_publ_contact_author 'Guochen Jia' _publ_contact_author_email 'chjiag@ust.hk' loop_ _publ_author_name 'Ran Lin, Ka Ho Lee, Herman Ho-Yung Sung, Ian Duncan Williams, Zhenyang Lin, Guochen Jia' _journal_name_full 'Organometallics' data_cpd6_ran27cult _audit_creation_date 2014-05-16 _audit_creation_method ; Olex2 1.2-beta (compiled May 9 2012 12:37:22, GUI svn.r4230) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H19 O8 Re' _chemical_formula_sum 'C24 H19 O8 Re' _chemical_formula_weight 621.59 _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' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 9.9323(2) _cell_length_b 8.46251(17) _cell_length_c 27.2348(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.0494(18) _cell_angle_gamma 90.00 _cell_volume 2276.40(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6230 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 75.3130 _cell_measurement_theta_min 4.4766 _exptl_absorpt_coefficient_mu 10.860 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.69712 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'red' _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'block' _exptl_crystal_F_000 1208 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_unetI/netI 0.0265 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_number 9371 _diffrn_reflns_theta_full 66.50 _diffrn_reflns_theta_max 75.45 _diffrn_reflns_theta_min 4.48 _diffrn_ambient_temperature 100.00(10) _diffrn_detector_area_resol_mean 10.3587 _diffrn_measured_fraction_theta_full 0.9868 _diffrn_measured_fraction_theta_max 0.9503 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 33.00 82.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -30.0000 90.0000 49 #__ type_ start__ end____ width___ exp.time_ 2 omega -115.00 -21.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -40.8203 -57.0000 -30.0000 94 #__ type_ start__ end____ width___ exp.time_ 3 omega -92.00 -2.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -40.8203 125.0000 120.0000 90 #__ type_ start__ end____ width___ exp.time_ 4 omega 78.00 178.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 77.0000 90.0000 100 #__ type_ start__ end____ width___ exp.time_ 5 omega 36.00 98.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -45.0000 0.0000 62 #__ type_ start__ end____ width___ exp.time_ 6 omega 34.00 69.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -111.0000 -60.0000 35 #__ type_ start__ end____ width___ exp.time_ 7 omega 74.00 112.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -111.0000 -60.0000 38 #__ type_ start__ end____ width___ exp.time_ 8 omega 36.00 98.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -45.0000 150.0000 62 #__ type_ start__ end____ width___ exp.time_ 9 omega 70.00 107.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -94.0000 30.0000 37 #__ type_ start__ end____ width___ exp.time_ 10 omega 26.00 53.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -94.0000 30.0000 27 #__ type_ start__ end____ width___ exp.time_ 11 omega -117.00 -56.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -40.8203 -37.0000 60.0000 61 #__ type_ start__ end____ width___ exp.time_ 12 omega -120.00 -7.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -40.8203 -77.0000 -150.0000 113 ; _diffrn_measurement_device 'kappa diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0711402000 _diffrn_orient_matrix_UB_12 0.1552353000 _diffrn_orient_matrix_UB_13 0.0116859000 _diffrn_orient_matrix_UB_21 0.0580689000 _diffrn_orient_matrix_UB_22 0.0806121000 _diffrn_orient_matrix_UB_23 -0.0439207000 _diffrn_orient_matrix_UB_31 -0.1259958000 _diffrn_orient_matrix_UB_32 -0.0505267000 _diffrn_orient_matrix_UB_33 -0.0342286000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 0.80 _diffrn_source_power 0.040 _diffrn_source_target Cu _diffrn_source_voltage 50 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4169 _reflns_number_total 4451 _reflns_odcompleteness_completeness 98.68 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 68.13 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.496 _refine_diff_density_min -0.873 _refine_diff_density_rms 0.095 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 301 _refine_ls_number_reflns 4451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0227 _refine_ls_R_factor_gt 0.0205 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.0505 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Re1 Re 0.772248(10) 0.132557(12) 0.414220(3) 0.01107(5) Uani 1 1 d . . . O1 O 0.3033(2) 0.3832(2) 0.35409(7) 0.0207(4) Uani 1 1 d . . . O2 O 0.4151(2) 0.6037(2) 0.37980(7) 0.0221(4) Uani 1 1 d . . . O3 O 0.36738(19) 0.3860(2) 0.46634(7) 0.0164(4) Uani 1 1 d . . . O5 O 0.74064(18) 0.0619(2) 0.51865(6) 0.0150(3) Uani 1 1 d . . . O6 O 0.5683(2) -0.1190(2) 0.36595(8) 0.0256(5) Uani 1 1 d . . . O7 O 0.9123(2) 0.1346(2) 0.31675(8) 0.0282(5) Uani 1 1 d . . . O8 O 0.9540(2) -0.1398(2) 0.46041(7) 0.0200(4) Uani 1 1 d . . . O9 O 0.9808(2) 0.3919(2) 0.45484(8) 0.0273(5) Uani 1 1 d . . . C1 C 0.6175(2) 0.2999(3) 0.38435(9) 0.0112(5) Uani 1 1 d . . . C2 C 0.5087(3) 0.3511(3) 0.40574(9) 0.0134(5) Uani 1 1 d . . . C3 C 0.4822(2) 0.3161(3) 0.45596(9) 0.0131(5) Uani 1 1 d . . . C4 C 0.5590(2) 0.2258(3) 0.49058(9) 0.0140(5) Uani 1 1 d . . . H4 H 0.5304 0.2181 0.5227 0.017 Uiso 1 1 calc R . . C5 C 0.6766(3) 0.1446(3) 0.48124(9) 0.0134(5) Uani 1 1 d . . . C6 C 0.6411(3) -0.0301(3) 0.38416(9) 0.0158(5) Uani 1 1 d . . . C7 C 0.8599(3) 0.1345(3) 0.35185(10) 0.0178(6) Uani 1 1 d . . . C8 C 0.8914(3) -0.0369(3) 0.44371(9) 0.0160(5) Uani 1 1 d . . . C9 C 0.9041(3) 0.2988(3) 0.44082(9) 0.0169(5) Uani 1 1 d . . . C11 C 0.6229(3) 0.3425(3) 0.33122(9) 0.0145(5) Uani 1 1 d . . . C12 C 0.5503(3) 0.2551(3) 0.29507(9) 0.0175(5) Uani 1 1 d . . . H12 H 0.4873 0.1791 0.3043 0.021 Uiso 1 1 calc R . . C13 C 0.5666(3) 0.2748(3) 0.24451(10) 0.0214(6) Uani 1 1 d . . . H13 H 0.5144 0.2134 0.2202 0.026 Uiso 1 1 calc R . . C14 C 0.6587(3) 0.3839(3) 0.23063(9) 0.0202(6) Uani 1 1 d . . . H14 H 0.6731 0.3939 0.1968 0.024 Uiso 1 1 calc R . . C15 C 0.7317(3) 0.4808(3) 0.26627(9) 0.0175(5) Uani 1 1 d . . . C16 C 0.8239(3) 0.5972(3) 0.25269(10) 0.0219(6) Uani 1 1 d . . . H16 H 0.8376 0.6097 0.2189 0.026 Uiso 1 1 calc R . . C17 C 0.8935(3) 0.6915(3) 0.28739(11) 0.0239(6) Uani 1 1 d . . . H17 H 0.9545 0.7691 0.2776 0.029 Uiso 1 1 calc R . . C18 C 0.8748(3) 0.6736(3) 0.33762(10) 0.0205(5) Uani 1 1 d . . . H18 H 0.9233 0.7391 0.3617 0.025 Uiso 1 1 calc R . . C19 C 0.7868(3) 0.5620(3) 0.35203(9) 0.0156(5) Uani 1 1 d . . . H19 H 0.7746 0.5520 0.3860 0.019 Uiso 1 1 calc R . . C20 C 0.7141(2) 0.4616(3) 0.31730(8) 0.0133(5) Uani 1 1 d . . . C21 C 0.4059(3) 0.4618(3) 0.37896(9) 0.0154(5) Uani 1 1 d . . . C22 C 0.1994(3) 0.4805(4) 0.32826(12) 0.0322(7) Uani 1 1 d . . . H22A H 0.2373 0.5382 0.3017 0.048 Uiso 1 1 calc R . . H22B H 0.1657 0.5560 0.3514 0.048 Uiso 1 1 calc R . . H22C H 0.1246 0.4135 0.3142 0.048 Uiso 1 1 calc R . . C31 C 0.3142(3) 0.3534(3) 0.51271(10) 0.0188(6) Uani 1 1 d . . . H31A H 0.2268 0.4067 0.5133 0.028 Uiso 1 1 calc R . . H31B H 0.3777 0.3923 0.5400 0.028 Uiso 1 1 calc R . . H31C H 0.3020 0.2392 0.5162 0.028 Uiso 1 1 calc R . . C51 C 0.6924(3) 0.0576(3) 0.56748(9) 0.0159(5) Uani 1 1 d . . . H51A H 0.6007 0.0108 0.5655 0.019 Uiso 1 1 calc R . . H51B H 0.6888 0.1656 0.5812 0.019 Uiso 1 1 calc R . . C52 C 0.7919(3) -0.0429(3) 0.59960(9) 0.0221(6) Uani 1 1 d . . . H52A H 0.8109 -0.1398 0.5819 0.033 Uiso 1 1 calc R . . H52B H 0.7532 -0.0703 0.6301 0.033 Uiso 1 1 calc R . . H52C H 0.8762 0.0162 0.6076 0.033 Uiso 1 1 calc R . . 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 Re1 0.01085(7) 0.01466(7) 0.00792(6) 0.00033(4) 0.00202(4) 0.00039(4) O1 0.0173(10) 0.0185(9) 0.0252(10) -0.0001(7) -0.0028(8) 0.0029(7) O2 0.0243(10) 0.0151(9) 0.0268(10) 0.0023(8) 0.0031(8) 0.0008(8) O3 0.0154(9) 0.0213(9) 0.0133(8) 0.0007(7) 0.0057(7) 0.0038(7) O5 0.0157(9) 0.0210(9) 0.0086(7) 0.0017(7) 0.0033(6) 0.0014(7) O6 0.0243(11) 0.0262(11) 0.0259(11) -0.0037(8) 0.0006(9) -0.0080(8) O7 0.0276(12) 0.0409(13) 0.0179(10) 0.0058(8) 0.0111(9) 0.0088(9) O8 0.0211(11) 0.0188(10) 0.0198(10) 0.0045(7) 0.0006(8) 0.0043(7) O9 0.0273(11) 0.0237(10) 0.0291(11) 0.0017(9) -0.0050(9) -0.0081(9) C1 0.0110(11) 0.0103(11) 0.0122(11) 0.0003(9) 0.0006(9) 0.0015(9) C2 0.0154(13) 0.0124(11) 0.0123(11) 0.0010(9) 0.0008(9) -0.0036(9) C3 0.0140(12) 0.0113(11) 0.0145(11) -0.0023(9) 0.0042(9) -0.0035(9) C4 0.0153(12) 0.0176(12) 0.0095(10) -0.0004(9) 0.0041(9) -0.0008(10) C5 0.0173(13) 0.0141(11) 0.0087(11) 0.0004(8) 0.0013(9) -0.0041(9) C6 0.0169(13) 0.0170(12) 0.0139(11) 0.0009(10) 0.0035(10) 0.0015(10) C7 0.0177(14) 0.0212(14) 0.0149(12) 0.0027(10) 0.0034(10) 0.0029(10) C8 0.0142(12) 0.0191(12) 0.0151(11) -0.0016(10) 0.0037(9) -0.0039(10) C9 0.0156(13) 0.0174(12) 0.0175(12) 0.0024(10) 0.0012(10) 0.0017(10) C11 0.0149(13) 0.0173(11) 0.0112(11) 0.0021(9) 0.0021(9) 0.0043(10) C12 0.0173(13) 0.0215(13) 0.0135(12) 0.0041(10) 0.0006(10) -0.0007(10) C13 0.0246(14) 0.0249(13) 0.0144(12) -0.0025(10) 0.0006(10) -0.0025(11) C14 0.0244(15) 0.0278(14) 0.0081(11) 0.0028(10) 0.0001(10) -0.0005(11) C15 0.0160(13) 0.0227(13) 0.0140(12) 0.0014(10) 0.0024(9) 0.0042(10) C16 0.0228(14) 0.0300(14) 0.0134(12) 0.0040(11) 0.0046(10) -0.0021(12) C17 0.0221(14) 0.0255(14) 0.0241(14) 0.0057(12) 0.0025(11) -0.0068(12) C18 0.0215(14) 0.0194(12) 0.0205(13) -0.0018(11) 0.0021(11) -0.0021(11) C19 0.0172(12) 0.0179(12) 0.0117(11) 0.0007(9) 0.0012(9) 0.0022(10) C20 0.0125(12) 0.0168(11) 0.0107(11) 0.0026(9) 0.0023(9) 0.0049(9) C21 0.0158(12) 0.0185(12) 0.0129(11) 0.0000(9) 0.0059(9) 0.0012(10) C22 0.0238(16) 0.0286(16) 0.0407(18) 0.0030(14) -0.0129(13) 0.0065(12) C31 0.0173(14) 0.0244(14) 0.0165(13) 0.0000(10) 0.0096(11) -0.0012(10) C51 0.0162(12) 0.0221(13) 0.0103(11) 0.0016(9) 0.0059(9) 0.0002(10) C52 0.0258(15) 0.0284(14) 0.0124(11) 0.0058(10) 0.0031(10) 0.0042(12) _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 Re1 C1 2.183(2) . ? Re1 C5 2.147(3) . ? Re1 C6 2.010(3) . ? Re1 C7 1.989(3) . ? Re1 C8 1.975(3) . ? Re1 C9 2.005(3) . ? O1 C21 1.340(3) . ? O1 C22 1.444(3) . ? O2 C21 1.204(3) . ? O3 C3 1.341(3) . ? O3 C31 1.446(3) . ? O5 C5 1.340(3) . ? O5 C51 1.460(3) . ? O6 C6 1.122(3) . ? O7 C7 1.136(4) . ? O8 C8 1.137(3) . ? O9 C9 1.134(3) . ? C1 C2 1.352(3) . ? C1 C11 1.498(3) . ? C2 C3 1.451(3) . ? C2 C21 1.514(3) . ? C3 C4 1.380(3) . ? C4 C5 1.401(4) . ? C11 C12 1.373(4) . ? C11 C20 1.433(4) . ? C12 C13 1.413(3) . ? C13 C14 1.381(4) . ? C14 C15 1.411(4) . ? C15 C16 1.421(4) . ? C15 C20 1.428(3) . ? C16 C17 1.368(4) . ? C17 C18 1.408(4) . ? C18 C19 1.371(4) . ? C19 C20 1.412(3) . ? C51 C52 1.511(4) . ? 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 C5 Re1 C1 85.91(9) . . ? C6 Re1 C1 83.78(10) . . ? C6 Re1 C5 93.03(10) . . ? C7 Re1 C1 91.76(10) . . ? C7 Re1 C5 176.78(10) . . ? C7 Re1 C6 88.93(11) . . ? C7 Re1 C9 88.54(11) . . ? C8 Re1 C1 172.11(9) . . ? C8 Re1 C5 89.35(10) . . ? C8 Re1 C6 90.19(11) . . ? C8 Re1 C7 93.21(10) . . ? C8 Re1 C9 91.25(11) . . ? C9 Re1 C1 94.99(10) . . ? C9 Re1 C5 89.45(10) . . ? C9 Re1 C6 177.15(10) . . ? C21 O1 C22 115.5(2) . . ? C3 O3 C31 119.8(2) . . ? C5 O5 C51 122.0(2) . . ? C2 C1 Re1 127.66(18) . . ? C2 C1 C11 116.8(2) . . ? C11 C1 Re1 114.86(16) . . ? C1 C2 C3 125.0(2) . . ? C1 C2 C21 121.3(2) . . ? C3 C2 C21 113.6(2) . . ? O3 C3 C2 110.6(2) . . ? O3 C3 C4 121.4(2) . . ? C4 C3 C2 128.0(2) . . ? C3 C4 C5 124.0(2) . . ? O5 C5 Re1 113.85(18) . . ? O5 C5 C4 117.1(2) . . ? C4 C5 Re1 129.02(18) . . ? O6 C6 Re1 177.8(2) . . ? O7 C7 Re1 178.6(3) . . ? O8 C8 Re1 176.2(2) . . ? O9 C9 Re1 178.1(2) . . ? C12 C11 C1 119.6(2) . . ? C12 C11 C20 119.2(2) . . ? C20 C11 C1 120.9(2) . . ? C11 C12 C13 122.0(2) . . ? C14 C13 C12 119.5(3) . . ? C13 C14 C15 120.5(2) . . ? C14 C15 C16 121.5(2) . . ? C14 C15 C20 119.8(2) . . ? C16 C15 C20 118.7(2) . . ? C17 C16 C15 121.2(2) . . ? C16 C17 C18 119.9(3) . . ? C19 C18 C17 120.4(3) . . ? C18 C19 C20 121.3(2) . . ? C15 C20 C11 118.9(2) . . ? C19 C20 C11 122.6(2) . . ? C19 C20 C15 118.5(2) . . ? O1 C21 C2 112.0(2) . . ? O2 C21 O1 123.8(2) . . ? O2 C21 C2 124.2(2) . . ? O5 C51 C52 106.51(19) . . ? 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 Re1 C1 C2 C3 7.1(4) . . . . ? Re1 C1 C2 C21 -176.79(17) . . . . ? Re1 C1 C11 C12 90.5(3) . . . . ? Re1 C1 C11 C20 -82.6(3) . . . . ? O3 C3 C4 C5 177.2(2) . . . . ? C1 Re1 C5 O5 -175.99(18) . . . . ? C1 Re1 C5 C4 4.0(2) . . . . ? C1 Re1 C6 O6 63(6) . . . . ? C1 Re1 C7 O7 158(10) . . . . ? C1 Re1 C8 O8 19(4) . . . . ? C1 Re1 C9 O9 -107(8) . . . . ? C1 C2 C3 O3 179.1(2) . . . . ? C1 C2 C3 C4 -0.6(4) . . . . ? C1 C2 C21 O1 92.0(3) . . . . ? C1 C2 C21 O2 -87.9(3) . . . . ? C1 C11 C12 C13 -170.7(2) . . . . ? C1 C11 C20 C15 170.1(2) . . . . ? C1 C11 C20 C19 -10.4(4) . . . . ? C2 C1 C11 C12 -80.8(3) . . . . ? C2 C1 C11 C20 106.1(3) . . . . ? C2 C3 C4 C5 -3.2(4) . . . . ? C3 C2 C21 O1 -91.4(3) . . . . ? C3 C2 C21 O2 88.6(3) . . . . ? C3 C4 C5 Re1 -0.1(4) . . . . ? C3 C4 C5 O5 179.9(2) . . . . ? C5 Re1 C1 C2 -7.3(2) . . . . ? C5 Re1 C1 C11 -177.44(19) . . . . ? C5 Re1 C6 O6 149(6) . . . . ? C5 Re1 C7 O7 115(9) . . . . ? C5 Re1 C8 O8 72(3) . . . . ? C5 Re1 C9 O9 168(8) . . . . ? C5 O5 C51 C52 -178.5(2) . . . . ? C6 Re1 C1 C2 86.2(2) . . . . ? C6 Re1 C1 C11 -83.94(18) . . . . ? C6 Re1 C5 O5 100.47(18) . . . . ? C6 Re1 C5 C4 -79.6(2) . . . . ? C6 Re1 C7 O7 -118(10) . . . . ? C6 Re1 C8 O8 -21(3) . . . . ? C6 Re1 C9 O9 -42(9) . . . . ? C7 Re1 C1 C2 175.0(2) . . . . ? C7 Re1 C1 C11 4.79(19) . . . . ? C7 Re1 C5 O5 -132.3(17) . . . . ? C7 Re1 C5 C4 47.7(18) . . . . ? C7 Re1 C6 O6 -29(6) . . . . ? C7 Re1 C8 O8 -110(3) . . . . ? C7 Re1 C9 O9 -15(8) . . . . ? C8 Re1 C1 C2 45.9(8) . . . . ? C8 Re1 C1 C11 -124.3(6) . . . . ? C8 Re1 C5 O5 10.31(18) . . . . ? C8 Re1 C5 C4 -169.7(2) . . . . ? C8 Re1 C6 O6 -122(6) . . . . ? C8 Re1 C7 O7 -28(10) . . . . ? C8 Re1 C9 O9 78(8) . . . . ? C9 Re1 C1 C2 -96.4(2) . . . . ? C9 Re1 C1 C11 93.48(19) . . . . ? C9 Re1 C5 O5 -80.95(18) . . . . ? C9 Re1 C5 C4 99.0(2) . . . . ? C9 Re1 C6 O6 -1(8) . . . . ? C9 Re1 C7 O7 63(10) . . . . ? C9 Re1 C8 O8 162(3) . . . . ? C11 C1 C2 C3 177.1(2) . . . . ? C11 C1 C2 C21 -6.8(3) . . . . ? C11 C12 C13 C14 0.6(4) . . . . ? C12 C11 C20 C15 -3.0(4) . . . . ? C12 C11 C20 C19 176.5(2) . . . . ? C12 C13 C14 C15 -3.1(4) . . . . ? C13 C14 C15 C16 -178.1(3) . . . . ? C13 C14 C15 C20 2.5(4) . . . . ? C14 C15 C16 C17 179.5(3) . . . . ? C14 C15 C20 C11 0.6(4) . . . . ? C14 C15 C20 C19 -179.0(2) . . . . ? C15 C16 C17 C18 0.3(5) . . . . ? C16 C15 C20 C11 -178.9(2) . . . . ? C16 C15 C20 C19 1.5(4) . . . . ? C16 C17 C18 C19 -0.1(5) . . . . ? C17 C18 C19 C20 0.6(4) . . . . ? C18 C19 C20 C11 179.1(2) . . . . ? C18 C19 C20 C15 -1.3(4) . . . . ? C20 C11 C12 C13 2.5(4) . . . . ? C20 C15 C16 C17 -1.1(4) . . . . ? C21 C2 C3 O3 2.7(3) . . . . ? C21 C2 C3 C4 -177.0(2) . . . . ? C22 O1 C21 O2 -1.2(4) . . . . ? C22 O1 C21 C2 178.9(2) . . . . ? C31 O3 C3 C2 173.6(2) . . . . ? C31 O3 C3 C4 -6.7(3) . . . . ? C51 O5 C5 Re1 178.96(16) . . . . ? C51 O5 C5 C4 -1.0(3) . . . . ? data_cpd8_ran28cult _audit_creation_date 2014-05-16 _audit_creation_method ; Olex2 1.2-beta (compiled May 9 2012 12:37:22, GUI svn.r4230) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H24 N O8 Re' _chemical_formula_sum 'C30 H24 N O8 Re' _chemical_formula_weight 712.70 _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' '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' 'Re' 'Re' -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _space_group_IT_number 2 _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 8.9083(5) _cell_length_b 10.5379(5) _cell_length_c 14.6963(6) _cell_angle_alpha 83.227(4) _cell_angle_beta 79.640(4) _cell_angle_gamma 88.482(4) _cell_volume 1347.62(11) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4727 _cell_measurement_temperature 99.93(16) _cell_measurement_theta_max 74.2520 _cell_measurement_theta_min 4.9390 _exptl_absorpt_coefficient_mu 9.278 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.89997 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'yellow' _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'block' _exptl_crystal_F_000 700 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_unetI/netI 0.0453 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 8023 _diffrn_reflns_theta_full 66.50 _diffrn_reflns_theta_max 75.00 _diffrn_reflns_theta_min 4.22 _diffrn_ambient_temperature 99.93(16) _diffrn_detector_area_resol_mean 10.3587 _diffrn_measured_fraction_theta_full 0.9872 _diffrn_measured_fraction_theta_max 0.5401 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 81.00 177.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 30.0000 -180.0000 96 #__ type_ start__ end____ width___ exp.time_ 2 omega -47.00 35.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -40.6953 37.0000 -60.0000 82 #__ type_ start__ end____ width___ exp.time_ 3 omega -92.00 -10.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -40.6953 125.0000 -90.0000 82 #__ type_ start__ end____ width___ exp.time_ 4 omega -115.00 -13.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -40.6953 -57.0000 150.0000 102 #__ type_ start__ end____ width___ exp.time_ 5 omega -36.00 69.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 40.6953 -77.0000 60.0000 105 #__ type_ start__ end____ width___ exp.time_ 6 omega 75.00 108.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -94.0000 -180.0000 33 #__ type_ start__ end____ width___ exp.time_ 7 omega 80.00 178.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 30.0000 -90.0000 98 #__ type_ start__ end____ width___ exp.time_ 8 omega 36.00 96.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -45.0000 -60.0000 60 #__ type_ start__ end____ width___ exp.time_ 9 omega 38.00 98.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -45.0000 -120.0000 60 #__ type_ start__ end____ width___ exp.time_ 10 omega 49.00 112.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -111.0000 90.0000 63 #__ type_ start__ end____ width___ exp.time_ 11 omega 37.00 141.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -61.0000 90.0000 104 #__ type_ start__ end____ width___ exp.time_ 12 omega 33.00 90.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -30.0000 0.0000 57 #__ type_ start__ end____ width___ exp.time_ 13 omega 32.00 115.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -111.0000 -60.0000 83 ; _diffrn_measurement_device 'kappa diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.1726027000 _diffrn_orient_matrix_UB_12 -0.0148859000 _diffrn_orient_matrix_UB_13 -0.0347516000 _diffrn_orient_matrix_UB_21 0.0196197000 _diffrn_orient_matrix_UB_22 0.1456125000 _diffrn_orient_matrix_UB_23 -0.0050319000 _diffrn_orient_matrix_UB_31 0.0270250000 _diffrn_orient_matrix_UB_32 -0.0158019000 _diffrn_orient_matrix_UB_33 0.1013684000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 0.80 _diffrn_source_power 0.040 _diffrn_source_target Cu _diffrn_source_voltage 50 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4742 _reflns_number_total 5209 _reflns_odcompleteness_completeness 98.72 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 68.13 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 1.163 _refine_diff_density_min -1.211 _refine_diff_density_rms 0.109 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 364 _refine_ls_number_reflns 5209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0352 _refine_ls_R_factor_gt 0.0299 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+0.5659P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0713 _refine_ls_wR_factor_ref 0.0740 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Re1 Re 0.210565(19) 0.527584(16) 0.152849(12) 0.02298(7) Uani 1 1 d . . . O6 O 0.5211(4) 0.6612(3) 0.0642(2) 0.0399(8) Uani 1 1 d . . . O7 O 0.1612(4) 0.4430(4) -0.0349(2) 0.0413(8) Uani 1 1 d . . . O8 O 0.0264(4) 0.7793(3) 0.1219(2) 0.0352(7) Uani 1 1 d . . . O9 O -0.0777(4) 0.3907(3) 0.2727(3) 0.0419(8) Uani 1 1 d . . . O31 O -0.1299(4) 0.9876(3) 0.4263(2) 0.0370(7) Uani 1 1 d . . . O41 O 0.3735(4) 0.1983(3) 0.3631(2) 0.0327(7) Uani 1 1 d . . . O51 O 0.6936(4) 0.5024(4) 0.4442(2) 0.0400(8) Uani 1 1 d . . . O52 O 0.6182(4) 0.5415(3) 0.3064(2) 0.0341(7) Uani 1 1 d . . . N1 N 0.2549(4) 0.5682(3) 0.3660(2) 0.0247(7) Uani 1 1 d . . . H1 H 0.2952 0.5333 0.4118 0.030 Uiso 1 1 calc R . . C1 C 0.3414(5) 0.3614(4) 0.1967(3) 0.0257(8) Uani 1 1 d . . . C2 C 0.3687(5) 0.3960(4) 0.2790(3) 0.0252(8) Uani 1 1 d . . . C3 C 0.2838(4) 0.5162(4) 0.2877(3) 0.0239(8) Uani 1 1 d . . . C4 C 0.4363(5) 0.3167(4) 0.3517(3) 0.0279(8) Uani 1 1 d . . . C5 C 0.5399(5) 0.3501(4) 0.4006(3) 0.0298(9) Uani 1 1 d . . . H5 H 0.5614 0.2893 0.4478 0.036 Uiso 1 1 calc R . . C6 C 0.4092(5) 0.6129(4) 0.0938(3) 0.0267(8) Uani 1 1 d . . . C7 C 0.1775(5) 0.4771(4) 0.0336(3) 0.0305(9) Uani 1 1 d . . . C8 C 0.0950(5) 0.6867(4) 0.1340(3) 0.0271(8) Uani 1 1 d . . . C9 C 0.0244(5) 0.4394(4) 0.2271(3) 0.0304(9) Uani 1 1 d . . . C11 C 0.3810(5) 0.2370(4) 0.1619(3) 0.0297(9) Uani 1 1 d . . . C12 C 0.2679(5) 0.1601(4) 0.1449(3) 0.0332(9) Uani 1 1 d . . . H12 H 0.1698 0.1939 0.1485 0.040 Uiso 1 1 calc R . . C13 C 0.2913(6) 0.0365(5) 0.1229(4) 0.0441(12) Uani 1 1 d . . . H13 H 0.2101 -0.0125 0.1153 0.053 Uiso 1 1 calc R . . C14 C 0.4391(7) -0.0135(5) 0.1123(4) 0.0439(12) Uani 1 1 d . . . H14 H 0.4570 -0.0974 0.0994 0.053 Uiso 1 1 calc R . . C15 C 0.5610(6) 0.0636(4) 0.1213(3) 0.0337(9) Uani 1 1 d . . . C16 C 0.7151(7) 0.0182(6) 0.1035(4) 0.0511(14) Uani 1 1 d . . . H16 H 0.7337 -0.0660 0.0914 0.061 Uiso 1 1 calc R . . C17 C 0.8346(6) 0.0948(6) 0.1038(4) 0.0527(14) Uani 1 1 d . . . H17 H 0.9340 0.0642 0.0904 0.063 Uiso 1 1 calc R . . C18 C 0.8068(6) 0.2219(5) 0.1245(4) 0.0440(12) Uani 1 1 d . . . H18 H 0.8894 0.2752 0.1220 0.053 Uiso 1 1 calc R . . C19 C 0.6609(5) 0.2691(4) 0.1484(3) 0.0319(9) Uani 1 1 d . . . H19 H 0.6452 0.3512 0.1656 0.038 Uiso 1 1 calc R . . C20 C 0.5340(5) 0.1894(4) 0.1462(3) 0.0316(9) Uani 1 1 d . . . C31 C 0.1610(5) 0.6791(4) 0.3803(3) 0.0254(8) Uani 1 1 d . . . C32 C 0.0495(5) 0.6778(4) 0.4599(3) 0.0302(9) Uani 1 1 d . . . H32 H 0.0396 0.6069 0.5047 0.036 Uiso 1 1 calc R . . C33 C -0.0460(5) 0.7814(4) 0.4725(3) 0.0320(9) Uani 1 1 d . . . H33 H -0.1219 0.7796 0.5251 0.038 Uiso 1 1 calc R . . C34 C -0.0299(5) 0.8888(4) 0.4071(3) 0.0299(9) Uani 1 1 d . . . C35 C 0.0827(6) 0.8914(4) 0.3290(3) 0.0350(10) Uani 1 1 d . . . H35 H 0.0946 0.9632 0.2852 0.042 Uiso 1 1 calc R . . C36 C 0.1783(5) 0.7863(4) 0.3162(3) 0.0300(9) Uani 1 1 d . . . H36 H 0.2547 0.7885 0.2638 0.036 Uiso 1 1 calc R . . C37 C -0.1106(6) 1.0997(5) 0.3608(4) 0.0438(12) Uani 1 1 d . . . H37A H -0.1330 1.0805 0.3024 0.066 Uiso 1 1 calc R . . H37B H -0.0072 1.1287 0.3521 0.066 Uiso 1 1 calc R . . H37C H -0.1787 1.1654 0.3839 0.066 Uiso 1 1 calc R . . C41 C 0.4410(6) 0.0954(5) 0.4138(4) 0.0420(11) Uani 1 1 d . . . H41A H 0.5497 0.0965 0.3934 0.063 Uiso 1 1 calc R . . H41B H 0.4011 0.0159 0.4030 0.063 Uiso 1 1 calc R . . H41C H 0.4179 0.1045 0.4790 0.063 Uiso 1 1 calc R . . C51 C 0.6225(5) 0.4704(4) 0.3882(3) 0.0307(9) Uani 1 1 d . . . C52 C 0.7106(6) 0.6577(5) 0.2843(4) 0.0442(12) Uani 1 1 d . . . H52A H 0.7407 0.6754 0.2173 0.053 Uiso 1 1 calc R . . H52B H 0.8025 0.6444 0.3110 0.053 Uiso 1 1 calc R . . C53 C 0.6249(7) 0.7687(5) 0.3211(5) 0.0561(15) Uani 1 1 d . . . H53A H 0.5305 0.7783 0.2982 0.084 Uiso 1 1 calc R . . H53B H 0.6847 0.8446 0.3012 0.084 Uiso 1 1 calc R . . H53C H 0.6041 0.7549 0.3879 0.084 Uiso 1 1 calc R . . 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 Re1 0.02178(10) 0.02371(10) 0.02322(10) -0.00310(6) -0.00368(6) 0.00394(6) O6 0.0259(16) 0.0437(19) 0.0421(19) 0.0060(15) 0.0083(14) -0.0024(14) O7 0.0337(17) 0.056(2) 0.0386(19) -0.0213(16) -0.0110(15) 0.0123(15) O8 0.0322(16) 0.0281(15) 0.0449(19) -0.0016(13) -0.0086(14) 0.0106(13) O9 0.0298(17) 0.0381(17) 0.052(2) -0.0065(15) 0.0112(15) -0.0089(14) O31 0.0344(16) 0.0343(16) 0.0402(19) -0.0079(14) -0.0006(14) 0.0129(13) O41 0.0331(16) 0.0269(15) 0.0317(16) 0.0073(12) 0.0036(13) 0.0050(12) O51 0.0318(16) 0.058(2) 0.0324(18) -0.0109(15) -0.0084(14) 0.0085(15) O52 0.0307(15) 0.0349(16) 0.0368(18) 0.0051(13) -0.0119(13) 0.0001(13) N1 0.0234(16) 0.0258(16) 0.0244(17) -0.0033(13) -0.0030(13) 0.0036(13) C1 0.029(2) 0.0204(18) 0.025(2) 0.0015(14) -0.0011(16) 0.0018(15) C2 0.0230(18) 0.0244(19) 0.026(2) 0.0003(15) 0.0007(15) 0.0008(15) C3 0.0209(17) 0.0195(17) 0.029(2) 0.0005(14) 0.0004(15) -0.0025(14) C4 0.028(2) 0.029(2) 0.023(2) -0.0006(16) 0.0054(16) 0.0057(16) C5 0.032(2) 0.034(2) 0.021(2) 0.0001(16) -0.0001(16) 0.0106(17) C6 0.028(2) 0.0278(19) 0.023(2) -0.0023(15) -0.0042(16) 0.0091(16) C7 0.027(2) 0.037(2) 0.030(2) -0.0090(18) -0.0100(17) 0.0083(17) C8 0.0239(19) 0.034(2) 0.023(2) -0.0043(16) -0.0036(16) -0.0011(16) C9 0.027(2) 0.027(2) 0.040(2) -0.0090(18) -0.0078(19) 0.0028(16) C11 0.032(2) 0.028(2) 0.026(2) 0.0005(16) -0.0003(17) 0.0037(16) C12 0.031(2) 0.034(2) 0.031(2) -0.0023(17) 0.0031(18) -0.0071(18) C13 0.052(3) 0.039(3) 0.038(3) -0.011(2) 0.005(2) -0.009(2) C14 0.061(3) 0.030(2) 0.037(3) -0.0014(19) 0.003(2) -0.003(2) C15 0.044(3) 0.027(2) 0.027(2) -0.0022(16) 0.0019(19) 0.0043(18) C16 0.059(3) 0.051(3) 0.045(3) -0.011(2) -0.012(3) 0.020(3) C17 0.041(3) 0.070(4) 0.050(3) -0.021(3) -0.010(2) 0.022(3) C18 0.043(3) 0.053(3) 0.036(3) -0.012(2) -0.007(2) 0.011(2) C19 0.029(2) 0.040(2) 0.026(2) -0.0011(17) -0.0064(17) -0.0004(18) C20 0.039(2) 0.031(2) 0.023(2) -0.0003(16) -0.0035(18) 0.0049(18) C31 0.0242(19) 0.0257(19) 0.026(2) -0.0048(15) -0.0024(16) 0.0021(15) C32 0.029(2) 0.029(2) 0.031(2) -0.0038(17) -0.0022(17) 0.0020(17) C33 0.027(2) 0.035(2) 0.032(2) -0.0095(18) 0.0034(17) 0.0014(17) C34 0.031(2) 0.030(2) 0.030(2) -0.0096(17) -0.0047(17) 0.0075(17) C35 0.045(3) 0.027(2) 0.030(2) -0.0008(17) -0.0006(19) 0.0069(19) C36 0.035(2) 0.027(2) 0.026(2) -0.0048(16) 0.0010(17) 0.0042(17) C37 0.049(3) 0.034(2) 0.049(3) -0.005(2) -0.010(2) 0.015(2) C41 0.048(3) 0.032(2) 0.041(3) 0.009(2) -0.003(2) 0.008(2) C51 0.027(2) 0.040(2) 0.024(2) -0.0078(17) -0.0005(16) 0.0117(17) C52 0.036(2) 0.043(3) 0.053(3) 0.007(2) -0.012(2) -0.003(2) C53 0.048(3) 0.046(3) 0.071(4) 0.000(3) -0.005(3) -0.004(2) _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 Re1 C1 2.176(4) . ? Re1 C3 2.184(4) . ? Re1 C6 2.010(4) . ? Re1 C7 1.964(4) . ? Re1 C8 1.963(4) . ? Re1 C9 1.999(4) . ? O6 C6 1.123(5) . ? O7 C7 1.142(5) . ? O8 C8 1.150(5) . ? O9 C9 1.124(6) . ? O31 C34 1.373(5) . ? O31 C37 1.427(6) . ? O41 C4 1.361(5) . ? O41 C41 1.424(5) . ? O51 C51 1.207(6) . ? O52 C51 1.346(5) . ? O52 C52 1.465(6) . ? N1 C3 1.313(5) . ? N1 C31 1.433(5) . ? C1 C2 1.368(6) . ? C1 C11 1.474(6) . ? C2 C3 1.464(5) . ? C2 C4 1.482(6) . ? C4 C5 1.344(6) . ? C5 C51 1.459(6) . ? C11 C12 1.384(6) . ? C11 C20 1.429(6) . ? C12 C13 1.380(7) . ? C13 C14 1.394(8) . ? C14 C15 1.407(7) . ? C15 C16 1.432(7) . ? C15 C20 1.419(6) . ? C16 C17 1.353(9) . ? C17 C18 1.414(8) . ? C18 C19 1.379(7) . ? C19 C20 1.433(6) . ? C31 C32 1.391(6) . ? C31 C36 1.376(6) . ? C32 C33 1.376(6) . ? C33 C34 1.388(6) . ? C34 C35 1.380(6) . ? C35 C36 1.388(6) . ? C52 C53 1.482(8) . ? 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 C1 Re1 C3 61.26(15) . . ? C6 Re1 C1 88.09(15) . . ? C6 Re1 C3 88.84(15) . . ? C7 Re1 C1 98.40(17) . . ? C7 Re1 C3 159.59(16) . . ? C7 Re1 C6 92.26(18) . . ? C7 Re1 C9 94.52(18) . . ? C8 Re1 C1 170.23(16) . . ? C8 Re1 C3 108.97(16) . . ? C8 Re1 C6 92.16(16) . . ? C8 Re1 C7 91.35(17) . . ? C8 Re1 C9 91.09(17) . . ? C9 Re1 C1 87.55(16) . . ? C9 Re1 C3 83.62(16) . . ? C9 Re1 C6 172.41(17) . . ? C34 O31 C37 116.3(4) . . ? C4 O41 C41 119.4(4) . . ? C51 O52 C52 117.6(4) . . ? C3 N1 C31 124.5(4) . . ? C2 C1 Re1 99.4(3) . . ? C2 C1 C11 125.5(4) . . ? C11 C1 Re1 134.8(3) . . ? C1 C2 C3 103.3(3) . . ? C1 C2 C4 127.7(4) . . ? C3 C2 C4 127.6(4) . . ? N1 C3 Re1 140.4(3) . . ? N1 C3 C2 122.5(4) . . ? C2 C3 Re1 95.9(3) . . ? O41 C4 C2 107.8(4) . . ? C5 C4 O41 123.6(4) . . ? C5 C4 C2 128.6(4) . . ? C4 C5 C51 127.6(4) . . ? O6 C6 Re1 177.4(4) . . ? O7 C7 Re1 177.1(4) . . ? O8 C8 Re1 179.0(4) . . ? O9 C9 Re1 176.6(4) . . ? C12 C11 C1 120.2(4) . . ? C12 C11 C20 117.3(4) . . ? C20 C11 C1 122.5(4) . . ? C13 C12 C11 124.3(5) . . ? C12 C13 C14 118.7(5) . . ? C13 C14 C15 119.7(5) . . ? C14 C15 C16 120.8(5) . . ? C14 C15 C20 120.7(5) . . ? C20 C15 C16 118.5(5) . . ? C17 C16 C15 121.6(5) . . ? C16 C17 C18 119.4(5) . . ? C19 C18 C17 121.9(5) . . ? C18 C19 C20 118.9(5) . . ? C11 C20 C19 121.3(4) . . ? C15 C20 C11 119.0(4) . . ? C15 C20 C19 119.5(4) . . ? C32 C31 N1 119.4(4) . . ? C36 C31 N1 121.1(4) . . ? C36 C31 C32 119.5(4) . . ? C33 C32 C31 120.0(4) . . ? C32 C33 C34 120.5(4) . . ? O31 C34 C33 116.0(4) . . ? O31 C34 C35 124.3(4) . . ? C35 C34 C33 119.6(4) . . ? C34 C35 C36 119.8(4) . . ? C31 C36 C35 120.6(4) . . ? O51 C51 O52 122.2(4) . . ? O51 C51 C5 123.7(4) . . ? O52 C51 C5 114.1(4) . . ? O52 C52 C53 111.3(4) . . ? data_cpd10_ran31cult _audit_creation_date 2014-05-16 _audit_creation_method ; Olex2 1.2-beta (compiled May 9 2012 12:37:22, GUI svn.r4230) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C26 H23 O8 Re' _chemical_formula_sum 'C26 H23 O8 Re' _chemical_formula_weight 649.64 _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' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M I2/a _space_group_IT_number 15 _space_group_name_Hall '-I 2ya' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y, -z' 3 'x+1/2, y+1/2, z+1/2' 4 '-x+1, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x-1/2, -y, z' 7 '-x+1/2, -y+1/2, -z+1/2' 8 'x, -y+1/2, z+1/2' _cell_length_a 21.2127(7) _cell_length_b 8.8364(2) _cell_length_c 27.3229(9) _cell_angle_alpha 90.00 _cell_angle_beta 106.562(3) _cell_angle_gamma 90.00 _cell_volume 4909.0(3) _cell_formula_units_Z 8 _cell_measurement_reflns_used 6403 _cell_measurement_temperature 100.0(2) _cell_measurement_theta_max 74.8390 _cell_measurement_theta_min 5.2470 _exptl_absorpt_coefficient_mu 10.101 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.52064 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'red' _exptl_crystal_density_diffrn 1.758 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'needle' _exptl_crystal_F_000 2544 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_unetI/netI 0.0403 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 10023 _diffrn_reflns_theta_full 66.50 _diffrn_reflns_theta_max 67.98 _diffrn_reflns_theta_min 4.35 _diffrn_ambient_temperature 100.0(2) _diffrn_detector_area_resol_mean 10.3587 _diffrn_measured_fraction_theta_full 0.9903 _diffrn_measured_fraction_theta_max 0.6694 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 45.00 98.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -45.0000 -60.0000 53 #__ type_ start__ end____ width___ exp.time_ 2 omega -107.00 -12.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -40.9453 -57.0000 120.0000 95 #__ type_ start__ end____ width___ exp.time_ 3 omega -96.00 -35.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -40.9453 125.0000 60.0000 61 #__ type_ start__ end____ width___ exp.time_ 4 omega 27.00 82.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 40.9453 -99.0000 -60.0000 55 #__ type_ start__ end____ width___ exp.time_ 5 omega 37.00 85.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -45.0000 -120.0000 48 #__ type_ start__ end____ width___ exp.time_ 6 omega 26.00 107.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -94.0000 -120.0000 81 #__ type_ start__ end____ width___ exp.time_ 7 omega 80.00 175.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 61.0000 60.0000 95 #__ type_ start__ end____ width___ exp.time_ 8 omega 32.00 113.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -111.0000 -180.0000 81 #__ type_ start__ end____ width___ exp.time_ 9 omega -117.00 -15.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -40.9453 -37.0000 0.0000 102 #__ type_ start__ end____ width___ exp.time_ 10 omega -120.00 -7.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -40.9453 -77.0000 -60.0000 113 #__ type_ start__ end____ width___ exp.time_ 11 omega 49.00 83.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 15.0000 -60.0000 34 ; _diffrn_measurement_device 'kappa diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0208968000 _diffrn_orient_matrix_UB_12 -0.1309814000 _diffrn_orient_matrix_UB_13 -0.0292660000 _diffrn_orient_matrix_UB_21 -0.0728284000 _diffrn_orient_matrix_UB_22 -0.0356130000 _diffrn_orient_matrix_UB_23 -0.0265657000 _diffrn_orient_matrix_UB_31 0.0012904000 _diffrn_orient_matrix_UB_32 0.1094346000 _diffrn_orient_matrix_UB_33 -0.0435327000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 0.80 _diffrn_source_power 0.040 _diffrn_source_target Cu _diffrn_source_voltage 50 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 3927 _reflns_number_total 4407 _reflns_odcompleteness_completeness 99.03 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 68.13 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 1.624 _refine_diff_density_min -1.270 _refine_diff_density_rms 0.119 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 319 _refine_ls_number_reflns 4407 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0314 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0811 _refine_ls_wR_factor_ref 0.0844 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Re1 Re 0.357892(8) 0.10269(2) 0.369352(6) 0.02018(9) Uani 1 1 d . . . O1 O 0.52897(16) 0.5595(4) 0.38807(13) 0.0325(7) Uani 1 1 d . . . O2 O 0.58424(15) 0.3487(4) 0.38101(12) 0.0288(7) Uani 1 1 d . . . O3 O 0.54904(15) 0.3564(4) 0.48159(11) 0.0300(7) Uani 1 1 d . . . O5 O 0.36377(16) 0.0625(4) 0.47834(12) 0.0353(8) Uani 1 1 d . . . O6 O 0.25175(17) 0.3466(5) 0.37052(14) 0.0424(9) Uani 1 1 d . . . O7 O 0.30006(18) 0.0862(4) 0.25035(13) 0.0367(8) Uani 1 1 d . . . O8 O 0.26341(17) -0.1459(4) 0.38743(14) 0.0398(8) Uani 1 1 d . . . O9 O 0.46811(17) -0.1332(4) 0.37003(14) 0.0348(8) Uani 1 1 d . . . C1 C 0.4335(2) 0.2609(5) 0.36229(16) 0.0248(9) Uani 1 1 d . . . C2 C 0.4834(2) 0.3186(5) 0.40032(16) 0.0222(8) Uani 1 1 d . . . C3 C 0.4953(2) 0.2866(5) 0.45435(15) 0.0242(9) Uani 1 1 d . . . C4 C 0.4574(2) 0.1989(5) 0.47704(16) 0.0244(9) Uani 1 1 d . . . H4 H 0.4719 0.1869 0.5131 0.029 Uiso 1 1 calc R . . C5 C 0.3994(2) 0.1271(5) 0.45044(16) 0.0235(9) Uani 1 1 d . . . C6 C 0.2910(2) 0.2603(5) 0.37010(16) 0.0246(9) Uani 1 1 d . . . C7 C 0.3218(2) 0.0922(5) 0.29353(17) 0.0244(10) Uani 1 1 d . . . C8 C 0.2977(2) -0.0535(6) 0.38030(17) 0.0279(10) Uani 1 1 d . . . C9 C 0.4275(2) -0.0518(6) 0.36929(16) 0.0269(9) Uani 1 1 d . . . C11 C 0.43433(19) 0.3003(5) 0.30882(16) 0.0232(9) Uani 1 1 d . . . C12 C 0.4664(2) 0.2095(5) 0.28300(17) 0.0269(9) Uani 1 1 d . . . H12 H 0.4901 0.1244 0.3000 0.032 Uiso 1 1 calc R . . C13 C 0.4653(2) 0.2380(5) 0.23197(17) 0.0282(9) Uani 1 1 d . . . H13 H 0.4878 0.1724 0.2151 0.034 Uiso 1 1 calc R . . C14 C 0.4317(2) 0.3607(6) 0.20681(17) 0.0288(10) Uani 1 1 d . . . H14 H 0.4306 0.3795 0.1723 0.035 Uiso 1 1 calc R . . C15 C 0.3981(2) 0.4607(5) 0.23219(15) 0.0248(9) Uani 1 1 d . . . C16 C 0.3662(2) 0.5933(5) 0.20844(18) 0.0304(11) Uani 1 1 d . . . H16 H 0.3662 0.6161 0.1745 0.036 Uiso 1 1 calc R . . C17 C 0.3356(2) 0.6880(6) 0.23302(17) 0.0325(10) Uani 1 1 d . . . H17 H 0.3135 0.7750 0.2160 0.039 Uiso 1 1 calc R . . C18 C 0.3364(2) 0.6580(5) 0.28405(18) 0.0283(10) Uani 1 1 d . . . H18 H 0.3150 0.7254 0.3013 0.034 Uiso 1 1 calc R . . C19 C 0.3677(2) 0.5325(5) 0.30874(17) 0.0254(9) Uani 1 1 d . . . H19 H 0.3680 0.5138 0.3430 0.031 Uiso 1 1 calc R . . C20 C 0.40015(19) 0.4291(5) 0.28363(16) 0.0228(9) Uani 1 1 d . . . C21 C 0.5336(2) 0.4244(5) 0.38934(17) 0.0242(9) Uani 1 1 d . . . C22 C 0.6338(2) 0.4426(6) 0.36912(19) 0.0338(11) Uani 1 1 d . . . H22A H 0.6160 0.4864 0.3350 0.051 Uiso 1 1 calc R . . H22B H 0.6725 0.3809 0.3699 0.051 Uiso 1 1 calc R . . H22C H 0.6464 0.5240 0.3944 0.051 Uiso 1 1 calc R . . C31 C 0.5772(2) 0.3281(6) 0.53573(16) 0.0301(10) Uani 1 1 d . . . H31A H 0.5890 0.2199 0.5417 0.036 Uiso 1 1 calc R . . H31B H 0.5450 0.3540 0.5545 0.036 Uiso 1 1 calc R . . C32 C 0.6373(2) 0.4250(6) 0.55368(19) 0.0344(11) Uani 1 1 d . . . H32A H 0.6237 0.5324 0.5521 0.041 Uiso 1 1 calc R . . H32B H 0.6596 0.4005 0.5898 0.041 Uiso 1 1 calc R . . C33 C 0.6853(3) 0.4056(7) 0.5232(2) 0.0479(15) Uani 1 1 d . . . H33A H 0.6637 0.4297 0.4873 0.072 Uiso 1 1 calc R . . H33B H 0.7009 0.3006 0.5260 0.072 Uiso 1 1 calc R . . H33C H 0.7228 0.4737 0.5364 0.072 Uiso 1 1 calc R . . C51 C 0.3833(3) 0.0738(7) 0.53434(19) 0.0454(14) Uani 1 1 d D . . H51A H 0.3910 0.1810 0.5449 0.054 Uiso 1 1 calc R . . H51B H 0.4245 0.0167 0.5491 0.054 Uiso 1 1 calc R . . C52 C 0.3299(4) 0.0106(15) 0.5528(2) 0.108(4) Uani 1 1 d D . . H52A H 0.3202 -0.0928 0.5399 0.163 Uiso 1 1 calc R . . H52B H 0.2904 0.0733 0.5405 0.163 Uiso 1 1 calc R . . H52C H 0.3436 0.0093 0.5902 0.163 Uiso 1 1 calc R . . 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 Re1 0.01997(12) 0.02222(13) 0.01735(13) 0.00186(6) 0.00372(8) -0.00158(6) O1 0.0296(16) 0.0252(17) 0.0409(19) 0.0065(15) 0.0069(14) 0.0016(14) O2 0.0266(15) 0.0280(16) 0.0337(17) -0.0039(14) 0.0114(13) -0.0044(13) O3 0.0304(17) 0.0349(17) 0.0187(15) 0.0050(13) -0.0025(13) -0.0068(14) O5 0.0288(16) 0.056(2) 0.0218(16) 0.0084(15) 0.0080(13) -0.0048(16) O6 0.0322(18) 0.051(2) 0.042(2) -0.0072(18) 0.0079(16) 0.0072(18) O7 0.0389(19) 0.044(2) 0.0229(18) -0.0001(14) 0.0021(15) -0.0095(15) O8 0.0344(18) 0.040(2) 0.044(2) 0.0109(17) 0.0089(16) -0.0098(17) O9 0.0316(18) 0.0344(18) 0.042(2) 0.0054(16) 0.0163(15) 0.0112(15) C1 0.025(2) 0.027(2) 0.021(2) 0.0058(18) 0.0036(17) 0.0041(18) C2 0.024(2) 0.020(2) 0.022(2) 0.0045(17) 0.0059(16) 0.0007(17) C3 0.026(2) 0.026(2) 0.019(2) 0.0012(17) 0.0018(16) 0.0040(17) C4 0.028(2) 0.027(2) 0.0166(19) 0.0033(17) 0.0036(16) 0.0045(18) C5 0.027(2) 0.030(2) 0.015(2) 0.0041(17) 0.0085(17) 0.0047(18) C6 0.0162(19) 0.028(2) 0.028(2) -0.0015(19) 0.0033(16) -0.0022(17) C7 0.027(2) 0.024(2) 0.020(2) -0.0003(16) 0.0032(18) -0.0030(17) C8 0.027(2) 0.029(2) 0.026(2) 0.000(2) 0.0048(18) 0.000(2) C9 0.030(2) 0.030(2) 0.021(2) 0.0010(19) 0.0075(18) -0.006(2) C11 0.0212(19) 0.026(2) 0.022(2) -0.0006(17) 0.0046(16) -0.0017(17) C12 0.028(2) 0.026(2) 0.029(2) -0.0030(19) 0.0132(18) -0.0004(18) C13 0.029(2) 0.030(2) 0.030(2) -0.0031(19) 0.0152(19) 0.0017(18) C14 0.029(2) 0.038(3) 0.022(2) -0.001(2) 0.0112(18) -0.003(2) C15 0.023(2) 0.029(2) 0.019(2) 0.0013(18) 0.0018(16) -0.0037(18) C16 0.030(2) 0.037(3) 0.022(2) 0.0082(18) 0.0048(19) 0.0012(19) C17 0.028(2) 0.036(3) 0.031(2) 0.007(2) 0.0049(19) 0.007(2) C18 0.027(2) 0.027(2) 0.031(2) 0.002(2) 0.0082(18) 0.0023(19) C19 0.025(2) 0.026(2) 0.025(2) -0.0008(18) 0.0060(17) -0.0013(17) C20 0.0163(18) 0.028(2) 0.022(2) 0.0026(18) 0.0022(16) -0.0064(17) C21 0.022(2) 0.026(2) 0.021(2) 0.0028(17) 0.0003(17) 0.0021(17) C22 0.029(2) 0.038(3) 0.038(3) -0.005(2) 0.015(2) -0.007(2) C31 0.037(2) 0.034(3) 0.015(2) 0.0015(18) -0.0009(18) 0.000(2) C32 0.035(3) 0.035(3) 0.028(3) 0.000(2) -0.001(2) 0.002(2) C33 0.040(3) 0.071(4) 0.027(3) -0.003(2) 0.001(2) -0.013(3) C51 0.045(3) 0.070(4) 0.022(3) 0.009(2) 0.011(2) -0.007(3) C52 0.075(5) 0.218(12) 0.031(3) -0.006(5) 0.012(3) -0.067(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C1 2.178(5) . ? Re1 C5 2.149(4) . ? Re1 C6 1.993(4) . ? Re1 C7 1.996(4) . ? Re1 C8 1.960(5) . ? Re1 C9 2.011(5) . ? O1 C21 1.198(5) . ? O2 C21 1.339(6) . ? O2 C22 1.447(5) . ? O3 C3 1.323(5) . ? O3 C31 1.450(5) . ? O5 C5 1.344(5) . ? O5 C51 1.470(6) . ? O6 C6 1.131(6) . ? O7 C7 1.139(6) . ? O8 C8 1.146(6) . ? O9 C9 1.118(6) . ? C1 C2 1.353(6) . ? C1 C11 1.507(6) . ? C2 C3 1.453(6) . ? C2 C21 1.511(6) . ? C3 C4 1.384(6) . ? C4 C5 1.391(6) . ? C11 C12 1.370(6) . ? C11 C20 1.417(6) . ? C12 C13 1.411(6) . ? C13 C14 1.370(7) . ? C14 C15 1.432(7) . ? C15 C16 1.415(6) . ? C15 C20 1.421(6) . ? C16 C17 1.348(7) . ? C17 C18 1.415(6) . ? C18 C19 1.368(6) . ? C19 C20 1.431(6) . ? C31 C32 1.499(7) . ? C32 C33 1.497(8) . ? C51 C52 1.474(8) . ? 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 C5 Re1 C1 86.07(17) . . ? C6 Re1 C1 95.57(18) . . ? C6 Re1 C5 90.14(17) . . ? C6 Re1 C7 88.82(18) . . ? C6 Re1 C9 178.34(17) . . ? C7 Re1 C1 90.72(17) . . ? C7 Re1 C5 176.51(17) . . ? C7 Re1 C9 91.84(18) . . ? C8 Re1 C1 173.69(17) . . ? C8 Re1 C5 90.37(18) . . ? C8 Re1 C6 89.6(2) . . ? C8 Re1 C7 92.95(18) . . ? C8 Re1 C9 91.8(2) . . ? C9 Re1 C1 82.91(19) . . ? C9 Re1 C5 89.11(17) . . ? C21 O2 C22 114.9(4) . . ? C3 O3 C31 122.1(3) . . ? C5 O5 C51 121.6(4) . . ? C2 C1 Re1 127.4(3) . . ? C2 C1 C11 115.8(4) . . ? C11 C1 Re1 116.5(3) . . ? C1 C2 C3 125.4(4) . . ? C1 C2 C21 121.4(4) . . ? C3 C2 C21 113.2(4) . . ? O3 C3 C2 110.7(4) . . ? O3 C3 C4 121.8(4) . . ? C4 C3 C2 127.5(4) . . ? C3 C4 C5 124.2(4) . . ? O5 C5 Re1 114.3(3) . . ? O5 C5 C4 117.0(4) . . ? C4 C5 Re1 128.7(3) . . ? O6 C6 Re1 178.1(4) . . ? O7 C7 Re1 178.8(4) . . ? O8 C8 Re1 178.8(4) . . ? O9 C9 Re1 177.1(4) . . ? C12 C11 C1 120.5(4) . . ? C12 C11 C20 118.7(4) . . ? C20 C11 C1 120.7(4) . . ? C11 C12 C13 122.2(4) . . ? C14 C13 C12 119.8(4) . . ? C13 C14 C15 120.3(4) . . ? C16 C15 C14 121.9(4) . . ? C16 C15 C20 119.5(4) . . ? C20 C15 C14 118.6(4) . . ? C17 C16 C15 121.4(4) . . ? C16 C17 C18 120.2(4) . . ? C19 C18 C17 120.3(4) . . ? C18 C19 C20 120.9(4) . . ? C11 C20 C15 120.3(4) . . ? C11 C20 C19 121.9(4) . . ? C15 C20 C19 117.7(4) . . ? O1 C21 O2 123.8(4) . . ? O1 C21 C2 124.5(4) . . ? O2 C21 C2 111.7(4) . . ? O3 C31 C32 107.4(4) . . ? C33 C32 C31 113.8(4) . . ? O5 C51 C52 108.3(5) . . ? data_cpd12_ran43cult _audit_creation_date 2014-06-19 _audit_creation_method ; Olex2 1.2-beta (compiled May 9 2012 12:37:22, GUI svn.r4230) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H7 N O8 Re' _chemical_formula_sum 'C32 H27 N O8 Re' _chemical_formula_weight 739.75 _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' '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' 'Re' 'Re' -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _space_group_IT_number 2 _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 7.5891(4) _cell_length_b 9.1757(5) _cell_length_c 22.2233(10) _cell_angle_alpha 79.342(4) _cell_angle_beta 88.070(4) _cell_angle_gamma 76.320(4) _cell_volume 1477.60(13) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4430 _cell_measurement_temperature 99.96(17) _cell_measurement_theta_max 74.7580 _cell_measurement_theta_min 5.0520 _exptl_absorpt_coefficient_mu 8.487 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.11974 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 730 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_unetI/netI 0.0687 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 7802 _diffrn_reflns_theta_full 66.50 _diffrn_reflns_theta_max 67.00 _diffrn_reflns_theta_min 5.05 _diffrn_ambient_temperature 99.96(17) _diffrn_detector_area_resol_mean 10.3587 _diffrn_measured_fraction_theta_full 0.9841 _diffrn_measured_fraction_theta_max 0.5266 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 59.00 96.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 178.0000 -60.0000 37 #__ type_ start__ end____ width___ exp.time_ 2 omega -47.00 12.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -40.6953 37.0000 0.0000 59 #__ type_ start__ end____ width___ exp.time_ 3 omega -110.00 -7.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -40.6953 -19.0000 0.0000 103 #__ type_ start__ end____ width___ exp.time_ 4 omega -47.00 35.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - -40.6953 37.0000 -180.0000 82 #__ type_ start__ end____ width___ exp.time_ 5 omega 95.00 121.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 40.6953 164.0000 165.0000 26 #__ type_ start__ end____ width___ exp.time_ 6 omega 24.00 97.00 1.0000 3.0000 omega____ theta____ kappa____ phi______ frames - 40.6953 -125.0000 -60.0000 73 #__ type_ start__ end____ width___ exp.time_ 7 omega 80.00 172.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 30.0000 90.0000 92 #__ type_ start__ end____ width___ exp.time_ 8 omega 37.00 73.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -30.0000 -180.0000 36 #__ type_ start__ end____ width___ exp.time_ 9 omega 38.00 144.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -77.0000 -30.0000 106 #__ type_ start__ end____ width___ exp.time_ 10 omega 87.00 178.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 45.0000 150.0000 91 #__ type_ start__ end____ width___ exp.time_ 11 omega 116.00 151.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 178.0000 -60.0000 35 #__ type_ start__ end____ width___ exp.time_ 12 omega 36.00 138.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -61.0000 90.0000 102 #__ type_ start__ end____ width___ exp.time_ 13 omega 36.00 115.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -111.0000 -60.0000 79 #__ type_ start__ end____ width___ exp.time_ 14 omega 41.00 66.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -30.0000 -30.0000 25 #__ type_ start__ end____ width___ exp.time_ 15 omega 43.00 87.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 110.5703 -30.0000 -120.0000 44 ; _diffrn_measurement_device 'kappa diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0515060000 _diffrn_orient_matrix_UB_12 -0.0521282000 _diffrn_orient_matrix_UB_13 -0.0616042000 _diffrn_orient_matrix_UB_21 0.1492849000 _diffrn_orient_matrix_UB_22 -0.1332138000 _diffrn_orient_matrix_UB_23 0.0325173000 _diffrn_orient_matrix_UB_31 -0.1367875000 _diffrn_orient_matrix_UB_32 -0.1020861000 _diffrn_orient_matrix_UB_33 0.0111591000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 0.80 _diffrn_source_power 0.040 _diffrn_source_target Cu _diffrn_source_voltage 50 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4569 _reflns_number_total 5075 _reflns_odcompleteness_completeness 98.41 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 68.13 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'J. Appl. Cryst. (2007) 40, 786-790' _refine_diff_density_max 2.776 _refine_diff_density_min -3.444 _refine_diff_density_rms 0.204 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 359 _refine_ls_number_reflns 5075 _refine_ls_number_restraints 219 _refine_ls_R_factor_all 0.0752 _refine_ls_R_factor_gt 0.0658 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0945P)^2^+13.6995P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1589 _refine_ls_wR_factor_ref 0.1662 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap 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 Re1 Re 0.54421(6) 0.93483(4) 0.160629(16) 0.03147(17) Uani 1 1 d DU . . O6 O 0.1387(10) 1.0389(10) 0.1132(4) 0.0491(19) Uani 1 1 d . . . O7 O 0.5170(9) 1.2560(7) 0.1893(3) 0.0355(15) Uani 1 1 d . . . O8 O 0.6981(9) 1.0030(8) 0.0298(3) 0.0388(13) Uani 1 1 d U . . O9 O 0.9426(13) 0.8297(11) 0.2109(5) 0.080(4) Uani 1 1 d . . . O31 O 0.8047(8) 0.4911(7) -0.0802(3) 0.0304(13) Uani 1 1 d U . . O41A O 0.659(4) 0.545(3) 0.3487(10) 0.024(7) Uiso 0.25 1 d PD A 2 O41 O 0.2657(16) 0.5137(12) 0.2494(5) 0.031(2) Uiso 0.75 1 d P A 1 O51 O 0.7297(14) 0.5960(12) 0.3319(5) 0.044(2) Uiso 0.75 1 d P A 1 O51A O 0.244(3) 0.577(3) 0.2148(10) 0.033(5) Uiso 0.25 1 d PD A 2 O52 O 0.654(2) 0.4471(18) 0.4162(7) 0.036(4) Uiso 0.50 1 d P A 1 O52A O 0.196(2) 0.391(2) 0.2828(8) 0.041(5) Uiso 0.50 1 d PD A 2 N1 N 0.5678(10) 0.5714(8) 0.1530(3) 0.0291(14) Uani 1 1 d U . . C1A C 0.505(3) 0.839(2) 0.2535(7) 0.031(4) Uiso 0.50 1 d PD A 2 C1 C 0.425(3) 0.830(2) 0.2470(7) 0.028(4) Uiso 0.50 1 d PD A 1 C2 C 0.4411(18) 0.6891(14) 0.2364(5) 0.020(2) Uiso 0.65 1 d PU A 1 C2A C 0.523(3) 0.695(3) 0.2449(10) 0.020(4) Uiso 0.35 1 d P A 2 C3 C 0.5279(12) 0.6944(10) 0.1758(4) 0.0269(14) Uani 1 1 d U A . C4 C 0.4029(16) 0.5533(14) 0.2757(5) 0.031(2) Uiso 0.75 1 d PU A 1 C4A C 0.546(5) 0.559(4) 0.2974(16) 0.032(7) Uiso 0.25 1 d P A 2 C5 C 0.4877(18) 0.4757(16) 0.3286(6) 0.036(3) Uiso 0.75 1 d PU A 1 C5A C 0.449(3) 0.453(4) 0.3040(13) 0.024(6) Uiso 0.25 1 d PD A 2 C6 C 0.2818(14) 0.9997(10) 0.1306(4) 0.032(2) Uani 1 1 d . A . C7 C 0.5312(12) 1.1405(10) 0.1763(4) 0.0299(18) Uani 1 1 d U A . C8 C 0.6376(13) 0.9776(10) 0.0769(4) 0.0308(15) Uani 1 1 d U A . C9 C 0.7997(19) 0.8646(11) 0.1932(5) 0.053(3) Uani 1 1 d . A . C11A C 0.4603(18) 0.9049(18) 0.3062(7) 0.025(3) Uiso 0.50 1 d PD A 2 C11 C 0.3283(19) 0.8638(19) 0.3081(7) 0.030(4) Uiso 0.50 1 d PD A 1 C12 C 0.1740(12) 0.8149(11) 0.3300(4) 0.038(2) Uani 1 1 d D . . C12A C 0.591(2) 0.9839(19) 0.3191(8) 0.023(4) Uiso 0.50 1 d PD A 2 C13 C 0.063(3) 0.848(2) 0.3793(7) 0.037(5) Uiso 0.50 1 d PD A 1 C13A C 0.575(2) 1.051(2) 0.3730(6) 0.020(4) Uiso 0.50 1 d PD A 2 C14A C 0.4331(18) 1.0355(19) 0.4146(7) 0.029(3) Uiso 0.50 1 d PD A 2 C14 C 0.126(2) 0.937(3) 0.4153(10) 0.046(5) Uiso 0.50 1 d PD A 1 C15 C 0.2951(11) 0.9686(11) 0.3998(4) 0.035(2) Uani 1 1 d D . . C16A C 0.155(2) 0.940(2) 0.4418(9) 0.041(5) Uiso 0.50 1 d PD A 2 C16 C 0.350(3) 1.068(2) 0.4353(9) 0.048(5) Uiso 0.50 1 d PD A 1 C17A C 0.024(2) 0.864(2) 0.4278(7) 0.033(4) Uiso 0.50 1 d PD A 2 C17 C 0.514(2) 1.114(3) 0.4243(9) 0.047(5) Uiso 0.50 1 d PD A 1 C18 C 0.623(3) 1.077(3) 0.3742(8) 0.043(6) Uiso 0.50 1 d PD A 1 C18A C 0.032(2) 0.805(3) 0.3721(7) 0.035(4) Uiso 0.50 1 d PD A 2 C19 C 0.556(2) 0.995(2) 0.3356(10) 0.031(5) Uiso 0.50 1 d PD A 1 C20A C 0.3120(16) 0.8897(16) 0.3472(5) 0.019(3) Uiso 0.50 1 d PD A 2 C20 C 0.3920(19) 0.9472(19) 0.3463(6) 0.029(3) Uiso 0.50 1 d PD A 1 C31 C 0.6367(11) 0.5549(10) 0.0940(4) 0.0243(15) Uani 1 1 d U A . C32 C 0.7640(11) 0.4211(9) 0.0872(4) 0.0256(15) Uani 1 1 d U . . H32 H 0.8098 0.3473 0.1224 0.031 Uiso 1 1 calc R A . C33 C 0.8237(11) 0.3950(9) 0.0299(4) 0.0242(14) Uani 1 1 d U A . H33 H 0.9074 0.3027 0.0255 0.029 Uiso 1 1 calc R . . C34 C 0.7600(10) 0.5057(9) -0.0213(4) 0.0215(14) Uani 1 1 d U . . C35 C 0.6367(11) 0.6423(9) -0.0147(4) 0.0228(14) Uani 1 1 d U A . H35 H 0.5960 0.7186 -0.0497 0.027 Uiso 1 1 calc R . . C36 C 0.5750(10) 0.6656(9) 0.0425(4) 0.0232(14) Uani 1 1 d U . . H36 H 0.4902 0.7574 0.0469 0.028 Uiso 1 1 calc R A . C37 C 0.9133(13) 0.3477(11) -0.0895(4) 0.035(2) Uani 1 1 d . . . H37A H 0.9274 0.3479 -0.1335 0.052 Uiso 1 1 calc R A . H37B H 0.8544 0.2662 -0.0710 0.052 Uiso 1 1 calc R . . H37C H 1.0329 0.3303 -0.0705 0.052 Uiso 1 1 calc R . . C41 C 0.198(3) 0.360(3) 0.2730(11) 0.034(6) Uiso 0.50 1 d P A 1 C41A C 0.688(3) 0.424(2) 0.4025(9) 0.028(5) Uiso 0.50 1 d PD A 2 C42 C 0.047(4) 0.361(3) 0.2326(14) 0.042(8) Uiso 0.50 1 d P A 1 C42A C 0.824(4) 0.463(3) 0.4404(12) 0.044(6) Uiso 0.50 1 d P A 2 C43A C 0.739(6) 0.602(5) 0.4746(18) 0.064(11) Uiso 0.50 1 d P A 2 C43 C -0.020(3) 0.227(3) 0.2594(11) 0.037(5) Uiso 0.50 1 d P A 1 C51 C 0.634(3) 0.509(3) 0.3554(10) 0.057(6) Uiso 0.75 1 d PU A 1 C51A C 0.297(4) 0.494(3) 0.2590(12) 0.06(2) Uiso 0.25 1 d PD A 2 C52A C 0.045(3) 0.384(3) 0.2444(10) 0.023(5) Uiso 0.50 1 d P A 2 C52 C 0.780(3) 0.486(3) 0.4535(11) 0.040(6) Uiso 0.50 1 d P A 1 C53A C -0.044(3) 0.252(3) 0.2752(12) 0.038(6) Uiso 0.50 1 d P A 2 C53 C 0.695(6) 0.631(5) 0.4728(19) 0.069(12) Uiso 0.50 1 d P A 1 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 Re1 0.0535(3) 0.0104(2) 0.0309(2) -0.00511(14) -0.01515(17) -0.00497(17) O6 0.030(4) 0.059(5) 0.067(5) -0.018(4) -0.006(3) -0.021(4) O7 0.049(4) 0.013(3) 0.049(4) -0.013(3) -0.007(3) -0.012(3) O8 0.041(2) 0.031(2) 0.044(2) -0.0018(19) -0.0022(18) -0.013(2) O9 0.070(6) 0.066(6) 0.092(7) -0.037(5) -0.058(6) 0.032(5) O31 0.035(3) 0.030(3) 0.030(2) -0.011(2) 0.006(2) -0.013(3) N1 0.040(3) 0.016(2) 0.033(3) -0.006(2) 0.009(2) -0.011(2) C3 0.033(2) 0.0210(19) 0.029(2) -0.0058(16) 0.0027(17) -0.0105(17) C6 0.051(6) 0.017(4) 0.035(4) -0.010(3) 0.008(4) -0.017(4) C7 0.036(4) 0.025(4) 0.036(3) -0.017(3) -0.010(3) -0.012(3) C8 0.037(3) 0.018(3) 0.042(3) -0.003(2) -0.008(2) -0.017(3) C9 0.082(9) 0.017(5) 0.058(6) -0.018(4) -0.034(6) 0.009(5) C12 0.045(5) 0.028(5) 0.034(5) 0.002(4) 0.002(4) -0.002(4) C15 0.031(4) 0.052(6) 0.025(4) -0.009(4) 0.002(3) -0.013(4) C31 0.026(3) 0.024(3) 0.027(2) -0.008(2) 0.004(2) -0.011(2) C32 0.030(3) 0.021(3) 0.028(2) -0.004(2) 0.000(2) -0.010(2) C33 0.024(3) 0.021(3) 0.030(2) -0.008(2) 0.000(2) -0.008(2) C34 0.023(3) 0.020(3) 0.027(2) -0.007(2) 0.002(2) -0.013(2) C35 0.024(3) 0.020(3) 0.027(2) -0.005(2) 0.000(2) -0.011(2) C36 0.021(3) 0.022(3) 0.029(3) -0.007(2) 0.000(2) -0.009(2) C37 0.043(5) 0.030(5) 0.038(5) -0.013(4) 0.007(4) -0.016(4) _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 Re1 C1A 2.129(14) . ? Re1 C1 2.246(14) . ? Re1 C3 2.201(9) . ? Re1 C6 2.036(11) . ? Re1 C7 1.961(9) . ? Re1 C8 1.972(9) . ? Re1 C9 2.007(12) . ? O6 C6 1.118(13) . ? O7 C7 1.129(11) . ? O8 C8 1.135(12) . ? O9 C9 1.119(15) . ? O31 C34 1.365(10) . ? O31 C37 1.425(11) . ? O41A C4A 1.42(5) . ? O41A C41A 1.455(18) . ? O41 C4 1.363(16) . ? O41 C41 1.61(3) . ? O51 C51 1.24(3) . ? O51A C51A 1.15(2) . ? O52 C51 1.36(3) . ? O52 C52 1.43(3) . ? O52A C51A 1.37(2) . ? O52A C52A 1.48(3) . ? N1 C3 1.289(11) . ? N1 C31 1.416(10) . ? C1A C2A 1.35(3) . ? C1A C11A 1.41(2) . ? C1 C2 1.33(2) . ? C1 C11 1.57(2) . ? C2 C3 1.478(13) . ? C2 C4 1.467(17) . ? C2A C3 1.53(2) . ? C2A C4A 1.53(4) . ? C4 C5 1.352(18) . ? C4A C5A 1.33(5) . ? C5 C51 1.40(3) . ? C5A C51A 1.481(19) . ? C11A C12A 1.422(13) . ? C11A C20A 1.440(12) . ? C11 C12 1.392(12) . ? C11 C20 1.408(13) . ? C12 C13 1.392(13) . ? C12 C18A 1.411(13) . ? C12 C20A 1.475(11) . ? C12A C13A 1.433(13) . ? C13 C14 1.409(15) . ? C13A C14A 1.412(13) . ? C14A C15 1.408(12) . ? C14 C15 1.403(13) . ? C15 C16A 1.429(13) . ? C15 C16 1.445(13) . ? C15 C20A 1.473(11) . ? C15 C20 1.397(11) . ? C16A C17A 1.421(14) . ? C16 C17 1.409(14) . ? C17A C18A 1.431(14) . ? C17 C18 1.409(14) . ? C18 C19 1.417(14) . ? C19 C20 1.413(13) . ? C31 C32 1.401(12) . ? C31 C36 1.395(12) . ? C32 C33 1.379(11) . ? C33 C34 1.392(11) . ? C34 C35 1.404(11) . ? C35 C36 1.377(11) . ? C41 C42 1.48(4) . ? C41A C42A 1.50(3) . ? C42 C43 1.46(4) . ? C42A C43A 1.60(5) . ? C52A C53A 1.56(3) . ? C52 C53 1.47(5) . ? 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 C1A Re1 C1 17.1(6) . . ? C1A Re1 C3 65.5(6) . . ? C3 Re1 C1 59.3(5) . . ? C6 Re1 C1A 99.8(6) . . ? C6 Re1 C1 83.8(6) . . ? C6 Re1 C3 89.7(3) . . ? C7 Re1 C1A 95.1(6) . . ? C7 Re1 C1 101.1(5) . . ? C7 Re1 C3 160.3(4) . . ? C7 Re1 C6 90.4(3) . . ? C7 Re1 C8 94.2(4) . . ? C7 Re1 C9 90.6(4) . . ? C8 Re1 C1A 164.6(6) . . ? C8 Re1 C1 164.2(6) . . ? C8 Re1 C3 105.5(3) . . ? C8 Re1 C6 92.4(4) . . ? C8 Re1 C9 89.7(5) . . ? C9 Re1 C1A 77.9(7) . . ? C9 Re1 C1 93.8(7) . . ? C9 Re1 C3 88.5(4) . . ? C9 Re1 C6 177.6(4) . . ? C34 O31 C37 116.9(7) . . ? C4A O41A C41A 127(3) . . ? C4 O41 C41 124.6(14) . . ? C51 O52 C52 120.9(18) . . ? C51A O52A C52A 116.5(18) . . ? C3 N1 C31 127.5(8) . . ? C2A C1A Re1 96.6(12) . . ? C2A C1A C11A 131.0(16) . . ? C11A C1A Re1 132.2(13) . . ? C2 C1 Re1 100.2(10) . . ? C2 C1 C11 115.7(13) . . ? C11 C1 Re1 143.9(12) . . ? C1 C2 C3 103.0(11) . . ? C1 C2 C4 130.7(11) . . ? C4 C2 C3 126.0(10) . . ? C1A C2A C3 108.7(16) . . ? C1A C2A C4A 123(2) . . ? C4A C2A C3 128(2) . . ? N1 C3 Re1 144.1(6) . . ? N1 C3 C2 118.4(8) . . ? N1 C3 C2A 123.4(11) . . ? C2 C3 Re1 97.5(6) . . ? C2 C3 C2A 25.7(8) . . ? C2A C3 Re1 88.3(10) . . ? O41 C4 C2 108.3(11) . . ? C5 C4 O41 124.2(13) . . ? C5 C4 C2 127.5(13) . . ? O41A C4A C2A 121(3) . . ? C5A C4A O41A 113(3) . . ? C5A C4A C2A 125(3) . . ? C4 C5 C51 125.6(15) . . ? C4A C5A C51A 112(3) . . ? O6 C6 Re1 178.1(9) . . ? O7 C7 Re1 174.8(8) . . ? O8 C8 Re1 177.0(8) . . ? O9 C9 Re1 178.0(11) . . ? C1A C11A C12A 111.7(14) . . ? C1A C11A C20A 127.4(14) . . ? C12A C11A C20A 120.7(13) . . ? C12 C11 C1 124.0(13) . . ? C12 C11 C20 113.7(12) . . ? C20 C11 C1 122.3(12) . . ? C11 C12 C13 130.8(13) . . ? C11 C12 C18A 153.3(13) . . ? C11 C12 C20A 38.1(8) . . ? C13 C12 C18A 22.7(10) . . ? C13 C12 C20A 93.6(11) . . ? C18A C12 C20A 115.5(11) . . ? C11A C12A C13A 120.3(17) . . ? C12 C13 C14 114.2(16) . . ? C14A C13A C12A 120.3(17) . . ? C15 C14A C13A 119.8(14) . . ? C15 C14 C13 116.1(16) . . ? C14A C15 C16A 122.3(11) . . ? C14A C15 C16 32.6(9) . . ? C14A C15 C20A 121.1(9) . . ? C14 C15 C14A 146.7(12) . . ? C14 C15 C16A 26.2(9) . . ? C14 C15 C16 114.6(13) . . ? C14 C15 C20A 92.2(11) . . ? C16A C15 C16 92.6(12) . . ? C16A C15 C20A 114.9(11) . . ? C16 C15 C20A 152.5(11) . . ? C20 C15 C14A 86.0(10) . . ? C20 C15 C14 126.9(12) . . ? C20 C15 C16A 151.0(12) . . ? C20 C15 C16 116.4(11) . . ? C20 C15 C20A 36.1(7) . . ? C17A C16A C15 121.7(16) . . ? C17 C16 C15 121.8(17) . . ? C16A C17A C18A 120.9(16) . . ? C16 C17 C18 121(2) . . ? C17 C18 C19 117(2) . . ? C12 C18A C17A 122.0(16) . . ? C20 C19 C18 123(2) . . ? C11A C20A C12 118.7(10) . . ? C11A C20A C15 117.0(10) . . ? C15 C20A C12 123.7(9) . . ? C11 C20 C19 122.8(13) . . ? C15 C20 C11 116.9(11) . . ? C15 C20 C19 120.0(13) . . ? C32 C31 N1 119.0(7) . . ? C36 C31 N1 121.5(7) . . ? C36 C31 C32 119.4(7) . . ? C33 C32 C31 120.9(8) . . ? C32 C33 C34 119.2(7) . . ? O31 C34 C33 124.6(7) . . ? O31 C34 C35 115.0(7) . . ? C33 C34 C35 120.4(7) . . ? C36 C35 C34 119.9(7) . . ? C35 C36 C31 120.2(7) . . ? C42 C41 O41 107.5(19) . . ? O41A C41A C42A 104(2) . . ? C43 C42 C41 105(2) . . ? C41A C42A C43A 113(2) . . ? O51 C51 O52 119.5(19) . . ? O51 C51 C5 127.6(19) . . ? O52 C51 C5 112.6(19) . . ? O51A C51A O52A 117(2) . . ? O51A C51A C5A 142(3) . . ? O52A C51A C5A 101.5(19) . . ? O52A C52A C53A 109.9(17) . . ? O52 C52 C53 109(2) . . ? 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 Re1 C1A C2A C3 -8.9(19) . . . . ? Re1 C1A C2A C4A 168(2) . . . . ? Re1 C1A C11A C12A -60(2) . . . . ? Re1 C1A C11A C20A 125.1(19) . . . . ? Re1 C1 C2 C3 0.7(13) . . . . ? Re1 C1 C2 C4 174.8(13) . . . . ? Re1 C1 C11 C12 132.9(19) . . . . ? Re1 C1 C11 C20 -48(3) . . . . ? O31 C34 C35 C36 176.6(7) . . . . ? O41A C4A C5A C51A 164(2) . . . . ? O41A C41A C42A C43A 75(3) . . . . ? O41 C4 C5 C51 177.0(15) . . . . ? O41 C41 C42 C43 -174.9(19) . . . . ? N1 C31 C32 C33 174.9(8) . . . . ? N1 C31 C36 C35 -176.2(8) . . . . ? C1A Re1 C1 C2 -107(3) . . . . ? C1A Re1 C1 C11 77(3) . . . . ? C1A Re1 C3 N1 -159.3(14) . . . . ? C1A Re1 C3 C2 18.4(9) . . . . ? C1A Re1 C3 C2A -5.6(12) . . . . ? C1A Re1 C6 O6 139(25) . . . . ? C1A Re1 C7 O7 -21(9) . . . . ? C1A Re1 C8 O8 -61(16) . . . . ? C1A Re1 C9 O9 -118(33) . . . . ? C1A C2A C3 Re1 8.5(18) . . . . ? C1A C2A C3 N1 170.4(15) . . . . ? C1A C2A C3 C2 -103(3) . . . . ? C1A C2A C4A O41A -41(4) . . . . ? C1A C2A C4A C5A 130(4) . . . . ? C1A C11A C12A C13A -176.1(15) . . . . ? C1A C11A C20A C12 -9(2) . . . . ? C1A C11A C20A C15 179.1(15) . . . . ? C1 Re1 C1A C2A 71(3) . . . . ? C1 Re1 C1A C11A -104(3) . . . . ? C1 Re1 C3 N1 -177.3(14) . . . . ? C1 Re1 C3 C2 0.5(9) . . . . ? C1 Re1 C3 C2A -23.6(12) . . . . ? C1 Re1 C6 O6 144(26) . . . . ? C1 Re1 C7 O7 -5(9) . . . . ? C1 Re1 C8 O8 -129(15) . . . . ? C1 Re1 C9 O9 -124(33) . . . . ? C1 C2 C3 Re1 -0.7(13) . . . . ? C1 C2 C3 N1 177.8(12) . . . . ? C1 C2 C3 C2A 69(3) . . . . ? C1 C2 C4 O41 116.3(19) . . . . ? C1 C2 C4 C5 -65(2) . . . . ? C1 C11 C12 C13 -172.7(16) . . . . ? C1 C11 C12 C18A -177(2) . . . . ? C1 C11 C12 C20A 173(2) . . . . ? C1 C11 C20 C15 -179.3(14) . . . . ? C1 C11 C20 C19 -6(3) . . . . ? C2 C1 C11 C12 -42(2) . . . . ? C2 C1 C11 C20 137.7(18) . . . . ? C2 C4 C5 C51 -2(2) . . . . ? C2A C1A C11A C12A 127(3) . . . . ? C2A C1A C11A C20A -48(3) . . . . ? C2A C4A C5A C51A -8(4) . . . . ? C3 Re1 C1A C2A 6.4(14) . . . . ? C3 Re1 C1A C11A -169(2) . . . . ? C3 Re1 C1 C2 -0.5(10) . . . . ? C3 Re1 C1 C11 -176(3) . . . . ? C3 Re1 C6 O6 -156(25) . . . . ? C3 Re1 C7 O7 -11(9) . . . . ? C3 Re1 C8 O8 -114(15) . . . . ? C3 Re1 C9 O9 177(100) . . . . ? C3 N1 C31 C32 143.4(9) . . . . ? C3 N1 C31 C36 -39.3(14) . . . . ? C3 C2 C4 O41 -70.8(15) . . . . ? C3 C2 C4 C5 108.1(16) . . . . ? C3 C2A C4A O41A 135(3) . . . . ? C3 C2A C4A C5A -54(5) . . . . ? C4 O41 C41 C42 179.5(16) . . . . ? C4 C2 C3 Re1 -175.2(12) . . . . ? C4 C2 C3 N1 3.3(18) . . . . ? C4 C2 C3 C2A -105(3) . . . . ? C4 C5 C51 O51 -13(3) . . . . ? C4 C5 C51 O52 160.1(16) . . . . ? C4A O41A C41A C42A 178(3) . . . . ? C4A C2A C3 Re1 -168(3) . . . . ? C4A C2A C3 N1 -6(3) . . . . ? C4A C2A C3 C2 81(3) . . . . ? C4A C5A C51A O51A 13(4) . . . . ? C4A C5A C51A O52A -167(3) . . . . ? C6 Re1 C1A C2A 91.6(15) . . . . ? C6 Re1 C1A C11A -83.4(19) . . . . ? C6 Re1 C1 C2 92.9(12) . . . . ? C6 Re1 C1 C11 -82(2) . . . . ? C6 Re1 C3 N1 99.8(12) . . . . ? C6 Re1 C3 C2 -82.5(7) . . . . ? C6 Re1 C3 C2A -106.5(10) . . . . ? C6 Re1 C7 O7 79(9) . . . . ? C6 Re1 C8 O8 156(15) . . . . ? C6 Re1 C9 O9 -139(30) . . . . ? C7 Re1 C1A C2A -177.0(15) . . . . ? C7 Re1 C1A C11A 7.9(19) . . . . ? C7 Re1 C1 C2 -177.9(11) . . . . ? C7 Re1 C1 C11 7(2) . . . . ? C7 Re1 C3 N1 -169.6(10) . . . . ? C7 Re1 C3 C2 8.1(14) . . . . ? C7 Re1 C3 C2A -15.9(15) . . . . ? C7 Re1 C6 O6 43(25) . . . . ? C7 Re1 C8 O8 65(15) . . . . ? C7 Re1 C9 O9 -23(33) . . . . ? C8 Re1 C1A C2A -50(3) . . . . ? C8 Re1 C1A C11A 134.5(18) . . . . ? C8 Re1 C1 C2 16(3) . . . . ? C8 Re1 C1 C11 -159.0(15) . . . . ? C8 Re1 C3 N1 7.4(12) . . . . ? C8 Re1 C3 C2 -174.9(7) . . . . ? C8 Re1 C3 C2A 161.1(10) . . . . ? C8 Re1 C6 O6 -51(25) . . . . ? C8 Re1 C7 O7 172(9) . . . . ? C8 Re1 C9 O9 71(33) . . . . ? C9 Re1 C1A C2A -87.5(15) . . . . ? C9 Re1 C1A C11A 97.5(19) . . . . ? C9 Re1 C1 C2 -86.5(12) . . . . ? C9 Re1 C1 C11 98(2) . . . . ? C9 Re1 C3 N1 -81.9(12) . . . . ? C9 Re1 C3 C2 95.8(8) . . . . ? C9 Re1 C3 C2A 71.8(10) . . . . ? C9 Re1 C6 O6 160(23) . . . . ? C9 Re1 C7 O7 -99(9) . . . . ? C9 Re1 C8 O8 -25(15) . . . . ? C11A C1A C2A C3 166.2(19) . . . . ? C11A C1A C2A C4A -17(4) . . . . ? C11A C12A C13A C14A 2(3) . . . . ? C11 C1 C2 C3 177.5(13) . . . . ? C11 C1 C2 C4 -8(3) . . . . ? C11 C12 C13 C14 -5(3) . . . . ? C11 C12 C18A C17A -7(4) . . . . ? C11 C12 C20A C11A -4.5(15) . . . . ? C11 C12 C20A C15 167(2) . . . . ? C12 C11 C20 C15 0(2) . . . . ? C12 C11 C20 C19 173.8(15) . . . . ? C12 C13 C14 C15 -5(3) . . . . ? C12A C11A C20A C12 176.4(14) . . . . ? C12A C11A C20A C15 4(2) . . . . ? C12A C13A C14A C15 -7(2) . . . . ? C13 C12 C18A C17A -16(3) . . . . ? C13 C12 C20A C11A -173.5(15) . . . . ? C13 C12 C20A C15 -2.1(16) . . . . ? C13 C14 C15 C14A -176(2) . . . . ? C13 C14 C15 C16A -148(4) . . . . ? C13 C14 C15 C16 176.4(18) . . . . ? C13 C14 C15 C20A 3(2) . . . . ? C13 C14 C15 C20 13(3) . . . . ? C13A C14A C15 C14 -171(2) . . . . ? C13A C14A C15 C16A 175.5(16) . . . . ? C13A C14A C15 C16 -157(3) . . . . ? C13A C14A C15 C20A 11(2) . . . . ? C13A C14A C15 C20 2.2(17) . . . . ? C14A C15 C16A C17A -175.8(17) . . . . ? C14A C15 C16 C17 9.8(18) . . . . ? C14A C15 C20A C11A -9.7(19) . . . . ? C14A C15 C20A C12 178.8(12) . . . . ? C14A C15 C20 C11 174.3(16) . . . . ? C14A C15 C20 C19 0.5(18) . . . . ? C14 C15 C16A C17A 22(2) . . . . ? C14 C15 C16 C17 -178(2) . . . . ? C14 C15 C20A C11A 171.2(15) . . . . ? C14 C15 C20A C12 -0.4(17) . . . . ? C14 C15 C20 C11 -11(2) . . . . ? C14 C15 C20 C19 175.6(18) . . . . ? C15 C16A C17A C18A 3(3) . . . . ? C15 C16 C17 C18 6(3) . . . . ? C16A C15 C16 C17 167(2) . . . . ? C16A C15 C20A C11A -175.3(14) . . . . ? C16A C15 C20A C12 13.2(19) . . . . ? C16A C15 C20 C11 6(4) . . . . ? C16A C15 C20 C19 -168(2) . . . . ? C16A C17A C18A C12 3(3) . . . . ? C16 C15 C16A C17A 170(2) . . . . ? C16 C15 C20A C11A 4(3) . . . . ? C16 C15 C20A C12 -168(2) . . . . ? C16 C15 C20 C11 -173.6(16) . . . . ? C16 C15 C20 C19 13(2) . . . . ? C16 C17 C18 C19 1(3) . . . . ? C17 C18 C19 C20 -2(3) . . . . ? C18 C19 C20 C11 -179.2(19) . . . . ? C18 C19 C20 C15 -6(3) . . . . ? C18A C12 C13 C14 169(5) . . . . ? C18A C12 C20A C11A -179.6(14) . . . . ? C18A C12 C20A C15 -8.2(19) . . . . ? C20A C11A C12A C13A -1(2) . . . . ? C20A C12 C13 C14 3.7(19) . . . . ? C20A C12 C18A C17A 0(2) . . . . ? C20A C15 C16A C17A -10(2) . . . . ? C20A C15 C16 C17 -12(4) . . . . ? C20A C15 C20 C11 7.0(13) . . . . ? C20A C15 C20 C19 -167(3) . . . . ? C20 C11 C12 C13 8(2) . . . . ? C20 C11 C12 C18A 3(4) . . . . ? C20 C11 C12 C20A -6.9(12) . . . . ? C20 C15 C16A C17A -10(4) . . . . ? C20 C15 C16 C17 -13(3) . . . . ? C20 C15 C20A C11A 5.3(14) . . . . ? C20 C15 C20A C12 -166(2) . . . . ? C31 N1 C3 Re1 -8.3(18) . . . . ? C31 N1 C3 C2 174.3(9) . . . . ? C31 N1 C3 C2A -156.3(14) . . . . ? C31 C32 C33 C34 1.9(13) . . . . ? C32 C31 C36 C35 1.0(13) . . . . ? C32 C33 C34 O31 -177.9(8) . . . . ? C32 C33 C34 C35 0.2(12) . . . . ? C33 C34 C35 C36 -1.6(12) . . . . ? C34 C35 C36 C31 1.0(12) . . . . ? C36 C31 C32 C33 -2.5(13) . . . . ? C37 O31 C34 C33 4.9(12) . . . . ? C37 O31 C34 C35 -173.2(7) . . . . ? C41 O41 C4 C2 172.2(14) . . . . ? C41 O41 C4 C5 -7(2) . . . . ? C41A O41A C4A C2A 178(3) . . . . ? C41A O41A C4A C5A 5(5) . . . . ? C51 O52 C52 C53 82(3) . . . . ? C51A O52A C52A C53A 175(2) . . . . ? C52A O52A C51A O51A 9(3) . . . . ? C52A O52A C51A C5A -172(2) . . . . ? C52 O52 C51 O51 2(3) . . . . ? C52 O52 C51 C5 -171.3(19) . . . . ?