Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Kohtaro Osakada' _publ_contact_author_address ; Chemical Resources Lab R1-3 Tokyo Institute of Technology Yokohama 226-8503 JAPAN ; _publ_contact_author_email KOSAKADA@RES.TITECH.AC.JP _publ_section_title ; Ferrocene-Containing [2]- and [3]Rotaxanes. Preparation via End-Capping Cross-Metathesis Reaction and Their Electrochmical Properties ; loop_ _publ_author_name 'Kohtaro Osakada' 'Yuji Suzaki' data_FcCH=NCH2C6H4OCH2CH2CH=CH2 _database_code_depnum_ccdc_archive 'CCDC 637664' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C22 H23 Fe N O ' _chemical_formula_moiety 'C22 H23 Fe N O ' _chemical_formula_weight 373.28 _chemical_melting_point ? _chemical_absolute_configuration ad #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,-Z #------------------------------------------------------------------------------ _cell_length_a 19.257(3) _cell_length_b 8.2868(14) _cell_length_c 5.8376(7) _cell_angle_alpha 90.0000 _cell_angle_beta 95.480(12) _cell_angle_gamma 90.0000 _cell_volume 927.3(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.0 _cell_measurement_theta_max 16.9 _cell_measurement_temperature 298.1 #------------------------------------------------------------------------------ _exptl_crystal_description prismatic _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_meas 4.000 _exptl_crystal_density_method ? _exptl_crystal_F_000 392.00 _exptl_absorpt_coefficient_mu 0.821 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.792 _exptl_absorpt_correction_T_max 0.884 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 2401 _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_standards_number 3 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 1.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2278 _reflns_number_gt 1730 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0739 _refine_ls_wR_factor_ref 0.1071 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 1894 _refine_ls_number_parameters 250 _refine_ls_goodness_of_fit_ref 1.305 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]' _refine_ls_shift/su_max 0.0117 _refine_diff_density_max 2.05 _refine_diff_density_min -1.73 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 0 Friedel Pairs' _refine_ls_abs_structure_Flack -0.08(19) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Fe Fe 0.346 0.844 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Fe(1) Fe 0.88638(8) 0.1419(8) -0.3123(2) 0.0425(3) Uani 1.00 1 d . . . O(1) O 0.5567(6) 0.3557(13) 0.5926(19) 0.082(3) Uani 1.00 1 d . . . N(1) N 0.8297(5) 0.4974(13) 0.0875(15) 0.050(2) Uani 1.00 1 d . . . C(1) C 0.3747(13) 0.462(3) 1.061(4) 0.133(10) Uani 1.00 1 d . . . C(2) C 0.4344(11) 0.421(2) 1.040(4) 0.113(8) Uani 1.00 1 d . . . C(3) C 0.4668(11) 0.350(2) 0.843(3) 0.108(7) Uani 1.00 1 d . . . C(4) C 0.5222(8) 0.449(2) 0.756(2) 0.077(5) Uani 1.00 1 d . . . C(5) C 0.6104(7) 0.4274(18) 0.495(2) 0.065(4) Uani 1.00 1 d . . . C(6) C 0.6429(7) 0.5709(17) 0.556(2) 0.064(4) Uani 1.00 1 d . . . C(7) C 0.6965(6) 0.630(2) 0.441(2) 0.062(3) Uani 1.00 1 d . . . C(8) C 0.7199(6) 0.5485(15) 0.2567(19) 0.046(3) Uani 1.00 1 d . . . C(9) C 0.6866(7) 0.4023(18) 0.198(2) 0.063(4) Uani 1.00 1 d . . . C(10) C 0.6343(8) 0.3397(18) 0.313(2) 0.067(4) Uani 1.00 1 d . . . C(11) C 0.7768(7) 0.6152(17) 0.124(2) 0.063(4) Uani 1.00 1 d . . . C(12) C 0.8439(6) 0.4752(15) -0.115(2) 0.049(3) Uani 1.00 1 d . . . C(13) C 0.9010(6) 0.3691(15) -0.1701(17) 0.046(3) Uani 1.00 1 d . . . C(14) C 0.9276(6) 0.3568(16) -0.3896(19) 0.048(3) Uani 1.00 1 d . . . C(15) C 0.9788(7) 0.2364(17) -0.378(2) 0.057(3) Uani 1.00 1 d . . . C(16) C 0.9832(6) 0.1721(19) -0.150(2) 0.058(4) Uani 1.00 1 d . . . C(17) C 0.9343(5) 0.2474(14) -0.0278(17) 0.043(3) Uani 1.00 1 d . . . C(18) C 0.7817(7) 0.1031(18) -0.370(2) 0.062(4) Uani 1.00 1 d . . . C(19) C 0.8160(5) 0.0908(17) -0.575(2) 0.057(4) Uani 1.00 1 d . . . C(20) C 0.8644(8) -0.0300(18) -0.549(2) 0.067(4) Uani 1.00 1 d . . . C(21) C 0.8624(10) -0.0947(19) -0.325(2) 0.077(5) Uani 1.00 1 d . . . C(22) C 0.8134(7) -0.015(2) -0.215(2) 0.066(4) Uani 1.00 1 d . . . H(1) H 0.3397 0.4552 0.9349 0.165 Uiso 1.00 1 c R . . H(2) H 0.3633 0.5017 1.2052 0.165 Uiso 1.00 1 c R . . H(3) H 0.4659 0.4364 1.1733 0.141 Uiso 1.00 1 c R . . H(4) H 0.4314 0.3311 0.7208 0.133 Uiso 1.00 1 c R . . H(5) H 0.4873 0.2497 0.8917 0.133 Uiso 1.00 1 c R . . H(6) H 0.5015 0.5413 0.6798 0.094 Uiso 1.00 1 c R . . H(7) H 0.5547 0.4833 0.8791 0.094 Uiso 1.00 1 c R . . H(8) H 0.6278 0.6306 0.6815 0.078 Uiso 1.00 1 c R . . H(9) H 0.7179 0.7294 0.4897 0.074 Uiso 1.00 1 c R . . H(10) H 0.7015 0.3431 0.0723 0.076 Uiso 1.00 1 c R . . H(11) H 0.6141 0.2383 0.2697 0.082 Uiso 1.00 1 c R . . H(12) H 0.7564 0.6513 -0.0217 0.077 Uiso 1.00 1 c R . . H(13) H 0.7979 0.7039 0.2070 0.077 Uiso 1.00 1 c R . . H(14) H 0.8166 0.5285 -0.2362 0.058 Uiso 1.00 1 c R . . H(15) H 0.9134 0.4214 -0.5202 0.058 Uiso 1.00 1 c R . . H(16) H 1.0049 0.2041 -0.5008 0.070 Uiso 1.00 1 c R . . H(17) H 1.0130 0.0863 -0.0952 0.068 Uiso 1.00 1 c R . . H(18) H 0.9247 0.2241 0.1254 0.050 Uiso 1.00 1 c R . . H(19) H 0.7449 0.1749 -0.3429 0.076 Uiso 1.00 1 c R . . H(20) H 0.8058 0.1537 -0.7096 0.066 Uiso 1.00 1 c R . . H(21) H 0.8936 -0.0648 -0.6620 0.082 Uiso 1.00 1 c R . . H(22) H 0.8913 -0.1794 -0.2612 0.094 Uiso 1.00 1 c R . . H(23) H 0.8022 -0.0344 -0.0624 0.079 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe(1) 0.0452(7) 0.0444(7) 0.0392(6) -0.0073(10) 0.0102(5) 0.0024(10) O(1) 0.088(7) 0.065(7) 0.100(7) -0.010(6) 0.041(6) -0.009(6) N(1) 0.043(5) 0.057(6) 0.048(5) -0.003(5) 0.003(4) -0.008(5) C(1) 0.14(2) 0.118(19) 0.16(2) 0.018(17) 0.082(17) 0.034(17) C(2) 0.104(15) 0.083(13) 0.17(2) -0.000(12) 0.080(16) 0.019(14) C(3) 0.131(17) 0.088(14) 0.114(14) -0.023(13) 0.059(13) -0.003(12) C(4) 0.088(11) 0.064(9) 0.084(10) -0.008(8) 0.035(9) -0.008(8) C(5) 0.063(9) 0.057(8) 0.078(9) 0.002(7) 0.021(7) 0.006(7) C(6) 0.060(8) 0.064(8) 0.070(8) 0.010(7) 0.019(7) -0.012(7) C(7) 0.066(7) 0.053(8) 0.066(6) -0.005(9) 0.011(5) -0.008(9) C(8) 0.042(6) 0.047(7) 0.048(6) 0.002(5) -0.003(5) -0.003(5) C(9) 0.064(9) 0.061(9) 0.064(7) -0.001(7) 0.014(6) -0.008(7) C(10) 0.069(9) 0.051(8) 0.085(9) -0.009(6) 0.019(8) -0.016(7) C(11) 0.087(9) 0.039(10) 0.066(7) -0.004(6) 0.027(7) -0.004(6) C(12) 0.042(6) 0.049(7) 0.055(6) -0.014(5) -0.002(5) 0.007(5) C(13) 0.062(8) 0.046(7) 0.029(4) -0.011(6) -0.005(4) 0.002(4) C(14) 0.047(7) 0.051(7) 0.046(6) -0.018(5) 0.003(5) 0.005(5) C(15) 0.057(8) 0.063(8) 0.055(7) -0.016(7) 0.025(6) -0.005(6) C(16) 0.045(6) 0.058(11) 0.068(6) -0.003(6) -0.017(5) -0.012(7) C(17) 0.038(6) 0.055(7) 0.034(4) -0.024(5) -0.014(4) -0.019(5) C(18) 0.052(7) 0.080(14) 0.057(6) -0.008(6) 0.013(5) -0.013(7) C(19) 0.029(5) 0.086(12) 0.051(6) -0.013(5) -0.018(4) -0.022(6) C(20) 0.091(11) 0.060(9) 0.055(7) -0.030(8) 0.024(7) -0.032(6) C(21) 0.109(13) 0.043(8) 0.082(10) -0.010(8) 0.019(10) 0.001(7) C(22) 0.063(9) 0.086(11) 0.049(6) -0.034(8) 0.010(6) 0.006(7) #============================================================================== _computing_data_collection WinAFC _computing_cell_refinement WinAFC _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.7.0' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Fe(1) C(13) 2.066(13) No . . Fe(1) C(14) 2.018(14) No . . Fe(1) C(15) 2.015(14) No . . Fe(1) C(16) 2.025(12) No . . Fe(1) C(17) 2.020(11) No . . Fe(1) C(18) 2.038(13) No . . Fe(1) C(19) 1.991(11) No . . Fe(1) C(20) 2.003(15) No . . Fe(1) C(21) 2.014(17) No . . Fe(1) C(22) 2.037(16) No . . O(1) C(4) 1.44(2) No . . O(1) C(5) 1.364(19) No . . N(1) C(11) 1.441(18) No . . N(1) C(12) 1.251(15) No . . C(1) C(2) 1.22(3) No . . C(2) C(3) 1.48(3) No . . C(3) C(4) 1.48(2) No . . C(5) C(6) 1.38(2) No . . C(5) C(10) 1.40(2) No . . C(6) C(7) 1.38(2) No . . C(7) C(8) 1.384(19) No . . C(8) C(9) 1.397(19) No . . C(8) C(11) 1.507(19) No . . C(9) C(10) 1.37(2) No . . C(12) C(13) 1.468(18) No . . C(13) C(14) 1.428(16) No . . C(13) C(17) 1.420(16) No . . C(14) C(15) 1.401(18) No . . C(15) C(16) 1.429(18) No . . C(16) C(17) 1.385(17) No . . C(18) C(19) 1.422(18) No . . C(18) C(22) 1.43(2) No . . C(19) C(20) 1.37(2) No . . C(20) C(21) 1.42(2) No . . C(21) C(22) 1.36(2) No . . C(1) H(1) 0.950 No . . C(1) H(2) 0.950 No . . C(2) H(3) 0.950 No . . C(3) H(4) 0.950 No . . C(3) H(5) 0.950 No . . C(4) H(6) 0.950 No . . C(4) H(7) 0.950 No . . C(6) H(8) 0.950 No . . C(7) H(9) 0.950 No . . C(9) H(10) 0.950 No . . C(10) H(11) 0.950 No . . C(11) H(12) 0.950 No . . C(11) H(13) 0.950 No . . C(12) H(14) 0.950 No . . C(14) H(15) 0.950 No . . C(15) H(16) 0.950 No . . C(16) H(17) 0.950 No . . C(17) H(18) 0.950 No . . C(18) H(19) 0.950 No . . C(19) H(20) 0.950 No . . C(20) H(21) 0.950 No . . C(21) H(22) 0.950 No . . C(22) H(23) 0.950 No . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C(13) Fe(1) C(14) 40.9(4) No . . . C(13) Fe(1) C(15) 68.5(5) No . . . C(13) Fe(1) C(16) 67.4(5) No . . . C(13) Fe(1) C(17) 40.7(4) No . . . C(13) Fe(1) C(18) 107.8(6) No . . . C(13) Fe(1) C(19) 124.0(5) No . . . C(13) Fe(1) C(20) 159.6(5) No . . . C(13) Fe(1) C(21) 157.6(5) No . . . C(13) Fe(1) C(22) 122.9(5) No . . . C(14) Fe(1) C(15) 40.6(5) No . . . C(14) Fe(1) C(16) 68.4(5) No . . . C(14) Fe(1) C(17) 69.1(5) No . . . C(14) Fe(1) C(18) 120.4(6) No . . . C(14) Fe(1) C(19) 105.6(5) No . . . C(14) Fe(1) C(20) 122.3(5) No . . . C(14) Fe(1) C(21) 160.7(6) No . . . C(14) Fe(1) C(22) 157.5(6) No . . . C(15) Fe(1) C(16) 41.4(5) No . . . C(15) Fe(1) C(17) 69.3(5) No . . . C(15) Fe(1) C(18) 155.2(5) No . . . C(15) Fe(1) C(19) 118.9(5) No . . . C(15) Fe(1) C(20) 106.0(6) No . . . C(15) Fe(1) C(21) 125.0(7) No . . . C(15) Fe(1) C(22) 161.3(6) No . . . C(16) Fe(1) C(17) 40.1(5) No . . . C(16) Fe(1) C(18) 161.8(5) No . . . C(16) Fe(1) C(19) 156.1(5) No . . . C(16) Fe(1) C(20) 122.3(6) No . . . C(16) Fe(1) C(21) 109.6(7) No . . . C(16) Fe(1) C(22) 125.3(5) No . . . C(17) Fe(1) C(18) 124.9(5) No . . . C(17) Fe(1) C(19) 161.5(5) No . . . C(17) Fe(1) C(20) 157.7(6) No . . . C(17) Fe(1) C(21) 122.5(6) No . . . C(17) Fe(1) C(22) 108.7(5) No . . . C(18) Fe(1) C(19) 41.3(5) No . . . C(18) Fe(1) C(20) 68.5(6) No . . . C(18) Fe(1) C(21) 67.7(7) No . . . C(18) Fe(1) C(22) 41.2(5) No . . . C(19) Fe(1) C(20) 40.0(6) No . . . C(19) Fe(1) C(21) 68.1(6) No . . . C(19) Fe(1) C(22) 69.0(5) No . . . C(20) Fe(1) C(21) 41.3(6) No . . . C(20) Fe(1) C(22) 68.4(6) No . . . C(21) Fe(1) C(22) 39.3(7) No . . . C(4) O(1) C(5) 117.2(12) No . . . C(11) N(1) C(12) 117.4(10) No . . . C(1) C(2) C(3) 131(2) No . . . C(2) C(3) C(4) 114.6(17) No . . . O(1) C(4) C(3) 108.6(14) No . . . O(1) C(5) C(6) 127.6(14) No . . . O(1) C(5) C(10) 114.1(13) No . . . C(6) C(5) C(10) 118.3(14) No . . . C(5) C(6) C(7) 121.6(14) No . . . C(6) C(7) C(8) 121.4(16) No . . . C(7) C(8) C(9) 116.1(12) No . . . C(7) C(8) C(11) 121.8(12) No . . . C(9) C(8) C(11) 122.1(11) No . . . C(8) C(9) C(10) 123.5(13) No . . . C(5) C(10) C(9) 119.1(14) No . . . N(1) C(11) C(8) 112.7(11) No . . . N(1) C(12) C(13) 122.2(10) No . . . Fe(1) C(13) C(12) 123.9(9) No . . . Fe(1) C(13) C(14) 67.7(7) No . . . Fe(1) C(13) C(17) 67.9(6) No . . . C(12) C(13) C(14) 125.5(10) No . . . C(12) C(13) C(17) 127.0(10) No . . . C(14) C(13) C(17) 107.1(10) No . . . Fe(1) C(14) C(13) 71.4(7) No . . . Fe(1) C(14) C(15) 69.6(7) No . . . C(13) C(14) C(15) 108.7(10) No . . . Fe(1) C(15) C(14) 69.8(7) No . . . Fe(1) C(15) C(16) 69.6(7) No . . . C(14) C(15) C(16) 106.7(11) No . . . Fe(1) C(16) C(15) 68.9(7) No . . . Fe(1) C(16) C(17) 69.8(6) No . . . C(15) C(16) C(17) 109.3(11) No . . . Fe(1) C(17) C(13) 71.4(6) No . . . Fe(1) C(17) C(16) 70.2(6) No . . . C(13) C(17) C(16) 108.0(10) No . . . Fe(1) C(18) C(19) 67.6(7) No . . . Fe(1) C(18) C(22) 69.4(8) No . . . C(19) C(18) C(22) 106.1(12) No . . . Fe(1) C(19) C(18) 71.1(7) No . . . Fe(1) C(19) C(20) 70.5(7) No . . . C(18) C(19) C(20) 109.2(11) No . . . Fe(1) C(20) C(19) 69.5(8) No . . . Fe(1) C(20) C(21) 69.8(8) No . . . C(19) C(20) C(21) 107.4(13) No . . . Fe(1) C(21) C(20) 68.9(8) No . . . Fe(1) C(21) C(22) 71.3(9) No . . . C(20) C(21) C(22) 109.6(14) No . . . Fe(1) C(22) C(18) 69.4(8) No . . . Fe(1) C(22) C(21) 69.4(9) No . . . C(18) C(22) C(21) 107.8(12) No . . . C(2) C(1) H(1) 120.8 No . . . C(2) C(1) H(2) 119.2 No . . . H(1) C(1) H(2) 120.0 No . . . C(1) C(2) H(3) 114.5 No . . . C(3) C(2) H(3) 114.1 No . . . C(2) C(3) H(4) 108.6 No . . . C(2) C(3) H(5) 107.7 No . . . C(4) C(3) H(4) 109.0 No . . . C(4) C(3) H(5) 107.4 No . . . H(4) C(3) H(5) 109.5 No . . . O(1) C(4) H(6) 108.9 No . . . O(1) C(4) H(7) 110.5 No . . . C(3) C(4) H(6) 108.8 No . . . C(3) C(4) H(7) 110.5 No . . . H(6) C(4) H(7) 109.5 No . . . C(5) C(6) H(8) 119.1 No . . . C(7) C(6) H(8) 119.2 No . . . C(6) C(7) H(9) 119.3 No . . . C(8) C(7) H(9) 119.4 No . . . C(8) C(9) H(10) 118.2 No . . . C(10) C(9) H(10) 118.4 No . . . C(5) C(10) H(11) 120.4 No . . . C(9) C(10) H(11) 120.4 No . . . N(1) C(11) H(12) 108.6 No . . . N(1) C(11) H(13) 109.0 No . . . C(8) C(11) H(12) 108.5 No . . . C(8) C(11) H(13) 108.5 No . . . H(12) C(11) H(13) 109.5 No . . . N(1) C(12) H(14) 118.7 No . . . C(13) C(12) H(14) 119.1 No . . . Fe(1) C(14) H(15) 126.0 No . . . C(13) C(14) H(15) 125.4 No . . . C(15) C(14) H(15) 125.9 No . . . Fe(1) C(15) H(16) 125.1 No . . . C(14) C(15) H(16) 125.9 No . . . C(16) C(15) H(16) 127.4 No . . . Fe(1) C(16) H(17) 124.4 No . . . C(15) C(16) H(17) 125.1 No . . . C(17) C(16) H(17) 125.5 No . . . Fe(1) C(17) H(18) 124.8 No . . . C(13) C(17) H(18) 125.3 No . . . C(16) C(17) H(18) 126.7 No . . . Fe(1) C(18) H(19) 127.9 No . . . C(19) C(18) H(19) 126.8 No . . . C(22) C(18) H(19) 127.1 No . . . Fe(1) C(19) H(20) 126.3 No . . . C(18) C(19) H(20) 125.5 No . . . C(20) C(19) H(20) 125.2 No . . . Fe(1) C(20) H(21) 126.5 No . . . C(19) C(20) H(21) 126.1 No . . . C(21) C(20) H(21) 126.5 No . . . Fe(1) C(21) H(22) 125.6 No . . . C(20) C(21) H(22) 125.2 No . . . C(22) C(21) H(22) 125.2 No . . . Fe(1) C(22) H(23) 126.3 No . . . C(18) C(22) H(23) 125.8 No . . . C(21) C(22) H(23) 126.5 No . . . # End of CIF #============================================================================== #============================================================================== data__Fe(CH2OCOCHCH2)2 _database_code_depnum_ccdc_archive 'CCDC 637665' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C18 H18 Fe O4 ' _chemical_formula_moiety 'C18 H18 Fe O4 ' _chemical_formula_weight 354.18 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,1/2-Z 3 -X,-Y,-Z 4 +X,-Y,1/2+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,1/2-Z 7 1/2-X,1/2-Y,-Z 8 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 22.261(5) _cell_length_b 7.449(3) _cell_length_c 11.557(3) _cell_angle_alpha 90.0000 _cell_angle_beta 119.668(15) _cell_angle_gamma 90.0000 _cell_volume 1665.1(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.6 _cell_measurement_theta_max 15.0 _cell_measurement_temperature 298.1 #------------------------------------------------------------------------------ _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 736.00 _exptl_absorpt_coefficient_mu 0.921 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.819 _exptl_absorpt_correction_T_max 0.912 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w _diffrn_reflns_number 2069 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 3 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1919 _reflns_number_gt 1437 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0552 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 1439 _refine_ls_number_parameters 114 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0014Fo^2^ + 1.0000\s(Fo^2^)]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.31 _refine_diff_density_min -0.26 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Fe Fe 0.346 0.844 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Fe(1) Fe 0.0000 0.45522(6) 0.2500 0.03648(14) Uani 1.00 2 d S . . O(1) O 0.10800(13) 0.0513(3) 0.6410(2) 0.0773(8) Uani 1.00 1 d . . . O(2) O 0.14485(12) 0.0307(3) 0.4944(2) 0.0545(5) Uani 1.00 1 d . . . C(1) C 0.2454(2) -0.0483(6) 0.8401(4) 0.0907(14) Uani 1.00 1 d . . . C(2) C 0.2243(2) -0.0404(5) 0.7150(4) 0.0719(11) Uani 1.00 1 d . . . C(3) C 0.15258(18) 0.0184(4) 0.6164(3) 0.0530(8) Uani 1.00 1 d . . . C(4) C 0.07826(16) 0.0958(4) 0.3889(2) 0.0482(7) Uani 1.00 1 d . . . C(5) C 0.07911(12) 0.2949(3) 0.3801(2) 0.0406(6) Uani 1.00 1 d . . . C(6) C 0.06052(14) 0.4176(4) 0.4511(2) 0.0452(7) Uani 1.00 1 d . . . C(7) C 0.06913(16) 0.5942(4) 0.4164(2) 0.0515(7) Uani 1.00 1 d . . . C(8) C 0.09351(16) 0.5824(4) 0.3244(3) 0.0554(8) Uani 1.00 1 d . . . C(9) C 0.10002(13) 0.3983(4) 0.3018(2) 0.0485(7) Uani 1.00 1 d . . . H(1) H 0.2148 -0.0144 0.8712 0.097 Uiso 1.00 1 c R . . H(2) H 0.2910 -0.0866 0.9015 0.097 Uiso 1.00 1 c R . . H(3) H 0.2550 -0.0743 0.6842 0.081 Uiso 1.00 1 c R . . H(4) H 0.0688 0.0445 0.3064 0.054 Uiso 1.00 1 c R . . H(5) H 0.0431 0.0616 0.4085 0.053 Uiso 1.00 1 c R . . H(6) H 0.0442 0.3861 0.5104 0.051 Uiso 1.00 1 c R . . H(7) H 0.0594 0.7019 0.4481 0.056 Uiso 1.00 1 c R . . H(8) H 0.1031 0.6810 0.2839 0.063 Uiso 1.00 1 c R . . H(9) H 0.1153 0.3518 0.2442 0.058 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe(1) 0.0385(2) 0.0354(2) 0.0312(2) 0.0000 0.0139(2) 0.0000 O(1) 0.0703(16) 0.112(2) 0.0514(13) 0.0219(15) 0.0311(12) 0.0194(14) O(2) 0.0537(11) 0.0602(13) 0.0454(10) 0.0174(10) 0.0214(9) 0.0102(10) C(1) 0.065(2) 0.118(3) 0.059(2) 0.012(2) 0.0085(18) 0.018(2) C(2) 0.062(2) 0.079(2) 0.061(2) 0.0135(19) 0.0204(17) 0.0160(19) C(3) 0.0570(17) 0.0488(16) 0.0421(15) 0.0061(13) 0.0161(13) 0.0063(13) C(4) 0.0520(16) 0.0479(15) 0.0338(13) 0.0104(12) 0.0129(11) 0.0023(11) C(5) 0.0398(13) 0.0445(14) 0.0312(12) 0.0023(11) 0.0127(10) 0.0005(11) C(6) 0.0451(14) 0.0516(16) 0.0305(12) 0.0032(12) 0.0123(10) -0.0010(11) C(7) 0.0538(16) 0.0424(14) 0.0434(15) -0.0045(13) 0.0127(12) -0.0106(12) C(8) 0.0472(15) 0.0547(18) 0.0551(17) -0.0115(13) 0.0183(13) 0.0048(14) C(9) 0.0383(13) 0.0624(17) 0.0434(14) 0.0014(13) 0.0192(11) 0.0040(13) #============================================================================== _computing_data_collection WinAFC _computing_cell_refinement WinAFC _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.7.0' #============================================================================== # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Fe(1) C(5) 2.041(2) No . . Fe(1) C(5) 2.041(2) No . 55502 Fe(1) C(6) 2.048(2) No . . Fe(1) C(6) 2.048(2) No . 55502 Fe(1) C(7) 2.052(2) No . . Fe(1) C(7) 2.052(2) No . 55502 Fe(1) C(8) 2.049(3) No . . Fe(1) C(8) 2.049(3) No . 55502 Fe(1) C(9) 2.044(3) No . . Fe(1) C(9) 2.044(3) No . 55502 O(1) C(3) 1.185(5) No . . O(2) C(3) 1.337(4) No . . O(2) C(4) 1.459(3) No . . C(1) C(2) 1.281(6) No . . C(2) C(3) 1.495(4) No . . C(4) C(5) 1.487(4) No . . C(5) C(6) 1.420(4) No . . C(5) C(9) 1.430(5) No . . C(6) C(7) 1.416(4) No . . C(7) C(8) 1.416(6) No . . C(8) C(9) 1.417(4) No . . C(1) H(1) 0.950 No . . C(1) H(2) 0.950 No . . C(2) H(3) 0.950 No . . C(4) H(4) 0.950 No . . C(4) H(5) 0.950 No . . C(6) H(6) 0.950 No . . C(7) H(7) 0.950 No . . C(8) H(8) 0.950 No . . C(9) H(9) 0.950 No . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C(5) Fe(1) C(5) 108.38(10) No . . 55502 C(5) Fe(1) C(6) 40.63(12) No . . . C(5) Fe(1) C(6) 126.77(12) No . . 55502 C(5) Fe(1) C(7) 68.38(11) No . . . C(5) Fe(1) C(7) 163.54(14) No . . 55502 C(5) Fe(1) C(8) 68.56(11) No . . . C(5) Fe(1) C(8) 155.03(15) No . . 55502 C(5) Fe(1) C(9) 41.00(13) No . . . C(5) Fe(1) C(9) 120.80(12) No . . 55502 C(5) Fe(1) C(6) 126.77(12) No 55502 . . C(5) Fe(1) C(6) 40.63(12) No 55502 . 55502 C(5) Fe(1) C(7) 163.54(14) No 55502 . . C(5) Fe(1) C(7) 68.38(11) No 55502 . 55502 C(5) Fe(1) C(8) 155.03(15) No 55502 . . C(5) Fe(1) C(8) 68.56(11) No 55502 . 55502 C(5) Fe(1) C(9) 120.80(12) No 55502 . . C(5) Fe(1) C(9) 41.00(13) No 55502 . 55502 C(6) Fe(1) C(6) 164.26(12) No . . 55502 C(6) Fe(1) C(7) 40.40(12) No . . . C(6) Fe(1) C(7) 154.12(13) No . . 55502 C(6) Fe(1) C(8) 68.03(14) No . . . C(6) Fe(1) C(8) 120.05(15) No . . 55502 C(6) Fe(1) C(9) 68.28(14) No . . . C(6) Fe(1) C(9) 108.25(13) No . . 55502 C(6) Fe(1) C(7) 154.12(13) No 55502 . . C(6) Fe(1) C(7) 40.40(12) No 55502 . 55502 C(6) Fe(1) C(8) 120.05(15) No 55502 . . C(6) Fe(1) C(8) 68.03(14) No 55502 . 55502 C(6) Fe(1) C(9) 108.25(13) No 55502 . . C(6) Fe(1) C(9) 68.28(14) No 55502 . 55502 C(7) Fe(1) C(7) 119.39(12) No . . 55502 C(7) Fe(1) C(8) 40.39(16) No . . . C(7) Fe(1) C(8) 107.16(13) No . . 55502 C(7) Fe(1) C(9) 68.12(14) No . . . C(7) Fe(1) C(9) 125.60(15) No . . 55502 C(7) Fe(1) C(8) 107.16(13) No 55502 . . C(7) Fe(1) C(8) 40.39(16) No 55502 . 55502 C(7) Fe(1) C(9) 125.60(15) No 55502 . . C(7) Fe(1) C(9) 68.12(14) No 55502 . 55502 C(8) Fe(1) C(8) 124.93(13) No . . 55502 C(8) Fe(1) C(9) 40.51(13) No . . . C(8) Fe(1) C(9) 162.20(14) No . . 55502 C(8) Fe(1) C(9) 162.20(14) No 55502 . . C(8) Fe(1) C(9) 40.51(13) No 55502 . 55502 C(9) Fe(1) C(9) 156.05(13) No . . 55502 C(3) O(2) C(4) 116.8(3) No . . . C(1) C(2) C(3) 122.1(4) No . . . O(1) C(3) O(2) 123.6(2) No . . . O(1) C(3) C(2) 125.6(3) No . . . O(2) C(3) C(2) 110.8(3) No . . . O(2) C(4) C(5) 110.3(2) No . . . Fe(1) C(5) C(4) 126.76(16) No . . . Fe(1) C(5) C(6) 69.94(14) No . . . Fe(1) C(5) C(9) 69.59(15) No . . . C(4) C(5) C(6) 125.8(3) No . . . C(4) C(5) C(9) 126.9(3) No . . . C(6) C(5) C(9) 107.3(2) No . . . Fe(1) C(6) C(5) 69.43(14) No . . . Fe(1) C(6) C(7) 69.94(15) No . . . C(5) C(6) C(7) 108.4(3) No . . . Fe(1) C(7) C(6) 69.66(15) No . . . Fe(1) C(7) C(8) 69.70(17) No . . . C(6) C(7) C(8) 108.1(3) No . . . Fe(1) C(8) C(7) 69.91(19) No . . . Fe(1) C(8) C(9) 69.55(17) No . . . C(7) C(8) C(9) 108.1(3) No . . . Fe(1) C(9) C(5) 69.41(17) No . . . Fe(1) C(9) C(8) 69.94(19) No . . . C(5) C(9) C(8) 108.0(3) No . . . C(2) C(1) H(1) 118.9 No . . . C(2) C(1) H(2) 121.1 No . . . H(1) C(1) H(2) 120.0 No . . . C(1) C(2) H(3) 118.7 No . . . C(3) C(2) H(3) 119.2 No . . . O(2) C(4) H(4) 109.4 No . . . O(2) C(4) H(5) 109.1 No . . . C(5) C(4) H(4) 109.6 No . . . C(5) C(4) H(5) 108.9 No . . . H(4) C(4) H(5) 109.5 No . . . Fe(1) C(6) H(6) 125.5 No . . . C(5) C(6) H(6) 125.6 No . . . C(7) C(6) H(6) 125.9 No . . . Fe(1) C(7) H(7) 125.4 No . . . C(6) C(7) H(7) 126.0 No . . . C(8) C(7) H(7) 125.9 No . . . Fe(1) C(8) H(8) 125.4 No . . . C(7) C(8) H(8) 125.8 No . . . C(9) C(8) H(8) 126.1 No . . . Fe(1) C(9) H(9) 125.9 No . . . C(5) C(9) H(9) 126.0 No . . . C(8) C(9) H(9) 126.0 No . . . # End of CIF