# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email thierry.ollevier@chm.ulaval.ca _publ_contact_author_name 'Thierry Ollevier' loop_ _publ_author_name 'Baptiste Plancq' 'Thierry Ollevier' data_olev34 _database_code_depnum_ccdc_archive 'CCDC 850236' #TrackingRef '7781_web_deposit_cif_file_0_ThierryOllevier_1319463456.OLEV34.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H36 Fe N4 O3, 2(Cl O4)' _chemical_formula_sum 'C24 H36 Cl2 Fe N4 O11' _chemical_formula_weight 683.32 _chemical_compound_source 'Synthesized by the authors. See text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P3121 _symmetry_space_group_name_hall 'P 31 2"' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' 'y, x, -z' _cell_length_a 11.1665(5) _cell_length_b 11.1665 _cell_length_c 22.5811(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 2438.4(2) _cell_formula_units_Z 3 _cell_measurement_temperature 100 _cell_measurement_reflns_used 10191 _cell_measurement_theta_min 4.97 _cell_measurement_theta_max 69.20 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 5.745 _exptl_absorpt_correction_Type multi-scan _exptl_absorpt_correction_T_min 0.3684 _exptl_absorpt_correction_T_max 0.7084 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 2008)' _exptl_special_details ; X-ray crystallographic data for I were collected from a single crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker smart diffractometer equiped with an APEX II CCD Detector, a graphite monochromator. The crystal-to-detector distance was 5.0 cm, and the data collection was carried out in 512 x 512 pixel mode. The initial unit cell parameters were determined by a least-squares fit of the angular setting of strong reflections, collected by a 10.0 degree scan in 33 frames over four different parts of the reciprocal space (132 frames total). ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Incoatec I\muS Microsource ' _diffrn_radiation_monochromator 'Quazar MX' _diffrn_measurement_device_type 'Bruker APEX II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 53659 _diffrn_reflns_av_R_equivalents 0.072 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 4.57 _diffrn_reflns_theta_max 70.61 _reflns_number_total 3129 _reflns_number_gt 2813 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT V7.68A(Bruker AXS, 2009)' _computing_data_reduction 'SAINT V7.68A(Bruker AXS, 2009)' _computing_structure_solution 'SIR2004 (Burla et al., 2004)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)' _computing_publication_material 'UdMX (Maris, 2004)' _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^)+(0.1062P)^2^+0.2417P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), 1311 Friedel Pairs' _chemical_absolute_configuration rmad _refine_ls_abs_structure_Flack -0.005(9) _refine_ls_number_reflns 3129 _refine_ls_number_parameters 241 _refine_ls_number_restraints 144 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1373 _refine_ls_wR_factor_gt 0.1306 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.66964(6) 0.0000 0.3333 0.0374(2) Uani 1 2 d S . . O1 O 0.6541(3) 0.0766(3) 0.42043(10) 0.0495(7) Uani 1 1 d D . . H1 H 0.596(4) 0.103(5) 0.424(2) 0.063(14) Uiso 1 1 d D . . O2 O 0.4649(4) 0.0000 0.3333 0.0592(11) Uani 1 2 d SD . . H2 H 0.385(3) -0.065(4) 0.326(3) 0.079(18) Uiso 1 1 d D . . N1 N 0.8588(3) 0.0572(3) 0.38628(11) 0.0368(6) Uani 1 1 d . . . N11 N 0.5464(4) -0.2103(4) 0.36338(14) 0.0493(8) Uani 1 1 d . . . C1 C 0.9598(3) 0.0444(4) 0.36000(13) 0.0368(7) Uani 1 1 d . . . C2 C 1.0943(4) 0.1124(4) 0.38178(15) 0.0444(8) Uani 1 1 d . . . H2A H 1.1645 0.1005 0.3637 0.053 Uiso 1 1 calc R . . C3 C 1.1232(4) 0.1977(4) 0.43046(16) 0.0510(10) Uani 1 1 d . . . H3 H 1.2149 0.2473 0.4455 0.061 Uiso 1 1 calc R . . C4 C 1.0210(5) 0.2106(5) 0.45681(17) 0.0521(9) Uani 1 1 d . . . H4 H 1.0409 0.2699 0.4900 0.062 Uiso 1 1 calc R . . C5 C 0.8867(4) 0.1365(4) 0.43483(15) 0.0434(8) Uani 1 1 d . . . C6 C 0.7630(4) 0.1345(5) 0.46308(15) 0.0478(9) Uani 1 1 d . . . H6 H 0.7870 0.2323 0.4706 0.057 Uiso 1 1 calc R . . C7 C 0.7138(5) 0.0541(6) 0.52205(16) 0.0577(11) Uani 1 1 d . . . C8 C 0.7005(8) -0.0851(8) 0.5157(2) 0.097(2) Uani 1 1 d . . . H8A H 0.7918 -0.0743 0.5081 0.146 Uiso 1 1 calc R . . H8B H 0.6385 -0.1344 0.4826 0.146 Uiso 1 1 calc R . . H8C H 0.6625 -0.1378 0.5523 0.146 Uiso 1 1 calc R . . C9 C 0.8176(6) 0.1362(9) 0.5712(2) 0.109(3) Uani 1 1 d . . . H9A H 0.7814 0.0904 0.6094 0.164 Uiso 1 1 calc R . . H9B H 0.8319 0.2301 0.5726 0.164 Uiso 1 1 calc R . . H9C H 0.9059 0.1404 0.5630 0.164 Uiso 1 1 calc R . . C10 C 0.5749(6) 0.0399(7) 0.53929(19) 0.0770(16) Uani 1 1 d . . . H10A H 0.5009 -0.0345 0.5161 0.115 Uiso 1 1 calc R . . H10B H 0.5768 0.1271 0.5312 0.115 Uiso 1 1 calc R . . H10C H 0.5579 0.0181 0.5816 0.115 Uiso 1 1 calc R . . C11 C 0.4609(4) -0.3195(5) 0.37328(17) 0.0501(9) Uani 1 1 d . . . C12 C 0.3494(5) -0.4598(5) 0.3861(2) 0.0628(11) Uani 1 1 d . . . H12A H 0.3403 -0.4740 0.4290 0.094 Uiso 1 1 calc R . . H12B H 0.3707 -0.5267 0.3680 0.094 Uiso 1 1 calc R . . H12C H 0.2624 -0.4726 0.3698 0.094 Uiso 1 1 calc R . . Cl1 Cl 0.52452(11) 0.31304(11) 0.41671(4) 0.0522(3) Uani 1 1 d D . . O11 O 0.6576(8) 0.3394(13) 0.4218(5) 0.080(3) Uani 0.731(15) 1 d PDU A 1 O12 O 0.4338(8) 0.1605(5) 0.4119(4) 0.098(3) Uani 0.731(15) 1 d PDU A 1 O13 O 0.4701(9) 0.3487(10) 0.4650(3) 0.070(2) Uani 0.731(15) 1 d PDU A 1 O14 O 0.5026(8) 0.3626(11) 0.3629(2) 0.083(2) Uani 0.731(15) 1 d PDU A 1 O15 O 0.4874(16) 0.1909(16) 0.4497(8) 0.069(6) Uani 0.269(15) 1 d PDU A 2 O16 O 0.498(3) 0.400(3) 0.4496(11) 0.091(8) Uani 0.269(15) 1 d PDU A 2 O17 O 0.4836(16) 0.281(2) 0.3602(4) 0.064(5) Uani 0.269(15) 1 d PDU A 2 O18 O 0.6740(14) 0.375(3) 0.4193(10) 0.063(6) Uani 0.269(15) 1 d PDU A 2 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 0.0401(3) 0.0523(4) 0.0239(3) -0.0018(3) -0.00088(13) 0.0261(2) O1 0.0600(16) 0.084(2) 0.0273(11) -0.0103(11) -0.0089(10) 0.0535(16) O2 0.0528(16) 0.091(4) 0.047(2) 0.004(2) 0.0020(11) 0.0454(18) N1 0.0425(15) 0.0464(15) 0.0264(12) -0.0033(10) -0.0050(10) 0.0260(12) N11 0.0510(19) 0.058(2) 0.0374(15) 0.0040(12) 0.0057(13) 0.0263(17) C1 0.0387(16) 0.0477(19) 0.0255(14) 0.0009(14) -0.0023(11) 0.0226(15) C2 0.0420(18) 0.061(2) 0.0305(15) 0.0060(14) 0.0022(12) 0.0259(17) C3 0.0426(19) 0.063(2) 0.0339(17) 0.0002(15) -0.0084(13) 0.0167(18) C4 0.059(2) 0.059(2) 0.0342(17) -0.0082(15) -0.0072(16) 0.027(2) C5 0.053(2) 0.051(2) 0.0293(16) -0.0040(13) -0.0079(14) 0.0290(17) C6 0.061(2) 0.067(2) 0.0311(16) -0.0138(15) -0.0127(15) 0.044(2) C7 0.067(2) 0.102(3) 0.0278(16) -0.0038(18) -0.0007(16) 0.060(3) C8 0.149(6) 0.135(6) 0.058(3) 0.049(3) 0.050(3) 0.109(6) C9 0.069(3) 0.230(9) 0.029(2) -0.014(3) -0.013(2) 0.075(5) C10 0.077(3) 0.143(5) 0.0359(19) -0.015(2) 0.0000(19) 0.074(4) C11 0.054(2) 0.064(3) 0.0390(18) 0.0085(17) 0.0055(16) 0.035(2) C12 0.060(3) 0.063(3) 0.070(3) 0.025(2) 0.013(2) 0.033(2) Cl1 0.0655(6) 0.0705(6) 0.0345(4) -0.0064(4) 0.0004(4) 0.0444(5) O11 0.071(4) 0.113(7) 0.095(6) 0.006(4) 0.004(4) 0.075(5) O12 0.110(5) 0.071(3) 0.076(5) -0.021(3) 0.036(4) 0.018(3) O13 0.082(4) 0.111(6) 0.042(2) -0.021(3) -0.003(2) 0.066(4) O14 0.105(5) 0.120(7) 0.045(2) 0.012(3) -0.007(3) 0.072(5) O15 0.075(9) 0.075(9) 0.076(11) 0.021(8) 0.015(7) 0.053(7) O16 0.115(14) 0.108(14) 0.105(15) -0.055(11) -0.032(11) 0.096(12) O17 0.090(9) 0.071(9) 0.030(5) -0.006(5) -0.027(5) 0.040(7) O18 0.071(11) 0.077(11) 0.042(8) -0.001(7) -0.015(6) 0.037(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 N11 . 4 2.153(3) y Fe1 N11 . . 2.153(4) y Fe1 O1 . 4 2.186(2) y Fe1 O1 . . 2.186(2) y Fe1 N1 . . 2.225(3) y Fe1 N1 . 4 2.225(3) y Fe1 O2 . . 2.286(4) y O1 C6 . . 1.428(4) y O1 H1 . . 0.840(11) ? O2 H2 . . 0.837(11) ? N1 C1 . . 1.343(4) y N1 C5 . . 1.344(4) y N11 C11 . . 1.134(5) y C1 C2 . . 1.391(5) y C1 C1 . 4 1.480(6) y C2 C3 . . 1.383(5) y C2 H2a . . 0.9500 ? C3 C4 . . 1.358(6) y C3 H3 . . 0.9500 ? C4 C5 . . 1.392(6) y C4 H4 . . 0.9500 ? C5 C6 . . 1.512(5) y C6 C7 . . 1.545(6) y C6 H6 . . 1.0000 ? C7 C8 . . 1.491(8) y C7 C10 . . 1.530(6) y C7 C9 . . 1.534(7) y C8 H8a . . 0.9800 ? C8 H8b . . 0.9800 ? C8 H8c . . 0.9800 ? C9 H9a . . 0.9800 ? C9 H9b . . 0.9800 ? C9 H9c . . 0.9800 ? C10 H10a . . 0.9800 ? C10 H10b . . 0.9800 ? C10 H10c . . 0.9800 ? C11 C12 . . 1.462(6) y C12 H12a . . 0.9800 ? C12 H12b . . 0.9800 ? C12 H12c . . 0.9800 ? Cl1 O17 . . 1.343(9) y Cl1 O11 . . 1.367(6) y Cl1 O16 . . 1.371(12) y Cl1 O13 . . 1.400(5) y Cl1 O14 . . 1.406(5) y Cl1 O15 . . 1.421(9) y Cl1 O18 . . 1.454(13) y Cl1 O12 . . 1.488(5) y loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N11 FE1 N11 4 . . 169.24(19) y N11 FE1 O1 4 . 4 90.61(12) y N11 FE1 O1 . . 4 86.43(12) y N11 FE1 O1 4 . . 86.43(12) y N11 FE1 O1 . . . 90.61(12) y O1 FE1 O1 4 . . 148.05(14) y N11 FE1 N1 4 . . 90.57(12) y N11 FE1 N1 . . . 98.11(12) y O1 FE1 N1 4 . . 142.14(10) y O1 FE1 N1 . . . 69.76(10) y N11 FE1 N1 4 . 4 98.11(12) y N11 FE1 N1 . . 4 90.57(12) y O1 FE1 N1 4 . 4 69.76(10) y O1 FE1 N1 . . 4 142.14(10) y N1 FE1 N1 . . 4 72.61(14) y N11 FE1 O2 4 . . 84.62(9) y N11 FE1 O2 . . . 84.62(9) y O1 FE1 O2 4 . . 74.02(7) y O1 FE1 O2 . . . 74.02(7) y N1 FE1 O2 . . . 143.69(7) y N1 FE1 O2 4 . . 143.69(7) y C6 O1 FE1 . . . 124.6(2) y C6 O1 H1 . . . 114(4) ? FE1 O1 H1 . . . 117(4) ? FE1 O2 H2 . . . 129(4) ? C1 N1 C5 . . . 120.0(3) y C1 N1 FE1 . . . 117.3(2) y C5 N1 FE1 . . . 120.1(2) y C11 N11 FE1 . . . 166.1(3) y N1 C1 C2 . . . 121.4(3) y N1 C1 C1 . . 4 114.40(19) y C2 C1 C1 . . 4 124.2(2) y C3 C2 C1 . . . 118.2(3) y C3 C2 H2A . . . 120.9 ? C1 C2 H2A . . . 120.9 ? C4 C3 C2 . . . 120.2(3) y C4 C3 H3 . . . 119.9 ? C2 C3 H3 . . . 119.9 ? C3 C4 C5 . . . 119.6(4) y C3 C4 H4 . . . 120.2 ? C5 C4 H4 . . . 120.2 ? N1 C5 C4 . . . 120.6(4) y N1 C5 C6 . . . 115.2(3) y C4 C5 C6 . . . 124.3(3) y O1 C6 C5 . . . 106.7(3) y O1 C6 C7 . . . 110.1(4) y C5 C6 C7 . . . 115.4(3) y O1 C6 H6 . . . 108.1 ? C5 C6 H6 . . . 108.1 ? C7 C6 H6 . . . 108.1 ? C8 C7 C10 . . . 110.4(6) y C8 C7 C9 . . . 110.1(5) y C10 C7 C9 . . . 107.6(4) y C8 C7 C6 . . . 110.2(3) y C10 C7 C6 . . . 109.0(3) y C9 C7 C6 . . . 109.5(5) y C7 C8 H8A . . . 109.5 ? C7 C8 H8B . . . 109.5 ? H8A C8 H8B . . . 109.5 ? C7 C8 H8C . . . 109.5 ? H8A C8 H8C . . . 109.5 ? H8B C8 H8C . . . 109.5 ? C7 C9 H9A . . . 109.5 ? C7 C9 H9B . . . 109.5 ? H9A C9 H9B . . . 109.5 ? C7 C9 H9C . . . 109.5 ? H9A C9 H9C . . . 109.5 ? H9B C9 H9C . . . 109.5 ? C7 C10 H10A . . . 109.5 ? C7 C10 H10B . . . 109.5 ? H10A C10 H10B . . . 109.5 ? C7 C10 H10C . . . 109.5 ? H10A C10 H10C . . . 109.5 ? H10B C10 H10C . . . 109.5 ? N11 C11 C12 . . . 179.3(5) y C11 C12 H12A . . . 109.5 ? C11 C12 H12B . . . 109.5 ? H12A C12 H12B . . . 109.5 ? C11 C12 H12C . . . 109.5 ? H12A C12 H12C . . . 109.5 ? H12B C12 H12C . . . 109.5 ? O17 CL1 O16 . . . 122.5(11) y O11 CL1 O13 . . . 116.9(6) y O11 CL1 O14 . . . 111.9(6) y O13 CL1 O14 . . . 112.1(4) y O16 CL1 O15 . . . 109.7(11) y O17 CL1 O18 . . . 108.8(11) y O16 CL1 O18 . . . 104.0(14) y O15 CL1 O17 . . . 110.3(9) y O15 CL1 O18 . . . 98.8(11) y O11 CL1 O12 . . . 107.3(6) y O13 CL1 O12 . . . 103.9(4) y O14 CL1 O12 . . . 103.6(4) y 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N11 FE1 O1 C6 4 . . . -85.6(3) y N11 FE1 O1 C6 . . . . 104.8(3) y O1 FE1 O1 C6 4 . . . -171.0(3) y N1 FE1 O1 C6 . . . . 6.4(3) y N1 FE1 O1 C6 4 . . . 13.1(4) y O2 FE1 O1 C6 . . . . -171.0(3) y N11 FE1 N1 C1 4 . . . -91.7(3) y N11 FE1 N1 C1 . . . . 94.6(3) y O1 FE1 N1 C1 4 . . . 0.0(3) y O1 FE1 N1 C1 . . . . -177.7(3) y N1 FE1 N1 C1 4 . . . 6.59(18) y O2 FE1 N1 C1 . . . . -173.41(19) y N11 FE1 N1 C5 4 . . . 70.0(3) y N11 FE1 N1 C5 . . . . -103.6(3) y O1 FE1 N1 C5 4 . . . 161.8(2) y O1 FE1 N1 C5 . . . . -16.0(3) y N1 FE1 N1 C5 4 . . . 168.3(3) y O2 FE1 N1 C5 . . . . -11.7(3) y N11 FE1 N11 C11 4 . . . 26.7(14) y O1 FE1 N11 C11 4 . . . -47.6(14) y O1 FE1 N11 C11 . . . . 100.6(14) y N1 FE1 N11 C11 . . . . 170.2(14) y N1 FE1 N11 C11 4 . . . -117.2(14) y O2 FE1 N11 C11 . . . . 26.7(14) y C5 N1 C1 C2 . . . . -0.3(5) y FE1 N1 C1 C2 . . . . 161.5(3) y C5 N1 C1 C1 . . . 4 -179.3(3) y FE1 N1 C1 C1 . . . 4 -17.6(5) y N1 C1 C2 C3 . . . . -2.0(5) y C1 C1 C2 C3 4 . . . 176.9(4) y C1 C2 C3 C4 . . . . 1.8(6) y C2 C3 C4 C5 . . . . 0.6(6) y C1 N1 C5 C4 . . . . 2.8(5) y FE1 N1 C5 C4 . . . . -158.4(3) y C1 N1 C5 C6 . . . . -175.7(3) y FE1 N1 C5 C6 . . . . 23.1(4) y C3 C4 C5 N1 . . . . -3.0(6) y C3 C4 C5 C6 . . . . 175.3(4) y FE1 O1 C6 C5 . . . . 2.3(4) y FE1 O1 C6 C7 . . . . -123.6(3) y N1 C5 C6 O1 . . . . -15.6(5) y C4 C5 C6 O1 . . . . 166.0(4) y N1 C5 C6 C7 . . . . 107.1(4) y C4 C5 C6 C7 . . . . -71.3(5) y O1 C6 C7 C8 . . . . 72.0(5) y C5 C6 C7 C8 . . . . -48.9(6) y O1 C6 C7 C10 . . . . -49.4(5) y C5 C6 C7 C10 . . . . -170.2(4) y O1 C6 C7 C9 . . . . -166.8(4) y C5 C6 C7 C9 . . . . 72.4(5) y 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 _geom_hbond_publ_flag O1 H1 O15 0.840(11) 1.99(2) 2.811(13) 166(5) . y O1 H1 O12 0.840(11) 2.220(19) 3.044(10) 167(5) . y O1 H1 O11 0.840(11) 2.37(5) 2.916(13) 123(4) . y O2 H2 O12 0.837(11) 1.99(5) 2.665(6) 138(6) 4 y O2 H2 O17 0.837(11) 2.29(3) 3.10(2) 162(5) 4 y _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 70.61 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.477 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.071 _vrf_PLAT430_olev34 ; PROBLEM: Short Inter D...A Contact O13 .. O13 .. 2.83 Ang. RESPONSE: Disorder was identified in ClO4 anion. All the O atoms were affected and two orientations were identified. Similarity restraints were applied to Cl-O distances and to O-Cl-O angles. All O atoms were refined anisotropically with ISOR .02. The occupancies of each group of four partially-occupied O atoms were refined competitively using a free variapble. The final group occupancies of 0.73 and 0.27. ; _vrf_PLAT213_olev34 ; PROBLEM: Atom C9 has ADP max/min Ratio ..... 3.1 prola RESPONSE:Some degree of disorder as commonly observed in tBu group (C7-C8,C9,C10) is not solved, so the long ellipsoid remains. ; _iucr_refine_instructions_details ; TITL olev34 in P3(1)21 CELL 1.54178 11.1665 11.1665 22.5811 90.000 90.000 120.000 ZERR 3.00 0.0005 0.0005 0.0010 0.000 0.000 0.000 LATT -1 SYMM -Y,X-Y,1/3+Z SYMM -X+Y,-X,2/3+Z SYMM X-Y,-Y,2/3-Z SYMM -X,-X+Y,1/3-Z SYMM Y,X,-Z SFAC C H N O Cl Fe UNIT 72 108 12 33 6 3 SIZE 0.06 0.08 0.2 TEMP -173 L.S. 8 ACTA BOND $H CONF WPDB -1 FMAP 2 PLAN -5 TWIN DFIX 0.84 .01 O1 H1 O2 H2 HTAB REM O1-H1 0.840 1.990 165.33 2.811 O15_b REM O1-H1 0.840 2.218 167.20 3.043 O12_a REM O1-H1 0.840 2.378 122.42 2.916 O11_a REM O2-H2 0.837 1.988 137.25 2.664 O12_a [ x-y, -y, -z+2/3 ] REM O2-H2 0.837 2.292 162.30 3.100 O17_b [ x-y, -y, -z+2/3 ] EQIV $1 x-y, -y, -z+2/3 HTAB O1 O15 HTAB O1 O12 HTAB O1 O11 HTAB O2 O12_$1 HTAB O2 O17_$1 WGHT 0.106200 0.241700 BASF -0.00453 FVAR 0.13671 0.73077 FE1 6 0.669637 0.000000 0.333333 10.50000 0.04006 0.05227 = 0.02386 -0.00176 -0.00088 0.02613 O1 4 0.654055 0.076609 0.420431 11.00000 0.06001 0.08436 = 0.02732 -0.01026 -0.00890 0.05347 H1 2 0.595907 0.102887 0.424162 11.00000 0.06304 O2 4 0.464944 0.000000 0.333333 10.50000 0.05278 0.09077 = 0.04663 0.00400 0.00200 0.04539 H2 2 0.385380 -0.065187 0.325873 11.00000 0.07925 N1 3 0.858831 0.057240 0.386278 11.00000 0.04254 0.04640 = 0.02643 -0.00330 -0.00505 0.02599 N11 3 0.546440 -0.210253 0.363383 11.00000 0.05098 0.05825 = 0.03741 0.00404 0.00572 0.02631 C1 1 0.959769 0.044447 0.360001 11.00000 0.03871 0.04767 = 0.02550 0.00088 -0.00233 0.02261 C2 1 1.094347 0.112400 0.381780 11.00000 0.04203 0.06084 = 0.03052 0.00598 0.00223 0.02588 AFIX 43 H2A 2 1.164525 0.100526 0.363687 11.00000 -1.20000 AFIX 0 C3 1 1.123237 0.197671 0.430456 11.00000 0.04263 0.06350 = 0.03386 0.00018 -0.00844 0.01670 AFIX 43 H3 2 1.214868 0.247332 0.445504 11.00000 -1.20000 AFIX 0 C4 1 1.020974 0.210620 0.456809 11.00000 0.05928 0.05915 = 0.03420 -0.00820 -0.00724 0.02692 AFIX 43 H4 2 1.040918 0.269871 0.490023 11.00000 -1.20000 AFIX 0 C5 1 0.886746 0.136505 0.434835 11.00000 0.05346 0.05123 = 0.02929 -0.00403 -0.00789 0.02897 C6 1 0.763017 0.134502 0.463083 11.00000 0.06143 0.06672 = 0.03107 -0.01375 -0.01273 0.04379 AFIX 13 H6 2 0.787021 0.232270 0.470611 11.00000 -1.20000 AFIX 0 C7 1 0.713848 0.054057 0.522055 11.00000 0.06656 0.10222 = 0.02776 -0.00380 -0.00074 0.05987 C8 1 0.700508 -0.085063 0.515746 11.00000 0.14908 0.13498 = 0.05833 0.04943 0.04979 0.10911 AFIX 137 H8A 2 0.791758 -0.074342 0.508102 11.00000 -1.50000 H8B 2 0.638504 -0.134433 0.482642 11.00000 -1.50000 H8C 2 0.662495 -0.137827 0.552349 11.00000 -1.50000 AFIX 0 C9 1 0.817627 0.136163 0.571214 11.00000 0.06933 0.22999 = 0.02921 -0.01438 -0.01337 0.07498 AFIX 137 H9A 2 0.781428 0.090420 0.609376 11.00000 -1.50000 H9B 2 0.831898 0.230139 0.572628 11.00000 -1.50000 H9C 2 0.905852 0.140381 0.563044 11.00000 -1.50000 AFIX 0 C10 1 0.574857 0.039924 0.539287 11.00000 0.07657 0.14325 = 0.03591 -0.01524 0.00001 0.07354 AFIX 137 H10A 2 0.500872 -0.034481 0.516107 11.00000 -1.50000 H10B 2 0.576756 0.127095 0.531231 11.00000 -1.50000 H10C 2 0.557903 0.018103 0.581563 11.00000 -1.50000 AFIX 0 C11 1 0.460887 -0.319477 0.373275 11.00000 0.05397 0.06437 = 0.03896 0.00850 0.00550 0.03473 C12 1 0.349372 -0.459752 0.386069 11.00000 0.05955 0.06267 = 0.06992 0.02541 0.01348 0.03348 AFIX 137 H12A 2 0.340301 -0.474035 0.429024 11.00000 -1.50000 H12B 2 0.370681 -0.526701 0.367972 11.00000 -1.50000 H12C 2 0.262377 -0.472555 0.369788 11.00000 -1.50000 AFIX 0 SADI .02 CL1 O11 CL1 O12 CL1 O13 CL1 O14 CL1 O15 CL1 O16 CL1 O17 CL1 O18 SADI .04 O11 O12 O11 O13 O11 O14 O12 O13 O12 O14 O13 O14 = O15 O16 O15 O17 O15 O18 O16 O17 O16 O18 O17 O18 CL1 5 0.524520 0.313037 0.416714 11.00000 0.06550 0.07046 = 0.03451 -0.00641 0.00045 0.04436 REM SIMU 0.04 0.08 .7 O11 > O18 ISOR .02 O11 > O18 PART 1 O11 4 0.657566 0.339441 0.421826 21.00000 0.07056 0.11290 = 0.09472 0.00605 0.00381 0.07536 O12 4 0.433836 0.160496 0.411866 21.00000 0.11043 0.07070 = 0.07558 -0.02124 0.03587 0.01808 O13 4 0.470149 0.348720 0.465035 21.00000 0.08172 0.11080 = 0.04178 -0.02063 -0.00271 0.06574 O14 4 0.502605 0.362640 0.362926 21.00000 0.10452 0.12044 = 0.04465 0.01151 -0.00730 0.07185 PART 2 O15 4 0.487378 0.190894 0.449668 -21.00000 0.07525 0.07471 = 0.07638 0.02135 0.01495 0.05295 O16 4 0.498097 0.400488 0.449577 -21.00000 0.11506 0.10811 = 0.10461 -0.05543 -0.03181 0.09591 O17 4 0.483582 0.281236 0.360150 -21.00000 0.09007 0.07069 = 0.03047 -0.00636 -0.02704 0.04009 O18 4 0.674033 0.375414 0.419256 -21.00000 0.07087 0.07672 = 0.04216 -0.00135 -0.01519 0.03691 part 0 HKLF 4 REM olev34 in P3(1)21 REM R1 = 0.0497 for 2813 Fo > 4sig(Fo) and 0.0559 for all 3129 data REM 241 parameters refined using 144 restraints END WGHT 0.1060 0.2474 REM Highest difference peak 0.477, deepest hole -0.266, 1-sigma level 0.071 Q1 1 0.5779 -0.1062 0.3374 11.00000 0.05 0.48 Q2 1 0.5639 0.0000 0.3333 10.50000 0.05 0.42 Q3 1 0.7691 0.0000 0.3333 10.50000 0.05 0.39 Q4 1 0.7794 0.0847 0.3423 11.00000 0.05 0.39 Q5 1 0.6089 0.4149 0.3918 11.00000 0.05 0.36 ;