# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c1_new _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H16 Cl2 F10 Fe N14 O2 S2, 2(C H4 O)' _chemical_formula_sum 'C42 H24 Cl2 F10 Fe N14 O4 S2' _chemical_formula_weight 1169.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0020 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' H H 0.0000 0.0000 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' N N -0.0031 0.0040 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' O O -0.0041 0.0074 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' F F -0.0053 0.0125 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' S S 0.1206 0.1480 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' Cl Cl 0.1408 0.1896 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' Fe Fe 0.2064 0.9930 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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, -z' _cell_length_a 9.084(4) _cell_length_b 10.766(5) _cell_length_c 12.658(5) _cell_angle_alpha 96.115(6) _cell_angle_beta 103.282(5) _cell_angle_gamma 98.341(5) _cell_volume 1179.4(9) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5605 _cell_measurement_theta_min 3.34 _cell_measurement_theta_max 31.09 _exptl_crystal_description parallelepiped _exptl_crystal_colour purple _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_F_000 588 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.110 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 0.781 _shelx_estimated_absorpt_T_min 0.919 _shelx_estimated_absorpt_T_max 0.985 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.571 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'SADABS Bruker AXS Madison WI US' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7749 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Advanced Light Source station 11.3.1' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13506 _diffrn_reflns_av_unetI/netI 0.0562 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.345 _diffrn_reflns_theta_max 30.208 _diffrn_reflns_theta_full 31.100 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measured_fraction_theta_full 0.918 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_Laue_measured_fraction_full 0.918 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_point_group_measured_fraction_full 0.918 _reflns_number_total 5362 _reflns_number_gt 3992 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; All non-hydrogens were refined anisotropically. The lattice methanol molecule is disordered over two equivalent positions and was refined with displacement parameters restraints. Hydrogens were placed on their carrier atom and refined with a riding model. The hydroxyl hydrogens of the two components of the disordered lattice methanol could not be found and their refinement at calculated positions did not converge satisfactorily. These were thus eventually omitted from the structural model although they are taken into account in the formula. ; _vrf_PLAT019_c1_new ; PROBLEM: Check _diffrn_measured_fraction_theta_full/_max 0.926 RESPONSE: This low ratio is due to poor diffraction at high resolution. Although data up to 0.75 angstrom resolution have been used, the completeness over the 0.85 to 0.75 resolution range is only 0.927. The dataset has however a reasonable completeness of at least 0.975 up to 0.77 angstrom resolution. ; _vrf_PLAT309_c1_new ; PROBLEM: Single Bonded Oxygen (C-O > 1.3 Ang) ........... O1S RESPONSE: The hydroxyl hydrogens of the two components of the disordered lattice methanol could not be found and their refinement at calculated positions did not converge satisfactorily. These were thus eventually omitted from the structural model resulting in apparently single bonded oxygens. ; _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^)+(0.0741P)^2^+2.7108P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5362 _refine_ls_number_parameters 360 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0866 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.1820 _refine_ls_wR_factor_gt 0.1700 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.050 _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_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 0.5000 0.5000 0.5000 0.0283(2) Uani 1 2 d S . P . . Cl1 Cl 0.43563(12) 0.17088(10) 0.92963(9) 0.0426(3) Uani 1 1 d . . . . . S1 S 0.27822(13) 0.77454(10) 0.26753(9) 0.0416(3) Uani 1 1 d . . . . . O1 O 0.8247(3) 0.5491(3) 1.0224(2) 0.0358(6) Uani 1 1 d . . . . . N1 N 0.3933(4) 0.5920(3) 0.3899(3) 0.0323(7) Uani 1 1 d . . . . . N2 N 0.5252(4) 0.6572(3) 0.6075(3) 0.0349(7) Uani 1 1 d . . . . . N3 N 0.2994(4) 0.4448(3) 0.5378(3) 0.0341(7) Uani 1 1 d . . . . . N4 N 0.4176(4) 0.5304(3) 0.7210(3) 0.0316(7) Uani 1 1 d . . . . . N5 N 0.4291(4) 0.3629(3) 0.8221(3) 0.0331(7) Uani 1 1 d . . . . . N6 N 0.6234(4) 0.5478(3) 0.8717(3) 0.0336(7) Uani 1 1 d . . . . . N7 N 0.6366(4) 0.3786(3) 0.9818(3) 0.0330(7) Uani 1 1 d . . . . . C1 C 0.3451(4) 0.6680(4) 0.3392(3) 0.0330(8) Uani 1 1 d . . . . . C2 C 0.5766(5) 0.7739(4) 0.5844(4) 0.0420(9) Uani 1 1 d . . . . . H2A H 0.6076 0.7794 0.5180 0.050 Uiso 1 1 calc R U . . . C3 C 0.5858(6) 0.8845(4) 0.6532(4) 0.0524(12) Uani 1 1 d . . . . . H3A H 0.6244 0.9642 0.6353 0.063 Uiso 1 1 calc R U . . . C4 C 0.5381(6) 0.8775(4) 0.7482(4) 0.0508(11) Uani 1 1 d . . . . . H4A H 0.5433 0.9528 0.7965 0.061 Uiso 1 1 calc R U . . . C5 C 0.4828(5) 0.7614(4) 0.7732(4) 0.0433(10) Uani 1 1 d . . . . . H5A H 0.4480 0.7548 0.8380 0.052 Uiso 1 1 calc R U . . . C6 C 0.4795(4) 0.6529(4) 0.6999(3) 0.0347(8) Uani 1 1 d . . . . . C7 C 0.1734(5) 0.3871(4) 0.4590(3) 0.0382(9) Uani 1 1 d . . . . . H7A H 0.1791 0.3790 0.3846 0.046 Uiso 1 1 calc R U . . . C8 C 0.0367(5) 0.3397(4) 0.4822(4) 0.0443(10) Uani 1 1 d . . . . . H8A H -0.0488 0.2972 0.4252 0.053 Uiso 1 1 calc R U . . . C9 C 0.0263(5) 0.3550(5) 0.5909(4) 0.0444(10) Uani 1 1 d . . . . . H9A H -0.0661 0.3222 0.6090 0.053 Uiso 1 1 calc R U . . . C10 C 0.1512(5) 0.4182(4) 0.6715(4) 0.0390(9) Uani 1 1 d . . . . . H10A H 0.1454 0.4328 0.7457 0.047 Uiso 1 1 calc R U . . . C11 C 0.2859(4) 0.4602(4) 0.6421(3) 0.0330(8) Uani 1 1 d . . . . . C12 C 0.4915(4) 0.4781(4) 0.8080(3) 0.0312(8) Uani 1 1 d . . . . . C13 C 0.5080(4) 0.3211(4) 0.9076(3) 0.0336(8) Uani 1 1 d . . . . . C14 C 0.6872(4) 0.4904(4) 0.9529(3) 0.0323(8) Uani 1 1 d . . . . . C15 C 0.9079(5) 0.6506(4) 0.9928(4) 0.0379(9) Uani 1 1 d . . . . . C16 C 0.9570(5) 0.7618(4) 1.0658(4) 0.0412(9) Uani 1 1 d . . . . . C17 C 1.0575(6) 0.8599(4) 1.0464(5) 0.0522(12) Uani 1 1 d . . . . . C18 C 1.1119(5) 0.8472(5) 0.9540(5) 0.0558(13) Uani 1 1 d . . . . . C19 C 1.0645(5) 0.7382(5) 0.8798(4) 0.0526(12) Uani 1 1 d . . . . . C20 C 0.9633(5) 0.6396(4) 0.8987(4) 0.0411(10) Uani 1 1 d . . . . . F1 F 0.9055(3) 0.7730(3) 1.1576(2) 0.0502(6) Uani 1 1 d . . . . . F2 F 1.1049(4) 0.9667(3) 1.1195(3) 0.0681(9) Uani 1 1 d . . . . . F3 F 1.2127(4) 0.9426(3) 0.9358(3) 0.0835(12) Uani 1 1 d . . . . . F4 F 1.1184(3) 0.7253(4) 0.7893(3) 0.0705(9) Uani 1 1 d . . . . . F5 F 0.9226(3) 0.5322(3) 0.8286(2) 0.0477(6) Uani 1 1 d . . . . . O1S O 0.2897(12) 0.1299(10) 0.6255(7) 0.092(3) Uani 0.5 1 d D U P A 1 C1S C 0.214(2) -0.0017(15) 0.5486(13) 0.116(5) Uani 0.5 1 d D U P A 1 H1S1 H 0.2762 -0.0192 0.4967 0.173 Uiso 0.5 1 calc R U P A 1 H1S2 H 0.1098 0.0031 0.5081 0.173 Uiso 0.5 1 calc R U P A 1 H1S3 H 0.2100 -0.0700 0.5938 0.173 Uiso 0.5 1 calc R U P A 1 O2S O 0.1754(13) 0.0345(10) 0.6401(10) 0.099(3) Uani 0.5 1 d D U P B 2 C2S C 0.0128(18) -0.0097(16) 0.6580(14) 0.109(5) Uani 0.5 1 d D U P B 2 H2S1 H -0.0009 0.0440 0.7213 0.164 Uiso 0.5 1 calc R U P B 2 H2S2 H 0.0028 -0.0982 0.6714 0.164 Uiso 0.5 1 calc R U P B 2 H2S3 H -0.0658 -0.0028 0.5924 0.164 Uiso 0.5 1 calc R U P B 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 0.0284(4) 0.0314(4) 0.0314(4) 0.0078(3) 0.0159(3) 0.0093(3) Cl1 0.0434(6) 0.0383(5) 0.0473(6) 0.0080(4) 0.0160(5) 0.0024(4) S1 0.0435(6) 0.0433(6) 0.0471(6) 0.0149(5) 0.0191(5) 0.0182(5) O1 0.0315(14) 0.0393(15) 0.0365(15) 0.0117(12) 0.0068(12) 0.0041(11) N1 0.0321(16) 0.0371(17) 0.0343(17) 0.0084(14) 0.0167(14) 0.0110(13) N2 0.0308(16) 0.0359(17) 0.0399(18) 0.0088(14) 0.0101(14) 0.0071(13) N3 0.0318(16) 0.0370(17) 0.0388(18) 0.0093(14) 0.0145(14) 0.0111(13) N4 0.0290(16) 0.0354(17) 0.0337(16) 0.0048(13) 0.0126(13) 0.0086(13) N5 0.0302(16) 0.0390(18) 0.0341(17) 0.0042(13) 0.0158(13) 0.0073(13) N6 0.0281(16) 0.0386(17) 0.0375(17) 0.0075(14) 0.0124(14) 0.0081(13) N7 0.0312(16) 0.0338(17) 0.0365(17) 0.0028(13) 0.0142(14) 0.0059(13) C1 0.0295(18) 0.037(2) 0.038(2) 0.0039(16) 0.0188(16) 0.0071(15) C2 0.044(2) 0.037(2) 0.047(2) 0.0098(18) 0.0148(19) 0.0043(18) C3 0.065(3) 0.037(2) 0.055(3) 0.006(2) 0.017(2) 0.004(2) C4 0.059(3) 0.039(2) 0.052(3) -0.001(2) 0.012(2) 0.010(2) C5 0.046(2) 0.048(2) 0.038(2) 0.0042(18) 0.0121(19) 0.0138(19) C6 0.0302(19) 0.038(2) 0.038(2) 0.0067(16) 0.0091(16) 0.0111(16) C7 0.036(2) 0.044(2) 0.038(2) 0.0068(17) 0.0153(17) 0.0076(17) C8 0.033(2) 0.052(3) 0.048(2) 0.007(2) 0.0102(18) 0.0039(18) C9 0.031(2) 0.063(3) 0.048(2) 0.015(2) 0.0208(19) 0.0102(19) C10 0.037(2) 0.048(2) 0.040(2) 0.0125(18) 0.0203(18) 0.0137(18) C11 0.0287(18) 0.039(2) 0.037(2) 0.0086(16) 0.0150(16) 0.0105(15) C12 0.0264(17) 0.039(2) 0.0325(19) 0.0030(15) 0.0149(15) 0.0102(15) C13 0.0337(19) 0.036(2) 0.036(2) 0.0065(16) 0.0173(16) 0.0085(16) C14 0.0289(18) 0.038(2) 0.0321(19) 0.0026(15) 0.0122(15) 0.0075(15) C15 0.0304(19) 0.040(2) 0.045(2) 0.0148(18) 0.0083(17) 0.0089(16) C16 0.034(2) 0.048(2) 0.043(2) 0.0139(19) 0.0068(18) 0.0108(18) C17 0.044(2) 0.039(2) 0.068(3) 0.014(2) -0.001(2) 0.0046(19) C18 0.039(2) 0.058(3) 0.072(3) 0.036(3) 0.009(2) 0.004(2) C19 0.037(2) 0.069(3) 0.055(3) 0.026(3) 0.011(2) 0.006(2) C20 0.0271(19) 0.054(3) 0.045(2) 0.019(2) 0.0082(17) 0.0093(17) F1 0.0424(14) 0.0512(15) 0.0551(16) 0.0037(12) 0.0095(12) 0.0090(12) F2 0.0600(18) 0.0408(15) 0.090(2) 0.0135(15) -0.0057(17) -0.0001(13) F3 0.0557(19) 0.078(2) 0.110(3) 0.053(2) 0.0083(19) -0.0167(16) F4 0.0465(16) 0.110(3) 0.0604(19) 0.0313(18) 0.0239(14) 0.0002(16) F5 0.0393(13) 0.0592(16) 0.0469(15) 0.0068(12) 0.0153(11) 0.0096(12) O1S 0.094(7) 0.117(7) 0.060(5) 0.015(5) 0.026(5) -0.008(6) C1S 0.131(11) 0.111(9) 0.089(9) 0.025(7) 0.029(9) -0.038(9) O2S 0.114(7) 0.083(6) 0.101(7) -0.001(5) 0.033(6) 0.018(6) C2S 0.111(9) 0.104(11) 0.100(10) -0.047(9) 0.033(9) 0.010(8) _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 N1 1.953(3) 2_666 ? Fe1 N1 1.953(3) . ? Fe1 N2 2.005(3) . ? Fe1 N2 2.005(3) 2_666 ? Fe1 N3 2.012(3) 2_666 ? Fe1 N3 2.012(3) . ? Cl1 C13 1.731(4) . ? S1 C1 1.637(4) . ? O1 C14 1.372(5) . ? O1 C15 1.372(5) . ? N1 C1 1.166(5) . ? N2 C6 1.332(5) . ? N2 C2 1.361(5) . ? N3 C11 1.349(5) . ? N3 C7 1.352(5) . ? N4 C12 1.373(5) . ? N4 C11 1.423(5) . ? N4 C6 1.433(5) . ? N5 C13 1.315(5) . ? N5 C12 1.335(5) . ? N6 C14 1.319(5) . ? N6 C12 1.347(5) . ? N7 C13 1.339(5) . ? N7 C14 1.343(5) . ? C2 C3 1.379(6) . ? C2 H2A 0.9500 . ? C3 C4 1.375(7) . ? C3 H3A 0.9500 . ? C4 C5 1.375(7) . ? C4 H4A 0.9500 . ? C5 C6 1.405(6) . ? C5 H5A 0.9500 . ? C7 C8 1.380(6) . ? C7 H7A 0.9500 . ? C8 C9 1.395(6) . ? C8 H8A 0.9500 . ? C9 C10 1.374(6) . ? C9 H9A 0.9500 . ? C10 C11 1.388(5) . ? C10 H10A 0.9500 . ? C15 C16 1.381(6) . ? C15 C20 1.396(6) . ? C16 F1 1.349(5) . ? C16 C17 1.374(6) . ? C17 F2 1.346(6) . ? C17 C18 1.372(8) . ? C18 F3 1.349(5) . ? C18 C19 1.371(8) . ? C19 F4 1.348(6) . ? C19 C20 1.379(6) . ? C20 F5 1.329(5) . ? O1S C1S 1.595(14) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? O2S C2S 1.559(14) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 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 N1 Fe1 N1 180.0 2_666 . ? N1 Fe1 N2 93.63(14) 2_666 . ? N1 Fe1 N2 86.37(14) . . ? N1 Fe1 N2 86.36(14) 2_666 2_666 ? N1 Fe1 N2 93.64(14) . 2_666 ? N2 Fe1 N2 180.0 . 2_666 ? N1 Fe1 N3 88.94(13) 2_666 2_666 ? N1 Fe1 N3 91.06(13) . 2_666 ? N2 Fe1 N3 93.40(13) . 2_666 ? N2 Fe1 N3 86.60(13) 2_666 2_666 ? N1 Fe1 N3 91.06(13) 2_666 . ? N1 Fe1 N3 88.94(13) . . ? N2 Fe1 N3 86.60(13) . . ? N2 Fe1 N3 93.40(13) 2_666 . ? N3 Fe1 N3 180.0 2_666 . ? C14 O1 C15 119.1(3) . . ? C1 N1 Fe1 166.4(3) . . ? C6 N2 C2 117.1(4) . . ? C6 N2 Fe1 121.3(3) . . ? C2 N2 Fe1 121.3(3) . . ? C11 N3 C7 117.4(3) . . ? C11 N3 Fe1 121.8(3) . . ? C7 N3 Fe1 120.8(3) . . ? C12 N4 C11 121.3(3) . . ? C12 N4 C6 121.0(3) . . ? C11 N4 C6 117.4(3) . . ? C13 N5 C12 113.5(3) . . ? C14 N6 C12 112.6(3) . . ? C13 N7 C14 109.4(3) . . ? N1 C1 S1 179.7(3) . . ? N2 C2 C3 122.8(4) . . ? N2 C2 H2A 118.6 . . ? C3 C2 H2A 118.6 . . ? C4 C3 C2 118.9(4) . . ? C4 C3 H3A 120.5 . . ? C2 C3 H3A 120.5 . . ? C3 C4 C5 119.8(4) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? C4 C5 C6 117.9(4) . . ? C4 C5 H5A 121.1 . . ? C6 C5 H5A 121.1 . . ? N2 C6 C5 123.4(4) . . ? N2 C6 N4 116.9(3) . . ? C5 C6 N4 119.6(4) . . ? N3 C7 C8 122.6(4) . . ? N3 C7 H7A 118.7 . . ? C8 C7 H7A 118.7 . . ? C7 C8 C9 118.8(4) . . ? C7 C8 H8A 120.6 . . ? C9 C8 H8A 120.6 . . ? C10 C9 C8 119.3(4) . . ? C10 C9 H9A 120.4 . . ? C8 C9 H9A 120.4 . . ? C9 C10 C11 118.5(4) . . ? C9 C10 H10A 120.8 . . ? C11 C10 H10A 120.8 . . ? N3 C11 C10 123.2(4) . . ? N3 C11 N4 115.4(3) . . ? C10 C11 N4 121.3(4) . . ? N5 C12 N6 125.4(4) . . ? N5 C12 N4 118.0(3) . . ? N6 C12 N4 116.6(3) . . ? N5 C13 N7 129.3(4) . . ? N5 C13 Cl1 116.1(3) . . ? N7 C13 Cl1 114.6(3) . . ? N6 C14 N7 129.6(4) . . ? N6 C14 O1 118.8(3) . . ? N7 C14 O1 111.6(3) . . ? O1 C15 C16 118.9(4) . . ? O1 C15 C20 122.0(4) . . ? C16 C15 C20 118.5(4) . . ? F1 C16 C17 120.0(4) . . ? F1 C16 C15 119.0(4) . . ? C17 C16 C15 121.0(4) . . ? F2 C17 C18 120.3(5) . . ? F2 C17 C16 119.8(5) . . ? C18 C17 C16 119.8(5) . . ? F3 C18 C19 119.7(5) . . ? F3 C18 C17 119.9(5) . . ? C19 C18 C17 120.4(4) . . ? F4 C19 C18 120.5(4) . . ? F4 C19 C20 119.5(5) . . ? C18 C19 C20 120.0(5) . . ? F5 C20 C19 119.6(4) . . ? F5 C20 C15 120.1(4) . . ? C19 C20 C15 120.3(5) . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? O2S C2S H2S1 109.5 . . ? O2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? O2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? _refine_diff_density_max 0.857 _refine_diff_density_min -0.721 _refine_diff_density_rms 0.089 _shelxl_version_number 2013-3 _shelx_res_file ; TITL c1_new in P-1 CELL 0.77490 9.084 10.766 12.658 96.115 103.282 98.341 ZERR 1.00 0.004 0.005 0.005 0.006 0.005 0.005 LATT 1 SFAC C H N O F S CL FE DISP Fe 0.20639 0.99298 4412.23 DISP Cl 0.14076 0.18956 859.19 DISP S 0.12060 0.14800 674.22 DISP F -0.00532 0.01246 64.36 DISP O -0.00415 0.00737 40.17 DISP N -0.00306 0.00403 23.92 DISP C -0.00202 0.00197 13.60 DISP H 0.00000 0.00000 0.67 UNIT 42 24 14 4 10 2 2 1 TEMP -173 SIZE 0.11 0.05 0.02 REM yellow parallelepiped purple at 100 K REM integrated to 0.75 angstrom L.S. 10 BOND $H ACTA 62.2 FMAP 2 PLAN 10 DFIX 1.45 O1S C1S O2S C2S SIMU 0.012 O1S > C2S DELU 0.003 O1S > C2S WGHT 0.074100 2.710800 FVAR 0.33785 FE1 8 0.500000 0.500000 0.500000 10.50000 0.02840 0.03141 = 0.03140 0.00776 0.01589 0.00930 CL1 7 0.435635 0.170883 0.929628 11.00000 0.04345 0.03826 = 0.04733 0.00795 0.01596 0.00241 S1 6 0.278222 0.774535 0.267530 11.00000 0.04348 0.04331 = 0.04711 0.01491 0.01914 0.01817 O1 4 0.824684 0.549132 1.022437 11.00000 0.03146 0.03930 = 0.03648 0.01173 0.00685 0.00410 N1 3 0.393333 0.592021 0.389925 11.00000 0.03214 0.03708 = 0.03428 0.00840 0.01670 0.01105 N2 3 0.525152 0.657173 0.607465 11.00000 0.03083 0.03589 = 0.03993 0.00883 0.01014 0.00715 N3 3 0.299392 0.444758 0.537786 11.00000 0.03176 0.03704 = 0.03875 0.00928 0.01447 0.01115 N4 3 0.417594 0.530432 0.720953 11.00000 0.02897 0.03541 = 0.03374 0.00480 0.01257 0.00860 N5 3 0.429053 0.362863 0.822064 11.00000 0.03016 0.03897 = 0.03410 0.00419 0.01577 0.00728 N6 3 0.623407 0.547795 0.871710 11.00000 0.02806 0.03855 = 0.03745 0.00747 0.01243 0.00812 N7 3 0.636596 0.378637 0.981833 11.00000 0.03116 0.03377 = 0.03653 0.00284 0.01418 0.00588 C1 1 0.345110 0.667955 0.339178 11.00000 0.02955 0.03697 = 0.03780 0.00388 0.01880 0.00715 C2 1 0.576633 0.773886 0.584370 11.00000 0.04379 0.03727 = 0.04656 0.00975 0.01482 0.00431 AFIX 43 H2A 2 0.607563 0.779353 0.517995 11.00000 -1.20000 AFIX 0 C3 1 0.585786 0.884472 0.653208 11.00000 0.06482 0.03663 = 0.05548 0.00647 0.01717 0.00432 AFIX 43 H3A 2 0.624437 0.964201 0.635253 11.00000 -1.20000 AFIX 0 C4 1 0.538096 0.877529 0.748236 11.00000 0.05920 0.03890 = 0.05218 -0.00107 0.01191 0.01017 AFIX 43 H4A 2 0.543310 0.952788 0.796532 11.00000 -1.20000 AFIX 0 C5 1 0.482843 0.761426 0.773216 11.00000 0.04629 0.04757 = 0.03799 0.00425 0.01210 0.01381 AFIX 43 H5A 2 0.448042 0.754813 0.838001 11.00000 -1.20000 AFIX 0 C6 1 0.479464 0.652876 0.699931 11.00000 0.03020 0.03774 = 0.03819 0.00670 0.00909 0.01113 C7 1 0.173356 0.387133 0.458986 11.00000 0.03565 0.04412 = 0.03834 0.00682 0.01534 0.00761 AFIX 43 H7A 2 0.179103 0.378998 0.384634 11.00000 -1.20000 AFIX 0 C8 1 0.036728 0.339666 0.482209 11.00000 0.03279 0.05158 = 0.04750 0.00690 0.01015 0.00394 AFIX 43 H8A 2 -0.048771 0.297242 0.425152 11.00000 -1.20000 AFIX 0 C9 1 0.026319 0.355047 0.590899 11.00000 0.03083 0.06252 = 0.04756 0.01464 0.02076 0.01022 AFIX 43 H9A 2 -0.066140 0.322188 0.608995 11.00000 -1.20000 AFIX 0 C10 1 0.151199 0.418223 0.671511 11.00000 0.03693 0.04832 = 0.04035 0.01247 0.02033 0.01374 AFIX 43 H10A 2 0.145443 0.432824 0.745687 11.00000 -1.20000 AFIX 0 C11 1 0.285930 0.460220 0.642127 11.00000 0.02866 0.03901 = 0.03671 0.00862 0.01503 0.01045 C12 1 0.491516 0.478092 0.808007 11.00000 0.02643 0.03930 = 0.03247 0.00300 0.01487 0.01024 C13 1 0.508010 0.321060 0.907605 11.00000 0.03372 0.03643 = 0.03599 0.00646 0.01732 0.00849 C14 1 0.687177 0.490355 0.952898 11.00000 0.02892 0.03799 = 0.03212 0.00260 0.01218 0.00754 C15 1 0.907871 0.650573 0.992787 11.00000 0.03036 0.04011 = 0.04550 0.01481 0.00827 0.00894 C16 1 0.956997 0.761803 1.065798 11.00000 0.03433 0.04780 = 0.04290 0.01391 0.00683 0.01082 C17 1 1.057521 0.859858 1.046439 11.00000 0.04361 0.03895 = 0.06751 0.01357 -0.00057 0.00465 C18 1 1.111916 0.847216 0.954039 11.00000 0.03892 0.05842 = 0.07218 0.03562 0.00924 0.00368 C19 1 1.064465 0.738186 0.879828 11.00000 0.03667 0.06888 = 0.05477 0.02608 0.01077 0.00573 C20 1 0.963277 0.639556 0.898729 11.00000 0.02706 0.05396 = 0.04528 0.01877 0.00819 0.00930 F1 5 0.905500 0.773018 1.157586 11.00000 0.04243 0.05120 = 0.05507 0.00366 0.00953 0.00904 F2 5 1.104866 0.966734 1.119500 11.00000 0.05998 0.04077 = 0.08956 0.01355 -0.00570 -0.00008 F3 5 1.212651 0.942632 0.935816 11.00000 0.05569 0.07812 = 0.11040 0.05261 0.00825 -0.01669 F4 5 1.118434 0.725304 0.789259 11.00000 0.04646 0.11013 = 0.06036 0.03130 0.02392 0.00018 F5 5 0.922575 0.532221 0.828619 11.00000 0.03926 0.05915 = 0.04690 0.00677 0.01529 0.00957 PART 1 O1S 4 0.289699 0.129945 0.625519 10.50000 0.09449 0.11734 = 0.06034 0.01526 0.02607 -0.00807 C1S 1 0.214156 -0.001708 0.548609 10.50000 0.13084 0.11109 = 0.08943 0.02487 0.02879 -0.03753 AFIX 137 H1S1 2 0.276201 -0.019197 0.496650 10.50000 -1.50000 H1S2 2 0.109845 0.003143 0.508091 10.50000 -1.50000 H1S3 2 0.210012 -0.069951 0.593833 10.50000 -1.50000 AFIX 0 PART 2 O2S 4 0.175388 0.034457 0.640139 10.50000 0.11358 0.08327 = 0.10114 -0.00123 0.03253 0.01822 C2S 1 0.012782 -0.009726 0.657957 10.50000 0.11084 0.10373 = 0.09983 -0.04704 0.03254 0.01036 AFIX 137 H2S1 2 -0.000857 0.044001 0.721299 10.50000 -1.50000 H2S2 2 0.002767 -0.098171 0.671398 10.50000 -1.50000 H2S3 2 -0.065766 -0.002779 0.592375 10.50000 -1.50000 PART 0 AFIX 0 HKLF 4 REM c1_new in P-1 REM R1 = 0.0662 for 3992 Fo > 4sig(Fo) and 0.0866 for all 5362 data REM 360 parameters refined using 28 restraints END WGHT 0.0744 2.7010 REM Highest difference peak 0.857, deepest hole -0.721, 1-sigma level 0.089 Q1 1 0.4734 0.5065 0.4337 11.00000 0.05 0.86 Q2 1 0.4076 0.1759 0.8634 11.00000 0.05 0.84 Q3 1 0.2298 -0.0505 0.5348 11.00000 0.05 0.80 Q4 1 0.3073 0.7796 0.3349 11.00000 0.05 0.69 Q5 1 0.4504 0.4275 0.4833 11.00000 0.05 0.64 Q6 1 0.2204 0.7039 0.2538 11.00000 0.05 0.56 Q7 1 -0.0224 -0.0436 0.6672 11.00000 0.05 0.45 Q8 1 0.6780 0.3588 1.0397 11.00000 0.05 0.43 Q9 1 0.1729 0.0958 0.5339 11.00000 0.05 0.42 Q10 1 0.2559 0.0483 0.7354 11.00000 0.05 0.41 ; _shelx_res_checksum 60523 _shelx_hkl_file ; -3 0 0 216.56 11.27 3 0 0 205.53 12.01 3 0 0 209.36 9.73 -4 0 0 5.19 1.03 4 0 0 2.12 0.86 4 0 0 2.53 0.53 -5 0 0 183.94 10.02 5 0 0 187.43 10.69 -6 0 0 8.16 1.37 6 0 0 6.63 1.19 -7 0 0 -0.35 1.13 -7 0 0 -0.68 0.98 7 0 0 0.80 1.03 -8 0 0 1.16 1.06 -8 0 0 0.68 1.25 8 0 0 0.77 1.12 -9 0 0 23.87 2.19 -9 0 0 24.09 2.04 9 0 0 27.71 2.16 -10 0 0 6.30 1.41 10 0 0 10.18 1.54 -11 0 0 -0.81 1.34 11 0 0 0.41 1.24 11 -1 0 -0.71 1.22 -11 1 0 -0.90 1.19 10 -1 0 0.64 1.29 -10 1 0 -0.64 1.31 9 -1 0 28.85 2.23 -9 1 0 26.02 2.18 8 -1 0 0.51 1.07 -8 1 0 -0.04 1.05 -8 1 0 -0.44 1.23 7 -1 0 112.87 6.82 -7 1 0 123.02 6.42 -7 1 0 110.59 5.66 6 -1 0 96.14 5.54 -6 1 0 87.31 5.14 -6 1 0 95.93 4.60 5 -1 0 212.35 12.31 -5 1 0 218.27 10.04 -5 1 0 213.18 11.50 4 -1 0 162.62 9.05 4 -1 0 153.18 7.90 -4 1 0 160.38 7.39 -4 1 0 153.15 8.46 3 -1 0 228.42 13.58 3 -1 0 238.25 11.90 -3 1 0 239.74 11.06 -3 1 0 247.42 12.71 2 -1 0 210.38 11.82 2 -1 0 199.11 10.36 -2 1 0 212.26 11.04 -2 1 0 208.66 9.61 -2 -1 0 144.74 7.34 2 1 0 131.49 6.29 2 1 0 131.30 7.78 -3 -1 0 306.30 16.19 3 1 0 304.68 17.27 3 1 0 299.77 13.99 -4 -1 0 71.70 3.94 4 1 0 64.87 3.28 4 1 0 69.10 4.14 -5 -1 0 2.66 1.13 5 1 0 3.50 0.67 5 1 0 3.75 1.01 -6 -1 0 117.92 7.02 6 1 0 129.35 7.47 6 1 0 134.67 6.02 -7 -1 0 -0.40 1.41 7 1 0 0.56 1.17 -8 -1 0 15.99 1.88 8 1 0 19.69 1.87 -9 -1 0 87.60 4.66 -9 -1 0 68.29 4.11 9 1 0 79.59 4.93 -10 -1 0 27.53 2.34 10 1 0 30.25 2.46 -11 -1 0 3.93 1.34 11 1 0 8.20 1.62 11 -2 0 11.48 1.56 -11 2 0 7.82 1.48 10 -2 0 30.36 2.36 -10 2 0 28.55 2.19 9 -2 0 11.70 1.53 -9 2 0 7.96 1.37 8 -2 0 1.23 1.09 -8 2 0 1.70 1.03 7 -2 0 80.12 4.67 -7 2 0 77.57 4.00 -7 2 0 73.78 4.32 6 -2 0 54.79 3.39 6 -2 0 56.90 2.90 -6 2 0 54.33 2.89 -6 2 0 50.42 3.10 5 -2 0 2.43 0.77 5 -2 0 1.87 0.85 -5 2 0 1.24 0.91 -5 2 0 3.01 0.74 4 -2 0 111.06 6.44 4 -2 0 113.57 5.67 -4 2 0 102.44 5.97 -4 2 0 117.29 5.30 3 -2 0 7.96 0.92 3 -2 0 7.35 0.86 -3 2 0 6.50 0.84 -3 2 0 4.90 0.60 1 -2 0 221.94 11.18 1 -2 0 223.95 12.69 -1 2 0 224.79 10.33 0 -2 0 48.43 2.76 0 -2 0 48.89 2.60 0 2 0 50.46 2.39 -1 -2 0 14.01 1.02 -1 -2 0 15.77 1.30 1 2 0 15.28 0.88 1 2 0 16.08 1.30 -2 -2 0 350.81 18.05 2 2 0 332.69 15.59 2 2 0 332.25 19.23 -3 -2 0 185.36 9.80 3 2 0 179.62 10.41 3 2 0 179.99 8.41 -4 -2 0 62.22 3.66 4 2 0 62.89 3.02 4 2 0 62.88 3.85 -5 -2 0 17.42 1.63 5 2 0 16.09 1.13 5 2 0 15.53 1.60 -6 -2 0 102.72 5.79 6 2 0 100.71 6.12 6 2 0 104.43 4.89 -7 -2 0 8.97 1.69 7 2 0 6.10 1.34 7 2 0 6.05 0.89 -8 -2 0 14.06 1.91 8 2 0 17.12 1.82 -9 -2 0 3.72 1.50 9 2 0 2.72 1.32 -10 -2 0 2.11 1.25 -10 -2 0 6.07 1.55 10 2 0 6.15 1.56 11 -3 0 1.04 1.11 -11 3 0 1.28 1.28 -10 3 0 42.30 2.69 9 -3 0 17.06 1.72 -9 3 0 15.68 1.73 8 -3 0 59.79 3.79 -8 3 0 60.28 3.28 7 -3 0 0.46 0.97 7 -3 0 1.35 0.93 -7 3 0 0.09 0.99 6 -3 0 15.21 1.29 6 -3 0 12.66 1.36 -6 3 0 12.94 1.39 -6 3 0 11.90 1.03 5 -3 0 78.96 4.16 5 -3 0 82.20 4.73 -5 3 0 74.01 4.28 -5 3 0 83.02 3.94 4 -3 0 3.62 0.97 4 -3 0 3.01 0.84 -4 3 0 3.21 0.85 3 -3 0 11.75 1.07 3 -3 0 11.87 1.23 -3 3 0 11.59 1.08 2 -3 0 19.33 1.47 2 -3 0 19.26 1.38 -2 3 0 20.65 1.33 0 -3 0 73.09 3.95 0 -3 0 70.13 3.71 0 3 0 70.52 3.38 0 3 0 70.64 4.15 -1 -3 0 39.64 2.21 -1 -3 0 39.55 2.46 1 3 0 42.25 2.52 1 3 0 39.08 1.99 -2 -3 0 14.77 1.54 2 3 0 17.89 1.40 2 3 0 16.88 1.02 -3 -3 0 59.38 3.69 3 3 0 65.08 3.05 3 3 0 63.86 3.86 -4 -3 0 21.24 1.79 4 3 0 22.78 1.30 4 3 0 21.55 1.80 -5 -3 0 30.05 2.34 5 3 0 31.53 2.34 5 3 0 31.85 1.70 -6 -3 0 88.30 5.15 6 3 0 92.32 4.31 6 3 0 87.01 5.42 -7 -3 0 51.88 3.33 7 3 0 49.30 3.50 7 3 0 53.88 2.69 -8 -3 0 1.33 1.58 8 3 0 0.48 0.85 8 3 0 0.39 1.38 -9 -3 0 1.76 1.49 9 3 0 2.29 1.39 -10 -3 0 0.24 1.45 10 3 0 0.78 1.57 11 -4 0 0.22 1.13 -11 4 0 -1.26 1.26 10 -4 0 29.65 2.34 -10 4 0 30.74 2.32 9 -4 0 8.16 1.26 -9 4 0 8.67 1.41 8 -4 0 40.91 2.85 -8 4 0 44.08 2.59 7 -4 0 23.46 1.69 7 -4 0 20.04 1.76 -7 4 0 20.93 1.78 6 -4 0 4.44 0.95 6 -4 0 5.62 1.04 -6 4 0 4.74 1.01 5 -4 0 191.50 10.95 5 -4 0 188.63 9.64 -5 4 0 191.24 8.97 4 -4 0 115.67 5.92 4 -4 0 114.38 6.64 -4 4 0 112.98 5.47 3 -4 0 127.99 7.47 3 -4 0 129.29 6.65 -3 4 0 131.87 6.15 2 -4 0 109.74 5.68 2 -4 0 109.17 6.35 -2 4 0 111.30 5.89 -2 4 0 111.06 5.23 1 -4 0 123.68 6.27 -1 4 0 132.48 5.79 -1 4 0 113.23 7.05 0 -4 0 103.35 5.44 0 -4 0 105.41 5.81 0 4 0 113.08 6.17 0 4 0 102.60 4.98 -1 -4 0 348.97 18.55 -1 -4 0 359.35 19.85 1 4 0 407.82 21.18 1 4 0 373.05 17.15 -2 -4 0 0.69 1.09 -2 -4 0 2.29 0.72 2 4 0 2.12 1.05 2 4 0 1.91 0.61 -3 -4 0 0.78 1.12 3 4 0 0.69 0.57 3 4 0 0.82 1.04 -4 -4 0 3.00 1.34 4 4 0 0.92 0.67 4 4 0 1.31 1.06 -5 -4 0 169.09 9.25 5 4 0 168.98 9.83 5 4 0 167.88 7.88 -6 -4 0 0.93 1.37 6 4 0 0.85 1.30 6 4 0 1.23 0.77 -7 -4 0 1.68 1.54 7 4 0 1.73 0.86 7 4 0 1.21 1.32 -8 -4 0 -0.52 1.59 8 4 0 -1.10 1.41 8 4 0 -0.65 0.87 -9 -4 0 19.93 2.15 9 4 0 18.18 2.20 9 4 0 17.94 1.50 -10 -4 0 9.78 1.79 10 4 0 9.86 1.76 11 -5 0 15.79 1.81 -11 5 0 17.24 1.85 10 -5 0 41.01 2.86 -10 5 0 38.51 2.57 9 -5 0 4.66 1.20 -9 5 0 4.04 1.19 8 -5 0 30.78 2.12 8 -5 0 27.99 2.23 -8 5 0 29.35 2.07 7 -5 0 80.17 4.89 7 -5 0 80.81 4.38 -7 5 0 81.36 4.12 6 -5 0 8.67 1.21 6 -5 0 12.11 1.34 -6 5 0 9.80 1.22 5 -5 0 11.34 1.24 5 -5 0 11.26 1.48 -5 5 0 13.99 1.27 4 -5 0 5.31 1.15 4 -5 0 5.10 0.87 -4 5 0 5.47 0.94 3 -5 0 9.74 1.26 3 -5 0 6.63 0.91 -3 5 0 7.91 0.95 2 -5 0 43.25 2.70 2 -5 0 46.21 2.79 -2 5 0 47.15 2.37 1 -5 0 33.58 2.21 1 -5 0 35.63 2.21 -1 5 0 35.69 2.24 -1 5 0 34.94 1.98 0 -5 0 10.98 1.40 0 -5 0 15.76 1.49 0 5 0 14.10 1.09 -1 -5 0 69.68 4.10 -1 -5 0 69.46 3.78 1 5 0 76.45 4.33 1 5 0 69.44 3.42 -2 -5 0 112.74 6.46 -2 -5 0 106.42 5.90 2 5 0 121.89 5.46 2 5 0 123.75 6.82 -3 -5 0 49.55 3.24 3 5 0 54.87 2.61 3 5 0 53.17 3.41 -4 -5 0 154.94 8.88 4 5 0 165.80 7.57 4 5 0 164.35 9.42 -5 -5 0 237.97 12.84 5 5 0 241.30 11.00 5 5 0 230.15 13.67 -6 -5 0 66.78 4.09 6 5 0 65.24 4.38 6 5 0 68.95 3.34 -7 -5 0 39.15 2.75 7 5 0 33.35 2.92 7 5 0 37.42 2.06 -8 -5 0 0.90 1.71 8 5 0 1.68 0.97 8 5 0 1.12 1.47 -9 -5 0 -0.50 1.68 9 5 0 0.28 0.85 9 5 0 -0.24 1.40 11 -6 0 18.47 1.86 -11 6 0 19.04 1.94 10 -6 0 40.58 2.89 -10 6 0 42.54 2.63 9 -6 0 0.84 1.04 -9 6 0 1.94 1.17 8 -6 0 0.60 1.18 8 -6 0 0.52 0.99 -8 6 0 -0.01 1.15 7 -6 0 9.71 1.23 7 -6 0 9.58 1.38 -7 6 0 10.11 1.34 6 -6 0 58.67 3.66 6 -6 0 60.01 3.39 -6 6 0 57.39 3.17 5 -6 0 15.25 1.48 5 -6 0 12.39 1.33 -5 6 0 12.46 1.44 4 -6 0 18.93 1.75 4 -6 0 18.95 1.47 -4 6 0 19.33 1.49 3 -6 0 14.81 1.33 3 -6 0 16.07 1.60 -3 6 0 14.71 1.32 2 -6 0 590.03 30.62 2 -6 0 582.07 28.75 -2 6 0 557.22 26.57 1 -6 0 393.89 19.26 1 -6 0 397.17 20.53 -1 6 0 368.70 21.87 -1 6 0 379.99 17.78 0 -6 0 127.38 7.19 0 -6 0 127.25 6.73 0 6 0 129.76 6.17 0 6 0 139.29 7.65 -1 -6 0 4.45 1.01 -1 -6 0 5.00 1.31 1 6 0 4.07 1.10 1 6 0 4.99 0.75 -2 -6 0 108.87 5.92 -2 -6 0 112.29 6.49 2 6 0 124.62 6.85 2 6 0 118.39 5.47 -3 -6 0 154.42 8.67 3 6 0 160.35 9.20 3 6 0 157.97 7.37 -4 -6 0 48.78 3.24 4 6 0 49.79 2.49 4 6 0 48.38 3.32 -5 -6 0 36.13 2.61 5 6 0 32.59 2.74 5 6 0 33.23 1.94 -6 -6 0 3.18 1.55 6 6 0 1.45 0.85 6 6 0 3.48 1.60 -7 -6 0 7.99 1.70 7 6 0 7.57 0.99 7 6 0 7.48 1.65 -8 -6 0 -1.29 1.70 8 6 0 0.43 0.95 8 6 0 0.29 1.55 -9 -6 0 2.40 1.73 9 6 0 2.34 0.98 9 6 0 2.56 1.60 10 -7 0 30.37 2.38 -10 7 0 31.71 2.30 9 -7 0 5.60 1.23 9 -7 0 10.52 1.52 -9 7 0 5.95 1.33 8 -7 0 -1.00 0.98 8 -7 0 1.74 1.25 -8 7 0 0.48 1.13 7 -7 0 14.26 1.56 7 -7 0 18.49 1.74 -7 7 0 13.32 1.58 6 -7 0 15.61 1.71 6 -7 0 16.51 1.53 -6 7 0 17.19 1.60 5 -7 0 99.70 5.41 5 -7 0 100.43 6.03 -5 7 0 107.61 5.04 4 -7 0 84.97 4.63 4 -7 0 87.27 5.09 -4 7 0 84.76 4.25 3 -7 0 3.33 0.93 3 -7 0 2.45 0.92 3 -7 0 2.09 1.22 -3 7 0 3.56 0.95 2 -7 0 135.74 7.36 2 -7 0 133.02 6.96 -2 7 0 132.72 7.79 -2 7 0 136.72 6.40 1 -7 0 126.23 6.79 1 -7 0 115.99 6.38 -1 7 0 124.57 5.86 -1 7 0 124.82 7.17 0 -7 0 147.65 7.48 0 -7 0 142.85 8.00 0 7 0 146.71 8.51 0 7 0 145.53 6.86 -1 -7 0 7.12 1.46 -1 -7 0 7.70 1.28 1 7 0 8.56 0.91 1 7 0 7.37 1.23 -2 -7 0 2.22 1.33 -2 -7 0 1.72 0.90 2 7 0 1.59 0.73 2 7 0 3.75 1.26 -3 -7 0 1.78 1.49 3 7 0 1.71 0.74 3 7 0 0.95 1.40 -4 -7 0 67.29 4.26 4 7 0 70.28 4.46 4 7 0 70.59 3.43 -5 -7 0 3.39 1.67 5 7 0 0.60 0.83 5 7 0 2.31 1.48 -6 -7 0 2.21 1.58 6 7 0 2.80 1.63 6 7 0 1.31 0.94 -7 -7 0 3.47 1.67 7 7 0 2.51 0.82 7 7 0 2.97 1.62 -8 -7 0 8.26 1.89 8 7 0 5.26 1.07 8 7 0 4.34 1.74 10 -8 0 2.68 1.17 -10 8 0 -0.30 1.29 9 -8 0 7.40 1.46 9 -8 0 5.76 1.26 -9 8 0 5.11 1.33 8 -8 0 19.04 1.82 8 -8 0 19.65 1.88 -8 8 0 19.65 1.79 7 -8 0 1.86 1.26 7 -8 0 1.25 0.96 -7 8 0 0.90 1.04 6 -8 0 7.03 1.35 6 -8 0 6.63 1.14 -6 8 0 7.33 1.20 5 -8 0 29.43 2.33 5 -8 0 31.57 2.25 -5 8 0 30.76 2.04 4 -8 0 -0.09 1.24 4 -8 0 1.43 0.98 -4 8 0 0.51 1.00 3 -8 0 122.74 6.39 -3 8 0 115.75 7.12 -3 8 0 127.26 5.87 2 -8 0 -3.14 1.26 2 -8 0 -1.98 1.07 -2 8 0 0.38 0.98 -2 8 0 1.79 1.07 1 -8 0 14.91 1.52 1 -8 0 15.21 1.62 -1 8 0 11.97 1.31 -1 8 0 11.93 1.46 0 -8 0 45.29 3.08 0 -8 0 48.93 2.87 0 8 0 44.11 3.21 0 8 0 48.89 2.50 -1 -8 0 -0.42 1.05 -1 -8 0 -1.87 1.31 1 8 0 1.02 0.79 1 8 0 2.40 1.28 -2 -8 0 190.03 10.68 -2 -8 0 194.94 9.89 2 8 0 204.99 9.15 2 8 0 191.52 11.38 -3 -8 0 49.91 3.23 3 8 0 47.74 2.47 3 8 0 44.51 3.33 -4 -8 0 47.28 3.05 4 8 0 43.31 2.33 4 8 0 42.85 3.26 -5 -8 0 13.17 2.00 5 8 0 10.80 1.14 5 8 0 11.58 1.86 -6 -8 0 14.71 2.00 6 8 0 14.42 1.25 -7 -8 0 15.12 2.08 7 8 0 14.68 1.33 -8 -8 0 0.09 1.82 8 8 0 0.06 0.88 9 -9 0 6.00 1.46 -9 9 0 3.13 1.20 8 -9 0 0.51 1.31 -8 9 0 0.19 1.13 7 -9 0 9.05 1.48 -7 9 0 9.41 1.34 6 -9 0 -1.29 1.24 -6 9 0 -0.71 1.08 5 -9 0 1.52 1.23 -5 9 0 2.59 1.09 4 -9 0 2.83 1.39 -4 9 0 3.17 1.09 3 -9 0 40.20 2.70 -3 9 0 41.88 2.44 2 -9 0 14.69 1.75 2 -9 0 14.41 1.83 -2 9 0 16.31 1.51 1 -9 0 12.17 1.62 1 -9 0 11.00 1.70 -1 9 0 11.49 1.19 0 -9 0 9.51 1.61 0 -9 0 10.35 1.40 0 9 0 12.55 1.25 -1 -9 0 8.19 1.70 -1 -9 0 10.55 1.42 1 9 0 11.68 1.19 -2 -9 0 10.00 1.83 -2 -9 0 12.36 1.50 2 9 0 6.22 1.04 -3 -9 0 17.17 2.15 3 9 0 16.70 1.31 -4 -9 0 0.21 1.62 4 9 0 -0.04 0.83 -5 -9 0 9.81 1.94 5 9 0 7.16 0.99 -6 -9 0 2.49 1.70 6 9 0 3.43 0.94 -7 -9 0 -1.08 1.72 7 9 0 0.49 1.04 9 -10 0 1.22 1.41 -9 10 0 1.61 1.29 8 -10 0 3.12 1.37 -8 10 0 1.16 1.22 7 -10 0 0.69 1.24 -7 10 0 2.42 1.23 6 -10 0 29.08 2.26 -6 10 0 30.45 2.10 5 -10 0 15.81 1.73 -5 10 0 13.80 1.56 4 -10 0 -2.63 1.22 -4 10 0 -0.35 1.09 3 -10 0 0.84 1.27 -3 10 0 0.45 1.17 2 -10 0 0.35 1.31 -2 10 0 2.91 1.08 1 -10 0 31.92 2.67 1 -10 0 34.62 2.41 -1 10 0 37.40 2.11 0 -10 0 29.23 2.66 0 -10 0 34.98 2.40 0 10 0 35.26 2.05 -1 -10 0 1.69 1.69 -1 -10 0 1.02 1.19 1 10 0 1.79 0.90 -2 -10 0 4.65 1.70 2 10 0 2.84 0.94 -3 -10 0 4.21 1.66 3 10 0 3.33 0.90 -4 -10 0 -0.13 1.79 4 10 0 1.00 0.88 -5 -10 0 3.73 1.79 5 10 0 2.69 0.94 -6 -10 0 0.16 1.70 6 10 0 -0.52 0.91 8 -11 0 23.59 2.03 -8 11 0 22.45 2.00 7 -11 0 4.20 1.33 -7 11 0 4.48 1.32 6 -11 0 1.27 1.23 -6 11 0 1.08 1.16 5 -11 0 17.83 1.89 -5 11 0 16.94 1.73 4 -11 0 16.01 1.78 -4 11 0 15.99 1.69 3 -11 0 0.72 1.27 -3 11 0 0.66 1.22 2 -11 0 1.97 1.23 -2 11 0 1.12 1.03 1 -11 0 0.43 1.34 -1 11 0 -0.13 0.99 0 -11 0 11.92 1.54 0 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1.02 0 -13 1 6.64 1.47 -1 13 -1 1.75 1.16 1 -13 1 0.04 1.23 -2 13 -1 -0.65 1.05 2 -13 1 -0.33 1.34 -3 13 -1 2.42 1.08 3 -13 1 2.45 1.37 -4 13 -1 0.53 1.16 4 -13 1 -2.17 1.31 -5 13 -1 -0.28 1.28 5 -13 1 -2.19 1.26 4 12 -1 10.42 1.20 -4 -12 1 11.48 2.18 3 12 -1 0.54 0.93 -3 -12 1 -0.63 1.69 2 12 -1 3.52 1.04 -2 -12 1 1.98 1.87 1 12 -1 4.72 1.07 -1 -12 1 3.76 1.91 0 12 -1 1.26 0.96 0 -12 1 0.81 1.70 0 -12 1 1.57 1.40 -1 12 -1 0.31 1.03 1 -12 1 0.58 1.29 -2 12 -1 3.20 1.10 2 -12 1 2.70 1.37 -3 12 -1 15.15 1.51 3 -12 1 14.77 1.84 -4 12 -1 -0.02 1.25 4 -12 1 -0.83 1.31 -5 12 -1 1.45 1.27 5 -12 1 0.67 1.32 -6 12 -1 5.41 1.30 6 -12 1 6.26 1.35 -7 12 -1 12.45 1.57 7 -12 1 13.99 1.70 5 11 -1 2.29 1.00 -5 -11 1 1.30 1.82 4 11 -1 7.13 1.07 -4 -11 1 11.83 1.94 3 11 -1 -0.62 0.86 -3 -11 1 -1.26 1.71 2 11 -1 17.32 1.45 -2 -11 1 16.66 2.28 1 11 -1 38.00 2.20 -1 -11 1 38.47 2.51 -1 -11 1 35.21 2.88 0 11 -1 22.64 1.71 0 -11 1 21.19 2.36 0 -11 1 24.75 2.15 -1 11 -1 9.06 1.19 1 -11 1 9.99 1.63 1 -11 1 9.66 1.91 -2 11 -1 1.64 1.02 2 -11 1 4.95 1.50 -3 11 -1 16.43 1.72 3 -11 1 18.95 1.95 -4 11 -1 1.16 1.21 4 -11 1 1.05 1.39 -5 11 -1 49.41 2.92 5 -11 1 53.12 3.14 -6 11 -1 16.78 1.68 6 -11 1 15.08 1.86 -7 11 -1 -0.75 1.28 7 -11 1 -0.93 1.24 -8 11 -1 2.13 1.37 8 -11 1 2.22 1.32 6 10 -1 2.32 0.94 -6 -10 1 1.04 1.87 5 10 -1 36.62 2.17 -5 -10 1 38.52 2.91 4 10 -1 3.59 0.89 -4 -10 1 1.93 1.87 3 10 -1 39.06 2.20 -3 -10 1 38.38 2.99 2 10 -1 6.29 1.03 -2 -10 1 7.00 1.71 -1 -10 1 4.40 1.47 -1 -10 1 4.45 1.78 0 10 -1 92.27 4.49 0 -10 1 97.21 4.96 0 -10 1 83.57 5.33 -1 10 -1 39.15 2.25 1 -10 1 38.52 2.64 1 -10 1 37.47 2.85 -2 10 -1 6.75 1.15 2 -10 1 8.72 1.49 -3 10 -1 2.63 1.20 3 -10 1 2.06 1.41 -4 10 -1 49.02 2.63 4 -10 1 41.49 2.89 -5 10 -1 4.96 1.19 5 -10 1 3.98 1.43 -6 10 -1 24.59 1.95 6 -10 1 26.20 2.18 -7 10 -1 -0.07 1.22 7 -10 1 0.31 1.35 -8 10 -1 7.79 1.35 8 -10 1 6.42 1.48 -9 10 -1 29.72 2.25 9 -10 1 31.17 2.44 7 9 -1 18.49 1.48 -7 -9 1 19.64 2.22 6 9 -1 1.75 0.90 -6 -9 1 3.10 1.81 5 9 -1 1.06 0.92 -5 -9 1 1.57 1.60 4 9 -1 -0.40 0.77 -4 -9 1 1.27 1.58 3 9 -1 13.16 1.20 -3 -9 1 14.30 1.93 2 9 -1 1.09 0.86 -2 -9 1 0.86 1.52 -2 -9 1 3.19 1.21 1 9 -1 30.50 1.78 -1 -9 1 28.65 2.53 -1 -9 1 26.12 2.18 0 9 -1 1.58 0.98 0 -9 1 -0.17 1.43 0 -9 1 -1.34 1.36 -1 9 -1 28.76 1.90 1 -9 1 28.55 2.25 1 -9 1 29.92 2.38 -2 9 -1 105.54 5.29 2 -9 1 109.90 5.80 2 -9 1 111.59 6.17 -3 9 -1 61.36 3.23 3 -9 1 60.17 3.57 -4 9 -1 0.22 1.04 4 -9 1 -0.43 1.35 -5 9 -1 9.84 1.32 5 -9 1 7.24 1.51 -6 9 -1 39.71 2.38 6 -9 1 39.07 2.66 -7 9 -1 27.59 2.06 7 -9 1 25.80 2.20 -8 9 -1 3.37 1.21 8 -9 1 5.00 1.42 -9 9 -1 19.25 1.86 9 -9 1 21.29 2.08 8 8 -1 0.41 0.95 -8 -8 1 0.22 1.69 7 8 -1 -0.56 0.91 -7 -8 1 -0.12 1.66 6 8 -1 0.07 0.84 -6 -8 1 -0.30 1.72 5 8 -1 42.14 2.36 -5 -8 1 46.76 3.17 4 8 -1 2.18 0.79 -4 -8 1 1.27 1.66 3 8 -1 109.94 5.26 -3 -8 1 110.47 6.32 2 8 -1 3.15 0.80 -2 -8 1 2.41 1.50 -2 -8 1 4.49 1.14 1 8 -1 206.37 9.69 -1 -8 1 202.40 10.54 -1 -8 1 213.74 11.32 0 8 -1 21.71 1.54 0 -8 1 22.73 1.99 0 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1.58 4 -1 -14 18.06 1.53 -4 1 14 17.84 2.55 3 -1 -14 1.63 0.96 3 -1 -14 0.73 0.93 -3 1 14 -2.32 1.68 2 -1 -14 5.06 1.03 2 -1 -14 5.06 1.01 -2 1 14 1.31 1.87 1 -1 -14 3.01 1.01 1 -1 -14 4.07 1.15 -1 1 14 2.58 2.00 0 -1 -14 0.56 0.86 0 -1 -14 -1.82 1.04 0 1 14 -0.35 1.62 -1 -1 -14 -0.08 1.09 1 1 14 0.50 1.59 -2 -1 -14 0.33 1.08 2 1 14 0.69 1.72 2 1 14 -0.36 1.52 8 -2 -14 13.18 1.28 -8 2 14 9.69 1.87 7 -2 -14 0.06 0.86 -7 2 14 0.94 1.61 6 -2 -14 0.65 0.85 -6 2 14 -0.98 1.65 5 -2 -14 3.13 0.89 -5 2 14 3.50 1.63 4 -2 -14 2.49 0.96 -4 2 14 1.48 1.87 3 -2 -14 -0.34 0.83 3 -2 -14 0.15 1.00 -3 2 14 -0.72 1.73 2 -2 -14 0.40 0.91 2 -2 -14 -0.57 0.99 -2 2 14 -3.34 1.77 1 -2 -14 1.28 0.88 1 -2 -14 1.09 1.03 -1 2 14 -0.69 2.02 0 -2 -14 1.08 1.11 0 -2 -14 1.13 0.98 0 2 14 1.30 1.70 -1 -2 -14 6.13 1.12 -1 -2 -14 7.86 1.27 1 2 14 5.00 1.78 -2 -2 -14 -0.13 1.18 2 2 14 0.73 1.63 7 -3 -14 4.28 1.03 -7 3 14 3.72 1.70 6 -3 -14 0.78 0.95 -6 3 14 -1.30 1.68 5 -3 -14 3.53 0.98 -5 3 14 1.70 1.80 4 -3 -14 0.24 0.84 -4 3 14 0.92 1.99 3 -3 -14 3.61 0.91 -3 3 14 5.27 1.97 2 -3 -14 29.02 2.00 2 -3 -14 30.10 2.25 -2 3 14 31.75 3.15 1 -3 -14 5.98 1.10 1 -3 -14 3.81 1.14 -1 3 14 5.36 2.28 0 -3 -14 3.54 1.28 0 -3 -14 2.47 1.03 0 3 14 4.13 1.81 -1 -3 -14 1.04 1.25 -1 -3 -14 1.39 0.94 1 3 14 1.47 1.64 7 -4 -14 1.11 0.97 -7 4 14 -0.42 1.71 6 -4 -14 11.56 1.35 -6 4 14 10.08 2.08 5 -4 -14 11.78 1.40 -5 4 14 10.81 2.27 4 -4 -14 18.33 1.57 -4 4 14 20.48 2.72 3 -4 -14 10.78 1.28 -3 4 14 9.34 2.18 2 -4 -14 21.02 1.58 -2 4 14 20.77 3.04 1 -4 -14 13.40 1.41 1 -4 -14 12.48 1.56 -1 4 14 9.11 2.45 0 -4 -14 5.35 1.09 0 -4 -14 5.30 1.27 0 4 14 3.49 1.85 -1 -4 -14 -0.53 1.28 -1 -4 -14 -0.10 1.09 1 4 14 0.14 1.69 6 -5 -14 -0.28 1.01 -6 5 14 0.90 1.73 5 -5 -14 0.25 0.96 -5 5 14 -1.45 1.99 4 -5 -14 4.65 1.00 -4 5 14 1.83 1.66 3 -5 -14 0.92 0.93 -3 5 14 -0.35 2.01 2 -5 -14 0.04 0.87 -2 5 14 -2.23 2.30 1 -5 -14 0.84 0.91 -1 5 14 0.73 2.16 3 -6 -14 0.54 0.93 -3 6 14 -2.63 2.19 2 7 -15 33.77 2.17 -2 -7 15 34.99 2.94 4 6 -15 0.74 0.89 -4 -6 15 -0.56 1.67 3 6 -15 1.09 0.88 -3 -6 15 -0.52 1.50 2 6 -15 0.23 0.84 -2 -6 15 2.56 1.57 1 6 -15 -0.84 0.89 -1 -6 15 0.57 1.60 0 6 -15 0.60 1.06 0 -6 15 4.16 1.87 5 5 -15 0.35 0.88 -5 -5 15 0.17 1.50 4 5 -15 1.26 0.98 -4 -5 15 2.11 1.48 3 5 -15 1.45 0.89 -3 -5 15 3.19 1.61 2 5 -15 3.15 0.94 -2 -5 15 5.31 1.66 1 5 -15 3.44 1.04 -1 -5 15 4.55 1.62 0 5 -15 19.48 1.53 0 -5 15 19.09 2.14 -1 5 -15 33.21 2.19 1 -5 15 32.09 2.68 6 4 -15 1.75 0.88 -6 -4 15 2.43 1.71 5 4 -15 1.43 0.85 -5 -4 15 -0.07 1.62 4 4 -15 10.25 1.20 -4 -4 15 11.71 1.91 3 4 -15 13.22 1.28 -3 -4 15 8.51 1.57 2 4 -15 14.96 1.32 -2 -4 15 10.46 1.71 1 4 -15 5.99 1.01 -1 -4 15 4.91 1.54 0 4 -15 2.96 1.01 0 -4 15 1.05 1.61 -1 4 -15 26.22 1.91 -2 4 -15 2.36 1.13 2 -4 15 1.98 1.58 6 3 -15 11.09 1.26 -6 -3 15 13.11 2.09 5 3 -15 0.50 0.97 -5 -3 15 0.11 1.83 4 3 -15 0.69 0.84 -4 -3 15 1.15 1.76 3 3 -15 4.03 1.03 -3 -3 15 5.77 1.70 2 3 -15 -0.28 0.89 -2 -3 15 0.43 1.44 1 3 -15 1.17 0.96 -1 -3 15 0.66 1.65 0 3 -15 -0.89 0.93 0 -3 15 -0.94 1.46 -1 3 -15 2.34 1.06 1 -3 15 2.04 1.67 -2 3 -15 1.35 0.96 2 -3 15 0.70 1.58 6 2 -15 0.90 0.90 5 2 -15 2.01 0.94 5 2 -15 2.46 0.92 4 2 -15 -0.08 0.95 3 2 -15 4.20 1.05 2 2 -15 1.86 0.91 1 2 -15 -0.21 0.95 -1 -2 15 0.92 1.62 0 2 -15 7.79 1.18 0 -2 15 6.83 1.66 -1 2 -15 1.41 0.96 1 -2 15 3.33 1.56 -2 2 -15 4.37 1.07 2 -2 15 6.61 1.77 7 1 -15 5.37 1.10 6 1 -15 0.18 0.94 5 1 -15 3.65 1.00 5 1 -15 5.86 1.08 4 1 -15 24.67 1.84 4 1 -15 28.11 1.76 3 1 -15 17.16 1.49 3 1 -15 19.75 1.55 2 1 -15 2.75 0.94 2 1 -15 2.68 0.93 1 1 -15 0.01 1.01 0 1 -15 3.78 1.01 0 -1 15 2.77 1.67 0 -1 15 -0.36 1.66 -1 1 -15 7.71 1.20 1 -1 15 7.13 1.71 1 -1 15 6.84 1.83 -2 1 -15 4.04 1.15 2 -1 15 3.86 1.84 2 -1 15 2.34 1.58 7 0 -15 19.72 1.62 -7 0 15 14.38 2.26 6 0 -15 4.26 1.13 -6 0 15 1.70 1.90 5 0 -15 9.13 1.25 -5 0 15 4.22 2.04 4 0 -15 3.97 1.11 4 0 -15 3.68 1.03 -4 0 15 0.67 1.65 3 0 -15 5.24 1.00 3 0 -15 7.16 1.15 -3 0 15 4.36 2.19 2 0 -15 9.58 1.19 2 0 -15 7.43 1.05 -2 0 15 5.89 2.13 1 0 -15 1.23 0.96 1 0 -15 0.52 0.94 -1 0 15 -3.40 1.91 0 0 -15 4.05 1.08 0 0 15 1.66 1.53 -1 0 -15 1.05 1.02 1 0 15 1.23 1.50 1 0 15 1.97 1.66 7 -1 -15 1.94 1.10 -7 1 15 0.49 1.75 6 -1 -15 3.85 1.12 -6 1 15 2.46 1.87 5 -1 -15 3.64 1.03 -5 1 15 5.59 2.12 4 -1 -15 -0.55 0.97 -4 1 15 -1.69 1.59 3 -1 -15 -0.16 0.92 3 -1 -15 -0.82 0.98 -3 1 15 -2.98 2.01 2 -1 -15 2.41 1.07 2 -1 -15 1.46 1.01 -2 1 15 -0.11 1.85 1 -1 -15 0.70 0.97 1 -1 -15 0.91 0.92 -1 1 15 -0.43 2.06 0 -1 -15 1.01 0.98 0 -1 -15 1.70 1.07 0 1 15 1.39 1.70 -1 -1 -15 0.88 1.00 1 1 15 1.58 1.43 6 -2 -15 1.41 0.91 -6 2 15 1.84 1.75 5 -2 -15 7.11 1.06 -5 2 15 11.25 2.23 4 -2 -15 9.27 1.14 -4 2 15 8.59 1.88 3 -2 -15 1.09 1.08 -3 2 15 -0.01 2.05 2 -2 -15 -0.24 0.97 2 -2 -15 -0.35 0.87 -2 2 15 -1.48 1.92 1 -2 -15 0.57 1.09 1 -2 -15 0.12 1.22 -1 2 15 1.31 2.08 0 -2 -15 4.32 0.98 0 -2 -15 4.76 1.26 0 2 15 2.65 1.74 6 -3 -15 3.24 0.92 -6 3 15 2.64 1.67 5 -3 -15 2.89 0.90 -5 3 15 2.99 1.91 4 -3 -15 6.64 1.09 -4 3 15 4.11 1.95 3 -3 -15 1.55 0.88 -3 3 15 -1.47 2.09 2 -3 -15 1.56 1.03 -2 3 15 0.49 2.06 1 -3 -15 10.34 1.24 1 -3 -15 10.60 1.43 -1 3 15 8.61 2.31 4 -4 -15 0.89 0.83 -4 4 15 0.20 1.88 3 -4 -15 0.75 0.91 -3 4 15 -0.89 2.06 2 -4 -15 0.24 0.88 -2 4 15 -1.34 2.32 3 4 -16 3.50 0.93 -3 -4 16 3.80 1.54 2 4 -16 -0.21 0.96 -2 -4 16 -0.17 1.48 1 4 -16 1.71 0.99 -1 -4 16 2.07 1.64 4 3 -16 3.89 0.98 -4 -3 16 5.59 1.79 3 3 -16 12.49 1.33 -3 -3 16 12.34 1.71 2 3 -16 18.37 1.52 -2 -3 16 20.69 2.29 1 3 -16 10.31 1.21 -1 -3 16 8.29 1.67 5 2 -16 17.12 1.49 4 2 -16 -0.43 0.95 3 2 -16 -0.21 0.97 2 2 -16 2.78 0.97 -2 -2 16 3.92 1.72 1 2 -16 6.65 1.09 -1 -2 16 5.81 1.64 5 1 -16 1.43 1.02 4 1 -16 -0.30 0.92 4 1 -16 -1.00 1.04 3 1 -16 1.61 0.95 3 1 -16 1.63 0.99 2 1 -16 1.52 1.03 1 1 -16 2.54 1.04 -1 -1 16 3.46 2.00 5 0 -16 0.65 0.89 4 0 -16 3.79 1.01 -4 0 16 0.93 2.11 3 0 -16 11.10 1.25 3 0 -16 10.59 1.29 -3 0 16 10.09 2.50 2 0 -16 0.67 1.03 2 0 -16 0.52 0.95 -2 0 16 -4.31 2.21 1 0 -16 2.53 1.07 -1 0 16 0.59 1.83 4 -1 -16 0.13 1.10 -4 1 16 -2.65 1.97 3 -1 -16 4.05 1.09 3 -1 -16 3.53 1.05 -3 1 16 0.90 2.19 2 -1 -16 1.67 1.20 2 -1 -16 0.92 0.97 -2 1 16 -3.89 2.11 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 54411 _database_code_depnum_ccdc_archive 'CCDC 968835' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c1_200K _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H16 Cl2 F10 Fe N14 O2 S2, 2(C H4 O)' _chemical_formula_sum 'C42 H24 Cl2 F10 Fe N14 O4 S2' _chemical_formula_weight 1169.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0020 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' H H 0.0000 0.0000 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' N N -0.0031 0.0040 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' O O -0.0041 0.0074 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' F F -0.0053 0.0125 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' S S 0.1206 0.1480 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' Cl Cl 0.1408 0.1896 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' Fe Fe 0.2064 0.9930 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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, -z' _cell_length_a 9.173(2) _cell_length_b 11.167(3) _cell_length_c 12.759(3) _cell_angle_alpha 94.784(4) _cell_angle_beta 105.483(3) _cell_angle_gamma 100.902(3) _cell_volume 1224.4(5) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 5307 _cell_measurement_theta_min 3.18 _cell_measurement_theta_max 28.58 _exptl_crystal_description parallelepiped _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.586 _exptl_crystal_F_000 588 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.110 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 0.752 _shelx_estimated_absorpt_T_min 0.922 _shelx_estimated_absorpt_T_max 0.985 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.640 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'SADABS Bruker AXS Madison WI US' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.7749 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Advanced Light Source station 11.3.1' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13341 _diffrn_reflns_av_unetI/netI 0.0439 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.189 _diffrn_reflns_theta_max 29.051 _diffrn_reflns_theta_full 28.950 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_point_group_measured_fraction_full 0.992 _reflns_number_total 4973 _reflns_number_gt 3664 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; All non-hydrogens were refined anisotropically. The lattice methanol molecule is disordered over two positions with relative occupancies of 0.46:0.54 and was refined with displacement parameters restraints. Hydrogens were placed on their carrier atom and refined with a riding model. The hydroxyl hydrogens of the two components of the disordered lattice methanol could not be found and their refinement at calculated positions did not converge satisfactorily. These were thus eventually omitted from the structural model although they are taken into account in the formula. ; _vrf_PLAT309_c1_200K ; PROBLEM: Single Bonded Oxygen (C-O > 1.3 Ang) ........... O1S RESPONSE: The hydroxyl hydrogens of the two components of the disordered lattice methanol could not be found and their refinement at calculated positions did not converge satisfactorily. These were thus eventually omitted from the structural model resulting in apparently single bonded oxygens. ; _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^)+(0.0797P)^2^+1.0973P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4973 _refine_ls_number_parameters 361 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1619 _refine_ls_wR_factor_gt 0.1519 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.046 _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_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 0.5000 0.5000 0.5000 0.0372(2) Uani 1 2 d S . P . . Cl1 Cl 0.42981(12) 0.17797(9) 0.92988(9) 0.0619(3) Uani 1 1 d . . . . . S1 S 0.30283(14) 0.78386(10) 0.26568(10) 0.0658(3) Uani 1 1 d . . . . . O1 O 0.8299(3) 0.5504(2) 1.0236(2) 0.0506(6) Uani 1 1 d . . . . . N1 N 0.3903(3) 0.5967(3) 0.3823(2) 0.0474(7) Uani 1 1 d . . . . . N2 N 0.5315(3) 0.6625(3) 0.6233(2) 0.0462(7) Uani 1 1 d . . . . . N3 N 0.2780(3) 0.4403(3) 0.5415(2) 0.0426(6) Uani 1 1 d . . . . . N4 N 0.4096(3) 0.5295(3) 0.7236(2) 0.0401(6) Uani 1 1 d . . . . . N5 N 0.4224(3) 0.3652(3) 0.8235(2) 0.0433(6) Uani 1 1 d . . . . . N6 N 0.6226(3) 0.5477(3) 0.8740(2) 0.0422(6) Uani 1 1 d . . . . . N7 N 0.6378(3) 0.3817(3) 0.9826(2) 0.0465(7) Uani 1 1 d . . . . . C1 C 0.3540(4) 0.6750(3) 0.3337(3) 0.0426(8) Uani 1 1 d . . . . . C2 C 0.5852(5) 0.7766(3) 0.6047(4) 0.0607(10) Uani 1 1 d . . . . . H2A H 0.6256 0.7860 0.5439 0.073 Uiso 1 1 calc R U . . . C3 C 0.5842(6) 0.8808(4) 0.6701(4) 0.0774(13) Uani 1 1 d . . . . . H3A H 0.6256 0.9602 0.6556 0.093 Uiso 1 1 calc R U . . . C4 C 0.5232(6) 0.8686(4) 0.7554(4) 0.0734(13) Uani 1 1 d . . . . . H4A H 0.5207 0.9395 0.8009 0.088 Uiso 1 1 calc R U . . . C5 C 0.4643(5) 0.7519(4) 0.7760(3) 0.0576(10) Uani 1 1 d . . . . . H5A H 0.4205 0.7408 0.8350 0.069 Uiso 1 1 calc R U . . . C6 C 0.4719(4) 0.6525(3) 0.7073(3) 0.0427(7) Uani 1 1 d . . . . . C7 C 0.1500(4) 0.3809(4) 0.4642(3) 0.0525(9) Uani 1 1 d . . . . . H7A H 0.1532 0.3682 0.3904 0.063 Uiso 1 1 calc R U . . . C8 C 0.0116(4) 0.3365(4) 0.4876(4) 0.0606(10) Uani 1 1 d . . . . . H8A H -0.0780 0.2934 0.4310 0.073 Uiso 1 1 calc R U . . . C9 C 0.0075(4) 0.3563(4) 0.5944(4) 0.0611(10) Uani 1 1 d . . . . . H9A H -0.0849 0.3252 0.6128 0.073 Uiso 1 1 calc R U . . . C10 C 0.1360(4) 0.4206(4) 0.6739(3) 0.0521(9) Uani 1 1 d . . . . . H10A H 0.1336 0.4383 0.7475 0.063 Uiso 1 1 calc R U . . . C11 C 0.2711(4) 0.4598(3) 0.6445(3) 0.0407(7) Uani 1 1 d . . . . . C12 C 0.4862(4) 0.4787(3) 0.8100(3) 0.0403(7) Uani 1 1 d . . . . . C13 C 0.5045(4) 0.3251(3) 0.9094(3) 0.0441(8) Uani 1 1 d . . . . . C14 C 0.6887(4) 0.4920(3) 0.9547(3) 0.0428(7) Uani 1 1 d . . . . . C15 C 0.9127(4) 0.6508(3) 0.9932(3) 0.0478(8) Uani 1 1 d . . . . . C16 C 0.9627(4) 0.7602(4) 1.0629(3) 0.0552(9) Uani 1 1 d . . . . . C17 C 1.0612(5) 0.8576(4) 1.0408(4) 0.0690(13) Uani 1 1 d . . . . . C18 C 1.1095(5) 0.8453(5) 0.9481(5) 0.0762(14) Uani 1 1 d . . . . . C19 C 1.0598(5) 0.7391(5) 0.8781(4) 0.0699(12) Uani 1 1 d . . . . . C20 C 0.9621(4) 0.6403(4) 0.8994(3) 0.0536(9) Uani 1 1 d . . . . . F1 F 0.9167(3) 0.7702(2) 1.1546(2) 0.0711(7) Uani 1 1 d . . . . . F2 F 1.1094(4) 0.9632(2) 1.1122(3) 0.0973(10) Uani 1 1 d . . . . . F3 F 1.2080(4) 0.9414(3) 0.9295(3) 0.1205(14) Uani 1 1 d . . . . . F4 F 1.1083(3) 0.7276(4) 0.7878(3) 0.1049(11) Uani 1 1 d . . . . . F5 F 0.9178(3) 0.5355(2) 0.8317(2) 0.0676(6) Uani 1 1 d . . . . . O1S O 0.820(2) 0.9621(18) 0.3549(16) 0.183(6) Uani 0.430(11) 1 d D U P A 1 C1S C 0.973(3) 1.0037(19) 0.3414(17) 0.157(7) Uani 0.430(11) 1 d D U P A 1 H1S1 H 0.9795 1.0834 0.3141 0.235 Uiso 0.430(11) 1 calc R U P A 1 H1S2 H 0.9911 0.9433 0.2887 0.235 Uiso 0.430(11) 1 calc R U P A 1 H1S3 H 1.0518 1.0124 0.4124 0.235 Uiso 0.430(11) 1 calc R U P A 1 O2S O 0.740(2) 0.8906(17) 0.3868(12) 0.224(6) Uani 0.570(11) 1 d D U P A 2 C2S C 0.772(2) 1.0018(14) 0.4635(15) 0.171(6) Uani 0.570(11) 1 d D U P A 2 H2S1 H 0.8465 0.9944 0.5326 0.257 Uiso 0.570(11) 1 calc R U P A 2 H2S2 H 0.6758 1.0140 0.4775 0.257 Uiso 0.570(11) 1 calc R U P A 2 H2S3 H 0.8163 1.0724 0.4323 0.257 Uiso 0.570(11) 1 calc R U P 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 0.0349(3) 0.0408(4) 0.0441(4) 0.0137(3) 0.0193(3) 0.0133(3) Cl1 0.0611(6) 0.0498(5) 0.0711(6) 0.0198(5) 0.0172(5) 0.0016(4) S1 0.0715(7) 0.0590(6) 0.0817(8) 0.0300(6) 0.0288(6) 0.0321(5) O1 0.0421(13) 0.0506(14) 0.0527(15) 0.0173(12) 0.0053(11) 0.0028(11) N1 0.0454(16) 0.0545(17) 0.0525(17) 0.0167(14) 0.0219(14) 0.0204(14) N2 0.0495(16) 0.0427(16) 0.0517(17) 0.0115(13) 0.0204(14) 0.0122(13) N3 0.0333(14) 0.0503(16) 0.0477(16) 0.0115(13) 0.0154(12) 0.0102(12) N4 0.0326(13) 0.0473(16) 0.0440(15) 0.0102(12) 0.0140(12) 0.0112(11) N5 0.0379(14) 0.0468(16) 0.0483(16) 0.0098(13) 0.0169(13) 0.0092(12) N6 0.0351(14) 0.0451(15) 0.0482(16) 0.0117(13) 0.0131(12) 0.0099(12) N7 0.0431(16) 0.0451(16) 0.0526(17) 0.0085(13) 0.0165(14) 0.0080(13) C1 0.0368(17) 0.0467(19) 0.051(2) 0.0085(16) 0.0203(15) 0.0133(14) C2 0.075(3) 0.042(2) 0.067(3) 0.0132(18) 0.028(2) 0.0050(18) C3 0.101(4) 0.042(2) 0.088(3) 0.010(2) 0.031(3) 0.006(2) C4 0.094(3) 0.048(2) 0.076(3) -0.002(2) 0.023(3) 0.018(2) C5 0.063(2) 0.059(2) 0.057(2) 0.0040(18) 0.0225(19) 0.0225(19) C6 0.0395(17) 0.0448(18) 0.0469(19) 0.0111(15) 0.0118(15) 0.0154(14) C7 0.047(2) 0.062(2) 0.050(2) 0.0102(17) 0.0167(17) 0.0089(17) C8 0.0386(19) 0.070(3) 0.067(3) 0.012(2) 0.0120(18) 0.0030(17) C9 0.0368(19) 0.080(3) 0.072(3) 0.019(2) 0.0252(19) 0.0092(18) C10 0.0386(18) 0.066(2) 0.059(2) 0.0146(18) 0.0237(17) 0.0141(17) C11 0.0365(16) 0.0447(18) 0.0479(19) 0.0122(14) 0.0197(14) 0.0126(14) C12 0.0347(16) 0.0471(18) 0.0455(18) 0.0074(14) 0.0192(14) 0.0128(14) C13 0.0405(17) 0.0462(19) 0.050(2) 0.0113(15) 0.0188(16) 0.0109(15) C14 0.0386(17) 0.0458(18) 0.0454(18) 0.0095(15) 0.0136(15) 0.0090(14) C15 0.0357(17) 0.049(2) 0.055(2) 0.0141(17) 0.0061(15) 0.0076(15) C16 0.045(2) 0.062(2) 0.057(2) 0.0157(19) 0.0089(17) 0.0144(17) C17 0.056(2) 0.045(2) 0.087(3) 0.011(2) -0.008(2) 0.0029(18) C18 0.053(2) 0.080(3) 0.088(4) 0.044(3) 0.011(2) -0.003(2) C19 0.044(2) 0.092(3) 0.071(3) 0.026(3) 0.014(2) 0.005(2) C20 0.0350(17) 0.065(2) 0.061(2) 0.019(2) 0.0105(16) 0.0106(16) F1 0.0600(14) 0.0741(16) 0.0733(16) 0.0010(13) 0.0142(12) 0.0117(12) F2 0.092(2) 0.0535(16) 0.118(2) 0.0109(16) -0.0061(18) -0.0003(14) F3 0.086(2) 0.109(2) 0.142(3) 0.064(2) 0.016(2) -0.0322(19) F4 0.0659(17) 0.167(3) 0.080(2) 0.032(2) 0.0348(15) -0.0041(19) F5 0.0519(13) 0.0816(17) 0.0674(15) 0.0003(13) 0.0163(11) 0.0157(12) O1S 0.191(11) 0.171(12) 0.165(11) 0.017(9) 0.049(9) -0.006(10) C1S 0.195(12) 0.142(12) 0.126(11) -0.036(9) 0.063(10) 0.021(10) O2S 0.234(13) 0.246(13) 0.141(10) 0.007(8) 0.028(9) -0.021(11) C2S 0.181(11) 0.151(9) 0.173(10) 0.064(7) 0.060(9) -0.015(8) _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 N1 2.076(3) . ? Fe1 N1 2.076(3) 2_666 ? Fe1 N2 2.221(3) . ? Fe1 N2 2.221(3) 2_666 ? Fe1 N3 2.235(3) . ? Fe1 N3 2.235(3) 2_666 ? Cl1 C13 1.726(4) . ? S1 C1 1.620(4) . ? O1 C14 1.361(4) . ? O1 C15 1.377(4) . ? N1 C1 1.163(4) . ? N2 C6 1.330(4) . ? N2 C2 1.342(5) . ? N3 C7 1.330(5) . ? N3 C11 1.334(4) . ? N4 C12 1.368(4) . ? N4 C11 1.431(4) . ? N4 C6 1.439(4) . ? N5 C13 1.318(4) . ? N5 C12 1.338(4) . ? N6 C14 1.315(4) . ? N6 C12 1.346(4) . ? N7 C13 1.330(5) . ? N7 C14 1.344(4) . ? C2 C3 1.377(6) . ? C2 H2A 0.9500 . ? C3 C4 1.356(7) . ? C3 H3A 0.9500 . ? C4 C5 1.387(6) . ? C4 H4A 0.9500 . ? C5 C6 1.379(5) . ? C5 H5A 0.9500 . ? C7 C8 1.391(5) . ? C7 H7A 0.9500 . ? C8 C9 1.375(6) . ? C8 H8A 0.9500 . ? C9 C10 1.361(6) . ? C9 H9A 0.9500 . ? C10 C11 1.392(5) . ? C10 H10A 0.9500 . ? C15 C16 1.373(6) . ? C15 C20 1.391(5) . ? C16 F1 1.348(5) . ? C16 C17 1.375(6) . ? C17 F2 1.351(5) . ? C17 C18 1.375(7) . ? C18 C19 1.347(7) . ? C18 F3 1.348(5) . ? C19 F4 1.346(6) . ? C19 C20 1.379(6) . ? C20 F5 1.321(5) . ? O1S C1S 1.451(17) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? O2S C2S 1.447(15) . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 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 N1 Fe1 N1 180.00(13) . 2_666 ? N1 Fe1 N2 87.31(12) . . ? N1 Fe1 N2 92.69(12) 2_666 . ? N1 Fe1 N2 92.69(12) . 2_666 ? N1 Fe1 N2 87.31(12) 2_666 2_666 ? N2 Fe1 N2 180.00(16) . 2_666 ? N1 Fe1 N3 89.77(11) . . ? N1 Fe1 N3 90.23(11) 2_666 . ? N2 Fe1 N3 83.13(11) . . ? N2 Fe1 N3 96.86(11) 2_666 . ? N1 Fe1 N3 90.23(11) . 2_666 ? N1 Fe1 N3 89.77(11) 2_666 2_666 ? N2 Fe1 N3 96.87(11) . 2_666 ? N2 Fe1 N3 83.14(11) 2_666 2_666 ? N3 Fe1 N3 180.0 . 2_666 ? C14 O1 C15 118.7(3) . . ? C1 N1 Fe1 163.3(3) . . ? C6 N2 C2 117.1(3) . . ? C6 N2 Fe1 121.0(2) . . ? C2 N2 Fe1 120.7(3) . . ? C7 N3 C11 118.3(3) . . ? C7 N3 Fe1 120.6(2) . . ? C11 N3 Fe1 121.1(2) . . ? C12 N4 C11 121.1(3) . . ? C12 N4 C6 120.3(3) . . ? C11 N4 C6 118.6(3) . . ? C13 N5 C12 113.6(3) . . ? C14 N6 C12 112.6(3) . . ? C13 N7 C14 109.6(3) . . ? N1 C1 S1 179.8(5) . . ? N2 C2 C3 122.7(4) . . ? N2 C2 H2A 118.6 . . ? C3 C2 H2A 118.6 . . ? C4 C3 C2 119.1(4) . . ? C4 C3 H3A 120.5 . . ? C2 C3 H3A 120.5 . . ? C3 C4 C5 119.7(4) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? C6 C5 C4 117.4(4) . . ? C6 C5 H5A 121.3 . . ? C4 C5 H5A 121.3 . . ? N2 C6 C5 123.9(3) . . ? N2 C6 N4 116.4(3) . . ? C5 C6 N4 119.7(3) . . ? N3 C7 C8 122.4(4) . . ? N3 C7 H7A 118.8 . . ? C8 C7 H7A 118.8 . . ? C9 C8 C7 118.4(4) . . ? C9 C8 H8A 120.8 . . ? C7 C8 H8A 120.8 . . ? C10 C9 C8 119.9(4) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C9 C10 C11 118.3(4) . . ? C9 C10 H10A 120.9 . . ? C11 C10 H10A 120.9 . . ? N3 C11 C10 122.7(3) . . ? N3 C11 N4 116.1(3) . . ? C10 C11 N4 121.1(3) . . ? N5 C12 N6 125.2(3) . . ? N5 C12 N4 118.3(3) . . ? N6 C12 N4 116.5(3) . . ? N5 C13 N7 129.2(3) . . ? N5 C13 Cl1 115.8(3) . . ? N7 C13 Cl1 115.0(3) . . ? N6 C14 N7 129.7(3) . . ? N6 C14 O1 118.5(3) . . ? N7 C14 O1 111.7(3) . . ? C16 C15 O1 119.3(3) . . ? C16 C15 C20 119.0(4) . . ? O1 C15 C20 121.3(3) . . ? F1 C16 C15 119.1(4) . . ? F1 C16 C17 120.4(4) . . ? C15 C16 C17 120.4(4) . . ? F2 C17 C18 121.6(4) . . ? F2 C17 C16 118.7(5) . . ? C18 C17 C16 119.8(4) . . ? C19 C18 F3 121.0(5) . . ? C19 C18 C17 120.5(4) . . ? F3 C18 C17 118.5(5) . . ? F4 C19 C18 120.1(4) . . ? F4 C19 C20 119.4(5) . . ? C18 C19 C20 120.5(5) . . ? F5 C20 C19 119.9(4) . . ? F5 C20 C15 120.4(3) . . ? C19 C20 C15 119.8(4) . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? O2S C2S H2S1 109.5 . . ? O2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? O2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? _refine_diff_density_max 0.411 _refine_diff_density_min -0.386 _refine_diff_density_rms 0.064 _shelxl_version_number 2013-3 _shelx_res_file ; TITL c1_200K in P-1 CELL 0.77490 9.173 11.167 12.759 94.784 105.483 100.902 ZERR 1.00 0.002 0.003 0.003 0.004 0.003 0.003 LATT 1 SFAC C H N O F S CL FE DISP Fe 0.20639 0.99298 4412.23 DISP Cl 0.14076 0.18956 859.19 DISP S 0.12060 0.14800 674.22 DISP F -0.00532 0.01246 64.36 DISP O -0.00415 0.00737 40.17 DISP N -0.00306 0.00403 23.92 DISP C -0.00202 0.00197 13.60 DISP H 0.00000 0.00000 0.67 UNIT 42 24 14 4 10 2 2 1 TEMP -73 SIZE 0.11 0.05 0.02 REM yellow parallelepiped same cristal as measured at 100K REM integrated to 0.80 angstrom L.S. 12 BOND $H ACTA 57.9 FMAP 2 PLAN 10 DFIX 1.45 O1S C1S O2S C2S ISOR 0.008 C1S C2S SIMU 0.012 O1S > C2S DELU 0.003 O1S > C2S WGHT 0.079700 1.097300 FVAR 0.37308 0.43041 FE1 8 0.500000 0.500000 0.500000 10.50000 0.03489 0.04084 = 0.04411 0.01374 0.01931 0.01331 CL1 7 0.429806 0.177967 0.929877 11.00000 0.06115 0.04983 = 0.07112 0.01977 0.01723 0.00161 S1 6 0.302833 0.783857 0.265677 11.00000 0.07150 0.05903 = 0.08174 0.03002 0.02876 0.03214 O1 4 0.829883 0.550359 1.023630 11.00000 0.04211 0.05058 = 0.05271 0.01727 0.00528 0.00275 N1 3 0.390336 0.596740 0.382336 11.00000 0.04543 0.05448 = 0.05250 0.01674 0.02188 0.02043 N2 3 0.531503 0.662454 0.623334 11.00000 0.04951 0.04273 = 0.05166 0.01153 0.02039 0.01221 N3 3 0.277954 0.440340 0.541496 11.00000 0.03330 0.05033 = 0.04772 0.01153 0.01540 0.01024 N4 3 0.409558 0.529490 0.723599 11.00000 0.03256 0.04730 = 0.04396 0.01017 0.01402 0.01125 N5 3 0.422406 0.365160 0.823462 11.00000 0.03786 0.04681 = 0.04831 0.00982 0.01687 0.00920 N6 3 0.622636 0.547660 0.874022 11.00000 0.03515 0.04512 = 0.04824 0.01166 0.01311 0.00988 N7 3 0.637798 0.381737 0.982648 11.00000 0.04309 0.04509 = 0.05256 0.00850 0.01654 0.00795 C1 1 0.353979 0.675047 0.333664 11.00000 0.03682 0.04674 = 0.05075 0.00847 0.02029 0.01328 C2 1 0.585199 0.776632 0.604728 11.00000 0.07514 0.04195 = 0.06703 0.01318 0.02774 0.00504 AFIX 43 H2A 2 0.625627 0.785971 0.543935 11.00000 -1.20000 AFIX 0 C3 1 0.584160 0.880833 0.670060 11.00000 0.10134 0.04158 = 0.08752 0.01035 0.03051 0.00602 AFIX 43 H3A 2 0.625604 0.960238 0.655550 11.00000 -1.20000 AFIX 0 C4 1 0.523168 0.868551 0.755396 11.00000 0.09398 0.04788 = 0.07616 -0.00197 0.02289 0.01764 AFIX 43 H4A 2 0.520736 0.939527 0.800891 11.00000 -1.20000 AFIX 0 C5 1 0.464328 0.751873 0.775972 11.00000 0.06309 0.05918 = 0.05652 0.00397 0.02246 0.02254 AFIX 43 H5A 2 0.420523 0.740835 0.835014 11.00000 -1.20000 AFIX 0 C6 1 0.471930 0.652547 0.707349 11.00000 0.03948 0.04482 = 0.04687 0.01111 0.01180 0.01540 C7 1 0.149978 0.380859 0.464236 11.00000 0.04673 0.06172 = 0.04985 0.01018 0.01669 0.00890 AFIX 43 H7A 2 0.153216 0.368240 0.390405 11.00000 -1.20000 AFIX 0 C8 1 0.011596 0.336459 0.487572 11.00000 0.03864 0.07031 = 0.06747 0.01208 0.01201 0.00296 AFIX 43 H8A 2 -0.077951 0.293433 0.431032 11.00000 -1.20000 AFIX 0 C9 1 0.007543 0.356345 0.594432 11.00000 0.03683 0.08027 = 0.07187 0.01899 0.02522 0.00920 AFIX 43 H9A 2 -0.084855 0.325244 0.612824 11.00000 -1.20000 AFIX 0 C10 1 0.136042 0.420643 0.673887 11.00000 0.03856 0.06644 = 0.05912 0.01460 0.02369 0.01407 AFIX 43 H10A 2 0.133579 0.438302 0.747450 11.00000 -1.20000 AFIX 0 C11 1 0.271144 0.459844 0.644533 11.00000 0.03650 0.04467 = 0.04793 0.01221 0.01969 0.01265 C12 1 0.486165 0.478739 0.810036 11.00000 0.03467 0.04707 = 0.04546 0.00737 0.01924 0.01278 C13 1 0.504520 0.325077 0.909365 11.00000 0.04052 0.04625 = 0.05022 0.01128 0.01883 0.01092 C14 1 0.688697 0.492044 0.954748 11.00000 0.03857 0.04575 = 0.04536 0.00948 0.01364 0.00896 C15 1 0.912672 0.650847 0.993155 11.00000 0.03568 0.04945 = 0.05453 0.01406 0.00605 0.00758 C16 1 0.962747 0.760235 1.062933 11.00000 0.04547 0.06219 = 0.05677 0.01574 0.00894 0.01440 C17 1 1.061195 0.857551 1.040836 11.00000 0.05582 0.04453 = 0.08681 0.01072 -0.00754 0.00291 C18 1 1.109470 0.845273 0.948110 11.00000 0.05323 0.08024 = 0.08803 0.04364 0.01083 -0.00275 C19 1 1.059847 0.739067 0.878131 11.00000 0.04384 0.09233 = 0.07054 0.02649 0.01405 0.00508 C20 1 0.962096 0.640262 0.899413 11.00000 0.03498 0.06488 = 0.06073 0.01895 0.01053 0.01062 F1 5 0.916721 0.770215 1.154555 11.00000 0.06000 0.07414 = 0.07326 0.00100 0.01417 0.01169 F2 5 1.109433 0.963216 1.112243 11.00000 0.09206 0.05348 = 0.11779 0.01087 -0.00610 -0.00026 F3 5 1.208007 0.941448 0.929498 11.00000 0.08621 0.10906 = 0.14223 0.06382 0.01629 -0.03218 F4 5 1.108260 0.727565 0.787847 11.00000 0.06592 0.16695 = 0.08024 0.03238 0.03478 -0.00409 F5 5 0.917835 0.535523 0.831697 11.00000 0.05191 0.08155 = 0.06739 0.00028 0.01629 0.01565 PART 1 O1S 4 0.820235 0.962080 0.354914 21.00000 0.19091 0.17090 = 0.16488 0.01693 0.04869 -0.00613 C1S 1 0.973079 1.003655 0.341447 21.00000 0.19521 0.14175 = 0.12557 -0.03605 0.06266 0.02061 AFIX 137 H1S1 2 0.979507 1.083371 0.314119 21.00000 -1.50000 H1S2 2 0.991090 0.943258 0.288731 21.00000 -1.50000 H1S3 2 1.051843 1.012408 0.412399 21.00000 -1.50000 AFIX 0 PART 2 O2S 4 0.740473 0.890584 0.386817 -21.00000 0.23423 0.24588 = 0.14101 0.00684 0.02816 -0.02082 C2S 1 0.772358 1.001821 0.463481 -21.00000 0.18111 0.15118 = 0.17295 0.06385 0.05968 -0.01501 AFIX 137 H2S1 2 0.846540 0.994429 0.532590 -21.00000 -1.50000 H2S2 2 0.675823 1.013961 0.477496 -21.00000 -1.50000 H2S3 2 0.816312 1.072432 0.432294 -21.00000 -1.50000 PART 0 AFIX 0 HKLF 4 REM c1_200K in P-1 REM R1 = 0.0547 for 3664 Fo > 4sig(Fo) and 0.0741 for all 4973 data REM 361 parameters refined using 40 restraints END WGHT 0.0797 1.0934 REM Highest difference peak 0.411, deepest hole -0.386, 1-sigma level 0.064 Q1 1 0.7486 1.0327 0.4791 11.00000 0.05 0.41 Q2 1 1.1974 1.0014 1.0068 11.00000 0.05 0.41 Q3 1 0.2020 0.7113 0.2279 11.00000 0.05 0.40 Q4 1 0.8520 0.9056 0.4628 11.00000 0.05 0.36 Q5 1 0.7371 0.8256 0.3763 11.00000 0.05 0.33 Q6 1 0.8799 0.9883 0.5149 11.00000 0.05 0.33 Q7 1 0.8637 1.0172 0.3069 11.00000 0.05 0.31 Q8 1 1.0748 0.9910 1.1812 11.00000 0.05 0.31 Q9 1 0.9161 0.9894 0.4372 11.00000 0.05 0.30 Q10 1 0.4815 0.4964 0.4324 11.00000 0.05 0.30 ; _shelx_res_checksum 9778 _shelx_hkl_file ; -3 0 0 103.32 4.09 3 0 0 106.78 4.57 3 0 0 104.02 3.71 -4 0 0 9.45 0.94 4 0 0 9.41 0.73 4 0 0 9.48 1.17 -5 0 0 129.67 5.70 5 0 0 152.15 5.18 5 0 0 155.91 6.36 -6 0 0 3.57 0.98 6 0 0 3.59 0.68 6 0 0 1.77 1.06 -7 0 0 0.41 0.86 7 0 0 0.89 0.99 -8 0 0 0.90 0.86 -8 0 0 1.90 0.93 8 0 0 1.88 1.09 -9 0 0 9.62 1.18 -9 0 0 12.96 1.32 9 0 0 14.27 1.66 -10 0 0 5.07 1.04 10 -1 0 0.77 1.08 -10 1 0 0.13 0.91 9 -1 0 31.44 2.01 -9 1 0 28.80 1.68 8 -1 0 2.68 1.16 -8 1 0 3.70 0.91 -8 1 0 1.41 0.98 7 -1 0 10.50 1.32 -7 1 0 10.64 1.15 -7 1 0 9.97 1.02 6 -1 0 45.76 2.42 -6 1 0 47.34 2.13 -6 1 0 46.93 1.99 5 -1 0 234.75 10.03 5 -1 0 236.09 9.12 -5 1 0 250.29 8.31 -5 1 0 224.69 9.03 4 -1 0 218.26 9.33 4 -1 0 211.50 8.52 -4 1 0 227.83 7.72 -4 1 0 225.29 8.42 3 -1 0 153.07 5.88 3 -1 0 144.73 6.43 -3 1 0 154.42 5.79 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