data_hklf5 _audit_creation_date 2014-04-30 _audit_creation_method ; Olex2 1.2 (compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816) ; _shelxl_version_number 2013-3 _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C20 H30 Cl2 N2 O8 Rh2' _chemical_formula_sum 'C20 H30 Cl2 N2 O8 Rh2' _chemical_formula_weight 703.18 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.2575(17) _cell_length_b 19.844(5) _cell_length_c 9.142(2) _cell_angle_alpha 90 _cell_angle_beta 99.336(5) _cell_angle_gamma 90 _cell_volume 1299.2(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9817 _cell_measurement_temperature 100.0 _cell_measurement_theta_max 66.88 _cell_measurement_theta_min 4.46 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 12.573 _exptl_absorpt_correction_T_max 0.753 _exptl_absorpt_correction_T_min 0.174 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; TWINABS-2012/1 (Bruker,2012) was used for absorption correction. For component 1: wR2(int) was 0.1353 before and 0.0737 after correction. The Ratio of minimum to maximum transmission not present. The \l/2 correction factor is Not present For component 2: wR2(int) was 0.1678 before and 0.0782 after correction. The Ratio of minimum to maximum transmission is 0.23. The \l/2 correction factor is Not present Final HKLF 4 output contains 23905 reflections, Rint = 0.0725 (22594 with I > 3sig(I), Rint = 0.0725) ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.797 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description ? _exptl_crystal_F_000 704 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.11 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_unetI/netI 0.0452 _diffrn_reflns_Laue_measured_fraction_full 0.972 _diffrn_reflns_Laue_measured_fraction_max 0.980 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2291 _diffrn_reflns_point_group_measured_fraction_full 0.972 _diffrn_reflns_point_group_measured_fraction_max 0.980 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 67.258 _diffrn_reflns_theta_min 4.456 _diffrn_ambient_temperature 100.0 _diffrn_detector 'Bruker Proteum CCD' _diffrn_detector_area_resol_mean ? _diffrn_detector_type 'Bruker Proteum CCD' _diffrn_measured_fraction_theta_full 0.972 _diffrn_measured_fraction_theta_max 0.980 _diffrn_measurement_device 'Bruker Mircostar Rotating anode' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'micro-focus rotating anode' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2289 _reflns_number_total 2291 _reflns_special_details ; _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution ? _refine_diff_density_max 1.442 _refine_diff_density_min -1.397 _refine_diff_density_rms 0.182 _refine_ls_extinction_coef 0.0024(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 159 _refine_ls_number_reflns 2291 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0362 _refine_ls_restrained_S_all 1.351 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+0.9613P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0937 _refine_ls_wR_factor_ref 0.0938 _refine_special_details ; Structure is twinned 7.8 degree rotation around reciprocal axis 1 -0.25 0.20, direct axis 1 0 0.25. The BASF refines to 0.412(4). ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints C3 \\sim C2 \\sim O2: within 1.7A with sigma of 0.003 and sigma for terminal atoms of 0.006 Uanis(Rh1) \\sim Ueq: with sigma of 0.0003 and sigma for terminal atoms of 0.0006 3.a Ternary CH refined with riding coordinates: C5(H5), C4(H4) 3.b Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C3(H3A,H3B) 3.c Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? 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 Rh1 Rh 0.62156(3) 0.58178(2) 0.49947(2) 0.01065(16) Uani 1 1 d . U . . . Cl1 Cl 0.32122(9) 0.54175(4) 0.56661(8) 0.0144(2) Uani 1 1 d . . . . . O4 O 0.5892(3) 0.59029(12) 0.0522(3) 0.0200(5) Uani 1 1 d . . . . . O3 O 0.4982(3) 0.59310(12) 0.2774(3) 0.0157(5) Uani 1 1 d . . . . . N1 N 0.8040(4) 0.60257(14) 0.2563(3) 0.0168(6) Uani 1 1 d . . . . . O1 O 0.8315(4) 0.56203(15) 0.8030(3) 0.0268(6) Uani 1 1 d . . . . . C6 C 0.6244(5) 0.59540(16) 0.1991(4) 0.0154(7) Uani 1 1 d . . . . . C1 C 0.7499(5) 0.57062(17) 0.6881(4) 0.0175(7) Uani 1 1 d . . . . . C7 C 0.3935(5) 0.58211(17) -0.0163(4) 0.0220(9) Uani 1 1 d . . . . . H7A H 0.3261 0.5558 0.0505 0.026 Uiso 1 1 calc R . . . . H7B H 0.3866 0.5570 -0.1106 0.026 Uiso 1 1 calc R . . . . C8 C 0.3024(5) 0.65005(18) -0.0457(4) 0.0254(8) Uani 1 1 d . . . . . H8A H 0.3686 0.6758 -0.1126 0.038 Uiso 1 1 calc GR . . . . H8B H 0.3077 0.6745 0.0480 0.038 Uiso 1 1 calc GR . . . . H8C H 0.1718 0.6440 -0.0917 0.038 Uiso 1 1 calc GR . . . . C10 C 0.9516(5) 0.6001(2) 0.1664(4) 0.0225(7) Uani 1 1 d . . . . . H10A H 0.9498 0.5561 0.1173 0.034 Uiso 1 1 calc GR . . . . H10B H 1.0727 0.6067 0.2298 0.034 Uiso 1 1 calc GR . . . . H10C H 0.9317 0.6358 0.0914 0.034 Uiso 1 1 calc GR . . . . C5 C 0.8535(4) 0.61338(16) 0.4174(3) 0.0147(6) Uani 1 1 d . . . . . H5 H 0.9641 0.5853 0.4588 0.018 Uiso 1 1 calc R . . . . O2 O 0.4934(3) 0.70275(12) 0.6224(3) 0.0244(5) Uani 1 1 d . . . . . C2 C 0.5887(4) 0.68077(16) 0.5382(4) 0.0183(6) Uani 1 1 d . . . . . C3 C 0.7037(5) 0.72286(17) 0.4485(4) 0.0202(7) Uani 1 1 d . . . . . H3A H 0.7215 0.7688 0.4907 0.024 Uiso 1 1 calc R . . . . H3B H 0.6394 0.7266 0.3447 0.024 Uiso 1 1 calc R . . . . C4 C 0.8927(4) 0.68797(16) 0.4537(4) 0.0181(6) Uani 1 1 d . . . . . H4 H 0.9579 0.7080 0.3757 0.022 Uiso 1 1 calc R . . . . C9 C 1.0145(5) 0.69723(18) 0.6038(4) 0.0228(7) Uani 1 1 d . . . . . H9A H 0.9463 0.6822 0.6820 0.034 Uiso 1 1 calc GR . . . . H9B H 1.0471 0.7449 0.6186 0.034 Uiso 1 1 calc GR . . . . H9C H 1.1288 0.6705 0.6078 0.034 Uiso 1 1 calc GR . . . . 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 Rh1 0.0060(2) 0.0155(2) 0.0083(2) -0.00010(6) -0.00515(11) -0.00005(6) Cl1 0.0078(4) 0.0179(4) 0.0163(4) -0.0017(3) -0.0020(3) 0.0010(3) O4 0.0153(12) 0.0316(13) 0.0104(13) -0.0005(9) -0.0057(10) 0.0025(9) O3 0.0099(11) 0.0255(12) 0.0099(12) 0.0023(9) -0.0037(9) 0.0010(9) N1 0.0102(13) 0.0255(14) 0.0134(14) -0.0004(11) -0.0017(10) -0.0002(11) O1 0.0249(13) 0.0385(14) 0.0127(13) 0.0027(11) -0.0099(10) -0.0014(12) C6 0.0115(16) 0.0184(14) 0.0137(16) -0.0006(12) -0.0062(13) 0.0014(12) C1 0.0116(16) 0.0208(15) 0.0189(19) -0.0013(13) -0.0013(14) -0.0019(13) C7 0.017(2) 0.035(2) 0.0111(19) -0.0028(12) -0.0091(16) -0.0050(12) C8 0.0139(16) 0.0352(19) 0.0237(18) 0.0068(15) -0.0073(14) -0.0033(14) C10 0.0127(16) 0.0332(18) 0.0221(19) 0.0011(15) 0.0043(14) 0.0027(15) C5 0.0102(14) 0.0222(16) 0.0100(14) 0.0003(11) -0.0029(11) -0.0001(12) O2 0.0193(12) 0.0251(12) 0.0280(13) -0.0055(10) 0.0017(10) 0.0016(9) C2 0.0104(13) 0.0216(14) 0.0191(14) 0.0008(12) -0.0089(12) -0.0006(12) C3 0.0154(15) 0.0211(15) 0.0214(15) 0.0026(12) -0.0055(13) 0.0007(12) C4 0.0123(15) 0.0207(16) 0.0202(16) 0.0002(13) -0.0010(12) -0.0033(12) C9 0.0135(16) 0.0265(18) 0.0261(19) -0.0041(14) -0.0037(14) -0.0028(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 Rh1 Cl1 2.4885(9) . ? Rh1 Cl1 2.5744(9) 3_666 ? Rh1 O3 2.094(2) . ? Rh1 C1 1.836(4) . ? Rh1 C5 2.049(3) . ? Rh1 C2 2.017(3) . ? Cl1 Rh1 2.5745(9) 3_666 ? O4 C6 1.329(4) . ? O4 C7 1.465(4) . ? O3 C6 1.252(4) . ? N1 C6 1.331(4) . ? N1 C10 1.453(5) . ? N1 C5 1.474(4) . ? O1 C1 1.131(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.506(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C5 H5 1.0000 . ? C5 C4 1.533(4) . ? O2 C2 1.198(5) . ? C2 C3 1.513(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.530(5) . ? C4 H4 1.0000 . ? C4 C9 1.519(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 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 Cl1 Rh1 Cl1 86.28(3) . 3_666 ? O3 Rh1 Cl1 91.12(7) . . ? O3 Rh1 Cl1 86.24(7) . 3_666 ? C1 Rh1 Cl1 93.51(12) . . ? C1 Rh1 Cl1 91.67(11) . 3_666 ? C1 Rh1 O3 174.79(12) . . ? C1 Rh1 C5 93.38(14) . . ? C1 Rh1 C2 90.50(14) . . ? C5 Rh1 Cl1 91.84(9) . 3_666 ? C5 Rh1 Cl1 172.91(9) . . ? C5 Rh1 O3 81.93(11) . . ? C2 Rh1 Cl1 175.33(11) . 3_666 ? C2 Rh1 Cl1 97.72(10) . . ? C2 Rh1 O3 91.24(11) . . ? C2 Rh1 C5 83.90(14) . . ? Rh1 Cl1 Rh1 93.72(3) . 3_666 ? C6 O4 C7 117.0(3) . . ? C6 O3 Rh1 108.7(2) . . ? C6 N1 C10 122.6(3) . . ? C6 N1 C5 118.2(3) . . ? C10 N1 C5 119.2(3) . . ? O4 C6 N1 114.9(3) . . ? O3 C6 O4 122.4(3) . . ? O3 C6 N1 122.7(3) . . ? O1 C1 Rh1 177.9(3) . . ? O4 C7 H7A 109.6 . . ? O4 C7 H7B 109.6 . . ? O4 C7 C8 110.1(3) . . ? H7A C7 H7B 108.2 . . ? C8 C7 H7A 109.6 . . ? C8 C7 H7B 109.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Rh1 C5 H5 110.3 . . ? N1 C5 Rh1 103.87(19) . . ? N1 C5 H5 110.3 . . ? N1 C5 C4 111.3(3) . . ? C4 C5 Rh1 110.6(2) . . ? C4 C5 H5 110.3 . . ? O2 C2 Rh1 124.4(3) . . ? O2 C2 C3 125.1(3) . . ? C3 C2 Rh1 110.5(2) . . ? C2 C3 H3A 110.2 . . ? C2 C3 H3B 110.2 . . ? C2 C3 C4 107.7(3) . . ? H3A C3 H3B 108.5 . . ? C4 C3 H3A 110.2 . . ? C4 C3 H3B 110.2 . . ? C5 C4 H4 108.8 . . ? C3 C4 C5 107.2(2) . . ? C3 C4 H4 108.8 . . ? C9 C4 C5 111.9(3) . . ? C9 C4 C3 111.2(3) . . ? C9 C4 H4 108.8 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Rh1 O3 C6 O4 167.7(2) . . . . ? Rh1 O3 C6 N1 -11.7(4) . . . . ? Rh1 C5 C4 C3 -34.2(3) . . . . ? Rh1 C5 C4 C9 87.9(3) . . . . ? Rh1 C2 C3 C4 -41.1(3) . . . . ? N1 C5 C4 C3 80.7(3) . . . . ? N1 C5 C4 C9 -157.2(3) . . . . ? C6 O4 C7 C8 87.5(4) . . . . ? C6 N1 C5 Rh1 18.3(3) . . . . ? C6 N1 C5 C4 -100.7(3) . . . . ? C7 O4 C6 O3 0.4(5) . . . . ? C7 O4 C6 N1 179.8(3) . . . . ? C10 N1 C6 O4 -4.3(5) . . . . ? C10 N1 C6 O3 175.2(3) . . . . ? C10 N1 C5 Rh1 -161.7(3) . . . . ? C10 N1 C5 C4 79.4(4) . . . . ? C5 N1 C6 O4 175.8(3) . . . . ? C5 N1 C6 O3 -4.8(5) . . . . ? O2 C2 C3 C4 137.9(3) . . . . ? C2 C3 C4 C5 48.3(3) . . . . ? C2 C3 C4 C9 -74.2(3) . . . . ? _shelx_res_file ; TITL CELL 1.54178 7.2575 19.8438 9.1424 90 99.3362 90 ZERR 2 0.0017 0.0045 0.0021 0 0.005 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl N O Rh UNIT 40 60 4 4 16 4 SIMU 0.003 0.006 1.7 C3 C2 O2 ISOR 0.0003 0.0006 Rh1 L.S. 20 PLAN 10 TEMP -173.15 MORE -1 BOND $H CONF fmap 2 ACTA REM C:/Users/hs14463/Desktop/Bristol%20X-ray/MS1528a/work/hklf5.hkl WGHT 0.058000 0.961300 EXTI 0.002402 BASF 0.41214 FVAR 0.53519 RH1 6 0.621556 0.581776 0.499470 11.00000 0.00601 0.01550 = 0.00832 -0.00010 -0.00515 -0.00005 CL1 3 0.321223 0.541755 0.566612 11.00000 0.00777 0.01794 = 0.01634 -0.00173 -0.00195 0.00101 O4 5 0.589169 0.590291 0.052220 11.00000 0.01533 0.03164 = 0.01037 -0.00051 -0.00568 0.00245 O3 5 0.498183 0.593098 0.277393 11.00000 0.00990 0.02554 = 0.00989 0.00232 -0.00375 0.00102 N1 4 0.803972 0.602573 0.256350 11.00000 0.01021 0.02554 = 0.01336 -0.00039 -0.00170 -0.00017 O1 5 0.831456 0.562027 0.802966 11.00000 0.02488 0.03851 = 0.01272 0.00267 -0.00987 -0.00137 C6 1 0.624445 0.595402 0.199064 11.00000 0.01148 0.01837 = 0.01366 -0.00059 -0.00617 0.00138 C1 1 0.749940 0.570622 0.688116 11.00000 0.01159 0.02077 = 0.01888 -0.00126 -0.00130 -0.00189 C7 1 0.393460 0.582115 -0.016257 11.00000 0.01657 0.03458 = 0.01110 -0.00277 -0.00909 -0.00498 AFIX 23 H7A 2 0.326145 0.555819 0.050495 11.00000 -1.20000 H7B 2 0.386607 0.557010 -0.110563 11.00000 -1.20000 AFIX 0 C8 1 0.302449 0.650055 -0.045716 11.00000 0.01389 0.03518 = 0.02374 0.00677 -0.00726 -0.00327 AFIX 137 H8A 2 0.368564 0.675803 -0.112600 11.00000 -1.50000 H8B 2 0.307744 0.674525 0.047982 11.00000 -1.50000 H8C 2 0.171822 0.644040 -0.091698 11.00000 -1.50000 AFIX 0 C10 1 0.951571 0.600099 0.166409 11.00000 0.01274 0.03324 = 0.02208 0.00112 0.00432 0.00269 AFIX 137 H10A 2 0.949838 0.556149 0.117317 11.00000 -1.50000 H10B 2 1.072671 0.606687 0.229834 11.00000 -1.50000 H10C 2 0.931741 0.635794 0.091423 11.00000 -1.50000 AFIX 0 C5 1 0.853465 0.613375 0.417440 11.00000 0.01024 0.02223 = 0.00998 0.00025 -0.00286 -0.00007 AFIX 13 H5 2 0.964055 0.585261 0.458814 11.00000 -1.20000 AFIX 0 O2 5 0.493367 0.702746 0.622395 11.00000 0.01933 0.02511 = 0.02797 -0.00546 0.00167 0.00155 C2 1 0.588732 0.680775 0.538226 11.00000 0.01042 0.02160 = 0.01907 0.00076 -0.00894 -0.00057 C3 1 0.703741 0.722859 0.448469 11.00000 0.01539 0.02107 = 0.02137 0.00256 -0.00553 0.00068 AFIX 23 H3A 2 0.721540 0.768778 0.490739 11.00000 -1.20000 H3B 2 0.639360 0.726582 0.344693 11.00000 -1.20000 AFIX 0 C4 1 0.892699 0.687974 0.453661 11.00000 0.01227 0.02072 = 0.02024 0.00024 -0.00099 -0.00327 AFIX 13 H4 2 0.957871 0.708033 0.375669 11.00000 -1.20000 AFIX 0 C9 1 1.014539 0.697230 0.603819 11.00000 0.01349 0.02650 = 0.02608 -0.00410 -0.00374 -0.00284 AFIX 137 H9A 2 0.946267 0.682189 0.682001 11.00000 -1.50000 H9B 2 1.047139 0.744948 0.618558 11.00000 -1.50000 H9C 2 1.128835 0.670527 0.607793 11.00000 -1.50000 AFIX 0 HKLF 5 REM REM R1 = 0.0362 for 2289 Fo > 4sig(Fo) and 0.0362 for all 2291 data REM 159 parameters refined using 18 restraints END WGHT 0.0580 0.9613 REM Highest difference peak 1.442, deepest hole -1.397, 1-sigma level 0.182 Q1 1 0.5466 0.6262 0.4675 11.00000 0.05 1.44 Q2 1 0.6731 0.5460 0.5232 11.00000 0.05 1.41 Q3 1 0.6820 0.6209 0.5236 11.00000 0.05 1.41 Q4 1 0.5421 0.5335 0.4681 11.00000 0.05 1.40 Q5 1 0.3899 0.4990 0.5994 11.00000 0.05 0.84 Q6 1 0.3016 0.5727 0.5608 11.00000 0.05 0.75 Q7 1 0.4297 0.5801 0.4383 11.00000 0.05 0.66 Q8 1 0.3903 0.5818 0.5953 11.00000 0.05 0.66 Q9 1 0.2489 0.5020 0.5421 11.00000 0.05 0.63 Q10 1 0.3771 0.6082 -0.0064 11.00000 0.05 0.54 ; _shelx_res_checksum 51351 _shelx_hkl_file ; 1 0 0 9999.99 644.139 -2 1 0 0 9999.99 644.139 1 2 0 0 16.0351 1.03711 -2 2 0 0 16.0351 1.03711 1 3 0 0 4239.71 441.065 -2 3 0 0 4239.71 441.065 1 4 0 0 2890.94 300.983 1 5 0 0 682.586 21.8956 1 6 0 0 119.782 4.43946 1 7 0 0 364.305 15.5416 1 8 0 0 632.839 26.7985 1 1 1 0 3213.31 246.602 -2 1 1 0 3213.31 246.602 1 2 1 0 330.143 12.4495 1 3 1 0 1819.86 189.492 -2 3 1 0 1819.86 189.492 1 4 1 0 181.348 19.3147 1 5 1 0 241.074 12.1226 -2 5 1 0 241.074 12.1226 1 6 1 0 860.528 58.8659 -2 6 1 0 860.528 58.8659 1 7 1 0 761.203 52.1128 -2 7 1 0 761.203 52.1128 1 8 1 0 44.6240 1.59236 1 0 2 0 1991.39 230.260 1 1 2 0 1242.46 62.8493 1 2 2 0 483.134 19.2505 1 3 2 0 689.858 27.4865 1 4 2 0 1267.25 132.184 1 5 2 0 339.375 7.69618 1 6 2 0 22.4496 0.82329 1 7 2 0 172.856 4.82138 1 8 2 0 65.0820 2.24148 1 0 3 0 0.37096 0.45034 1 1 3 0 2502.69 109.297 1 2 3 0 862.103 37.1053 1 3 3 0 2490.65 107.044 1 4 3 0 867.411 38.4325 1 5 3 0 379.779 8.72371 1 6 3 0 2542.81 69.2312 1 7 3 0 1023.27 29.9737 1 8 3 0 123.880 4.13326 1 0 4 0 2897.80 200.756 1 1 4 0 366.602 17.8053 1 2 4 0 95.8725 3.96599 1 3 4 0 5.52842 0.55207 1 4 4 0 735.108 19.3248 1 5 4 0 748.290 17.2058 1 6 4 0 58.7653 1.63271 1 7 4 0 129.748 4.36715 1 8 4 0 325.416 12.1444 1 0 5 0 0.76347 0.44048 1 1 5 0 484.090 23.4979 1 2 5 0 230.355 9.38535 1 3 5 0 146.634 6.48789 1 4 5 0 168.758 3.47362 1 5 5 0 38.3918 1.00344 1 6 5 0 517.022 13.1894 1 7 5 0 445.621 14.6095 1 8 5 0 68.7105 2.68042 1 0 6 0 7938.50 549.986 1 1 6 0 2606.30 113.851 1 2 6 0 3.63805 0.36701 1 3 6 0 648.362 28.0336 1 4 6 0 1911.61 37.3141 1 5 6 0 1644.92 37.7249 1 6 6 0 14.0612 0.60925 1 7 6 0 580.511 18.9855 1 8 6 0 906.705 38.3256 1 0 7 0 1.15947 1.02656 1 1 7 0 2294.80 100.279 1 2 7 0 1455.24 58.6970 1 3 7 0 134.849 6.02764 1 4 7 0 126.241 2.58705 1 5 7 0 349.232 7.89369 1 6 7 0 244.121 6.29024 1 7 7 0 22.3809 0.86044 1 8 7 0 5.08061 0.47719 1 0 8 0 4013.38 278.146 1 1 8 0 930.695 40.7747 1 2 8 0 30.7476 1.44507 1 3 8 0 453.342 15.6105 1 4 8 0 596.604 11.9152 1 5 8 0 242.635 5.51954 1 6 8 0 1.11152 0.31061 1 7 8 0 102.103 3.87687 1 8 8 0 251.943 19.0312 1 1 9 0 3935.17 171.903 1 2 9 0 3013.71 124.849 1 3 9 0 1249.79 26.8190 1 4 9 0 14.0033 0.47704 1 5 9 0 778.028 19.0665 1 6 9 0 1045.82 30.7377 1 7 9 0 488.066 17.8399 1 0 10 0 1484.37 103.131 1 1 10 0 303.388 12.7656 1 2 10 0 978.580 46.3907 1 3 10 0 47.1966 1.14344 1 4 10 0 132.136 2.96854 1 5 10 0 569.650 14.1540 1 6 10 0 58.7457 1.93268 1 7 10 0 172.385 6.39444 1 0 11 0 1.15698 0.63522 1 1 11 0 265.404 11.2090 1 2 11 0 774.755 21.6431 1 3 11 0 173.959 3.90580 1 4 11 0 5.82643 0.34915 1 5 11 0 112.690 3.36345 1 6 11 0 339.451 10.3303 1 7 11 0 151.839 6.40128 1 0 12 0 1535.06 78.3475 1 1 12 0 1268.99 43.2600 1 2 12 0 105.766 3.07289 1 3 12 0 285.071 6.74219 1 4 12 0 1590.93 42.1593 1 5 12 0 1730.83 49.2731 1 6 12 0 447.152 13.5567 1 7 12 0 340.839 14.1413 1 0 13 0 0.82959 0.53168 1 1 13 0 298.772 10.6926 1 2 13 0 538.272 16.4346 1 3 13 0 389.764 10.7629 1 4 13 0 3.27395 0.37049 1 5 13 0 60.6579 2.05813 1 6 13 0 258.354 10.7883 1 7 13 0 56.3323 2.97809 1 0 14 0 126.893 5.34382 1 1 14 0 270.193 9.69997 1 2 14 0 3.62022 0.32889 1 3 14 0 71.3372 2.23009 1 4 14 0 153.396 5.31624 1 5 14 0 313.499 10.3674 1 6 14 0 74.1015 3.22584 1 0 15 0 0.58310 0.30522 1 1 15 0 789.732 26.6006 1 2 15 0 2234.84 68.2921 1 3 15 0 410.966 12.1320 1 4 15 0 60.4842 2.22668 1 5 15 0 380.814 13.9596 1 6 15 0 749.657 37.0501 1 0 16 0 508.015 22.5846 1 1 16 0 477.089 17.9268 1 2 16 0 1.96950 0.35084 1 3 16 0 273.899 8.13058 1 4 16 0 96.3870 3.66031 1 5 16 0 10.9424 0.66484 1 6 16 0 19.5517 1.23531 1 0 17 0 3.48254 0.48848 1 1 17 0 421.266 13.0238 1 2 17 0 647.699 23.6765 1 3 17 0 116.025 3.52789 1 4 17 0 50.1696 1.99989 1 5 17 0 241.270 8.87405 1 0 18 0 1158.16 66.0918 1 1 18 0 748.372 23.0309 1 2 18 0 112.720 3.76158 1 3 18 0 417.741 13.0703 1 4 18 0 667.985 24.3529 1 5 18 0 407.646 17.2109 1 0 19 0 1.21476 0.33590 1 1 19 0 36.7438 1.43951 1 2 19 0 21.0246 0.81362 1 3 19 0 187.588 6.46778 1 4 19 0 89.4500 3.37183 1 5 19 0 1.72066 0.35642 1 0 20 0 59.6757 2.92119 1 1 20 0 134.829 5.36517 1 2 20 0 7.73819 0.43123 1 3 20 0 84.8780 2.98340 1 4 20 0 309.646 13.1653 1 0 21 0 1.26574 0.32500 1 1 21 0 137.287 4.35214 1 2 21 0 643.755 20.1224 1 3 21 0 401.441 14.7173 1 0 22 0 279.199 15.0250 1 1 22 0 171.912 5.75025 1 2 22 0 2.01117 0.23964 1 3 22 0 180.496 9.06991 1 0 23 0 0.60719 0.28819 1 1 23 0 22.9420 0.92827 1 -8 0 1 2.67923 0.60123 1 -7 0 1 0.89992 0.54149 1 -6 0 1 0.72744 0.42490 1 -5 0 1 0.46195 0.30872 1 -4 0 1 1.44755 0.96641 1 -3 0 1 1.60675 0.42123 1 -2 0 1 1.62120 0.34337 1 -1 0 1 0.92289 0.28435 1 0 0 1 1.33876 0.23059 1 1 0 1 1.96182 0.30558 1 2 0 1 0.22225 0.27613 1 3 0 1 0.79853 1.01574 1 5 0 1 0.29245 0.52352 1 6 0 1 1.05485 0.60974 1 7 0 1 0.98210 0.54359 1 8 0 1 0.59923 0.41913 1 -8 1 1 413.872 15.8375 1 -7 1 1 152.996 4.71145 1 -6 1 1 146.645 4.52350 1 -5 1 1 81.7020 2.19889 1 -4 1 1 989.117 73.0391 1 -3 1 1 2209.20 120.849 1 -2 1 1 484.974 23.4228 1 -1 1 1 507.622 32.3994 1 0 1 1 4526.27 346.136 1 1 1 1 2843.56 160.021 1 2 1 1 14.0091 0.81056 1 3 1 1 1427.59 118.654 -2 3 1 1 1427.59 118.654 1 4 1 1 2561.12 185.370 -2 4 1 1 2561.12 185.370 1 5 1 1 460.394 11.8111 -2 5 1 1 460.394 11.8111 1 6 1 1 55.7587 1.80967 -2 6 1 1 55.7587 1.80967 1 7 1 1 853.066 27.5276 -2 7 1 1 853.066 27.5276 1 8 1 1 845.560 43.2617 -2 8 1 1 845.560 43.2617 1 -8 2 1 33.7418 1.71222 1 -7 1 1 705.737 48.3541 -2 -7 2 1 705.737 48.3541 1 -6 2 1 842.506 23.0197 1 -5 2 1 694.668 16.3078 1 -4 2 1 33.7544 2.88346 1 -3 2 1 1713.90 72.2236 1 -2 2 1 3757.67 158.225 1 -1 2 1 2564.97 118.133 1 0 2 1 257.875 16.4872 1 1 2 1 2140.56 93.4743 1 2 2 1 981.659 37.4976 1 3 2 1 733.939 34.7379 1 4 2 1 108.845 3.33573 -2 4 2 1 108.845 3.33573 1 5 2 1 765.446 24.5464 -2 5 2 1 765.446 24.5464 1 6 2 1 1437.26 46.0045 -2 6 2 1 1437.26 46.0045 1 7 2 1 2204.90 78.5612 -2 7 2 1 2204.90 78.5612 1 8 2 1 133.373 5.76266 -2 8 2 1 133.373 5.76266 1 -8 3 1 106.462 4.85699 1 -7 3 1 2.89546 0.33544 1 -6 3 1 15.8303 0.67480 1 -5 3 1 52.3372 1.33843 1 -4 3 1 12.1534 0.85640 1 -3 3 1 452.077 20.5764 1 -2 3 1 1370.70 57.7685 1 -1 3 1 558.984 28.9403 1 0 3 1 41.3571 2.17932 1 1 3 1 1.36603 0.20386 1 2 3 1 135.824 5.94013 1 3 3 1 501.069 23.7888 1 4 3 1 52.3214 1.33250 1 5 3 1 30.4292 0.81059 1 6 3 1 115.485 4.41610 -2 6 3 1 115.485 4.41610 1 7 3 1 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