# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Schindler, Siegfried' 'Nebe, Thomas' 'Beitat, Alexander' 'Wuertele, Christian' 'Duecker-Benfer, Carlos' 'Van Eldik, R.' 'McKenzie, Christine' _publ_contact_author_name 'Schindler, Siegfried' _publ_contact_author_email siegfried.schindler@chemie.uni-giessen.de _publ_section_title ; Reinvestigation of the formation of a mononuclear Fe(III) hydroperoxido complex using high pressure kinetics ; # Attachment '- alldata.cif' data_shin129s _database_code_depnum_ccdc_archive 'CCDC 772151' #TrackingRef '- alldata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H29 N5' _chemical_formula_weight 423.55 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.242(5) _cell_length_b 6.2333(12) _cell_length_c 17.286(4) _cell_angle_alpha 90.00 _cell_angle_beta 123.39(3) _cell_angle_gamma 90.00 _cell_volume 2360.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'STOE IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10191 _diffrn_reflns_av_R_equivalents 0.1232 _diffrn_reflns_av_sigmaI/netI 0.0804 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 28.06 _reflns_number_total 2748 _reflns_number_gt 1919 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS Software (1997)' _computing_cell_refinement 'STOE IPDS Software (1997)' _computing_data_reduction 'STOE IPDS Software (1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0890P)^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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2748 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0801 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1590 _refine_ls_wR_factor_gt 0.1448 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 C2 C 0.24395(8) 0.8631(4) 0.11240(15) 0.0531(5) Uani 1 1 d . . . C3 C 0.25502(8) 1.0731(4) 0.14055(13) 0.0532(5) Uani 1 1 d . . . C4 C 0.21643(7) 1.1751(3) 0.15923(13) 0.0462(5) Uani 1 1 d . . . C5 C 0.16809(6) 1.0600(3) 0.14941(11) 0.0382(4) Uani 1 1 d . . . C6 C 0.16013(6) 0.8484(2) 0.12067(10) 0.0312(4) Uani 1 1 d . . . C7 C 0.11034(6) 0.7101(3) 0.11277(11) 0.0340(4) Uani 1 1 d . . . C8 C 0.02645(7) 0.7103(3) 0.13148(12) 0.0409(4) Uani 1 1 d . . . C9 C 0.06390(6) 0.6790(3) 0.23533(12) 0.0359(4) Uani 1 1 d . . . C10 C 0.09005(8) 0.8532(3) 0.29443(12) 0.0408(4) Uani 1 1 d . . . C11 C 0.12412(9) 0.8214(3) 0.38975(13) 0.0464(4) Uani 1 1 d . . . C12 C 0.13093(9) 0.6169(3) 0.42422(13) 0.0465(4) Uani 1 1 d . . . C13 C 0.10435(9) 0.4509(3) 0.36378(15) 0.0518(5) Uani 1 1 d . . . C14 C 0.07131(8) 0.4785(3) 0.26964(12) 0.0467(4) Uani 0.50 1 d P . . C15 C 0.01903(7) 0.9039(3) 0.00412(10) 0.0371(4) Uani 1 1 d . . . N1 N 0.19700(6) 0.7485(2) 0.10178(10) 0.0424(4) Uani 1 1 d . . . N2 N 0.07131(8) 0.4785(3) 0.26964(12) 0.0467(4) Uani 0.50 1 d P . . N3 N 0.05916(5) 0.8326(2) 0.10056(9) 0.0323(3) Uani 1 1 d . . . H2 H 0.2694(11) 0.779(4) 0.0964(19) 0.065(7) Uiso 1 1 d . . . H3 H 0.2867(12) 1.158(4) 0.145(2) 0.083(8) Uiso 1 1 d . . . H4 H 0.2205(9) 1.326(3) 0.1786(16) 0.049(6) Uiso 1 1 d . . . H5 H 0.1401(10) 1.131(3) 0.1631(16) 0.048(5) Uiso 1 1 d . . . H7A H 0.0983(8) 0.608(3) 0.0632(14) 0.036(5) Uiso 1 1 d . . . H7B H 0.1263(8) 0.629(3) 0.1703(14) 0.035(5) Uiso 1 1 d . . . H8A H -0.0096(9) 0.799(3) 0.1192(15) 0.043(5) Uiso 1 1 d . . . H8B H 0.0135(11) 0.562(4) 0.1014(17) 0.065(7) Uiso 1 1 d . . . H10 H 0.0852(9) 0.998(3) 0.2709(15) 0.050(5) Uiso 1 1 d . . . H11 H 0.1416(10) 0.947(3) 0.4293(16) 0.053(6) Uiso 1 1 d . . . H12 H 0.1529(10) 0.589(4) 0.4900(17) 0.060(6) Uiso 1 1 d . . . H13 H 0.1064(10) 0.299(3) 0.3854(17) 0.053(6) Uiso 1 1 d . . . H14 H 0.0498(16) 0.361(6) 0.229(3) 0.035(9) Uiso 0.50 1 d P . . H15A H -0.0068(9) 0.782(3) -0.0329(15) 0.046(5) Uiso 1 1 d . . . H15B H 0.0467(10) 0.947(3) -0.0204(16) 0.053(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C2 0.0320(8) 0.0829(14) 0.0441(10) -0.0101(9) 0.0208(8) -0.0075(8) C3 0.0326(8) 0.0807(14) 0.0382(9) -0.0023(9) 0.0145(7) -0.0189(8) C4 0.0361(8) 0.0517(10) 0.0359(9) -0.0020(7) 0.0103(7) -0.0119(7) C5 0.0263(6) 0.0446(8) 0.0323(8) -0.0014(6) 0.0089(6) -0.0026(6) C6 0.0206(6) 0.0443(8) 0.0197(6) 0.0003(5) 0.0054(5) -0.0002(5) C7 0.0244(6) 0.0400(8) 0.0304(7) -0.0015(6) 0.0105(6) -0.0009(5) C8 0.0247(6) 0.0572(10) 0.0321(8) 0.0018(7) 0.0100(6) -0.0069(6) C9 0.0258(6) 0.0459(8) 0.0353(8) 0.0047(6) 0.0164(6) 0.0019(6) C10 0.0436(8) 0.0419(8) 0.0341(9) 0.0071(6) 0.0196(7) 0.0086(7) C11 0.0513(9) 0.0515(9) 0.0335(9) 0.0031(7) 0.0215(8) 0.0107(8) C12 0.0482(9) 0.0601(10) 0.0348(8) 0.0139(8) 0.0251(8) 0.0154(8) C13 0.0580(10) 0.0463(9) 0.0487(10) 0.0181(8) 0.0279(9) 0.0094(8) C14 0.0464(8) 0.0461(9) 0.0443(9) 0.0063(7) 0.0229(7) -0.0033(7) C15 0.0275(6) 0.0499(9) 0.0202(6) -0.0019(6) 0.0044(5) 0.0022(6) N1 0.0300(6) 0.0590(9) 0.0344(7) -0.0092(6) 0.0153(6) -0.0034(6) N2 0.0464(8) 0.0461(9) 0.0443(9) 0.0063(7) 0.0229(7) -0.0033(7) N3 0.0196(5) 0.0468(7) 0.0222(6) 0.0024(5) 0.0062(4) 0.0006(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 C2 N1 1.347(2) . ? C2 C3 1.370(3) . ? C3 C4 1.376(3) . ? C4 C5 1.384(2) . ? C5 C6 1.384(2) . ? C6 N1 1.333(2) . ? C6 C7 1.508(2) . ? C7 N3 1.4560(19) . ? C8 N3 1.452(2) . ? C8 C9 1.512(2) . ? C9 C14 1.351(2) . ? C9 C10 1.386(2) . ? C10 C11 1.390(2) . ? C11 C12 1.376(3) . ? C12 C13 1.359(3) . ? C13 C14 1.370(3) . ? C15 N3 1.4672(19) . ? C15 C15 1.516(3) 5_575 ? 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 C2 C3 123.7(2) . . ? C2 C3 C4 119.00(17) . . ? C3 C4 C5 118.36(18) . . ? C6 C5 C4 119.01(17) . . ? N1 C6 C5 123.12(14) . . ? N1 C6 C7 114.85(14) . . ? C5 C6 C7 121.97(15) . . ? N3 C7 C6 113.41(13) . . ? N3 C8 C9 112.04(12) . . ? C14 C9 C10 120.53(17) . . ? C14 C9 C8 118.89(16) . . ? C10 C9 C8 120.58(15) . . ? C9 C10 C11 119.75(16) . . ? C12 C11 C10 119.40(18) . . ? C13 C12 C11 118.89(18) . . ? C12 C13 C14 122.63(17) . . ? C9 C14 C13 118.79(17) . . ? N3 C15 C15 111.70(17) . 5_575 ? C6 N1 C2 116.85(16) . . ? C8 N3 C7 110.85(13) . . ? C8 N3 C15 112.16(12) . . ? C7 N3 C15 110.58(14) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 28.06 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.262 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.047 #===END OF DATA FOR 1 # 4.2 REAULTS FOR 2 data_shin160s _database_code_depnum_ccdc_archive 'CCDC 772152' #TrackingRef '- alldata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H52 B Fe N5 O2' _chemical_formula_weight 857.66 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' O O 0.0106 0.0060 '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 13.243(3) _cell_length_b 13.507(3) _cell_length_c 13.992(3) _cell_angle_alpha 96.03(3) _cell_angle_beta 114.15(3) _cell_angle_gamma 101.42(3) _cell_volume 2189.5(8) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 0.393 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'STOE IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20022 _diffrn_reflns_av_R_equivalents 0.0679 _diffrn_reflns_av_sigmaI/netI 0.1098 _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 -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 28.22 _reflns_number_total 9774 _reflns_number_gt 5396 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS Software (1997)' _computing_cell_refinement 'STOE IPDS Software (1997)' _computing_data_reduction 'STOE IPDS Software (1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0694P)^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 9774 _refine_ls_number_parameters 560 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1079 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1442 _refine_ls_wR_factor_gt 0.1239 _refine_ls_goodness_of_fit_ref 0.882 _refine_ls_restrained_S_all 0.882 _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 B1 B 0.6093(3) 0.4020(3) 0.8403(2) 0.0328(8) Uani 1 1 d . . . C1 C 0.7506(3) 0.7428(2) 0.7705(2) 0.0337(7) Uani 1 1 d . . . H1A H 0.7952 0.7040 0.8209 0.040 Uiso 1 1 calc R . . H1B H 0.6689 0.7167 0.7545 0.040 Uiso 1 1 calc R . . C2 C 0.7919(3) 0.8557(2) 0.8222(2) 0.0332(7) Uani 1 1 d . . . C3 C 0.7486(3) 0.8978(3) 0.8878(2) 0.0425(8) Uani 1 1 d . . . H3 H 0.6889 0.8559 0.8982 0.051 Uiso 1 1 calc R . . C4 C 0.7932(4) 1.0005(3) 0.9373(3) 0.0497(9) Uani 1 1 d . . . H4 H 0.7641 1.0306 0.9816 0.060 Uiso 1 1 calc R . . C5 C 0.8808(4) 1.0592(3) 0.9215(3) 0.0475(9) Uani 1 1 d . . . H5 H 0.9143 1.1299 0.9560 0.057 Uiso 1 1 calc R . . C6 C 0.9187(3) 1.0132(3) 0.8550(2) 0.0423(8) Uani 1 1 d . . . H6 H 0.9780 1.0543 0.8434 0.051 Uiso 1 1 calc R . . C7 C 0.7762(3) 0.6204(2) 0.6479(2) 0.0353(7) Uani 1 1 d . . . H7A H 0.7658 0.6038 0.5733 0.042 Uiso 1 1 calc R . . H7B H 0.7160 0.5696 0.6551 0.042 Uiso 1 1 calc R . . C8 C 0.8914(3) 0.6120(2) 0.7226(2) 0.0326(7) Uani 1 1 d . . . C9 C 0.9119(3) 0.5173(3) 0.7386(2) 0.0401(8) Uani 1 1 d . . . H9 H 0.8521 0.4554 0.7024 0.048 Uiso 1 1 calc R . . C10 C 1.0198(4) 0.5140(3) 0.8075(3) 0.0485(9) Uani 1 1 d . . . H10 H 1.0362 0.4497 0.8190 0.058 Uiso 1 1 calc R . . C11 C 1.1042(3) 0.6053(3) 0.8599(3) 0.0482(9) Uani 1 1 d . . . H11 H 1.1790 0.6048 0.9092 0.058 Uiso 1 1 calc R . . C12 C 1.0790(3) 0.6959(3) 0.8402(3) 0.0419(8) Uani 1 1 d . . . H12 H 1.1380 0.7584 0.8759 0.050 Uiso 1 1 calc R . . C13 C 0.6667(3) 0.7441(2) 0.5806(2) 0.0325(7) Uani 1 1 d . . . H13A H 0.6396 0.7993 0.6073 0.039 Uiso 1 1 calc R . . H13B H 0.6023 0.6806 0.5483 0.039 Uiso 1 1 calc R . . C14 C 0.7029(3) 0.7761(2) 0.4964(2) 0.0318(7) Uani 1 1 d . . . H14A H 0.7237 0.7186 0.4652 0.038 Uiso 1 1 calc R . . H14B H 0.6380 0.7915 0.4380 0.038 Uiso 1 1 calc R . . C15 C 0.8594(3) 0.8791(2) 0.4728(2) 0.0364(7) Uani 1 1 d . . . H15A H 0.9107 0.9498 0.4936 0.044 Uiso 1 1 calc R . . H15B H 0.8004 0.8696 0.3983 0.044 Uiso 1 1 calc R . . C16 C 0.9275(3) 0.8029(2) 0.4776(2) 0.0352(7) Uani 1 1 d . . . C17 C 0.9527(3) 0.7741(3) 0.3932(3) 0.0420(8) Uani 1 1 d . . . H17 H 0.9249 0.8020 0.3307 0.050 Uiso 1 1 calc R . . C18 C 1.0176(4) 0.7056(3) 0.4004(3) 0.0512(10) Uani 1 1 d . . . H18 H 1.0352 0.6853 0.3431 0.061 Uiso 1 1 calc R . . C19 C 1.0570(4) 0.6665(3) 0.4920(3) 0.0540(10) Uani 1 1 d . . . H19 H 1.1019 0.6185 0.4991 0.065 Uiso 1 1 calc R . . C20 C 1.0301(4) 0.6984(3) 0.5730(3) 0.0505(9) Uani 1 1 d . . . H20 H 1.0580 0.6716 0.6362 0.061 Uiso 1 1 calc R . . C21 C 0.7687(3) 0.9649(2) 0.5636(2) 0.0340(7) Uani 1 1 d . . . H21A H 0.8394 1.0222 0.6022 0.041 Uiso 1 1 calc R . . H21B H 0.7316 0.9559 0.6120 0.041 Uiso 1 1 calc R . . C22 C 0.6886(3) 0.9973(2) 0.4662(2) 0.0339(7) Uani 1 1 d . . . C23 C 0.7327(3) 1.0666(2) 0.4171(2) 0.0411(8) Uani 1 1 d . . . H23 H 0.8134 1.0896 0.4414 0.049 Uiso 1 1 calc R . . C24 C 0.6602(4) 1.1022(3) 0.3332(3) 0.0503(9) Uani 1 1 d . . . H24 H 0.6913 1.1504 0.3011 0.060 Uiso 1 1 calc R . . C25 C 0.5438(4) 1.0683(3) 0.2963(3) 0.0550(10) Uani 1 1 d . . . H25 H 0.4944 1.0934 0.2390 0.066 Uiso 1 1 calc R . . C26 C 0.4979(4) 0.9978(3) 0.3419(3) 0.0495(9) Uani 1 1 d . . . H26 H 0.4170 0.9730 0.3153 0.059 Uiso 1 1 calc R . . C27 C 0.5710(3) 0.9634(3) 0.4273(3) 0.0415(8) Uani 1 1 d . . . H27 H 0.5395 0.9156 0.4595 0.050 Uiso 1 1 calc R . . C28 C 0.7041(3) 0.5124(2) 0.9144(2) 0.0324(7) Uani 1 1 d . . . C29 C 0.8195(3) 0.5389(2) 0.9364(2) 0.0355(7) Uani 1 1 d . . . H29 H 0.8473 0.4912 0.9055 0.043 Uiso 1 1 calc R . . C30 C 0.8961(3) 0.6320(3) 1.0015(2) 0.0449(9) Uani 1 1 d . . . H30 H 0.9741 0.6468 1.0136 0.054 Uiso 1 1 calc R . . C31 C 0.8591(4) 0.7024(3) 1.0482(3) 0.0517(10) Uani 1 1 d . . . H31 H 0.9111 0.7656 1.0936 0.062 Uiso 1 1 calc R . . C32 C 0.7453(4) 0.6797(3) 1.0279(3) 0.0521(10) Uani 1 1 d . . . H32 H 0.7186 0.7278 1.0597 0.063 Uiso 1 1 calc R . . C33 C 0.6697(3) 0.5880(3) 0.9622(3) 0.0435(8) Uani 1 1 d . . . H33 H 0.5914 0.5752 0.9486 0.052 Uiso 1 1 calc R . . C34 C 0.4886(3) 0.4301(2) 0.7711(2) 0.0362(7) Uani 1 1 d . . . C35 C 0.4816(3) 0.4987(3) 0.7012(3) 0.0480(9) Uani 1 1 d . . . H35 H 0.5477 0.5264 0.6915 0.058 Uiso 1 1 calc R . . C36 C 0.3826(5) 0.5275(3) 0.6462(3) 0.0654(13) Uani 1 1 d . . . H36 H 0.3808 0.5728 0.5984 0.079 Uiso 1 1 calc R . . C37 C 0.2861(4) 0.4907(4) 0.6606(3) 0.0676(13) Uani 1 1 d . . . H37 H 0.2176 0.5105 0.6231 0.081 Uiso 1 1 calc R . . C38 C 0.2905(4) 0.4257(3) 0.7292(3) 0.0592(11) Uani 1 1 d . . . H38 H 0.2252 0.4010 0.7411 0.071 Uiso 1 1 calc R . . C39 C 0.3884(3) 0.3955(3) 0.7816(2) 0.0432(8) Uani 1 1 d . . . H39 H 0.3876 0.3485 0.8274 0.052 Uiso 1 1 calc R . . C40 C 0.5902(3) 0.3237(2) 0.9184(2) 0.0342(7) Uani 1 1 d . . . C41 C 0.5962(3) 0.3579(3) 1.0187(2) 0.0406(8) Uani 1 1 d . . . H41 H 0.6129 0.4300 1.0443 0.049 Uiso 1 1 calc R . . C42 C 0.5788(4) 0.2910(3) 1.0827(3) 0.0543(10) Uani 1 1 d . . . H42 H 0.5839 0.3179 1.1506 0.065 Uiso 1 1 calc R . . C43 C 0.5542(4) 0.1868(3) 1.0487(3) 0.0561(11) Uani 1 1 d . . . H43 H 0.5433 0.1409 1.0928 0.067 Uiso 1 1 calc R . . C44 C 0.5454(4) 0.1492(3) 0.9496(3) 0.0546(10) Uani 1 1 d . . . H44 H 0.5277 0.0768 0.9247 0.065 Uiso 1 1 calc R . . C45 C 0.5623(3) 0.2166(3) 0.8857(3) 0.0467(9) Uani 1 1 d . . . H45 H 0.5545 0.1887 0.8171 0.056 Uiso 1 1 calc R . . C46 C 0.6565(3) 0.3446(2) 0.7637(2) 0.0330(7) Uani 1 1 d . . . C47 C 0.7469(3) 0.2992(3) 0.8073(3) 0.0411(8) Uani 1 1 d . . . H47 H 0.7817 0.3039 0.8826 0.049 Uiso 1 1 calc R . . C48 C 0.7883(4) 0.2476(3) 0.7462(3) 0.0474(9) Uani 1 1 d . . . H48 H 0.8516 0.2200 0.7799 0.057 Uiso 1 1 calc R . . C49 C 0.7370(4) 0.2364(3) 0.6358(3) 0.0507(10) Uani 1 1 d . . . H49 H 0.7629 0.1993 0.5929 0.061 Uiso 1 1 calc R . . C50 C 0.6483(3) 0.2799(3) 0.5897(3) 0.0494(10) Uani 1 1 d . . . H50 H 0.6129 0.2737 0.5143 0.059 Uiso 1 1 calc R . . C51 C 0.6094(3) 0.3331(3) 0.6526(2) 0.0393(8) Uani 1 1 d . . . H51 H 0.5481 0.3628 0.6183 0.047 Uiso 1 1 calc R . . C52 C 1.1252(3) 0.9891(3) 0.7657(2) 0.0398(8) Uani 1 1 d . . . C53 C 1.2455(4) 1.0590(3) 0.8201(3) 0.0580(11) Uani 1 1 d . . . H53A H 1.3001 1.0186 0.8226 0.087 Uiso 1 1 calc R . . H53B H 1.2626 1.0906 0.8932 0.087 Uiso 1 1 calc R . . H53C H 1.2522 1.1132 0.7800 0.087 Uiso 1 1 calc R . . Fe1 Fe 0.93436(4) 0.83611(3) 0.69960(3) 0.03208(13) Uani 1 1 d . . . N1 N 0.7634(2) 0.72502(18) 0.67053(17) 0.0290(5) Uani 1 1 d . . . N2 N 0.8760(2) 0.91307(19) 0.80558(19) 0.0351(6) Uani 1 1 d . . . N3 N 0.9741(2) 0.7014(2) 0.77225(19) 0.0353(6) Uani 1 1 d . . . N4 N 0.8026(2) 0.86868(18) 0.54374(18) 0.0306(6) Uani 1 1 d . . . N5 N 0.9665(3) 0.7652(2) 0.5675(2) 0.0400(7) Uani 1 1 d . . . O1 O 1.1066(2) 0.90604(18) 0.79619(19) 0.0489(6) Uani 1 1 d . . . O2 O 1.0469(3) 1.0130(2) 0.6943(2) 0.0606(8) 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 B1 0.035(2) 0.0347(17) 0.0261(15) 0.0041(12) 0.0133(13) 0.0041(15) C1 0.0342(17) 0.0394(16) 0.0276(13) 0.0117(11) 0.0140(12) 0.0068(14) C2 0.0362(18) 0.0395(16) 0.0228(12) 0.0117(11) 0.0107(12) 0.0098(14) C3 0.048(2) 0.055(2) 0.0334(15) 0.0152(14) 0.0228(14) 0.0192(17) C4 0.065(3) 0.054(2) 0.0383(17) 0.0108(15) 0.0266(17) 0.0233(19) C5 0.068(3) 0.0367(17) 0.0365(16) 0.0015(13) 0.0228(17) 0.0139(17) C6 0.050(2) 0.0396(17) 0.0348(16) 0.0067(13) 0.0178(15) 0.0077(16) C7 0.0346(18) 0.0300(14) 0.0345(15) 0.0037(12) 0.0118(13) 0.0035(13) C8 0.0344(17) 0.0363(15) 0.0287(13) 0.0086(11) 0.0168(12) 0.0054(13) C9 0.049(2) 0.0374(16) 0.0346(15) 0.0090(12) 0.0193(14) 0.0108(15) C10 0.063(3) 0.048(2) 0.0425(18) 0.0165(15) 0.0233(17) 0.0273(19) C11 0.042(2) 0.064(2) 0.0404(17) 0.0179(16) 0.0132(15) 0.0243(19) C12 0.0339(19) 0.0498(19) 0.0379(16) 0.0120(14) 0.0113(14) 0.0107(16) C13 0.0263(16) 0.0383(15) 0.0295(14) 0.0085(11) 0.0097(12) 0.0064(13) C14 0.0330(17) 0.0336(15) 0.0265(13) 0.0061(11) 0.0115(12) 0.0077(13) C15 0.045(2) 0.0383(16) 0.0325(14) 0.0116(12) 0.0240(14) 0.0084(15) C16 0.0352(18) 0.0331(15) 0.0375(15) 0.0025(12) 0.0205(13) 0.0019(13) C17 0.044(2) 0.0441(18) 0.0382(16) 0.0036(13) 0.0229(15) 0.0046(16) C18 0.053(2) 0.050(2) 0.055(2) 0.0012(16) 0.0335(18) 0.0071(18) C19 0.054(3) 0.055(2) 0.069(2) 0.0126(19) 0.038(2) 0.024(2) C20 0.054(3) 0.054(2) 0.052(2) 0.0166(17) 0.0268(18) 0.024(2) C21 0.0398(19) 0.0335(15) 0.0284(14) 0.0055(11) 0.0157(13) 0.0085(14) C22 0.0434(19) 0.0297(14) 0.0273(13) 0.0013(11) 0.0157(13) 0.0088(14) C23 0.045(2) 0.0400(17) 0.0362(16) 0.0085(13) 0.0171(14) 0.0091(15) C24 0.062(3) 0.054(2) 0.0405(17) 0.0197(15) 0.0249(17) 0.0185(19) C25 0.062(3) 0.070(2) 0.0337(17) 0.0159(16) 0.0151(17) 0.029(2) C26 0.043(2) 0.060(2) 0.0432(18) 0.0043(16) 0.0164(16) 0.0178(18) C27 0.045(2) 0.0430(18) 0.0406(16) 0.0048(14) 0.0225(15) 0.0130(16) C28 0.0363(18) 0.0329(14) 0.0256(13) 0.0049(11) 0.0142(12) 0.0034(13) C29 0.0373(18) 0.0390(16) 0.0278(13) 0.0093(12) 0.0133(12) 0.0060(14) C30 0.0364(19) 0.0503(19) 0.0373(16) 0.0136(14) 0.0115(14) -0.0029(16) C31 0.063(3) 0.0368(17) 0.0372(17) 0.0037(13) 0.0157(16) -0.0089(18) C32 0.074(3) 0.0358(17) 0.0476(19) 0.0007(14) 0.0348(19) 0.0043(18) C33 0.047(2) 0.0394(17) 0.0480(18) 0.0041(14) 0.0275(16) 0.0068(16) C34 0.0349(18) 0.0362(16) 0.0281(14) -0.0024(11) 0.0096(12) 0.0036(14) C35 0.047(2) 0.050(2) 0.0414(17) 0.0099(15) 0.0147(16) 0.0117(17) C36 0.078(3) 0.062(3) 0.044(2) 0.0137(18) 0.010(2) 0.028(2) C37 0.049(3) 0.078(3) 0.052(2) -0.007(2) -0.0020(19) 0.031(2) C38 0.038(2) 0.071(3) 0.051(2) -0.0056(19) 0.0091(17) 0.010(2) C39 0.0351(19) 0.0493(19) 0.0343(15) -0.0013(13) 0.0111(13) 0.0028(16) C40 0.0284(16) 0.0411(16) 0.0286(14) 0.0032(12) 0.0126(12) 0.0013(14) C41 0.042(2) 0.0472(18) 0.0322(15) 0.0040(13) 0.0191(14) 0.0068(16) C42 0.060(3) 0.067(2) 0.0330(16) 0.0100(16) 0.0239(16) 0.005(2) C43 0.061(3) 0.063(2) 0.050(2) 0.0253(18) 0.0299(19) 0.008(2) C44 0.065(3) 0.0396(18) 0.060(2) 0.0114(16) 0.033(2) 0.0031(18) C45 0.058(2) 0.0423(18) 0.0404(17) 0.0049(14) 0.0276(16) 0.0028(17) C46 0.0331(17) 0.0319(14) 0.0304(14) 0.0038(11) 0.0144(12) 0.0017(13) C47 0.048(2) 0.0433(18) 0.0389(16) 0.0110(14) 0.0245(15) 0.0145(16) C48 0.056(2) 0.0408(18) 0.063(2) 0.0125(16) 0.0390(19) 0.0186(17) C49 0.062(3) 0.0377(17) 0.057(2) -0.0071(15) 0.042(2) -0.0023(18) C50 0.050(2) 0.057(2) 0.0321(15) -0.0073(14) 0.0227(15) -0.0062(19) C51 0.0369(19) 0.0465(18) 0.0290(14) 0.0002(12) 0.0150(13) 0.0024(15) C52 0.040(2) 0.0447(18) 0.0335(15) -0.0007(13) 0.0213(14) 0.0008(15) C53 0.050(2) 0.059(2) 0.052(2) -0.0073(17) 0.0268(18) -0.0152(19) Fe1 0.0314(3) 0.0335(2) 0.0277(2) 0.00580(16) 0.01191(17) 0.00372(19) N1 0.0271(13) 0.0344(12) 0.0244(11) 0.0068(9) 0.0098(9) 0.0087(11) N2 0.0410(16) 0.0330(13) 0.0279(12) 0.0047(10) 0.0144(11) 0.0050(12) N3 0.0300(15) 0.0410(14) 0.0328(12) 0.0091(10) 0.0126(11) 0.0070(12) N4 0.0341(15) 0.0313(12) 0.0281(11) 0.0051(9) 0.0170(10) 0.0060(11) N5 0.0433(17) 0.0405(14) 0.0389(14) 0.0100(11) 0.0203(12) 0.0114(13) O1 0.0495(16) 0.0411(13) 0.0502(13) 0.0071(10) 0.0222(12) 0.0001(12) O2 0.0549(18) 0.0679(18) 0.0539(15) 0.0179(13) 0.0198(14) 0.0117(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 C34 1.639(5) . ? B1 C46 1.644(5) . ? B1 C28 1.656(4) . ? B1 C40 1.656(4) . ? C1 N1 1.478(4) . ? C1 C2 1.504(4) . ? C2 N2 1.342(4) . ? C2 C3 1.394(5) . ? C3 C4 1.376(5) . ? C4 C5 1.380(6) . ? C5 C6 1.373(5) . ? C6 N2 1.345(4) . ? C7 N1 1.474(4) . ? C7 C8 1.490(5) . ? C8 N3 1.348(4) . ? C8 C9 1.381(5) . ? C9 C10 1.371(5) . ? C10 C11 1.379(5) . ? C11 C12 1.358(5) . ? C12 N3 1.346(4) . ? C13 N1 1.473(4) . ? C13 C14 1.515(4) . ? C14 N4 1.484(4) . ? C15 N4 1.472(4) . ? C15 C16 1.487(5) . ? C16 N5 1.347(4) . ? C16 C17 1.391(4) . ? C17 C18 1.366(6) . ? C18 C19 1.379(6) . ? C19 C20 1.373(5) . ? C20 N5 1.339(5) . ? C21 N4 1.492(4) . ? C21 C22 1.516(4) . ? C22 C27 1.379(5) . ? C22 C23 1.393(4) . ? C23 C24 1.382(5) . ? C24 C25 1.368(6) . ? C25 C26 1.378(6) . ? C26 C27 1.389(5) . ? C28 C29 1.391(5) . ? C28 C33 1.410(5) . ? C29 C30 1.392(4) . ? C30 C31 1.374(6) . ? C31 C32 1.377(6) . ? C32 C33 1.378(5) . ? C34 C39 1.390(5) . ? C34 C35 1.404(5) . ? C35 C36 1.380(6) . ? C36 C37 1.378(7) . ? C37 C38 1.360(6) . ? C38 C39 1.370(6) . ? C40 C41 1.396(4) . ? C40 C45 1.396(5) . ? C41 C42 1.388(5) . ? C42 C43 1.366(6) . ? C43 C44 1.375(5) . ? C44 C45 1.390(5) . ? C46 C51 1.396(4) . ? C46 C47 1.397(5) . ? C47 C48 1.389(5) . ? C48 C49 1.387(5) . ? C49 C50 1.369(6) . ? C50 C51 1.392(5) . ? C52 O2 1.237(5) . ? C52 O1 1.256(4) . ? C52 C53 1.507(5) . ? Fe1 O1 2.068(3) . ? Fe1 N2 2.193(3) . ? Fe1 N5 2.224(3) . ? Fe1 N3 2.226(3) . ? Fe1 N1 2.306(3) . ? Fe1 N4 2.321(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C34 B1 C46 112.6(2) . . ? C34 B1 C28 106.7(3) . . ? C46 B1 C28 110.1(3) . . ? C34 B1 C40 109.5(3) . . ? C46 B1 C40 107.9(3) . . ? C28 B1 C40 109.9(2) . . ? N1 C1 C2 111.2(2) . . ? N2 C2 C3 121.6(3) . . ? N2 C2 C1 116.6(3) . . ? C3 C2 C1 121.7(3) . . ? C4 C3 C2 119.4(3) . . ? C3 C4 C5 119.0(4) . . ? C6 C5 C4 118.7(3) . . ? N2 C6 C5 123.3(3) . . ? N1 C7 C8 111.2(2) . . ? N3 C8 C9 122.2(3) . . ? N3 C8 C7 116.4(3) . . ? C9 C8 C7 121.4(3) . . ? C10 C9 C8 119.0(3) . . ? C9 C10 C11 119.1(3) . . ? C12 C11 C10 119.2(3) . . ? N3 C12 C11 123.0(3) . . ? N1 C13 C14 110.6(3) . . ? N4 C14 C13 110.6(2) . . ? N4 C15 C16 112.3(2) . . ? N5 C16 C17 121.4(3) . . ? N5 C16 C15 117.7(3) . . ? C17 C16 C15 120.9(3) . . ? C18 C17 C16 119.8(3) . . ? C17 C18 C19 118.9(3) . . ? C20 C19 C18 118.6(4) . . ? N5 C20 C19 123.4(4) . . ? N4 C21 C22 116.8(2) . . ? C27 C22 C23 118.3(3) . . ? C27 C22 C21 121.3(3) . . ? C23 C22 C21 120.3(3) . . ? C24 C23 C22 120.6(4) . . ? C25 C24 C23 120.2(3) . . ? C24 C25 C26 120.3(4) . . ? C25 C26 C27 119.3(4) . . ? C22 C27 C26 121.3(3) . . ? C29 C28 C33 114.7(3) . . ? C29 C28 B1 125.5(3) . . ? C33 C28 B1 119.8(3) . . ? C28 C29 C30 123.1(3) . . ? C31 C30 C29 120.1(3) . . ? C30 C31 C32 118.8(3) . . ? C31 C32 C33 120.8(4) . . ? C32 C33 C28 122.5(4) . . ? C39 C34 C35 114.4(3) . . ? C39 C34 B1 123.9(3) . . ? C35 C34 B1 121.5(3) . . ? C36 C35 C34 122.6(4) . . ? C37 C36 C35 120.2(4) . . ? C38 C37 C36 118.8(4) . . ? C37 C38 C39 120.7(4) . . ? C38 C39 C34 123.4(4) . . ? C41 C40 C45 114.9(3) . . ? C41 C40 B1 123.6(3) . . ? C45 C40 B1 121.5(3) . . ? C42 C41 C40 122.8(3) . . ? C43 C42 C41 120.4(3) . . ? C42 C43 C44 119.0(3) . . ? C43 C44 C45 120.3(4) . . ? C44 C45 C40 122.6(3) . . ? C51 C46 C47 114.5(3) . . ? C51 C46 B1 124.5(3) . . ? C47 C46 B1 120.9(3) . . ? C48 C47 C46 123.3(3) . . ? C49 C48 C47 119.9(4) . . ? C50 C49 C48 118.7(3) . . ? C49 C50 C51 120.5(3) . . ? C50 C51 C46 123.0(4) . . ? O2 C52 O1 120.9(3) . . ? O2 C52 C53 121.3(3) . . ? O1 C52 C53 117.7(4) . . ? O1 Fe1 N2 94.48(11) . . ? O1 Fe1 N5 93.37(11) . . ? N2 Fe1 N5 169.16(11) . . ? O1 Fe1 N3 83.80(10) . . ? N2 Fe1 N3 101.87(10) . . ? N5 Fe1 N3 86.40(10) . . ? O1 Fe1 N1 150.37(9) . . ? N2 Fe1 N1 74.54(10) . . ? N5 Fe1 N1 101.83(10) . . ? N3 Fe1 N1 72.09(10) . . ? O1 Fe1 N4 132.30(9) . . ? N2 Fe1 N4 95.21(10) . . ? N5 Fe1 N4 73.96(10) . . ? N3 Fe1 N4 138.68(9) . . ? N1 Fe1 N4 76.82(9) . . ? C13 N1 C7 111.8(2) . . ? C13 N1 C1 110.8(3) . . ? C7 N1 C1 110.7(2) . . ? C13 N1 Fe1 110.57(17) . . ? C7 N1 Fe1 105.48(19) . . ? C1 N1 Fe1 107.24(17) . . ? C2 N2 C6 118.0(3) . . ? C2 N2 Fe1 117.4(2) . . ? C6 N2 Fe1 124.6(2) . . ? C12 N3 C8 117.6(3) . . ? C12 N3 Fe1 125.6(2) . . ? C8 N3 Fe1 114.6(2) . . ? C15 N4 C14 109.8(2) . . ? C15 N4 C21 109.9(2) . . ? C14 N4 C21 112.1(3) . . ? C15 N4 Fe1 106.0(2) . . ? C14 N4 Fe1 106.45(17) . . ? C21 N4 Fe1 112.40(16) . . ? C20 N5 C16 117.8(3) . . ? C20 N5 Fe1 126.5(2) . . ? C16 N5 Fe1 115.3(2) . . ? C52 O1 Fe1 104.2(2) . . ? _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 28.22 _diffrn_measured_fraction_theta_full 0.904 _refine_diff_density_max 0.562 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.069 #===END OF DATA FOR 2 # 4.3 REAULTS FOR 3 data_shin170s _database_code_depnum_ccdc_archive 'CCDC 772153' #TrackingRef '- alldata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H28 B Cl Co F4 N5' _chemical_formula_weight 603.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.309(3) _cell_length_b 17.791(4) _cell_length_c 18.066(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5241.9(18) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2480 _exptl_absorpt_coefficient_mu 0.813 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'STOE IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44894 _diffrn_reflns_av_R_equivalents 0.0684 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 28.09 _reflns_number_total 6334 _reflns_number_gt 4754 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS Software (1997)' _computing_cell_refinement 'STOE IPDS Software (1997)' _computing_data_reduction 'STOE IPDS Software (1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1086P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6334 _refine_ls_number_parameters 492 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1449 _refine_ls_wR_factor_gt 0.1314 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _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 B1 B 0.3365(2) 0.03156(19) 0.4564(2) 0.0431(8) Uani 1 1 d . . . C1 C 0.52466(19) 0.11112(14) 0.35507(14) 0.0305(5) Uani 1 1 d . . . C2 C 0.59199(17) 0.06675(13) 0.31895(13) 0.0278(5) Uani 1 1 d . . . C3 C 0.5992(2) -0.01012(14) 0.32943(16) 0.0357(6) Uani 1 1 d . . . C4 C 0.6640(2) -0.04727(16) 0.29679(17) 0.0414(7) Uani 1 1 d . . . C5 C 0.7185(2) -0.00736(16) 0.25403(16) 0.0385(7) Uani 1 1 d . . . C6 C 0.70824(18) 0.06928(15) 0.24640(14) 0.0309(5) Uani 1 1 d . . . C7 C 0.46881(17) 0.16630(14) 0.24334(14) 0.0271(5) Uani 1 1 d . . . C8 C 0.48849(16) 0.22672(13) 0.18797(13) 0.0254(5) Uani 1 1 d . . . C9 C 0.43160(18) 0.25170(15) 0.13672(15) 0.0329(6) Uani 1 1 d . . . C10 C 0.4563(2) 0.30578(16) 0.08558(15) 0.0365(6) Uani 1 1 d . . . C11 C 0.5347(2) 0.33263(16) 0.08759(14) 0.0356(6) Uani 1 1 d . . . C12 C 0.58791(18) 0.30553(15) 0.14129(13) 0.0293(5) Uani 1 1 d . . . C13 C 0.46485(18) 0.23815(14) 0.35754(14) 0.0277(5) Uani 1 1 d . . . C14 C 0.52299(17) 0.28554(13) 0.40358(13) 0.0253(5) Uani 1 1 d . . . C15 C 0.65975(17) 0.33992(13) 0.40366(13) 0.0253(5) Uani 1 1 d . . . C16 C 0.69855(16) 0.27245(12) 0.43854(13) 0.0242(5) Uani 1 1 d . . . C17 C 0.73535(19) 0.27656(15) 0.50756(14) 0.0313(6) Uani 1 1 d . . . C18 C 0.76908(19) 0.21266(17) 0.53764(14) 0.0350(6) Uani 1 1 d . . . C19 C 0.76541(19) 0.14644(16) 0.49837(14) 0.0339(6) Uani 1 1 d . . . C20 C 0.72860(17) 0.14671(14) 0.42967(14) 0.0294(5) Uani 1 1 d . . . C21 C 0.56045(18) 0.38255(13) 0.31207(13) 0.0268(5) Uani 1 1 d . . . C22 C 0.52773(17) 0.44903(13) 0.35472(12) 0.0256(5) Uani 1 1 d . . . C23 C 0.44459(18) 0.45674(14) 0.36633(14) 0.0298(5) Uani 1 1 d . . . C24 C 0.4128(2) 0.51870(16) 0.40330(15) 0.0358(6) Uani 1 1 d . . . C25 C 0.4656(2) 0.57338(15) 0.42889(14) 0.0364(6) Uani 1 1 d . . . C26 C 0.5480(2) 0.56614(14) 0.41918(14) 0.0341(6) Uani 1 1 d . . . C27 C 0.58020(19) 0.50464(13) 0.38174(14) 0.0306(5) Uani 1 1 d . . . Cl2 Cl 0.75813(4) 0.27011(3) 0.24217(3) 0.03083(16) Uani 1 1 d . . . Co1 Co 0.63383(2) 0.223806(16) 0.288159(16) 0.02105(12) Uani 1 1 d . . . F1 F 0.3222(8) -0.0047(8) 0.3956(5) 0.127(5) Uani 0.545(15) 1 d P A 1 F2 F 0.3919(5) -0.0140(5) 0.4985(4) 0.078(2) Uani 0.545(15) 1 d P A 1 F3 F 0.26801(15) 0.03366(12) 0.50149(16) 0.0686(7) Uani 1 1 d . A . F4 F 0.3675(5) 0.1001(3) 0.4533(7) 0.086(4) Uani 0.545(15) 1 d P A 1 F1A F 0.3284(8) -0.0259(5) 0.4058(6) 0.088(4) Uani 0.455(15) 1 d P A 2 F2A F 0.4073(4) 0.0332(10) 0.4862(4) 0.102(5) Uani 0.455(15) 1 d P A 2 F4A F 0.3322(5) 0.0958(4) 0.4038(5) 0.059(2) Uani 0.455(15) 1 d P A 2 H1A H 0.541(2) 0.1236(16) 0.4059(17) 0.028(7) Uiso 1 1 d . . . H1B H 0.476(2) 0.082(2) 0.357(2) 0.042(9) Uiso 1 1 d . . . H3 H 0.561(3) -0.035(2) 0.360(2) 0.049(10) Uiso 1 1 d . . . H4 H 0.671(2) -0.099(2) 0.303(2) 0.045(10) Uiso 1 1 d . . . H5 H 0.758(2) -0.030(2) 0.230(2) 0.043(10) Uiso 1 1 d . . . H6 H 0.742(2) 0.0974(18) 0.2176(17) 0.028(8) Uiso 1 1 d . . . H7A H 0.488(2) 0.1163(19) 0.2243(18) 0.033(8) Uiso 1 1 d . . . H7B H 0.412(2) 0.1614(16) 0.2494(16) 0.024(7) Uiso 1 1 d . . . H10 H 0.420(2) 0.324(2) 0.053(2) 0.046(9) Uiso 1 1 d . . . H11 H 0.552(2) 0.368(2) 0.056(2) 0.047(10) Uiso 1 1 d . . . H12 H 0.644(2) 0.3239(17) 0.1470(17) 0.028(8) Uiso 1 1 d . . . H13A H 0.4298(19) 0.2107(16) 0.3889(16) 0.021(7) Uiso 1 1 d . . . H13B H 0.4395(19) 0.2694(15) 0.3234(16) 0.020(7) Uiso 1 1 d . . . H14A H 0.5483(18) 0.2543(15) 0.4411(16) 0.020(6) Uiso 1 1 d . . . H14B H 0.491(2) 0.3247(18) 0.4269(17) 0.030(8) Uiso 1 1 d . . . H15A H 0.697(2) 0.366(2) 0.3732(19) 0.038(9) Uiso 1 1 d . . . H15B H 0.6449(18) 0.3757(17) 0.4406(16) 0.022(7) Uiso 1 1 d . . . H17 H 0.738(2) 0.3207(18) 0.5335(18) 0.032(8) Uiso 1 1 d . . . H18 H 0.794(2) 0.2146(18) 0.584(2) 0.038(9) Uiso 1 1 d . . . H19 H 0.784(2) 0.101(2) 0.5165(18) 0.036(8) Uiso 1 1 d . . . H20 H 0.725(2) 0.1024(19) 0.4017(18) 0.037(8) Uiso 1 1 d . . . H21A H 0.518(2) 0.3659(17) 0.2789(17) 0.026(7) Uiso 1 1 d . . . H21B H 0.601(2) 0.3973(17) 0.2837(16) 0.024(7) Uiso 1 1 d . . . H23 H 0.406(2) 0.4179(18) 0.3484(18) 0.033(8) Uiso 1 1 d . . . H24 H 0.355(2) 0.521(2) 0.411(2) 0.040(9) Uiso 1 1 d . . . H25 H 0.446(2) 0.616(2) 0.448(2) 0.046(9) Uiso 1 1 d . . . H26 H 0.581(2) 0.602(2) 0.434(2) 0.044(9) Uiso 1 1 d . . . H27 H 0.638(2) 0.503(2) 0.3710(19) 0.039(9) Uiso 1 1 d . . . N1 N 0.51108(13) 0.18144(11) 0.31402(11) 0.0234(4) Uani 1 1 d . . . N2 N 0.56566(13) 0.25348(12) 0.19112(11) 0.0245(4) Uani 1 1 d . . . N3 N 0.69475(14) 0.20804(11) 0.39943(11) 0.0250(4) Uani 1 1 d . . . N4 N 0.64597(14) 0.10617(11) 0.27838(11) 0.0260(4) Uani 1 1 d . . . N5 N 0.58919(13) 0.31765(10) 0.35738(10) 0.0228(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 B1 0.037(2) 0.0336(15) 0.058(2) -0.0068(14) 0.0037(16) 0.0012(13) C1 0.0395(16) 0.0237(11) 0.0284(12) 0.0001(9) 0.0081(11) -0.0031(10) C2 0.0381(15) 0.0212(10) 0.0242(11) -0.0036(8) -0.0018(10) -0.0011(10) C3 0.0498(18) 0.0229(11) 0.0346(13) 0.0010(10) -0.0059(12) -0.0017(11) C4 0.056(2) 0.0252(12) 0.0428(16) -0.0042(11) -0.0154(14) 0.0095(13) C5 0.0442(18) 0.0354(13) 0.0360(14) -0.0121(11) -0.0080(12) 0.0172(13) C6 0.0326(14) 0.0336(12) 0.0264(11) -0.0069(10) -0.0021(10) 0.0037(10) C7 0.0261(13) 0.0276(11) 0.0277(11) -0.0050(9) -0.0014(10) -0.0076(9) C8 0.0291(14) 0.0250(11) 0.0222(10) -0.0092(8) 0.0012(9) 0.0005(9) C9 0.0371(15) 0.0312(12) 0.0305(12) -0.0080(10) -0.0037(11) 0.0043(11) C10 0.0389(16) 0.0400(14) 0.0306(12) -0.0040(11) -0.0094(12) 0.0087(12) C11 0.0503(18) 0.0343(13) 0.0223(11) 0.0002(10) 0.0015(11) 0.0019(12) C12 0.0335(15) 0.0337(12) 0.0209(10) -0.0040(9) 0.0018(10) -0.0013(10) C13 0.0326(14) 0.0242(11) 0.0264(11) -0.0050(9) 0.0066(10) -0.0004(10) C14 0.0345(14) 0.0217(10) 0.0196(10) -0.0038(8) 0.0048(9) 0.0001(10) C15 0.0312(13) 0.0209(10) 0.0238(11) -0.0046(8) -0.0008(9) -0.0033(9) C16 0.0277(13) 0.0239(10) 0.0210(10) -0.0020(8) 0.0016(9) -0.0046(9) C17 0.0367(16) 0.0341(13) 0.0230(11) -0.0038(9) -0.0019(10) -0.0088(10) C18 0.0349(16) 0.0486(15) 0.0214(11) 0.0033(10) -0.0048(10) -0.0091(12) C19 0.0363(16) 0.0343(13) 0.0311(13) 0.0100(10) -0.0023(11) -0.0014(11) C20 0.0324(14) 0.0266(11) 0.0291(12) 0.0000(9) -0.0033(10) -0.0007(10) C21 0.0365(15) 0.0235(11) 0.0203(10) 0.0005(8) 0.0015(10) 0.0003(10) C22 0.0352(14) 0.0206(10) 0.0209(10) 0.0022(8) -0.0006(9) 0.0029(9) C23 0.0331(14) 0.0280(11) 0.0284(12) 0.0011(9) -0.0025(10) 0.0022(10) C24 0.0397(17) 0.0371(13) 0.0305(13) 0.0043(10) 0.0053(11) 0.0109(12) C25 0.059(2) 0.0274(12) 0.0230(11) -0.0004(9) 0.0015(11) 0.0131(12) C26 0.0534(19) 0.0206(10) 0.0285(12) 0.0009(9) -0.0076(12) -0.0004(11) C27 0.0371(16) 0.0230(11) 0.0318(12) 0.0037(9) 0.0000(11) 0.0008(10) Cl2 0.0280(3) 0.0381(3) 0.0263(3) 0.0007(2) 0.0016(2) -0.0062(2) Co1 0.0252(2) 0.01959(17) 0.01836(17) -0.00322(10) 0.00198(11) -0.00132(11) F1 0.165(9) 0.158(10) 0.057(4) -0.016(5) -0.062(5) -0.024(7) F2 0.066(4) 0.097(5) 0.069(4) 0.001(3) -0.003(3) 0.037(4) F3 0.0544(14) 0.0476(12) 0.104(2) 0.0024(11) 0.0254(13) -0.0008(10) F4 0.082(5) 0.038(2) 0.139(9) -0.019(3) 0.066(6) -0.021(3) F1A 0.150(9) 0.042(3) 0.071(6) -0.015(3) 0.046(6) 0.001(4) F2A 0.043(4) 0.197(15) 0.067(4) 0.029(6) -0.016(3) -0.019(5) F4A 0.066(4) 0.044(3) 0.068(5) 0.008(3) 0.020(3) 0.009(2) N1 0.0260(11) 0.0204(9) 0.0239(9) -0.0040(7) 0.0035(8) -0.0039(7) N2 0.0261(11) 0.0289(9) 0.0186(8) -0.0052(7) 0.0016(8) -0.0012(8) N3 0.0322(12) 0.0223(9) 0.0203(9) -0.0024(7) 0.0000(8) 0.0010(8) N4 0.0314(12) 0.0227(9) 0.0238(9) -0.0061(7) 0.0004(8) 0.0001(8) N5 0.0284(11) 0.0207(8) 0.0192(8) -0.0012(7) 0.0015(8) -0.0015(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 B1 F2A 1.276(8) . ? B1 F1 1.294(9) . ? B1 F4 1.321(5) . ? B1 F1A 1.377(10) . ? B1 F3 1.383(5) . ? B1 F2 1.433(7) . ? B1 F4A 1.487(6) . ? C1 N1 1.471(3) . ? C1 C2 1.502(4) . ? C2 N4 1.343(3) . ? C2 C3 1.386(3) . ? C3 C4 1.379(5) . ? C4 C5 1.376(5) . ? C5 C6 1.381(4) . ? C6 N4 1.340(3) . ? C7 N1 1.476(3) . ? C7 C8 1.503(3) . ? C8 N2 1.347(3) . ? C8 C9 1.384(4) . ? C9 C10 1.393(4) . ? C10 C11 1.365(5) . ? C11 C12 1.388(4) . ? C12 N2 1.342(3) . ? C13 N1 1.485(3) . ? C13 C14 1.517(4) . ? C14 N5 1.479(3) . ? C15 N5 1.477(3) . ? C15 C16 1.496(3) . ? C16 N3 1.348(3) . ? C16 C17 1.386(3) . ? C17 C18 1.375(4) . ? C18 C19 1.377(4) . ? C19 C20 1.379(4) . ? C20 N3 1.339(3) . ? C21 N5 1.491(3) . ? C21 C22 1.509(3) . ? C22 C23 1.379(4) . ? C22 C27 1.396(4) . ? C23 C24 1.389(4) . ? C24 C25 1.379(5) . ? C25 C26 1.361(5) . ? C26 C27 1.390(4) . ? Cl2 Co1 2.3408(8) . ? Co1 N4 2.110(2) . ? Co1 N2 2.142(2) . ? Co1 N1 2.189(2) . ? Co1 N5 2.2093(19) . ? Co1 N3 2.260(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F2A B1 F1 122.2(8) . . ? F2A B1 F4 69.5(7) . . ? F1 B1 F4 119.6(7) . . ? F2A B1 F1A 112.6(9) . . ? F1 B1 F1A 18.2(8) . . ? F4 B1 F1A 133.9(7) . . ? F2A B1 F3 118.8(5) . . ? F1 B1 F3 111.6(7) . . ? F4 B1 F3 108.0(3) . . ? F1A B1 F3 109.5(6) . . ? F2A B1 F2 38.4(5) . . ? F1 B1 F2 106.3(7) . . ? F4 B1 F2 107.6(6) . . ? F1A B1 F2 89.6(6) . . ? F3 B1 F2 102.2(5) . . ? F2A B1 F4A 107.2(6) . . ? F1 B1 F4A 80.5(6) . . ? F4 B1 F4A 44.1(4) . . ? F1A B1 F4A 98.2(6) . . ? F3 B1 F4A 108.5(3) . . ? F2 B1 F4A 143.4(5) . . ? N1 C1 C2 109.8(2) . . ? N4 C2 C3 122.3(3) . . ? N4 C2 C1 116.2(2) . . ? C3 C2 C1 121.4(2) . . ? C4 C3 C2 118.7(3) . . ? C5 C4 C3 119.2(3) . . ? C4 C5 C6 119.1(3) . . ? N4 C6 C5 122.2(3) . . ? N1 C7 C8 110.21(19) . . ? N2 C8 C9 122.8(2) . . ? N2 C8 C7 115.1(2) . . ? C9 C8 C7 122.1(2) . . ? C8 C9 C10 118.1(3) . . ? C11 C10 C9 119.6(3) . . ? C10 C11 C12 118.9(3) . . ? N2 C12 C11 122.7(3) . . ? N1 C13 C14 110.5(2) . . ? N5 C14 C13 111.18(19) . . ? N5 C15 C16 110.65(19) . . ? N3 C16 C17 122.5(2) . . ? N3 C16 C15 116.2(2) . . ? C17 C16 C15 121.3(2) . . ? C18 C17 C16 119.0(2) . . ? C17 C18 C19 119.1(2) . . ? C18 C19 C20 118.7(3) . . ? N3 C20 C19 123.3(2) . . ? N5 C21 C22 115.97(19) . . ? C23 C22 C27 118.6(2) . . ? C23 C22 C21 120.2(2) . . ? C27 C22 C21 121.1(2) . . ? C22 C23 C24 121.2(3) . . ? C25 C24 C23 119.2(3) . . ? C26 C25 C24 120.4(3) . . ? C25 C26 C27 120.7(3) . . ? C26 C27 C22 119.8(3) . . ? N4 Co1 N2 102.99(8) . . ? N4 Co1 N1 76.24(8) . . ? N2 Co1 N1 77.58(8) . . ? N4 Co1 N5 145.89(8) . . ? N2 Co1 N5 96.08(8) . . ? N1 Co1 N5 80.68(7) . . ? N4 Co1 N3 84.84(7) . . ? N2 Co1 N3 170.70(8) . . ? N1 Co1 N3 99.76(8) . . ? N5 Co1 N3 74.64(7) . . ? N4 Co1 Cl2 103.78(7) . . ? N2 Co1 Cl2 94.14(6) . . ? N1 Co1 Cl2 171.41(6) . . ? N5 Co1 Cl2 102.73(6) . . ? N3 Co1 Cl2 88.77(6) . . ? C1 N1 C7 110.56(19) . . ? C1 N1 C13 112.79(19) . . ? C7 N1 C13 110.2(2) . . ? C1 N1 Co1 105.23(16) . . ? C7 N1 Co1 107.78(15) . . ? C13 N1 Co1 110.09(15) . . ? C12 N2 C8 117.9(2) . . ? C12 N2 Co1 125.38(18) . . ? C8 N2 Co1 115.62(16) . . ? C20 N3 C16 117.4(2) . . ? C20 N3 Co1 130.18(16) . . ? C16 N3 Co1 112.40(16) . . ? C6 N4 C2 118.4(2) . . ? C6 N4 Co1 126.37(18) . . ? C2 N4 Co1 114.25(16) . . ? C15 N5 C14 110.67(19) . . ? C15 N5 C21 110.36(18) . . ? C14 N5 C21 112.3(2) . . ? C15 N5 Co1 105.46(15) . . ? C14 N5 Co1 105.55(13) . . ? C21 N5 Co1 112.22(13) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.09 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.903 _refine_diff_density_min -1.193 _refine_diff_density_rms 0.098 #===END OF DATA FOR 3 # 4.4 REAULTS FOR 4 data_shin172sa _database_code_depnum_ccdc_archive 'CCDC 772154' #TrackingRef '- alldata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H25 Cl Co F6 N5 Sb' _chemical_formula_weight 677.59 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 18.260(4) _cell_length_b 9.1630(18) _cell_length_c 15.057(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2519.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.787 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 1.901 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'STOE IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20623 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.24 _diffrn_reflns_theta_max 28.05 _reflns_number_total 6001 _reflns_number_gt 5449 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS Software (1997)' _computing_cell_refinement 'STOE IPDS Software (1997)' _computing_data_reduction 'STOE IPDS Software (1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0640P)^2^+0.3112P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.011(18) _refine_ls_number_reflns 6001 _refine_ls_number_parameters 318 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0976 _refine_ls_wR_factor_gt 0.0945 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 C1 C 0.0740(3) 0.7602(6) 0.8247(3) 0.0589(13) Uani 1 1 d . . . H1A H 0.0454 0.8514 0.8315 0.071 Uiso 1 1 calc R . . H1B H 0.0643 0.6978 0.8770 0.071 Uiso 1 1 calc R . . C2 C 0.0504(2) 0.6826(5) 0.7422(3) 0.0454(9) Uani 1 1 d . . . C3 C -0.0219(3) 0.6738(7) 0.7156(4) 0.0626(14) Uani 1 1 d . . . H3 H -0.0588 0.7222 0.7489 0.075 Uiso 1 1 calc R . . C4 C -0.0402(3) 0.5971(6) 0.6429(4) 0.0608(14) Uani 1 1 d . . . H4 H -0.0900 0.5903 0.6249 0.073 Uiso 1 1 calc R . . C5 C 0.0145(3) 0.5277(6) 0.5940(3) 0.0524(11) Uani 1 1 d . . . H5 H 0.0030 0.4756 0.5413 0.063 Uiso 1 1 calc R . . C6 C 0.0857(2) 0.5367(5) 0.6243(2) 0.0372(7) Uani 1 1 d . . . H6 H 0.1232 0.4866 0.5929 0.045 Uiso 1 1 calc R . . C7 C 0.1659(4) 0.9135(4) 0.7567(3) 0.0585(14) Uani 1 1 d . . . H7A H 0.1580 1.0087 0.7862 0.070 Uiso 1 1 calc R . . H7B H 0.1309 0.9058 0.7067 0.070 Uiso 1 1 calc R . . C8 C 0.2411(4) 0.9058(4) 0.7227(3) 0.0552(14) Uani 1 1 d . . . C9 C 0.2821(5) 1.0278(6) 0.7002(4) 0.084(2) Uani 1 1 d . . . H9 H 0.2617 1.1226 0.7069 0.100 Uiso 1 1 calc R . . C10 C 0.3508(5) 1.0122(8) 0.6687(4) 0.104(4) Uani 1 1 d . . . H10 H 0.3791 1.0957 0.6539 0.125 Uiso 1 1 calc R . . C11 C 0.3793(5) 0.8755(10) 0.6584(3) 0.088(3) Uani 1 1 d . . . H11 H 0.4277 0.8625 0.6365 0.105 Uiso 1 1 calc R . . C12 C 0.3366(3) 0.7563(6) 0.6806(3) 0.0534(11) Uani 1 1 d . . . H12 H 0.3563 0.6611 0.6733 0.064 Uiso 1 1 calc R . . C13 C 0.1856(3) 0.8272(5) 0.9075(3) 0.0539(11) Uani 1 1 d . . . H13A H 0.1500 0.8809 0.9449 0.065 Uiso 1 1 calc R . . H13B H 0.2292 0.8899 0.8993 0.065 Uiso 1 1 calc R . . C14 C 0.2076(3) 0.6873(5) 0.9536(2) 0.0470(9) Uani 1 1 d . . . H14A H 0.2340 0.7106 1.0092 0.056 Uiso 1 1 calc R . . H14B H 0.1632 0.6308 0.9692 0.056 Uiso 1 1 calc R . . C15 C 0.3310(3) 0.6509(6) 0.8954(3) 0.0533(11) Uani 1 1 d . . . H15A H 0.3488 0.6556 0.9567 0.080 Uiso 1 1 calc R . . H15B H 0.3328 0.7485 0.8689 0.080 Uiso 1 1 calc R . . H15C H 0.3620 0.5843 0.8610 0.080 Uiso 1 1 calc R . . C16 C 0.2548(2) 0.4454(4) 0.9272(3) 0.0411(8) Uani 1 1 d . . . H16A H 0.2654 0.4444 0.9916 0.049 Uiso 1 1 calc R . . H16B H 0.2938 0.3895 0.8967 0.049 Uiso 1 1 calc R . . C17 C 0.1832(2) 0.3739(4) 0.9110(2) 0.0349(7) Uani 1 1 d . . . C18 C 0.1577(2) 0.2622(4) 0.9659(3) 0.0411(8) Uani 1 1 d . . . H18 H 0.1856 0.2314 1.0157 0.049 Uiso 1 1 calc R . . C19 C 0.0923(3) 0.1978(5) 0.9470(3) 0.0488(10) Uani 1 1 d . . . H19 H 0.0736 0.1229 0.9843 0.059 Uiso 1 1 calc R . . C20 C 0.0534(3) 0.2421(5) 0.8736(3) 0.0486(9) Uani 1 1 d . . . H20 H 0.0079 0.1981 0.8589 0.058 Uiso 1 1 calc R . . C21 C 0.0823(2) 0.3523(5) 0.8218(3) 0.0453(9) Uani 1 1 d . . . H21 H 0.0561 0.3816 0.7704 0.054 Uiso 1 1 calc R . . Cl1 Cl 0.26686(5) 0.41919(9) 0.68569(8) 0.0414(2) Uani 1 1 d . . . Co1 Co 0.20438(2) 0.59800(4) 0.76507(3) 0.02511(10) Uani 1 1 d . . . F1 F 0.4065(4) -0.0960(4) 0.0438(4) 0.121(3) Uani 1 1 d . . . F2 F 0.50723(18) 0.1013(4) 0.0057(3) 0.0792(10) Uani 1 1 d . . . F3 F 0.4184(2) 0.0106(5) -0.1143(2) 0.0845(11) Uani 1 1 d . . . F4 F 0.4081(2) 0.2760(4) -0.0488(4) 0.0898(12) Uani 1 1 d . . . F5 F 0.3049(2) 0.0827(7) -0.0157(7) 0.151(3) Uani 1 1 d . . . F6 F 0.3962(3) 0.1658(5) 0.1115(3) 0.1143(19) Uani 1 1 d . . . N1 N 0.1524(2) 0.7950(4) 0.8203(2) 0.0452(8) Uani 1 1 d . . . N2 N 0.10376(17) 0.6149(4) 0.6974(2) 0.0339(6) Uani 1 1 d . . . N3 N 0.2690(2) 0.7710(3) 0.71158(19) 0.0412(8) Uani 1 1 d . . . N4 N 0.2555(2) 0.5978(3) 0.8948(2) 0.0356(6) Uani 1 1 d . . . N5 N 0.14509(19) 0.4194(3) 0.8404(2) 0.0364(7) Uani 1 1 d . . . Sb1 Sb 0.404201(15) 0.08824(3) -0.001728(19) 0.04439(9) 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 C1 0.064(3) 0.070(3) 0.043(2) -0.005(2) 0.011(2) 0.041(3) C2 0.046(2) 0.053(2) 0.0375(18) 0.0115(15) 0.0056(15) 0.0225(18) C3 0.042(2) 0.081(3) 0.065(3) 0.023(3) 0.012(2) 0.035(2) C4 0.030(2) 0.085(4) 0.067(3) 0.033(3) -0.009(2) 0.001(2) C5 0.042(2) 0.068(3) 0.048(2) 0.015(2) -0.0106(17) -0.005(2) C6 0.0370(19) 0.0437(19) 0.0308(15) 0.0052(14) 0.0004(13) -0.0015(16) C7 0.104(4) 0.0276(18) 0.044(2) -0.0007(14) -0.006(3) 0.0214(19) C8 0.109(4) 0.0276(16) 0.0294(17) 0.0067(13) -0.012(2) -0.014(2) C9 0.161(7) 0.040(2) 0.049(3) 0.0148(19) -0.028(4) -0.046(4) C10 0.174(9) 0.088(5) 0.049(3) 0.022(3) -0.023(4) -0.103(6) C11 0.101(5) 0.123(6) 0.039(2) 0.010(3) 0.003(3) -0.082(5) C12 0.057(3) 0.066(3) 0.0368(18) -0.0001(18) 0.0087(17) -0.030(2) C13 0.085(4) 0.041(2) 0.0354(18) -0.0102(16) 0.000(2) 0.007(2) C14 0.070(3) 0.048(2) 0.0227(14) -0.0026(14) 0.0001(16) 0.002(2) C15 0.054(3) 0.059(3) 0.047(2) 0.0100(19) -0.0165(19) -0.020(2) C16 0.040(2) 0.0430(18) 0.0398(18) 0.0178(16) -0.0055(15) -0.0012(17) C17 0.0362(18) 0.0318(15) 0.0367(16) 0.0098(13) 0.0083(14) 0.0067(15) C18 0.051(2) 0.0345(17) 0.0377(16) 0.0102(13) 0.0081(15) 0.0022(16) C19 0.063(3) 0.0344(18) 0.049(2) 0.0066(16) 0.0219(19) -0.0059(18) C20 0.044(2) 0.042(2) 0.061(2) 0.0050(17) 0.0125(18) -0.0147(17) C21 0.039(2) 0.046(2) 0.051(2) 0.0078(18) -0.0006(17) -0.0032(18) Cl1 0.0349(5) 0.0309(4) 0.0583(5) -0.0083(3) 0.0100(4) 0.0047(3) Co1 0.0286(2) 0.02074(17) 0.02604(18) 0.00203(17) 0.00262(16) 0.00142(14) F1 0.231(8) 0.047(2) 0.085(3) 0.0133(16) 0.034(3) -0.011(2) F2 0.0456(16) 0.106(3) 0.086(2) -0.011(2) -0.0113(18) 0.0116(15) F3 0.105(3) 0.096(3) 0.0521(17) -0.0241(17) -0.0071(17) -0.005(2) F4 0.100(3) 0.0541(18) 0.115(3) 0.0167(19) -0.015(2) 0.0093(18) F5 0.0411(19) 0.158(5) 0.254(10) -0.057(5) 0.003(4) -0.008(2) F6 0.173(5) 0.088(3) 0.081(2) -0.040(2) 0.060(3) -0.026(3) N1 0.068(2) 0.0338(15) 0.0337(14) -0.0001(12) -0.0014(15) 0.0174(16) N2 0.0318(15) 0.0364(14) 0.0337(14) 0.0070(12) 0.0049(11) 0.0091(11) N3 0.062(2) 0.0326(14) 0.0287(13) 0.0038(11) 0.0008(13) -0.0190(15) N4 0.0380(17) 0.0373(15) 0.0315(13) 0.0060(11) -0.0009(12) -0.0030(12) N5 0.0309(16) 0.0348(15) 0.0435(16) 0.0105(12) 0.0059(13) 0.0023(12) Sb1 0.04162(15) 0.03831(13) 0.05323(15) -0.00638(13) 0.00595(12) 0.00461(9) _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 C1 N1 1.468(7) . ? C1 C2 1.494(7) . ? C2 N2 1.337(5) . ? C2 C3 1.382(7) . ? C3 C4 1.343(9) . ? C4 C5 1.393(8) . ? C5 C6 1.381(6) . ? C6 N2 1.354(5) . ? C7 N1 1.468(5) . ? C7 C8 1.468(9) . ? C8 N3 1.347(6) . ? C8 C9 1.387(7) . ? C9 C10 1.349(12) . ? C10 C11 1.366(13) . ? C11 C12 1.383(7) . ? C12 N3 1.327(6) . ? C13 N1 1.477(5) . ? C13 C14 1.512(6) . ? C14 N4 1.490(5) . ? C15 N4 1.462(6) . ? C16 N4 1.480(5) . ? C16 C17 1.483(6) . ? C17 N5 1.336(5) . ? C17 C18 1.396(5) . ? C18 C19 1.362(7) . ? C19 C20 1.374(7) . ? C20 C21 1.381(6) . ? C21 N5 1.330(6) . ? Cl1 Co1 2.3271(10) . ? Co1 N2 2.106(3) . ? Co1 N3 2.134(3) . ? Co1 N4 2.165(3) . ? Co1 N1 2.203(3) . ? Co1 N5 2.267(3) . ? F1 Sb1 1.822(4) . ? F2 Sb1 1.889(3) . ? F3 Sb1 1.856(3) . ? F4 Sb1 1.863(4) . ? F5 Sb1 1.827(4) . ? F6 Sb1 1.852(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 110.2(3) . . ? N2 C2 C3 121.5(4) . . ? N2 C2 C1 115.5(4) . . ? C3 C2 C1 122.9(4) . . ? C4 C3 C2 120.3(4) . . ? C3 C4 C5 119.4(4) . . ? C6 C5 C4 118.3(5) . . ? N2 C6 C5 122.0(4) . . ? N1 C7 C8 110.5(4) . . ? N3 C8 C9 120.4(7) . . ? N3 C8 C7 116.2(4) . . ? C9 C8 C7 123.5(5) . . ? C10 C9 C8 120.1(6) . . ? C9 C10 C11 119.5(5) . . ? C10 C11 C12 118.8(7) . . ? N3 C12 C11 122.0(6) . . ? N1 C13 C14 110.3(3) . . ? N4 C14 C13 110.5(3) . . ? N4 C16 C17 111.7(3) . . ? N5 C17 C18 121.7(4) . . ? N5 C17 C16 116.9(3) . . ? C18 C17 C16 121.4(3) . . ? C19 C18 C17 119.1(4) . . ? C18 C19 C20 119.5(4) . . ? C19 C20 C21 118.2(4) . . ? N5 C21 C20 123.3(4) . . ? N2 Co1 N3 104.21(13) . . ? N2 Co1 N4 144.32(13) . . ? N3 Co1 N4 95.90(12) . . ? N2 Co1 N1 75.29(14) . . ? N3 Co1 N1 76.83(15) . . ? N4 Co1 N1 81.15(13) . . ? N2 Co1 N5 83.01(13) . . ? N3 Co1 N5 171.64(13) . . ? N4 Co1 N5 75.75(13) . . ? N1 Co1 N5 101.36(13) . . ? N2 Co1 Cl1 103.35(9) . . ? N3 Co1 Cl1 93.32(10) . . ? N4 Co1 Cl1 104.58(10) . . ? N1 Co1 Cl1 169.19(10) . . ? N5 Co1 Cl1 89.02(9) . . ? C7 N1 C1 110.7(4) . . ? C7 N1 C13 111.3(4) . . ? C1 N1 C13 113.8(4) . . ? C7 N1 Co1 106.7(3) . . ? C1 N1 Co1 105.1(3) . . ? C13 N1 Co1 108.8(3) . . ? C2 N2 C6 118.6(4) . . ? C2 N2 Co1 115.2(3) . . ? C6 N2 Co1 124.5(3) . . ? C12 N3 C8 119.2(4) . . ? C12 N3 Co1 124.9(3) . . ? C8 N3 Co1 115.2(3) . . ? C15 N4 C16 108.7(3) . . ? C15 N4 C14 111.5(4) . . ? C16 N4 C14 108.6(3) . . ? C15 N4 Co1 114.3(2) . . ? C16 N4 Co1 107.1(2) . . ? C14 N4 Co1 106.4(2) . . ? C21 N5 C17 118.1(3) . . ? C21 N5 Co1 129.8(3) . . ? C17 N5 Co1 112.0(3) . . ? F1 Sb1 F5 92.3(3) . . ? F1 Sb1 F6 90.6(3) . . ? F5 Sb1 F6 92.2(4) . . ? F1 Sb1 F3 89.1(2) . . ? F5 Sb1 F3 91.3(3) . . ? F6 Sb1 F3 176.5(2) . . ? F1 Sb1 F4 176.4(3) . . ? F5 Sb1 F4 91.1(3) . . ? F6 Sb1 F4 90.0(2) . . ? F3 Sb1 F4 90.1(2) . . ? F1 Sb1 F2 90.7(3) . . ? F5 Sb1 F2 176.2(4) . . ? F6 Sb1 F2 90.0(2) . . ? F3 Sb1 F2 86.5(2) . . ? F4 Sb1 F2 85.76(17) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 28.05 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.552 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.086 #===END OF DATA FOR 4 # 4.5 REAULTS FOR 5 data_shin184s _database_code_depnum_ccdc_archive 'CCDC 772155' #TrackingRef '- alldata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H52 B Co N5 O2' _chemical_formula_weight 860.74 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 13.234(3) _cell_length_b 13.491(3) _cell_length_c 13.920(3) _cell_angle_alpha 96.33(3) _cell_angle_beta 114.02(3) _cell_angle_gamma 101.27(3) _cell_volume 2175.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 906 _exptl_absorpt_coefficient_mu 0.443 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'STOE IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19812 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0732 _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 -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 28.17 _reflns_number_total 9719 _reflns_number_gt 6327 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS Software (1997)' _computing_cell_refinement 'STOE IPDS Software (1997)' _computing_data_reduction 'STOE IPDS Software (1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0963P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9719 _refine_ls_number_parameters 756 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0856 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1560 _refine_ls_wR_factor_gt 0.1370 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _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 B1 B 0.6104(3) 0.4020(2) 0.8419(2) 0.0309(7) Uani 1 1 d . . . C1 C 0.7735(3) 0.6181(2) 0.6477(2) 0.0337(6) Uani 1 1 d . . . C2 C 0.8910(3) 0.6123(2) 0.7231(2) 0.0324(6) Uani 1 1 d . . . C3 C 0.9143(3) 0.5180(2) 0.7405(2) 0.0412(7) Uani 1 1 d . . . C4 C 1.0238(3) 0.5183(3) 0.8098(3) 0.0494(9) Uani 1 1 d . . . C5 C 1.1051(3) 0.6105(3) 0.8604(3) 0.0485(9) Uani 1 1 d . . . C6 C 1.0761(3) 0.7012(3) 0.8384(3) 0.0445(8) Uani 1 1 d . . . C7 C 0.7473(3) 0.7409(2) 0.7705(2) 0.0346(6) Uani 1 1 d . . . C8 C 0.7913(2) 0.8552(2) 0.8224(2) 0.0304(6) Uani 1 1 d . . . C9 C 0.7493(3) 0.8974(3) 0.8890(2) 0.0412(7) Uani 1 1 d . . . C10 C 0.7962(3) 1.0015(3) 0.9384(3) 0.0484(9) Uani 1 1 d . . . C11 C 0.8826(3) 1.0583(2) 0.9212(2) 0.0451(8) Uani 1 1 d . . . C12 C 0.9196(3) 1.0108(2) 0.8536(2) 0.0400(7) Uani 1 1 d . . . C13 C 0.6643(2) 0.7413(2) 0.5790(2) 0.0314(6) Uani 1 1 d . . . C14 C 0.7018(2) 0.7734(2) 0.4955(2) 0.0310(6) Uani 1 1 d . . . C15 C 0.8585(3) 0.8768(2) 0.4740(2) 0.0371(7) Uani 1 1 d . . . C16 C 0.9267(3) 0.7988(2) 0.4784(2) 0.0363(7) Uani 1 1 d . . . C17 C 0.9517(3) 0.7708(3) 0.3941(3) 0.0425(7) Uani 1 1 d . . . C18 C 1.0166(3) 0.7005(3) 0.4019(3) 0.0520(9) Uani 1 1 d . . . C19 C 1.0537(3) 0.6613(3) 0.4928(3) 0.0558(10) Uani 1 1 d . . . C20 C 1.0270(3) 0.6934(3) 0.5733(3) 0.0503(9) Uani 1 1 d . . . C21 C 0.7684(3) 0.9630(2) 0.5654(2) 0.0323(6) Uani 1 1 d . . . C22 C 0.6892(3) 0.9957(2) 0.4675(2) 0.0319(6) Uani 1 1 d . . . C23 C 0.5707(3) 0.9621(2) 0.4280(3) 0.0396(7) Uani 1 1 d . . . C24 C 0.4988(3) 0.9980(3) 0.3430(3) 0.0488(9) Uani 1 1 d . . . C25 C 0.5441(4) 1.0681(3) 0.2981(3) 0.0542(10) Uani 1 1 d . . . C26 C 0.6621(4) 1.1018(3) 0.3351(3) 0.0498(9) Uani 1 1 d . . . C27 C 0.7342(3) 1.0654(2) 0.4192(2) 0.0405(7) Uani 1 1 d . . . C28 C 1.1152(3) 0.9891(2) 0.7579(3) 0.0403(7) Uani 1 1 d . . . C29 C 1.2419(3) 1.0541(3) 0.8198(3) 0.0611(10) Uani 1 1 d . . . H29A H 1.2581 1.1041 0.7785 0.092 Uiso 1 1 calc R . . H29B H 1.2927 1.0082 0.8297 0.092 Uiso 1 1 calc R . . H29C H 1.2550 1.0911 0.8902 0.092 Uiso 1 1 calc R . . C30 C 0.6578(2) 0.3445(2) 0.7647(2) 0.0302(6) Uani 1 1 d . . . C31 C 0.7487(3) 0.2989(2) 0.8094(2) 0.0390(7) Uani 1 1 d . . . C32 C 0.7895(3) 0.2471(3) 0.7477(3) 0.0467(8) Uani 1 1 d . . . C33 C 0.7401(3) 0.2363(3) 0.6376(3) 0.0489(9) Uani 1 1 d . . . C34 C 0.6516(3) 0.2807(3) 0.5903(3) 0.0477(8) Uani 1 1 d . . . C35 C 0.6123(3) 0.3337(2) 0.6533(2) 0.0385(7) Uani 1 1 d . . . C36 C 0.5906(2) 0.3243(2) 0.9186(2) 0.0330(6) Uani 1 1 d . . . C37 C 0.5605(3) 0.2163(3) 0.8850(3) 0.0469(8) Uani 1 1 d . . . C38 C 0.5433(4) 0.1490(3) 0.9473(3) 0.0575(10) Uani 1 1 d . . . C39 C 0.5509(4) 0.1852(3) 1.0472(3) 0.0568(9) Uani 1 1 d . . . C40 C 0.5775(3) 0.2903(3) 1.0823(3) 0.0527(9) Uani 1 1 d . . . C41 C 0.5966(3) 0.3572(2) 1.0197(2) 0.0385(7) Uani 1 1 d . . . C42 C 0.4902(2) 0.4311(2) 0.7711(2) 0.0335(6) Uani 1 1 d . . . C43 C 0.3900(3) 0.3961(3) 0.7815(3) 0.0422(8) Uani 1 1 d . . . C44 C 0.2920(3) 0.4282(3) 0.7288(3) 0.0583(11) Uani 1 1 d . . . C45 C 0.2888(3) 0.4931(4) 0.6604(3) 0.0664(13) Uani 1 1 d . . . C46 C 0.4844(3) 0.4998(3) 0.7023(3) 0.0475(8) Uani 1 1 d . . . C47 C 0.3856(4) 0.5297(3) 0.6460(3) 0.0645(12) Uani 1 1 d . . . C48 C 0.7047(2) 0.5124(2) 0.9163(2) 0.0297(6) Uani 1 1 d . . . C49 C 0.8205(2) 0.5387(2) 0.9378(2) 0.0336(6) Uani 1 1 d . . . C50 C 0.8967(3) 0.6321(3) 1.0030(3) 0.0442(8) Uani 1 1 d . . . C51 C 0.8604(3) 0.7031(2) 1.0512(3) 0.0483(8) Uani 1 1 d . . . C52 C 0.7469(3) 0.6803(2) 1.0312(3) 0.0489(8) Uani 1 1 d . . . C53 C 0.6710(3) 0.5879(2) 0.9648(3) 0.0413(7) Uani 1 1 d . . . Co1 Co 0.92446(3) 0.83111(3) 0.69604(3) 0.03086(12) Uani 1 1 d . . . N1 N 0.76086(18) 0.72281(16) 0.67021(17) 0.0266(5) Uani 1 1 d . . . N2 N 0.9705(2) 0.70254(18) 0.76983(19) 0.0353(6) Uani 1 1 d . . . N3 N 0.8746(2) 0.91013(17) 0.80475(17) 0.0303(5) Uani 1 1 d . . . N4 N 0.80096(19) 0.86548(16) 0.54470(17) 0.0290(5) Uani 1 1 d . . . N5 N 0.9631(2) 0.76127(19) 0.5680(2) 0.0375(6) Uani 1 1 d . . . O1 O 1.0940(2) 0.90587(19) 0.7855(2) 0.0572(7) Uani 1 1 d . . . O2 O 1.0480(3) 1.0222(3) 0.6933(3) 0.0805(9) Uani 1 1 d . . . H1A H 0.765(3) 0.604(2) 0.580(3) 0.032(8) Uiso 1 1 d . . . H1B H 0.713(3) 0.564(3) 0.653(3) 0.042(9) Uiso 1 1 d . . . H3 H 0.853(3) 0.455(3) 0.704(3) 0.052(10) Uiso 1 1 d . . . H4 H 1.043(3) 0.449(3) 0.826(3) 0.058(11) Uiso 1 1 d . . . H5 H 1.178(3) 0.612(3) 0.907(3) 0.055(11) Uiso 1 1 d . . . H6 H 1.124(3) 0.768(3) 0.862(3) 0.046(10) Uiso 1 1 d . . . H7A H 0.663(3) 0.714(3) 0.758(3) 0.039(9) Uiso 1 1 d . . . H7B H 0.795(3) 0.706(2) 0.821(3) 0.035(8) Uiso 1 1 d . . . H9 H 0.689(4) 0.854(3) 0.903(3) 0.056(11) Uiso 1 1 d . . . H10 H 0.772(3) 1.030(3) 0.990(3) 0.053(10) Uiso 1 1 d . . . H11 H 0.920(3) 1.131(3) 0.956(3) 0.062(11) Uiso 1 1 d . . . H12 H 0.979(3) 1.047(3) 0.829(3) 0.056(11) Uiso 1 1 d . . . H13A H 0.599(3) 0.676(3) 0.548(3) 0.033(8) Uiso 1 1 d . . . H13B H 0.639(3) 0.793(3) 0.609(2) 0.034(8) Uiso 1 1 d . . . H14A H 0.639(3) 0.785(2) 0.434(2) 0.028(7) Uiso 1 1 d . . . H14B H 0.723(3) 0.718(3) 0.467(3) 0.035(8) Uiso 1 1 d . . . H15A H 0.806(3) 0.870(3) 0.404(3) 0.050(10) Uiso 1 1 d . . . H15B H 0.907(3) 0.946(3) 0.496(3) 0.052(10) Uiso 1 1 d . . . H17 H 0.924(3) 0.800(3) 0.334(3) 0.042(9) Uiso 1 1 d . . . H18 H 1.034(3) 0.682(3) 0.343(3) 0.057(11) Uiso 1 1 d . . . H19 H 1.100(3) 0.619(3) 0.504(3) 0.053(10) Uiso 1 1 d . . . H20 H 1.052(4) 0.667(3) 0.636(4) 0.065(12) Uiso 1 1 d . . . H21A H 0.733(3) 0.955(2) 0.613(3) 0.034(8) Uiso 1 1 d . . . H21B H 0.841(3) 1.017(2) 0.605(3) 0.033(8) Uiso 1 1 d . . . H23 H 0.542(3) 0.919(3) 0.463(3) 0.046(10) Uiso 1 1 d . . . H24 H 0.421(4) 0.975(3) 0.320(3) 0.054(11) Uiso 1 1 d . . . H25 H 0.499(4) 1.096(3) 0.243(3) 0.064(12) Uiso 1 1 d . . . H26 H 0.697(3) 1.153(3) 0.306(3) 0.054(11) Uiso 1 1 d . . . H27 H 0.816(4) 1.086(4) 0.446(4) 0.077(14) Uiso 1 1 d . . . H31 H 0.782(3) 0.305(3) 0.887(3) 0.050(10) Uiso 1 1 d . . . H32 H 0.857(3) 0.227(3) 0.782(3) 0.056(11) Uiso 1 1 d . . . H33 H 0.766(4) 0.205(3) 0.593(3) 0.061(11) Uiso 1 1 d . . . H34 H 0.616(3) 0.272(3) 0.516(3) 0.054(11) Uiso 1 1 d . . . H35 H 0.548(3) 0.360(3) 0.619(3) 0.043(9) Uiso 1 1 d . . . H37 H 0.557(3) 0.194(3) 0.818(3) 0.060(11) Uiso 1 1 d . . . H38 H 0.516(4) 0.079(4) 0.918(4) 0.082(15) Uiso 1 1 d . . . H39 H 0.539(4) 0.138(4) 1.091(4) 0.082(15) Uiso 1 1 d . . . H40 H 0.580(3) 0.311(3) 1.149(3) 0.054(10) Uiso 1 1 d . . . H41 H 0.620(3) 0.430(3) 1.050(3) 0.044(9) Uiso 1 1 d . . . H43 H 0.388(3) 0.351(3) 0.825(3) 0.045(10) Uiso 1 1 d . . . H44 H 0.228(4) 0.409(3) 0.742(3) 0.056(11) Uiso 1 1 d . . . H45 H 0.226(4) 0.516(4) 0.627(4) 0.078(14) Uiso 1 1 d . . . H46 H 0.546(4) 0.527(3) 0.693(3) 0.058(12) Uiso 1 1 d . . . H47 H 0.392(3) 0.578(3) 0.601(3) 0.056(11) Uiso 1 1 d . . . H49 H 0.848(3) 0.492(3) 0.906(3) 0.042(9) Uiso 1 1 d . . . H50 H 0.971(3) 0.645(3) 1.013(3) 0.046(10) Uiso 1 1 d . . . H51 H 0.914(3) 0.761(3) 1.099(3) 0.060(11) Uiso 1 1 d . . . H52 H 0.716(4) 0.724(4) 1.057(4) 0.069(13) Uiso 1 1 d . . . H53 H 0.593(3) 0.583(3) 0.952(3) 0.052(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0337(15) 0.0281(14) 0.0281(13) 0.0017(11) 0.0118(12) 0.0088(12) C1 0.0371(15) 0.0237(12) 0.0323(14) 0.0021(11) 0.0099(12) 0.0051(11) C2 0.0406(14) 0.0283(12) 0.0299(12) 0.0074(10) 0.0157(12) 0.0113(11) C3 0.0574(19) 0.0334(15) 0.0388(15) 0.0116(12) 0.0221(15) 0.0210(14) C4 0.067(2) 0.0495(18) 0.0398(16) 0.0167(14) 0.0217(16) 0.0336(17) C5 0.0476(18) 0.063(2) 0.0397(16) 0.0196(15) 0.0137(15) 0.0326(17) C6 0.0411(16) 0.0477(18) 0.0376(15) 0.0079(14) 0.0091(14) 0.0154(14) C7 0.0439(16) 0.0313(13) 0.0285(12) 0.0086(11) 0.0142(12) 0.0128(12) C8 0.0348(13) 0.0343(13) 0.0223(11) 0.0099(10) 0.0097(11) 0.0136(11) C9 0.0513(18) 0.0462(17) 0.0338(14) 0.0121(13) 0.0218(14) 0.0207(15) C10 0.070(2) 0.0482(18) 0.0398(16) 0.0087(14) 0.0316(17) 0.0269(18) C11 0.067(2) 0.0321(15) 0.0370(15) 0.0036(13) 0.0236(16) 0.0150(15) C12 0.0504(17) 0.0330(14) 0.0317(13) 0.0047(12) 0.0141(14) 0.0107(13) C13 0.0290(13) 0.0335(13) 0.0289(12) 0.0054(11) 0.0094(11) 0.0103(11) C14 0.0346(14) 0.0274(12) 0.0267(12) 0.0034(10) 0.0095(11) 0.0093(11) C15 0.0480(17) 0.0338(15) 0.0349(14) 0.0078(12) 0.0212(14) 0.0153(13) C16 0.0401(15) 0.0281(13) 0.0392(14) 0.0011(11) 0.0180(13) 0.0079(11) C17 0.0468(17) 0.0411(16) 0.0423(16) 0.0028(14) 0.0255(15) 0.0081(14) C18 0.0528(19) 0.0491(19) 0.062(2) -0.0032(17) 0.0363(18) 0.0132(16) C19 0.056(2) 0.055(2) 0.074(2) 0.0117(19) 0.038(2) 0.0312(18) C20 0.0540(19) 0.0524(19) 0.059(2) 0.0160(17) 0.0311(18) 0.0283(16) C21 0.0430(15) 0.0275(13) 0.0277(12) 0.0046(11) 0.0154(13) 0.0129(12) C22 0.0446(15) 0.0244(12) 0.0282(12) 0.0020(10) 0.0162(12) 0.0141(11) C23 0.0476(17) 0.0365(15) 0.0411(15) 0.0070(13) 0.0233(15) 0.0172(13) C24 0.0456(19) 0.057(2) 0.0451(17) 0.0062(16) 0.0179(16) 0.0231(16) C25 0.068(2) 0.066(2) 0.0354(15) 0.0160(16) 0.0183(17) 0.039(2) C26 0.071(2) 0.0458(18) 0.0404(16) 0.0203(15) 0.0260(17) 0.0232(17) C27 0.0507(18) 0.0327(14) 0.0355(14) 0.0072(12) 0.0154(14) 0.0129(13) C28 0.0605(19) 0.0359(15) 0.0456(16) 0.0172(13) 0.0390(16) 0.0184(14) C29 0.058(2) 0.054(2) 0.053(2) -0.0099(17) 0.0232(18) -0.0092(17) C30 0.0332(13) 0.0256(12) 0.0290(12) 0.0003(10) 0.0141(11) 0.0040(10) C31 0.0479(17) 0.0376(15) 0.0364(14) 0.0087(12) 0.0195(14) 0.0196(13) C32 0.056(2) 0.0368(16) 0.0593(19) 0.0105(14) 0.0329(17) 0.0214(15) C33 0.060(2) 0.0349(15) 0.0562(19) -0.0086(14) 0.0372(18) 0.0051(14) C34 0.0516(19) 0.0500(18) 0.0310(14) -0.0092(13) 0.0199(14) -0.0034(15) C35 0.0362(15) 0.0424(15) 0.0276(12) -0.0014(12) 0.0087(12) 0.0071(13) C36 0.0338(13) 0.0330(13) 0.0289(12) 0.0024(11) 0.0113(11) 0.0095(11) C37 0.064(2) 0.0359(16) 0.0422(16) 0.0033(13) 0.0287(16) 0.0074(15) C38 0.077(3) 0.0358(17) 0.062(2) 0.0110(16) 0.035(2) 0.0086(17) C39 0.072(3) 0.057(2) 0.052(2) 0.0250(18) 0.035(2) 0.0159(19) C40 0.063(2) 0.065(2) 0.0362(16) 0.0119(16) 0.0269(17) 0.0167(18) C41 0.0421(16) 0.0391(15) 0.0331(14) 0.0033(12) 0.0174(13) 0.0088(13) C42 0.0320(13) 0.0327(13) 0.0299(12) -0.0030(11) 0.0104(11) 0.0083(11) C43 0.0333(15) 0.0486(18) 0.0360(15) -0.0038(14) 0.0097(13) 0.0118(13) C44 0.0337(17) 0.072(3) 0.051(2) -0.0130(19) 0.0064(16) 0.0160(17) C45 0.045(2) 0.077(3) 0.055(2) -0.008(2) -0.0019(18) 0.035(2) C46 0.0507(19) 0.0441(17) 0.0414(16) 0.0087(14) 0.0125(16) 0.0163(15) C47 0.077(3) 0.056(2) 0.0459(19) 0.0106(17) 0.0065(19) 0.033(2) C48 0.0345(13) 0.0277(12) 0.0246(11) 0.0046(10) 0.0110(11) 0.0080(10) C49 0.0344(14) 0.0349(14) 0.0275(12) 0.0086(11) 0.0088(11) 0.0099(11) C50 0.0383(17) 0.0430(17) 0.0379(15) 0.0118(13) 0.0070(14) 0.0015(13) C51 0.061(2) 0.0291(14) 0.0392(15) 0.0014(13) 0.0156(16) -0.0045(14) C52 0.070(2) 0.0286(14) 0.0495(18) -0.0003(13) 0.0312(18) 0.0086(15) C53 0.0462(17) 0.0314(14) 0.0449(16) 0.0010(12) 0.0203(15) 0.0108(13) Co1 0.0322(2) 0.02576(18) 0.03027(19) 0.00311(13) 0.01025(15) 0.00753(14) N1 0.0257(10) 0.0239(10) 0.0266(10) 0.0049(8) 0.0092(9) 0.0042(8) N2 0.0339(12) 0.0349(12) 0.0326(11) 0.0082(10) 0.0085(10) 0.0123(10) N3 0.0341(11) 0.0308(11) 0.0246(10) 0.0065(9) 0.0120(9) 0.0075(9) N4 0.0349(11) 0.0251(10) 0.0300(10) 0.0051(9) 0.0169(10) 0.0091(9) N5 0.0397(13) 0.0367(12) 0.0419(13) 0.0079(10) 0.0213(11) 0.0149(11) O1 0.0584(15) 0.0401(12) 0.0673(16) 0.0058(12) 0.0263(13) 0.0066(11) O2 0.0663(18) 0.107(3) 0.0717(19) 0.0338(19) 0.0295(16) 0.0244(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 B1 C36 1.636(5) . ? B1 C30 1.644(4) . ? B1 C42 1.645(4) . ? B1 C48 1.652(4) . ? C1 N1 1.470(3) . ? C1 C2 1.504(4) . ? C2 N2 1.334(4) . ? C2 C3 1.390(4) . ? C3 C4 1.374(5) . ? C4 C5 1.367(6) . ? C5 C6 1.381(5) . ? C6 N2 1.339(4) . ? C7 N1 1.478(4) . ? C7 C8 1.517(4) . ? C8 N3 1.329(4) . ? C8 C9 1.386(4) . ? C9 C10 1.389(5) . ? C10 C11 1.369(6) . ? C11 C12 1.378(5) . ? C12 N3 1.346(4) . ? C13 N1 1.476(3) . ? C13 C14 1.511(4) . ? C14 N4 1.475(4) . ? C15 N4 1.474(4) . ? C15 C16 1.504(4) . ? C16 N5 1.337(4) . ? C16 C17 1.377(4) . ? C17 C18 1.383(5) . ? C18 C19 1.366(6) . ? C19 C20 1.359(5) . ? C20 N5 1.351(4) . ? C21 N4 1.497(3) . ? C21 C22 1.517(4) . ? C22 C23 1.390(5) . ? C22 C27 1.393(5) . ? C23 C24 1.389(5) . ? C24 C25 1.365(6) . ? C25 C26 1.388(6) . ? C26 C27 1.387(5) . ? C28 O2 1.179(4) . ? C28 O1 1.244(4) . ? C28 C29 1.551(5) . ? C30 C35 1.394(4) . ? C30 C31 1.407(4) . ? C31 C32 1.382(4) . ? C32 C33 1.377(5) . ? C33 C34 1.376(5) . ? C34 C35 1.390(4) . ? C36 C41 1.394(4) . ? C36 C37 1.404(4) . ? C37 C38 1.372(6) . ? C38 C39 1.378(6) . ? C39 C40 1.373(6) . ? C40 C41 1.379(5) . ? C42 C43 1.390(5) . ? C42 C46 1.394(5) . ? C43 C44 1.386(5) . ? C44 C45 1.356(7) . ? C45 C47 1.382(7) . ? C46 C47 1.388(5) . ? C48 C49 1.398(4) . ? C48 C53 1.402(4) . ? C49 C50 1.391(4) . ? C50 C51 1.378(5) . ? C51 C52 1.374(6) . ? C52 C53 1.385(4) . ? Co1 O1 2.041(3) . ? Co1 N3 2.143(2) . ? Co1 N2 2.175(2) . ? Co1 N5 2.211(3) . ? Co1 N1 2.228(2) . ? Co1 N4 2.243(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C36 B1 C30 108.0(2) . . ? C36 B1 C42 110.1(3) . . ? C30 B1 C42 112.0(2) . . ? C36 B1 C48 110.3(2) . . ? C30 B1 C48 110.1(2) . . ? C42 B1 C48 106.4(2) . . ? N1 C1 C2 110.1(2) . . ? N2 C2 C3 122.8(3) . . ? N2 C2 C1 115.8(2) . . ? C3 C2 C1 121.4(3) . . ? C4 C3 C2 118.3(3) . . ? C5 C4 C3 119.3(3) . . ? C4 C5 C6 119.2(3) . . ? N2 C6 C5 122.5(3) . . ? N1 C7 C8 110.2(2) . . ? N3 C8 C9 122.7(3) . . ? N3 C8 C7 116.7(2) . . ? C9 C8 C7 120.5(3) . . ? C8 C9 C10 118.2(4) . . ? C11 C10 C9 119.4(3) . . ? C10 C11 C12 118.9(3) . . ? N3 C12 C11 122.3(4) . . ? N1 C13 C14 110.4(2) . . ? N4 C14 C13 110.2(2) . . ? N4 C15 C16 111.8(3) . . ? N5 C16 C17 122.7(3) . . ? N5 C16 C15 116.9(3) . . ? C17 C16 C15 120.4(3) . . ? C16 C17 C18 118.8(3) . . ? C19 C18 C17 119.0(3) . . ? C20 C19 C18 119.0(3) . . ? N5 C20 C19 123.5(4) . . ? N4 C21 C22 116.5(2) . . ? C23 C22 C27 118.5(3) . . ? C23 C22 C21 121.1(3) . . ? C27 C22 C21 120.3(3) . . ? C24 C23 C22 120.8(4) . . ? C25 C24 C23 120.1(4) . . ? C24 C25 C26 120.2(3) . . ? C27 C26 C25 119.9(4) . . ? C26 C27 C22 120.5(3) . . ? O2 C28 O1 126.0(4) . . ? O2 C28 C29 119.4(4) . . ? O1 C28 C29 114.6(3) . . ? C35 C30 C31 114.7(3) . . ? C35 C30 B1 124.9(2) . . ? C31 C30 B1 120.4(2) . . ? C32 C31 C30 122.7(3) . . ? C33 C32 C31 120.5(3) . . ? C34 C33 C32 118.9(3) . . ? C33 C34 C35 120.0(3) . . ? C34 C35 C30 123.1(3) . . ? C41 C36 C37 113.7(3) . . ? C41 C36 B1 124.2(3) . . ? C37 C36 B1 122.0(2) . . ? C38 C37 C36 123.5(3) . . ? C37 C38 C39 120.7(4) . . ? C40 C39 C38 117.8(4) . . ? C39 C40 C41 120.9(3) . . ? C40 C41 C36 123.4(3) . . ? C43 C42 C46 114.9(3) . . ? C43 C42 B1 122.9(3) . . ? C46 C42 B1 122.0(3) . . ? C44 C43 C42 122.6(4) . . ? C45 C44 C43 120.6(4) . . ? C44 C45 C47 119.4(4) . . ? C47 C46 C42 123.1(4) . . ? C45 C47 C46 119.3(4) . . ? C49 C48 C53 114.8(3) . . ? C49 C48 B1 125.2(2) . . ? C53 C48 B1 120.0(3) . . ? C50 C49 C48 122.7(3) . . ? C51 C50 C49 120.5(3) . . ? C52 C51 C50 118.4(3) . . ? C51 C52 C53 120.8(3) . . ? C52 C53 C48 122.7(3) . . ? O1 Co1 N3 92.91(10) . . ? O1 Co1 N2 84.67(10) . . ? N3 Co1 N2 102.11(9) . . ? O1 Co1 N5 90.16(11) . . ? N3 Co1 N5 172.21(9) . . ? N2 Co1 N5 85.31(10) . . ? O1 Co1 N1 152.82(10) . . ? N3 Co1 N1 76.52(9) . . ? N2 Co1 N1 73.49(9) . . ? N5 Co1 N1 103.66(10) . . ? O1 Co1 N4 127.38(11) . . ? N3 Co1 N4 97.21(8) . . ? N2 Co1 N4 141.57(9) . . ? N5 Co1 N4 75.28(9) . . ? N1 Co1 N4 79.27(9) . . ? C1 N1 C13 111.5(2) . . ? C1 N1 C7 110.5(2) . . ? C13 N1 C7 111.0(2) . . ? C1 N1 Co1 106.06(17) . . ? C13 N1 Co1 109.48(17) . . ? C7 N1 Co1 108.04(17) . . ? C2 N2 C6 117.8(3) . . ? C2 N2 Co1 114.57(17) . . ? C6 N2 Co1 125.8(2) . . ? C8 N3 C12 118.5(3) . . ? C8 N3 Co1 116.79(17) . . ? C12 N3 Co1 124.7(2) . . ? C15 N4 C14 109.5(2) . . ? C15 N4 C21 109.1(2) . . ? C14 N4 C21 112.9(2) . . ? C15 N4 Co1 106.93(17) . . ? C14 N4 Co1 105.76(16) . . ? C21 N4 Co1 112.41(15) . . ? C16 N5 C20 117.0(3) . . ? C16 N5 Co1 114.78(18) . . ? C20 N5 Co1 127.9(2) . . ? C28 O1 Co1 109.2(2) . . ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 28.17 _diffrn_measured_fraction_theta_full 0.909 _refine_diff_density_max 0.693 _refine_diff_density_min -1.228 _refine_diff_density_rms 0.069 #===END OF DATA FOR 5 # 4.6 REAULTS FOR 6 data_shin223so _database_code_depnum_ccdc_archive 'CCDC 772156' #TrackingRef '- alldata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H29 F6 Fe N6 O7 S2' _chemical_formula_weight 807.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.105(4) _cell_length_b 17.251(4) _cell_length_c 19.897(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6558(2) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3304 _exptl_absorpt_coefficient_mu 0.678 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'STOE IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26467 _diffrn_reflns_av_R_equivalents 0.1650 _diffrn_reflns_av_sigmaI/netI 0.1740 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 25.04 _reflns_number_total 5755 _reflns_number_gt 2726 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS Software (1997)' _computing_cell_refinement 'STOE IPDS Software (1997)' _computing_data_reduction 'STOE IPDS Software (1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0494P)^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 5755 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1384 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1367 _refine_ls_wR_factor_gt 0.1168 _refine_ls_goodness_of_fit_ref 0.871 _refine_ls_restrained_S_all 0.871 _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 C1 C 0.5056(3) 0.6192(3) 0.8140(3) 0.0230(15) Uani 1 1 d . . . H1A H 0.5017 0.5782 0.8486 0.028 Uiso 1 1 calc R . . H1B H 0.4697 0.6094 0.7792 0.028 Uiso 1 1 calc R . . C2 C 0.4936(3) 0.6977(3) 0.8456(3) 0.0201(13) Uani 1 1 d . . . C3 C 0.4287(3) 0.7277(3) 0.8577(3) 0.0264(15) Uani 1 1 d . . . H3 H 0.3879 0.7010 0.8430 0.032 Uiso 1 1 calc R . . C4 C 0.4230(4) 0.7980(3) 0.8918(4) 0.0325(17) Uani 1 1 d . . . H4 H 0.3784 0.8196 0.9018 0.039 Uiso 1 1 calc R . . C5 C 0.4837(4) 0.8356(3) 0.9108(3) 0.0271(16) Uani 1 1 d . . . H5 H 0.4815 0.8834 0.9344 0.032 Uiso 1 1 calc R . . C6 C 0.5466(4) 0.8032(3) 0.8952(3) 0.0280(16) Uani 1 1 d . . . H6 H 0.5879 0.8307 0.9070 0.034 Uiso 1 1 calc R . . C7 C 0.5739(4) 0.6571(3) 0.7169(3) 0.0231(15) Uani 1 1 d . . . H7A H 0.5286 0.6845 0.7118 0.028 Uiso 1 1 calc R . . H7B H 0.5770 0.6176 0.6809 0.028 Uiso 1 1 calc R . . C8 C 0.6325(4) 0.7142(3) 0.7085(3) 0.0242(15) Uani 1 1 d . . . C9 C 0.6504(4) 0.7451(3) 0.6477(4) 0.0353(17) Uani 1 1 d . . . H9 H 0.6261 0.7292 0.6084 0.042 Uiso 1 1 calc R . . C10 C 0.7029(4) 0.7987(3) 0.6429(4) 0.043(2) Uani 1 1 d . . . H10 H 0.7161 0.8194 0.6005 0.051 Uiso 1 1 calc R . . C11 C 0.7359(4) 0.8215(3) 0.7006(4) 0.0315(16) Uani 1 1 d . . . H11 H 0.7721 0.8592 0.6987 0.038 Uiso 1 1 calc R . . C12 C 0.7168(4) 0.7903(3) 0.7607(4) 0.0273(16) Uani 1 1 d . . . H12 H 0.7405 0.8064 0.8003 0.033 Uiso 1 1 calc R . . C13 C 0.6044(3) 0.5377(3) 0.7793(3) 0.0185(14) Uani 1 1 d . . . H13A H 0.5824 0.5093 0.7416 0.022 Uiso 1 1 calc R . . H13B H 0.5949 0.5090 0.8214 0.022 Uiso 1 1 calc R . . C14 C 0.6819(3) 0.5439(3) 0.7681(3) 0.0187(14) Uani 1 1 d . . . H14A H 0.7029 0.4914 0.7680 0.022 Uiso 1 1 calc R . . H14B H 0.6910 0.5680 0.7238 0.022 Uiso 1 1 calc R . . C15 C 0.7279(3) 0.5453(3) 0.8835(3) 0.0227(14) Uani 1 1 d . . . H15A H 0.7691 0.5667 0.9072 0.027 Uiso 1 1 calc R . . H15B H 0.7390 0.4914 0.8701 0.027 Uiso 1 1 calc R . . C16 C 0.6668(3) 0.5446(3) 0.9304(3) 0.0184(14) Uani 1 1 d . . . C17 C 0.6593(3) 0.4904(3) 0.9802(4) 0.0280(16) Uani 1 1 d . . . H17 H 0.6886 0.4459 0.9811 0.034 Uiso 1 1 calc R . . C18 C 0.6093(4) 0.5007(4) 1.0290(3) 0.0310(16) Uani 1 1 d . . . H18 H 0.6046 0.4642 1.0644 0.037 Uiso 1 1 calc R . . C19 C 0.5662(4) 0.5642(4) 1.0261(4) 0.0315(17) Uani 1 1 d . . . H19 H 0.5317 0.5727 1.0596 0.038 Uiso 1 1 calc R . . C20 C 0.5741(4) 0.6145(3) 0.9742(3) 0.0270(16) Uani 1 1 d . . . H20 H 0.5436 0.6579 0.9719 0.032 Uiso 1 1 calc R . . C21 C 0.7841(3) 0.6221(3) 0.7968(3) 0.0196(14) Uani 1 1 d . . . H21A H 0.8015 0.6616 0.8288 0.024 Uiso 1 1 calc R . . H21B H 0.7758 0.6485 0.7533 0.024 Uiso 1 1 calc R . . C22 C 0.8410(3) 0.5620(3) 0.7868(3) 0.0180(14) Uani 1 1 d . . . C23 C 0.8429(3) 0.5155(3) 0.7297(3) 0.0248(15) Uani 1 1 d . . . H23 H 0.8090 0.5220 0.6952 0.030 Uiso 1 1 calc R . . C24 C 0.8952(4) 0.4592(3) 0.7233(4) 0.0297(17) Uani 1 1 d . . . H24 H 0.8960 0.4267 0.6847 0.036 Uiso 1 1 calc R . . C25 C 0.9454(4) 0.4505(3) 0.7723(4) 0.0300(17) Uani 1 1 d . . . H25 H 0.9808 0.4121 0.7677 0.036 Uiso 1 1 calc R . . C26 C 0.9440(4) 0.4981(3) 0.8285(3) 0.0282(16) Uani 1 1 d . . . H26 H 0.9788 0.4929 0.8623 0.034 Uiso 1 1 calc R . . C27 C 0.8919(3) 0.5530(3) 0.8349(3) 0.0231(15) Uani 1 1 d . . . H27 H 0.8913 0.5854 0.8735 0.028 Uiso 1 1 calc R . . C28 C 0.8749(4) 0.0419(3) 0.5180(4) 0.0328(18) Uani 1 1 d . . . C29 C 0.9158(4) 0.7713(3) 0.9279(4) 0.0329(17) Uani 1 1 d . . . F1 F 0.9237(3) -0.0053(3) 0.4928(2) 0.0554(13) Uani 1 1 d . . . F2 F 0.8372(2) 0.0670(2) 0.4659(2) 0.0456(12) Uani 1 1 d . . . F3 F 0.9089(3) 0.1022(2) 0.5431(3) 0.0637(15) Uani 1 1 d . . . F4 F 0.9747(3) 0.7306(3) 0.9321(3) 0.0681(15) Uani 1 1 d . . . F5 F 0.8644(3) 0.7212(2) 0.9379(2) 0.0570(13) Uani 1 1 d . . . F6 F 0.9165(3) 0.8203(2) 0.9787(2) 0.0531(12) Uani 1 1 d . . . Fe1 Fe 0.64303(4) 0.67707(4) 0.84873(4) 0.0178(2) Uani 1 1 d . . . N1 N 0.5752(3) 0.6172(2) 0.7838(2) 0.0171(11) Uani 1 1 d . . . N2 N 0.5535(3) 0.7346(2) 0.8641(3) 0.0201(12) Uani 1 1 d . . . N3 N 0.6648(3) 0.7367(2) 0.7658(3) 0.0204(12) Uani 1 1 d . . . N4 N 0.7148(3) 0.5919(2) 0.8224(3) 0.0172(11) Uani 1 1 d . . . N5 N 0.6237(3) 0.6061(2) 0.9253(3) 0.0212(12) Uani 1 1 d . . . N6 N 0.6957(3) 0.7311(3) 0.9019(3) 0.0254(13) Uani 1 1 d . . . O1 O 0.7056(3) 0.7458(3) 0.9593(3) 0.0568(17) Uani 1 1 d . . . O2 O 0.7731(3) 0.0521(3) 0.5998(3) 0.0430(13) Uani 1 1 d . . . O3 O 0.8723(3) -0.0266(2) 0.6310(2) 0.0388(13) Uani 1 1 d . . . O4 O 0.7938(3) -0.0708(2) 0.5442(3) 0.0390(13) Uani 1 1 d . . . O5 O 0.8431(3) 0.8591(2) 0.8513(3) 0.0489(15) Uani 1 1 d . . . O6 O 0.9679(3) 0.8690(3) 0.8471(3) 0.0673(19) Uani 1 1 d . . . O7 O 0.9097(3) 0.7560(3) 0.8007(3) 0.0512(15) Uani 1 1 d . . . S1 S 0.82208(9) -0.00656(8) 0.58038(9) 0.0258(4) Uani 1 1 d . . . S2 S 0.90868(9) 0.81921(9) 0.84696(10) 0.0317(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 C1 0.018(4) 0.025(3) 0.027(4) 0.001(3) -0.001(3) -0.003(2) C2 0.025(4) 0.022(3) 0.013(3) -0.001(2) 0.002(3) 0.003(2) C3 0.018(4) 0.029(3) 0.032(4) -0.004(3) 0.002(3) 0.001(2) C4 0.032(5) 0.032(3) 0.034(4) 0.003(3) 0.004(4) 0.012(3) C5 0.039(5) 0.016(3) 0.026(4) -0.004(2) 0.004(3) 0.011(3) C6 0.035(5) 0.019(3) 0.030(4) -0.007(2) 0.005(3) -0.001(3) C7 0.021(4) 0.031(3) 0.018(4) -0.003(2) -0.004(3) -0.002(3) C8 0.022(4) 0.021(3) 0.029(4) -0.006(3) -0.002(3) 0.008(3) C9 0.045(5) 0.031(3) 0.030(4) -0.001(3) -0.007(4) -0.003(3) C10 0.050(6) 0.032(3) 0.046(5) 0.006(3) 0.008(4) -0.006(3) C11 0.029(4) 0.019(3) 0.046(5) 0.007(3) 0.004(3) -0.001(3) C12 0.023(4) 0.015(2) 0.044(5) -0.003(3) -0.007(3) 0.000(2) C13 0.020(4) 0.016(2) 0.019(3) -0.007(2) 0.002(3) -0.002(2) C14 0.019(4) 0.019(3) 0.018(3) -0.009(2) 0.000(3) 0.005(2) C15 0.013(4) 0.027(3) 0.029(4) -0.002(3) 0.003(3) 0.005(2) C16 0.016(4) 0.024(3) 0.016(3) -0.006(2) -0.001(3) -0.001(2) C17 0.022(4) 0.029(3) 0.033(4) -0.001(3) -0.006(3) -0.003(3) C18 0.036(5) 0.038(3) 0.020(4) 0.007(3) 0.005(3) -0.006(3) C19 0.026(5) 0.043(4) 0.026(4) -0.002(3) 0.004(3) 0.003(3) C20 0.027(4) 0.032(3) 0.022(4) -0.003(3) 0.005(3) 0.004(3) C21 0.010(4) 0.021(3) 0.028(4) -0.001(2) 0.001(3) -0.005(2) C22 0.011(4) 0.016(3) 0.027(4) 0.005(2) 0.002(3) -0.002(2) C23 0.018(4) 0.027(3) 0.029(4) -0.006(3) 0.003(3) -0.005(3) C24 0.021(4) 0.030(3) 0.039(4) -0.014(3) 0.010(3) -0.006(3) C25 0.025(5) 0.022(3) 0.043(5) 0.006(3) 0.005(4) 0.005(3) C26 0.020(4) 0.033(3) 0.031(4) 0.011(3) 0.004(3) 0.006(3) C27 0.016(4) 0.032(3) 0.021(4) -0.003(3) 0.005(3) 0.000(3) C28 0.038(5) 0.031(3) 0.030(4) -0.005(3) 0.000(4) -0.001(3) C29 0.032(5) 0.026(3) 0.040(5) 0.006(3) -0.005(4) -0.004(3) F1 0.041(3) 0.079(3) 0.046(3) -0.006(2) 0.013(3) 0.012(2) F2 0.052(3) 0.048(2) 0.036(3) 0.0139(19) 0.000(2) -0.005(2) F3 0.073(4) 0.064(3) 0.054(3) -0.006(2) -0.003(3) -0.042(3) F4 0.059(4) 0.084(3) 0.061(4) 0.021(3) 0.000(3) 0.032(3) F5 0.068(4) 0.056(2) 0.047(3) 0.004(2) 0.005(3) -0.031(2) F6 0.078(4) 0.047(2) 0.035(3) -0.011(2) -0.012(2) -0.007(2) Fe1 0.0144(5) 0.0191(3) 0.0199(4) -0.0032(4) -0.0011(4) 0.0007(4) N1 0.012(3) 0.020(2) 0.019(3) -0.0052(19) 0.000(2) 0.0005(19) N2 0.018(3) 0.020(2) 0.023(3) 0.003(2) -0.001(2) 0.000(2) N3 0.019(3) 0.018(2) 0.024(3) -0.002(2) 0.000(2) 0.002(2) N4 0.016(3) 0.017(2) 0.019(3) -0.0002(19) 0.002(2) 0.0031(19) N5 0.019(3) 0.021(2) 0.024(3) -0.002(2) 0.003(2) -0.001(2) N6 0.025(3) 0.030(3) 0.021(3) -0.007(2) -0.003(3) 0.000(2) O1 0.057(5) 0.070(3) 0.043(4) -0.023(3) -0.009(3) -0.006(3) O2 0.040(4) 0.052(3) 0.037(3) 0.002(2) 0.012(3) 0.016(2) O3 0.043(4) 0.049(3) 0.024(3) -0.0004(19) -0.012(2) 0.013(2) O4 0.040(4) 0.035(2) 0.042(4) 0.005(2) -0.005(3) -0.011(2) O5 0.046(4) 0.045(2) 0.056(4) -0.006(3) -0.018(3) 0.011(2) O6 0.060(4) 0.086(4) 0.056(4) 0.034(3) -0.019(4) -0.048(3) O7 0.061(4) 0.060(3) 0.032(3) -0.003(3) 0.001(3) 0.004(3) S1 0.0284(10) 0.0273(7) 0.0217(9) 0.0019(6) 0.0016(8) 0.0016(7) S2 0.0305(10) 0.0347(7) 0.0299(10) 0.0040(8) -0.0066(9) -0.0084(8) _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 C1 N1 1.459(8) . ? C1 C2 1.511(7) . ? C2 N2 1.360(8) . ? C2 C3 1.364(8) . ? C3 C4 1.395(8) . ? C4 C5 1.381(10) . ? C5 C6 1.361(9) . ? C6 N2 1.342(7) . ? C7 N1 1.498(7) . ? C7 C8 1.501(9) . ? C8 N3 1.353(8) . ? C8 C9 1.365(9) . ? C9 C10 1.367(10) . ? C10 C11 1.368(10) . ? C11 C12 1.362(9) . ? C12 N3 1.361(8) . ? C13 N1 1.483(7) . ? C13 C14 1.500(8) . ? C14 N4 1.499(7) . ? C15 N4 1.478(8) . ? C15 C16 1.495(9) . ? C16 N5 1.347(7) . ? C16 C17 1.370(8) . ? C17 C18 1.373(9) . ? C18 C19 1.371(9) . ? C19 C20 1.357(9) . ? C20 N5 1.367(8) . ? C21 N4 1.511(8) . ? C21 C22 1.516(8) . ? C22 C27 1.374(9) . ? C22 C23 1.391(8) . ? C23 C24 1.399(9) . ? C24 C25 1.376(10) . ? C25 C26 1.387(9) . ? C26 C27 1.380(8) . ? C28 F3 1.323(8) . ? C28 F2 1.335(8) . ? C28 F1 1.336(8) . ? C28 S1 1.804(8) . ? C29 F6 1.316(8) . ? C29 F5 1.323(8) . ? C29 F4 1.330(8) . ? C29 S2 1.816(7) . ? Fe1 N6 1.733(5) . ? Fe1 N5 1.988(5) . ? Fe1 N3 1.988(5) . ? Fe1 N2 2.002(5) . ? Fe1 N4 2.077(5) . ? Fe1 N1 2.102(5) . ? N6 O1 1.184(7) . ? O2 S1 1.431(5) . ? O3 S1 1.433(5) . ? O4 S1 1.428(5) . ? O5 S2 1.432(5) . ? O6 S2 1.420(5) . ? O7 S2 1.427(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 109.4(5) . . ? N2 C2 C3 122.7(5) . . ? N2 C2 C1 113.8(5) . . ? C3 C2 C1 123.4(5) . . ? C2 C3 C4 119.1(6) . . ? C5 C4 C3 118.4(6) . . ? C6 C5 C4 119.2(5) . . ? N2 C6 C5 123.5(6) . . ? N1 C7 C8 112.8(5) . . ? N3 C8 C9 121.3(6) . . ? N3 C8 C7 115.8(6) . . ? C9 C8 C7 122.8(6) . . ? C8 C9 C10 120.7(7) . . ? C9 C10 C11 118.3(7) . . ? C12 C11 C10 120.0(6) . . ? N3 C12 C11 122.0(6) . . ? N1 C13 C14 108.3(4) . . ? N4 C14 C13 110.2(5) . . ? N4 C15 C16 112.7(5) . . ? N5 C16 C17 121.9(6) . . ? N5 C16 C15 115.0(5) . . ? C17 C16 C15 122.6(5) . . ? C16 C17 C18 119.7(6) . . ? C19 C18 C17 119.5(6) . . ? C20 C19 C18 118.4(7) . . ? C19 C20 N5 123.5(6) . . ? N4 C21 C22 115.8(4) . . ? C27 C22 C23 119.1(5) . . ? C27 C22 C21 119.6(5) . . ? C23 C22 C21 121.3(6) . . ? C22 C23 C24 119.6(6) . . ? C25 C24 C23 120.6(6) . . ? C24 C25 C26 119.5(6) . . ? C27 C26 C25 119.7(7) . . ? C22 C27 C26 121.6(6) . . ? F3 C28 F2 107.6(5) . . ? F3 C28 F1 106.1(6) . . ? F2 C28 F1 106.4(6) . . ? F3 C28 S1 112.3(5) . . ? F2 C28 S1 112.5(5) . . ? F1 C28 S1 111.5(5) . . ? F6 C29 F5 108.1(6) . . ? F6 C29 F4 106.4(6) . . ? F5 C29 F4 105.9(5) . . ? F6 C29 S2 112.9(4) . . ? F5 C29 S2 112.0(5) . . ? F4 C29 S2 111.1(5) . . ? N6 Fe1 N5 88.4(2) . . ? N6 Fe1 N3 96.2(2) . . ? N5 Fe1 N3 173.15(19) . . ? N6 Fe1 N2 97.8(2) . . ? N5 Fe1 N2 91.7(2) . . ? N3 Fe1 N2 92.8(2) . . ? N6 Fe1 N4 98.7(2) . . ? N5 Fe1 N4 83.12(19) . . ? N3 Fe1 N4 91.08(19) . . ? N2 Fe1 N4 162.49(19) . . ? N6 Fe1 N1 176.6(2) . . ? N5 Fe1 N1 93.1(2) . . ? N3 Fe1 N1 82.7(2) . . ? N2 Fe1 N1 79.1(2) . . ? N4 Fe1 N1 84.48(19) . . ? C1 N1 C13 113.0(4) . . ? C1 N1 C7 109.8(5) . . ? C13 N1 C7 112.2(5) . . ? C1 N1 Fe1 107.3(4) . . ? C13 N1 Fe1 105.0(4) . . ? C7 N1 Fe1 109.3(3) . . ? C6 N2 C2 117.1(5) . . ? C6 N2 Fe1 126.3(4) . . ? C2 N2 Fe1 116.5(4) . . ? C8 N3 C12 117.7(6) . . ? C8 N3 Fe1 117.1(4) . . ? C12 N3 Fe1 124.5(5) . . ? C15 N4 C14 111.3(4) . . ? C15 N4 C21 108.4(5) . . ? C14 N4 C21 108.4(5) . . ? C15 N4 Fe1 106.8(4) . . ? C14 N4 Fe1 107.2(3) . . ? C21 N4 Fe1 114.7(3) . . ? C16 N5 C20 116.9(5) . . ? C16 N5 Fe1 115.4(4) . . ? C20 N5 Fe1 127.6(4) . . ? O1 N6 Fe1 142.8(5) . . ? O4 S1 O2 115.9(3) . . ? O4 S1 O3 114.9(3) . . ? O2 S1 O3 114.7(3) . . ? O4 S1 C28 103.0(3) . . ? O2 S1 C28 102.9(3) . . ? O3 S1 C28 102.8(3) . . ? O6 S2 O7 116.9(4) . . ? O6 S2 O5 113.9(4) . . ? O7 S2 O5 114.7(3) . . ? O6 S2 C29 102.3(3) . . ? O7 S2 C29 102.9(3) . . ? O5 S2 C29 103.4(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.754 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.102 #===END OF ALL DATA