0.2105 0.5212 0.030 Uiso 1 1 calc R . . C31 C 0.01908(6) 0.2466(2) 0.60218(11) 0.0282(6) Uani 1 1 d . . . H31A H 0.0008 0.2219 0.6113 0.034 Uiso 1 1 calc R . . C32 C 0.04021(6) 0.2897(2) 0.64263(11) 0.0289(6) Uani 1 1 d . . . H32A H 0.0368 0.2934 0.6797 0.035 Uiso 1 1 calc R . . C33 C 0.06666(6) 0.3278(2) 0.62777(11) 0.0285(6) Uani 1 1 d . . . H33A H 0.0811 0.3597 0.6547 0.034 Uiso 1 1 calc R . . C34 C 0.07183(6) 0.3189(2) 0.57384(11) 0.0242(6) Uani 1 1 d . . . H34A H 0.0900 0.3453 0.5648 0.029 Uiso 1 1 calc R . . C35 C 0.09088(6) 0.3047(2) 0.46394(9) 0.0203(5) Uani 1 1 d . . . C36 C 0.09581(6) 0.4104(2) 0.45029(10) 0.0261(6) Uani 1 1 d . . . H36A H 0.0792 0.4560 0.4419 0.031 Uiso 1 1 calc R . . C37 C 0.12385(6) 0.4514(2) 0.44844(11) 0.0315(7) Uani 1 1 d . . . H37A H 0.1260 0.5233 0.4385 0.038 Uiso 1 1 calc R . . C38 C 0.14859(6) 0.3878(3) 0.46106(11) 0.0334(7) Uani 1 1 d . . . H38A H 0.1678 0.4154 0.4596 0.040 Uiso 1 1 calc R . . C39 C 0.14506(6) 0.2834(3) 0.47581(11) 0.0321(7) Uani 1 1 d . . . H39A H 0.1619 0.2394 0.4852 0.039 Uiso 1 1 calc R . . C40 C 0.11666(6) 0.2426(2) 0.47689(10) 0.0247(6) Uani 1 1 d . . . H40A H 0.1147 0.1705 0.4867 0.030 Uiso 1 1 calc R . . C41 C 0.05673(5) 0.1308(2) 0.45077(10) 0.0212(5) Uani 1 1 d . . . C42 C 0.06737(5) 0.0979(2) 0.40279(10) 0.0203(5) Uani 1 1 d . . . H42A H 0.0750 0.1500 0.3809 0.024 Uiso 1 1 calc R . . C43 C 0.06731(5) -0.0073(2) 0.38591(11) 0.0235(6) Uani 1 1 d . . . H43A H 0.0747 -0.0253 0.3531 0.028 Uiso 1 1 calc R . . C44 C 0.05640(6) -0.0861(2) 0.41699(12) 0.0286(6) Uani 1 1 d . . . H44A H 0.0560 -0.1579 0.4055 0.034 Uiso 1 1 calc R . . C45 C 0.04613(7) -0.0573(2) 0.46510(12) 0.0332(7) Uani 1 1 d . . . H45A H 0.0389 -0.1101 0.4871 0.040 Uiso 1 1 calc R . . C46 C 0.04627(6) 0.0484(2) 0.48139(12) 0.0291(6) Uani 1 1 d . . . H46A H 0.0390 0.0656 0.5145 0.035 Uiso 1 1 calc R . . C47 C 0.03292(5) 0.3255(2) 0.42678(10) 0.0197(5) Uani 1 1 d . . . C48 C 0.02425(6) 0.3020(2) 0.37095(11) 0.0238(6) Uani 1 1 d . . . H48A H 0.0320 0.2404 0.3562 0.029 Uiso 1 1 calc R . . C49 C 0.00476(6) 0.3656(2) 0.33635(10) 0.0271(6) Uani 1 1 d . . . H49A H -0.0009 0.3458 0.2990 0.033 Uiso 1 1 calc R . . C50 C -0.00643(6) 0.4575(2) 0.35580(11) 0.0276(6) Uani 1 1 d . . . H50A H -0.0194 0.5018 0.3319 0.033 Uiso 1 1 calc R . . C51 C 0.00148(6) 0.4839(2) 0.41040(11) 0.0267(6) Uani 1 1 d . . . H51A H -0.0061 0.5467 0.4244 0.032 Uiso 1 1 calc R . . C52 C 0.02058(6) 0.4183(2) 0.44512(10) 0.0227(6) Uani 1 1 d . . . H52A H 0.0254 0.4372 0.4828 0.027 Uiso 1 1 calc R . . C53 C 0.14697(5) 0.7064(2) 0.28885(11) 0.0205(5) Uani 1 1 d . . . C54 C 0.12534(6) 0.7530(2) 0.24963(11) 0.0235(6) Uani 1 1 d . . . H54A H 0.1300 0.7672 0.2141 0.028 Uiso 1 1 calc R . . C55 C 0.09725(6) 0.7793(2) 0.26059(11) 0.0268(6) Uani 1 1 d . . . H55A H 0.0831 0.8088 0.2324 0.032 Uiso 1 1 calc R . . C56 C 0.08986(6) 0.7627(2) 0.31211(12) 0.0279(6) Uani 1 1 d . . . H56A H 0.0706 0.7798 0.3195 0.033 Uiso 1 1 calc R . . C57 C 0.11088(6) 0.7208(2) 0.35299(12) 0.0271(6) Uani 1 1 d . . . H57A H 0.1063 0.7107 0.3890 0.033 Uiso 1 1 calc R . . C58 C 0.13892(6) 0.6935(2) 0.34116(11) 0.0238(6) Uani 1 1 d . . . H58A H 0.1531 0.6651 0.3697 0.029 Uiso 1 1 calc R . . C59 C 0.20141(5) 0.7721(2) 0.30806(11) 0.0229(6) Uani 1 1 d . . . C60 C 0.20641(6) 0.8690(2) 0.28296(12) 0.0275(6) Uani 1 1 d . . . H60A H 0.1989 0.8782 0.2451 0.033 Uiso 1 1 calc R . . C61 C 0.22192(6) 0.9522(2) 0.31141(14) 0.0362(7) Uani 1 1 d . . . H61A H 0.2254 1.0156 0.2926 0.043 Uiso 1 1 calc R . . C62 C 0.23229(7) 0.9423(3) 0.36698(15) 0.0435(8) Uani 1 1 d . . . H62A H 0.2426 0.9991 0.3867 0.052 Uiso 1 1 calc R . . C63 C 0.22750(7) 0.8489(3) 0.39357(13) 0.0410(8) Uani 1 1 d . . . H63A H 0.2343 0.8418 0.4318 0.049 Uiso 1 1 calc R . . C64 C 0.21275(6) 0.7654(2) 0.36443(11) 0.0291(6) Uani 1 1 d . . . H64A H 0.2102 0.7012 0.3833 0.035 Uiso 1 1 calc R . . C65 C 0.19207(6) 0.5602(2) 0.30181(10) 0.0228(6) Uani 1 1 d . . . C66 C 0.22149(6) 0.5287(2) 0.29962(12) 0.0323(7) Uani 1 1 d . . . H66A H 0.2346 0.5788 0.2876 0.039 Uiso 1 1 calc R . . C67 C 0.23214(7) 0.4289(3) 0.31403(13) 0.0397(8) Uani 1 1 d . . . H67A H 0.2520 0.4111 0.3109 0.048 Uiso 1 1 calc R . . C68 C 0.21385(7) 0.3540(2) 0.33322(13) 0.0378(7) Uani 1 1 d . . . H68A H 0.2210 0.2852 0.3434 0.045 Uiso 1 1 calc R . . C69 C 0.18531(7) 0.3817(2) 0.33715(12) 0.0345(7) Uani 1 1 d . . . H69A H 0.1726 0.3320 0.3509 0.041 Uiso 1 1 calc R . . C70 C 0.17454(6) 0.4828(2) 0.32113(11) 0.0248(6) Uani 1 1 d . . . H70A H 0.1545 0.4991 0.3236 0.030 Uiso 1 1 calc R . . C71 C 0.18306(6) 0.6674(2) 0.21095(11) 0.0218(6) Uani 1 1 d . . . C72 C 0.20877(6) 0.6950(2) 0.18949(11) 0.0249(6) Uani 1 1 d . . . H72A H 0.2245 0.7289 0.2128 0.030 Uiso 1 1 calc R . . C73 C 0.21202(6) 0.6745(2) 0.13530(12) 0.0301(6) Uani 1 1 d . . . H73A H 0.2299 0.6937 0.1225 0.036 Uiso 1 1 calc R . . C74 C 0.18968(6) 0.6267(2) 0.09988(11) 0.0311(7) Uani 1 1 d . . . H74A H 0.1920 0.6131 0.0628 0.037 Uiso 1 1 calc R . . C75 C 0.16384(6) 0.5988(2) 0.11898(11) 0.0275(6) Uani 1 1 d . . . H75A H 0.1481 0.5665 0.0949 0.033 Uiso 1 1 calc R . . C76 C 0.16082(6) 0.6178(2) 0.17341(11) 0.0232(6) Uani 1 1 d . . . H76A H 0.1430 0.5965 0.1859 0.028 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 0.02087(19) 0.01347(19) 0.01774(18) -0.00189(14) 0.00352(14) -0.00058(14) N1 0.0189(10) 0.0148(11) 0.0204(10) -0.0009(9) 0.0040(8) -0.0009(8) N2 0.0321(12) 0.0184(12) 0.0177(10) -0.0011(9) 0.0051(9) -0.0002(9) N3 0.0432(14) 0.0202(12) 0.0183(11) 0.0006(9) 0.0083(10) 0.0057(10) N4 0.0215(10) 0.0142(11) 0.0198(10) -0.0012(8) 0.0032(8) -0.0003(8) N5 0.0230(11) 0.0151(11) 0.0200(10) 0.0000(9) 0.0044(9) 0.0006(9) N6 0.0231(11) 0.0273(13) 0.0285(12) 0.0033(10) -0.0039(9) -0.0029(10) N7 0.0263(12) 0.0273(13) 0.0228(11) 0.0044(10) -0.0007(9) 0.0011(10) N8 0.0288(12) 0.0155(11) 0.0188(10) -0.0022(9) 0.0049(9) 0.0020(9) N9 0.0244(11) 0.0157(11) 0.0165(10) -0.0001(8) 0.0037(8) -0.0012(9) N10 0.0249(11) 0.0169(11) 0.0187(10) -0.0043(9) 0.0020(9) -0.0036(9) C1 0.0232(13) 0.0192(14) 0.0225(13) -0.0006(11) 0.0019(10) 0.0027(11) C2 0.0253(13) 0.0190(14) 0.0271(14) 0.0029(11) 0.0070(11) -0.0003(11) C3 0.0337(15) 0.0274(15) 0.0201(13) 0.0045(11) 0.0008(11) 0.0001(12) C4 0.0200(12) 0.0164(13) 0.0193(12) -0.0005(10) 0.0041(10) -0.0048(10) C5 0.0218(12) 0.0109(12) 0.0228(13) -0.0015(10) 0.0046(10) -0.0041(10) C6 0.0523(19) 0.0184(15) 0.0332(16) 0.0003(12) 0.0140(14) 0.0072(13) C8 0.0323(15) 0.0173(14) 0.0276(14) 0.0002(11) 0.0020(11) 0.0086(11) C9 0.0239(13) 0.0213(14) 0.0225(13) 0.0025(11) 0.0036(10) 0.0006(11) C10 0.0256(14) 0.0272(16) 0.0358(16) 0.0042(13) 0.0037(12) -0.0032(12) C11 0.0283(15) 0.0277(16) 0.0406(17) 0.0074(13) 0.0032(13) -0.0029(12) C12 0.0236(13) 0.0137(13) 0.0234(13) -0.0029(10) 0.0024(10) 0.0009(10) C13 0.0269(14) 0.0150(13) 0.0179(12) -0.0047(10) 0.0008(10) 0.0034(11) C14 0.0403(17) 0.0395(18) 0.0262(15) 0.0130(13) 0.0048(13) 0.0003(14) C15 0.052(2) 0.0378(19) 0.0336(17) 0.0051(14) 0.0056(14) -0.0042(15) C16 0.0316(14) 0.0240(15) 0.0258(14) 0.0068(12) 0.0057(11) -0.0029(12) C17 0.0270(14) 0.0197(14) 0.0241(13) -0.0025(11) 0.0021(11) -0.0040(11) C18 0.0440(18) 0.0246(16) 0.0479(19) -0.0129(14) 0.0130(15) -0.0070(14) C19 0.0393(16) 0.0211(15) 0.0378(16) -0.0063(12) 0.0044(13) 0.0053(13) C20 0.0263(14) 0.0208(14) 0.0313(15) -0.0068(12) 0.0019(11) 0.0073(11) C21 0.0253(13) 0.0189(14) 0.0186(12) -0.0022(10) -0.0002(10) 0.0034(11) C22 0.0235(13) 0.0194(14) 0.0222(12) -0.0030(11) 0.0059(10) 0.0008(11) C23 0.0233(14) 0.0278(16) 0.0430(17) -0.0094(13) 0.0098(12) -0.0006(12) C24 0.0298(16) 0.0343(18) 0.062(2) -0.0122(16) 0.0170(15) -0.0089(13) C25 0.0312(15) 0.0206(15) 0.057(2) -0.0097(14) 0.0042(14) -0.0079(13) C26 0.0279(14) 0.0180(14) 0.0285(14) -0.0045(11) 0.0079(11) -0.0007(11) B1 0.0245(15) 0.0186(15) 0.0173(14) 0.0021(12) 0.0019(11) 0.0003(12) B2 0.0183(14) 0.0202(16) 0.0232(14) -0.0018(12) 0.0041(11) -0.0007(12) C27 0.0414(19) 0.042(2) 0.075(3) -0.0170(19) 0.0107(18) 0.0078(16) C28 0.0333(18) 0.042(2) 0.086(3) -0.0138(19) 0.0141(18) 0.0014(15) C29 0.0277(13) 0.0145(13) 0.0205(12) 0.0009(10) 0.0018(10) 0.0037(11) C30 0.0285(14) 0.0216(14) 0.0230(13) 0.0013(11) 0.0015(11) 0.0039(11) C31 0.0327(15) 0.0269(16) 0.0263(14) 0.0062(12) 0.0090(12) 0.0072(12) C32 0.0422(17) 0.0254(15) 0.0199(13) 0.0052(11) 0.0069(12) 0.0128(13) C33 0.0385(16) 0.0243(15) 0.0200(13) -0.0015(11) -0.0036(12) 0.0066(12) C34 0.0266(13) 0.0204(14) 0.0245(13) 0.0013(11) 0.0005(11) 0.0019(11) C35 0.0264(13) 0.0226(14) 0.0114(11) -0.0031(10) 0.0012(10) 0.0001(11) C36 0.0289(14) 0.0272(15) 0.0217(13) 0.0045(11) 0.0026(11) -0.0027(12) C37 0.0360(16) 0.0345(17) 0.0232(14) 0.0027(12) 0.0026(12) -0.0104(13) C38 0.0288(15) 0.051(2) 0.0206(14) -0.0064(13) 0.0061(11) -0.0143(14) C39 0.0265(14) 0.0449(19) 0.0240(14) -0.0151(13) 0.0005(11) 0.0034(13) C40 0.0294(14) 0.0232(15) 0.0204(13) -0.0056(11) 0.0007(11) -0.0013(11) C41 0.0211(13) 0.0196(14) 0.0222(13) -0.0020(11) 0.0012(10) -0.0004(11) C42 0.0190(12) 0.0183(14) 0.0237(13) 0.0014(11) 0.0038(10) -0.0004(10) C43 0.0192(13) 0.0234(15) 0.0278(14) -0.0039(11) 0.0029(11) 0.0000(11) C44 0.0299(14) 0.0187(15) 0.0380(16) -0.0029(12) 0.0077(12) 0.0021(12) C45 0.0429(17) 0.0202(15) 0.0392(17) 0.0058(13) 0.0149(14) -0.0021(13) C46 0.0359(15) 0.0215(15) 0.0314(15) 0.0021(12) 0.0102(12) 0.0017(12) C47 0.0221(12) 0.0164(13) 0.0209(12) 0.0009(10) 0.0041(10) -0.0038(10) C48 0.0258(13) 0.0229(15) 0.0232(13) -0.0047(11) 0.0050(11) -0.0021(11) C49 0.0304(14) 0.0339(17) 0.0161(12) -0.0020(11) 0.0004(11) 0.0006(13) C50 0.0269(14) 0.0285(16) 0.0262(14) 0.0063(12) 0.0008(11) 0.0009(12) C51 0.0300(14) 0.0196(14) 0.0304(14) -0.0032(12) 0.0041(12) 0.0005(12) C52 0.0296(14) 0.0203(14) 0.0177(12) 0.0002(10) 0.0023(11) -0.0018(11) C53 0.0192(12) 0.0147(13) 0.0278(14) -0.0037(10) 0.0038(10) -0.0050(10) C54 0.0241(13) 0.0199(14) 0.0262(13) -0.0064(11) 0.0033(11) 0.0014(11) C55 0.0240(14) 0.0218(15) 0.0330(15) -0.0095(12) -0.0002(11) 0.0049(11) C56 0.0225(13) 0.0191(14) 0.0436(17) -0.0122(13) 0.0102(12) -0.0012(11) C57 0.0280(14) 0.0206(14) 0.0357(15) -0.0034(12) 0.0142(12) -0.0030(12) C58 0.0236(13) 0.0209(14) 0.0275(14) -0.0017(11) 0.0055(11) -0.0015(11) C59 0.0135(12) 0.0264(15) 0.0299(14) -0.0042(12) 0.0067(10) 0.0002(11) C60 0.0192(13) 0.0242(15) 0.0400(16) -0.0056(13) 0.0077(12) -0.0002(11) C61 0.0251(14) 0.0247(16) 0.061(2) -0.0063(15) 0.0140(14) -0.0027(12) C62 0.0305(16) 0.045(2) 0.057(2) -0.0266(17) 0.0120(15) -0.0125(15) C63 0.0310(16) 0.056(2) 0.0367(17) -0.0157(16) 0.0068(13) -0.0132(15) C64 0.0231(14) 0.0360(17) 0.0290(15) -0.0055(13) 0.0061(11) -0.0079(12) C65 0.0243(13) 0.0242(15) 0.0205(13) -0.0010(11) 0.0052(10) 0.0029(11) C66 0.0294(15) 0.0313(17) 0.0385(16) 0.0128(13) 0.0128(13) 0.0081(13) C67 0.0343(16) 0.043(2) 0.0442(18) 0.0105(15) 0.0132(14) 0.0158(15) C68 0.0485(19) 0.0229(16) 0.0419(18) 0.0090(14) 0.0070(14) 0.0090(14) C69 0.0367(16) 0.0268(16) 0.0402(17) 0.0066(13) 0.0062(13) -0.0005(13) C70 0.0254(13) 0.0187(14) 0.0306(14) 0.0002(11) 0.0048(11) -0.0008(11) C71 0.0231(13) 0.0149(13) 0.0277(14) 0.0006(11) 0.0046(11) 0.0051(10) C72 0.0238(13) 0.0228(15) 0.0283(14) 0.0030(11) 0.0050(11) 0.0023(11) C73 0.0298(15) 0.0308(17) 0.0320(15) 0.0061(13) 0.0124(12) 0.0070(12) C74 0.0384(16) 0.0351(17) 0.0208(13) -0.0017(12) 0.0079(12) 0.0135(13) C75 0.0305(14) 0.0222(15) 0.0287(14) -0.0043(12) 0.0010(12) 0.0044(12) C76 0.0254(13) 0.0167(13) 0.0280(14) -0.0014(11) 0.0060(11) 0.0021(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 N9 1.962(2) . ? Fe1 N10 1.967(2) . ? Fe1 N8 1.974(2) . ? Fe1 N5 1.976(2) . ? Fe1 N1 1.982(2) . ? Fe1 N4 1.983(2) . ? N1 C4 1.300(3) . ? N1 C1 1.471(3) . ? N2 C4 1.356(3) . ? N2 C3 1.466(3) . ? N2 H2 0.8800 . ? N3 C5 1.340(3) . ? N3 C6 1.465(4) . ? N3 H3 0.8800 . ? N4 C5 1.303(3) . ? N4 C8 1.477(3) . ? N5 C12 1.308(3) . ? N5 C9 1.465(3) . ? N6 C12 1.351(3) . ? N6 C11 1.454(4) . ? N6 H6 0.8800 . ? N7 C13 1.360(3) . ? N7 C14 1.470(4) . ? N7 H7 0.8800 . ? N8 C13 1.298(3) . ? N8 C16 1.468(3) . ? N9 C21 1.359(3) . ? N9 C17 1.360(3) . ? N10 C22 1.353(3) . ? N10 C26 1.355(3) . ? C1 C2 1.513(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.517(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.489(3) . ? C6 C7B 1.361(11) . ? C6 C7A 1.507(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6 H6C 0.9900 . ? C6 H6D 0.9900 . ? C7A C8 1.490(4) . ? C7A H7A 0.9900 . ? C7A H7B 0.9900 . ? C7B C8 1.517(12) . ? C7B H7C 0.9900 . ? C7B H7D 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 H8C 0.9900 . ? C8 H8D 0.9900 . ? C9 C10 1.519(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.515(4) . ? C10 H10B 0.9900 . ? C10 H10A 0.9900 . ? C11 H11B 0.9900 . ? C11 H11A 0.9900 . ? C12 C13 1.491(4) . ? C14 C15 1.485(4) . ? C14 H14B 0.9900 . ? C14 H14A 0.9900 . ? C15 C16 1.536(4) . ? C15 H15B 0.9900 . ? C15 H15A 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.388(4) . ? C17 H17A 0.9500 . ? C18 C19 1.370(4) . ? C18 H18A 0.9500 . ? C19 C20 1.411(4) . ? C19 H19A 0.9500 . ? C20 C21 1.401(4) . ? C20 C27 1.416(4) . ? C21 C22 1.433(4) . ? C22 C23 1.395(4) . ? C23 C28 1.416(4) . ? C23 C24 1.417(4) . ? C24 C25 1.367(4) . ? C24 H24A 0.9500 . ? C25 C26 1.407(4) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? B1 C29 1.643(4) . ? B1 C47 1.649(4) . ? B1 C35 1.651(4) . ? B1 C41 1.656(4) . ? B2 C59 1.645(4) . ? B2 C65 1.647(4) . ? B2 C71 1.649(4) . ? B2 C53 1.655(4) . ? C27 C28 1.374(5) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.405(4) . ? C29 C34 1.406(4) . ? C30 C31 1.392(4) . ? C30 H30A 0.9500 . ? C31 C32 1.388(4) . ? C31 H31A 0.9500 . ? C32 C33 1.400(4) . ? C32 H32A 0.9500 . ? C33 C34 1.389(4) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C36 1.404(4) . ? C35 C40 1.410(4) . ? C36 C37 1.388(4) . ? C36 H36A 0.9500 . ? C37 C38 1.382(4) . ? C37 H37A 0.9500 . ? C38 C39 1.383(4) . ? C38 H38A 0.9500 . ? C39 C40 1.400(4) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 C42 1.407(4) . ? C41 C46 1.411(4) . ? C42 C43 1.391(4) . ? C42 H42A 0.9500 . ? C43 C44 1.394(4) . ? C43 H43A 0.9500 . ? C44 C45 1.388(4) . ? C44 H44A 0.9500 . ? C45 C46 1.394(4) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C47 C48 1.402(3) . ? C47 C52 1.405(4) . ? C48 C49 1.389(4) . ? C48 H48A 0.9500 . ? C49 C50 1.383(4) . ? C49 H49A 0.9500 . ? C50 C51 1.378(4) . ? C50 H50A 0.9500 . ? C51 C52 1.397(4) . ? C51 H51A 0.9500 . ? C52 H52A 0.9500 . ? C53 C54 1.400(4) . ? C53 C58 1.402(4) . ? C54 C55 1.391(4) . ? C54 H54A 0.9500 . ? C55 C56 1.377(4) . ? C55 H55A 0.9500 . ? C56 C57 1.385(4) . ? C56 H56A 0.9500 . ? C57 C58 1.399(4) . ? C57 H57A 0.9500 . ? C58 H58A 0.9500 . ? C59 C60 1.406(4) . ? C59 C64 1.407(4) . ? C60 C61 1.394(4) . ? C60 H60A 0.9500 . ? C61 C62 1.383(5) . ? C61 H61A 0.9500 . ? C62 C63 1.382(5) . ? C62 H62A 0.9500 . ? C63 C64 1.390(4) . ? C63 H63A 0.9500 . ? C64 H64A 0.9500 . ? C65 C70 1.393(4) . ? C65 C66 1.410(4) . ? C66 C67 1.378(4) . ? C66 H66A 0.9500 . ? C67 C68 1.391(4) . ? C67 H67A 0.9500 . ? C68 C69 1.367(4) . ? C68 H68A 0.9500 . ? C69 C70 1.403(4) . ? C69 H69A 0.9500 . ? C70 H70A 0.9500 . ? C71 C72 1.403(4) . ? C71 C76 1.411(4) . ? C72 C73 1.389(4) . ? C72 H72A 0.9500 . ? C73 C74 1.376(4) . ? C73 H73A 0.9500 . ? C74 C75 1.382(4) . ? C74 H74A 0.9500 . ? C75 C76 1.389(4) . ? C75 H75A 0.9500 . ? C76 H76A 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 N9 Fe1 N10 82.59(8) . . ? N9 Fe1 N8 92.55(8) . . ? N10 Fe1 N8 96.41(9) . . ? N9 Fe1 N5 93.70(8) . . ? N10 Fe1 N5 174.93(8) . . ? N8 Fe1 N5 80.25(9) . . ? N9 Fe1 N1 93.35(8) . . ? N10 Fe1 N1 88.71(8) . . ? N8 Fe1 N1 172.64(9) . . ? N5 Fe1 N1 94.98(8) . . ? N9 Fe1 N4 172.90(8) . . ? N10 Fe1 N4 94.48(8) . . ? N8 Fe1 N4 94.21(8) . . ? N5 Fe1 N4 89.59(8) . . ? N1 Fe1 N4 80.08(8) . . ? C4 N1 C1 117.5(2) . . ? C4 N1 Fe1 115.72(17) . . ? C1 N1 Fe1 126.56(16) . . ? C4 N2 C3 120.8(2) . . ? C4 N2 H2 119.6 . . ? C3 N2 H2 119.6 . . ? C5 N3 C6 121.6(2) . . ? C5 N3 H3 119.2 . . ? C6 N3 H3 119.2 . . ? C5 N4 C8 117.4(2) . . ? C5 N4 Fe1 115.73(16) . . ? C8 N4 Fe1 126.35(16) . . ? C12 N5 C9 117.9(2) . . ? C12 N5 Fe1 115.79(17) . . ? C9 N5 Fe1 126.29(16) . . ? C12 N6 C11 120.8(2) . . ? C12 N6 H6 119.6 . . ? C11 N6 H6 119.6 . . ? C13 N7 C14 118.2(2) . . ? C13 N7 H7 120.9 . . ? C14 N7 H7 120.9 . . ? C13 N8 C16 118.4(2) . . ? C13 N8 Fe1 115.91(17) . . ? C16 N8 Fe1 125.49(16) . . ? C21 N9 C17 117.0(2) . . ? C21 N9 Fe1 113.07(16) . . ? C17 N9 Fe1 129.87(17) . . ? C22 N10 C26 117.2(2) . . ? C22 N10 Fe1 113.17(16) . . ? C26 N10 Fe1 129.50(18) . . ? N1 C1 C2 113.5(2) . . ? N1 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? N1 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C1 C2 C3 109.9(2) . . ? C1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N2 C3 C2 108.7(2) . . ? N2 C3 H3A 110.0 . . ? C2 C3 H3A 110.0 . . ? N2 C3 H3B 110.0 . . ? C2 C3 H3B 110.0 . . ? H3A C3 H3B 108.3 . . ? N1 C4 N2 126.1(2) . . ? N1 C4 C5 114.3(2) . . ? N2 C4 C5 119.6(2) . . ? N4 C5 N3 126.1(2) . . ? N4 C5 C4 113.7(2) . . ? N3 C5 C4 120.2(2) . . ? C7B C6 N3 110.9(5) . . ? N3 C6 C7A 109.5(2) . . ? C7B C6 H6A 136.4 . . ? N3 C6 H6A 109.8 . . ? C7A C6 H6A 109.8 . . ? C7B C6 H6B 71.8 . . ? N3 C6 H6B 109.8 . . ? C7A C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? C7B C6 H6C 109.7 . . ? N3 C6 H6C 109.5 . . ? C7A C6 H6C 138.1 . . ? H6A C6 H6C 70.0 . . ? C7B C6 H6D 109.2 . . ? N3 C6 H6D 109.5 . . ? C7A C6 H6D 72.1 . . ? H6B C6 H6D 137.0 . . ? H6C C6 H6D 108.1 . . ? C8 C7A C6 112.3(3) . . ? C8 C7A H6D 143.0 . . ? C8 C7A H7A 109.1 . . ? C6 C7A H7A 109.1 . . ? H6D C7A H7A 103.5 . . ? C8 C7A H7B 109.1 . . ? C6 C7A H7B 109.1 . . ? H6D C7A H7B 75.8 . . ? H7A C7A H7B 107.9 . . ? C6 C7A H8D 144.0 . . ? H6D C7A H8D 146.3 . . ? H7A C7A H8D 102.4 . . ? H7B C7A H8D 76.0 . . ? C6 C7B C8 119.7(8) . . ? C6 C7B H7C 107.4 . . ? C8 C7B H7C 107.4 . . ? C6 C7B H7D 107.4 . . ? C8 C7B H7D 107.4 . . ? H7C C7B H7D 106.9 . . ? N4 C8 C7A 113.3(2) . . ? N4 C8 C7B 112.3(5) . . ? N4 C8 H8A 108.9 . . ? C7A C8 H8A 108.9 . . ? C7B C8 H8A 73.2 . . ? N4 C8 H8B 108.9 . . ? C7A C8 H8B 108.9 . . ? C7B C8 H8B 135.8 . . ? H8A C8 H8B 107.7 . . ? N4 C8 H8C 109.2 . . ? C7A C8 H8C 134.6 . . ? C7B C8 H8C 109.3 . . ? H8B C8 H8C 70.1 . . ? N4 C8 H8D 109.2 . . ? C7A C8 H8D 72.4 . . ? C7B C8 H8D 108.9 . . ? H8A C8 H8D 137.2 . . ? H8C C8 H8D 107.9 . . ? N5 C9 C10 113.6(2) . . ? N5 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? N5 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C11 C10 C9 110.7(2) . . ? C11 C10 H10B 109.5 . . ? C9 C10 H10B 109.5 . . ? C11 C10 H10A 109.5 . . ? C9 C10 H10A 109.5 . . ? H10B C10 H10A 108.1 . . ? N6 C11 C10 109.0(2) . . ? N6 C11 H11B 109.9 . . ? C10 C11 H11B 109.9 . . ? N6 C11 H11A 109.9 . . ? C10 C11 H11A 109.9 . . ? H11B C11 H11A 108.3 . . ? N5 C12 N6 126.0(2) . . ? N5 C12 C13 113.5(2) . . ? N6 C12 C13 120.4(2) . . ? N8 C13 N7 127.0(2) . . ? N8 C13 C12 114.0(2) . . ? N7 C13 C12 119.0(2) . . ? N7 C14 C15 109.5(2) . . ? N7 C14 H14B 109.8 . . ? C15 C14 H14B 109.8 . . ? N7 C14 H14A 109.8 . . ? C15 C14 H14A 109.8 . . ? H14B C14 H14A 108.2 . . ? C14 C15 C16 110.1(3) . . ? C14 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? C14 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? H15B C15 H15A 108.1 . . ? N8 C16 C15 112.0(2) . . ? N8 C16 H16A 109.2 . . ? C15 C16 H16A 109.2 . . ? N8 C16 H16B 109.2 . . ? C15 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? N9 C17 C18 121.7(2) . . ? N9 C17 H17A 119.2 . . ? C18 C17 H17A 119.2 . . ? C19 C18 C17 121.2(3) . . ? C19 C18 H18A 119.4 . . ? C17 C18 H18A 119.4 . . ? C18 C19 C20 118.4(3) . . ? C18 C19 H19A 120.8 . . ? C20 C19 H19A 120.8 . . ? C21 C20 C19 117.4(2) . . ? C21 C20 C27 118.1(3) . . ? C19 C20 C27 124.6(3) . . ? N9 C21 C20 124.1(2) . . ? N9 C21 C22 115.4(2) . . ? C20 C21 C22 120.5(2) . . ? N10 C22 C23 124.6(2) . . ? N10 C22 C21 115.3(2) . . ? C23 C22 C21 120.2(2) . . ? C22 C23 C28 118.6(3) . . ? C22 C23 C24 117.0(3) . . ? C28 C23 C24 124.4(3) . . ? C25 C24 C23 119.0(3) . . ? C25 C24 H24A 120.5 . . ? C23 C24 H24A 120.5 . . ? C24 C25 C26 120.1(3) . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? N10 C26 C25 121.8(2) . . ? N10 C26 H26A 119.1 . . ? C25 C26 H26A 119.1 . . ? C29 B1 C47 109.2(2) . . ? C29 B1 C35 108.6(2) . . ? C47 B1 C35 108.4(2) . . ? C29 B1 C41 111.4(2) . . ? C47 B1 C41 110.6(2) . . ? C35 B1 C41 108.5(2) . . ? C59 B2 C65 110.8(2) . . ? C59 B2 C71 113.0(2) . . ? C65 B2 C71 103.8(2) . . ? C59 B2 C53 103.6(2) . . ? C65 B2 C53 112.7(2) . . ? C71 B2 C53 113.2(2) . . ? C28 C27 C20 121.4(3) . . ? C28 C27 H27A 119.3 . . ? C20 C27 H27A 119.3 . . ? C27 C28 C23 121.1(3) . . ? C27 C28 H28A 119.4 . . ? C23 C28 H28A 119.4 . . ? C30 C29 C34 115.2(2) . . ? C30 C29 B1 121.4(2) . . ? C34 C29 B1 123.4(2) . . ? C31 C30 C29 123.0(2) . . ? C31 C30 H30A 118.5 . . ? C29 C30 H30A 118.5 . . ? C32 C31 C30 120.1(3) . . ? C32 C31 H31A 120.0 . . ? C30 C31 H31A 120.0 . . ? C31 C32 C33 118.7(3) . . ? C31 C32 H32A 120.7 . . ? C33 C32 H32A 120.7 . . ? C34 C33 C32 120.2(3) . . ? C34 C33 H33A 119.9 . . ? C32 C33 H33A 119.9 . . ? C33 C34 C29 122.8(3) . . ? C33 C34 H34A 118.6 . . ? C29 C34 H34A 118.6 . . ? C36 C35 C40 115.1(2) . . ? C36 C35 B1 123.0(2) . . ? C40 C35 B1 121.8(2) . . ? C37 C36 C35 123.0(3) . . ? C37 C36 H36A 118.5 . . ? C35 C36 H36A 118.5 . . ? C38 C37 C36 120.1(3) . . ? C38 C37 H37A 119.9 . . ? C36 C37 H37A 119.9 . . ? C37 C38 C39 119.3(3) . . ? C37 C38 H38A 120.4 . . ? C39 C38 H38A 120.4 . . ? C38 C39 C40 120.1(3) . . ? C38 C39 H39A 119.9 . . ? C40 C39 H39A 119.9 . . ? C39 C40 C35 122.3(3) . . ? C39 C40 H40A 118.8 . . ? C35 C40 H40A 118.8 . . ? C42 C41 C46 114.8(2) . . ? C42 C41 B1 120.6(2) . . ? C46 C41 B1 124.6(2) . . ? C43 C42 C41 123.2(2) . . ? C43 C42 H42A 118.4 . . ? C41 C42 H42A 118.4 . . ? C42 C43 C44 120.2(2) . . ? C42 C43 H43A 119.9 . . ? C44 C43 H43A 119.9 . . ? C45 C44 C43 118.5(3) . . ? C45 C44 H44A 120.7 . . ? C43 C44 H44A 120.7 . . ? C44 C45 C46 120.6(3) . . ? C44 C45 H45A 119.7 . . ? C46 C45 H45A 119.7 . . ? C45 C46 C41 122.7(3) . . ? C45 C46 H46A 118.7 . . ? C41 C46 H46A 118.7 . . ? C48 C47 C52 115.1(2) . . ? C48 C47 B1 124.4(2) . . ? C52 C47 B1 120.3(2) . . ? C49 C48 C47 122.5(2) . . ? C49 C48 H48A 118.8 . . ? C47 C48 H48A 118.8 . . ? C50 C49 C48 120.6(2) . . ? C50 C49 H49A 119.7 . . ? C48 C49 H49A 119.7 . . ? C51 C50 C49 119.0(2) . . ? C51 C50 H50A 120.5 . . ? C49 C50 H50A 120.5 . . ? C50 C51 C52 119.9(3) . . ? C50 C51 H51A 120.0 . . ? C52 C51 H51A 120.0 . . ? C51 C52 C47 122.9(2) . . ? C51 C52 H52A 118.6 . . ? C47 C52 H52A 118.6 . . ? C54 C53 C58 115.2(2) . . ? C54 C53 B2 123.4(2) . . ? C58 C53 B2 121.2(2) . . ? C55 C54 C53 122.7(3) . . ? C55 C54 H54A 118.7 . . ? C53 C54 H54A 118.7 . . ? C56 C55 C54 120.4(3) . . ? C56 C55 H55A 119.8 . . ? C54 C55 H55A 119.8 . . ? C55 C56 C57 119.1(2) . . ? C55 C56 H56A 120.4 . . ? C57 C56 H56A 120.4 . . ? C56 C57 C58 119.8(3) . . ? C56 C57 H57A 120.1 . . ? C58 C57 H57A 120.1 . . ? C57 C58 C53 122.7(2) . . ? C57 C58 H58A 118.7 . . ? C53 C58 H58A 118.7 . . ? C60 C59 C64 115.2(2) . . ? C60 C59 B2 123.6(2) . . ? C64 C59 B2 120.9(2) . . ? C61 C60 C59 122.7(3) . . ? C61 C60 H60A 118.7 . . ? C59 C60 H60A 118.7 . . ? C62 C61 C60 119.9(3) . . ? C62 C61 H61A 120.0 . . ? C60 C61 H61A 120.0 . . ? C63 C62 C61 119.4(3) . . ? C63 C62 H62A 120.3 . . ? C61 C62 H62A 120.3 . . ? C62 C63 C64 120.2(3) . . ? C62 C63 H63A 119.9 . . ? C64 C63 H63A 119.9 . . ? C63 C64 C59 122.6(3) . . ? C63 C64 H64A 118.7 . . ? C59 C64 H64A 118.7 . . ? C70 C65 C66 114.5(2) . . ? C70 C65 B2 126.1(2) . . ? C66 C65 B2 119.1(2) . . ? C67 C66 C65 123.3(3) . . ? C67 C66 H66A 118.3 . . ? C65 C66 H66A 118.3 . . ? C66 C67 C68 120.2(3) . . ? C66 C67 H67A 119.9 . . ? C68 C67 H67A 119.9 . . ? C69 C68 C67 118.6(3) . . ? C69 C68 H68A 120.7 . . ? C67 C68 H68A 120.7 . . ? C68 C69 C70 120.6(3) . . ? C68 C69 H69A 119.7 . . ? C70 C69 H69A 119.7 . . ? C65 C70 C69 122.7(3) . . ? C65 C70 H70A 118.7 . . ? C69 C70 H70A 118.7 . . ? C72 C71 C76 115.1(2) . . ? C72 C71 B2 122.5(2) . . ? C76 C71 B2 121.9(2) . . ? C73 C72 C71 122.3(3) . . ? C73 C72 H72A 118.9 . . ? C71 C72 H72A 118.9 . . ? C74 C73 C72 120.8(3) . . ? C74 C73 H73A 119.6 . . ? C72 C73 H73A 119.6 . . ? C73 C74 C75 119.0(3) . . ? C73 C74 H74A 120.5 . . ? C75 C74 H74A 120.5 . . ? C74 C75 C76 120.1(3) . . ? C74 C75 H75A 120.0 . . ? C76 C75 H75A 120.0 . . ? C75 C76 C71 122.7(2) . . ? C75 C76 H76A 118.6 . . ? C71 C76 H76A 118.6 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.810 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.130 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.250 0.050 0.000 487.4 185.1 2 0.250 -0.091 0.500 487.3 185.2 3 0.750 -0.089 0.000 487.4 185.1 4 0.750 0.063 0.500 487.3 185.2 5 0.500 0.171 0.250 97.5 29.4 6 0.000 0.329 0.750 97.5 29.1 7 0.000 0.671 0.250 97.5 29.4 8 0.500 0.829 0.750 97.5 29.1 _platon_squeeze_details ; ;