Electronic Supplementary Material for CrystEngComm This Journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Prof Michael Schmittel' _publ_contact_author_address ; Center of Micro and Nanochemistry and Engineering, Organische Chemie I Universitat Siegen Adolf-Reichwein Str. Siegen D-57068 GERMANY ; _publ_contact_author_phone '049 271 740 4356' _publ_contact_author_fax '049 271 740 3270' _publ_contact_author_email schmittel@chemie.uni-siegen.de _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication in "CrystEngComm". M. Schmittel ; #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Unusual ladder like supramolecular arrangment by cooperative effect of bifurcated O-H...O hydrogen bonding in crystals of racemic 4-ferrocenylbutan-1,2-diol ; loop_ _publ_author_name _publ_author_address M.Schmittel ; Center of Micro and Nanochemistry and Engineering, Organic Chemistry I University of Siegen Adolf-Reichwein-Str. D-57068 Siegen, Germany ; L.Mukul ; Center of Micro and Nanochemistry and Engineering, Organic Chemistry I University of Siegen Adolf-Reichwein-Str. D-57068 Siegen, Germany ; M.Schlosser ; Center of Micro and Nanochemistry and Engineering, Inorganic Chemistry I University of Siegen Adolf-Reichwein-Str. D-57068 Siegen, Germany ; H.-J.Deiseroth ; Center of Micro and Nanochemistry and Engineering, Inorganic Chemistry I University of Siegen Adolf-Reichwein-Str. D-57068 Siegen, Germany ; data_C14H18FeO2 _database_code_CSD 208961 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C14H18FeO2 _chemical_formula_sum 'C14 H18 Fe O2' _chemical_formula_weight 274.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.2583(10) _cell_length_b 9.7626(8) _cell_length_c 8.2940(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.460(8) _cell_angle_gamma 90.00 _cell_volume 1225.02(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.25 _cell_measurement_theta_max 31.6 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 1.217 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6787 _exptl_absorpt_correction_T_max 0.8898 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method '170 exposures, \D\f=1.3\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17434 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 31.65 _reflns_number_total 3912 _reflns_number_gt 3211 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE (STOE IPDS-Software, 1999)' _computing_cell_refinement 'CELL/SELECT (STOE IPDS-Software, 1999)' _computing_data_reduction 'X-RED (STOE, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 2.1 (Crystal Impact, 1999)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+0.2061P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0039(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3912 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0674 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.660610(11) 0.986786(15) 0.22362(2) 0.01567(6) Uani 1 1 d . . . O1 O 1.03194(6) 1.14830(10) 0.85685(12) 0.0277(2) Uani 1 1 d . . . H1 H 1.0431 1.1332 0.9571 0.042 Uiso 1 1 calc R . . O2 O 0.93529(7) 0.88412(9) 0.81123(11) 0.0248(2) Uani 1 1 d . . . H2 H 0.9389 0.8124 0.7565 0.037 Uiso 1 1 calc R . . C1 C 0.93987(8) 1.12788(12) 0.80606(17) 0.0247(3) Uani 1 1 d . . . H1A H 0.9159 1.2082 0.7421 0.030 Uiso 1 1 calc R . . H1B H 0.9086 1.1208 0.9032 0.030 Uiso 1 1 calc R . . C2 C 0.92232(8) 0.99960(11) 0.70386(15) 0.0185(2) Uani 1 1 d . . . H2A H 0.9655 0.9948 0.6231 0.022 Uiso 1 1 calc R . . C3 C 0.82847(8) 1.00227(11) 0.61359(15) 0.0195(2) Uani 1 1 d . . . H3A H 0.7861 1.0083 0.6942 0.023 Uiso 1 1 calc R . . H3B H 0.8212 1.0856 0.5452 0.023 Uiso 1 1 calc R . . C4 C 0.80562(8) 0.87704(11) 0.50588(15) 0.0191(2) Uani 1 1 d . . . H4A H 0.8458 0.8738 0.4214 0.023 Uiso 1 1 calc R . . H4B H 0.8158 0.7933 0.5731 0.023 Uiso 1 1 calc R . . C5 C 0.71169(7) 0.87710(10) 0.42440(14) 0.0162(2) Uani 1 1 d . . . C6 C 0.64060(8) 0.96299(12) 0.46103(15) 0.0196(2) Uani 1 1 d . . . H6 H 0.6445 1.0323 0.5420 0.024 Uiso 1 1 calc R . . C7 C 0.56275(8) 0.92627(13) 0.35446(16) 0.0239(2) Uani 1 1 d . . . H7 H 0.5061 0.9674 0.3519 0.029 Uiso 1 1 calc R . . C8 C 0.58487(8) 0.81754(12) 0.25303(16) 0.0233(2) Uani 1 1 d . . . H8 H 0.5457 0.7729 0.1713 0.028 Uiso 1 1 calc R . . C9 C 0.67640(8) 0.78754(10) 0.29600(14) 0.0191(2) Uani 1 1 d . . . H9 H 0.7086 0.7192 0.2472 0.023 Uiso 1 1 calc R . . C10 C 0.63573(10) 1.04509(15) -0.01437(17) 0.0309(3) Uani 1 1 d . . . H10 H 0.5952 1.0028 -0.0960 0.037 Uiso 1 1 calc R . . C11 C 0.72630(10) 1.01104(12) 0.02614(17) 0.0255(3) Uani 1 1 d . . . H11 H 0.7572 0.9422 -0.0246 0.031 Uiso 1 1 calc R . . C12 C 0.76298(10) 1.09732(13) 0.15530(18) 0.0287(3) Uani 1 1 d . . . H12 H 0.8224 1.0959 0.2064 0.034 Uiso 1 1 calc R . . C13 C 0.69520(12) 1.18618(13) 0.19475(19) 0.0354(3) Uani 1 1 d . . . H13 H 0.7013 1.2548 0.2767 0.042 Uiso 1 1 calc R . . C14 C 0.61667(11) 1.15418(15) 0.0897(2) 0.0372(4) Uani 1 1 d . . . H14 H 0.5610 1.1980 0.0890 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01936(9) 0.01425(8) 0.01325(9) 0.00116(5) 0.00157(6) 0.00023(5) O1 0.0266(4) 0.0307(4) 0.0231(5) 0.0041(4) -0.0069(4) -0.0110(4) O2 0.0357(5) 0.0184(4) 0.0178(4) 0.0004(3) -0.0061(4) 0.0035(3) C1 0.0236(6) 0.0201(5) 0.0281(7) -0.0026(4) -0.0055(5) -0.0022(4) C2 0.0185(5) 0.0200(5) 0.0160(5) 0.0016(4) -0.0014(4) -0.0012(4) C3 0.0196(5) 0.0189(5) 0.0187(5) -0.0005(4) -0.0022(4) 0.0005(4) C4 0.0186(5) 0.0200(5) 0.0178(6) -0.0021(4) -0.0014(4) 0.0020(4) C5 0.0196(5) 0.0164(4) 0.0124(5) 0.0011(3) 0.0008(4) -0.0003(3) C6 0.0200(5) 0.0250(5) 0.0142(5) -0.0004(4) 0.0029(4) 0.0012(4) C7 0.0175(5) 0.0331(6) 0.0213(6) 0.0031(5) 0.0027(5) -0.0015(4) C8 0.0242(5) 0.0240(5) 0.0207(6) 0.0023(4) -0.0015(5) -0.0087(4) C9 0.0266(5) 0.0134(4) 0.0169(5) 0.0011(3) 0.0006(4) -0.0023(4) C10 0.0392(7) 0.0334(6) 0.0182(6) 0.0104(5) -0.0029(6) -0.0019(5) C11 0.0379(7) 0.0209(5) 0.0198(6) 0.0027(4) 0.0115(5) -0.0014(4) C12 0.0326(7) 0.0255(6) 0.0284(7) 0.0040(5) 0.0060(6) -0.0116(5) C13 0.0625(10) 0.0135(5) 0.0331(8) -0.0002(5) 0.0173(7) -0.0060(5) C14 0.0446(8) 0.0286(6) 0.0400(9) 0.0188(6) 0.0113(7) 0.0158(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C12 2.0384(13) . ? Fe1 C13 2.0392(12) . ? Fe1 C14 2.0398(13) . ? Fe1 C9 2.0407(10) . ? Fe1 C11 2.0420(14) . ? Fe1 C10 2.0420(13) . ? Fe1 C7 2.0438(13) . ? Fe1 C6 2.0446(12) . ? Fe1 C5 2.0470(11) . ? Fe1 C8 2.0490(12) . ? O1 C1 1.4272(15) . ? O1 H1 0.8400 . ? O2 C2 1.4344(14) . ? O2 H2 0.8400 . ? C1 C2 1.5165(16) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.5276(16) . ? C2 H2A 1.0000 . ? C3 C4 1.5275(15) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.5031(15) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C9 1.4282(15) . ? C5 C6 1.4343(16) . ? C6 C7 1.4312(16) . ? C6 H6 0.9500 . ? C7 C8 1.4220(19) . ? C7 H7 0.9500 . ? C8 C9 1.4261(17) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.419(2) . ? C10 C14 1.424(2) . ? C10 H10 0.9500 . ? C11 C12 1.4194(19) . ? C11 H11 0.9500 . ? C12 C13 1.420(2) . ? C12 H12 0.9500 . ? C13 C14 1.422(2) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Fe1 C13 40.77(6) . . ? C12 Fe1 C14 68.54(6) . . ? C13 Fe1 C14 40.80(7) . . ? C12 Fe1 C9 121.39(6) . . ? C13 Fe1 C9 157.22(6) . . ? C14 Fe1 C9 160.35(6) . . ? C12 Fe1 C11 40.71(5) . . ? C13 Fe1 C11 68.51(6) . . ? C14 Fe1 C11 68.36(6) . . ? C9 Fe1 C11 107.16(5) . . ? C12 Fe1 C10 68.70(6) . . ? C13 Fe1 C10 68.83(6) . . ? C14 Fe1 C10 40.85(6) . . ? C9 Fe1 C10 123.37(5) . . ? C11 Fe1 C10 40.65(6) . . ? C12 Fe1 C7 160.00(6) . . ? C13 Fe1 C7 123.81(6) . . ? C14 Fe1 C7 108.03(6) . . ? C9 Fe1 C7 68.58(5) . . ? C11 Fe1 C7 158.12(6) . . ? C10 Fe1 C7 122.47(6) . . ? C12 Fe1 C6 122.92(5) . . ? C13 Fe1 C6 107.15(6) . . ? C14 Fe1 C6 122.40(6) . . ? C9 Fe1 C6 68.60(5) . . ? C11 Fe1 C6 159.37(6) . . ? C10 Fe1 C6 158.49(6) . . ? C7 Fe1 C6 40.98(5) . . ? C12 Fe1 C5 106.17(5) . . ? C13 Fe1 C5 121.19(6) . . ? C14 Fe1 C5 157.77(6) . . ? C9 Fe1 C5 40.90(4) . . ? C11 Fe1 C5 122.58(5) . . ? C10 Fe1 C5 159.32(6) . . ? C7 Fe1 C5 69.15(5) . . ? C6 Fe1 C5 41.04(5) . . ? C12 Fe1 C8 157.57(6) . . ? C13 Fe1 C8 160.46(6) . . ? C14 Fe1 C8 124.08(6) . . ? C9 Fe1 C8 40.82(5) . . ? C11 Fe1 C8 122.15(5) . . ? C10 Fe1 C8 107.63(5) . . ? C7 Fe1 C8 40.66(5) . . ? C6 Fe1 C8 68.70(5) . . ? C5 Fe1 C8 69.04(5) . . ? C1 O1 H1 109.5 . . ? C2 O2 H2 109.5 . . ? O1 C1 C2 112.08(11) . . ? O1 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? O1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? O2 C2 C1 107.57(10) . . ? O2 C2 C3 111.26(9) . . ? C1 C2 C3 110.25(9) . . ? O2 C2 H2A 109.2 . . ? C1 C2 H2A 109.2 . . ? C3 C2 H2A 109.2 . . ? C4 C3 C2 113.66(9) . . ? C4 C3 H3A 108.8 . . ? C2 C3 H3A 108.8 . . ? C4 C3 H3B 108.8 . . ? C2 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C5 C4 C3 113.24(9) . . ? C5 C4 H4A 108.9 . . ? C3 C4 H4A 108.9 . . ? C5 C4 H4B 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C9 C5 C6 107.07(10) . . ? C9 C5 C4 125.47(10) . . ? C6 C5 C4 127.45(10) . . ? C9 C5 Fe1 69.31(6) . . ? C6 C5 Fe1 69.39(6) . . ? C4 C5 Fe1 127.30(8) . . ? C7 C6 C5 108.22(10) . . ? C7 C6 Fe1 69.48(7) . . ? C5 C6 Fe1 69.57(7) . . ? C7 C6 H6 125.9 . . ? C5 C6 H6 125.9 . . ? Fe1 C6 H6 126.6 . . ? C8 C7 C6 108.09(11) . . ? C8 C7 Fe1 69.86(7) . . ? C6 C7 Fe1 69.54(7) . . ? C8 C7 H7 126.0 . . ? C6 C7 H7 126.0 . . ? Fe1 C7 H7 126.2 . . ? C7 C8 C9 107.79(10) . . ? C7 C8 Fe1 69.47(7) . . ? C9 C8 Fe1 69.28(6) . . ? C7 C8 H8 126.1 . . ? C9 C8 H8 126.1 . . ? Fe1 C8 H8 126.7 . . ? C8 C9 C5 108.83(11) . . ? C8 C9 Fe1 69.90(6) . . ? C5 C9 Fe1 69.79(6) . . ? C8 C9 H9 125.6 . . ? C5 C9 H9 125.6 . . ? Fe1 C9 H9 126.3 . . ? C11 C10 C14 107.52(13) . . ? C11 C10 Fe1 69.67(8) . . ? C14 C10 Fe1 69.49(8) . . ? C11 C10 H10 126.2 . . ? C14 C10 H10 126.2 . . ? Fe1 C10 H10 126.2 . . ? C10 C11 C12 108.43(13) . . ? C10 C11 Fe1 69.67(8) . . ? C12 C11 Fe1 69.51(8) . . ? C10 C11 H11 125.8 . . ? C12 C11 H11 125.8 . . ? Fe1 C11 H11 126.6 . . ? C11 C12 C13 107.99(13) . . ? C11 C12 Fe1 69.78(8) . . ? C13 C12 Fe1 69.65(8) . . ? C11 C12 H12 126.0 . . ? C13 C12 H12 126.0 . . ? Fe1 C12 H12 126.1 . . ? C12 C13 C14 107.79(13) . . ? C12 C13 Fe1 69.59(7) . . ? C14 C13 Fe1 69.62(7) . . ? C12 C13 H13 126.1 . . ? C14 C13 H13 126.1 . . ? Fe1 C13 H13 126.3 . . ? C13 C14 C10 108.27(13) . . ? C13 C14 Fe1 69.58(7) . . ? C10 C14 Fe1 69.66(7) . . ? C13 C14 H14 125.9 . . ? C10 C14 H14 125.9 . . ? Fe1 C14 H14 126.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 O2 74.37(14) . . . . ? O1 C1 C2 C3 -164.15(10) . . . . ? O2 C2 C3 C4 -61.38(14) . . . . ? C1 C2 C3 C4 179.35(11) . . . . ? C2 C3 C4 C5 177.01(10) . . . . ? C3 C4 C5 C9 168.16(11) . . . . ? C3 C4 C5 C6 -13.19(17) . . . . ? C3 C4 C5 Fe1 78.31(13) . . . . ? C12 Fe1 C5 C9 -119.58(8) . . . . ? C13 Fe1 C5 C9 -161.31(8) . . . . ? C14 Fe1 C5 C9 167.73(15) . . . . ? C11 Fe1 C5 C9 -78.28(8) . . . . ? C10 Fe1 C5 C9 -47.21(17) . . . . ? C7 Fe1 C5 C9 80.95(8) . . . . ? C6 Fe1 C5 C9 118.51(10) . . . . ? C8 Fe1 C5 C9 37.28(8) . . . . ? C12 Fe1 C5 C6 121.91(7) . . . . ? C13 Fe1 C5 C6 80.18(9) . . . . ? C14 Fe1 C5 C6 49.22(17) . . . . ? C9 Fe1 C5 C6 -118.51(10) . . . . ? C11 Fe1 C5 C6 163.21(7) . . . . ? C10 Fe1 C5 C6 -165.72(14) . . . . ? C7 Fe1 C5 C6 -37.56(7) . . . . ? C8 Fe1 C5 C6 -81.22(8) . . . . ? C12 Fe1 C5 C4 -0.10(11) . . . . ? C13 Fe1 C5 C4 -41.84(12) . . . . ? C14 Fe1 C5 C4 -72.80(19) . . . . ? C9 Fe1 C5 C4 119.47(13) . . . . ? C11 Fe1 C5 C4 41.19(11) . . . . ? C10 Fe1 C5 C4 72.27(18) . . . . ? C7 Fe1 C5 C4 -159.57(11) . . . . ? C6 Fe1 C5 C4 -122.02(12) . . . . ? C8 Fe1 C5 C4 156.76(11) . . . . ? C9 C5 C6 C7 -0.41(13) . . . . ? C4 C5 C6 C7 -179.25(11) . . . . ? Fe1 C5 C6 C7 58.91(8) . . . . ? C9 C5 C6 Fe1 -59.32(8) . . . . ? C4 C5 C6 Fe1 121.84(12) . . . . ? C12 Fe1 C6 C7 164.08(8) . . . . ? C13 Fe1 C6 C7 122.19(8) . . . . ? C14 Fe1 C6 C7 80.13(9) . . . . ? C9 Fe1 C6 C7 -81.55(8) . . . . ? C11 Fe1 C6 C7 -163.39(12) . . . . ? C10 Fe1 C6 C7 46.54(17) . . . . ? C5 Fe1 C6 C7 -119.71(10) . . . . ? C8 Fe1 C6 C7 -37.57(7) . . . . ? C12 Fe1 C6 C5 -76.21(8) . . . . ? C13 Fe1 C6 C5 -118.10(8) . . . . ? C14 Fe1 C6 C5 -160.16(8) . . . . ? C9 Fe1 C6 C5 38.17(6) . . . . ? C11 Fe1 C6 C5 -43.68(16) . . . . ? C10 Fe1 C6 C5 166.25(13) . . . . ? C7 Fe1 C6 C5 119.71(10) . . . . ? C8 Fe1 C6 C5 82.14(7) . . . . ? C5 C6 C7 C8 0.48(14) . . . . ? Fe1 C6 C7 C8 59.44(9) . . . . ? C5 C6 C7 Fe1 -58.96(8) . . . . ? C12 Fe1 C7 C8 -161.65(14) . . . . ? C13 Fe1 C7 C8 163.95(8) . . . . ? C14 Fe1 C7 C8 121.69(8) . . . . ? C9 Fe1 C7 C8 -37.73(7) . . . . ? C11 Fe1 C7 C8 44.99(16) . . . . ? C10 Fe1 C7 C8 79.06(9) . . . . ? C6 Fe1 C7 C8 -119.33(10) . . . . ? C5 Fe1 C7 C8 -81.72(7) . . . . ? C12 Fe1 C7 C6 -42.32(18) . . . . ? C13 Fe1 C7 C6 -76.72(9) . . . . ? C14 Fe1 C7 C6 -118.98(8) . . . . ? C9 Fe1 C7 C6 81.60(7) . . . . ? C11 Fe1 C7 C6 164.32(12) . . . . ? C10 Fe1 C7 C6 -161.61(7) . . . . ? C5 Fe1 C7 C6 37.61(7) . . . . ? C8 Fe1 C7 C6 119.33(10) . . . . ? C6 C7 C8 C9 -0.36(14) . . . . ? Fe1 C7 C8 C9 58.88(8) . . . . ? C6 C7 C8 Fe1 -59.24(9) . . . . ? C12 Fe1 C8 C7 163.60(13) . . . . ? C13 Fe1 C8 C7 -43.37(19) . . . . ? C14 Fe1 C8 C7 -77.65(9) . . . . ? C9 Fe1 C8 C7 119.36(10) . . . . ? C11 Fe1 C8 C7 -161.87(7) . . . . ? C10 Fe1 C8 C7 -119.64(8) . . . . ? C6 Fe1 C8 C7 37.86(7) . . . . ? C5 Fe1 C8 C7 82.01(8) . . . . ? C12 Fe1 C8 C9 44.24(17) . . . . ? C13 Fe1 C8 C9 -162.73(15) . . . . ? C14 Fe1 C8 C9 162.99(8) . . . . ? C11 Fe1 C8 C9 78.77(9) . . . . ? C10 Fe1 C8 C9 121.00(8) . . . . ? C7 Fe1 C8 C9 -119.36(10) . . . . ? C6 Fe1 C8 C9 -81.51(8) . . . . ? C5 Fe1 C8 C9 -37.36(7) . . . . ? C7 C8 C9 C5 0.10(14) . . . . ? Fe1 C8 C9 C5 59.10(8) . . . . ? C7 C8 C9 Fe1 -59.00(9) . . . . ? C6 C5 C9 C8 0.19(13) . . . . ? C4 C5 C9 C8 179.06(11) . . . . ? Fe1 C5 C9 C8 -59.17(8) . . . . ? C6 C5 C9 Fe1 59.36(8) . . . . ? C4 C5 C9 Fe1 -121.76(11) . . . . ? C12 Fe1 C9 C8 -161.83(8) . . . . ? C13 Fe1 C9 C8 165.14(14) . . . . ? C14 Fe1 C9 C8 -46.1(2) . . . . ? C11 Fe1 C9 C8 -119.65(8) . . . . ? C10 Fe1 C9 C8 -78.01(9) . . . . ? C7 Fe1 C9 C8 37.59(8) . . . . ? C6 Fe1 C9 C8 81.77(8) . . . . ? C5 Fe1 C9 C8 120.06(11) . . . . ? C12 Fe1 C9 C5 78.10(9) . . . . ? C13 Fe1 C9 C5 45.07(17) . . . . ? C14 Fe1 C9 C5 -166.17(16) . . . . ? C11 Fe1 C9 C5 120.29(8) . . . . ? C10 Fe1 C9 C5 161.92(8) . . . . ? C7 Fe1 C9 C5 -82.47(8) . . . . ? C6 Fe1 C9 C5 -38.30(7) . . . . ? C8 Fe1 C9 C5 -120.06(11) . . . . ? C12 Fe1 C10 C11 37.37(8) . . . . ? C13 Fe1 C10 C11 81.25(9) . . . . ? C14 Fe1 C10 C11 118.77(12) . . . . ? C9 Fe1 C10 C11 -77.00(9) . . . . ? C7 Fe1 C10 C11 -161.31(7) . . . . ? C6 Fe1 C10 C11 164.34(12) . . . . ? C5 Fe1 C10 C11 -41.88(18) . . . . ? C8 Fe1 C10 C11 -119.14(8) . . . . ? C12 Fe1 C10 C14 -81.40(10) . . . . ? C13 Fe1 C10 C14 -37.52(10) . . . . ? C9 Fe1 C10 C14 164.23(9) . . . . ? C11 Fe1 C10 C14 -118.77(12) . . . . ? C7 Fe1 C10 C14 79.92(10) . . . . ? C6 Fe1 C10 C14 45.57(18) . . . . ? C5 Fe1 C10 C14 -160.65(13) . . . . ? C8 Fe1 C10 C14 122.09(10) . . . . ? C14 C10 C11 C12 0.55(15) . . . . ? Fe1 C10 C11 C12 -58.87(9) . . . . ? C14 C10 C11 Fe1 59.42(10) . . . . ? C12 Fe1 C11 C10 -119.89(11) . . . . ? C13 Fe1 C11 C10 -82.11(9) . . . . ? C14 Fe1 C11 C10 -38.08(9) . . . . ? C9 Fe1 C11 C10 121.61(8) . . . . ? C7 Fe1 C11 C10 46.50(17) . . . . ? C6 Fe1 C11 C10 -163.69(12) . . . . ? C5 Fe1 C11 C10 163.75(8) . . . . ? C8 Fe1 C11 C10 79.47(9) . . . . ? C13 Fe1 C11 C12 37.78(9) . . . . ? C14 Fe1 C11 C12 81.81(9) . . . . ? C9 Fe1 C11 C12 -118.49(8) . . . . ? C10 Fe1 C11 C12 119.89(11) . . . . ? C7 Fe1 C11 C12 166.40(12) . . . . ? C6 Fe1 C11 C12 -43.79(17) . . . . ? C5 Fe1 C11 C12 -76.35(9) . . . . ? C8 Fe1 C11 C12 -160.64(8) . . . . ? C10 C11 C12 C13 -0.41(15) . . . . ? Fe1 C11 C12 C13 -59.38(9) . . . . ? C10 C11 C12 Fe1 58.97(9) . . . . ? C13 Fe1 C12 C11 -119.19(12) . . . . ? C14 Fe1 C12 C11 -81.33(9) . . . . ? C9 Fe1 C12 C11 79.67(9) . . . . ? C10 Fe1 C12 C11 -37.32(8) . . . . ? C7 Fe1 C12 C11 -165.15(14) . . . . ? C6 Fe1 C12 C11 163.11(8) . . . . ? C5 Fe1 C12 C11 121.51(8) . . . . ? C8 Fe1 C12 C11 47.38(17) . . . . ? C14 Fe1 C12 C13 37.85(9) . . . . ? C9 Fe1 C12 C13 -161.15(8) . . . . ? C11 Fe1 C12 C13 119.19(12) . . . . ? C10 Fe1 C12 C13 81.87(10) . . . . ? C7 Fe1 C12 C13 -45.97(19) . . . . ? C6 Fe1 C12 C13 -77.70(10) . . . . ? C5 Fe1 C12 C13 -119.30(9) . . . . ? C8 Fe1 C12 C13 166.56(13) . . . . ? C11 C12 C13 C14 0.10(15) . . . . ? Fe1 C12 C13 C14 -59.36(10) . . . . ? C11 C12 C13 Fe1 59.46(9) . . . . ? C14 Fe1 C13 C12 -119.08(13) . . . . ? C9 Fe1 C13 C12 45.44(18) . . . . ? C11 Fe1 C13 C12 -37.73(9) . . . . ? C10 Fe1 C13 C12 -81.52(9) . . . . ? C7 Fe1 C13 C12 162.78(8) . . . . ? C6 Fe1 C13 C12 120.87(9) . . . . ? C5 Fe1 C13 C12 78.25(10) . . . . ? C8 Fe1 C13 C12 -164.63(15) . . . . ? C12 Fe1 C13 C14 119.08(13) . . . . ? C9 Fe1 C13 C14 164.52(13) . . . . ? C11 Fe1 C13 C14 81.35(10) . . . . ? C10 Fe1 C13 C14 37.56(10) . . . . ? C7 Fe1 C13 C14 -78.14(11) . . . . ? C6 Fe1 C13 C14 -120.05(9) . . . . ? C5 Fe1 C13 C14 -162.67(9) . . . . ? C8 Fe1 C13 C14 -45.6(2) . . . . ? C12 C13 C14 C10 0.24(16) . . . . ? Fe1 C13 C14 C10 -59.10(10) . . . . ? C12 C13 C14 Fe1 59.34(9) . . . . ? C11 C10 C14 C13 -0.49(16) . . . . ? Fe1 C10 C14 C13 59.05(10) . . . . ? C11 C10 C14 Fe1 -59.54(9) . . . . ? C12 Fe1 C14 C13 -37.82(9) . . . . ? C9 Fe1 C14 C13 -162.10(16) . . . . ? C11 Fe1 C14 C13 -81.75(10) . . . . ? C10 Fe1 C14 C13 -119.65(14) . . . . ? C7 Fe1 C14 C13 121.22(9) . . . . ? C6 Fe1 C14 C13 78.42(11) . . . . ? C5 Fe1 C14 C13 42.3(2) . . . . ? C8 Fe1 C14 C13 163.24(9) . . . . ? C12 Fe1 C14 C10 81.83(10) . . . . ? C13 Fe1 C14 C10 119.65(14) . . . . ? C9 Fe1 C14 C10 -42.5(2) . . . . ? C11 Fe1 C14 C10 37.91(9) . . . . ? C7 Fe1 C14 C10 -119.13(9) . . . . ? C6 Fe1 C14 C10 -161.93(8) . . . . ? C5 Fe1 C14 C10 161.99(13) . . . . ? C8 Fe1 C14 C10 -77.11(11) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O2 0.84 1.91 2.7516(13) 174.6 3_777 O2 H2 O1 0.84 1.94 2.7703(13) 170.5 2_746 _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 31.65 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.414 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.059 #============================================================================= # END of CIF #=============================================================================