data_Compound _publ_requested_journal '' _publ_contact_author_name 'Sascha Ott' _publ_contact_author_address ;Department of Chemistry, \%Angstr\"om Laboratories, Uppsala University. Box 523, 75120 Uppsala, Sweden. ; _publ_contact_author_email sascha.ott@kemi.uu.se _publ_contact_author_phone '+46 (0)18 - 471 7340' _publ_contact_author_fax '+46 (0)18 - 471 6844' loop_ _publ_author_name _publ_author_address 'Pullen, Sonja' ;Department of Chemistry, \%Angstr\"om Laboratories, Uppsala University. Box 523, 75120 Uppsala, Sweden. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _vrf_DIFMX01_Compound ; PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00 RESPONSE: Due to the badly define pentane molecule some of the electron density could not be modeled correctly. The largest hole however is close to the iron centers. ; _vrf_PLAT097_Compound ; PROBLEM: Large Reported Max. (Positive) Residual Density 3.37 eA-3 RESPONSE: Due to the badly define pentane molecule some of the electron density could not be modeled correctly. ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H4 Fe2 O10 S2, C5 H12' _chemical_formula_sum 'C19 H16 Fe2 O10 S2' _chemical_formula_weight 580.14 _chemical_compound_source synthetic 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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.641(7) _cell_length_b 9.564(5) _cell_length_c 20.250(10) _cell_angle_alpha 90.00 _cell_angle_beta 107.43(2) _cell_angle_gamma 90.00 _cell_volume 2336(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4431 _cell_measurement_theta_min 1.69 _cell_measurement_theta_max 28.51 _exptl_crystal_description 'block' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 1.472 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.5857 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; X-ray crystallographic data for I were collected from a single crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker smart diffractometer equiped with an APEX II CCD Detector, a graphite monochromator. The crystal-to-detector distance was 5.0 cm, and the data collection was carried out in 512 x 512 pixel mode. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart ApexII' _diffrn_measurement_method '\w -scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 34815 _diffrn_reflns_av_R_equivalents 0.0914 _diffrn_reflns_av_sigmaI/netI 0.0752 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.51 _reflns_number_total 5831 _reflns_number_gt 4431 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 1)' _computing_cell_refinement 'SAINT V7.68A(Bruker AXS, )' _computing_data_reduction 'SAINT V7.68A(Bruker AXS, )' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-III for Windows (Farrugia, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+96.0107P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5831 _refine_ls_number_parameters 276 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.1738 _refine_ls_R_factor_gt 0.1485 _refine_ls_wR_factor_ref 0.3398 _refine_ls_wR_factor_gt 0.3283 _refine_ls_goodness_of_fit_ref 1.243 _refine_ls_restrained_S_all 1.239 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9995(10) 0.7424(12) 0.5009(6) 0.022(2) Uani 1 1 d . . . C2 C 1.1683(10) 0.8698(12) 0.4643(7) 0.0188(17) Uani 1 1 d . . . C3 C 1.1644(10) 0.5987(12) 0.4695(6) 0.020(2) Uani 1 1 d . . . C4 C 1.1399(11) 0.5793(15) 0.3047(6) 0.025(3) Uani 1 1 d . . . C5 C 1.1407(10) 0.8470(12) 0.2981(7) 0.0188(17) Uani 1 1 d . . . C6 C 0.9544(10) 0.7099(15) 0.2204(6) 0.025(3) Uani 1 1 d . . . C7 C 0.8240(9) 0.6544(11) 0.3436(6) 0.0127(18) Uani 1 1 d U . . C8 C 0.8248(9) 0.8034(12) 0.3432(6) 0.017(2) Uani 1 1 d U . . C9 C 0.7269(9) 0.8793(11) 0.3297(6) 0.0149(19) Uani 1 1 d U . . C10 C 0.6256(10) 0.8060(12) 0.3140(6) 0.021(2) Uani 1 1 d U . . H7 H 0.5577 0.8561 0.3033 0.025 Uiso 1 1 calc R . . C11 C 0.6249(10) 0.6595(12) 0.3141(6) 0.019(2) Uani 1 1 d U . . H6 H 0.5564 0.6105 0.3024 0.022 Uiso 1 1 calc R . . C12 C 0.7239(9) 0.5858(11) 0.3314(6) 0.016(2) Uani 1 1 d U . . C13 C 0.7212(9) 1.0323(11) 0.3317(6) 0.016(2) Uani 1 1 d . . . C14 C 0.7182(10) 0.4306(13) 0.3345(6) 0.019(2) Uani 1 1 d . . . O1 O 0.9538(8) 0.7514(8) 0.5417(5) 0.028(2) Uani 1 1 d . . . O2 O 1.2326(9) 0.9513(12) 0.4832(6) 0.042(3) Uani 1 1 d . . . O3 O 1.2287(8) 0.5114(11) 0.4927(5) 0.033(2) Uani 1 1 d . . . O4 O 1.2020(8) 0.4973(12) 0.3031(5) 0.034(2) Uani 1 1 d . . . O5 O 1.2020(8) 0.9289(12) 0.2917(5) 0.038(2) Uani 1 1 d . . . O6 O 0.8936(8) 0.7039(13) 0.1654(5) 0.040(3) Uani 1 1 d . . . O7 O 0.6371(7) 1.0973(8) 0.2985(5) 0.0249(10) Uani 1 1 d . . . O10 O 0.6255(7) 0.3745(8) 0.2981(5) 0.0249(10) Uani 1 1 d D . . S1 S 0.9591(2) 0.8795(3) 0.35568(14) 0.0150(6) Uani 1 1 d . . . S2 S 0.9563(2) 0.5738(3) 0.36205(14) 0.0152(6) Uani 1 1 d . . . Fe1 Fe 1.04461(13) 0.71859(19) 0.30835(8) 0.0166(4) Uani 1 1 d . . . Fe2 Fe 1.06593(13) 0.73246(16) 0.43419(8) 0.0137(4) Uani 1 1 d . . . O8 O 0.8097(7) 1.0944(9) 0.3690(5) 0.0249(10) Uani 1 1 d D . . O9 O 0.7975(7) 0.3626(8) 0.3698(5) 0.0249(10) Uani 1 1 d . . . H10 H 0.646(13) 0.272(7) 0.302(8) 0.037 Uiso 1 1 d D . . H8 H 0.812(13) 1.202(5) 0.374(8) 0.037 Uiso 1 1 d D . . C53 C 1.503(4) 0.706(6) 0.529(3) 0.067(6) Uiso 0.50 1 d PU A 1 H53A H 1.4474 0.7775 0.5317 0.081 Uiso 0.50 1 calc PR A 1 H53B H 1.4671 0.6140 0.5310 0.081 Uiso 0.50 1 calc PR A 1 C54 C 1.516(4) 0.717(6) 0.457(3) 0.068(7) Uiso 0.50 1 d PU A 1 H54A H 1.5308 0.8155 0.4469 0.082 Uiso 0.50 1 calc PR A 1 H54B H 1.5787 0.6586 0.4535 0.082 Uiso 0.50 1 calc PR A 1 C51 C 1.609(3) 0.777(4) 0.6500(17) 0.044(7) Uiso 0.50 1 d PU A 1 H51A H 1.6418 0.7097 0.6867 0.066 Uiso 0.50 1 calc PR A 1 H51B H 1.5397 0.8137 0.6562 0.066 Uiso 0.50 1 calc PR A 1 H51C H 1.6604 0.8545 0.6522 0.066 Uiso 0.50 1 calc PR A 1 C52 C 1.587(4) 0.716(6) 0.590(3) 0.073(7) Uiso 0.50 1 d PU A 1 H52A H 1.6026 0.6171 0.6037 0.087 Uiso 0.50 1 calc PR A 1 H52B H 1.6500 0.7466 0.5743 0.087 Uiso 0.50 1 calc PR A 1 C55 C 1.409(4) 0.667(5) 0.407(2) 0.058(8) Uiso 0.50 1 d PU A 1 H55A H 1.4097 0.6823 0.3598 0.088 Uiso 0.50 1 calc PR A 1 H55B H 1.3468 0.7194 0.4154 0.088 Uiso 0.50 1 calc PR A 1 H55C H 1.3994 0.5673 0.4150 0.088 Uiso 0.50 1 calc PR A 1 C63 C 1.510(4) 0.767(5) 0.521(3) 0.065(6) Uiso 0.50 1 d PU B 2 H63A H 1.4878 0.6692 0.5265 0.078 Uiso 0.50 1 calc PR B 2 H63B H 1.4516 0.8282 0.5287 0.078 Uiso 0.50 1 calc PR B 2 C64 C 1.508(4) 0.782(6) 0.460(3) 0.071(7) Uiso 0.50 1 d PU B 2 H64A H 1.5740 0.7318 0.4550 0.085 Uiso 0.50 1 calc PR B 2 H64B H 1.5202 0.8822 0.4536 0.085 Uiso 0.50 1 calc PR B 2 C61 C 1.587(4) 0.853(5) 0.624(2) 0.068(9) Uiso 0.50 1 d PU B 2 H61A H 1.6537 0.8743 0.6626 0.102 Uiso 0.50 1 calc PR B 2 H61B H 1.5398 0.7886 0.6402 0.102 Uiso 0.50 1 calc PR B 2 H61C H 1.5467 0.9392 0.6073 0.102 Uiso 0.50 1 calc PR B 2 C62 C 1.615(4) 0.796(5) 0.576(2) 0.060(7) Uiso 0.50 1 d PU B 2 H62A H 1.6566 0.7085 0.5922 0.072 Uiso 0.50 1 calc PR B 2 H62B H 1.6629 0.8598 0.5588 0.072 Uiso 0.50 1 calc PR B 2 C65 C 1.410(3) 0.737(5) 0.400(2) 0.052(8) Uiso 0.50 1 d PU B 2 H65A H 1.4214 0.7694 0.3564 0.078 Uiso 0.50 1 calc PR B 2 H65B H 1.3422 0.7774 0.4049 0.078 Uiso 0.50 1 calc PR B 2 H65C H 1.4047 0.6346 0.3990 0.078 Uiso 0.50 1 calc PR 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 C1 0.023(6) 0.014(6) 0.025(6) -0.002(4) 0.002(4) -0.004(4) C2 0.018(4) 0.008(4) 0.034(5) 0.002(3) 0.014(3) -0.005(3) C3 0.027(6) 0.013(5) 0.022(6) -0.005(4) 0.009(5) 0.006(5) C4 0.027(7) 0.030(7) 0.020(6) -0.001(5) 0.010(5) -0.007(6) C5 0.018(4) 0.008(4) 0.034(5) 0.002(3) 0.014(3) -0.005(3) C6 0.020(6) 0.038(8) 0.020(5) 0.002(5) 0.007(5) 0.003(5) C7 0.012(4) 0.006(4) 0.020(4) 0.004(3) 0.005(3) 0.003(3) C8 0.012(4) 0.020(5) 0.019(4) -0.003(4) 0.005(3) 0.001(4) C9 0.018(4) 0.007(4) 0.021(4) -0.002(3) 0.007(4) 0.000(4) C10 0.020(4) 0.013(5) 0.028(5) -0.001(4) 0.004(4) 0.005(4) C11 0.016(4) 0.011(4) 0.029(5) 0.001(4) 0.006(4) -0.001(4) C12 0.016(4) 0.007(4) 0.026(5) 0.001(4) 0.007(4) 0.000(4) C13 0.016(5) 0.005(5) 0.027(6) 0.005(4) 0.009(4) 0.000(4) C14 0.022(6) 0.021(6) 0.017(5) 0.003(4) 0.009(5) -0.001(5) O1 0.050(6) 0.010(4) 0.037(5) 0.001(3) 0.031(5) 0.007(4) O2 0.038(6) 0.038(6) 0.047(6) -0.001(5) 0.007(5) -0.017(5) O3 0.033(5) 0.030(5) 0.031(5) 0.002(4) 0.004(4) 0.011(4) O4 0.025(5) 0.043(6) 0.036(5) -0.014(5) 0.012(4) 0.006(4) O5 0.026(5) 0.052(7) 0.036(6) 0.009(5) 0.012(4) -0.002(5) O6 0.034(5) 0.064(8) 0.019(4) 0.002(5) 0.004(4) 0.007(5) O7 0.023(2) 0.0068(18) 0.039(2) 0.0023(17) 0.0011(18) 0.0009(16) O10 0.023(2) 0.0068(18) 0.039(2) 0.0023(17) 0.0011(18) 0.0009(16) S1 0.0147(13) 0.0113(12) 0.0196(13) 0.0023(10) 0.0060(10) -0.0009(10) S2 0.0122(13) 0.0128(13) 0.0200(13) -0.0005(10) 0.0039(10) 0.0035(10) Fe1 0.0143(8) 0.0216(9) 0.0150(7) 0.0014(6) 0.0060(6) 0.0027(7) Fe2 0.0160(7) 0.0101(7) 0.0146(7) 0.0003(6) 0.0038(6) -0.0004(6) O8 0.023(2) 0.0068(18) 0.039(2) 0.0023(17) 0.0011(18) 0.0009(16) O9 0.023(2) 0.0068(18) 0.039(2) 0.0023(17) 0.0011(18) 0.0009(16) _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 C1 O1 1.145(15) . ? C1 Fe2 1.794(13) . ? C2 O2 1.108(15) . ? C2 Fe2 1.817(11) . ? C3 O3 1.162(15) . ? C3 Fe2 1.779(12) . ? C4 O4 1.118(17) . ? C4 Fe1 1.812(14) . ? C5 O5 1.137(15) . ? C5 Fe1 1.783(11) . ? C6 O6 1.149(15) . ? C6 Fe1 1.807(12) . ? C7 C12 1.380(15) . ? C7 C8 1.426(15) . ? C7 S2 1.776(11) . ? C8 C9 1.390(15) . ? C8 S1 1.794(11) . ? C9 C10 1.410(16) . ? C9 C13 1.466(15) . ? C10 C11 1.401(16) . ? C11 C12 1.387(16) . ? C12 C14 1.489(16) . ? C13 O7 1.242(14) . ? C13 O8 1.292(14) . ? C14 O9 1.228(15) . ? C14 O10 1.299(15) . ? S1 Fe2 2.245(3) . ? S1 Fe1 2.253(3) . ? S2 Fe1 2.252(3) . ? S2 Fe2 2.268(3) . ? Fe1 Fe2 2.484(3) . ? C53 C52 1.37(7) . ? C53 C54 1.53(7) . ? C54 C55 1.51(7) . ? C51 C52 1.29(6) . ? C63 C64 1.23(7) . ? C63 C62 1.49(6) . ? C64 C65 1.52(7) . ? C61 C62 1.25(6) . ? 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 O1 C1 Fe2 177.3(11) . . ? O2 C2 Fe2 178.3(13) . . ? O3 C3 Fe2 179.9(12) . . ? O4 C4 Fe1 177.2(12) . . ? O5 C5 Fe1 179.8(14) . . ? O6 C6 Fe1 177.3(11) . . ? C12 C7 C8 118.8(10) . . ? C12 C7 S2 125.9(8) . . ? C8 C7 S2 115.3(8) . . ? C9 C8 C7 121.1(10) . . ? C9 C8 S1 124.4(9) . . ? C7 C8 S1 114.4(8) . . ? C8 C9 C10 118.7(10) . . ? C8 C9 C13 124.3(10) . . ? C10 C9 C13 117.0(10) . . ? C11 C10 C9 120.2(11) . . ? C12 C11 C10 120.2(11) . . ? C7 C12 C11 120.9(10) . . ? C7 C12 C14 121.3(10) . . ? C11 C12 C14 117.8(10) . . ? O7 C13 O8 122.5(10) . . ? O7 C13 C9 121.7(11) . . ? O8 C13 C9 115.8(10) . . ? O9 C14 O10 123.5(11) . . ? O9 C14 C12 120.7(11) . . ? O10 C14 C12 115.8(10) . . ? C8 S1 Fe2 100.9(4) . . ? C8 S1 Fe1 102.6(4) . . ? Fe2 S1 Fe1 67.04(10) . . ? C7 S2 Fe1 101.7(4) . . ? C7 S2 Fe2 101.6(4) . . ? Fe1 S2 Fe2 66.67(10) . . ? C5 Fe1 C6 99.6(6) . . ? C5 Fe1 C4 91.0(5) . . ? C6 Fe1 C4 99.0(6) . . ? C5 Fe1 S2 159.0(4) . . ? C6 Fe1 S2 101.0(4) . . ? C4 Fe1 S2 89.9(4) . . ? C5 Fe1 S1 90.5(4) . . ? C6 Fe1 S1 102.1(4) . . ? C4 Fe1 S1 158.3(4) . . ? S2 Fe1 S1 81.05(11) . . ? C5 Fe1 Fe2 102.4(4) . . ? C6 Fe1 Fe2 148.9(4) . . ? C4 Fe1 Fe2 102.2(4) . . ? S2 Fe1 Fe2 56.97(9) . . ? S1 Fe1 Fe2 56.33(9) . . ? C3 Fe2 C1 99.4(6) . . ? C3 Fe2 C2 92.5(5) . . ? C1 Fe2 C2 99.0(5) . . ? C3 Fe2 S1 159.2(4) . . ? C1 Fe2 S1 100.5(4) . . ? C2 Fe2 S1 90.1(4) . . ? C3 Fe2 S2 89.8(4) . . ? C1 Fe2 S2 100.8(4) . . ? C2 Fe2 S2 159.4(4) . . ? S1 Fe2 S2 80.87(11) . . ? C3 Fe2 Fe1 102.8(4) . . ? C1 Fe2 Fe1 147.5(4) . . ? C2 Fe2 Fe1 103.3(4) . . ? S1 Fe2 Fe1 56.62(9) . . ? S2 Fe2 Fe1 56.36(9) . . ? C52 C53 C54 125(5) . . ? C55 C54 C53 106(4) . . ? C51 C52 C53 140(5) . . ? C64 C63 C62 118(5) . . ? C63 C64 C65 122(5) . . ? C61 C62 C63 106(4) . . ? _iucr_refine_instructions_details ; TITL AO_SP_dicarb_No5_0m in P2(1)/c CELL 0.71073 12.6408 9.5641 20.2502 90.000 107.432 90.000 ZERR 4.00 0.0067 0.0050 0.0104 0.000 0.020 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O S FE UNIT 76 64 40 8 8 MERG 4 DFIX 1.0 0.05 O8 H8 DFIX 1.0 0.05 O10 H10 SIMU 0.010 0.010 C7 C8 C9 C10 C11 C12 SIMU 0.01 0.01 C51 C61 C55 C65 SIMU 0.01 0.01 C52 C53 C53 C54 C62 C63 C64 EADP O9 O10 O8 O7 EADP C2 C5 FMAP 2 PLAN 10 ACTA LIST 4 WGHT 0.05350 96.01070 L.S. 20 TEMP -173.15 FVAR 0.06585 0.80000 C1 1 0.999567 0.742574 0.500901 11.00000 0.02336 0.01158 = 0.02593 -0.00221 0.00237 -0.00433 C2 1 1.168128 0.869772 0.464228 11.00000 0.01654 0.01075 = 0.03212 -0.00076 0.00866 -0.01134 C3 1 1.164406 0.598681 0.469493 11.00000 0.02749 0.01235 = 0.02236 -0.00446 0.00921 0.00509 C4 1 1.139705 0.579206 0.304687 11.00000 0.02656 0.03045 = 0.01984 0.00000 0.00914 -0.00682 C5 1 1.140659 0.847059 0.298092 11.00000 0.01884 0.00448 = 0.03775 0.00571 0.01849 -0.00064 C6 1 0.954428 0.709826 0.220341 11.00000 0.01960 0.03772 = 0.01965 0.00156 0.00662 0.00196 C7 1 0.824004 0.654379 0.343567 11.00000 0.01227 0.00632 = 0.02019 0.00453 0.00546 0.00269 C8 1 0.824774 0.803384 0.343246 11.00000 0.01168 0.01970 = 0.01856 -0.00302 0.00525 0.00039 C9 1 0.726926 0.879423 0.329705 11.00000 0.01772 0.00727 = 0.02073 -0.00196 0.00711 -0.00021 C10 1 0.625601 0.806049 0.314027 11.00000 0.01972 0.01301 = 0.02768 -0.00063 0.00436 0.00474 AFIX 43 H7 2 0.557635 0.856071 0.303368 11.00000 -1.20000 AFIX 0 C11 1 0.624996 0.659534 0.314143 11.00000 0.01604 0.01089 = 0.02891 0.00076 0.00595 -0.00116 AFIX 43 H6 2 0.556502 0.610525 0.302371 11.00000 -1.20000 AFIX 0 C12 1 0.723901 0.585851 0.331358 11.00000 0.01589 0.00596 = 0.02614 0.00096 0.00692 0.00024 C13 1 0.721201 1.032250 0.331666 11.00000 0.01635 0.00542 = 0.02729 0.00547 0.00948 0.00014 C14 1 0.718199 0.430616 0.334490 11.00000 0.02197 0.02085 = 0.01657 0.00293 0.00909 -0.00149 O1 3 0.953739 0.751384 0.541698 11.00000 0.04973 0.01069 = 0.03680 0.00049 0.03169 0.00708 O2 3 1.232595 0.951147 0.483234 11.00000 0.03785 0.03980 = 0.04679 -0.00077 0.00705 -0.01531 O3 3 1.228700 0.511289 0.492719 11.00000 0.03340 0.03075 = 0.03128 0.00178 0.00433 0.01041 O4 3 1.202022 0.497254 0.303053 11.00000 0.02533 0.04384 = 0.03581 -0.01407 0.01203 0.00527 O5 3 1.202001 0.928925 0.291687 11.00000 0.02615 0.05168 = 0.03639 0.00938 0.01189 -0.00208 O6 3 0.893598 0.703809 0.165393 11.00000 0.03434 0.06345 = 0.01864 0.00185 0.00391 0.00699 O7 3 0.637126 1.097358 0.298464 11.00000 0.02325 0.00681 = 0.03920 0.00221 0.00107 0.00114 O10 3 0.625560 0.374504 0.298057 11.00000 0.02325 0.00681 = 0.03920 0.00221 0.00107 0.00114 S1 4 0.959103 0.879507 0.355676 11.00000 0.01462 0.01147 = 0.01957 0.00222 0.00596 -0.00096 S2 4 0.956318 0.573788 0.362055 11.00000 0.01218 0.01251 = 0.02010 -0.00051 0.00390 0.00355 FE1 5 1.044601 0.718591 0.308355 11.00000 0.01428 0.02163 = 0.01499 0.00135 0.00608 0.00267 FE2 5 1.065930 0.732461 0.434187 11.00000 0.01602 0.01018 = 0.01456 0.00035 0.00377 -0.00032 O8 3 0.809701 1.094434 0.368953 11.00000 0.02325 0.00681 = 0.03920 0.00221 0.00107 0.00114 O9 3 0.797490 0.362565 0.369772 11.00000 0.02325 0.00681 = 0.03920 0.00221 0.00107 0.00114 H10 2 0.646019 0.272214 0.302090 11.00000 -1.50000 H8 2 0.812106 1.202026 0.374598 11.00000 -1.50000 MOLE 2 PART 1 C53 1 1.502684 0.706023 0.529525 10.50000 0.06727 AFIX 23 H53A 2 1.447626 0.778089 0.531736 10.50000 -1.20000 H53B 2 1.467039 0.614461 0.531187 10.50000 -1.20000 AFIX 0 C54 1 1.516278 0.717165 0.457180 10.50000 0.06839 AFIX 23 H54A 2 1.531097 0.815155 0.446901 10.50000 -1.20000 H54B 2 1.578664 0.658084 0.453647 10.50000 -1.20000 AFIX 0 C51 1 1.608480 0.777065 0.649987 10.50000 0.04412 AFIX 33 H51A 2 1.641753 0.709200 0.686573 10.50000 -1.50000 H51B 2 1.539451 0.813045 0.656136 10.50000 -1.50000 H51C 2 1.660215 0.854614 0.652505 10.50000 -1.50000 AFIX 0 C52 1 1.587409 0.716859 0.590320 10.50000 0.07276 AFIX 23 H52A 2 1.603995 0.617646 0.603263 10.50000 -1.20000 H52B 2 1.649908 0.748704 0.574107 10.50000 -1.20000 AFIX 0 C55 1 1.408525 0.667091 0.407471 10.50000 0.05829 AFIX 33 H55A 2 1.409666 0.682231 0.359826 10.50000 -1.50000 H55B 2 1.346744 0.719337 0.415394 10.50000 -1.50000 H55C 2 1.399175 0.567179 0.414905 10.50000 -1.50000 AFIX 0 PART 2 C63 1 1.509503 0.766712 0.520645 10.50000 0.06506 AFIX 23 H63A 2 1.488076 0.668973 0.526453 10.50000 -1.20000 H63B 2 1.451360 0.827818 0.528695 10.50000 -1.20000 AFIX 0 C64 1 1.508093 0.781723 0.459973 10.50000 0.07102 AFIX 23 H64A 2 1.574055 0.732430 0.454850 10.50000 -1.20000 H64B 2 1.519759 0.882519 0.453466 10.50000 -1.20000 AFIX 0 C61 1 1.587318 0.852185 0.624214 10.50000 0.06786 AFIX 33 H61A 2 1.653688 0.873816 0.662611 10.50000 -1.50000 H61B 2 1.539910 0.787746 0.640220 10.50000 -1.50000 H61C 2 1.546440 0.938637 0.607507 10.50000 -1.50000 AFIX 0 C62 1 1.615311 0.796440 0.576068 10.50000 0.06017 AFIX 23 H62A 2 1.656864 0.708866 0.592020 10.50000 -1.20000 H62B 2 1.662601 0.860541 0.558828 10.50000 -1.20000 AFIX 0 C65 1 1.410502 0.736590 0.399709 10.50000 0.05195 AFIX 33 H65A 2 1.421304 0.769162 0.356298 10.50000 -1.50000 H65B 2 1.342155 0.777047 0.404818 10.50000 -1.50000 H65C 2 1.404921 0.634368 0.399031 10.50000 -1.50000 AFIX 0 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 END ; _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.51 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 3.370 _refine_diff_density_min -1.884 _refine_diff_density_rms 0.250