data_CB6 _audit_creation_method SHELXL-2014 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H27 Cl Fe N8 O2, 2(Cl O4), C3 H6 O' _chemical_formula_sum 'C41 H33 Cl3 Fe N8 O11' _chemical_formula_weight 975.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_H-M_alt 'P 21' _space_group_name_Hall 'P 2yb' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.471(6) _cell_length_b 22.725(18) _cell_length_c 10.833(8) _cell_angle_alpha 90 _cell_angle_beta 103.120(16) _cell_angle_gamma 90 _cell_volume 2031(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1115 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 19.36 _exptl_crystal_description parallelepiped _exptl_crystal_colour red _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_F_000 1000 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.040 _exptl_absorpt_coefficient_mu 0.643 _shelx_estimated_absorpt_T_min 0.910 _shelx_estimated_absorpt_T_max 0.975 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.610 _exptl_absorpt_correction_T_max 0.745 _exptl_absorpt_process_details 'SADABS-2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'multilayer monochromator ImuS' _diffrn_measurement_device_type 'Bruker APEX II QUAZAR' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6487 _diffrn_reflns_av_unetI/netI 0.1158 _diffrn_reflns_av_R_equivalents 0.0741 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.469 _diffrn_reflns_theta_max 19.389 _diffrn_reflns_theta_full 19.400 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_point_group_measured_fraction_full 0.991 _reflns_number_total 3427 _reflns_number_gt 2673 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.922 _reflns_Friedel_fraction_max 0.985 _reflns_Friedel_fraction_full 0.985 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS (Sheldrick 2008)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; All non-hydrogens were refined anisotropically. Likely n part due to the poor data over parameters ratio, a significant number of atoms of the main residue as well as the whole lattice acetone molecule required displacement parameters restraints to refine properly. Hydrogens were placed geometrically on their carrier atom and refined with a riding model, except that on O2 that was refined with distance restraints and its thermal parameter 1.2 times that of O2. ; _vrf_THETM01_CB6 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.4671 RESPONSE: Repeatedly on several crystals, there was significant diffraction only up to ca. 1.05 angstrom. The present data were cut at 1.07. Similar resolutions were obtained on crystals from another batch and synchrotron radiation (ALS beamline 11.3.1), indicating the diffraction drop is intrinsic to the available crystals. The results are low themamax and thefull and poor data over parameters ratio. ; _vrf_PLAT090_CB6 ; PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........ 3.07 RESPONSE: Repeatedly on several crystals, there was significant diffraction only up to ca. 1.05 angstrom. The present data were cut at 1.07. Similar resolutions were obtained on crystals from another batch and synchrotron radiation (ALS beamline 11.3.1), indicating the diffraction drop is intrinsic to the available crystals. The results are low themamax and thefull and poor data over parameters ratio. For the later, we have had to use a number of displacement restraints so that it cannot be improved in such a way. ; _vrf_REFNR01_CB6 ; PROBLEM: Ratio of reflections to parameters is < 6 for a non-centrosymmetric structure, where ZMAX > 18 sine(theta)/lambda 0.4671 Proportion of unique data used 1.0000 Ratio reflections to parameters 5.8782 RESPONSE: Repeatedly on several crystals, there was significant diffraction only up to ca. 1.05 angstrom. The present data were cut at 1.07. Similar resolutions were obtained on crystals from another batch and synchrotron radiation (ALS beamline 11.3.1), indicating the diffraction drop is intrinsic to the available crystals. The results are low themamax and thefull and poor data over parameters ratio. For the later, we have had to use a number of displacement restraints so that it cannot be improved in such a way. ; _vrf_PLAT341_CB6 ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0217 Ang. RESPONSE: This is clearly related to poor data over parameter ratio (see other alters). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0090P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 1021 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.08(3) _chemical_absolute_configuration ? _refine_ls_number_reflns 3427 _refine_ls_number_parameters 583 _refine_ls_number_restraints 425 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.0835 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.7066(2) 0.04030(10) 0.95425(17) 0.0165(6) Uani 1 1 d . . . . . Cl1 Cl 0.9793(5) 0.1891(2) 1.4489(3) 0.0367(13) Uani 1 1 d . . . . . O1 O 0.5644(14) 0.2701(5) 0.9305(9) 0.038(3) Uani 1 1 d . . . . . H1 H 0.6313 0.2963 0.9628 0.057 Uiso 1 1 calc R U . . . O2 O 1.1376(13) -0.0923(6) 1.2998(10) 0.049(4) Uani 1 1 d D . . . . H2 H 1.074(15) -0.072(6) 1.340(7) 0.073 Uiso 1 1 d D U . . . N1 N 0.5686(13) 0.1631(5) 0.8524(10) 0.019(3) Uani 1 1 d . U . . . H1A H 0.6050 0.1845 0.9207 0.022 Uiso 1 1 calc R U . . . N2 N 0.5927(13) 0.1050(6) 0.8446(10) 0.015(3) Uani 1 1 d . U . . . N3 N 0.6227(14) -0.0026(6) 0.7998(10) 0.018(3) Uani 1 1 d . U . . . N4 N 0.7927(14) -0.0411(5) 0.9998(11) 0.015(3) Uani 1 1 d . U . . . N5 N 0.8887(13) -0.0688(6) 1.0992(10) 0.018(3) Uani 1 1 d . . . . . H5B H 0.9341 -0.0515 1.1713 0.022 Uiso 1 1 calc R U . . . N7 N 0.9138(13) 0.0654(5) 0.9178(10) 0.014(3) Uani 1 1 d . U . . . N8 N 0.7880(16) 0.0853(6) 1.1010(10) 0.018(4) Uani 1 1 d . . . . . N9 N 0.5278(14) 0.0267(5) 1.0410(10) 0.017(3) Uani 1 1 d . . . . . C1 C 0.475(2) 0.2894(7) 0.8183(14) 0.028(4) Uani 1 1 d . U . . . C2 C 0.4263(19) 0.3461(7) 0.7962(15) 0.032(4) Uani 1 1 d . U . . . H2A H 0.4552 0.3744 0.8621 0.038 Uiso 1 1 calc R U . . . C3 C 0.3358(19) 0.3632(8) 0.6797(14) 0.034(4) Uani 1 1 d . U . . . H3A H 0.3059 0.4033 0.6649 0.040 Uiso 1 1 calc R U . . . C4 C 0.2873(18) 0.3218(8) 0.5828(14) 0.029(5) Uani 1 1 d . . . . . H4A H 0.2217 0.3331 0.5030 0.034 Uiso 1 1 calc R U . . . C5 C 0.3366(17) 0.2645(8) 0.6055(13) 0.025(4) Uani 1 1 d . U . . . H5A H 0.3049 0.2363 0.5400 0.030 Uiso 1 1 calc R U . . . C6 C 0.4314(17) 0.2467(7) 0.7216(13) 0.019(3) Uani 1 1 d . U . . . C7 C 0.4801(17) 0.1848(8) 0.7401(13) 0.017(3) Uani 1 1 d . U . . . C8 C 0.4476(16) 0.1377(7) 0.6574(13) 0.014(3) Uani 1 1 d . U . . . H8A H 0.3885 0.1385 0.5717 0.017 Uiso 1 1 calc R U . . . C9 C 0.5185(16) 0.0892(7) 0.7249(12) 0.016(4) Uani 1 1 d . . . . . C10 C 0.5343(16) 0.0277(7) 0.6980(12) 0.015(4) Uani 1 1 d . U . . . C11 C 0.4699(17) -0.0022(8) 0.5836(12) 0.020(4) Uani 1 1 d . U . . . H11A H 0.4057 0.0177 0.5127 0.024 Uiso 1 1 calc R U . . . C12 C 0.5035(18) -0.0618(8) 0.5781(15) 0.030(5) Uani 1 1 d . . . . . H12A H 0.4651 -0.0825 0.5010 0.035 Uiso 1 1 calc R U . . . C13 C 0.5924(17) -0.0919(7) 0.6837(13) 0.024(4) Uani 1 1 d . U . . . H13A H 0.6106 -0.1331 0.6804 0.028 Uiso 1 1 calc R U . . . C14 C 0.6522(17) -0.0606(7) 0.7913(14) 0.021(3) Uani 1 1 d . U . . . C15 C 0.7526(17) -0.0823(7) 0.9102(13) 0.019(3) Uani 1 1 d . U . . . C16 C 0.8209(17) -0.1366(7) 0.9503(13) 0.022(3) Uani 1 1 d . U . . . H16A H 0.8116 -0.1724 0.9040 0.026 Uiso 1 1 calc R U . . . C17 C 0.9061(18) -0.1264(8) 1.0739(13) 0.022(4) Uani 1 1 d . U . . . C18 C 1.0026(19) -0.1675(8) 1.1646(14) 0.020(4) Uani 1 1 d . U . . . C19 C 0.9904(19) -0.2282(9) 1.1411(14) 0.035(5) Uani 1 1 d . . . . . H19A H 0.9161 -0.2417 1.0671 0.042 Uiso 1 1 calc R U . . . C20 C 1.081(2) -0.2692(8) 1.2205(16) 0.037(5) Uani 1 1 d . . . . . H20A H 1.0701 -0.3100 1.2012 0.045 Uiso 1 1 calc R U . . . C21 C 1.1898(19) -0.2500(8) 1.3291(15) 0.032(4) Uani 1 1 d . U . . . H21A H 1.2522 -0.2778 1.3854 0.039 Uiso 1 1 calc R U . . . C22 C 1.2069(19) -0.1918(8) 1.3551(14) 0.031(4) Uani 1 1 d . U . . . H22A H 1.2824 -0.1788 1.4288 0.037 Uiso 1 1 calc R U . . . C23 C 1.1152(19) -0.1512(8) 1.2747(15) 0.027(4) Uani 1 1 d . U . . . C24 C 0.9640(18) 0.0544(7) 0.8131(12) 0.021(4) Uani 1 1 d . . . . . H24A H 0.9007 0.0299 0.7498 0.025 Uiso 1 1 calc R U . . . C25 C 1.110(2) 0.0785(7) 0.7938(14) 0.030(5) Uani 1 1 d . . . . . H25A H 1.1434 0.0702 0.7178 0.036 Uiso 1 1 calc R U . . . C26 C 1.2030(18) 0.1139(8) 0.8846(14) 0.029(4) Uani 1 1 d . U . . . H26A H 1.3009 0.1307 0.8721 0.034 Uiso 1 1 calc R U . . . C27 C 1.1511(16) 0.1245(7) 0.9943(13) 0.020(3) Uani 1 1 d . U . . . H27A H 1.2152 0.1475 1.0604 0.024 Uiso 1 1 calc R U . . . C28 C 1.0053(16) 0.1014(7) 1.0072(12) 0.016(3) Uani 1 1 d . U . . . C29 C 0.9347(18) 0.1108(7) 1.1169(13) 0.018(4) Uani 1 1 d . . . . . C30 C 1.0012(19) 0.1439(7) 1.2241(13) 0.024(4) Uani 1 1 d . U . . . H30A H 1.1053 0.1616 1.2372 0.028 Uiso 1 1 calc R U . . . C31 C 0.9030(18) 0.1491(7) 1.3110(13) 0.020(3) Uani 1 1 d . U . . . C32 C 0.7521(17) 0.1252(7) 1.2946(13) 0.021(4) Uani 1 1 d . U . . . H32A H 0.6881 0.1313 1.3551 0.025 Uiso 1 1 calc R U . . . C33 C 0.6949(18) 0.0916(7) 1.1862(13) 0.021(3) Uani 1 1 d . U . . . C34 C 0.5438(17) 0.0569(6) 1.1556(13) 0.018(3) Uani 1 1 d . U . . . C35 C 0.4320(17) 0.0503(7) 1.2291(12) 0.025(4) Uani 1 1 d . U . . . H35A H 0.4435 0.0723 1.3053 0.030 Uiso 1 1 calc R U . . . C36 C 0.3024(18) 0.0118(7) 1.1923(13) 0.030(4) Uani 1 1 d . U . . . H36A H 0.2241 0.0074 1.2421 0.036 Uiso 1 1 calc R U . . . C37 C 0.2902(18) -0.0195(7) 1.0829(14) 0.027(4) Uani 1 1 d . U . . . H37A H 0.2059 -0.0475 1.0571 0.032 Uiso 1 1 calc R U . . . C38 C 0.4016(17) -0.0099(7) 1.0108(13) 0.020(4) Uani 1 1 d . U . . . H38A H 0.3878 -0.0309 0.9333 0.024 Uiso 1 1 calc R U . . . Cl2 Cl 0.4251(5) 0.2292(2) 0.2820(4) 0.0292(13) Uani 1 1 d . . . . . O3 O 0.4493(13) 0.2104(5) 0.1622(10) 0.048(4) Uani 1 1 d . . . . . O4 O 0.2753(12) 0.2619(5) 0.2658(10) 0.041(3) Uani 1 1 d . . . . . O5 O 0.5606(13) 0.2649(5) 0.3423(10) 0.045(3) Uani 1 1 d . . . . . O6 O 0.4135(13) 0.1773(5) 0.3583(9) 0.041(3) Uani 1 1 d . . . . . Cl3 Cl 0.9760(7) 0.0073(2) 1.4546(4) 0.0517(16) Uani 1 1 d . . . . . O7 O 0.9064(14) 0.0016(5) 1.3209(9) 0.047(4) Uani 1 1 d D . . . . O8 O 1.1086(14) 0.0504(6) 1.4727(10) 0.062(4) Uani 1 1 d . . . . . O9 O 1.045(2) -0.0476(7) 1.5005(11) 0.099(6) Uani 1 1 d D U . . . O10 O 0.8534(15) 0.0266(8) 1.5162(10) 0.091(5) Uani 1 1 d . U . . . O1S O 0.6718(16) 0.3583(5) 1.0918(10) 0.062(4) Uani 1 1 d . U . . . C1S C 0.791(2) 0.3422(9) 1.1682(16) 0.050(6) Uani 1 1 d . U . . . C2S C 0.859(2) 0.2827(8) 1.1712(15) 0.057(5) Uani 1 1 d . U . . . H2SA H 0.8510 0.2689 1.0843 0.086 Uiso 1 1 calc R U . . . H2SB H 0.7978 0.2561 1.2144 0.086 Uiso 1 1 calc R U . . . H2SC H 0.9728 0.2833 1.2169 0.086 Uiso 1 1 calc R U . . . C3S C 0.869(2) 0.3817(10) 1.2717(17) 0.091(8) Uani 1 1 d . U . . . H3SA H 0.8167 0.4203 1.2596 0.136 Uiso 1 1 calc R U . . . H3SB H 0.9843 0.3859 1.2714 0.136 Uiso 1 1 calc R U . . . H3SC H 0.8588 0.3651 1.3530 0.136 Uiso 1 1 calc R U . . . 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 0.0202(13) 0.0198(16) 0.0089(11) 0.0001(12) 0.0020(10) -0.0013(13) Cl1 0.040(3) 0.051(4) 0.018(2) -0.019(2) 0.005(2) -0.007(3) O1 0.057(9) 0.032(9) 0.015(7) 0.004(6) -0.010(6) -0.005(7) O2 0.049(9) 0.037(10) 0.050(8) 0.003(7) -0.011(7) 0.003(8) N1 0.026(6) 0.022(5) 0.008(5) 0.001(5) 0.004(5) -0.003(6) N2 0.017(5) 0.019(5) 0.009(5) 0.005(4) 0.001(4) -0.002(5) N3 0.021(7) 0.027(6) 0.007(6) -0.001(5) 0.004(5) -0.001(6) N4 0.021(6) 0.011(6) 0.012(5) 0.007(5) 0.004(5) 0.001(6) N5 0.020(8) 0.015(10) 0.014(7) 0.002(7) -0.008(6) 0.002(7) N7 0.016(5) 0.019(6) 0.010(5) 0.002(4) 0.008(4) -0.003(4) N8 0.026(9) 0.017(10) 0.011(7) -0.003(7) 0.006(7) 0.008(8) N9 0.016(7) 0.016(10) 0.016(7) 0.001(7) 0.000(6) 0.000(8) C1 0.042(11) 0.024(10) 0.017(9) -0.004(8) 0.007(8) -0.001(9) C2 0.050(10) 0.026(9) 0.020(7) -0.009(8) 0.010(7) 0.006(9) C3 0.040(9) 0.031(10) 0.031(8) 0.004(8) 0.009(7) 0.006(8) C4 0.028(11) 0.029(13) 0.027(11) 0.016(10) 0.000(9) 0.009(11) C5 0.032(10) 0.020(9) 0.023(8) 0.003(7) 0.007(7) 0.009(8) C6 0.012(7) 0.024(6) 0.023(7) 0.004(6) 0.010(6) 0.001(6) C7 0.014(7) 0.022(6) 0.015(6) 0.002(5) 0.004(5) 0.003(6) C8 0.011(8) 0.028(7) 0.006(6) 0.002(6) 0.006(6) 0.004(7) C9 0.016(10) 0.023(14) 0.009(9) 0.000(9) 0.005(8) 0.000(10) C10 0.008(7) 0.023(10) 0.012(7) -0.002(7) 0.003(6) -0.004(7) C11 0.018(8) 0.026(9) 0.012(7) -0.001(7) -0.006(6) 0.003(8) C12 0.035(12) 0.027(14) 0.027(11) -0.008(10) 0.009(10) -0.004(11) C13 0.029(8) 0.021(8) 0.020(6) -0.001(6) 0.005(6) -0.009(8) C14 0.019(8) 0.027(7) 0.016(6) 0.000(5) 0.003(5) -0.003(7) C15 0.019(7) 0.020(6) 0.018(5) -0.002(4) 0.006(5) -0.001(6) C16 0.024(8) 0.019(6) 0.023(6) -0.004(5) 0.005(5) 0.003(6) C17 0.025(8) 0.019(8) 0.022(6) 0.005(6) 0.005(5) -0.005(7) C18 0.021(7) 0.024(9) 0.019(6) 0.006(6) 0.012(5) -0.001(6) C19 0.032(12) 0.051(17) 0.020(11) 0.002(11) 0.002(9) -0.001(12) C20 0.051(12) 0.032(14) 0.033(11) -0.004(11) 0.018(10) 0.017(12) C21 0.033(10) 0.037(8) 0.030(10) 0.006(9) 0.015(9) 0.005(9) C22 0.033(8) 0.036(8) 0.022(7) 0.012(7) 0.002(5) -0.005(8) C23 0.022(9) 0.033(9) 0.026(8) 0.007(7) 0.007(5) -0.001(7) C24 0.033(11) 0.017(12) 0.011(9) 0.002(8) 0.003(8) 0.003(10) C25 0.035(12) 0.039(14) 0.014(10) 0.013(9) 0.004(10) 0.001(11) C26 0.013(8) 0.049(12) 0.026(8) 0.002(9) 0.007(7) -0.003(9) C27 0.016(6) 0.029(9) 0.012(7) 0.003(7) -0.005(5) -0.001(6) C28 0.017(7) 0.024(8) 0.006(6) 0.003(6) 0.002(5) 0.003(6) C29 0.012(10) 0.018(12) 0.022(11) 0.004(9) -0.002(8) 0.004(10) C30 0.025(7) 0.029(9) 0.015(8) 0.003(8) 0.001(6) -0.012(8) C31 0.023(7) 0.022(8) 0.012(7) 0.001(6) -0.004(5) 0.003(6) C32 0.030(6) 0.021(9) 0.015(6) 0.000(6) 0.010(6) -0.003(6) C33 0.025(7) 0.013(9) 0.020(7) 0.002(6) -0.002(7) 0.004(6) C34 0.026(8) 0.015(10) 0.015(7) 0.004(7) 0.006(5) 0.003(6) C35 0.040(8) 0.028(10) 0.011(7) 0.000(7) 0.012(6) -0.003(7) C36 0.036(8) 0.037(11) 0.021(7) 0.004(6) 0.013(7) -0.006(6) C37 0.024(8) 0.028(8) 0.030(7) -0.002(6) 0.010(6) -0.009(7) C38 0.018(8) 0.022(9) 0.020(7) 0.000(7) 0.003(6) 0.000(8) Cl2 0.035(3) 0.031(4) 0.021(3) 0.001(3) 0.003(2) -0.003(3) O3 0.064(8) 0.055(10) 0.025(7) -0.009(7) 0.011(7) -0.014(8) O4 0.021(7) 0.040(9) 0.057(8) 0.018(7) -0.001(6) 0.013(7) O5 0.044(8) 0.038(9) 0.048(7) -0.017(7) 0.003(7) -0.015(7) O6 0.063(8) 0.029(9) 0.038(7) 0.013(7) 0.025(6) 0.006(7) Cl3 0.078(4) 0.056(4) 0.013(3) 0.001(3) -0.008(3) 0.009(4) O7 0.076(9) 0.038(9) 0.016(7) -0.001(6) -0.012(6) 0.022(8) O8 0.053(8) 0.071(12) 0.054(8) -0.006(8) -0.004(7) 0.004(9) O9 0.162(13) 0.072(11) 0.038(8) 0.018(8) -0.031(8) 0.007(10) O10 0.084(10) 0.163(16) 0.033(7) -0.003(9) 0.027(7) -0.006(11) O1S 0.094(10) 0.033(9) 0.039(8) -0.015(6) -0.027(6) 0.018(7) C1S 0.057(14) 0.050(11) 0.037(12) -0.011(9) -0.003(8) 0.013(9) C2S 0.060(13) 0.049(12) 0.062(13) 0.008(10) 0.013(11) 0.016(10) C3S 0.100(15) 0.096(14) 0.053(12) -0.038(10) -0.033(9) 0.030(13) _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 N8 1.885(11) . ? Fe1 N3 1.927(11) . ? Fe1 N7 1.969(11) . ? Fe1 N9 1.980(11) . ? Fe1 N2 1.995(12) . ? Fe1 N4 2.007(12) . ? Cl1 C31 1.744(15) . ? O1 C1 1.350(17) . ? O1 H1 0.8400 . ? O2 C23 1.37(2) . ? O2 H2 0.90(3) . ? N1 N2 1.343(16) . ? N1 C7 1.367(16) . ? N1 H1A 0.8800 . ? N2 C9 1.355(16) . ? N3 C14 1.348(19) . ? N3 C10 1.370(16) . ? N4 C15 1.337(17) . ? N4 N5 1.349(14) . ? N5 C17 1.353(18) . ? N5 H5B 0.8800 . ? N7 C24 1.322(15) . ? N7 C28 1.366(16) . ? N8 C29 1.346(17) . ? N8 C33 1.351(16) . ? N9 C38 1.335(16) . ? N9 C34 1.397(16) . ? C1 C2 1.36(2) . ? C1 C6 1.414(19) . ? C2 C3 1.376(19) . ? C2 H2A 0.9500 . ? C3 C4 1.40(2) . ? C3 H3A 0.9500 . ? C4 C5 1.37(2) . ? C4 H4A 0.9500 . ? C5 C6 1.391(18) . ? C5 H5A 0.9500 . ? C6 C7 1.47(2) . ? C7 C8 1.38(2) . ? C8 C9 1.381(19) . ? C8 H8A 0.9500 . ? C9 C10 1.44(2) . ? C10 C11 1.411(18) . ? C11 C12 1.39(2) . ? C11 H11A 0.9500 . ? C12 C13 1.40(2) . ? C12 H12A 0.9500 . ? C13 C14 1.362(19) . ? C13 H13A 0.9500 . ? C14 C15 1.459(19) . ? C15 C16 1.390(19) . ? C16 C17 1.389(18) . ? C16 H16A 0.9500 . ? C17 C18 1.46(2) . ? C18 C23 1.40(2) . ? C18 C19 1.40(2) . ? C19 C20 1.38(2) . ? C19 H19A 0.9500 . ? C20 C21 1.39(2) . ? C20 H20A 0.9500 . ? C21 C22 1.35(2) . ? C21 H21A 0.9500 . ? C22 C23 1.38(2) . ? C22 H22A 0.9500 . ? C24 C25 1.407(19) . ? C24 H24A 0.9500 . ? C25 C26 1.374(19) . ? C25 H25A 0.9500 . ? C26 C27 1.379(18) . ? C26 H26A 0.9500 . ? C27 C28 1.378(18) . ? C27 H27A 0.9500 . ? C28 C29 1.463(17) . ? C29 C30 1.391(19) . ? C30 C31 1.395(19) . ? C30 H30A 0.9500 . ? C31 C32 1.36(2) . ? C32 C33 1.393(19) . ? C32 H32A 0.9500 . ? C33 C34 1.476(19) . ? C34 C35 1.377(18) . ? C35 C36 1.390(19) . ? C35 H35A 0.9500 . ? C36 C37 1.37(2) . ? C36 H36A 0.9500 . ? C37 C38 1.372(18) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? Cl2 O3 1.425(11) . ? Cl2 O5 1.436(10) . ? Cl2 O4 1.447(11) . ? Cl2 O6 1.455(11) . ? Cl3 O9 1.418(15) . ? Cl3 O10 1.424(13) . ? Cl3 O7 1.441(10) . ? Cl3 O8 1.470(13) . ? O1S C1S 1.210(19) . ? C1S C2S 1.47(2) . ? C1S C3S 1.47(2) . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? C3S H3SA 0.9800 . ? C3S H3SB 0.9800 . ? C3S H3SC 0.9800 . ? 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 N8 Fe1 N3 177.5(6) . . ? N8 Fe1 N7 80.8(5) . . ? N3 Fe1 N7 98.2(5) . . ? N8 Fe1 N9 81.8(5) . . ? N3 Fe1 N9 99.3(5) . . ? N7 Fe1 N9 162.4(5) . . ? N8 Fe1 N2 97.9(5) . . ? N3 Fe1 N2 79.8(5) . . ? N7 Fe1 N2 90.0(5) . . ? N9 Fe1 N2 94.5(4) . . ? N8 Fe1 N4 104.5(5) . . ? N3 Fe1 N4 77.8(5) . . ? N7 Fe1 N4 91.5(5) . . ? N9 Fe1 N4 90.8(5) . . ? N2 Fe1 N4 157.6(5) . . ? C1 O1 H1 109.5 . . ? C23 O2 H2 122(10) . . ? N2 N1 C7 111.0(12) . . ? N2 N1 H1A 124.5 . . ? C7 N1 H1A 124.5 . . ? N1 N2 C9 106.0(11) . . ? N1 N2 Fe1 138.4(9) . . ? C9 N2 Fe1 115.6(11) . . ? C14 N3 C10 120.8(12) . . ? C14 N3 Fe1 121.1(10) . . ? C10 N3 Fe1 118.1(10) . . ? C15 N4 N5 105.1(12) . . ? C15 N4 Fe1 116.7(10) . . ? N5 N4 Fe1 138.2(10) . . ? N4 N5 C17 111.3(12) . . ? N4 N5 H5B 124.3 . . ? C17 N5 H5B 124.3 . . ? C24 N7 C28 118.7(11) . . ? C24 N7 Fe1 126.3(10) . . ? C28 N7 Fe1 114.8(9) . . ? C29 N8 C33 122.1(12) . . ? C29 N8 Fe1 119.5(10) . . ? C33 N8 Fe1 118.4(10) . . ? C38 N9 C34 115.7(12) . . ? C38 N9 Fe1 129.6(10) . . ? C34 N9 Fe1 114.5(10) . . ? O1 C1 C2 123.5(15) . . ? O1 C1 C6 116.4(15) . . ? C2 C1 C6 120.2(15) . . ? C1 C2 C3 120.9(16) . . ? C1 C2 H2A 119.6 . . ? C3 C2 H2A 119.6 . . ? C2 C3 C4 120.4(16) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C5 C4 C3 118.5(15) . . ? C5 C4 H4A 120.8 . . ? C3 C4 H4A 120.8 . . ? C4 C5 C6 122.0(16) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C5 C6 C1 118.0(15) . . ? C5 C6 C7 119.4(15) . . ? C1 C6 C7 122.6(14) . . ? N1 C7 C8 106.7(15) . . ? N1 C7 C6 123.1(14) . . ? C8 C7 C6 130.2(14) . . ? C9 C8 C7 106.0(13) . . ? C9 C8 H8A 127.0 . . ? C7 C8 H8A 127.0 . . ? N2 C9 C8 110.3(14) . . ? N2 C9 C10 113.9(13) . . ? C8 C9 C10 135.7(13) . . ? N3 C10 C11 119.7(14) . . ? N3 C10 C9 112.6(12) . . ? C11 C10 C9 127.6(14) . . ? C12 C11 C10 117.8(14) . . ? C12 C11 H11A 121.1 . . ? C10 C11 H11A 121.1 . . ? C11 C12 C13 121.4(15) . . ? C11 C12 H12A 119.3 . . ? C13 C12 H12A 119.3 . . ? C14 C13 C12 118.1(16) . . ? C14 C13 H13A 121.0 . . ? C12 C13 H13A 121.0 . . ? N3 C14 C13 122.1(14) . . ? N3 C14 C15 110.5(14) . . ? C13 C14 C15 127.4(16) . . ? N4 C15 C16 112.1(12) . . ? N4 C15 C14 113.8(14) . . ? C16 C15 C14 134.0(15) . . ? C17 C16 C15 103.9(14) . . ? C17 C16 H16A 128.0 . . ? C15 C16 H16A 128.0 . . ? N5 C17 C16 107.5(14) . . ? N5 C17 C18 123.5(14) . . ? C16 C17 C18 128.9(16) . . ? C23 C18 C19 115.1(16) . . ? C23 C18 C17 124.9(17) . . ? C19 C18 C17 120.0(15) . . ? C20 C19 C18 122.9(16) . . ? C20 C19 H19A 118.5 . . ? C18 C19 H19A 118.5 . . ? C19 C20 C21 119.0(18) . . ? C19 C20 H20A 120.5 . . ? C21 C20 H20A 120.5 . . ? C22 C21 C20 120.2(17) . . ? C22 C21 H21A 119.9 . . ? C20 C21 H21A 119.9 . . ? C21 C22 C23 120.2(16) . . ? C21 C22 H22A 119.9 . . ? C23 C22 H22A 119.9 . . ? O2 C23 C22 119.6(15) . . ? O2 C23 C18 117.7(16) . . ? C22 C23 C18 122.6(17) . . ? N7 C24 C25 121.2(14) . . ? N7 C24 H24A 119.4 . . ? C25 C24 H24A 119.4 . . ? C26 C25 C24 120.2(14) . . ? C26 C25 H25A 119.9 . . ? C24 C25 H25A 119.9 . . ? C25 C26 C27 118.3(14) . . ? C25 C26 H26A 120.8 . . ? C27 C26 H26A 120.8 . . ? C28 C27 C26 119.3(14) . . ? C28 C27 H27A 120.3 . . ? C26 C27 H27A 120.3 . . ? N7 C28 C27 122.3(12) . . ? N7 C28 C29 113.2(12) . . ? C27 C28 C29 124.6(14) . . ? N8 C29 C30 121.8(13) . . ? N8 C29 C28 111.6(12) . . ? C30 C29 C28 126.6(14) . . ? C29 C30 C31 114.7(14) . . ? C29 C30 H30A 122.6 . . ? C31 C30 H30A 122.6 . . ? C32 C31 C30 124.3(14) . . ? C32 C31 Cl1 118.3(12) . . ? C30 C31 Cl1 117.4(12) . . ? C31 C32 C33 117.7(14) . . ? C31 C32 H32A 121.2 . . ? C33 C32 H32A 121.2 . . ? N8 C33 C32 119.3(14) . . ? N8 C33 C34 113.6(13) . . ? C32 C33 C34 127.0(15) . . ? C35 C34 N9 121.4(14) . . ? C35 C34 C33 127.0(14) . . ? N9 C34 C33 111.5(12) . . ? C34 C35 C36 120.3(14) . . ? C34 C35 H35A 119.9 . . ? C36 C35 H35A 119.9 . . ? C37 C36 C35 118.4(15) . . ? C37 C36 H36A 120.8 . . ? C35 C36 H36A 120.8 . . ? C36 C37 C38 119.0(16) . . ? C36 C37 H37A 120.5 . . ? C38 C37 H37A 120.5 . . ? N9 C38 C37 125.1(15) . . ? N9 C38 H38A 117.4 . . ? C37 C38 H38A 117.4 . . ? O3 Cl2 O5 108.6(7) . . ? O3 Cl2 O4 110.4(7) . . ? O5 Cl2 O4 110.6(7) . . ? O3 Cl2 O6 108.5(7) . . ? O5 Cl2 O6 110.4(7) . . ? O4 Cl2 O6 108.3(7) . . ? O9 Cl3 O10 113.1(10) . . ? O9 Cl3 O7 108.4(8) . . ? O10 Cl3 O7 108.8(8) . . ? O9 Cl3 O8 107.3(8) . . ? O10 Cl3 O8 110.4(8) . . ? O7 Cl3 O8 108.7(8) . . ? O1S C1S C2S 123.8(18) . . ? O1S C1S C3S 119.9(19) . . ? C2S C1S C3S 116.1(17) . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? C1S C3S H3SA 109.5 . . ? C1S C3S H3SB 109.5 . . ? H3SA C3S H3SB 109.5 . . ? C1S C3S H3SC 109.5 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? _refine_diff_density_max 0.276 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.061 _shelxl_version_number 2014-3 _shelx_res_file ; TITL t1 in P2(1) CELL 0.71073 8.471 22.725 10.833 90.0000 103.120 90.0000 ZERR 2.00 0.006 0.018 0.008 0.0000 0.016 0.0000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H N O CL FE UNIT 82 66 16 22 6 2 TEMP -173 SIZE 0.15 0.05 0.04 REM data cut at 1.07 angstrom for completeness REM solved with shelxs REM most disagreeable negative Fo2 OMIT 0 2 0 OMIT 0 -2 0 OMIT 0 1 1 OMIT 0 -1 1 OMIT -2 12 7 OMIT 1 0 1 L.S. 24 BOND $H ACTA 38.8 FMAP 2 PLAN 10 ISOR 0.004 N2 N7 ISOR 0.006 O9 ISOR 0.008 N1 N3 N4 O10 O1S C3S ISOR 0.01 C3 C6 > C8 C10 C11 C13 C15 > C18 C22 C27 C28 ISOR 0.01 C30 > C32 C37 C38 SIMU 0.012 N1 > N4 N7 C5 > C8 C13 > C18 C21 > C23 C26 > C28 C30 > C38 DELU 0.003 N1 > N4 N7 C5 > C8 C13 > C18 C21 > C23 C26 > C28 C30 > C38 SIMU 0.012 C1 > C3 C10 C11 09 O10 O1S > C3S DELU 0.003 C1 > C3 C10 C11 O9 O10 O1S > C3S DFIX 0.9 O2 H2 DANG 1.9 H2 O9 DANG 2.1 H2 O7 WGHT 0.009000 FVAR 0.14158 FE1 6 0.706650 0.040299 0.954251 11.00000 0.02020 0.01983 = 0.00892 0.00005 0.00199 -0.00130 CL1 5 0.979290 0.189149 1.448946 11.00000 0.03976 0.05150 = 0.01825 -0.01895 0.00525 -0.00745 O1 4 0.564449 0.270149 0.930544 11.00000 0.05721 0.03191 = 0.01530 0.00378 -0.01025 -0.00499 AFIX 147 H1 2 0.631326 0.296270 0.962814 11.00000 -1.50000 AFIX 0 O2 4 1.137580 -0.092289 1.299769 11.00000 0.04857 0.03675 = 0.04955 0.00310 -0.01115 0.00290 H2 2 1.073732 -0.072123 1.340475 11.00000 -1.50000 N1 3 0.568631 0.163147 0.852422 11.00000 0.02628 0.02207 = 0.00784 0.00097 0.00427 -0.00252 AFIX 43 H1A 2 0.605041 0.184509 0.920706 11.00000 -1.20000 AFIX 0 N2 3 0.592679 0.104963 0.844640 11.00000 0.01732 0.01924 = 0.00851 0.00507 0.00102 -0.00226 N3 3 0.622669 -0.002604 0.799821 11.00000 0.02129 0.02731 = 0.00700 -0.00141 0.00445 -0.00053 N4 3 0.792718 -0.041057 0.999806 11.00000 0.02137 0.01051 = 0.01185 0.00739 0.00353 0.00080 N5 3 0.888664 -0.068751 1.099236 11.00000 0.01986 0.01502 = 0.01353 0.00196 -0.00780 0.00213 AFIX 43 H5B 2 0.934105 -0.051545 1.171322 11.00000 -1.20000 AFIX 0 N7 3 0.913790 0.065425 0.917773 11.00000 0.01609 0.01863 = 0.00969 0.00178 0.00809 -0.00269 N8 3 0.788023 0.085329 1.101013 11.00000 0.02565 0.01708 = 0.01110 -0.00295 0.00591 0.00819 N9 3 0.527827 0.026693 1.041047 11.00000 0.01634 0.01601 = 0.01570 0.00145 0.00037 0.00036 C1 1 0.475108 0.289365 0.818338 11.00000 0.04229 0.02382 = 0.01687 -0.00425 0.00727 -0.00128 C2 1 0.426344 0.346138 0.796220 11.00000 0.04980 0.02578 = 0.02007 -0.00878 0.01005 0.00558 AFIX 43 H2A 2 0.455174 0.374413 0.862085 11.00000 -1.20000 AFIX 0 C3 1 0.335755 0.363185 0.679653 11.00000 0.03981 0.03093 = 0.03088 0.00403 0.00914 0.00606 AFIX 43 H3A 2 0.305920 0.403307 0.664855 11.00000 -1.20000 AFIX 0 C4 1 0.287278 0.321815 0.582754 11.00000 0.02758 0.02870 = 0.02672 0.01599 0.00039 0.00910 AFIX 43 H4A 2 0.221735 0.333131 0.503036 11.00000 -1.20000 AFIX 0 C5 1 0.336571 0.264545 0.605517 11.00000 0.03181 0.01974 = 0.02336 0.00324 0.00676 0.00872 AFIX 43 H5A 2 0.304948 0.236253 0.540003 11.00000 -1.20000 AFIX 0 C6 1 0.431438 0.246668 0.721618 11.00000 0.01185 0.02386 = 0.02287 0.00422 0.00990 0.00062 C7 1 0.480059 0.184760 0.740135 11.00000 0.01412 0.02235 = 0.01451 0.00224 0.00387 0.00323 C8 1 0.447565 0.137654 0.657402 11.00000 0.01136 0.02766 = 0.00551 0.00219 0.00607 0.00405 AFIX 43 H8A 2 0.388507 0.138460 0.571655 11.00000 -1.20000 AFIX 0 C9 1 0.518477 0.089196 0.724853 11.00000 0.01612 0.02262 = 0.00933 -0.00050 0.00504 -0.00019 C10 1 0.534325 0.027719 0.698034 11.00000 0.00848 0.02286 = 0.01239 -0.00225 0.00270 -0.00398 C11 1 0.469949 -0.002237 0.583638 11.00000 0.01802 0.02610 = 0.01195 -0.00064 -0.00565 0.00268 AFIX 43 H11A 2 0.405739 0.017726 0.512696 11.00000 -1.20000 AFIX 0 C12 1 0.503460 -0.061764 0.578136 11.00000 0.03516 0.02694 = 0.02727 -0.00830 0.00865 -0.00394 AFIX 43 H12A 2 0.465148 -0.082500 0.501001 11.00000 -1.20000 AFIX 0 C13 1 0.592410 -0.091913 0.683663 11.00000 0.02901 0.02146 = 0.01996 -0.00123 0.00510 -0.00874 AFIX 43 H13A 2 0.610633 -0.133075 0.680434 11.00000 -1.20000 AFIX 0 C14 1 0.652222 -0.060560 0.791291 11.00000 0.01916 0.02664 = 0.01639 -0.00007 0.00276 -0.00273 C15 1 0.752578 -0.082335 0.910213 11.00000 0.01860 0.02024 = 0.01774 -0.00155 0.00553 -0.00077 C16 1 0.820934 -0.136623 0.950323 11.00000 0.02390 0.01861 = 0.02305 -0.00375 0.00451 0.00279 AFIX 43 H16A 2 0.811592 -0.172428 0.903964 11.00000 -1.20000 AFIX 0 C17 1 0.906061 -0.126364 1.073912 11.00000 0.02540 0.01933 = 0.02187 0.00479 0.00509 -0.00523 C18 1 1.002569 -0.167527 1.164567 11.00000 0.02143 0.02425 = 0.01903 0.00621 0.01189 -0.00092 C19 1 0.990383 -0.228240 1.141050 11.00000 0.03206 0.05085 = 0.01995 0.00219 0.00171 -0.00067 AFIX 43 H19A 2 0.916138 -0.241726 1.067100 11.00000 -1.20000 AFIX 0 C20 1 1.081392 -0.269222 1.220511 11.00000 0.05096 0.03243 = 0.03319 -0.00400 0.01824 0.01705 AFIX 43 H20A 2 1.070085 -0.310003 1.201249 11.00000 -1.20000 AFIX 0 C21 1 1.189849 -0.249978 1.329141 11.00000 0.03317 0.03743 = 0.03038 0.00574 0.01532 0.00493 AFIX 43 H21A 2 1.252193 -0.277752 1.385390 11.00000 -1.20000 AFIX 0 C22 1 1.206934 -0.191759 1.355055 11.00000 0.03250 0.03644 = 0.02188 0.01209 0.00211 -0.00493 AFIX 43 H22A 2 1.282370 -0.178760 1.428833 11.00000 -1.20000 AFIX 0 C23 1 1.115156 -0.151217 1.274681 11.00000 0.02155 0.03343 = 0.02567 0.00682 0.00654 -0.00095 C24 1 0.964034 0.054443 0.813120 11.00000 0.03255 0.01706 = 0.01131 0.00172 0.00264 0.00294 AFIX 43 H24A 2 0.900739 0.029877 0.749815 11.00000 -1.20000 AFIX 0 C25 1 1.109616 0.078499 0.793842 11.00000 0.03533 0.03941 = 0.01433 0.01266 0.00449 0.00101 AFIX 43 H25A 2 1.143426 0.070214 0.717835 11.00000 -1.20000 AFIX 0 C26 1 1.203042 0.113942 0.884621 11.00000 0.01349 0.04856 = 0.02560 0.00203 0.00737 -0.00280 AFIX 43 H26A 2 1.300910 0.130740 0.872098 11.00000 -1.20000 AFIX 0 C27 1 1.151111 0.124496 0.994321 11.00000 0.01580 0.02853 = 0.01153 0.00315 -0.00475 -0.00128 AFIX 43 H27A 2 1.215177 0.147463 1.060361 11.00000 -1.20000 AFIX 0 C28 1 1.005279 0.101378 1.007183 11.00000 0.01733 0.02354 = 0.00551 0.00257 0.00166 0.00301 C29 1 0.934729 0.110831 1.116930 11.00000 0.01228 0.01783 = 0.02205 0.00353 -0.00248 0.00433 C30 1 1.001185 0.143906 1.224132 11.00000 0.02504 0.02920 = 0.01490 0.00290 0.00098 -0.01208 AFIX 43 H30A 2 1.105301 0.161579 1.237207 11.00000 -1.20000 AFIX 0 C31 1 0.902960 0.149105 1.311000 11.00000 0.02320 0.02189 = 0.01193 0.00057 -0.00432 0.00344 C32 1 0.752091 0.125234 1.294637 11.00000 0.02956 0.02052 = 0.01518 -0.00015 0.00963 -0.00274 AFIX 43 H32A 2 0.688122 0.131319 1.355076 11.00000 -1.20000 AFIX 0 C33 1 0.694908 0.091608 1.186248 11.00000 0.02507 0.01268 = 0.02033 0.00179 -0.00248 0.00371 C34 1 0.543839 0.056853 1.155590 11.00000 0.02592 0.01474 = 0.01451 0.00392 0.00558 0.00342 C35 1 0.432015 0.050348 1.229132 11.00000 0.04044 0.02801 = 0.01075 -0.00049 0.01217 -0.00343 AFIX 43 H35A 2 0.443526 0.072273 1.305325 11.00000 -1.20000 AFIX 0 C36 1 0.302389 0.011840 1.192348 11.00000 0.03588 0.03712 = 0.02086 0.00392 0.01317 -0.00600 AFIX 43 H36A 2 0.224131 0.007396 1.242110 11.00000 -1.20000 AFIX 0 C37 1 0.290190 -0.019475 1.082898 11.00000 0.02351 0.02796 = 0.03029 -0.00211 0.01040 -0.00914 AFIX 43 H37A 2 0.205870 -0.047474 1.057107 11.00000 -1.20000 AFIX 0 C38 1 0.401618 -0.009855 1.010811 11.00000 0.01765 0.02173 = 0.02001 -0.00041 0.00259 -0.00025 AFIX 43 H38A 2 0.387831 -0.030866 0.933281 11.00000 -1.20000 AFIX 0 CL2 5 0.425088 0.229166 0.281969 11.00000 0.03464 0.03099 = 0.02071 0.00077 0.00349 -0.00344 O3 4 0.449335 0.210372 0.162182 11.00000 0.06351 0.05509 = 0.02490 -0.00912 0.01106 -0.01448 O4 4 0.275328 0.261904 0.265829 11.00000 0.02111 0.04033 = 0.05743 0.01830 -0.00115 0.01323 O5 4 0.560599 0.264897 0.342273 11.00000 0.04443 0.03803 = 0.04812 -0.01656 0.00254 -0.01465 O6 4 0.413476 0.177349 0.358314 11.00000 0.06264 0.02934 = 0.03840 0.01252 0.02515 0.00639 CL3 5 0.975999 0.007304 1.454626 11.00000 0.07791 0.05595 = 0.01257 0.00115 -0.00794 0.00880 O7 4 0.906365 0.001601 1.320895 11.00000 0.07637 0.03755 = 0.01582 -0.00146 -0.01209 0.02166 O8 4 1.108571 0.050444 1.472745 11.00000 0.05251 0.07115 = 0.05412 -0.00600 -0.00361 0.00397 O9 4 1.045131 -0.047553 1.500499 11.00000 0.16215 0.07154 = 0.03819 0.01847 -0.03084 0.00742 O10 4 0.853441 0.026578 1.516196 11.00000 0.08436 0.16334 = 0.03320 -0.00302 0.02718 -0.00559 O1S 4 0.671770 0.358299 1.091751 11.00000 0.09419 0.03344 = 0.03916 -0.01480 -0.02655 0.01830 C1S 1 0.791189 0.342187 1.168235 11.00000 0.05710 0.04981 = 0.03705 -0.01084 -0.00267 0.01319 C2S 1 0.858785 0.282695 1.171200 11.00000 0.06002 0.04937 = 0.06233 0.00805 0.01266 0.01633 AFIX 137 H2SA 2 0.851016 0.268898 1.084316 11.00000 -1.50000 H2SB 2 0.797778 0.256112 1.214366 11.00000 -1.50000 H2SC 2 0.972758 0.283299 1.216899 11.00000 -1.50000 AFIX 0 C3S 1 0.869252 0.381676 1.271688 11.00000 0.10014 0.09568 = 0.05276 -0.03834 -0.03349 0.02974 AFIX 137 H3SA 2 0.816675 0.420325 1.259647 11.00000 -1.50000 H3SB 2 0.984293 0.385933 1.271404 11.00000 -1.50000 H3SC 2 0.858817 0.365090 1.352962 11.00000 -1.50000 AFIX 0 HKLF 4 REM t1 in P2(1) REM R1 = 0.0493 for 2673 Fo > 4sig(Fo) and 0.0713 for all 3427 data REM 583 parameters refined using 425 restraints END WGHT 0.0089 0.0000 REM Highest difference peak 0.276, deepest hole -0.291, 1-sigma level 0.061 Q1 1 0.7246 0.0543 0.7286 11.00000 0.05 0.28 Q2 1 0.7716 0.1277 0.9436 11.00000 0.05 0.25 Q3 1 1.1072 -0.3531 1.1556 11.00000 0.05 0.25 Q4 1 0.9225 0.0211 1.0666 11.00000 0.05 0.25 Q5 1 1.1128 -0.1700 1.4009 11.00000 0.05 0.24 Q6 1 1.2662 0.1432 1.1923 11.00000 0.05 0.24 Q7 1 0.6255 0.0428 1.4577 11.00000 0.05 0.22 Q8 1 0.7330 -0.2245 0.9784 11.00000 0.05 0.22 Q9 1 0.9208 0.4505 1.1235 11.00000 0.05 0.22 Q10 1 0.7445 0.2475 0.8623 11.00000 0.05 0.22 ; _shelx_res_checksum 89322 _shelx_hkl_file ; 1 0 0 4.81 0.69 1 0 0 8.47 1.50 1 0 0 7.06 1.02 2 0 0 273.40 9.75 2 0 0 260.91 10.89 2 0 0 280.15 9.32 -2 0 0 271.61 9.24 3 0 0 0.08 1.45 3 0 0 -1.20 1.88 -3 0 0 0.24 0.65 4 0 0 19.18 4.35 -4 0 0 23.85 2.35 5 0 0 -0.17 2.61 -5 0 0 0.97 1.08 5 0 0 2.29 2.18 6 0 0 5.12 3.51 6 0 0 3.75 2.91 -6 0 0 5.62 1.66 -7 0 0 73.29 5.12 7 0 0 53.74 7.18 0 -1 0 -0.06 0.10 0 1 0 0.14 0.12 2 -1 0 152.09 6.14 -2 -1 0 152.49 5.61 2 -1 0 155.98 5.84 2 -1 0 157.14 7.63 2 1 0 149.83 6.50 -2 1 0 151.73 5.74 -2 1 0 141.84 7.19 2 1 0 160.60 7.42 2 1 0 155.74 5.72 3 -1 0 1.10 2.23 3 -1 0 1.92 1.60 -3 -1 0 1.06 0.70 3 1 0 1.96 1.61 -3 1 0 0.90 0.85 3 1 0 1.22 2.10 -4 -1 0 73.45 4.02 4 -1 0 70.41 6.55 -4 1 0 73.10 4.13 4 1 0 74.64 5.82 4 1 0 72.63 6.61 5 -1 0 19.52 3.42 -5 -1 0 28.32 2.68 5 -1 0 18.33 4.43 5 1 0 16.42 3.29 5 1 0 16.38 4.09 -5 1 0 29.82 2.78 6 -1 0 5.91 2.84 6 -1 0 3.34 3.30 -6 -1 0 7.24 1.87 6 1 0 0.95 3.01 6 1 0 6.68 2.76 -6 1 0 4.72 1.67 -7 -1 0 5.17 2.03 7 -1 0 6.03 3.22 7 -1 0 1.58 3.54 -7 1 0 2.67 1.63 7 1 0 6.97 4.23 7 1 0 3.86 3.28 0 -2 0 -0.25 0.31 0 -2 0 0.03 0.27 0 2 0 -0.32 0.19 0 2 0 -0.30 0.33 2 -2 0 150.04 7.46 -2 -2 0 142.79 5.15 2 2 0 140.18 5.23 -2 2 0 125.60 6.94 -2 2 0 130.87 5.38 2 2 0 136.89 6.25 3 -2 0 18.78 3.81 -3 -2 0 14.44 1.51 3 -2 0 10.06 2.00 3 2 0 10.72 3.00 3 2 0 14.25 2.60 -3 2 0 14.07 1.84 4 -2 0 40.36 4.12 -4 -2 0 30.15 2.54 4 -2 0 26.51 4.89 -4 2 0 35.21 2.86 4 2 0 31.89 4.83 4 2 0 28.68 4.03 -5 -2 0 76.33 4.41 5 -2 0 72.35 7.44 5 -2 0 82.38 6.06 -5 2 0 72.88 4.53 6 -2 0 6.40 2.87 -6 -2 0 7.86 1.97 6 -2 0 3.71 3.37 6 2 0 4.85 2.60 -6 2 0 5.03 1.97 7 -2 0 7.43 3.21 -7 -2 0 9.15 2.36 7 -2 0 1.78 3.77 -7 2 0 8.76 2.40 7 2 0 7.21 3.65 -7 2 0 12.76 2.65 0 -3 0 -0.48 0.49 0 -3 0 -0.07 0.50 0 3 0 -0.81 0.51 0 3 0 -0.48 0.31 1 -3 0 113.93 5.56 1 3 0 103.64 3.90 1 3 0 107.23 4.72 2 -3 0 80.81 5.68 -2 -3 0 85.12 3.58 2 3 0 89.88 4.95 -2 3 0 82.61 5.50 2 3 0 91.25 3.71 -2 3 0 85.55 3.15 -3 -3 0 4.30 1.02 3 -3 0 4.47 1.56 3 -3 0 3.83 2.65 -3 3 0 5.54 1.35 3 3 0 3.17 1.78 4 -3 0 24.85 4.80 4 -3 0 23.21 3.31 -4 -3 0 25.78 2.35 -4 3 0 31.96 2.74 4 3 0 24.09 3.78 5 -3 0 15.30 4.29 -5 -3 0 24.06 2.40 5 -3 0 19.28 3.30 5 3 0 19.08 3.84 -5 3 0 24.39 2.70 6 -3 0 28.55 4.17 -6 -3 0 34.52 3.15 -6 3 0 33.15 3.13 -6 3 0 35.54 3.44 6 3 0 23.21 4.69 -7 -3 0 4.56 1.89 7 -3 0 1.48 3.74 -7 3 0 5.45 2.12 7 3 0 3.67 3.18 -7 3 0 6.64 1.99 0 -4 0 217.76 7.33 0 -4 0 227.19 8.26 0 4 0 225.32 8.09 -1 -4 0 100.43 4.03 1 -4 0 104.81 5.60 -1 4 0 102.66 5.30 1 4 0 99.29 3.88 1 4 0 98.83 4.75 2 -4 0 113.17 7.03 -2 -4 0 121.08 4.68 2 4 0 121.52 6.05 2 4 0 119.83 4.73 3 -4 0 11.89 1.87 -3 -4 0 13.23 1.63 3 -4 0 11.66 3.34 3 4 0 10.05 2.44 -3 4 0 11.46 1.33 -3 4 0 11.14 1.80 4 -4 0 27.81 5.21 4 -4 0 23.86 3.05 -4 -4 0 22.13 2.22 -4 4 0 24.82 2.17 4 4 0 27.14 4.17 -4 4 0 22.74 2.52 5 -4 0 34.82 4.09 5 -4 0 36.15 5.94 -5 -4 0 39.90 3.03 -5 4 0 38.01 3.31 -5 4 0 41.29 2.97 5 4 0 37.03 4.99 6 -4 0 1.75 2.09 -6 -4 0 1.63 1.32 6 -4 0 1.42 3.18 -6 4 0 1.82 1.43 6 4 0 2.41 2.52 -6 4 0 3.64 1.55 7 -4 0 2.90 3.73 -7 -4 0 11.78 2.40 -7 4 0 14.05 3.03 7 4 0 6.58 3.74 0 -5 0 -0.90 1.14 0 -5 0 -0.73 0.81 0 5 0 -0.85 0.79 0 5 0 -1.06 0.95 1 -5 0 23.85 3.37 -1 -5 0 21.53 1.91 1 5 0 25.87 2.67 1 5 0 22.10 1.76 -1 5 0 26.18 3.06 -2 -5 0 121.43 4.86 2 -5 0 122.95 7.42 2 5 0 117.65 6.18 2 5 0 121.88 4.85 -3 -5 0 5.81 1.22 3 -5 0 6.67 3.00 3 5 0 6.22 2.19 -4 -5 0 57.68 3.39 4 -5 0 58.55 7.07 4 -5 0 51.57 3.77 4 5 0 51.71 5.29 -4 5 0 51.12 2.91 -4 5 0 53.00 3.77 -5 -5 0 11.39 1.96 5 -5 0 9.60 2.29 5 -5 0 8.27 3.65 5 5 0 6.87 2.92 -5 5 0 9.40 1.70 -5 5 0 9.76 2.22 -6 -5 0 8.06 1.99 6 -5 0 7.09 4.30 -6 5 0 11.16 2.10 6 5 0 9.87 3.78 -6 5 0 13.50 2.56 7 -5 0 7.94 4.75 -7 -5 0 30.85 3.77 7 5 0 14.36 4.46 -7 5 0 26.82 4.02 0 -6 0 92.26 4.98 0 6 0 85.28 4.04 0 6 0 94.17 4.66 -1 -6 0 16.67 2.03 1 -6 0 28.47 3.61 1 6 0 16.24 1.72 -1 6 0 29.78 3.18 1 6 0 18.58 2.61 2 -6 0 19.51 3.76 -2 -6 0 23.48 1.98 2 6 0 24.25 1.86 2 6 0 30.36 3.63 -3 -6 0 47.93 3.01 3 -6 0 55.89 6.00 3 6 0 45.99 4.61 -4 -6 0 12.72 1.85 4 -6 0 2.47 3.02 4 6 0 10.59 2.94 -4 6 0 10.44 2.11 5 -6 0 19.73 4.89 -5 -6 0 28.04 2.66 5 6 0 29.17 4.74 -5 6 0 28.63 3.00 -5 6 0 29.06 2.44 -6 -6 0 12.20 2.24 6 -6 0 4.63 3.77 -6 6 0 13.30 2.68 6 6 0 10.57 3.67 -7 -6 0 20.12 3.13 7 -6 0 1.71 3.70 7 6 0 6.90 3.87 -7 6 0 19.43 3.45 0 -7 0 -0.01 1.35 0 7 0 0.20 1.19 0 7 0 0.43 0.99 1 -7 0 39.22 4.17 -1 -7 0 41.85 3.01 1 7 0 41.67 3.45 1 7 0 38.65 2.58 2 -7 0 16.53 3.75 -2 -7 0 11.71 1.79 2 7 0 11.10 2.37 3 -7 0 94.90 7.72 -3 -7 0 80.37 4.18 3 7 0 84.30 6.07 -4 -7 0 56.58 3.52 4 -7 0 55.87 7.09 -4 7 0 56.03 4.07 4 7 0 64.68 5.92 -5 -7 0 10.50 1.93 5 -7 0 12.19 4.14 5 7 0 8.44 3.17 -5 7 0 9.62 2.25 -6 -7 0 5.55 1.77 6 -7 0 1.47 3.73 6 7 0 2.52 2.91 -6 7 0 8.71 2.35 -7 -7 0 7.67 2.18 7 -7 0 -0.49 3.96 7 7 0 5.23 3.54 -7 7 0 4.83 2.13 0 -8 0 59.73 4.50 0 8 0 54.95 3.40 1 -8 0 14.81 3.13 -1 -8 0 9.46 2.04 1 8 0 7.92 2.10 2 -8 0 5.50 2.81 -2 -8 0 3.12 1.38 2 8 0 2.94 1.98 -3 -8 0 1.72 1.24 3 -8 0 1.02 2.64 3 8 0 0.34 1.88 4 -8 0 13.35 4.13 -4 -8 0 18.26 2.31 4 8 0 15.91 3.82 -5 -8 0 46.62 3.38 5 -8 0 32.30 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