# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Jeffrey Long' _publ_contact_author_email jrlong@berkeley.edu loop_ _publ_author_name 'Joseph Zadrozny' 'Mihail Atansov' 'Jeffrey Long' data_cyl002 _database_code_depnum_ccdc_archive 'CCDC 888342' #TrackingRef '- Compound1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[Fe(N(H)(SiMe3)(Dipp))2]' _chemical_melting_point 209-211 _chemical_formula_moiety 'C30 H52 Fe N2 Si2' _chemical_formula_sum 'C30 H52 Fe N2 Si2' _chemical_formula_weight 552.77 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8101(5) _cell_length_b 9.1759(5) _cell_length_c 11.1624(6) _cell_angle_alpha 102.4670(10) _cell_angle_beta 92.5030(10) _cell_angle_gamma 113.9320(10) _cell_volume 796.59(8) _cell_formula_units_Z 1 _cell_measurement_temperature 95(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 27.41 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.368 _exptl_crystal_size_mid 0.367 _exptl_crystal_size_min 0.358 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.152 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 300 _exptl_absorpt_coefficient_mu 0.568 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_T_max 0.816 _exptl_absorpt_process_details SADABS _exptl_special_details ? _diffrn_ambient_temperature 95(1) _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8827 _diffrn_reflns_av_R_equivalents 0.0140 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 27.51 _reflns_number_total 3654 _reflns_number_gt 3338 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.6828P] 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 3654 _refine_ls_number_parameters 167 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.1065 _refine_ls_wR_factor_gt 0.1035 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.5000 0.0000 0.0000 0.02276(11) Uani 1 2 d S . . Si1 Si 0.28282(5) 0.09599(5) 0.19526(4) 0.01756(12) Uani 1 1 d . . . N1 N 0.45463(16) 0.05901(16) 0.15923(12) 0.0177(3) Uani 1 1 d . . . C1 C 0.58837(19) 0.07694(18) 0.24672(14) 0.0167(3) Uani 1 1 d . . . C2 C 0.57958(19) -0.05761(19) 0.29366(15) 0.0188(3) Uani 1 1 d . . . C3 C 0.7165(2) -0.0394(2) 0.37267(16) 0.0230(3) Uani 1 1 d . . . H3 H 0.7114 -0.1279 0.4029 0.028 Uiso 1 1 calc R . . C4 C 0.8602(2) 0.1081(2) 0.40720(16) 0.0235(3) Uani 1 1 d . . . H4 H 0.9501 0.1184 0.4605 0.028 Uiso 1 1 calc R . . C5 C 0.8687(2) 0.2400(2) 0.36163(15) 0.0213(3) Uani 1 1 d . . . H5 H 0.9655 0.3384 0.3844 0.026 Uiso 1 1 calc R . . C6 C 0.73482(19) 0.22788(19) 0.28241(14) 0.0174(3) Uani 1 1 d . . . C7 C 0.7512(2) 0.37441(19) 0.23206(15) 0.0195(3) Uani 1 1 d . . . H7 H 0.6386 0.3542 0.1966 0.023 Uiso 1 1 calc R . . C8 C 0.8209(2) 0.5370(2) 0.33335(17) 0.0258(4) Uani 1 1 d . . . H8A H 0.7533 0.5254 0.3989 0.039 Uiso 1 1 calc R . . H8B H 0.8187 0.6233 0.2988 0.039 Uiso 1 1 calc R . . H8C H 0.9344 0.5639 0.3658 0.039 Uiso 1 1 calc R . . C9 C 0.8596(2) 0.3885(2) 0.12759(17) 0.0297(4) Uani 1 1 d . . . H9A H 0.9708 0.4075 0.1597 0.045 Uiso 1 1 calc R . . H9B H 0.8651 0.4788 0.0950 0.045 Uiso 1 1 calc R . . H9C H 0.8109 0.2880 0.0628 0.045 Uiso 1 1 calc R . . C10 C 0.4258(2) -0.22263(19) 0.25442(16) 0.0221(3) Uani 1 1 d . . . H10 H 0.3345 -0.2031 0.2184 0.027 Uiso 1 1 calc R . . C11 C 0.4562(3) -0.3459(2) 0.15411(19) 0.0355(4) Uani 1 1 d . . . H11A H 0.4824 -0.3027 0.0828 0.053 Uiso 1 1 calc R . . H11B H 0.3571 -0.4482 0.1310 0.053 Uiso 1 1 calc R . . H11C H 0.5483 -0.3643 0.1854 0.053 Uiso 1 1 calc R . . C12 C 0.3671(3) -0.2957(2) 0.36403(19) 0.0330(4) Uani 1 1 d . . . H12A H 0.4490 -0.3269 0.3961 0.049 Uiso 1 1 calc R . . H12B H 0.2616 -0.3910 0.3369 0.049 Uiso 1 1 calc R . . H12C H 0.3537 -0.2149 0.4279 0.049 Uiso 1 1 calc R . . C13 C 0.1018(2) -0.0871(2) 0.21964(17) 0.0253(3) Uani 1 1 d . . . H13A H 0.0746 -0.1797 0.1497 0.038 Uiso 1 1 calc R . . H13B H 0.0063 -0.0623 0.2283 0.038 Uiso 1 1 calc R . . H13C H 0.1315 -0.1131 0.2935 0.038 Uiso 1 1 calc R . . C14 C 0.3408(2) 0.2668(2) 0.33862(18) 0.0289(4) Uani 1 1 d . . . H14A H 0.3880 0.2402 0.4054 0.043 Uiso 1 1 calc R . . H14B H 0.2424 0.2810 0.3600 0.043 Uiso 1 1 calc R . . H14C H 0.4218 0.3670 0.3243 0.043 Uiso 1 1 calc R . . C15 C 0.2138(2) 0.1546(2) 0.05927(18) 0.0294(4) Uani 1 1 d . . . H15A H 0.3011 0.2550 0.0504 0.044 Uiso 1 1 calc R . . H15B H 0.1140 0.1706 0.0722 0.044 Uiso 1 1 calc R . . H15C H 0.1907 0.0683 -0.0146 0.044 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 0.02585(19) 0.02252(19) 0.01771(18) 0.00258(13) 0.00158(13) 0.00957(14) Si1 0.0149(2) 0.0142(2) 0.0212(2) 0.00446(16) -0.00126(16) 0.00425(16) N1 0.0163(6) 0.0145(6) 0.0191(6) 0.0028(5) -0.0010(5) 0.0046(5) C1 0.0156(7) 0.0159(7) 0.0177(7) 0.0025(5) 0.0025(5) 0.0068(6) C2 0.0170(7) 0.0162(7) 0.0232(8) 0.0046(6) 0.0040(6) 0.0071(6) C3 0.0220(8) 0.0232(8) 0.0289(8) 0.0108(7) 0.0048(6) 0.0123(7) C4 0.0173(7) 0.0286(9) 0.0264(8) 0.0081(7) 0.0004(6) 0.0112(7) C5 0.0151(7) 0.0212(8) 0.0240(8) 0.0045(6) 0.0014(6) 0.0049(6) C6 0.0169(7) 0.0163(7) 0.0179(7) 0.0035(5) 0.0031(6) 0.0064(6) C7 0.0176(7) 0.0146(7) 0.0219(8) 0.0040(6) 0.0001(6) 0.0032(6) C8 0.0254(8) 0.0162(8) 0.0290(9) 0.0016(6) -0.0005(7) 0.0046(6) C9 0.0340(9) 0.0248(9) 0.0256(9) 0.0086(7) 0.0075(7) 0.0063(7) C10 0.0203(7) 0.0148(7) 0.0305(9) 0.0075(6) 0.0013(6) 0.0060(6) C11 0.0394(11) 0.0258(9) 0.0318(10) -0.0010(7) 0.0035(8) 0.0088(8) C12 0.0328(10) 0.0239(9) 0.0354(10) 0.0106(7) 0.0088(8) 0.0033(7) C13 0.0211(8) 0.0222(8) 0.0325(9) 0.0100(7) 0.0063(7) 0.0075(6) C14 0.0231(8) 0.0258(9) 0.0330(9) -0.0017(7) 0.0024(7) 0.0104(7) C15 0.0217(8) 0.0292(9) 0.0367(10) 0.0153(8) -0.0028(7) 0.0076(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.8532(13) . ? Fe1 N1 1.8532(13) 2_655 ? Si1 N1 1.7261(14) . ? Si1 C14 1.8637(18) . ? Si1 C15 1.8710(18) . ? Si1 C13 1.8712(17) . ? N1 C1 1.4289(19) . ? C1 C6 1.417(2) . ? C1 C2 1.418(2) . ? C2 C3 1.393(2) . ? C2 C10 1.523(2) . ? C3 C4 1.387(2) . ? C3 H3 0.9300 . ? C4 C5 1.388(2) . ? C4 H4 0.9300 . ? C5 C6 1.395(2) . ? C5 H5 0.9300 . ? C6 C7 1.523(2) . ? C7 C8 1.532(2) . ? C7 C9 1.533(2) . ? C7 H7 0.9800 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.527(2) . ? C10 C12 1.530(2) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N1 180.0 . 2_655 ? N1 Si1 C14 110.71(7) . . ? N1 Si1 C15 105.84(8) . . ? C14 Si1 C15 110.44(9) . . ? N1 Si1 C13 114.00(7) . . ? C14 Si1 C13 107.62(9) . . ? C15 Si1 C13 108.19(8) . . ? C1 N1 Si1 125.67(11) . . ? C1 N1 Fe1 109.18(10) . . ? Si1 N1 Fe1 125.08(8) . . ? C6 C1 C2 119.52(14) . . ? C6 C1 N1 119.83(14) . . ? C2 C1 N1 120.58(13) . . ? C3 C2 C1 119.19(14) . . ? C3 C2 C10 120.04(14) . . ? C1 C2 C10 120.72(14) . . ? C4 C3 C2 121.33(15) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 119.53(15) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C6 121.28(15) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C1 119.14(14) . . ? C5 C6 C7 119.53(14) . . ? C1 C6 C7 121.29(14) . . ? C6 C7 C8 112.60(14) . . ? C6 C7 C9 110.64(14) . . ? C8 C7 C9 110.45(14) . . ? C6 C7 H7 107.6 . . ? C8 C7 H7 107.6 . . ? C9 C7 H7 107.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C10 C11 111.42(14) . . ? C2 C10 C12 112.54(15) . . ? C11 C10 C12 110.49(15) . . ? C2 C10 H10 107.4 . . ? C11 C10 H10 107.4 . . ? C12 C10 H10 107.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.484 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.065 # Attachment '- Compound3.cif' data_bdr207x _database_code_depnum_ccdc_archive 'CCDC 888343' #TrackingRef '- Compound3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H76 Fe0.93 N2' _chemical_formula_sum 'C60 H76 Fe0.93 N2' _chemical_formula_weight 877.17 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' _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 10.8937(18) _cell_length_b 20.234(3) _cell_length_c 11.2231(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.829(3) _cell_angle_gamma 90.00 _cell_volume 2473.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 8898 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 27.88 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.178 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 949.4 _exptl_absorpt_coefficient_mu 0.325 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9246 _exptl_absorpt_correction_T_max 0.9565 _exptl_absorpt_process_details 'SADABS 2008/1 (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27437 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4534 _reflns_number_gt 3752 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (2010-11.3) (Bruker, 2010)' _computing_cell_refinement 'SAINT (8.18C) (Bruker, 2012)' _computing_data_reduction 'SAINT (8.18C) (Bruker, 2012)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+1.0979P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4534 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0800 _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 1.0000 1.0000 0.0000 0.01805(10) Uani 0.93 2 d SP . . N1 N 0.94359(12) 0.92214(7) 0.07496(12) 0.0183(3) Uani 1 1 d . . . H1 H 0.9978(18) 0.8959(9) 0.1048(16) 0.029(5) Uiso 1 1 d . . . C1 C 0.82689(14) 0.89503(7) 0.07596(13) 0.0161(3) Uani 1 1 d . . . C2 C 0.80544(14) 0.83017(7) 0.11998(13) 0.0165(3) Uani 1 1 d . . . C3 C 0.68605(14) 0.80514(8) 0.12039(13) 0.0194(3) Uani 1 1 d . . . H3 H 0.6721 0.7620 0.1506 0.023 Uiso 1 1 calc R . . C4 C 0.58713(14) 0.84198(8) 0.07751(14) 0.0206(3) Uani 1 1 d . . . H4 H 0.5065 0.8241 0.0779 0.025 Uiso 1 1 calc R . . C5 C 0.60793(14) 0.90526(8) 0.03405(14) 0.0189(3) Uani 1 1 d . . . H5 H 0.5407 0.9305 0.0041 0.023 Uiso 1 1 calc R . . C6 C 0.72550(14) 0.93254(7) 0.03350(13) 0.0173(3) Uani 1 1 d . . . C7 C 0.91072(14) 0.79037(7) 0.17001(13) 0.0163(3) Uani 1 1 d . . . C8 C 0.95698(14) 0.80512(8) 0.28502(14) 0.0187(3) Uani 1 1 d . . . C9 C 1.05639(15) 0.76932(8) 0.33112(14) 0.0224(3) Uani 1 1 d . . . H9 H 1.0887 0.7799 0.4078 0.027 Uiso 1 1 calc R . . C10 C 1.10824(15) 0.71880(8) 0.26668(15) 0.0251(4) Uani 1 1 d . . . H10 H 1.1757 0.6947 0.2990 0.030 Uiso 1 1 calc R . . C11 C 1.06154(15) 0.70336(8) 0.15461(15) 0.0240(4) Uani 1 1 d . . . H11 H 1.0968 0.6679 0.1114 0.029 Uiso 1 1 calc R . . C12 C 0.96382(14) 0.73860(8) 0.10368(14) 0.0196(3) Uani 1 1 d . . . C13 C 0.89574(15) 0.85668(8) 0.36364(14) 0.0236(4) Uani 1 1 d . . . H13 H 0.8319 0.8799 0.3142 0.028 Uiso 1 1 calc R . . C14 C 0.98400(18) 0.90839(9) 0.41176(19) 0.0389(5) Uani 1 1 d . . . H14A H 1.0457 0.8871 0.4633 0.058 Uiso 1 1 calc R . . H14B H 0.9386 0.9412 0.4578 0.058 Uiso 1 1 calc R . . H14C H 1.0248 0.9303 0.3453 0.058 Uiso 1 1 calc R . . C15 C 0.8308(2) 0.82198(10) 0.46620(19) 0.0474(6) Uani 1 1 d . . . H15A H 0.8919 0.8005 0.5181 0.071 Uiso 1 1 calc R . . H15B H 0.7741 0.7887 0.4339 0.071 Uiso 1 1 calc R . . H15C H 0.7848 0.8546 0.5122 0.071 Uiso 1 1 calc R . . C16 C 0.91825(16) 0.72296(8) -0.02264(15) 0.0255(4) Uani 1 1 d . . . H16 H 0.8281 0.7323 -0.0264 0.031 Uiso 1 1 calc R . . C17 C 0.9373(2) 0.65067(9) -0.05877(17) 0.0396(5) Uani 1 1 d . . . H17A H 1.0254 0.6414 -0.0632 0.059 Uiso 1 1 calc R . . H17B H 0.8985 0.6428 -0.1368 0.059 Uiso 1 1 calc R . . H17C H 0.9002 0.6216 0.0006 0.059 Uiso 1 1 calc R . . C18 C 0.98077(18) 0.76779(8) -0.11318(15) 0.0309(4) Uani 1 1 d . . . H18A H 0.9711 0.8141 -0.0892 0.046 Uiso 1 1 calc R . . H18B H 0.9430 0.7611 -0.1920 0.046 Uiso 1 1 calc R . . H18C H 1.0683 0.7569 -0.1163 0.046 Uiso 1 1 calc R . . C19 C 0.74325(13) 1.00295(8) -0.00710(14) 0.0177(3) Uani 1 1 d . . . C20 C 0.74930(14) 1.05429(8) 0.07978(14) 0.0193(3) Uani 1 1 d . . . C21 C 0.75574(14) 1.11980(8) 0.04108(15) 0.0225(4) Uani 1 1 d . . . H21 H 0.7578 1.1544 0.0983 0.027 Uiso 1 1 calc R . . C22 C 0.75919(14) 1.13531(8) -0.07896(15) 0.0228(4) Uani 1 1 d . . . H22 H 0.7648 1.1801 -0.1034 0.027 Uiso 1 1 calc R . . C23 C 0.75437(14) 1.08540(8) -0.16360(15) 0.0205(3) Uani 1 1 d . . . H23 H 0.7577 1.0965 -0.2457 0.025 Uiso 1 1 calc R . . C24 C 0.74464(14) 1.01888(7) -0.13037(14) 0.0180(3) Uani 1 1 d . . . C25 C 0.74277(15) 1.03836(8) 0.21235(14) 0.0231(4) Uani 1 1 d . . . H25 H 0.7862 0.9954 0.2261 0.028 Uiso 1 1 calc R . . C26 C 0.60925(16) 1.02972(10) 0.25094(16) 0.0312(4) Uani 1 1 d . . . H26A H 0.5647 1.0713 0.2391 0.047 Uiso 1 1 calc R . . H26B H 0.6075 1.0174 0.3353 0.047 Uiso 1 1 calc R . . H26C H 0.5702 0.9949 0.2030 0.047 Uiso 1 1 calc R . . C27 C 0.80432(16) 1.09063(9) 0.29251(16) 0.0302(4) Uani 1 1 d . . . H27A H 0.8864 1.1005 0.2627 0.045 Uiso 1 1 calc R . . H27B H 0.8111 1.0737 0.3742 0.045 Uiso 1 1 calc R . . H27C H 0.7547 1.1310 0.2918 0.045 Uiso 1 1 calc R . . C28 C 0.73668(15) 0.96466(8) -0.22484(14) 0.0201(3) Uani 1 1 d . . . H28 H 0.6759 0.9311 -0.1972 0.024 Uiso 1 1 calc R . . C29 C 0.86080(16) 0.92998(8) -0.23592(15) 0.0277(4) Uani 1 1 d . . . H29A H 0.9222 0.9617 -0.2633 0.042 Uiso 1 1 calc R . . H29B H 0.8535 0.8937 -0.2935 0.042 Uiso 1 1 calc R . . H29C H 0.8862 0.9123 -0.1581 0.042 Uiso 1 1 calc R . . C30 C 0.69331(16) 0.98940(8) -0.34794(14) 0.0239(4) Uani 1 1 d . . . H30A H 0.6183 1.0156 -0.3393 0.036 Uiso 1 1 calc R . . H30B H 0.6765 0.9515 -0.4000 0.036 Uiso 1 1 calc R . . H30C H 0.7575 1.0169 -0.3829 0.036 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 0.02116(19) 0.01258(17) 0.02037(18) 0.00244(14) -0.00063(13) -0.00473(14) N1 0.0153(7) 0.0162(7) 0.0233(7) 0.0025(5) -0.0024(5) 0.0009(5) C1 0.0188(8) 0.0157(8) 0.0138(7) -0.0018(6) -0.0008(6) -0.0011(6) C2 0.0194(8) 0.0150(8) 0.0149(7) -0.0007(6) -0.0014(6) 0.0002(6) C3 0.0242(8) 0.0157(8) 0.0184(8) 0.0005(6) 0.0000(6) -0.0031(6) C4 0.0175(8) 0.0206(8) 0.0235(8) -0.0010(7) -0.0004(6) -0.0040(6) C5 0.0164(8) 0.0196(8) 0.0207(8) -0.0009(6) -0.0025(6) 0.0016(6) C6 0.0205(8) 0.0157(8) 0.0155(7) -0.0014(6) -0.0012(6) -0.0004(6) C7 0.0176(8) 0.0123(7) 0.0191(8) 0.0026(6) 0.0006(6) -0.0024(6) C8 0.0204(8) 0.0157(8) 0.0200(8) 0.0026(6) 0.0001(6) -0.0015(6) C9 0.0247(8) 0.0233(9) 0.0190(8) 0.0041(7) -0.0033(6) 0.0004(7) C10 0.0231(9) 0.0194(8) 0.0327(9) 0.0078(7) -0.0024(7) 0.0034(7) C11 0.0236(9) 0.0142(8) 0.0344(10) -0.0016(7) 0.0052(7) 0.0021(6) C12 0.0196(8) 0.0155(8) 0.0238(8) -0.0009(6) 0.0025(6) -0.0040(6) C13 0.0271(9) 0.0238(9) 0.0197(8) -0.0051(7) -0.0034(7) 0.0037(7) C14 0.0380(11) 0.0304(10) 0.0487(12) -0.0156(9) 0.0111(9) -0.0087(9) C15 0.0523(13) 0.0388(12) 0.0518(13) -0.0178(10) 0.0262(11) -0.0145(10) C16 0.0233(8) 0.0275(9) 0.0256(9) -0.0090(7) 0.0005(7) -0.0021(7) C17 0.0623(14) 0.0257(10) 0.0309(10) -0.0079(8) 0.0025(9) -0.0126(9) C18 0.0473(11) 0.0216(9) 0.0235(9) -0.0013(7) -0.0063(8) 0.0009(8) C19 0.0132(7) 0.0154(8) 0.0245(8) 0.0005(6) -0.0022(6) 0.0015(6) C20 0.0143(8) 0.0188(8) 0.0248(8) -0.0022(7) -0.0029(6) 0.0016(6) C21 0.0195(8) 0.0166(8) 0.0313(9) -0.0053(7) -0.0037(7) 0.0010(6) C22 0.0199(8) 0.0138(8) 0.0347(9) 0.0022(7) -0.0026(7) 0.0009(6) C23 0.0175(8) 0.0178(8) 0.0262(8) 0.0032(7) -0.0016(6) 0.0011(6) C24 0.0141(7) 0.0161(8) 0.0239(8) 0.0001(6) -0.0017(6) 0.0020(6) C25 0.0249(9) 0.0204(9) 0.0238(9) -0.0036(7) -0.0015(7) 0.0024(7) C26 0.0315(10) 0.0362(10) 0.0261(9) -0.0076(8) 0.0028(7) -0.0049(8) C27 0.0284(10) 0.0331(10) 0.0289(9) -0.0084(8) -0.0042(7) 0.0003(8) C28 0.0232(8) 0.0153(8) 0.0218(8) 0.0012(6) -0.0017(6) -0.0010(6) C29 0.0351(10) 0.0237(9) 0.0243(9) -0.0013(7) -0.0019(7) 0.0082(7) C30 0.0295(9) 0.0189(8) 0.0232(8) 0.0011(7) -0.0035(7) -0.0004(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.8927(13) 3_775 ? Fe1 N1 1.8927(13) . ? N1 C1 1.385(2) . ? N1 H1 0.86(2) . ? C1 C6 1.417(2) . ? C1 C2 1.423(2) . ? C2 C3 1.396(2) . ? C2 C7 1.504(2) . ? C3 C4 1.391(2) . ? C3 H3 0.9500 . ? C4 C5 1.390(2) . ? C4 H4 0.9500 . ? C5 C6 1.395(2) . ? C5 H5 0.9500 . ? C6 C19 1.509(2) . ? C7 C8 1.411(2) . ? C7 C12 1.414(2) . ? C8 C9 1.396(2) . ? C8 C13 1.526(2) . ? C9 C10 1.378(2) . ? C9 H9 0.9500 . ? C10 C11 1.386(2) . ? C10 H10 0.9500 . ? C11 C12 1.397(2) . ? C11 H11 0.9500 . ? C12 C16 1.528(2) . ? C13 C14 1.515(2) . ? C13 C15 1.530(3) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C18 1.530(2) . ? C16 C17 1.533(2) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.421(2) . ? C19 C20 1.426(2) . ? C20 C21 1.397(2) . ? C20 C25 1.525(2) . ? C21 C22 1.384(2) . ? C21 H21 0.9500 . ? C22 C23 1.387(2) . ? C22 H22 0.9500 . ? C23 C24 1.401(2) . ? C23 H23 0.9500 . ? C24 C28 1.527(2) . ? C25 C26 1.534(2) . ? C25 C27 1.536(2) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.530(2) . ? C28 C30 1.537(2) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N1 180.00(7) 3_775 . ? C1 N1 Fe1 129.59(11) . . ? C1 N1 H1 112.2(13) . . ? Fe1 N1 H1 117.5(13) . . ? N1 C1 C6 119.76(14) . . ? N1 C1 C2 121.57(14) . . ? C6 C1 C2 118.66(14) . . ? C3 C2 C1 119.58(14) . . ? C3 C2 C7 120.67(13) . . ? C1 C2 C7 119.70(13) . . ? C4 C3 C2 121.45(14) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 119.07(14) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 C6 121.36(14) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 119.87(14) . . ? C5 C6 C19 119.78(13) . . ? C1 C6 C19 120.30(13) . . ? C8 C7 C12 119.68(14) . . ? C8 C7 C2 119.26(13) . . ? C12 C7 C2 121.06(13) . . ? C9 C8 C7 119.61(14) . . ? C9 C8 C13 118.93(14) . . ? C7 C8 C13 121.35(14) . . ? C10 C9 C8 120.81(15) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C9 C10 C11 119.72(15) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C12 121.60(15) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C11 C12 C7 118.56(14) . . ? C11 C12 C16 120.62(14) . . ? C7 C12 C16 120.80(14) . . ? C14 C13 C8 113.43(14) . . ? C14 C13 C15 110.28(15) . . ? C8 C13 C15 109.40(14) . . ? C14 C13 H13 107.8 . . ? C8 C13 H13 107.8 . . ? C15 C13 H13 107.8 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 C18 110.59(13) . . ? C12 C16 C17 113.55(15) . . ? C18 C16 C17 109.09(14) . . ? C12 C16 H16 107.8 . . ? C18 C16 H16 107.8 . . ? C17 C16 H16 107.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 119.98(14) . . ? C24 C19 C6 120.75(13) . . ? C20 C19 C6 119.09(13) . . ? C21 C20 C19 118.73(14) . . ? C21 C20 C25 120.48(14) . . ? C19 C20 C25 120.73(14) . . ? C22 C21 C20 121.32(15) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C21 C22 C23 120.02(15) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C24 121.29(15) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C23 C24 C19 118.62(14) . . ? C23 C24 C28 120.60(14) . . ? C19 C24 C28 120.78(13) . . ? C20 C25 C26 110.94(13) . . ? C20 C25 C27 113.56(14) . . ? C26 C25 C27 108.71(14) . . ? C20 C25 H25 107.8 . . ? C26 C25 H25 107.8 . . ? C27 C25 H25 107.8 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 C29 110.16(13) . . ? C24 C28 C30 113.80(13) . . ? C29 C28 C30 109.67(13) . . ? C24 C28 H28 107.7 . . ? C29 C28 H28 107.7 . . ? C30 C28 H28 107.7 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 N1 C1 C6 -11.7(2) . . . . ? Fe1 N1 C1 C2 168.98(11) . . . . ? N1 C1 C2 C3 179.34(14) . . . . ? C6 C1 C2 C3 0.0(2) . . . . ? N1 C1 C2 C7 1.8(2) . . . . ? C6 C1 C2 C7 -177.59(13) . . . . ? C1 C2 C3 C4 0.7(2) . . . . ? C7 C2 C3 C4 178.20(14) . . . . ? C2 C3 C4 C5 -0.4(2) . . . . ? C3 C4 C5 C6 -0.5(2) . . . . ? C4 C5 C6 C1 1.1(2) . . . . ? C4 C5 C6 C19 -176.11(14) . . . . ? N1 C1 C6 C5 179.79(14) . . . . ? C2 C1 C6 C5 -0.8(2) . . . . ? N1 C1 C6 C19 -3.0(2) . . . . ? C2 C1 C6 C19 176.36(13) . . . . ? C3 C2 C7 C8 -101.14(17) . . . . ? C1 C2 C7 C8 76.41(18) . . . . ? C3 C2 C7 C12 78.89(19) . . . . ? C1 C2 C7 C12 -103.56(17) . . . . ? C12 C7 C8 C9 1.3(2) . . . . ? C2 C7 C8 C9 -178.66(14) . . . . ? C12 C7 C8 C13 -174.87(14) . . . . ? C2 C7 C8 C13 5.2(2) . . . . ? C7 C8 C9 C10 -1.4(2) . . . . ? C13 C8 C9 C10 174.90(15) . . . . ? C8 C9 C10 C11 0.2(2) . . . . ? C9 C10 C11 C12 1.1(2) . . . . ? C10 C11 C12 C7 -1.2(2) . . . . ? C10 C11 C12 C16 176.82(15) . . . . ? C8 C7 C12 C11 -0.1(2) . . . . ? C2 C7 C12 C11 179.91(14) . . . . ? C8 C7 C12 C16 -178.05(14) . . . . ? C2 C7 C12 C16 1.9(2) . . . . ? C9 C8 C13 C14 55.8(2) . . . . ? C7 C8 C13 C14 -127.94(17) . . . . ? C9 C8 C13 C15 -67.7(2) . . . . ? C7 C8 C13 C15 108.48(18) . . . . ? C11 C12 C16 C18 -93.67(18) . . . . ? C7 C12 C16 C18 84.28(18) . . . . ? C11 C12 C16 C17 29.3(2) . . . . ? C7 C12 C16 C17 -152.71(15) . . . . ? C5 C6 C19 C24 -79.41(19) . . . . ? C1 C6 C19 C24 103.38(17) . . . . ? C5 C6 C19 C20 95.84(17) . . . . ? C1 C6 C19 C20 -81.37(18) . . . . ? C24 C19 C20 C21 0.4(2) . . . . ? C6 C19 C20 C21 -174.88(14) . . . . ? C24 C19 C20 C25 177.54(14) . . . . ? C6 C19 C20 C25 2.3(2) . . . . ? C19 C20 C21 C22 -1.5(2) . . . . ? C25 C20 C21 C22 -178.65(14) . . . . ? C20 C21 C22 C23 1.0(2) . . . . ? C21 C22 C23 C24 0.7(2) . . . . ? C22 C23 C24 C19 -1.8(2) . . . . ? C22 C23 C24 C28 178.68(14) . . . . ? C20 C19 C24 C23 1.2(2) . . . . ? C6 C19 C24 C23 176.41(13) . . . . ? C20 C19 C24 C28 -179.26(13) . . . . ? C6 C19 C24 C28 -4.1(2) . . . . ? C21 C20 C25 C26 94.76(18) . . . . ? C19 C20 C25 C26 -82.33(18) . . . . ? C21 C20 C25 C27 -28.0(2) . . . . ? C19 C20 C25 C27 154.88(14) . . . . ? C23 C24 C28 C29 102.38(17) . . . . ? C19 C24 C28 C29 -77.15(18) . . . . ? C23 C24 C28 C30 -21.3(2) . . . . ? C19 C24 C28 C30 159.21(14) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.359 _refine_diff_density_min -0.212 _refine_diff_density_rms 0.042 _iucr_refine_instructions_details ; TITL bdr207x in P2(1)/n BDR 17APR2012 CELL 0.71073 10.8937 20.2337 11.2231 90.000 90.829 90.000 ZERR 2.00 0.0018 0.0034 0.0019 0.000 0.003 0.000 LATT 1 SYMM -x+1/2, y+1/2, -z+1/2 SFAC C H N Fe UNIT 120 152 4 1.86 L.S. 19 OMIT -3 SHEL 999 0.83 ACTA BOND $H FMAP 2 PLAN 20 WPDB -2 CONF HTAB SIZE 0.138 0.167 0.245 TEMP -183.000 WGHT 0.039100 1.097900 FVAR 0.17881 FE1 4 1.000000 1.000000 0.000000 10.46500 0.02116 0.01258 = 0.02037 0.00244 -0.00063 -0.00473 N1 3 0.943588 0.922137 0.074963 11.00000 0.01532 0.01624 = 0.02328 0.00248 -0.00239 0.00090 H1 2 0.997835 0.895891 0.104758 11.00000 0.02900 C1 1 0.826894 0.895033 0.075962 11.00000 0.01881 0.01572 = 0.01384 -0.00181 -0.00085 -0.00112 C2 1 0.805435 0.830169 0.119977 11.00000 0.01939 0.01504 = 0.01492 -0.00070 -0.00138 0.00017 C3 1 0.686049 0.805136 0.120392 11.00000 0.02416 0.01572 = 0.01840 0.00051 0.00004 -0.00311 AFIX 43 H3 2 0.672066 0.761978 0.150636 11.00000 -1.20000 AFIX 0 C4 1 0.587131 0.841980 0.077509 11.00000 0.01749 0.02063 = 0.02352 -0.00103 -0.00041 -0.00404 AFIX 43 H4 2 0.506465 0.824148 0.077910 11.00000 -1.20000 AFIX 0 C5 1 0.607925 0.905257 0.034054 11.00000 0.01644 0.01959 = 0.02070 -0.00093 -0.00245 0.00155 AFIX 43 H5 2 0.540668 0.930451 0.004109 11.00000 -1.20000 AFIX 0 C6 1 0.725505 0.932537 0.033500 11.00000 0.02053 0.01569 = 0.01552 -0.00138 -0.00120 -0.00043 C7 1 0.910719 0.790369 0.170014 11.00000 0.01755 0.01235 = 0.01913 0.00259 0.00058 -0.00236 C8 1 0.956985 0.805125 0.285020 11.00000 0.02039 0.01573 = 0.02005 0.00264 0.00015 -0.00155 C9 1 1.056388 0.769318 0.331116 11.00000 0.02468 0.02330 = 0.01905 0.00406 -0.00333 0.00039 AFIX 43 H9 2 1.088675 0.779911 0.407849 11.00000 -1.20000 AFIX 0 C10 1 1.108244 0.718801 0.266684 11.00000 0.02308 0.01941 = 0.03272 0.00784 -0.00243 0.00337 AFIX 43 H10 2 1.175729 0.694663 0.298959 11.00000 -1.20000 AFIX 0 C11 1 1.061536 0.703356 0.154607 11.00000 0.02363 0.01420 = 0.03443 -0.00161 0.00523 0.00214 AFIX 43 H11 2 1.096838 0.667935 0.111362 11.00000 -1.20000 AFIX 0 C12 1 0.963824 0.738597 0.103677 11.00000 0.01964 0.01552 = 0.02380 -0.00090 0.00250 -0.00396 C13 1 0.895740 0.856675 0.363638 11.00000 0.02705 0.02385 = 0.01974 -0.00506 -0.00337 0.00374 AFIX 13 H13 2 0.831878 0.879851 0.314247 11.00000 -1.20000 AFIX 0 C14 1 0.983998 0.908390 0.411762 11.00000 0.03798 0.03039 = 0.04870 -0.01561 0.01111 -0.00873 AFIX 137 H14A 2 1.045710 0.887117 0.463288 11.00000 -1.50000 H14B 2 0.938581 0.941199 0.457849 11.00000 -1.50000 H14C 2 1.024783 0.930303 0.345273 11.00000 -1.50000 AFIX 0 C15 1 0.830781 0.821980 0.466204 11.00000 0.05229 0.03880 = 0.05178 -0.01780 0.02617 -0.01447 AFIX 137 H15A 2 0.891875 0.800476 0.518110 11.00000 -1.50000 H15B 2 0.774078 0.788673 0.433938 11.00000 -1.50000 H15C 2 0.784794 0.854575 0.512244 11.00000 -1.50000 AFIX 0 C16 1 0.918254 0.722955 -0.022643 11.00000 0.02326 0.02753 = 0.02561 -0.00903 0.00045 -0.00207 AFIX 13 H16 2 0.828143 0.732304 -0.026436 11.00000 -1.20000 AFIX 0 C17 1 0.937296 0.650666 -0.058769 11.00000 0.06228 0.02566 = 0.03092 -0.00793 0.00245 -0.01257 AFIX 137 H17A 2 1.025392 0.641358 -0.063243 11.00000 -1.50000 H17B 2 0.898463 0.642784 -0.136789 11.00000 -1.50000 H17C 2 0.900208 0.621636 0.000626 11.00000 -1.50000 AFIX 0 C18 1 0.980772 0.767792 -0.113181 11.00000 0.04729 0.02160 = 0.02348 -0.00127 -0.00628 0.00086 AFIX 137 H18A 2 0.971060 0.814051 -0.089222 11.00000 -1.50000 H18B 2 0.942986 0.761143 -0.192046 11.00000 -1.50000 H18C 2 1.068328 0.756911 -0.116287 11.00000 -1.50000 AFIX 0 C19 1 0.743252 1.002955 -0.007101 11.00000 0.01324 0.01538 = 0.02447 0.00046 -0.00224 0.00152 C20 1 0.749305 1.054292 0.079784 11.00000 0.01426 0.01877 = 0.02483 -0.00218 -0.00294 0.00159 C21 1 0.755742 1.119803 0.041081 11.00000 0.01955 0.01665 = 0.03134 -0.00527 -0.00365 0.00097 AFIX 43 H21 2 0.757797 1.154407 0.098287 11.00000 -1.20000 AFIX 0 C22 1 0.759186 1.135309 -0.078957 11.00000 0.01991 0.01377 = 0.03469 0.00223 -0.00265 0.00094 AFIX 43 H22 2 0.764846 1.180150 -0.103363 11.00000 -1.20000 AFIX 0 C23 1 0.754375 1.085404 -0.163598 11.00000 0.01751 0.01783 = 0.02620 0.00322 -0.00160 0.00111 AFIX 43 H23 2 0.757745 1.096541 -0.245717 11.00000 -1.20000 AFIX 0 C24 1 0.744640 1.018882 -0.130369 11.00000 0.01408 0.01606 = 0.02385 0.00006 -0.00174 0.00204 C25 1 0.742770 1.038362 0.212353 11.00000 0.02492 0.02037 = 0.02385 -0.00362 -0.00146 0.00236 AFIX 13 H25 2 0.786199 0.995437 0.226138 11.00000 -1.20000 AFIX 0 C26 1 0.609253 1.029724 0.250937 11.00000 0.03146 0.03615 = 0.02614 -0.00756 0.00285 -0.00488 AFIX 137 H26A 2 0.564729 1.071350 0.239099 11.00000 -1.50000 H26B 2 0.607540 1.017405 0.335344 11.00000 -1.50000 H26C 2 0.570167 0.994898 0.203022 11.00000 -1.50000 AFIX 0 C27 1 0.804318 1.090634 0.292515 11.00000 0.02839 0.03311 = 0.02890 -0.00843 -0.00418 0.00031 AFIX 137 H27A 2 0.886419 1.100515 0.262715 11.00000 -1.50000 H27B 2 0.811123 1.073703 0.374155 11.00000 -1.50000 H27C 2 0.754676 1.131027 0.291812 11.00000 -1.50000 AFIX 0 C28 1 0.736678 0.964663 -0.224835 11.00000 0.02324 0.01526 = 0.02182 0.00117 -0.00173 -0.00096 AFIX 13 H28 2 0.675949 0.931132 -0.197217 11.00000 -1.20000 AFIX 0 C29 1 0.860800 0.929976 -0.235923 11.00000 0.03513 0.02369 = 0.02433 -0.00131 -0.00189 0.00823 AFIX 137 H29A 2 0.922247 0.961709 -0.263257 11.00000 -1.50000 H29B 2 0.853479 0.893729 -0.293506 11.00000 -1.50000 H29C 2 0.886170 0.912273 -0.158108 11.00000 -1.50000 AFIX 0 C30 1 0.693312 0.989399 -0.347935 11.00000 0.02949 0.01888 = 0.02322 0.00105 -0.00352 -0.00042 AFIX 137 H30A 2 0.618284 1.015586 -0.339329 11.00000 -1.50000 H30B 2 0.676528 0.951486 -0.400010 11.00000 -1.50000 H30C 2 0.757481 1.016894 -0.382936 11.00000 -1.50000 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM bdr207x in P2(1)/n BDR 17APR2012 REM R1 = 0.0338 for 3752 Fo > 4sig(Fo) and 0.0449 for all 4534 data REM 298 parameters refined using 0 restraints END WGHT 0.0388 1.0979 REM Highest difference peak 0.359, deepest hole -0.212, 1-sigma level 0.042 Q1 1 0.7915 0.8474 0.4022 11.00000 0.05 0.36 Q2 1 0.9443 0.7353 0.0400 11.00000 0.05 0.25 Q3 1 0.7477 0.8153 0.0926 11.00000 0.05 0.23 Q4 1 0.7742 1.0117 -0.0676 11.00000 0.05 0.22 Q5 1 1.0572 1.0037 0.0654 11.00000 0.05 0.21 Q6 1 0.9292 0.8332 0.3196 11.00000 0.05 0.21 Q7 1 1.0663 0.9995 -0.0695 11.00000 0.05 0.21 Q8 1 0.8566 0.8100 0.1454 11.00000 0.05 0.21 Q9 1 0.7461 0.8237 0.1471 11.00000 0.05 0.20 Q10 1 0.6756 0.9114 0.0034 11.00000 0.05 0.20 Q11 1 0.8501 0.6736 -0.0606 11.00000 0.05 0.20 Q12 1 0.9979 0.8862 0.4753 11.00000 0.05 0.19 Q13 1 0.7718 1.0489 0.1382 11.00000 0.05 0.18 Q14 1 0.7344 1.0282 0.0337 11.00000 0.05 0.17 Q15 1 0.9366 0.8027 0.2238 11.00000 0.05 0.17 Q16 1 0.7705 0.9200 0.0788 11.00000 0.05 0.17 Q17 1 0.7029 1.0119 -0.0667 11.00000 0.05 0.17 Q18 1 0.7897 0.9049 0.0186 11.00000 0.05 0.17 Q19 1 0.7400 0.9936 -0.1801 11.00000 0.05 0.17 Q20 1 0.6276 0.8371 0.1444 11.00000 0.05 0.17 ;