# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_003rtrt12 _audit_creation_date 12-08-07 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title '003rtrt12 in P 1 21/c 1' _chemical_name_systematic . _chemical_melting_point . _cell_length_a 9.42890(10) _cell_length_b 10.16140(10) _cell_length_c 12.1495(2) _cell_angle_alpha 90 _cell_angle_beta 105.3181(6) _cell_angle_gamma 90 _cell_volume 1122.70(2) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C14 H11 Br1 Fe1 # Dc = 1.86 Fooo = 624.00 Mu = 48.66 M = 314.99 # Found Formula = C14 H11 Br1 Fe1 # Dc = 1.86 FOOO = 624.00 Mu = 48.66 M = 314.99 _chemical_formula_sum 'C14 H11 Br1 Fe1' _chemical_formula_moiety 'C14 H11 Br1 Fe1' _chemical_compound_source . _chemical_formula_weight 314.99 _cell_measurement_reflns_used 2686 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_min 0.090 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_max 0.210 _exptl_crystal_density_diffrn 1.863 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 4.866 # Sheldrick geometric approximatio 0.61 0.65 # No experimental values of Tmin/max available _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.61 _exptl_absorpt_correction_T_max 0.65 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 33225 _reflns_number_total 2553 _diffrn_reflns_av_R_equivalents 0.022 # Number of reflections without Friedels Law is 4943 # Number of reflections with Friedels Law is 2553 # Theoretical number of reflections is about 2574 _diffrn_reflns_theta_min 5.120 _diffrn_reflns_theta_max 27.481 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.481 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -12 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_diffrn_Wilson_B_factor 1.85 _oxford_diffrn_Wilson_scale 13.43 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.97 _refine_diff_density_max 0.96 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>0.0\s(I) _refine_ls_number_reflns 2553 _refine_ls_number_restraints 0 _refine_ls_number_parameters 145 _oxford_refine_ls_R_factor_ref 0.0425 _refine_ls_wR_factor_ref 0.0756 _refine_ls_goodness_of_fit_ref 0.9918 _refine_ls_shift/su_max 0.0062606 _refine_ls_shift/su_mean 0.0020564 # The values computed with all filters except I/sigma _oxford_reflns_number_all 2553 _refine_ls_R_factor_all 0.0425 _refine_ls_wR_factor_all 0.0756 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2166 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_gt 0.0715 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 2.81P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Br1 Br 1.11635(3) 0.82041(3) 0.51482(3) 0.0269 1.0000 Uani . . . . . . C2 C 1.0009(3) 0.6903(3) 0.4190(2) 0.0204 1.0000 Uani . . . . . . C3 C 1.0305(3) 0.6580(3) 0.3189(3) 0.0243 1.0000 Uani . . . . . . C4 C 0.9425(3) 0.5606(3) 0.2457(3) 0.0259 1.0000 Uani . . . . . . C5 C 0.8290(3) 0.4999(3) 0.2738(3) 0.0250 1.0000 Uani . . . . . . C6 C 0.7973(3) 0.5315(3) 0.3796(2) 0.0209 1.0000 Uani . . . . . . C7 C 0.8855(3) 0.6291(3) 0.4549(2) 0.0190 1.0000 Uani . . . . . . Fe8 Fe 0.66681(4) 0.68708(4) 0.40709(3) 0.0185 1.0000 Uani . . . . . . C9 C 0.8273(3) 0.6430(3) 0.5521(2) 0.0214 1.0000 Uani . . . . . . C10 C 0.7075(3) 0.5527(3) 0.5377(2) 0.0225 1.0000 Uani . . . . . . C11 C 0.6862(3) 0.4877(3) 0.4314(2) 0.0224 1.0000 Uani . . . . . . C12 C 0.6598(4) 0.8652(3) 0.3279(3) 0.0318 1.0000 Uani . . . . . . C13 C 0.5773(4) 0.7689(3) 0.2515(3) 0.0323 1.0000 Uani . . . . . . C14 C 0.4646(3) 0.7217(3) 0.2989(3) 0.0334 1.0000 Uani . . . . . . C15 C 0.4776(4) 0.7871(4) 0.4043(3) 0.0359 1.0000 Uani . . . . . . C16 C 0.5979(4) 0.8758(3) 0.4226(3) 0.0345 1.0000 Uani . . . . . . H31 H 1.1083 0.6988 0.2974 0.0300 1.0000 Uiso R . . . . . H41 H 0.9627 0.5388 0.1763 0.0312 1.0000 Uiso R . . . . . H51 H 0.7721 0.4386 0.2241 0.0314 1.0000 Uiso R . . . . . H91 H 0.8647 0.7017 0.6164 0.0260 1.0000 Uiso R . . . . . H101 H 0.6482 0.5392 0.5913 0.0279 1.0000 Uiso R . . . . . H111 H 0.6100 0.4232 0.3997 0.0270 1.0000 Uiso R . . . . . H121 H 0.7448 0.9139 0.3183 0.0383 1.0000 Uiso R . . . . . H131 H 0.5974 0.7385 0.1811 0.0395 1.0000 Uiso R . . . . . H141 H 0.3927 0.6545 0.2653 0.0403 1.0000 Uiso R . . . . . H151 H 0.4150 0.7724 0.4564 0.0432 1.0000 Uiso R . . . . . H161 H 0.6345 0.9318 0.4894 0.0431 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.02373(16) 0.02515(17) 0.03227(18) -0.00433(12) 0.00797(13) -0.00530(11) C2 0.0153(13) 0.0182(13) 0.0251(14) 0.0035(11) 0.0009(11) 0.0019(10) C3 0.0215(14) 0.0259(15) 0.0272(15) 0.0013(12) 0.0096(12) 0.0027(12) C4 0.0276(15) 0.0287(16) 0.0233(14) 0.0004(12) 0.0098(12) 0.0047(12) C5 0.0267(15) 0.0207(14) 0.0253(15) -0.0027(12) 0.0028(12) 0.0023(12) C6 0.0196(13) 0.0183(13) 0.0233(14) 0.0022(11) 0.0030(11) 0.0026(11) C7 0.0179(13) 0.0158(13) 0.0215(13) 0.0016(10) 0.0024(11) 0.0029(10) Fe8 0.0158(2) 0.0181(2) 0.0209(2) 0.00276(15) 0.00394(16) 0.00250(15) C9 0.0220(14) 0.0229(14) 0.0187(13) 0.0004(11) 0.0047(11) 0.0020(11) C10 0.0211(14) 0.0230(14) 0.0237(14) 0.0052(12) 0.0063(12) 0.0004(11) C11 0.0195(13) 0.0179(13) 0.0274(15) 0.0023(11) 0.0022(12) -0.0005(11) C12 0.0317(17) 0.0236(15) 0.0406(18) 0.0126(14) 0.0102(15) 0.0055(13) C13 0.0331(17) 0.0342(17) 0.0268(16) 0.0093(14) 0.0028(13) 0.0114(14) C14 0.0201(15) 0.0328(17) 0.0412(19) 0.0102(14) -0.0029(14) 0.0050(13) C15 0.0263(16) 0.0415(19) 0.043(2) 0.0143(15) 0.0140(15) 0.0162(14) C16 0.0376(18) 0.0258(16) 0.0389(18) 0.0008(14) 0.0079(15) 0.0118(14) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2728(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Br1 . C2 . 1.902(3) yes C2 . C3 . 1.358(4) yes C2 . C7 . 1.418(4) yes C3 . C4 . 1.438(4) yes C3 . H31 . 0.938 no C4 . C5 . 1.355(4) yes C4 . H41 . 0.938 no C5 . C6 . 1.431(4) yes C5 . H51 . 0.932 no C6 . C7 . 1.453(4) yes C6 . Fe8 . 2.084(3) yes C6 . C11 . 1.429(4) yes C7 . Fe8 . 2.075(3) yes C7 . C9 . 1.435(4) yes Fe8 . C9 . 2.046(3) yes Fe8 . C10 . 2.051(3) yes Fe8 . C11 . 2.048(3) yes Fe8 . C12 . 2.043(3) yes Fe8 . C13 . 2.033(3) yes Fe8 . C14 . 2.041(3) yes Fe8 . C15 . 2.045(3) yes Fe8 . C16 . 2.049(3) yes C9 . C10 . 1.429(4) yes C9 . H91 . 0.972 no C10 . C11 . 1.416(4) yes C10 . H101 . 0.975 no C11 . H111 . 0.974 no C12 . C13 . 1.429(5) yes C12 . C16 . 1.425(5) yes C12 . H121 . 0.975 no C13 . C14 . 1.419(5) yes C13 . H131 . 0.974 no C14 . C15 . 1.419(5) yes C14 . H141 . 0.973 no C15 . C16 . 1.419(5) yes C15 . H151 . 0.984 no C16 . H161 . 0.977 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Br1 . C2 . C3 . 119.7(2) yes Br1 . C2 . C7 . 118.5(2) yes C3 . C2 . C7 . 121.7(3) yes C2 . C3 . C4 . 119.9(3) yes C2 . C3 . H31 . 120.2 no C4 . C3 . H31 . 119.9 no C3 . C4 . C5 . 121.5(3) yes C3 . C4 . H41 . 119.8 no C5 . C4 . H41 . 118.7 no C4 . C5 . C6 . 119.4(3) yes C4 . C5 . H51 . 119.9 no C6 . C5 . H51 . 120.7 no C5 . C6 . C7 . 119.9(3) yes C5 . C6 . Fe8 . 125.9(2) yes C7 . C6 . Fe8 . 69.21(15) yes C5 . C6 . C11 . 132.7(3) yes C7 . C6 . C11 . 107.4(2) yes Fe8 . C6 . C11 . 68.44(16) yes C6 . C7 . C2 . 117.6(2) yes C6 . C7 . Fe8 . 69.88(15) yes C2 . C7 . Fe8 . 125.2(2) yes C6 . C7 . C9 . 107.8(2) yes C2 . C7 . C9 . 134.6(3) yes Fe8 . C7 . C9 . 68.56(15) yes C6 . Fe8 . C7 . 40.91(11) yes C6 . Fe8 . C9 . 68.80(11) yes C7 . Fe8 . C9 . 40.74(11) yes C6 . Fe8 . C10 . 67.74(11) yes C7 . Fe8 . C10 . 67.99(11) yes C9 . Fe8 . C10 . 40.83(11) yes C6 . Fe8 . C11 . 40.45(11) yes C7 . Fe8 . C11 . 68.58(11) yes C9 . Fe8 . C11 . 69.00(12) yes C10 . Fe8 . C11 . 40.42(12) yes C6 . Fe8 . C12 . 122.94(12) yes C7 . Fe8 . C12 . 106.83(12) yes C9 . Fe8 . C12 . 121.61(13) yes C10 . Fe8 . C12 . 158.47(13) yes C11 . Fe8 . C12 . 159.22(13) yes C6 . Fe8 . C13 . 106.18(12) yes C7 . Fe8 . C13 . 120.95(12) yes C9 . Fe8 . C13 . 157.09(13) yes C10 . Fe8 . C13 . 159.77(13) yes C11 . Fe8 . C13 . 122.54(13) yes C6 . Fe8 . C14 . 121.23(13) yes C7 . Fe8 . C14 . 156.93(13) yes C9 . Fe8 . C14 . 160.94(13) yes C10 . Fe8 . C14 . 124.43(13) yes C11 . Fe8 . C14 . 107.23(13) yes C6 . Fe8 . C15 . 157.46(14) yes C7 . Fe8 . C15 . 160.67(14) yes C9 . Fe8 . C15 . 124.50(13) yes C10 . Fe8 . C15 . 109.15(13) yes C11 . Fe8 . C15 . 122.54(13) yes C6 . Fe8 . C16 . 160.00(13) yes C7 . Fe8 . C16 . 123.76(13) yes C9 . Fe8 . C16 . 107.82(13) yes C10 . Fe8 . C16 . 123.43(13) yes C11 . Fe8 . C16 . 158.50(13) yes C12 . Fe8 . C13 . 41.06(14) yes C12 . Fe8 . C14 . 68.60(14) yes C13 . Fe8 . C14 . 40.78(13) yes C12 . Fe8 . C15 . 68.42(14) yes C13 . Fe8 . C15 . 68.62(14) yes C14 . Fe8 . C15 . 40.63(14) yes C12 . Fe8 . C16 . 40.75(14) yes C13 . Fe8 . C16 . 68.84(14) yes C14 . Fe8 . C16 . 68.45(14) yes C15 . Fe8 . C16 . 40.55(14) yes C7 . C9 . Fe8 . 70.69(15) yes C7 . C9 . C10 . 107.3(2) yes Fe8 . C9 . C10 . 69.75(16) yes C7 . C9 . H91 . 125.8 no Fe8 . C9 . H91 . 125.9 no C10 . C9 . H91 . 126.9 no C9 . C10 . Fe8 . 69.42(16) yes C9 . C10 . C11 . 109.2(2) yes Fe8 . C10 . C11 . 69.70(16) yes C9 . C10 . H101 . 125.7 no Fe8 . C10 . H101 . 126.0 no C11 . C10 . H101 . 125.1 no C6 . C11 . C10 . 108.2(2) yes C6 . C11 . Fe8 . 71.11(16) yes C10 . C11 . Fe8 . 69.88(16) yes C6 . C11 . H111 . 125.8 no C10 . C11 . H111 . 126.0 no Fe8 . C11 . H111 . 125.5 no Fe8 . C12 . C13 . 69.11(18) yes Fe8 . C12 . C16 . 69.89(18) yes C13 . C12 . C16 . 107.9(3) yes Fe8 . C12 . H121 . 125.5 no C13 . C12 . H121 . 126.4 no C16 . C12 . H121 . 125.7 no C12 . C13 . Fe8 . 69.82(18) yes C12 . C13 . C14 . 107.8(3) yes Fe8 . C13 . C14 . 69.90(18) yes C12 . C13 . H131 . 126.1 no Fe8 . C13 . H131 . 123.9 no C14 . C13 . H131 . 126.1 no C13 . C14 . Fe8 . 69.32(18) yes C13 . C14 . C15 . 108.2(3) yes Fe8 . C14 . C15 . 69.85(18) yes C13 . C14 . H141 . 125.5 no Fe8 . C14 . H141 . 125.3 no C15 . C14 . H141 . 126.3 no C14 . C15 . Fe8 . 69.51(18) yes C14 . C15 . C16 . 108.3(3) yes Fe8 . C15 . C16 . 69.88(18) yes C14 . C15 . H151 . 125.8 no Fe8 . C15 . H151 . 125.6 no C16 . C15 . H151 . 125.9 no C12 . C16 . C15 . 107.8(3) yes C12 . C16 . Fe8 . 69.36(18) yes C15 . C16 . Fe8 . 69.57(19) yes C12 . C16 . H161 . 125.8 no C15 . C16 . H161 . 126.4 no Fe8 . C16 . H161 . 124.8 no _iucr_refine_instruction_details_constraints ; # # Punched on 07/08/12 at 19:09:16 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 15,X'S) H ( 151,X'S) RIDE C ( 16,X'S) H ( 161,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 07/08/12 at 19:09:16 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _database_code_depnum_ccdc_archive 'CCDC 940844' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_006rtrt12 _audit_creation_date 13-03-28 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title '006rt12 in P2(1)/c' _chemical_name_systematic . _chemical_melting_point . _cell_length_a 12.18666(5) _cell_length_b 14.62360(6) _cell_length_c 14.43211(6) _cell_angle_alpha 90 _cell_angle_beta 91.0308(4) _cell_angle_gamma 90 _cell_volume 2571.570(18) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0090 0.0039 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe -1.1336 3.1974 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C33 H35 B1 Fe1 # Dc = 1.29 Fooo = 1024.00 Mu = 48.27 M = 498.30 # Found Formula = C32 H33 B1 Fe1 # Dc = 1.25 FOOO = 1024.00 Mu = 48.13 M = 484.27 _chemical_formula_sum 'C32 H33 B1 Fe1' _chemical_formula_moiety 'C32 H33 B1 Fe1' _chemical_compound_source . _chemical_formula_weight 484.27 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_min 0.160 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_max 0.220 _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1024.000 _exptl_absorpt_coefficient_mu 4.813 # Sheldrick geometric approximatio 0.42 0.46 _exptl_absorpt_correction_type none _diffrn_measurement_device_type Unknown _diffrn_measurement_device Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 60968 _reflns_number_total 5397 _diffrn_reflns_av_R_equivalents 0.026 # Number of reflections without Friedels Law is 60968 # Number of reflections with Friedels Law is 5397 # Theoretical number of reflections is about 5434 _diffrn_reflns_theta_min 3.628 _diffrn_reflns_theta_max 76.945 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 75.406 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 3.49 _oxford_diffrn_Wilson_scale 0.05 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.01 _refine_diff_density_max 0.82 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>0.0\s(I) _refine_ls_number_reflns 5376 _refine_ls_number_restraints 1248 _refine_ls_number_parameters 599 _oxford_refine_ls_R_factor_ref 0.0475 _refine_ls_wR_factor_ref 0.0897 _refine_ls_goodness_of_fit_ref 0.9278 _refine_ls_shift/su_max 0.0124903 _refine_ls_shift/su_mean 0.0008005 # The values computed with all filters except I/sigma _oxford_reflns_number_all 5376 _refine_ls_R_factor_all 0.0475 _refine_ls_wR_factor_all 0.0897 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5157 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_gt 0.0892 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.150E+04 0.245E+04 0.150E+04 625. 163. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens B1 B 0.67646(16) 0.47659(13) 0.28457(13) 0.0317 1.0000 Uani . . . . . . C1 C 0.5524(5) 0.4998(9) 0.2514(6) 0.0345 0.477(10) Uani D . P 1 1 . Fe1 Fe 0.81027(3) 0.71804(2) 0.15570(2) 0.0464 1.0000 Uani . . . . . . C2 C 0.5071(4) 0.4712(5) 0.1660(4) 0.0394 0.477(10) Uani D . P 1 1 . C3 C 0.5720(5) 0.4147(7) 0.0982(5) 0.0539 0.477(10) Uani D . P 1 1 . C4 C 0.3981(4) 0.4917(4) 0.1431(5) 0.0468 0.477(10) Uani D . P 1 1 . C5 C 0.3337(3) 0.5424(4) 0.2021(5) 0.0474 0.477(10) Uani D . P 1 1 . C6 C 0.2157(3) 0.5653(5) 0.1752(7) 0.0676 0.477(10) Uani D . P 1 1 . C7 C 0.3778(4) 0.5720(4) 0.2851(5) 0.0436 0.477(10) Uani D . P 1 1 . C8 C 0.4859(4) 0.5515(5) 0.3110(4) 0.0378 0.477(10) Uani D . P 1 1 . C9 C 0.5296(6) 0.5895(5) 0.4010(5) 0.0483 0.477(10) Uani D . P 1 1 . C11 C 0.5524(4) 0.5032(8) 0.2741(5) 0.0327 0.523(10) Uani D . P 1 2 . C12 C 0.4914(4) 0.4798(5) 0.1936(4) 0.0404 0.523(10) Uani D . P 1 2 . C13 C 0.5409(5) 0.4253(6) 0.1160(5) 0.0516 0.523(10) Uani D . P 1 2 . C14 C 0.3819(3) 0.5075(3) 0.1836(4) 0.0425 0.523(10) Uani D . P 1 2 . C15 C 0.3318(3) 0.5584(3) 0.2511(5) 0.0433 0.523(10) Uani D . P 1 2 . C16 C 0.2131(3) 0.5895(4) 0.2381(6) 0.0628 0.523(10) Uani D . P 1 2 . C17 C 0.3909(3) 0.5815(3) 0.3307(4) 0.0396 0.523(10) Uani D . P 1 2 . C18 C 0.5003(3) 0.5550(4) 0.3429(4) 0.0320 0.523(10) Uani D . P 1 2 . C19 C 0.5612(4) 0.5877(4) 0.4287(4) 0.0395 0.523(10) Uani D . P 1 2 . C21 C 0.7072(10) 0.4218(6) 0.3698(7) 0.0330 0.476(14) Uani D . P 1 3 . C22 C 0.7843(6) 0.4556(5) 0.4360(4) 0.0356 0.476(14) Uani D . P 1 3 . C23 C 0.8238(7) 0.5537(5) 0.4339(5) 0.0447 0.476(14) Uani D . P 1 3 . C24 C 0.8211(6) 0.4013(6) 0.5091(4) 0.0433 0.476(14) Uani D . P 1 3 . C25 C 0.7868(6) 0.3116(5) 0.5185(5) 0.0518 0.476(14) Uani D . P 1 3 . C26 C 0.8312(7) 0.2517(7) 0.5971(6) 0.0716 0.476(14) Uani D . P 1 3 . C27 C 0.7073(9) 0.2792(5) 0.4576(7) 0.0477 0.476(14) Uani D . P 1 3 . C28 C 0.6649(8) 0.3333(5) 0.3862(6) 0.0376 0.476(14) Uani D . P 1 3 . C29 C 0.5668(7) 0.2963(6) 0.3316(6) 0.0450 0.476(14) Uani D . P 1 3 . C31 C 0.7142(9) 0.4102(5) 0.3708(6) 0.0292 0.524(14) Uani D . P 1 4 . C32 C 0.8015(5) 0.4320(4) 0.4327(4) 0.0331 0.524(14) Uani D . P 1 4 . C33 C 0.8553(5) 0.5255(5) 0.4328(4) 0.0403 0.524(14) Uani D . P 1 4 . C34 C 0.8392(4) 0.3689(5) 0.4981(4) 0.0369 0.524(14) Uani D . P 1 4 . C35 C 0.7945(4) 0.2827(4) 0.5041(4) 0.0425 0.524(14) Uani D . P 1 4 . C36 C 0.8398(5) 0.2134(5) 0.5732(5) 0.0570 0.524(14) Uani D . P 1 4 . C37 C 0.7086(8) 0.2605(4) 0.4449(6) 0.0423 0.524(14) Uani D . P 1 4 . C38 C 0.6689(7) 0.3219(5) 0.3786(5) 0.0352 0.524(14) Uani D . P 1 4 . C39 C 0.5848(7) 0.2865(5) 0.3093(6) 0.0444 0.524(14) Uani D . P 1 4 . C41 C 0.8053(4) 0.8561(4) 0.1913(4) 0.0533 0.709(16) Uani D . P 2 1 . C42 C 0.7911(5) 0.8005(5) 0.2701(3) 0.0582 0.709(16) Uani D . P 2 1 . C43 C 0.8859(6) 0.7452(3) 0.2813(3) 0.0504 0.709(16) Uani D . P 2 1 . C44 C 0.9592(4) 0.7672(3) 0.2081(4) 0.0432 0.709(16) Uani D . P 2 1 . C45 C 0.9082(4) 0.8348(4) 0.1522(3) 0.0455 0.709(16) Uani D . P 2 1 . C46 C 0.8084(11) 0.8466(10) 0.1695(8) 0.0576 0.291(16) Uani D . P 2 2 . C47 C 0.7641(10) 0.8100(9) 0.2512(9) 0.0549 0.291(16) Uani D . P 2 2 . C48 C 0.8411(14) 0.7478(7) 0.2893(6) 0.0458 0.291(16) Uani D . P 2 2 . C49 C 0.9361(10) 0.7497(10) 0.2323(10) 0.0504 0.291(16) Uani D . P 2 2 . C50 C 0.9174(11) 0.8152(12) 0.1622(9) 0.0534 0.291(16) Uani D . P 2 2 . C51 C 0.7673(5) 0.5019(5) 0.2116(4) 0.0243 0.482(13) Uani D . P 2 3 . C52 C 0.8723(5) 0.4629(4) 0.2302(4) 0.0267 0.482(13) Uani D . P 2 3 . C53 C 0.9627(5) 0.4771(5) 0.1691(5) 0.0325 0.482(13) Uani D . P 2 3 . C54 C 0.9561(5) 0.5428(5) 0.1006(4) 0.0317 0.482(13) Uani D . P 2 3 . C55 C 0.8577(5) 0.5906(5) 0.0857(4) 0.0352 0.482(13) Uani D . P 2 3 . C56 C 0.8296(6) 0.6593(5) 0.0188(4) 0.0459 0.482(13) Uani D . P 2 3 . C57 C 0.7195(6) 0.6869(5) 0.0373(4) 0.0465 0.482(13) Uani D . P 2 3 . C58 C 0.6819(5) 0.6371(5) 0.1154(5) 0.0428 0.482(13) Uani D . P 2 3 . C59 C 0.7658(5) 0.5742(6) 0.1440(5) 0.0342 0.482(13) Uani D . P 2 3 . C61 C 0.7688(5) 0.5168(5) 0.2247(4) 0.0257 0.518(13) Uani D . P 2 4 . C62 C 0.8616(6) 0.4615(4) 0.2090(4) 0.0288 0.518(13) Uani D . P 2 4 . C63 C 0.9444(6) 0.4881(5) 0.1447(5) 0.0438 0.518(13) Uani D . P 2 4 . C64 C 0.9241(6) 0.5577(5) 0.0818(5) 0.0489 0.518(13) Uani D . P 2 4 . C65 C 0.8254(6) 0.6053(5) 0.0841(4) 0.0412 0.518(13) Uani D . P 2 4 . C66 C 0.7861(7) 0.6790(4) 0.0277(3) 0.0441 0.518(13) Uani D . P 2 4 . C67 C 0.6814(7) 0.7041(4) 0.0625(4) 0.0504 0.518(13) Uani D . P 2 4 . C68 C 0.6596(5) 0.6497(4) 0.1419(5) 0.0442 0.518(13) Uani D . P 2 4 . C69 C 0.7477(5) 0.5862(5) 0.1549(5) 0.0356 0.518(13) Uani D . P 2 4 . H31 H 0.5225 0.3896 0.0530 0.0821 0.477(10) Uiso R . P 1 1 . H32 H 0.6233 0.4544 0.0671 0.0820 0.477(10) Uiso R . P 1 1 . H33 H 0.6107 0.3657 0.1294 0.0820 0.477(10) Uiso R . P 1 1 . H41 H 0.3681 0.4709 0.0861 0.0562 0.477(10) Uiso R . P 1 1 . H61 H 0.1669 0.5413 0.2206 0.1005 0.477(10) Uiso R . P 1 1 . H62 H 0.2070 0.6307 0.1703 0.1007 0.477(10) Uiso R . P 1 1 . H63 H 0.1987 0.5374 0.1171 0.1008 0.477(10) Uiso R . P 1 1 . H71 H 0.3348 0.6069 0.3251 0.0525 0.477(10) Uiso R . P 1 1 . H91 H 0.4696 0.6087 0.4388 0.0722 0.477(10) Uiso R . P 1 1 . H92 H 0.5758 0.6424 0.3900 0.0720 0.477(10) Uiso R . P 1 1 . H93 H 0.5714 0.5446 0.4352 0.0720 0.477(10) Uiso R . P 1 1 . H131 H 0.5251 0.4503 0.0556 0.0772 0.523(10) Uiso R . P 1 2 . H132 H 0.6207 0.4229 0.1211 0.0770 0.523(10) Uiso R . P 1 2 . H133 H 0.5177 0.3628 0.1160 0.0771 0.523(10) Uiso R . P 1 2 . H141 H 0.3416 0.4909 0.1311 0.0513 0.523(10) Uiso R . P 1 2 . H161 H 0.2065 0.6524 0.2568 0.0941 0.523(10) Uiso R . P 1 2 . H162 H 0.1927 0.5844 0.1739 0.0943 0.523(10) Uiso R . P 1 2 . H163 H 0.1664 0.5528 0.2744 0.0939 0.523(10) Uiso R . P 1 2 . H171 H 0.3562 0.6162 0.3770 0.0470 0.523(10) Uiso R . P 1 2 . H191 H 0.5128 0.6209 0.4688 0.0600 0.523(10) Uiso R . P 1 2 . H192 H 0.6218 0.6272 0.4120 0.0597 0.523(10) Uiso R . P 1 2 . H193 H 0.5910 0.5374 0.4637 0.0601 0.523(10) Uiso R . P 1 2 . H231 H 0.9029 0.5532 0.4414 0.0675 0.476(14) Uiso R . P 1 3 . H232 H 0.8047 0.5819 0.3754 0.0670 0.476(14) Uiso R . P 1 3 . H233 H 0.7921 0.5872 0.4846 0.0669 0.476(14) Uiso R . P 1 3 . H241 H 0.8696 0.4262 0.5541 0.0519 0.476(14) Uiso R . P 1 3 . H261 H 0.7753 0.2091 0.6161 0.1081 0.476(14) Uiso R . P 1 3 . H262 H 0.8938 0.2176 0.5767 0.1082 0.476(14) Uiso R . P 1 3 . H263 H 0.8524 0.2885 0.6496 0.1082 0.476(14) Uiso R . P 1 3 . H271 H 0.6800 0.2197 0.4646 0.0573 0.476(14) Uiso R . P 1 3 . H291 H 0.5538 0.2338 0.3487 0.0678 0.476(14) Uiso R . P 1 3 . H292 H 0.5007 0.3304 0.3446 0.0677 0.476(14) Uiso R . P 1 3 . H293 H 0.5797 0.2993 0.2650 0.0678 0.476(14) Uiso R . P 1 3 . H331 H 0.8830 0.5412 0.4935 0.0603 0.524(14) Uiso R . P 1 4 . H332 H 0.9159 0.5280 0.3903 0.0605 0.524(14) Uiso R . P 1 4 . H333 H 0.8027 0.5724 0.4138 0.0603 0.524(14) Uiso R . P 1 4 . H341 H 0.8974 0.3856 0.5382 0.0440 0.524(14) Uiso R . P 1 4 . H361 H 0.8299 0.1527 0.5492 0.0847 0.524(14) Uiso R . P 1 4 . H362 H 0.7981 0.2186 0.6298 0.0851 0.524(14) Uiso R . P 1 4 . H363 H 0.9163 0.2255 0.5868 0.0852 0.524(14) Uiso R . P 1 4 . H371 H 0.6756 0.2022 0.4488 0.0512 0.524(14) Uiso R . P 1 4 . H391 H 0.5631 0.2259 0.3260 0.0659 0.524(14) Uiso R . P 1 4 . H392 H 0.6152 0.2845 0.2484 0.0659 0.524(14) Uiso R . P 1 4 . H393 H 0.5198 0.3257 0.3073 0.0658 0.524(14) Uiso R . P 1 4 . H411 H 0.7501 0.8978 0.1644 0.0642 0.709(16) Uiso R . P 2 1 . H421 H 0.7253 0.7993 0.3079 0.0702 0.709(16) Uiso R . P 2 1 . H431 H 0.8985 0.6997 0.3296 0.0611 0.709(16) Uiso R . P 2 1 . H441 H 1.0314 0.7407 0.1974 0.0515 0.709(16) Uiso R . P 2 1 . H451 H 0.9388 0.8612 0.0956 0.0552 0.709(16) Uiso R . P 2 1 . H461 H 0.7711 0.8898 0.1272 0.0691 0.291(16) Uiso R . P 2 2 . H471 H 0.6890 0.8190 0.2726 0.0661 0.291(16) Uiso R . P 2 2 . H481 H 0.8293 0.7076 0.3427 0.0549 0.291(16) Uiso R . P 2 2 . H491 H 1.0020 0.7122 0.2400 0.0601 0.291(16) Uiso R . P 2 2 . H501 H 0.9683 0.8307 0.1118 0.0632 0.291(16) Uiso R . P 2 2 . H521 H 0.8823 0.4225 0.2805 0.0317 0.482(13) Uiso R . P 2 3 . H531 H 1.0266 0.4416 0.1765 0.0388 0.482(13) Uiso R . P 2 3 . H541 H 1.0169 0.5554 0.0647 0.0378 0.482(13) Uiso R . P 2 3 . H561 H 0.8776 0.6836 -0.0306 0.0551 0.482(13) Uiso R . P 2 3 . H571 H 0.6763 0.7305 0.0012 0.0559 0.482(13) Uiso R . P 2 3 . H581 H 0.6094 0.6412 0.1419 0.0505 0.482(13) Uiso R . P 2 3 . H621 H 0.8708 0.4068 0.2444 0.0346 0.518(13) Uiso R . P 2 4 . H631 H 1.0110 0.4568 0.1449 0.0523 0.518(13) Uiso R . P 2 4 . H641 H 0.9783 0.5729 0.0385 0.0588 0.518(13) Uiso R . P 2 4 . H661 H 0.8226 0.7054 -0.0255 0.0530 0.518(13) Uiso R . P 2 4 . H671 H 0.6353 0.7546 0.0394 0.0600 0.518(13) Uiso R . P 2 4 . H681 H 0.5978 0.6579 0.1818 0.0527 0.518(13) Uiso R . P 2 4 . 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 0.0308(9) 0.0302(9) 0.0338(9) -0.0057(8) -0.0029(7) 0.0022(7) C1 0.025(2) 0.033(3) 0.045(3) 0.005(3) 0.0012(18) -0.0004(19) Fe1 0.0590(2) 0.04444(18) 0.03541(16) 0.01228(13) -0.01202(13) -0.00376(15) C2 0.025(2) 0.046(3) 0.046(3) 0.002(2) -0.006(2) -0.0035(18) C3 0.038(3) 0.076(4) 0.047(3) -0.018(3) -0.011(2) 0.003(3) C4 0.030(2) 0.053(3) 0.057(3) 0.011(3) -0.008(2) -0.0069(18) C5 0.0274(19) 0.046(3) 0.069(4) 0.020(3) -0.001(2) -0.0020(18) C6 0.030(2) 0.072(3) 0.101(5) 0.026(3) -0.005(3) 0.004(2) C7 0.032(2) 0.038(2) 0.061(4) 0.013(3) 0.006(2) 0.001(2) C8 0.033(2) 0.031(2) 0.050(3) 0.008(2) 0.001(2) -0.0021(18) C9 0.045(3) 0.048(3) 0.052(4) -0.003(3) 0.007(3) 0.007(3) C11 0.031(2) 0.029(2) 0.037(3) 0.004(2) -0.0076(17) -0.0017(18) C12 0.039(2) 0.037(2) 0.044(3) 0.003(2) -0.011(2) 0.0047(17) C13 0.047(3) 0.059(3) 0.048(3) -0.007(2) -0.018(3) 0.011(3) C14 0.035(2) 0.038(2) 0.053(3) 0.006(2) -0.014(2) -0.0015(17) C15 0.0274(18) 0.0340(19) 0.068(3) 0.009(2) -0.008(2) 0.0003(15) C16 0.032(2) 0.056(3) 0.099(5) 0.010(3) -0.014(2) 0.0049(18) C17 0.0257(17) 0.0326(18) 0.060(3) 0.005(2) 0.0010(18) 0.0023(14) C18 0.0243(17) 0.0269(17) 0.045(3) 0.003(2) 0.0004(17) -0.0001(14) C19 0.032(2) 0.041(2) 0.045(3) -0.013(2) 0.0019(19) 0.0036(19) C21 0.029(3) 0.035(3) 0.036(3) -0.003(2) 0.004(2) -0.003(3) C22 0.039(3) 0.041(3) 0.026(2) 0.0044(19) -0.0001(18) -0.002(2) C23 0.049(4) 0.046(3) 0.038(2) 0.003(2) -0.012(2) -0.014(3) C24 0.045(3) 0.048(3) 0.037(2) 0.007(2) -0.005(2) -0.001(2) C25 0.059(3) 0.049(3) 0.047(3) 0.014(2) -0.006(2) 0.006(3) C26 0.084(4) 0.063(4) 0.068(4) 0.024(3) -0.012(3) 0.011(4) C27 0.055(3) 0.029(3) 0.059(4) 0.008(3) 0.003(3) 0.002(2) C28 0.038(3) 0.030(3) 0.044(3) -0.002(2) 0.000(2) 0.006(2) C29 0.060(3) 0.024(3) 0.050(4) -0.011(2) -0.004(3) 0.000(2) C31 0.028(3) 0.032(2) 0.027(3) 0.0054(19) -0.002(2) 0.007(2) C32 0.0264(19) 0.040(2) 0.033(2) 0.0077(18) -0.0002(15) -0.0017(19) C33 0.036(3) 0.045(3) 0.040(2) 0.007(2) -0.0100(18) -0.005(2) C34 0.031(2) 0.048(3) 0.032(2) 0.0109(19) -0.0036(15) 0.003(2) C35 0.042(2) 0.043(3) 0.042(2) 0.014(2) -0.0004(18) 0.004(2) C36 0.061(3) 0.056(3) 0.053(3) 0.021(3) -0.010(2) 0.010(3) C37 0.047(2) 0.032(3) 0.047(3) 0.004(2) -0.005(2) 0.005(2) C38 0.040(3) 0.026(2) 0.039(2) -0.0028(19) -0.002(2) 0.004(2) C39 0.056(3) 0.027(2) 0.050(3) -0.009(2) -0.011(3) 0.002(2) C41 0.066(2) 0.048(2) 0.046(2) -0.0033(18) 0.0007(17) 0.0137(17) C42 0.063(2) 0.072(3) 0.040(2) -0.0030(19) 0.0020(19) -0.003(2) C43 0.068(3) 0.0461(19) 0.0366(18) 0.0080(15) -0.0155(19) -0.015(2) C44 0.0472(18) 0.0356(17) 0.046(2) 0.0078(15) -0.0126(15) -0.0045(14) C45 0.046(2) 0.037(2) 0.053(2) 0.0155(14) -0.0057(14) 0.0013(14) C46 0.078(5) 0.045(5) 0.050(4) 0.010(4) -0.001(4) 0.007(4) C47 0.071(5) 0.043(4) 0.050(4) -0.001(3) -0.008(4) 0.017(4) C48 0.070(5) 0.028(3) 0.038(3) -0.011(3) -0.011(4) 0.006(4) C49 0.069(5) 0.038(4) 0.044(4) -0.010(3) -0.012(3) 0.007(4) C50 0.071(5) 0.042(5) 0.048(4) -0.001(3) 0.001(4) 0.001(4) C51 0.033(2) 0.025(2) 0.015(2) -0.0129(18) -0.0029(16) -0.0010(17) C52 0.026(2) 0.041(2) 0.013(2) -0.0117(18) -0.0064(18) -0.0041(16) C53 0.032(2) 0.039(2) 0.026(3) -0.0033(19) 0.0018(18) -0.0009(17) C54 0.034(2) 0.043(3) 0.019(2) -0.0055(19) 0.0029(17) -0.001(2) C55 0.033(3) 0.050(3) 0.0224(18) 0.0016(18) -0.0029(18) -0.002(2) C56 0.041(3) 0.065(3) 0.031(2) 0.008(2) -0.004(2) -0.003(2) C57 0.041(3) 0.067(3) 0.031(3) 0.017(2) -0.008(2) 0.003(3) C58 0.036(2) 0.061(3) 0.031(3) 0.011(2) -0.0058(19) -0.001(2) C59 0.036(2) 0.042(3) 0.025(2) -0.001(2) -0.0065(17) -0.0018(19) C61 0.034(2) 0.029(2) 0.0143(19) -0.0132(17) -0.0065(14) 0.0005(16) C62 0.037(2) 0.038(2) 0.011(2) -0.0105(16) -0.0074(17) 0.0039(17) C63 0.047(3) 0.049(3) 0.035(3) -0.012(2) 0.009(2) 0.012(2) C64 0.062(3) 0.055(3) 0.030(3) -0.008(2) 0.011(3) -0.001(3) C65 0.053(3) 0.048(2) 0.0223(18) -0.0054(16) -0.001(2) 0.002(2) C66 0.058(4) 0.052(2) 0.0218(17) 0.0045(17) -0.001(2) 0.001(3) C67 0.056(3) 0.057(3) 0.038(3) 0.011(2) -0.012(2) 0.006(2) C68 0.048(3) 0.051(2) 0.034(3) 0.015(2) -0.0069(19) 0.0099(19) C69 0.042(2) 0.044(2) 0.0210(19) -0.0019(18) -0.0015(16) 0.0025(18) _refine_ls_extinction_method None _oxford_refine_ls_scale 4.97(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag B1 . C1 . 1.613(4) yes B1 . C51 . 1.585(5) yes B1 . C11 . 1.566(4) yes B1 . C51 . 1.585(5) yes B1 . C21 . 1.510(6) yes B1 . C51 . 1.585(5) yes B1 . C31 . 1.637(5) yes B1 . C51 . 1.585(5) yes B1 . C1 . 1.613(4) yes B1 . C61 . 1.547(5) yes B1 . C11 . 1.566(4) yes B1 . C61 . 1.547(5) yes B1 . C21 . 1.510(6) yes B1 . C61 . 1.547(5) yes B1 . C31 . 1.637(5) yes B1 . C61 . 1.547(5) yes C1 . C2 . 1.405(4) yes C1 . C8 . 1.412(4) yes Fe1 . C41 . 2.084(5) yes Fe1 . C42 . 2.062(5) yes Fe1 . C43 . 2.058(4) yes Fe1 . C44 . 2.081(4) yes Fe1 . C45 . 2.084(5) yes Fe1 . C46 . 1.891(15) yes Fe1 . C47 . 2.013(12) yes Fe1 . C48 . 2.005(10) yes Fe1 . C49 . 1.931(11) yes Fe1 . C50 . 1.931(15) yes Fe1 . C55 . 2.201(8) yes Fe1 . C56 . 2.172(7) yes Fe1 . C57 . 2.070(6) yes Fe1 . C58 . 2.038(7) yes Fe1 . C59 . 2.177(9) yes Fe1 . C65 . 1.956(7) yes Fe1 . C66 . 1.950(5) yes Fe1 . C67 . 2.060(5) yes Fe1 . C68 . 2.097(7) yes Fe1 . C69 . 2.073(8) yes C2 . C3 . 1.514(5) yes C2 . C4 . 1.396(4) yes C3 . H31 . 0.954 no C3 . H32 . 0.969 no C3 . H33 . 0.966 no C4 . C5 . 1.383(4) yes C4 . H41 . 0.944 no C5 . C6 . 1.520(4) yes C5 . C7 . 1.375(4) yes C6 . H61 . 0.959 no C6 . H62 . 0.965 no C6 . H63 . 0.953 no C7 . C8 . 1.396(4) yes C7 . H71 . 0.937 no C8 . C9 . 1.501(5) yes C9 . H91 . 0.962 no C9 . H92 . 0.971 no C9 . H93 . 0.962 no C11 . C12 . 1.411(4) yes C11 . C18 . 1.409(4) yes C12 . C13 . 1.509(5) yes C12 . C14 . 1.399(4) yes C13 . H131 . 0.960 no C13 . H132 . 0.975 no C13 . H133 . 0.957 no C14 . C15 . 1.376(4) yes C14 . H141 . 0.928 no C15 . C16 . 1.525(4) yes C15 . C17 . 1.386(4) yes C16 . H161 . 0.962 no C16 . H162 . 0.958 no C16 . H163 . 0.947 no C17 . C18 . 1.397(3) yes C17 . H171 . 0.945 no C18 . C19 . 1.510(4) yes C19 . H191 . 0.965 no C19 . H192 . 0.970 no C19 . H193 . 0.960 no C21 . C22 . 1.418(4) yes C21 . C28 . 1.414(4) yes C22 . C23 . 1.513(5) yes C22 . C24 . 1.388(4) yes C23 . H231 . 0.968 no C23 . H232 . 0.965 no C23 . H233 . 0.967 no C24 . C25 . 1.384(4) yes C24 . H241 . 0.944 no C25 . C26 . 1.524(5) yes C25 . C27 . 1.380(5) yes C26 . H261 . 0.967 no C26 . H262 . 0.963 no C26 . H263 . 0.960 no C27 . C28 . 1.391(4) yes C27 . H271 . 0.937 no C28 . C29 . 1.521(5) yes C29 . H291 . 0.961 no C29 . H292 . 0.969 no C29 . H293 . 0.977 no C31 . C32 . 1.412(4) yes C31 . C38 . 1.411(4) yes C32 . C33 . 1.517(4) yes C32 . C34 . 1.393(4) yes C33 . H331 . 0.962 no C33 . H332 . 0.969 no C33 . H333 . 0.975 no C34 . C35 . 1.376(4) yes C34 . H341 . 0.940 no C35 . C36 . 1.518(4) yes C35 . C37 . 1.379(4) yes C36 . H361 . 0.960 no C36 . H362 . 0.972 no C36 . H363 . 0.965 no C37 . C38 . 1.393(4) yes C37 . H371 . 0.945 no C38 . C39 . 1.509(5) yes C39 . H391 . 0.957 no C39 . H392 . 0.961 no C39 . H393 . 0.978 no C41 . C42 . 1.411(3) yes C41 . C45 . 1.419(3) yes C41 . H411 . 0.982 no C42 . C43 . 1.417(3) yes C42 . H421 . 0.978 no C43 . C44 . 1.432(3) yes C43 . H431 . 0.975 no C44 . C45 . 1.412(3) yes C44 . H441 . 0.977 no C45 . H451 . 0.983 no C46 . C47 . 1.412(5) yes C46 . C50 . 1.412(5) yes C46 . H461 . 0.984 no C47 . C48 . 1.410(5) yes C47 . H471 . 0.980 no C48 . C49 . 1.433(5) yes C48 . H481 . 0.983 no C49 . C50 . 1.409(5) yes C49 . H491 . 0.977 no C50 . H501 . 0.990 no C51 . C52 . 1.422(4) yes C51 . C59 . 1.439(4) yes C52 . C53 . 1.439(4) yes C52 . H521 . 0.942 no C53 . C54 . 1.380(4) yes C53 . H531 . 0.940 no C54 . C55 . 1.401(4) yes C54 . H541 . 0.930 no C55 . C56 . 1.431(4) yes C55 . C59 . 1.433(3) yes C56 . C57 . 1.431(4) yes C56 . H561 . 0.996 no C57 . C58 . 1.425(4) yes C57 . H571 . 0.972 no C58 . C59 . 1.431(4) yes C58 . H581 . 0.971 no C61 . C62 . 1.412(4) yes C61 . C69 . 1.451(4) yes C62 . C63 . 1.437(4) yes C62 . H621 . 0.954 no C63 . C64 . 1.382(4) yes C63 . H631 . 0.932 no C64 . C65 . 1.391(4) yes C64 . H641 . 0.944 no C65 . C66 . 1.429(4) yes C65 . C69 . 1.432(3) yes C66 . C67 . 1.427(4) yes C66 . H661 . 0.975 no C67 . C68 . 1.424(4) yes C67 . H671 . 0.981 no C68 . C69 . 1.428(4) yes C68 . H681 . 0.964 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 . B1 . C51 . 114.6(5) yes C11 . B1 . C51 . 124.3(5) yes C21 . B1 . C51 . 119.9(6) yes C31 . B1 . C51 . 116.9(5) yes C1 . B1 . C61 . 116.2(5) yes C11 . B1 . C61 . 124.3(5) yes C21 . B1 . C61 . 119.0(5) yes C31 . B1 . C61 . 116.9(5) yes B1 . C1 . C2 . 123.3(3) yes B1 . C1 . C8 . 118.5(3) yes C2 . C1 . C8 . 118.24(6) yes C41 . Fe1 . C42 . 39.79(12) yes C41 . Fe1 . C43 . 67.07(14) yes C42 . Fe1 . C43 . 40.24(12) yes C41 . Fe1 . C44 . 66.73(15) yes C42 . Fe1 . C44 . 67.50(14) yes C43 . Fe1 . C44 . 40.49(11) yes C41 . Fe1 . C45 . 39.81(14) yes C42 . Fe1 . C45 . 67.24(15) yes C43 . Fe1 . C45 . 67.37(14) yes C44 . Fe1 . C45 . 39.62(11) yes C46 . Fe1 . C47 . 42.3(3) yes C46 . Fe1 . C48 . 71.6(4) yes C47 . Fe1 . C48 . 41.1(2) yes C46 . Fe1 . C49 . 73.3(4) yes C47 . Fe1 . C49 . 71.1(4) yes C48 . Fe1 . C49 . 42.6(2) yes C46 . Fe1 . C50 . 43.3(3) yes C47 . Fe1 . C50 . 70.9(4) yes C48 . Fe1 . C50 . 71.3(4) yes C49 . Fe1 . C50 . 42.8(3) yes C55 . Fe1 . C56 . 38.21(15) yes C55 . Fe1 . C57 . 64.94(19) yes C56 . Fe1 . C57 . 39.34(13) yes C55 . Fe1 . C58 . 65.5(2) yes C56 . Fe1 . C58 . 66.78(18) yes C57 . Fe1 . C58 . 40.58(14) yes C55 . Fe1 . C59 . 38.19(14) yes C56 . Fe1 . C59 . 65.1(2) yes C57 . Fe1 . C59 . 66.1(2) yes C58 . Fe1 . C59 . 39.52(17) yes C65 . Fe1 . C66 . 42.91(14) yes C65 . Fe1 . C67 . 69.50(18) yes C66 . Fe1 . C67 . 41.59(13) yes C65 . Fe1 . C68 . 68.79(19) yes C66 . Fe1 . C68 . 69.71(17) yes C67 . Fe1 . C68 . 40.06(13) yes C65 . Fe1 . C69 . 41.51(16) yes C66 . Fe1 . C69 . 70.9(2) yes C67 . Fe1 . C69 . 68.2(2) yes C68 . Fe1 . C69 . 40.06(15) yes C1 . C2 . C3 . 121.84(6) yes C1 . C2 . C4 . 120.07(5) yes C3 . C2 . C4 . 118.04(5) yes C2 . C3 . H31 . 108.7 no C2 . C3 . H32 . 108.8 no H31 . C3 . H32 . 108.5 no C2 . C3 . H33 . 111.1 no H31 . C3 . H33 . 109.3 no H32 . C3 . H33 . 110.3 no C2 . C4 . C5 . 121.17(6) yes C2 . C4 . H41 . 119.3 no C5 . C4 . H41 . 119.5 no C4 . C5 . C6 . 120.39(5) yes C4 . C5 . C7 . 119.22(5) yes C6 . C5 . C7 . 120.38(5) yes C5 . C6 . H61 . 109.9 no C5 . C6 . H62 . 109.8 no H61 . C6 . H62 . 110.1 no C5 . C6 . H63 . 108.7 no H61 . C6 . H63 . 108.5 no H62 . C6 . H63 . 109.7 no C5 . C7 . C8 . 121.17(6) yes C5 . C7 . H71 . 119.6 no C8 . C7 . H71 . 119.2 no C1 . C8 . C7 . 120.09(5) yes C1 . C8 . C9 . 121.80(6) yes C7 . C8 . C9 . 118.04(6) yes C8 . C9 . H91 . 109.7 no C8 . C9 . H92 . 110.5 no H91 . C9 . H92 . 108.1 no C8 . C9 . H93 . 111.5 no H91 . C9 . H93 . 108.0 no H92 . C9 . H93 . 108.9 no B1 . C11 . C12 . 120.8(2) yes B1 . C11 . C18 . 120.8(2) yes C12 . C11 . C18 . 118.25(6) yes C11 . C12 . C13 . 121.85(5) yes C11 . C12 . C14 . 120.11(5) yes C13 . C12 . C14 . 118.04(5) yes C12 . C13 . H131 . 113.4 no C12 . C13 . H132 . 112.0 no H131 . C13 . H132 . 105.4 no C12 . C13 . H133 . 112.5 no H131 . C13 . H133 . 108.0 no H132 . C13 . H133 . 105.0 no C12 . C14 . C15 . 121.19(6) yes C12 . C14 . H141 . 119.8 no C15 . C14 . H141 . 119.0 no C14 . C15 . C16 . 120.38(5) yes C14 . C15 . C17 . 119.22(5) yes C16 . C15 . C17 . 120.40(5) yes C15 . C16 . H161 . 109.6 no C15 . C16 . H162 . 109.0 no H161 . C16 . H162 . 108.9 no C15 . C16 . H163 . 109.9 no H161 . C16 . H163 . 109.4 no H162 . C16 . H163 . 110.1 no C15 . C17 . C18 . 121.15(6) yes C15 . C17 . H171 . 119.1 no C18 . C17 . H171 . 119.8 no C11 . C18 . C17 . 120.07(5) yes C11 . C18 . C19 . 121.78(6) yes C17 . C18 . C19 . 118.06(6) yes C18 . C19 . H191 . 110.7 no C18 . C19 . H192 . 110.5 no H191 . C19 . H192 . 109.1 no C18 . C19 . H193 . 111.3 no H191 . C19 . H193 . 107.4 no H192 . C19 . H193 . 107.8 no B1 . C21 . C22 . 121.0(3) yes B1 . C21 . C28 . 122.4(3) yes C22 . C21 . C28 . 116.46(6) yes C21 . C22 . C23 . 121.64(6) yes C21 . C22 . C24 . 120.89(5) yes C23 . C22 . C24 . 117.33(6) yes C22 . C23 . H231 . 107.9 no C22 . C23 . H232 . 110.6 no H231 . C23 . H232 . 109.0 no C22 . C23 . H233 . 109.5 no H231 . C23 . H233 . 109.2 no H232 . C23 . H233 . 110.6 no C22 . C24 . C25 . 121.55(6) yes C22 . C24 . H241 . 119.4 no C25 . C24 . H241 . 119.0 no C24 . C25 . C26 . 120.89(6) yes C24 . C25 . C27 . 118.16(5) yes C26 . C25 . C27 . 120.86(6) yes C25 . C26 . H261 . 109.8 no C25 . C26 . H262 . 110.0 no H261 . C26 . H262 . 108.6 no C25 . C26 . H263 . 110.7 no H261 . C26 . H263 . 108.5 no H262 . C26 . H263 . 109.2 no C25 . C27 . C28 . 121.56(6) yes C25 . C27 . H271 . 119.7 no C28 . C27 . H271 . 118.7 no C21 . C28 . C27 . 120.89(5) yes C21 . C28 . C29 . 121.65(6) yes C27 . C28 . C29 . 117.33(6) yes C28 . C29 . H291 . 109.7 no C28 . C29 . H292 . 111.4 no H291 . C29 . H292 . 107.4 no C28 . C29 . H293 . 110.7 no H291 . C29 . H293 . 109.1 no H292 . C29 . H293 . 108.5 no B1 . C31 . C32 . 123.0(3) yes B1 . C31 . C38 . 119.9(3) yes C32 . C31 . C38 . 116.58(6) yes C31 . C32 . C33 . 121.63(5) yes C31 . C32 . C34 . 120.99(5) yes C33 . C32 . C34 . 117.36(5) yes C32 . C33 . H331 . 111.1 no C32 . C33 . H332 . 111.6 no H331 . C33 . H332 . 108.0 no C32 . C33 . H333 . 110.6 no H331 . C33 . H333 . 107.9 no H332 . C33 . H333 . 107.5 no C32 . C34 . C35 . 121.61(6) yes C32 . C34 . H341 . 118.8 no C35 . C34 . H341 . 119.6 no C34 . C35 . C36 . 120.90(5) yes C34 . C35 . C37 . 118.23(5) yes C36 . C35 . C37 . 120.87(5) yes C35 . C36 . H361 . 109.7 no C35 . C36 . H362 . 108.1 no H361 . C36 . H362 . 108.1 no C35 . C36 . H363 . 110.4 no H361 . C36 . H363 . 111.0 no H362 . C36 . H363 . 109.4 no C35 . C37 . C38 . 121.66(6) yes C35 . C37 . H371 . 119.7 no C38 . C37 . H371 . 118.7 no C31 . C38 . C37 . 120.90(5) yes C31 . C38 . C39 . 121.53(6) yes C37 . C38 . C39 . 117.22(6) yes C38 . C39 . H391 . 109.8 no C38 . C39 . H392 . 110.4 no H391 . C39 . H392 . 108.4 no C38 . C39 . H393 . 111.1 no H391 . C39 . H393 . 108.8 no H392 . C39 . H393 . 108.4 no Fe1 . C41 . C42 . 69.2(3) yes Fe1 . C41 . C45 . 70.1(2) yes C42 . C41 . C45 . 108.39(6) yes Fe1 . C41 . H411 . 121.8 no C42 . C41 . H411 . 125.6 no C45 . C41 . H411 . 125.7 no C41 . C42 . Fe1 . 71.0(2) yes C41 . C42 . C43 . 108.03(6) yes Fe1 . C42 . C43 . 69.7(2) yes C41 . C42 . H421 . 125.0 no Fe1 . C42 . H421 . 122.8 no C43 . C42 . H421 . 126.9 no C42 . C43 . Fe1 . 70.0(2) yes C42 . C43 . C44 . 107.77(6) yes Fe1 . C43 . C44 . 70.6(2) yes C42 . C43 . H431 . 126.2 no Fe1 . C43 . H431 . 124.1 no C44 . C43 . H431 . 126.1 no C43 . C44 . Fe1 . 68.9(2) yes C43 . C44 . C45 . 107.76(6) yes Fe1 . C44 . C45 . 70.3(2) yes C43 . C44 . H441 . 127.0 no Fe1 . C44 . H441 . 126.0 no C45 . C44 . H441 . 125.2 no Fe1 . C45 . C41 . 70.1(2) yes Fe1 . C45 . C44 . 70.1(2) yes C41 . C45 . C44 . 108.04(6) yes Fe1 . C45 . H451 . 124.6 no C41 . C45 . H451 . 126.4 no C44 . C45 . H451 . 125.5 no Fe1 . C46 . C47 . 73.5(6) yes Fe1 . C46 . C50 . 69.8(6) yes C47 . C46 . C50 . 108.29(7) yes Fe1 . C46 . H461 . 125.3 no C47 . C46 . H461 . 125.6 no C50 . C46 . H461 . 126.0 no C46 . C47 . Fe1 . 64.3(6) yes C46 . C47 . C48 . 107.94(6) yes Fe1 . C47 . C48 . 69.2(5) yes C46 . C47 . H471 . 125.8 no Fe1 . C47 . H471 . 125.5 no C48 . C47 . H471 . 125.6 no C47 . C48 . Fe1 . 69.8(6) yes C47 . C48 . C49 . 107.66(6) yes Fe1 . C48 . C49 . 65.9(5) yes C47 . C48 . H481 . 125.9 no Fe1 . C48 . H481 . 126.6 no C49 . C48 . H481 . 126.3 no C48 . C49 . Fe1 . 71.4(5) yes C48 . C49 . C50 . 107.65(6) yes Fe1 . C49 . C50 . 68.6(6) yes C48 . C49 . H491 . 126.5 no Fe1 . C49 . H491 . 125.0 no C50 . C49 . H491 . 125.9 no C46 . C50 . C49 . 107.92(7) yes C46 . C50 . Fe1 . 66.9(5) yes C49 . C50 . Fe1 . 68.6(5) yes C46 . C50 . H501 . 125.7 no C49 . C50 . H501 . 126.0 no Fe1 . C50 . H501 . 124.4 no B1 . C51 . C52 . 114.7(3) yes B1 . C51 . C59 . 128.4(3) yes C52 . C51 . C59 . 115.03(7) yes C51 . C52 . C53 . 121.51(7) yes C51 . C52 . H521 . 120.0 no C53 . C52 . H521 . 118.3 no C52 . C53 . C54 . 120.27(6) yes C52 . C53 . H531 . 119.4 no C54 . C53 . H531 . 120.3 no C53 . C54 . C55 . 119.76(6) yes C53 . C54 . H541 . 120.0 no C55 . C54 . H541 . 120.3 no Fe1 . C55 . C54 . 125.7(5) yes Fe1 . C55 . C56 . 69.8(3) yes C54 . C55 . C56 . 130.37(9) yes Fe1 . C55 . C59 . 70.0(3) yes C54 . C55 . C59 . 120.16(6) yes C56 . C55 . C59 . 109.46(6) yes Fe1 . C56 . C55 . 72.0(3) yes Fe1 . C56 . C57 . 66.5(3) yes C55 . C56 . C57 . 106.63(6) yes Fe1 . C56 . H561 . 125.8 no C55 . C56 . H561 . 126.6 no C57 . C56 . H561 . 126.8 no C56 . C57 . Fe1 . 74.2(3) yes C56 . C57 . C58 . 108.62(6) yes Fe1 . C57 . C58 . 68.5(3) yes C56 . C57 . H571 . 125.9 no Fe1 . C57 . H571 . 125.0 no C58 . C57 . H571 . 125.5 no C57 . C58 . Fe1 . 70.9(3) yes C57 . C58 . C59 . 108.58(6) yes Fe1 . C58 . C59 . 75.5(4) yes C57 . C58 . H581 . 126.0 no Fe1 . C58 . H581 . 123.5 no C59 . C58 . H581 . 125.2 no Fe1 . C59 . C51 . 131.1(5) yes Fe1 . C59 . C55 . 71.8(3) yes C51 . C59 . C55 . 121.37(6) yes Fe1 . C59 . C58 . 65.0(3) yes C51 . C59 . C58 . 131.94(11) yes C55 . C59 . C58 . 106.59(6) yes B1 . C61 . C62 . 117.7(3) yes B1 . C61 . C69 . 122.2(3) yes C62 . C61 . C69 . 114.98(6) yes C61 . C62 . C63 . 121.46(7) yes C61 . C62 . H621 . 118.7 no C63 . C62 . H621 . 119.7 no C62 . C63 . C64 . 120.28(6) yes C62 . C63 . H631 . 119.1 no C64 . C63 . H631 . 120.6 no C63 . C64 . C65 . 119.80(6) yes C63 . C64 . H641 . 119.3 no C65 . C64 . H641 . 120.9 no C64 . C65 . Fe1 . 121.6(5) yes C64 . C65 . C66 . 130.19(10) yes Fe1 . C65 . C66 . 68.3(3) yes C64 . C65 . C69 . 120.20(6) yes Fe1 . C65 . C69 . 73.6(4) yes C66 . C65 . C69 . 109.50(6) yes C65 . C66 . Fe1 . 68.8(3) yes C65 . C66 . C67 . 106.65(6) yes Fe1 . C66 . C67 . 73.3(3) yes C65 . C66 . H661 . 126.5 no Fe1 . C66 . H661 . 124.6 no C67 . C66 . H661 . 126.8 no C66 . C67 . Fe1 . 65.1(3) yes C66 . C67 . C68 . 108.63(6) yes Fe1 . C67 . C68 . 71.4(3) yes C66 . C67 . H671 . 125.7 no Fe1 . C67 . H671 . 124.9 no C68 . C67 . H671 . 125.4 no Fe1 . C68 . C67 . 68.5(3) yes Fe1 . C68 . C69 . 69.1(4) yes C67 . C68 . C69 . 108.57(6) yes Fe1 . C68 . H681 . 125.1 no C67 . C68 . H681 . 124.7 no C69 . C68 . H681 . 126.6 no C61 . C69 . C65 . 121.34(6) yes C61 . C69 . C68 . 132.03(10) yes C65 . C69 . C68 . 106.55(6) yes C61 . C69 . Fe1 . 125.9(5) yes C65 . C69 . Fe1 . 64.9(3) yes C68 . C69 . Fe1 . 70.9(3) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C17 . H71 . C16 . 131.4(5) 0.781 1.942 2.527(10) yes C13 . H132 . C51 . 137.0(2) 0.975 2.480 3.262(10) yes C4 . H141 . C6 . 131.6(6) 0.707 1.995 2.520(10) yes C16 . H161 . C26 2_666 140.0(2) 0.962 2.580 3.374(10) yes C17 . H171 . C25 2_666 163.35(18) 0.945 2.555 3.471(10) yes C23 . H232 . C61 . 131.2(2) 0.965 2.407 3.128(10) yes C26 . H263 . C16 2_666 144.17(19) 0.960 2.548 3.374(10) yes C52 . H521 . C32 . 127.79(19) 0.942 2.426 3.095(10) yes _iucr_refine_instruction_details_constraints ; # # Punched on 28/03/13 at 13:08:13 # #LIST 12 BLOCK SCALE X'S,U'S EQUIV PART(1001,OCC) PART(1002,OCC) WEIGHT -1 PART(1002,OCC) EQUIV PART(1003,OCC) PART(1004,OCC) WEIGHT -1 PART(1004,OCC) EQUIV PART(2001,OCC) PART(2002,OCC) WEIGHT -1 PART(2002,OCC) EQUIV PART(2003,OCC) PART(2004,OCC) WEIGHT -1 PART(2004,OCC) RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S) H ( 33,X'S) RIDE C ( 4,X'S) H ( 41,X'S) RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,X'S) H ( 63,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S) H ( 93,X'S) RIDE C ( 13,X'S) H ( 131,X'S) H ( 132,X'S) H ( 133,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 16,X'S) H ( 161,X'S) H ( 162,X'S) H ( 163,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 19,X'S) H ( 191,X'S) H ( 192,X'S) H ( 193,X'S) RIDE C ( 23,X'S) H ( 231,X'S) H ( 232,X'S) H ( 233,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 26,X'S) H ( 261,X'S) H ( 262,X'S) H ( 263,X'S) RIDE C ( 27,X'S) H ( 271,X'S) RIDE C ( 29,X'S) H ( 291,X'S) H ( 292,X'S) H ( 293,X'S) RIDE C ( 33,X'S) H ( 331,X'S) H ( 332,X'S) H ( 333,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 36,X'S) H ( 361,X'S) H ( 362,X'S) H ( 363,X'S) RIDE C ( 37,X'S) H ( 371,X'S) RIDE C ( 39,X'S) H ( 391,X'S) H ( 392,X'S) H ( 393,X'S) RIDE C ( 41,X'S) H ( 411,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) RIDE C ( 45,X'S) H ( 451,X'S) RIDE C ( 46,X'S) H ( 461,X'S) RIDE C ( 47,X'S) H ( 471,X'S) RIDE C ( 48,X'S) H ( 481,X'S) RIDE C ( 49,X'S) H ( 491,X'S) RIDE C ( 50,X'S) H ( 501,X'S) RIDE C ( 52,X'S) H ( 521,X'S) RIDE C ( 53,X'S) H ( 531,X'S) RIDE C ( 54,X'S) H ( 541,X'S) RIDE C ( 56,X'S) H ( 561,X'S) RIDE C ( 57,X'S) H ( 571,X'S) RIDE C ( 58,X'S) H ( 581,X'S) RIDE C ( 62,X'S) H ( 621,X'S) RIDE C ( 63,X'S) H ( 631,X'S) RIDE C ( 64,X'S) H ( 641,X'S) RIDE C ( 66,X'S) H ( 661,X'S) RIDE C ( 67,X'S) H ( 671,X'S) RIDE C ( 68,X'S) H ( 681,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 28/03/13 at 13:08:13 # #LIST 16 SAME C(1) C(2) C(3) C(4) C(5) C(6) C(7) C(8) C(9) AND CONT C(1) C(8) C(9) C(7) C(5) C(6) C(4) C(2) C(3) AND CONT C(11) C(12) C(13) C(14) C(15) C(16) C(17) C(18) C(19) AND CONT C(11) C(18) C(19) C(17) C(15) C(16) C(14) C(12) C(13) SIMU 0.01 C(1) C(2) C(3) C(4) C(5) C(6) C(7) C(8) C(9) AND CONT C(1) C(8) C(9) C(7) C(5) C(6) C(4) C(2) C(3) AND CONT C(11) C(12) C(13) C(14) C(15) C(16) C(17) C(18) C(19) AND CONT C(11) C(18) C(19) C(17) C(15) C(16) C(14) C(12) C(13) DELU 0.01 C(1) C(2) C(3) C(4) C(5) C(6) C(7) C(8) C(9) AND CONT C(1) C(8) C(9) C(7) C(5) C(6) C(4) C(2) C(3) AND CONT C(11) C(12) C(13) C(14) C(15) C(16) C(17) C(18) C(19) AND CONT C(11) C(18) C(19) C(17) C(15) C(16) C(14) C(12) C(13) SAME C(21) C(22) C(23) C(24) C(25) C(26) C(27) C(28) C(29) AND CONT C(21) C(28) C(29) C(27) C(25) C(26) C(24) C(22) C(23) AND CONT C(31) C(32) C(33) C(34) C(35) C(36) C(37) C(38) C(39) AND CONT C(31) C(38) C(39) C(37) C(35) C(36) C(34) C(32) C(33) SIMU 0.01 C(21) C(22) C(23) C(24) C(25) C(26) C(27) C(28) C(29) AND CONT C(21) C(28) C(29) C(27) C(25) C(26) C(24) C(22) C(23) AND CONT C(31) C(32) C(33) C(34) C(35) C(36) C(37) C(38) C(39) AND CONT C(31) C(38) C(39) C(37) C(35) C(36) C(34) C(32) C(33) DELU 0.01 C(21) C(22) C(23) C(24) C(25) C(26) C(27) C(28) C(29) AND CONT C(21) C(28) C(29) C(27) C(25) C(26) C(24) C(22) C(23) AND CONT C(31) C(32) C(33) C(34) C(35) C(36) C(37) C(38) C(39) AND CONT C(31) C(38) C(39) C(37) C(35) C(36) C(34) C(32) C(33) SAME C(41) C(42) C(43) C(44) C(45) AND CONT C(41) C(45) C(44) C(43) C(42) AND CONT C(46) C(47) C(48) C(49) C(50) AND CONT C(46) C(50) C(49) C(48) C(47) SIMU 0.01 C(41) C(42) C(43) C(44) C(45) AND CONT C(41) C(45) C(44) C(43) C(42) AND CONT C(46) C(47) C(48) C(49) C(50) AND CONT C(46) C(50) C(49) C(48) C(47) DELU 0.01 C(41) C(42) C(43) C(44) C(45) AND CONT C(41) C(45) C(44) C(43) C(42) AND CONT C(46) C(47) C(48) C(49) C(50) AND CONT C(46) C(50) C(49) C(48) C(47) SAME C(55) C(56) C(57) C(58) C(59) C(55) AND CONT C(55) C(59) C(58) C(57) C(56) C(55) AND CONT C(65) C(66) C(67) C(68) C(69) C(65) AND CONT C(65) C(69) C(68) C(67) C(66) C(65) SAME C(51) C(52) C(53) C(54) C(55) C(59) C(51) AND CONT C(51) C(59) C(55) C(54) C(53) C(52) C(51) AND CONT C(61) C(62) C(63) C(64) C(65) C(69) C(61) AND CONT C(61) C(69) C(65) C(64) C(63) C(62) C(61) SIMU 0.01 C(55) C(56) C(57) C(58) C(59) C(55) AND CONT C(55) C(59) C(58) C(57) C(56) C(55) AND CONT C(65) C(66) C(67) C(68) C(69) C(65) AND CONT C(65) C(69) C(68) C(67) C(66) C(65) SIMU 0.01 C(51) C(52) C(53) C(54) C(55) C(59) C(51) AND CONT C(51) C(59) C(55) C(54) C(53) C(52) C(51) AND CONT C(61) C(62) C(63) C(64) C(65) C(69) C(61) AND CONT C(61) C(69) C(65) C(64) C(63) C(62) C(61) DELU 0.01 C(55) C(56) C(57) C(58) C(59) C(55) AND CONT C(55) C(59) C(58) C(57) C(56) C(55) AND CONT C(65) C(66) C(67) C(68) C(69) C(65) AND CONT C(65) C(69) C(68) C(67) C(66) C(65) DELU 0.01 C(51) C(52) C(53) C(54) C(55) C(59) C(51) AND CONT C(51) C(59) C(55) C(54) C(53) C(52) C(51) AND CONT C(61) C(62) C(63) C(64) C(65) C(69) C(61) AND CONT C(61) C(69) C(65) C(64) C(63) C(62) C(61) END ; _database_code_depnum_ccdc_archive 'CCDC 940845' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_017rtrt12 _audit_creation_date 13-05-23 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title '017rtrt12 in P -1' _chemical_name_systematic . _chemical_melting_point . _cell_length_a 11.80090(10) _cell_length_b 12.70250(10) _cell_length_c 14.5226(2) _cell_angle_alpha 76.3891(5) _cell_angle_beta 84.0128(5) _cell_angle_gamma 82.2242(6) _cell_volume 2090.42(4) _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841 1.4228 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C40 H50 B1 Fe1 K0.50 N1 O6 # Dc = 1.16 Fooo = 864.00 Mu = 4.52 M = 727.05 # Found Formula = C45 H57 B1 Fe1 K1 N1 O6 # Dc = 1.29 FOOO = 864.00 Mu = 5.08 M = 813.71 _chemical_formula_sum 'C45 H57 B1 Fe1 K1 N1 O6' _chemical_formula_moiety 'C45 H57 B1 Fe1 K1 N1 O6' _chemical_compound_source . _chemical_formula_weight 813.71 _cell_measurement_reflns_used 8792 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_min 0.180 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_max 0.250 _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 0.508 # Sheldrick geometric approximatio 0.90 0.91 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.91 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 65025 _reflns_number_total 9499 _diffrn_reflns_av_R_equivalents 0.021 # Number of reflections without Friedels Law is 16521 # Number of reflections with Friedels Law is 9499 # Theoretical number of reflections is about 9584 _diffrn_reflns_theta_min 5.124 _diffrn_reflns_theta_max 27.479 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.655 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min -15 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 2.16 _oxford_diffrn_Wilson_scale 2.36 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.41 _refine_diff_density_max 0.39 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>0.0\s(I) _refine_ls_number_reflns 9499 _refine_ls_number_restraints 0 _refine_ls_number_parameters 496 _oxford_refine_ls_R_factor_ref 0.0465 _refine_ls_wR_factor_ref 0.0923 _refine_ls_goodness_of_fit_ref 0.9115 _refine_ls_shift/su_max 0.0008655 _refine_ls_shift/su_mean 0.0000477 # The values computed with all filters except I/sigma _oxford_reflns_number_all 9499 _refine_ls_R_factor_all 0.0465 _refine_ls_wR_factor_all 0.0923 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 8136 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_gt 0.0853 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr #undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 33.8 54.1 32.3 13.5 3.30 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Fe1 Fe 0.17181(2) 0.983889(18) 0.330465(16) 0.0264 1.0000 Uani . . . . . . C2 C 0.24962(15) 0.82723(13) 0.37688(11) 0.0300 1.0000 Uani . . . . . . C3 C 0.30519(13) 0.87425(12) 0.28628(11) 0.0249 1.0000 Uani . . . . . . C4 C 0.34820(14) 0.97256(13) 0.29646(13) 0.0299 1.0000 Uani . . . . . . C5 C 0.31892(16) 0.98321(15) 0.39273(13) 0.0366 1.0000 Uani . . . . . . C6 C 0.26123(16) 0.89293(15) 0.44178(12) 0.0364 1.0000 Uani . . . . . . C7 C 0.40414(14) 1.03932(14) 0.21628(14) 0.0340 1.0000 Uani . . . . . . C8 C 0.41929(14) 1.00547(14) 0.13370(13) 0.0325 1.0000 Uani . . . . . . C9 C 0.38177(13) 0.90567(13) 0.12545(11) 0.0268 1.0000 Uani . . . . . . C10 C 0.32601(12) 0.83654(12) 0.19846(11) 0.0237 1.0000 Uani . . . . . . B11 B 0.29220(14) 0.71889(14) 0.18663(12) 0.0225 1.0000 Uani . . . . . . C12 C 0.16214(13) 0.70859(13) 0.23588(11) 0.0257 1.0000 Uani . . . . . . N13 N 0.07285(12) 0.69686(12) 0.27465(11) 0.0341 1.0000 Uani . . . . . . C14 C 0.29439(13) 0.72524(12) 0.07095(11) 0.0239 1.0000 Uani . . . . . . C15 C 0.20665(14) 0.78922(13) 0.01631(11) 0.0265 1.0000 Uani . . . . . . C16 C 0.10535(14) 0.85249(15) 0.05917(12) 0.0339 1.0000 Uani . . . . . . C17 C 0.21191(15) 0.80222(14) -0.08286(11) 0.0308 1.0000 Uani . . . . . . C18 C 0.30404(17) 0.75519(14) -0.13227(12) 0.0340 1.0000 Uani . . . . . . C19 C 0.3105(2) 0.77157(18) -0.23935(13) 0.0469 1.0000 Uani . . . . . . C20 C 0.39170(16) 0.69412(14) -0.08011(12) 0.0330 1.0000 Uani . . . . . . C21 C 0.38863(14) 0.67823(13) 0.01892(12) 0.0284 1.0000 Uani . . . . . . C22 C 0.49272(15) 0.61186(17) 0.06475(13) 0.0387 1.0000 Uani . . . . . . C23 C 0.36211(13) 0.60622(12) 0.25074(10) 0.0238 1.0000 Uani . . . . . . C24 C 0.32342(14) 0.50380(13) 0.25533(12) 0.0286 1.0000 Uani . . . . . . C25 C 0.23090(18) 0.48960(15) 0.19602(15) 0.0409 1.0000 Uani . . . . . . C26 C 0.37193(15) 0.40756(14) 0.31331(13) 0.0326 1.0000 Uani . . . . . . C27 C 0.45825(15) 0.40689(14) 0.37157(12) 0.0331 1.0000 Uani . . . . . . C28 C 0.50055(14) 0.50520(14) 0.36406(12) 0.0314 1.0000 Uani . . . . . . C29 C 0.45716(13) 0.60267(13) 0.30420(11) 0.0265 1.0000 Uani . . . . . . C30 C 0.52399(14) 0.69837(14) 0.29660(13) 0.0323 1.0000 Uani . . . . . . C31 C 0.50255(18) 0.30410(16) 0.43937(15) 0.0459 1.0000 Uani . . . . . . C32 C 0.07671(15) 1.05634(15) 0.21776(12) 0.0344 1.0000 Uani . . . . . . C33 C 0.10416(16) 1.13545(14) 0.26378(13) 0.0363 1.0000 Uani . . . . . . C34 C 0.05772(15) 1.10895(14) 0.35977(13) 0.0342 1.0000 Uani . . . . . . C35 C 0.00156(15) 1.01401(15) 0.37222(12) 0.0330 1.0000 Uani . . . . . . C36 C 0.01332(14) 0.98092(15) 0.28425(12) 0.0322 1.0000 Uani . . . . . . K37 K -0.14848(3) 0.65062(3) 0.25568(2) 0.0270 1.0000 Uani . . . . . . O38 O -0.12801(10) 0.47957(9) 0.41685(8) 0.0316 1.0000 Uani . . . . . . C39 C -0.17396(15) 0.50004(15) 0.50705(12) 0.0348 1.0000 Uani . . . . . . C40 C -0.15005(15) 0.61202(16) 0.50890(12) 0.0344 1.0000 Uani . . . . . . O41 O -0.21650(10) 0.68936(10) 0.44119(8) 0.0311 1.0000 Uani . . . . . . C42 C -0.19943(18) 0.79774(16) 0.44099(15) 0.0407 1.0000 Uani . . . . . . C43 C -0.27087(17) 0.87476(16) 0.36826(15) 0.0417 1.0000 Uani . . . . . . O44 O -0.22809(10) 0.85936(10) 0.27707(9) 0.0350 1.0000 Uani . . . . . . C45 C -0.29450(16) 0.92651(14) 0.20373(15) 0.0407 1.0000 Uani . . . . . . C46 C -0.23662(18) 0.91510(15) 0.10980(15) 0.0433 1.0000 Uani . . . . . . O47 O -0.23729(12) 0.80592(10) 0.10069(9) 0.0379 1.0000 Uani . . . . . . C48 C -0.19052(17) 0.79201(17) 0.00936(13) 0.0415 1.0000 Uani . . . . . . C49 C -0.20061(17) 0.67847(18) 0.00187(13) 0.0415 1.0000 Uani . . . . . . O50 O -0.13460(11) 0.60300(11) 0.07002(9) 0.0372 1.0000 Uani . . . . . . C51 C -0.14788(18) 0.49274(17) 0.07031(14) 0.0421 1.0000 Uani . . . . . . C52 C -0.08306(17) 0.41901(16) 0.14786(13) 0.0385 1.0000 Uani . . . . . . O53 O -0.13569(10) 0.43591(10) 0.23715(8) 0.0323 1.0000 Uani . . . . . . C54 C -0.08635(16) 0.35813(14) 0.31384(13) 0.0353 1.0000 Uani . . . . . . C55 C -0.14732(16) 0.37577(14) 0.40548(13) 0.0349 1.0000 Uani . . . . . . H21 H 0.2122 0.7613 0.3902 0.0351 1.0000 Uiso R . . . . . H51 H 0.3366 1.0433 0.4183 0.0438 1.0000 Uiso R . . . . . H61 H 0.2297 0.8792 0.5087 0.0432 1.0000 Uiso R . . . . . H71 H 0.4311 1.1033 0.2220 0.0417 1.0000 Uiso R . . . . . H81 H 0.4555 1.0483 0.0799 0.0388 1.0000 Uiso R . . . . . H91 H 0.3972 0.8852 0.0667 0.0315 1.0000 Uiso R . . . . . H161 H 0.0679 0.9067 0.0096 0.0504 1.0000 Uiso R . . . . . H162 H 0.1287 0.8894 0.1050 0.0495 1.0000 Uiso R . . . . . H163 H 0.0488 0.8047 0.0923 0.0506 1.0000 Uiso R . . . . . H171 H 0.1513 0.8448 -0.1169 0.0371 1.0000 Uiso R . . . . . H191 H 0.3147 0.7020 -0.2565 0.0695 1.0000 Uiso R . . . . . H193 H 0.3765 0.8083 -0.2673 0.0696 1.0000 Uiso R . . . . . H192 H 0.2419 0.8159 -0.2642 0.0701 1.0000 Uiso R . . . . . H201 H 0.4573 0.6619 -0.1139 0.0407 1.0000 Uiso R . . . . . H221 H 0.5489 0.5935 0.0163 0.0563 1.0000 Uiso R . . . . . H223 H 0.5267 0.6527 0.1009 0.0564 1.0000 Uiso R . . . . . H222 H 0.4737 0.5435 0.1071 0.0578 1.0000 Uiso R . . . . . H251 H 0.2356 0.4150 0.1909 0.0614 1.0000 Uiso R . . . . . H253 H 0.1548 0.5043 0.2282 0.0619 1.0000 Uiso R . . . . . H252 H 0.2303 0.5356 0.1350 0.0615 1.0000 Uiso R . . . . . H261 H 0.3450 0.3415 0.3134 0.0390 1.0000 Uiso R . . . . . H281 H 0.5618 0.5075 0.4004 0.0383 1.0000 Uiso R . . . . . H303 H 0.5955 0.6734 0.3270 0.0469 1.0000 Uiso R . . . . . H302 H 0.4819 0.7531 0.3278 0.0479 1.0000 Uiso R . . . . . H301 H 0.5419 0.7336 0.2319 0.0478 1.0000 Uiso R . . . . . H313 H 0.5751 0.3085 0.4568 0.0716 1.0000 Uiso R . . . . . H312 H 0.4524 0.2903 0.4936 0.0694 1.0000 Uiso R . . . . . H311 H 0.5056 0.2439 0.4125 0.0709 1.0000 Uiso R . . . . . H321 H 0.1017 1.0504 0.1534 0.0418 1.0000 Uiso R . . . . . H331 H 0.1484 1.1954 0.2361 0.0436 1.0000 Uiso R . . . . . H341 H 0.0656 1.1484 0.4086 0.0408 1.0000 Uiso R . . . . . H351 H -0.0377 0.9771 0.4309 0.0407 1.0000 Uiso R . . . . . H361 H -0.0130 0.9171 0.2716 0.0392 1.0000 Uiso R . . . . . H392 H -0.1367 0.4473 0.5578 0.0423 1.0000 Uiso R . . . . . H391 H -0.2565 0.4942 0.5157 0.0408 1.0000 Uiso R . . . . . H401 H -0.0698 0.6211 0.4933 0.0411 1.0000 Uiso R . . . . . H402 H -0.1712 0.6253 0.5730 0.0410 1.0000 Uiso R . . . . . H422 H -0.1172 0.8071 0.4249 0.0482 1.0000 Uiso R . . . . . H421 H -0.2230 0.8128 0.5032 0.0489 1.0000 Uiso R . . . . . H432 H -0.2638 0.9499 0.3717 0.0503 1.0000 Uiso R . . . . . H431 H -0.3515 0.8612 0.3803 0.0493 1.0000 Uiso R . . . . . H451 H -0.2990 1.0020 0.2093 0.0495 1.0000 Uiso R . . . . . H452 H -0.3716 0.9043 0.2126 0.0486 1.0000 Uiso R . . . . . H462 H -0.1574 0.9323 0.1054 0.0511 1.0000 Uiso R . . . . . H461 H -0.2780 0.9661 0.0592 0.0522 1.0000 Uiso R . . . . . H481 H -0.1112 0.8047 -0.0007 0.0489 1.0000 Uiso R . . . . . H482 H -0.2339 0.8438 -0.0394 0.0497 1.0000 Uiso R . . . . . H492 H -0.1734 0.6682 -0.0623 0.0503 1.0000 Uiso R . . . . . H491 H -0.2813 0.6655 0.0130 0.0493 1.0000 Uiso R . . . . . H511 H -0.1171 0.4765 0.0094 0.0497 1.0000 Uiso R . . . . . H512 H -0.2291 0.4820 0.0802 0.0492 1.0000 Uiso R . . . . . H522 H -0.0023 0.4348 0.1419 0.0448 1.0000 Uiso R . . . . . H521 H -0.0848 0.3432 0.1450 0.0462 1.0000 Uiso R . . . . . H542 H -0.0044 0.3654 0.3132 0.0419 1.0000 Uiso R . . . . . H541 H -0.0940 0.2854 0.3061 0.0413 1.0000 Uiso R . . . . . H551 H -0.1156 0.3197 0.4571 0.0413 1.0000 Uiso R . . . . . H552 H -0.2287 0.3707 0.4057 0.0418 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02759(12) 0.02366(11) 0.02549(12) -0.00358(8) -0.00221(8) 0.00212(8) C2 0.0352(8) 0.0268(8) 0.0247(7) -0.0024(6) -0.0039(6) 0.0041(6) C3 0.0239(7) 0.0226(7) 0.0267(7) -0.0036(6) -0.0056(6) 0.0025(6) C4 0.0255(7) 0.0270(8) 0.0379(9) -0.0094(6) -0.0083(6) 0.0024(6) C5 0.0373(9) 0.0361(9) 0.0403(10) -0.0175(8) -0.0136(7) 0.0060(7) C6 0.0436(10) 0.0364(9) 0.0263(8) -0.0070(7) -0.0082(7) 0.0096(8) C7 0.0245(8) 0.0263(8) 0.0525(11) -0.0101(7) -0.0050(7) -0.0037(6) C8 0.0239(7) 0.0269(8) 0.0427(9) 0.0002(7) -0.0017(7) -0.0043(6) C9 0.0227(7) 0.0279(8) 0.0280(8) -0.0027(6) -0.0028(6) -0.0018(6) C10 0.0202(7) 0.0235(7) 0.0251(7) -0.0022(6) -0.0040(5) 0.0011(5) B11 0.0199(7) 0.0244(8) 0.0218(7) -0.0022(6) -0.0028(6) -0.0017(6) C12 0.0252(7) 0.0258(7) 0.0243(7) -0.0012(6) -0.0045(6) -0.0018(6) N13 0.0261(7) 0.0360(8) 0.0363(8) -0.0004(6) -0.0015(6) -0.0049(6) C14 0.0228(7) 0.0246(7) 0.0240(7) -0.0030(6) -0.0026(5) -0.0052(6) C15 0.0268(7) 0.0265(7) 0.0256(7) -0.0022(6) -0.0043(6) -0.0061(6) C16 0.0283(8) 0.0369(9) 0.0316(8) 0.0005(7) -0.0073(7) 0.0034(7) C17 0.0377(9) 0.0290(8) 0.0258(8) -0.0001(6) -0.0096(6) -0.0091(7) C18 0.0498(10) 0.0309(8) 0.0236(8) -0.0055(6) -0.0020(7) -0.0151(7) C19 0.0720(14) 0.0454(11) 0.0263(9) -0.0086(8) -0.0018(9) -0.0179(10) C20 0.0390(9) 0.0325(8) 0.0291(8) -0.0104(7) 0.0057(7) -0.0095(7) C21 0.0274(8) 0.0299(8) 0.0290(8) -0.0082(6) 0.0001(6) -0.0058(6) C22 0.0270(8) 0.0520(11) 0.0362(9) -0.0151(8) 0.0015(7) 0.0045(7) C23 0.0226(7) 0.0250(7) 0.0224(7) -0.0035(6) -0.0018(5) -0.0013(6) C24 0.0293(8) 0.0269(8) 0.0285(8) -0.0042(6) -0.0012(6) -0.0037(6) C25 0.0472(11) 0.0300(9) 0.0490(11) -0.0069(8) -0.0152(9) -0.0114(8) C26 0.0346(9) 0.0239(7) 0.0357(9) -0.0031(6) 0.0036(7) -0.0014(6) C27 0.0305(8) 0.0323(8) 0.0274(8) 0.0025(6) 0.0044(6) 0.0067(7) C28 0.0250(7) 0.0394(9) 0.0256(8) -0.0029(7) -0.0038(6) 0.0051(6) C29 0.0243(7) 0.0303(8) 0.0238(7) -0.0049(6) -0.0031(6) 0.0003(6) C30 0.0247(7) 0.0356(9) 0.0382(9) -0.0095(7) -0.0103(6) -0.0008(6) C31 0.0444(11) 0.0382(10) 0.0407(10) 0.0079(8) 0.0036(8) 0.0110(8) C32 0.0338(8) 0.0373(9) 0.0252(8) 0.0001(7) -0.0021(6) 0.0077(7) C33 0.0357(9) 0.0264(8) 0.0395(9) 0.0018(7) 0.0001(7) 0.0035(7) C34 0.0357(9) 0.0288(8) 0.0359(9) -0.0090(7) -0.0026(7) 0.0071(7) C35 0.0297(8) 0.0366(9) 0.0293(8) -0.0052(7) 0.0023(6) 0.0008(7) C36 0.0284(8) 0.0361(9) 0.0306(8) -0.0065(7) -0.0040(6) 0.0010(7) K37 0.02962(17) 0.02485(16) 0.02488(16) -0.00235(12) -0.00302(12) -0.00190(12) O38 0.0361(6) 0.0291(6) 0.0253(6) -0.0006(4) 0.0031(5) -0.0027(5) C39 0.0317(8) 0.0444(10) 0.0218(7) 0.0005(7) 0.0013(6) 0.0016(7) C40 0.0285(8) 0.0490(10) 0.0243(8) -0.0075(7) -0.0041(6) 0.0004(7) O41 0.0297(6) 0.0335(6) 0.0312(6) -0.0090(5) -0.0061(5) -0.0013(5) C42 0.0440(10) 0.0401(10) 0.0430(10) -0.0187(8) -0.0042(8) -0.0055(8) C43 0.0413(10) 0.0317(9) 0.0549(12) -0.0183(8) -0.0017(9) -0.0002(8) O44 0.0309(6) 0.0288(6) 0.0438(7) -0.0058(5) -0.0069(5) 0.0008(5) C45 0.0352(9) 0.0235(8) 0.0588(12) 0.0007(8) -0.0110(8) 0.0003(7) C46 0.0453(10) 0.0269(9) 0.0511(11) 0.0098(8) -0.0127(9) -0.0066(8) O47 0.0447(7) 0.0338(6) 0.0318(6) 0.0042(5) -0.0068(5) -0.0099(5) C48 0.0373(9) 0.0540(11) 0.0275(8) 0.0081(8) -0.0078(7) -0.0124(8) C49 0.0362(9) 0.0627(12) 0.0267(8) -0.0062(8) -0.0060(7) -0.0133(9) O50 0.0428(7) 0.0429(7) 0.0281(6) -0.0047(5) -0.0069(5) -0.0151(6) C51 0.0490(11) 0.0505(11) 0.0336(9) -0.0175(8) 0.0018(8) -0.0188(9) C52 0.0416(10) 0.0393(10) 0.0385(10) -0.0186(8) 0.0063(8) -0.0087(8) O53 0.0352(6) 0.0292(6) 0.0308(6) -0.0074(5) 0.0011(5) 0.0005(5) C54 0.0354(9) 0.0258(8) 0.0426(10) -0.0058(7) -0.0044(7) 0.0019(7) C55 0.0347(9) 0.0263(8) 0.0370(9) 0.0056(7) -0.0017(7) -0.0028(7) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.6197(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . C2 . 2.0641(16) yes Fe1 . C3 . 2.1084(15) yes Fe1 . C4 . 2.0822(17) yes Fe1 . C5 . 2.0375(18) yes Fe1 . C6 . 2.0515(17) yes Fe1 . C32 . 2.0446(17) yes Fe1 . C33 . 2.0371(17) yes Fe1 . C34 . 2.0340(16) yes Fe1 . C35 . 2.0488(17) yes Fe1 . C36 . 2.0598(17) yes C2 . C3 . 1.440(2) yes C2 . C6 . 1.425(2) yes C2 . H21 . 0.970 no C3 . C4 . 1.454(2) yes C3 . C10 . 1.451(2) yes C4 . C5 . 1.438(2) yes C4 . C7 . 1.427(3) yes C5 . C6 . 1.418(3) yes C5 . H51 . 0.978 no C6 . H61 . 0.987 no C7 . C8 . 1.354(3) yes C7 . H71 . 0.936 no C8 . C9 . 1.432(2) yes C8 . H81 . 0.940 no C9 . C10 . 1.379(2) yes C9 . H91 . 0.943 no C10 . B11 . 1.649(2) yes B11 . C12 . 1.633(2) yes B11 . C14 . 1.661(2) yes B11 . C23 . 1.676(2) yes C12 . N13 . 1.153(2) yes C14 . C15 . 1.415(2) yes C14 . C21 . 1.422(2) yes C15 . C16 . 1.511(2) yes C15 . C17 . 1.406(2) yes C16 . H161 . 0.969 no C16 . H162 . 0.979 no C16 . H163 . 0.975 no C17 . C18 . 1.385(3) yes C17 . H171 . 0.944 no C18 . C19 . 1.515(2) yes C18 . C20 . 1.384(3) yes C19 . H191 . 0.966 no C19 . H193 . 0.966 no C19 . H192 . 0.972 no C20 . C21 . 1.402(2) yes C20 . H201 . 0.968 no C21 . C22 . 1.513(2) yes C22 . H221 . 0.963 no C22 . H223 . 0.966 no C22 . H222 . 0.977 no C23 . C24 . 1.421(2) yes C23 . C29 . 1.419(2) yes C24 . C25 . 1.513(2) yes C24 . C26 . 1.399(2) yes C25 . H251 . 0.961 no C25 . H253 . 0.983 no C25 . H252 . 0.939 no C26 . C27 . 1.388(3) yes C26 . H261 . 0.937 no C27 . C28 . 1.383(3) yes C27 . C31 . 1.505(2) yes C28 . C29 . 1.402(2) yes C28 . H281 . 0.945 no C29 . C30 . 1.513(2) yes C30 . H303 . 0.973 no C30 . H302 . 0.971 no C30 . H301 . 0.956 no C31 . H313 . 0.930 no C31 . H312 . 0.931 no C31 . H311 . 0.932 no C32 . C33 . 1.418(3) yes C32 . C36 . 1.420(2) yes C32 . H321 . 0.967 no C33 . C34 . 1.424(3) yes C33 . H331 . 0.966 no C34 . C35 . 1.419(3) yes C34 . H341 . 0.977 no C35 . C36 . 1.424(2) yes C35 . H351 . 0.974 no C36 . H361 . 0.968 no O38 . C39 . 1.432(2) yes O38 . C55 . 1.418(2) yes C39 . C40 . 1.494(3) yes C39 . H392 . 0.970 no C39 . H391 . 0.980 no C40 . O41 . 1.430(2) yes C40 . H401 . 0.967 no C40 . H402 . 0.985 no O41 . C42 . 1.417(2) yes C42 . C43 . 1.503(3) yes C42 . H422 . 0.991 no C42 . H421 . 0.972 no C43 . O44 . 1.415(2) yes C43 . H432 . 0.982 no C43 . H431 . 0.981 no O44 . C45 . 1.429(2) yes C45 . C46 . 1.490(3) yes C45 . H451 . 0.975 no C45 . H452 . 0.975 no C46 . O47 . 1.425(2) yes C46 . H462 . 0.981 no C46 . H461 . 0.981 no O47 . C48 . 1.423(2) yes C48 . C49 . 1.493(3) yes C48 . H481 . 0.961 no C48 . H482 . 0.981 no C49 . O50 . 1.420(2) yes C49 . H492 . 0.986 no C49 . H491 . 0.979 no O50 . C51 . 1.429(2) yes C51 . C52 . 1.490(3) yes C51 . H511 . 0.977 no C51 . H512 . 0.977 no C52 . O53 . 1.428(2) yes C52 . H522 . 0.991 no C52 . H521 . 0.977 no O53 . C54 . 1.420(2) yes C54 . C55 . 1.495(3) yes C54 . H542 . 0.983 no C54 . H541 . 0.974 no C55 . H551 . 0.972 no C55 . H552 . 0.971 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 . Fe1 . C3 . 40.36(6) yes C2 . Fe1 . C4 . 68.23(7) yes C3 . Fe1 . C4 . 40.58(6) yes C2 . Fe1 . C5 . 68.58(7) yes C3 . Fe1 . C5 . 68.53(6) yes C4 . Fe1 . C5 . 40.84(7) yes C2 . Fe1 . C6 . 40.52(7) yes C3 . Fe1 . C6 . 67.90(6) yes C4 . Fe1 . C6 . 68.08(7) yes C5 . Fe1 . C6 . 40.59(8) yes C2 . Fe1 . C32 . 132.88(7) yes C3 . Fe1 . C32 . 108.76(7) yes C4 . Fe1 . C32 . 113.95(7) yes C5 . Fe1 . C32 . 145.23(8) yes C6 . Fe1 . C32 . 172.76(8) yes C2 . Fe1 . C33 . 170.98(7) yes C3 . Fe1 . C33 . 131.30(7) yes C4 . Fe1 . C33 . 107.32(7) yes C5 . Fe1 . C33 . 113.64(8) yes C6 . Fe1 . C33 . 146.34(8) yes C2 . Fe1 . C34 . 147.78(7) yes C3 . Fe1 . C34 . 170.68(7) yes C4 . Fe1 . C34 . 131.48(7) yes C5 . Fe1 . C34 . 108.34(7) yes C6 . Fe1 . C34 . 115.90(7) yes C2 . Fe1 . C35 . 116.93(7) yes C3 . Fe1 . C35 . 147.59(7) yes C4 . Fe1 . C35 . 171.54(7) yes C5 . Fe1 . C35 . 133.06(7) yes C6 . Fe1 . C35 . 110.97(7) yes C2 . Fe1 . C36 . 110.42(7) yes C3 . Fe1 . C36 . 115.59(7) yes C4 . Fe1 . C36 . 145.93(7) yes C5 . Fe1 . C36 . 172.91(7) yes C6 . Fe1 . C36 . 134.26(8) yes C32 . Fe1 . C33 . 40.66(8) yes C32 . Fe1 . C34 . 68.44(7) yes C33 . Fe1 . C34 . 40.93(7) yes C32 . Fe1 . C35 . 68.11(7) yes C33 . Fe1 . C35 . 68.51(7) yes C34 . Fe1 . C35 . 40.69(7) yes C32 . Fe1 . C36 . 40.49(7) yes C33 . Fe1 . C36 . 68.52(8) yes C34 . Fe1 . C36 . 68.52(7) yes C35 . Fe1 . C36 . 40.56(7) yes Fe1 . C2 . C3 . 71.47(9) yes Fe1 . C2 . C6 . 69.26(9) yes C3 . C2 . C6 . 108.37(15) yes Fe1 . C2 . H21 . 125.8 no C3 . C2 . H21 . 124.7 no C6 . C2 . H21 . 126.9 no Fe1 . C3 . C2 . 68.17(9) yes Fe1 . C3 . C4 . 68.74(9) yes C2 . C3 . C4 . 106.96(14) yes Fe1 . C3 . C10 . 130.52(11) yes C2 . C3 . C10 . 131.26(15) yes C4 . C3 . C10 . 121.70(14) yes C3 . C4 . Fe1 . 70.68(9) yes C3 . C4 . C5 . 107.70(15) yes Fe1 . C4 . C5 . 67.91(10) yes C3 . C4 . C7 . 119.69(15) yes Fe1 . C4 . C7 . 125.06(12) yes C5 . C4 . C7 . 132.57(16) yes C4 . C5 . Fe1 . 71.25(10) yes C4 . C5 . C6 . 108.21(15) yes Fe1 . C5 . C6 . 70.24(10) yes C4 . C5 . H51 . 124.6 no Fe1 . C5 . H51 . 124.2 no C6 . C5 . H51 . 127.2 no C2 . C6 . C5 . 108.70(16) yes C2 . C6 . Fe1 . 70.22(9) yes C5 . C6 . Fe1 . 69.17(10) yes C2 . C6 . H61 . 124.8 no C5 . C6 . H61 . 126.4 no Fe1 . C6 . H61 . 123.8 no C4 . C7 . C8 . 117.96(15) yes C4 . C7 . H71 . 120.3 no C8 . C7 . H71 . 121.7 no C7 . C8 . C9 . 122.01(16) yes C7 . C8 . H81 . 119.5 no C9 . C8 . H81 . 118.5 no C8 . C9 . C10 . 124.22(15) yes C8 . C9 . H91 . 118.0 no C10 . C9 . H91 . 117.8 no C3 . C10 . C9 . 114.22(14) yes C3 . C10 . B11 . 123.76(13) yes C9 . C10 . B11 . 121.96(14) yes C10 . B11 . C12 . 106.26(12) yes C10 . B11 . C14 . 107.11(12) yes C12 . B11 . C14 . 110.13(12) yes C10 . B11 . C23 . 116.59(12) yes C12 . B11 . C23 . 100.26(11) yes C14 . B11 . C23 . 115.84(12) yes B11 . C12 . N13 . 176.20(16) yes B11 . C14 . C15 . 120.89(13) yes B11 . C14 . C21 . 122.97(13) yes C15 . C14 . C21 . 115.77(14) yes C14 . C15 . C16 . 122.66(14) yes C14 . C15 . C17 . 121.53(15) yes C16 . C15 . C17 . 115.73(14) yes C15 . C16 . H161 . 109.9 no C15 . C16 . H162 . 111.6 no H161 . C16 . H162 . 108.7 no C15 . C16 . H163 . 111.3 no H161 . C16 . H163 . 107.6 no H162 . C16 . H163 . 107.6 no C15 . C17 . C18 . 121.88(16) yes C15 . C17 . H171 . 119.2 no C18 . C17 . H171 . 118.9 no C17 . C18 . C19 . 121.64(18) yes C17 . C18 . C20 . 117.33(15) yes C19 . C18 . C20 . 121.02(18) yes C18 . C19 . H191 . 110.0 no C18 . C19 . H193 . 109.7 no H191 . C19 . H193 . 110.6 no C18 . C19 . H192 . 110.1 no H191 . C19 . H192 . 107.7 no H193 . C19 . H192 . 108.7 no C18 . C20 . C21 . 122.34(16) yes C18 . C20 . H201 . 118.2 no C21 . C20 . H201 . 119.5 no C14 . C21 . C20 . 121.13(15) yes C14 . C21 . C22 . 123.18(15) yes C20 . C21 . C22 . 115.66(15) yes C21 . C22 . H221 . 109.6 no C21 . C22 . H223 . 110.7 no H221 . C22 . H223 . 108.7 no C21 . C22 . H222 . 111.9 no H221 . C22 . H222 . 107.4 no H223 . C22 . H222 . 108.5 no B11 . C23 . C24 . 118.72(13) yes B11 . C23 . C29 . 125.90(14) yes C24 . C23 . C29 . 115.36(14) yes C23 . C24 . C25 . 123.08(15) yes C23 . C24 . C26 . 121.77(15) yes C25 . C24 . C26 . 115.11(15) yes C24 . C25 . H251 . 110.6 no C24 . C25 . H253 . 110.0 no H251 . C25 . H253 . 104.8 no C24 . C25 . H252 . 115.0 no H251 . C25 . H252 . 109.4 no H253 . C25 . H252 . 106.4 no C24 . C26 . C27 . 122.08(16) yes C24 . C26 . H261 . 119.2 no C27 . C26 . H261 . 118.7 no C26 . C27 . C28 . 116.55(15) yes C26 . C27 . C31 . 121.28(18) yes C28 . C27 . C31 . 122.17(18) yes C27 . C28 . C29 . 122.98(16) yes C27 . C28 . H281 . 119.1 no C29 . C28 . H281 . 117.9 no C23 . C29 . C28 . 120.90(15) yes C23 . C29 . C30 . 123.90(14) yes C28 . C29 . C30 . 115.06(14) yes C29 . C30 . H303 . 109.8 no C29 . C30 . H302 . 112.0 no H303 . C30 . H302 . 107.5 no C29 . C30 . H301 . 111.8 no H303 . C30 . H301 . 108.3 no H302 . C30 . H301 . 107.4 no C27 . C31 . H313 . 111.5 no C27 . C31 . H312 . 110.4 no H313 . C31 . H312 . 109.3 no C27 . C31 . H311 . 110.7 no H313 . C31 . H311 . 109.2 no H312 . C31 . H311 . 105.6 no Fe1 . C32 . C33 . 69.39(10) yes Fe1 . C32 . C36 . 70.33(9) yes C33 . C32 . C36 . 108.68(15) yes Fe1 . C32 . H321 . 122.5 no C33 . C32 . H321 . 126.3 no C36 . C32 . H321 . 124.9 no C32 . C33 . Fe1 . 69.96(10) yes C32 . C33 . C34 . 107.65(16) yes Fe1 . C33 . C34 . 69.42(10) yes C32 . C33 . H331 . 126.7 no Fe1 . C33 . H331 . 124.6 no C34 . C33 . H331 . 125.7 no C33 . C34 . Fe1 . 69.65(10) yes C33 . C34 . C35 . 108.00(16) yes Fe1 . C34 . C35 . 70.22(10) yes C33 . C34 . H341 . 125.5 no Fe1 . C34 . H341 . 124.3 no C35 . C34 . H341 . 126.5 no C34 . C35 . Fe1 . 69.10(10) yes C34 . C35 . C36 . 108.29(15) yes Fe1 . C35 . C36 . 70.14(10) yes C34 . C35 . H351 . 126.1 no Fe1 . C35 . H351 . 126.0 no C36 . C35 . H351 . 125.6 no C35 . C36 . C32 . 107.38(16) yes C35 . C36 . Fe1 . 69.31(10) yes C32 . C36 . Fe1 . 69.18(10) yes C35 . C36 . H361 . 127.3 no C32 . C36 . H361 . 125.3 no Fe1 . C36 . H361 . 124.5 no C39 . O38 . C55 . 112.75(13) yes O38 . C39 . C40 . 107.25(14) yes O38 . C39 . H392 . 110.0 no C40 . C39 . H392 . 109.5 no O38 . C39 . H391 . 110.4 no C40 . C39 . H391 . 111.0 no H392 . C39 . H391 . 108.7 no C39 . C40 . O41 . 108.62(14) yes C39 . C40 . H401 . 111.6 no O41 . C40 . H401 . 109.0 no C39 . C40 . H402 . 109.5 no O41 . C40 . H402 . 109.9 no H401 . C40 . H402 . 108.1 no C40 . O41 . C42 . 111.37(14) yes O41 . C42 . C43 . 108.75(15) yes O41 . C42 . H422 . 109.2 no C43 . C42 . H422 . 110.0 no O41 . C42 . H421 . 109.9 no C43 . C42 . H421 . 109.1 no H422 . C42 . H421 . 109.7 no C42 . C43 . O44 . 108.51(15) yes C42 . C43 . H432 . 108.7 no O44 . C43 . H432 . 109.2 no C42 . C43 . H431 . 110.5 no O44 . C43 . H431 . 110.2 no H432 . C43 . H431 . 109.8 no C43 . O44 . C45 . 112.15(14) yes O44 . C45 . C46 . 108.80(15) yes O44 . C45 . H451 . 108.5 no C46 . C45 . H451 . 109.9 no O44 . C45 . H452 . 108.7 no C46 . C45 . H452 . 111.8 no H451 . C45 . H452 . 109.1 no C45 . C46 . O47 . 108.95(15) yes C45 . C46 . H462 . 109.6 no O47 . C46 . H462 . 110.0 no C45 . C46 . H461 . 109.1 no O47 . C46 . H461 . 110.0 no H462 . C46 . H461 . 109.2 no C46 . O47 . C48 . 111.54(14) yes O47 . C48 . C49 . 109.04(15) yes O47 . C48 . H481 . 111.0 no C49 . C48 . H481 . 109.4 no O47 . C48 . H482 . 109.1 no C49 . C48 . H482 . 109.3 no H481 . C48 . H482 . 109.0 no C48 . C49 . O50 . 109.65(15) yes C48 . C49 . H492 . 110.6 no O50 . C49 . H492 . 109.4 no C48 . C49 . H491 . 109.2 no O50 . C49 . H491 . 110.1 no H492 . C49 . H491 . 107.9 no C49 . O50 . C51 . 111.82(14) yes O50 . C51 . C52 . 108.66(15) yes O50 . C51 . H511 . 109.7 no C52 . C51 . H511 . 109.3 no O50 . C51 . H512 . 109.9 no C52 . C51 . H512 . 110.3 no H511 . C51 . H512 . 109.0 no C51 . C52 . O53 . 108.83(15) yes C51 . C52 . H522 . 110.6 no O53 . C52 . H522 . 108.9 no C51 . C52 . H521 . 109.7 no O53 . C52 . H521 . 109.4 no H522 . C52 . H521 . 109.3 no C52 . O53 . C54 . 111.15(13) yes O53 . C54 . C55 . 109.31(14) yes O53 . C54 . H542 . 110.0 no C55 . C54 . H542 . 110.1 no O53 . C54 . H541 . 108.6 no C55 . C54 . H541 . 110.2 no H542 . C54 . H541 . 108.6 no C54 . C55 . O38 . 108.45(14) yes C54 . C55 . H551 . 108.5 no O38 . C55 . H551 . 109.3 no C54 . C55 . H552 . 110.3 no O38 . C55 . H552 . 111.1 no H551 . C55 . H552 . 109.1 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C25 . H252 . C14 . 131.29(6) 0.939 2.556 3.253(3) yes C30 . H302 . C3 . 129.87(5) 0.971 2.457 3.169(3) yes _iucr_refine_instruction_details_constraints ; # # Punched on 23/05/13 at 10:23:00 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 16,X'S) H ( 161,X'S) H ( 162,X'S) H ( 163,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 19,X'S) H ( 191,X'S) H ( 193,X'S) H ( 192,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 22,X'S) H ( 221,X'S) H ( 223,X'S) H ( 222,X'S) RIDE C ( 25,X'S) H ( 251,X'S) H ( 253,X'S) H ( 252,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 30,X'S) H ( 303,X'S) H ( 302,X'S) H ( 301,X'S) RIDE C ( 31,X'S) H ( 313,X'S) H ( 312,X'S) H ( 311,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 36,X'S) H ( 361,X'S) RIDE C ( 39,X'S) H ( 392,X'S) H ( 391,X'S) RIDE C ( 40,X'S) H ( 401,X'S) H ( 402,X'S) RIDE C ( 42,X'S) H ( 422,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 432,X'S) H ( 431,X'S) RIDE C ( 45,X'S) H ( 451,X'S) H ( 452,X'S) RIDE C ( 46,X'S) H ( 462,X'S) H ( 461,X'S) RIDE C ( 48,X'S) H ( 481,X'S) H ( 482,X'S) RIDE C ( 49,X'S) H ( 492,X'S) H ( 491,X'S) RIDE C ( 51,X'S) H ( 511,X'S) H ( 512,X'S) RIDE C ( 52,X'S) H ( 522,X'S) H ( 521,X'S) RIDE C ( 54,X'S) H ( 542,X'S) H ( 541,X'S) RIDE C ( 55,X'S) H ( 551,X'S) H ( 552,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 23/05/13 at 10:23:00 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _database_code_depnum_ccdc_archive 'CCDC 940846'